data_L(salben)Ba _audit_creation_date 2019-08-07 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2014/7' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C27 H33 Ba F6 N3 O12 S2' _chemical_formula_sum 'C27 H33 Ba F6 N3 O12 S2' _chemical_formula_weight 907.02 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ba' 'Ba' -1.0456 8.4617 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'orthorhombic' _space_group_IT_number 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.9261(6) _cell_length_b 17.1581(9) _cell_length_c 37.691(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7065.9(7) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9239 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 68.509 _cell_measurement_theta_min 4.678 _shelx_estimated_absorpt_T_max 0.740 _shelx_estimated_absorpt_T_min 0.326 _exptl_absorpt_coefficient_mu 10.704 _exptl_absorpt_correction_T_max 0.7531 _exptl_absorpt_correction_T_min 0.4050 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1297 before and 0.0817 after correction. The Ratio of minimum to maximum transmission is 0.5378. The \l/2 correction factor is 0.00150.' _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description 'Square' _exptl_crystal_F_000 3632 _exptl_crystal_size_max 0.135 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_unetI/netI 0.0429 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_number 39237 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_theta_full 66.000 _diffrn_reflns_theta_max 68.503 _diffrn_reflns_theta_min 4.678 _diffrn_ambient_temperature 199.99 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'Bruker Platinum 135 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'Bruker MicroStar microfocus rotating anode' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 5820 _reflns_number_total 6423 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _refine_diff_density_max 0.573 _refine_diff_density_min -0.949 _refine_diff_density_rms 0.083 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 592 _refine_ls_number_reflns 6423 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0370 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+7.9915P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0980 _refine_ls_wR_factor_ref 0.1008 _refine_special_details ? _olex2_refinement_description ; ; _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary ? _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ba Ba 0.11052(2) 0.39333(2) 0.36003(2) 0.03716(9) Uani 1 1 d . . . . . O2 O -0.0382(2) 0.39844(13) 0.41696(7) 0.0394(5) Uani 1 1 d . . . . . O1 O 0.0101(2) 0.53202(13) 0.34323(6) 0.0365(5) Uani 1 1 d . . . . . N3 N -0.0914(3) 0.6395(2) 0.42488(8) 0.0438(7) Uani 1 1 d . . . . . C22 C -0.1074(4) 0.6275(3) 0.46291(11) 0.0516(10) Uani 1 1 d . . . . . H22A H -0.124(4) 0.672(3) 0.4753(12) 0.049(12) Uiso 1 1 d . . . . . H22B H -0.021(5) 0.608(2) 0.4713(13) 0.066(15) Uiso 1 1 d . . . . . C21 C -0.2090(4) 0.5698(3) 0.46990(11) 0.0514(9) Uani 1 1 d . . . . . H21A H -0.229(4) 0.563(3) 0.4955(12) 0.061(13) Uiso 1 1 d . . . . . H21B H -0.283(5) 0.587(3) 0.4550(15) 0.086(17) Uiso 1 1 d . . . . . N2 N -0.1703(3) 0.49143(19) 0.45847(8) 0.0445(7) Uani 1 1 d . . . . . H2 H -0.127(4) 0.489(2) 0.4381(12) 0.048(11) Uiso 1 1 d . . . . . C20 C -0.1870(4) 0.4292(2) 0.47746(10) 0.0465(9) Uani 1 1 d . . . . . H20 H -0.233(4) 0.436(2) 0.4993(10) 0.042(10) Uiso 1 1 d . . . . . C17 C -0.1569(5) 0.2941(3) 0.49446(11) 0.0558(11) Uani 1 1 d . . . . . H17 H -0.203(4) 0.304(2) 0.5138(11) 0.043(11) Uiso 1 1 d . . . . . C16 C -0.0991(5) 0.2252(3) 0.49108(12) 0.0603(13) Uani 1 1 d . . . . . H16 H -0.106(4) 0.185(3) 0.5071(15) 0.074(16) Uiso 1 1 d . . . . . C15 C -0.0211(4) 0.2119(2) 0.46160(12) 0.0544(11) Uani 1 1 d . . . . . H15 H 0.020(4) 0.166(3) 0.4581(12) 0.058(13) Uiso 1 1 d . . . . . C14 C -0.0060(3) 0.2686(2) 0.43624(10) 0.0426(8) Uani 1 1 d . . . . . O3 O 0.0599(2) 0.25898(14) 0.40559(7) 0.0471(6) Uani 1 1 d . . . . . C13 C 0.1186(4) 0.1845(3) 0.40017(15) 0.0595(12) Uani 1 1 d . . . . . H13A H 0.061(5) 0.142(4) 0.4084(14) 0.080(16) Uiso 1 1 d . . . . . H13B H 0.187(5) 0.189(3) 0.4178(13) 0.068(14) Uiso 1 1 d . . . . . C12 C 0.1513(5) 0.1771(3) 0.36234(14) 0.0617(12) Uani 1 1 d . . . . . H12A H 0.193(5) 0.126(3) 0.3577(12) 0.072(16) Uiso 1 1 d . . . . . H12B H 0.077(4) 0.174(2) 0.3479(11) 0.041(10) Uiso 1 1 d . . . . . O4 O 0.2265(3) 0.24064(16) 0.35271(7) 0.0527(7) Uani 1 1 d . . . . . C11 C 0.2800(6) 0.2297(3) 0.31884(15) 0.0739(15) Uani 1 1 d . . . . . H11A H 0.207(6) 0.237(4) 0.3019(16) 0.11(2) Uiso 1 1 d . . . . . H11B H 0.311(6) 0.181(4) 0.3167(16) 0.10(2) Uiso 1 1 d . . . . . C10 C 0.3732(4) 0.2909(3) 0.31262(14) 0.0634(12) Uani 1 1 d . . . . . H10A H 0.437(5) 0.287(3) 0.3312(15) 0.086(17) Uiso 1 1 d . . . . . H10B H 0.406(5) 0.284(3) 0.2886(15) 0.076(16) Uiso 1 1 d . . . . . C18 C -0.1374(4) 0.3557(2) 0.46964(10) 0.0438(8) Uani 1 1 d . . . . . C19 C -0.0599(3) 0.3441(2) 0.43951(9) 0.0390(8) Uani 1 1 d . . . . . O5 O 0.3144(3) 0.36262(19) 0.31564(9) 0.0670(9) Uani 1 1 d . . . . . C9 C 0.3782(4) 0.4275(3) 0.30009(14) 0.0592(11) Uani 1 1 d . . . . . H9A H 0.443(5) 0.406(3) 0.2846(14) 0.066(14) Uiso 1 1 d . . . . . H9B H 0.413(4) 0.456(3) 0.3186(14) 0.065(15) Uiso 1 1 d . . . . . C8 C 0.2901(4) 0.4711(3) 0.27814(11) 0.0501(9) Uani 1 1 d . . . . . H8A H 0.332(4) 0.515(3) 0.2680(12) 0.056(12) Uiso 1 1 d . . . . . H8B H 0.261(4) 0.438(3) 0.2579(12) 0.060(13) Uiso 1 1 d . . . . . O21 O -0.0783(3) 0.28350(18) 0.33134(8) 0.0607(8) Uani 1 1 d . . . . . O22 O -0.0482(3) 0.39325(15) 0.29342(8) 0.0550(7) Uani 1 1 d . . . . . O23 O -0.1922(3) 0.29243(17) 0.27630(8) 0.0597(7) Uani 1 1 d . . . . . O6 O 0.1921(2) 0.49464(14) 0.30105(6) 0.0409(5) Uani 1 1 d . . . . . C6 C 0.1055(3) 0.5439(2) 0.28704(9) 0.0370(7) Uani 1 1 d . . . . . C7 C 0.0104(3) 0.56233(18) 0.31188(8) 0.0334(7) Uani 1 1 d . . . . . C5 C 0.1075(4) 0.5751(2) 0.25383(10) 0.0441(9) Uani 1 1 d . . . . . H5 H 0.167(4) 0.562(3) 0.2397(13) 0.063(14) Uiso 1 1 d . . . . . C4 C 0.0181(4) 0.6287(2) 0.24280(10) 0.0483(9) Uani 1 1 d . . . . . H4 H 0.024(4) 0.654(2) 0.2186(11) 0.044(10) Uiso 1 1 d . . . . . C3 C -0.0738(4) 0.6494(2) 0.26547(10) 0.0441(8) Uani 1 1 d . . . . . H3 H -0.133(4) 0.685(3) 0.2594(12) 0.053(12) Uiso 1 1 d . . . . . C2 C -0.0793(4) 0.61689(19) 0.29988(10) 0.0371(7) Uani 1 1 d . . . . . C1 C -0.1726(3) 0.6417(2) 0.32328(9) 0.0382(7) Uani 1 1 d . . . . . H1 H -0.233(4) 0.685(2) 0.3145(10) 0.047(11) Uiso 1 1 d . . . . . N1 N -0.1819(3) 0.61697(19) 0.35563(8) 0.0414(7) Uani 1 1 d . . . . . H1A H -0.126(5) 0.586(3) 0.3619(13) 0.065(17) Uiso 1 1 d . . . . . C24 C -0.2623(4) 0.6495(2) 0.38266(11) 0.0460(9) Uani 1 1 d . . . . . H24A H -0.303(5) 0.609(3) 0.3950(13) 0.060(14) Uiso 1 1 d . . . . . H24B H -0.322(4) 0.684(3) 0.3723(12) 0.054(12) Uiso 1 1 d . . . . . C23 C -0.1848(4) 0.6912(2) 0.41007(11) 0.0472(9) Uani 1 1 d . . . . . H23A H -0.141(4) 0.732(3) 0.3986(12) 0.056(12) Uiso 1 1 d . . . . . H23B H -0.230(4) 0.710(3) 0.4284(12) 0.054(12) Uiso 1 1 d . . . . . C25 C 0.0333(4) 0.6645(3) 0.41621(15) 0.0613(11) Uani 1 1 d . . . . . H25A H 0.039(4) 0.667(3) 0.3904(13) 0.054(12) Uiso 1 1 d . . . . . H25B H 0.059(4) 0.715(3) 0.4274(13) 0.064(14) Uiso 1 1 d . . . . . H25C H 0.092(5) 0.622(3) 0.4280(17) 0.084(18) Uiso 1 1 d . . . . . S1 S 0.32664(9) 0.46280(5) 0.42407(2) 0.0450(2) Uani 1 1 d . . . . . O11 O 0.2650(3) 0.39368(19) 0.43463(11) 0.0746(10) Uani 1 1 d . . . . . O12 O 0.2934(3) 0.48906(19) 0.38929(7) 0.0641(8) Uani 1 1 d . . . . . O13 O 0.3338(4) 0.5243(2) 0.44952(9) 0.0767(10) Uani 1 1 d . . . . . C26 C 0.4841(4) 0.4329(3) 0.41840(15) 0.0680(13) Uani 1 1 d . . . . . F11 F 0.5320(4) 0.4065(3) 0.44782(13) 0.1271(16) Uani 1 1 d . . . . . F12 F 0.5533(3) 0.4911(2) 0.40759(12) 0.1063(12) Uani 1 1 d . . . . . F13 F 0.4936(4) 0.3761(2) 0.39480(14) 0.1193(15) Uani 1 1 d . . . . . S2 S -0.12939(8) 0.33236(5) 0.30403(2) 0.0413(2) Uani 1 1 d . . . . . C27 C -0.2510(4) 0.3829(2) 0.32791(12) 0.0498(9) Uani 1 1 d . . . . . F21 F -0.3362(3) 0.33299(18) 0.33845(9) 0.0796(8) Uani 1 1 d . . . . . F22 F -0.2087(3) 0.4185(2) 0.35661(7) 0.0716(7) Uani 1 1 d . . . . . F23 F -0.3056(3) 0.43637(19) 0.30822(8) 0.0849(9) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba 0.03883(14) 0.02926(13) 0.04340(15) 0.00178(7) 0.00799(8) 0.00494(8) O2 0.0429(13) 0.0376(13) 0.0378(13) 0.0089(10) 0.0023(11) 0.0050(10) O1 0.0450(13) 0.0331(11) 0.0315(12) 0.0020(9) 0.0022(10) 0.0051(10) N3 0.0437(16) 0.0481(18) 0.0397(17) -0.0022(14) 0.0034(13) 0.0023(14) C22 0.058(3) 0.056(2) 0.041(2) -0.0085(19) -0.0031(18) 0.004(2) C21 0.058(2) 0.056(2) 0.041(2) 0.0015(18) 0.0094(18) 0.007(2) N2 0.0484(17) 0.0521(18) 0.0330(15) 0.0031(13) 0.0071(14) 0.0045(15) C20 0.046(2) 0.062(2) 0.0311(18) 0.0029(17) 0.0028(16) -0.0056(18) C17 0.069(3) 0.062(3) 0.036(2) 0.0094(18) -0.009(2) -0.023(2) C16 0.084(3) 0.051(2) 0.046(2) 0.0189(19) -0.023(2) -0.026(2) C15 0.068(3) 0.040(2) 0.056(2) 0.0137(18) -0.024(2) -0.009(2) C14 0.0460(19) 0.0382(18) 0.0436(19) 0.0084(15) -0.0143(16) -0.0077(15) O3 0.0519(15) 0.0325(12) 0.0569(16) 0.0055(11) -0.0079(13) 0.0072(11) C13 0.060(3) 0.036(2) 0.083(3) 0.009(2) -0.011(2) 0.0117(19) C12 0.062(3) 0.037(2) 0.086(4) -0.009(2) -0.008(2) 0.011(2) O4 0.0599(17) 0.0394(14) 0.0588(16) -0.0116(12) 0.0012(13) 0.0081(13) C11 0.078(3) 0.068(3) 0.076(3) -0.031(3) 0.011(3) 0.016(3) C10 0.057(3) 0.074(3) 0.060(3) -0.010(2) 0.009(2) 0.026(2) C18 0.0477(19) 0.050(2) 0.0333(18) 0.0068(15) -0.0033(15) -0.0097(17) C19 0.0391(18) 0.0403(18) 0.0378(18) 0.0063(14) -0.0095(14) -0.0051(15) O5 0.0644(19) 0.0624(18) 0.074(2) 0.0136(16) 0.0285(16) 0.0278(16) C9 0.046(2) 0.076(3) 0.056(3) 0.005(2) 0.016(2) 0.011(2) C8 0.045(2) 0.059(2) 0.047(2) 0.0026(19) 0.0161(17) 0.0016(19) O21 0.0570(16) 0.0610(18) 0.0639(19) 0.0149(15) -0.0067(14) 0.0096(15) O22 0.0559(17) 0.0471(16) 0.0619(18) -0.0042(12) 0.0130(14) -0.0172(13) O23 0.0653(18) 0.0557(17) 0.0582(17) -0.0102(14) -0.0099(14) -0.0100(14) O6 0.0412(13) 0.0438(13) 0.0377(13) 0.0000(10) 0.0064(10) 0.0008(11) C6 0.0397(18) 0.0332(17) 0.0381(18) -0.0016(14) 0.0001(14) -0.0086(14) C7 0.0411(17) 0.0268(15) 0.0322(16) -0.0027(12) -0.0014(13) -0.0062(13) C5 0.051(2) 0.045(2) 0.0361(19) -0.0015(16) 0.0067(16) -0.0121(17) C4 0.063(2) 0.046(2) 0.0361(19) 0.0066(16) -0.0018(17) -0.0118(19) C3 0.055(2) 0.0359(18) 0.042(2) 0.0013(15) -0.0085(17) -0.0040(17) C2 0.0455(18) 0.0275(15) 0.0382(19) -0.0005(13) -0.0058(15) -0.0037(14) C1 0.0425(18) 0.0318(16) 0.0402(19) 0.0000(14) -0.0067(15) -0.0008(15) N1 0.0426(17) 0.0395(16) 0.0420(17) 0.0012(13) -0.0005(13) 0.0081(14) C24 0.0408(19) 0.052(2) 0.045(2) 0.0069(17) 0.0053(16) 0.0086(18) C23 0.057(2) 0.0401(19) 0.044(2) -0.0013(16) 0.0109(18) 0.0081(18) C25 0.050(2) 0.069(3) 0.065(3) -0.008(2) 0.003(2) -0.008(2) S1 0.0501(5) 0.0470(5) 0.0379(5) -0.0010(4) -0.0002(4) -0.0030(4) O11 0.066(2) 0.064(2) 0.094(3) 0.0155(17) 0.0077(19) -0.0212(16) O12 0.071(2) 0.076(2) 0.0452(16) 0.0008(14) -0.0103(14) 0.0079(17) O13 0.106(3) 0.072(2) 0.0524(18) -0.0230(16) 0.0139(18) -0.011(2) C26 0.052(3) 0.063(3) 0.089(4) 0.012(3) 0.000(2) -0.003(2) F11 0.077(2) 0.155(4) 0.150(4) 0.070(3) -0.040(2) -0.001(2) F12 0.0658(19) 0.098(2) 0.155(3) 0.032(2) 0.022(2) -0.0258(18) F13 0.092(3) 0.089(2) 0.177(4) -0.030(3) 0.030(3) 0.025(2) S2 0.0416(4) 0.0369(4) 0.0454(5) 0.0025(4) -0.0038(4) -0.0050(4) C27 0.043(2) 0.051(2) 0.055(2) 0.0079(18) -0.0043(18) -0.0008(17) F21 0.0522(14) 0.090(2) 0.097(2) 0.0003(17) 0.0213(14) -0.0189(15) F22 0.0661(17) 0.090(2) 0.0582(16) -0.0209(14) 0.0027(12) -0.0005(16) F23 0.085(2) 0.097(2) 0.0730(18) 0.0180(16) 0.0020(15) 0.0460(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ba O2 2.693(2) . ? Ba O1 2.696(2) . ? Ba O3 2.927(3) . ? Ba O4 2.924(3) . ? Ba O5 2.836(3) . ? Ba O21 2.996(3) . ? Ba O22 3.051(3) . ? Ba O6 2.959(2) . ? Ba S1 3.5810(10) . ? Ba O11 3.279(4) . ? Ba O12 2.812(3) . ? Ba S2 3.5243(9) . ? O2 C19 1.284(4) . ? O1 C7 1.291(4) . ? N3 C22 1.458(5) . ? N3 C23 1.462(5) . ? N3 C25 1.466(5) . ? C22 H22A 0.92(5) . ? C22 H22B 1.05(5) . ? C22 C21 1.511(6) . ? C21 H21A 1.00(5) . ? C21 H21B 1.03(6) . ? C21 N2 1.474(5) . ? N2 H2 0.90(5) . ? N2 C20 1.298(5) . ? C20 H20 0.97(4) . ? C20 C18 1.405(6) . ? C17 H17 0.90(4) . ? C17 C16 1.346(7) . ? C17 C18 1.428(5) . ? C16 H16 0.92(6) . ? C16 C15 1.419(7) . ? C15 H15 0.92(5) . ? C15 C14 1.373(5) . ? C14 O3 1.372(5) . ? C14 C19 1.428(5) . ? O3 C13 1.445(5) . ? C13 H13A 1.01(6) . ? C13 H13B 1.01(5) . ? C13 C12 1.476(7) . ? C12 H12A 1.00(6) . ? C12 H12B 0.97(4) . ? C12 O4 1.413(6) . ? O4 C11 1.416(6) . ? C11 H11A 1.02(6) . ? C11 H11B 0.91(6) . ? C11 C10 1.481(8) . ? C10 H10A 0.99(6) . ? C10 H10B 0.98(6) . ? C10 O5 1.393(5) . ? C18 C19 1.431(5) . ? O5 C9 1.438(6) . ? C9 H9A 0.99(5) . ? C9 H9B 0.93(5) . ? C9 C8 1.473(6) . ? C8 H8A 0.97(5) . ? C8 H8B 1.00(5) . ? C8 O6 1.434(4) . ? O21 S2 1.440(3) . ? O22 S2 1.428(3) . ? O23 S2 1.426(3) . ? O6 C6 1.374(4) . ? C6 C7 1.434(5) . ? C6 C5 1.361(5) . ? C7 C2 1.429(5) . ? C5 H5 0.87(5) . ? C5 C4 1.405(6) . ? C4 H4 1.02(4) . ? C4 C3 1.365(6) . ? C3 H3 0.92(4) . ? C3 C2 1.413(5) . ? C2 C1 1.414(5) . ? C1 H1 1.04(4) . ? C1 N1 1.295(5) . ? N1 H1A 0.85(6) . ? N1 C24 1.457(5) . ? C24 H24A 0.94(5) . ? C24 H24B 0.97(5) . ? C24 C23 1.515(6) . ? C23 H23A 0.96(5) . ? C23 H23B 0.91(5) . ? C25 H25A 0.98(5) . ? C25 H25B 1.00(5) . ? C25 H25C 1.07(6) . ? S1 O11 1.420(3) . ? S1 O12 1.433(3) . ? S1 O13 1.428(3) . ? S1 C26 1.808(5) . ? C26 F11 1.307(6) . ? C26 F12 1.317(6) . ? C26 F13 1.323(7) . ? S2 C27 1.824(4) . ? C27 F21 1.326(5) . ? C27 F22 1.325(5) . ? C27 F23 1.322(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ba O1 85.00(7) . . ? O2 Ba O3 56.23(7) . . ? O2 Ba O4 111.47(7) . . ? O2 Ba O5 161.85(8) . . ? O2 Ba O21 83.83(8) . . ? O2 Ba O22 108.23(8) . . ? O2 Ba O6 139.56(7) . . ? O2 Ba S1 81.37(6) . . ? O2 Ba O11 68.12(9) . . ? O2 Ba O12 95.57(8) . . ? O2 Ba S2 92.18(6) . . ? O1 Ba O3 139.12(7) . . ? O1 Ba O4 160.97(7) . . ? O1 Ba O5 110.19(8) . . ? O1 Ba O21 100.96(7) . . ? O1 Ba O22 64.90(7) . . ? O1 Ba O6 55.08(7) . . ? O1 Ba S1 97.64(5) . . ? O1 Ba O11 114.16(8) . . ? O1 Ba O12 82.28(8) . . ? O1 Ba S2 79.55(5) . . ? O3 Ba O21 65.56(8) . . ? O3 Ba O22 112.02(7) . . ? O3 Ba O6 163.77(7) . . ? O3 Ba S1 89.50(5) . . ? O3 Ba O11 66.16(7) . . ? O3 Ba S2 88.68(5) . . ? O4 Ba O3 55.36(8) . . ? O4 Ba O21 72.60(8) . . ? O4 Ba O22 99.69(8) . . ? O4 Ba O6 108.96(7) . . ? O4 Ba S1 94.36(6) . . ? O4 Ba O11 81.92(8) . . ? O4 Ba S2 90.00(6) . . ? O5 Ba O3 110.38(8) . . ? O5 Ba O4 55.74(9) . . ? O5 Ba O21 102.20(10) . . ? O5 Ba O22 87.76(9) . . ? O5 Ba O6 55.20(8) . . ? O5 Ba S1 86.64(8) . . ? O5 Ba O11 95.84(10) . . ? O5 Ba S2 100.13(8) . . ? O21 Ba O22 46.48(7) . . ? O21 Ba S1 155.05(6) . . ? O21 Ba O11 131.69(8) . . ? O21 Ba S2 23.79(6) . . ? O22 Ba S1 158.36(5) . . ? O22 Ba O11 176.35(8) . . ? O22 Ba S2 23.71(5) . . ? O6 Ba O21 107.80(7) . . ? O6 Ba O22 63.47(7) . . ? O6 Ba S1 96.44(5) . . ? O6 Ba O11 119.20(7) . . ? O6 Ba S2 87.05(5) . . ? O11 Ba S1 23.37(5) . . ? O11 Ba S2 153.75(6) . . ? O12 Ba O3 111.36(8) . . ? O12 Ba O4 104.62(9) . . ? O12 Ba O5 77.39(10) . . ? O12 Ba O21 176.63(8) . . ? O12 Ba O22 136.62(8) . . ? O12 Ba O6 74.78(8) . . ? O12 Ba S1 21.97(6) . . ? O12 Ba O11 45.32(8) . . ? O12 Ba S2 159.53(6) . . ? S2 Ba S1 173.20(2) . . ? C19 O2 Ba 128.0(2) . . ? C7 O1 Ba 124.7(2) . . ? C22 N3 C23 112.2(3) . . ? C22 N3 C25 111.8(4) . . ? C23 N3 C25 112.7(4) . . ? N3 C22 H22A 114(3) . . ? N3 C22 H22B 104(3) . . ? N3 C22 C21 110.6(3) . . ? H22A C22 H22B 107(4) . . ? C21 C22 H22A 109(3) . . ? C21 C22 H22B 113(3) . . ? C22 C21 H21A 114(3) . . ? C22 C21 H21B 107(3) . . ? H21A C21 H21B 113(4) . . ? N2 C21 C22 109.6(3) . . ? N2 C21 H21A 104(3) . . ? N2 C21 H21B 110(3) . . ? C21 N2 H2 116(3) . . ? C20 N2 C21 123.3(3) . . ? C20 N2 H2 120(3) . . ? N2 C20 H20 116(2) . . ? N2 C20 C18 124.6(4) . . ? C18 C20 H20 119(2) . . ? C16 C17 H17 120(3) . . ? C16 C17 C18 121.2(4) . . ? C18 C17 H17 118(3) . . ? C17 C16 H16 124(3) . . ? C17 C16 C15 119.8(4) . . ? C15 C16 H16 116(3) . . ? C16 C15 H15 123(3) . . ? C14 C15 C16 120.2(4) . . ? C14 C15 H15 117(3) . . ? C15 C14 C19 122.2(4) . . ? O3 C14 C15 124.3(4) . . ? O3 C14 C19 113.5(3) . . ? C14 O3 Ba 119.9(2) . . ? C14 O3 C13 117.3(3) . . ? C13 O3 Ba 122.0(3) . . ? O3 C13 H13A 109(3) . . ? O3 C13 H13B 99(3) . . ? O3 C13 C12 108.7(4) . . ? H13A C13 H13B 109(4) . . ? C12 C13 H13A 113(3) . . ? C12 C13 H13B 118(3) . . ? C13 C12 H12A 111(3) . . ? C13 C12 H12B 110(3) . . ? H12A C12 H12B 103(4) . . ? O4 C12 C13 108.8(4) . . ? O4 C12 H12A 112(3) . . ? O4 C12 H12B 113(2) . . ? C12 O4 Ba 114.5(2) . . ? C12 O4 C11 111.7(4) . . ? C11 O4 Ba 112.5(3) . . ? O4 C11 H11A 103(3) . . ? O4 C11 H11B 111(4) . . ? O4 C11 C10 109.4(4) . . ? H11A C11 H11B 110(5) . . ? C10 C11 H11A 111(4) . . ? C10 C11 H11B 112(4) . . ? C11 C10 H10A 109(3) . . ? C11 C10 H10B 108(3) . . ? H10A C10 H10B 113(4) . . ? O5 C10 C11 107.3(4) . . ? O5 C10 H10A 109(3) . . ? O5 C10 H10B 110(3) . . ? C20 C18 C17 118.0(4) . . ? C20 C18 C19 121.3(3) . . ? C17 C18 C19 120.4(4) . . ? O2 C19 C14 121.7(3) . . ? O2 C19 C18 122.3(3) . . ? C14 C19 C18 116.0(3) . . ? C10 O5 Ba 125.1(3) . . ? C10 O5 C9 115.3(4) . . ? C9 O5 Ba 118.5(2) . . ? O5 C9 H9A 108(3) . . ? O5 C9 H9B 107(3) . . ? O5 C9 C8 107.8(4) . . ? H9A C9 H9B 110(4) . . ? C8 C9 H9A 109(3) . . ? C8 C9 H9B 115(3) . . ? C9 C8 H8A 108(3) . . ? C9 C8 H8B 110(3) . . ? H8A C8 H8B 107(4) . . ? O6 C8 C9 107.0(3) . . ? O6 C8 H8A 112(3) . . ? O6 C8 H8B 112(3) . . ? S2 O21 Ba 99.12(16) . . ? S2 O22 Ba 97.07(15) . . ? C8 O6 Ba 120.8(2) . . ? C6 O6 Ba 116.29(19) . . ? C6 O6 C8 117.1(3) . . ? O6 C6 C7 112.5(3) . . ? C5 C6 O6 125.7(3) . . ? C5 C6 C7 121.7(3) . . ? O1 C7 C6 120.7(3) . . ? O1 C7 C2 123.5(3) . . ? C2 C7 C6 115.8(3) . . ? C6 C5 H5 119(3) . . ? C6 C5 C4 121.2(4) . . ? C4 C5 H5 120(3) . . ? C5 C4 H4 121(2) . . ? C3 C4 C5 119.8(4) . . ? C3 C4 H4 120(2) . . ? C4 C3 H3 123(3) . . ? C4 C3 C2 120.2(4) . . ? C2 C3 H3 117(3) . . ? C3 C2 C7 121.3(4) . . ? C3 C2 C1 119.0(3) . . ? C1 C2 C7 119.6(3) . . ? C2 C1 H1 118(2) . . ? N1 C1 C2 123.0(3) . . ? N1 C1 H1 119(2) . . ? C1 N1 H1A 114(3) . . ? C1 N1 C24 125.4(3) . . ? C24 N1 H1A 119(3) . . ? N1 C24 H24A 110(3) . . ? N1 C24 H24B 111(3) . . ? N1 C24 C23 108.7(3) . . ? H24A C24 H24B 109(4) . . ? C23 C24 H24A 106(3) . . ? C23 C24 H24B 111(3) . . ? N3 C23 C24 111.4(3) . . ? N3 C23 H23A 106(3) . . ? N3 C23 H23B 108(3) . . ? C24 C23 H23A 109(3) . . ? C24 C23 H23B 113(3) . . ? H23A C23 H23B 110(4) . . ? N3 C25 H25A 107(3) . . ? N3 C25 H25B 115(3) . . ? N3 C25 H25C 105(3) . . ? H25A C25 H25B 111(4) . . ? H25A C25 H25C 114(4) . . ? H25B C25 H25C 104(4) . . ? O11 S1 Ba 66.32(17) . . ? O11 S1 O12 113.5(2) . . ? O11 S1 O13 117.1(2) . . ? O11 S1 C26 104.3(2) . . ? O12 S1 Ba 47.21(14) . . ? O12 S1 C26 102.8(2) . . ? O13 S1 Ba 137.30(18) . . ? O13 S1 O12 113.3(2) . . ? O13 S1 C26 103.7(3) . . ? C26 S1 Ba 116.95(19) . . ? S1 O11 Ba 90.31(18) . . ? S1 O12 Ba 110.82(18) . . ? F11 C26 S1 112.3(4) . . ? F11 C26 F12 107.2(5) . . ? F11 C26 F13 106.5(5) . . ? F12 C26 S1 111.6(4) . . ? F12 C26 F13 107.7(5) . . ? F13 C26 S1 111.3(4) . . ? O21 S2 Ba 57.09(14) . . ? O21 S2 C27 101.90(19) . . ? O22 S2 Ba 59.22(14) . . ? O22 S2 O21 112.7(2) . . ? O22 S2 C27 104.06(18) . . ? O23 S2 Ba 160.00(14) . . ? O23 S2 O21 115.51(19) . . ? O23 S2 O22 116.46(19) . . ? O23 S2 C27 103.86(19) . . ? C27 S2 Ba 96.03(14) . . ? F21 C27 S2 110.6(3) . . ? F22 C27 S2 111.6(3) . . ? F22 C27 F21 107.3(4) . . ? F23 C27 S2 112.4(3) . . ? F23 C27 F21 107.4(4) . . ? F23 C27 F22 107.2(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ba O2 C19 C14 -1.7(5) . . . . ? Ba O2 C19 C18 177.2(2) . . . . ? Ba O1 C7 C6 -27.6(4) . . . . ? Ba O1 C7 C2 154.3(2) . . . . ? Ba O3 C13 C12 -27.2(5) . . . . ? Ba O4 C11 C10 59.0(5) . . . . ? Ba O5 C9 C8 -59.7(5) . . . . ? Ba O21 S2 O22 21.4(2) . . . . ? Ba O21 S2 O23 158.65(15) . . . . ? Ba O21 S2 C27 -89.51(16) . . . . ? Ba O22 S2 O21 -20.9(2) . . . . ? Ba O22 S2 O23 -157.71(15) . . . . ? Ba O22 S2 C27 88.68(16) . . . . ? Ba O6 C6 C7 25.2(3) . . . . ? Ba O6 C6 C5 -156.5(3) . . . . ? Ba S1 C26 F11 -131.7(4) . . . . ? Ba S1 C26 F12 108.0(4) . . . . ? Ba S1 C26 F13 -12.4(5) . . . . ? Ba S2 C27 F21 -122.3(3) . . . . ? Ba S2 C27 F22 -2.9(3) . . . . ? Ba S2 C27 F23 117.6(3) . . . . ? O1 C7 C2 C3 178.9(3) . . . . ? O1 C7 C2 C1 1.8(5) . . . . ? N3 C22 C21 N2 69.4(5) . . . . ? C22 N3 C23 C24 -117.5(4) . . . . ? C22 C21 N2 C20 134.8(4) . . . . ? C21 N2 C20 C18 -171.2(4) . . . . ? N2 C20 C18 C17 175.6(4) . . . . ? N2 C20 C18 C19 1.4(6) . . . . ? C20 C18 C19 O2 -4.6(5) . . . . ? C20 C18 C19 C14 174.4(3) . . . . ? C17 C16 C15 C14 -1.1(6) . . . . ? C17 C18 C19 O2 -178.6(3) . . . . ? C17 C18 C19 C14 0.3(5) . . . . ? C16 C17 C18 C20 -171.3(4) . . . . ? C16 C17 C18 C19 3.0(6) . . . . ? C16 C15 C14 O3 -174.9(3) . . . . ? C16 C15 C14 C19 4.6(6) . . . . ? C15 C14 O3 Ba -171.1(3) . . . . ? C15 C14 O3 C13 -1.0(5) . . . . ? C15 C14 C19 O2 174.9(3) . . . . ? C15 C14 C19 C18 -4.1(5) . . . . ? C14 O3 C13 C12 162.9(4) . . . . ? O3 C14 C19 O2 -5.6(5) . . . . ? O3 C14 C19 C18 175.4(3) . . . . ? O3 C13 C12 O4 56.7(5) . . . . ? C13 C12 O4 Ba -61.8(4) . . . . ? C13 C12 O4 C11 168.9(4) . . . . ? C12 O4 C11 C10 -170.6(4) . . . . ? O4 C11 C10 O5 -57.8(6) . . . . ? C11 C10 O5 Ba 30.7(6) . . . . ? C11 C10 O5 C9 -161.7(4) . . . . ? C10 O5 C9 C8 131.8(4) . . . . ? C18 C17 C16 C15 -2.6(6) . . . . ? C19 C14 O3 Ba 9.4(4) . . . . ? C19 C14 O3 C13 179.5(3) . . . . ? O5 C9 C8 O6 58.3(5) . . . . ? C9 C8 O6 Ba -34.9(5) . . . . ? C9 C8 O6 C6 172.8(4) . . . . ? C8 O6 C6 C7 178.7(3) . . . . ? C8 O6 C6 C5 -3.0(5) . . . . ? O21 S2 C27 F21 -64.7(3) . . . . ? O21 S2 C27 F22 54.6(3) . . . . ? O21 S2 C27 F23 175.2(3) . . . . ? O22 S2 C27 F21 177.9(3) . . . . ? O22 S2 C27 F22 -62.7(3) . . . . ? O22 S2 C27 F23 57.9(4) . . . . ? O23 S2 C27 F21 55.6(3) . . . . ? O23 S2 C27 F22 175.0(3) . . . . ? O23 S2 C27 F23 -64.5(4) . . . . ? O6 C6 C7 O1 -1.7(4) . . . . ? O6 C6 C7 C2 176.6(3) . . . . ? O6 C6 C5 C4 -176.1(3) . . . . ? C6 C7 C2 C3 0.7(5) . . . . ? C6 C7 C2 C1 -176.5(3) . . . . ? C6 C5 C4 C3 -1.0(6) . . . . ? C7 C6 C5 C4 2.0(6) . . . . ? C7 C2 C1 N1 -0.4(5) . . . . ? C5 C6 C7 O1 179.8(3) . . . . ? C5 C6 C7 C2 -1.8(5) . . . . ? C5 C4 C3 C2 -0.2(6) . . . . ? C4 C3 C2 C7 0.3(5) . . . . ? C4 C3 C2 C1 177.5(3) . . . . ? C3 C2 C1 N1 -177.6(3) . . . . ? C2 C1 N1 C24 169.2(4) . . . . ? C1 N1 C24 C23 -109.5(4) . . . . ? N1 C24 C23 N3 -55.2(4) . . . . ? C23 N3 C22 C21 77.9(4) . . . . ? C25 N3 C22 C21 -154.3(4) . . . . ? C25 N3 C23 C24 115.1(4) . . . . ? O11 S1 O12 Ba 2.9(3) . . . . ? O11 S1 C26 F11 -61.3(5) . . . . ? O11 S1 C26 F12 178.4(4) . . . . ? O11 S1 C26 F13 58.0(5) . . . . ? O12 S1 O11 Ba -2.3(2) . . . . ? O12 S1 C26 F11 -180.0(4) . . . . ? O12 S1 C26 F12 59.7(5) . . . . ? O12 S1 C26 F13 -60.7(4) . . . . ? O13 S1 O11 Ba 132.6(2) . . . . ? O13 S1 O12 Ba -133.7(2) . . . . ? O13 S1 C26 F11 61.8(4) . . . . ? O13 S1 C26 F12 -58.6(5) . . . . ? O13 S1 C26 F13 -179.0(4) . . . . ? C26 S1 O11 Ba -113.5(2) . . . . ? C26 S1 O12 Ba 115.0(2) . . . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma -1 0 0 0.09 0.02 -2 0 0 8.85 0.75 3 0 0 0.07 0.04 -3 0 0 0.04 0.06 -4 0 0 212.04 15.91 4 0 0 187.18 15.91 -4 0 0 194.57 15.92 -5 0 0 0.04 0.07 -5 0 0 -0.12 0.11 -6 0 0 13.27 1.1 -7 0 0 0.06 0.11 -8 0 0 22.48 1.92 -9 0 0 -0.26 0.22 -10 0 0 65.79 5.52 -10 0 0 73.03 5.59 -10 0 0 62.84 5.43 -11 0 0 0.18 0.14 -11 0 0 -0.2 0.28 -11 0 0 -0.02 0.32 -12 0 0 5.13 0.65 -12 0 0 5.18 0.5 -12 0 0 6.35 0.71 -13 0 0 0.05 0.23 -13 0 0 0 0.1 0 1 0 -0.18 0.01 0 -1 0 -0.13 0.01 0 -1 0 -0.15 0.01 -1 1 0 0 0.02 -1 -1 0 0 0.03 -2 1 0 16.84 1.36 -2 -1 0 16.75 1.37 3 1 0 -0.04 0.04 -3 1 0 0.13 0.06 -3 -1 0 0.02 0.06 3 -1 0 -0.04 0.03 4 1 0 2.57 0.24 -4 1 0 2.54 0.25 -4 -1 0 2.59 0.26 -4 1 0 2.61 0.26 -5 1 0 0.16 0.08 -5 -1 0 -0.05 0.1 -5 1 0 -0.04 0.1 -5 -1 0 0.03 0.07 -6 -1 0 80.58 6.37 -6 1 0 84.47 6.38 -6 -1 0 71.61 6.4 -7 1 0 0.2 0.12 -8 1 0 33.99 2.91 -8 1 0 37.04 2.87 -8 -1 0 33.7 2.91 -9 1 0 -0.15 0.24 -9 -1 0 0.45 0.29 -10 -1 0 3.15 0.53 -10 -1 0 3.18 0.34 -10 1 0 2.89 0.51 -10 -1 0 2.82 0.48 -10 1 0 2.78 0.33 -10 1 0 2.62 0.45 -11 -1 0 -0.17 0.34 -11 1 0 0.21 0.31 -11 -1 0 -0.22 0.3 -11 1 0 -0.19 0.29 -11 1 0 0.18 0.15 -11 -1 0 0.19 0.13 -12 1 0 8.66 0.86 -12 1 0 7.77 0.81 -12 -1 0 7.73 0.66 -12 1 0 7.41 0.67 -12 -1 0 6.31 0.81 -13 -1 0 0.12 0.2 -13 1 0 0.03 0.15 -13 -1 0 0.23 0.1 0 -2 0 118.06 8.91 0 -2 0 101.4 8.91 -1 -2 0 -0.03 0.04 -2 -2 0 37.19 2.95 -2 2 0 38.3 2.94 2 -2 0 33.17 2.94 3 -2 0 -0.14 0.04 -3 2 0 -0.14 0.05 -3 -2 0 -0.07 0.06 -4 2 0 9.91 0.86 4 2 0 10.25 0.86 -4 2 0 10.45 0.91 4 -2 0 10.22 0.85 -4 -2 0 10.42 0.88 -5 -2 0 0.06 0.11 -5 2 0 -0.01 0.08 5 2 0 0.04 0.08 -6 2 0 31.53 2.49 -6 -2 0 29.31 2.52 -7 2 0 0.43 0.14 -8 2 0 4.52 0.47 -8 2 0 4.78 0.55 -8 -2 0 4.31 0.54 -9 2 0 0.23 0.25 -9 -2 0 -0.01 0.29 -9 2 0 0.13 0.2 -10 -2 0 13.8 1.19 -10 2 0 13.55 1.29 -10 2 0 14.65 1.36 -10 -2 0 14.78 1.4 -11 2 0 0.45 0.33 -11 -2 0 0.23 0.35 -11 -2 0 0.33 0.13 -11 2 0 0.07 0.29 -12 -2 0 0.14 0.28 -12 2 0 0.47 0.33 -12 -2 0 0.02 0.11 -12 2 0 0.08 0.26 -13 -2 0 0.01 0.09 -13 -2 0 0.12 0.27 0 -3 0 0.03 0.03 0 -3 0 -0.07 0.04 0 -3 0 0.01 0.03 0 3 0 0.07 0.06 -1 -3 0 -0.02 0.05 1 -3 0 -0.06 0.03 2 -3 0 243.05 21.48 -2 3 0 288.29 21.47 -2 -3 0 271.02 21.49 3 -3 0 -0.09 0.04 -3 -3 0 -0.14 0.17 -3 -3 0 -0.04 0.07 4 -3 0 50.62 4.12 4 3 0 51.65 4.12 -4 -3 0 49.79 4.14 -4 3 0 51.97 4.13 -5 -3 0 0.19 0.13 -5 3 0 0.3 0.11 5 3 0 -0.09 0.09 -6 3 0 232.99 19.82 -6 -3 0 261.33 19.95 -7 3 0 0.12 0.14 -7 -3 0 -0.08 0.34 -8 3 0 57.4 4.42 -8 -3 0 48 4.53 -8 3 0 53.99 4.37 -9 3 0 -0.37 0.2 -9 3 0 -0.21 0.26 -9 -3 0 0 0.29 -10 -3 0 4.66 0.69 -10 3 0 5.84 0.71 -10 3 0 5.29 0.73 -10 -3 0 6.68 0.54 -10 3 0 7.09 0.74 -11 -3 0 0.13 0.27 -11 3 0 -0.16 0.27 -11 -3 0 0.11 0.11 -11 3 0 0.13 0.29 -12 -3 0 16.57 1.48 -12 3 0 14.68 1.45 -12 3 0 14.04 1.51 -12 -3 0 17.46 1.32 -13 -3 0 -0.07 0.1 0 -4 0 837.62 63.17 0 -4 0 758.54 63.17 0 -4 0 763.67 63.17 -1 -4 0 -0.02 0.05 1 -4 0 -0.06 0.04 -1 -4 0 -0.04 0.04 -2 -4 0 115.82 10.49 2 -4 0 138.83 10.45 -2 -4 0 122.31 10.45 -2 -4 0 142.48 10.46 -3 -4 0 1.41 0.27 -4 4 0 243.14 18.14 -4 -4 0 196.04 18.2 -4 -4 0 220.75 18.15 4 4 0 236.69 18.13 4 -4 0 230.21 18.13 -5 -4 0 -0.09 0.13 5 4 0 -0.03 0.09 -5 -4 0 0.25 0.27 -5 4 0 0.17 0.11 -6 -4 0 72.56 6.47 6 4 0 75.19 6.35 -6 4 0 87.14 6.37 -7 -4 0 -0.49 0.32 -7 4 0 0.16 0.15 -8 4 0 102.53 8.02 -8 -4 0 83.36 8.12 -8 4 0 107.67 7.99 -9 4 0 -0.49 0.22 -9 -4 0 -0.36 0.29 -9 4 0 0.08 0.26 -10 4 0 14.48 1.26 -10 -4 0 12.78 1.31 -10 -4 0 13.02 1.12 -10 4 0 14.04 1.27 -11 -4 0 -0.04 0.28 -11 4 0 0.37 0.28 -11 4 0 0.24 0.3 -11 -4 0 -0.04 0.11 -12 -4 0 4.75 0.41 -12 -4 0 3.92 0.61 0 -5 0 -0.2 0.05 0 -5 0 -0.08 0.05 0 -5 0 -0.09 0.05 -1 -5 0 -0.01 0.06 -1 -5 0 0.14 0.2 1 -5 0 0.02 0.08 1 -5 0 0.03 0.05 -1 -5 0 -0.05 0.04 -2 -5 0 171.67 15.43 -2 -5 0 170.3 15.49 -2 -5 0 212.98 15.45 2 -5 0 212.61 15.44 3 -5 0 0 0.06 -3 -5 0 -0.06 0.19 3 -5 0 0.13 0.11 -3 -5 0 0.04 0.09 -3 5 0 0 0.09 -4 -5 0 1.51 0.32 4 5 0 1.6 0.19 4 -5 0 1.44 0.17 -4 -5 0 1.22 0.2 -4 5 0 1.71 0.21 -5 -5 0 0.09 0.15 -5 5 0 0.24 0.12 5 5 0 -0.11 0.1 -5 -5 0 -0.03 0.28 5 -5 0 0.02 0.08 6 5 0 20.09 1.75 -6 -5 0 19.05 1.91 -6 5 0 23.58 1.77 -7 5 0 0.08 0.15 -7 -5 0 -0.09 0.39 -8 -5 0 3.34 0.74 -8 5 0 4.82 0.5 -8 5 0 5.22 0.59 -9 -5 0 -0.01 0.32 -9 5 0 0.33 0.28 -9 -5 0 -0.21 0.41 -9 5 0 0.4 0.28 -9 -5 0 0.18 0.09 -10 -5 0 6.91 0.84 -10 5 0 7.53 0.77 -10 5 0 7.69 0.78 -10 -5 0 6.63 0.6 -11 -5 0 0.18 0.09 -11 5 0 -0.23 0.28 -11 -5 0 0.36 0.33 -11 5 0 0.07 0.27 -12 -5 0 15.16 1.24 -12 -5 0 15.09 1.4 0 -6 0 65 5.22 0 -6 0 63.74 5.21 0 -6 0 65.4 5.21 1 -6 0 0.18 0.08 1 -6 0 -0.01 0.12 1 -6 0 0.03 0.06 -1 -6 0 0.19 0.2 -1 -6 0 -0.01 0.08 -1 -6 0 -0.06 0.05 2 -6 0 36.28 3.1 2 -6 0 41.66 3.1 -2 -6 0 32.07 3.16 -2 -6 0 42.07 3.11 3 -6 0 0.24 0.11 -3 -6 0 0.5 0.26 3 -6 0 0.04 0.06 -3 6 0 -0.04 0.09 -3 -6 0 -0.05 0.11 -4 6 0 10.51 0.9 -4 -6 0 9.94 0.91 -4 -6 0 8.26 0.99 4 6 0 10.58 0.88 4 -6 0 11.86 0.88 5 -6 0 0.05 0.1 5 6 0 -0.17 0.12 -5 -6 0 0.38 0.29 -5 6 0 0.01 0.13 -6 6 0 80.33 6.11 -6 -6 0 68.26 6.23 6 6 0 76.03 6.09 -7 6 0 -0.13 0.22 -7 -6 0 0.05 0.42 -7 6 0 0.62 0.18 -8 6 0 25.45 2.23 -8 6 0 27.11 2.2 -9 -6 0 0.09 0.09 -9 -6 0 -0.26 0.36 -9 6 0 -0.21 0.27 -9 -6 0 -0.55 0.34 -9 6 0 -0.03 0.23 -10 -6 0 20.48 2.04 -10 6 0 23.16 1.97 -10 -6 0 23.59 1.85 -10 6 0 22.96 1.97 -11 -6 0 0.14 0.09 -11 -6 0 0.15 0.3 -11 6 0 0.09 0.25 -11 6 0 0.36 0.29 -12 -6 0 1.69 0.2 -12 6 0 2.12 0.3 -12 -6 0 1.22 0.35 0 -7 0 0.24 0.07 0 -7 0 0.26 0.08 -1 -7 0 -0.04 0.06 -1 -7 0 0.02 0.05 -1 -7 0 -0.03 0.25 1 -7 0 0 0.07 1 -7 0 -0.02 0.08 2 -7 0 591.85 44.89 -2 -7 0 538.49 44.89 2 -7 0 545.79 44.87 3 -7 0 -0.01 0.07 -3 -7 0 -0.1 0.25 3 -7 0 -0.04 0.11 -3 -7 0 0.09 0.12 -4 -7 0 21.2 1.87 -4 7 0 21.88 1.93 4 -7 0 24.77 1.87 -4 -7 0 17.92 1.95 4 7 0 23.46 1.85 4 -7 0 23.58 1.84 -5 7 0 0.07 0.14 5 7 0 -0.09 0.14 5 -7 0 0.06 0.11 -5 -7 0 0.4 0.33 -6 7 0 133.68 10.27 -6 -7 0 114.84 10.38 6 7 0 131.04 10.25 -7 7 0 -0.04 0.26 -7 7 0 0.4 0.18 -7 -7 0 0.45 0.47 -8 -7 0 37.14 3.16 -8 7 0 37.55 3.09 -8 7 0 37.16 3.12 -9 7 0 -0.09 0.28 -9 -7 0 0.08 0.33 -9 -7 0 0.04 0.08 -9 7 0 0.13 0.28 -9 -7 0 0.89 0.42 -10 7 0 21.01 1.83 -10 -7 0 21.54 1.7 -10 -7 0 18.78 1.91 -10 7 0 21.63 1.81 -11 7 0 0.07 0.23 -11 7 0 0.17 0.29 -11 -7 0 -0.06 0.07 0 -8 0 280.51 22.5 0 -8 0 279.43 22.5 1 -8 0 0.12 0.08 1 -8 0 -0.02 0.08 -1 -8 0 -0.01 0.06 -1 -8 0 -0.1 0.07 -2 -8 0 21.54 1.98 2 -8 0 23.58 1.88 -3 -8 0 0.45 0.3 3 -8 0 0.11 0.1 3 -8 0 -0.1 0.12 -3 -8 0 -0.03 0.13 4 8 0 5.6 0.47 -4 -8 0 4.41 0.64 4 -8 0 5.01 0.46 4 -8 0 4.26 0.47 5 -8 0 0.08 0.13 -5 -8 0 -0.43 0.36 5 8 0 -0.14 0.15 -6 -8 0 41.73 3.97 -6 8 0 49.94 3.82 -7 -8 0 0.29 0.6 -7 8 0 0.45 0.21 -8 8 0 1.68 0.34 -8 -8 0 1.3 0.56 -8 -8 0 1.31 0.4 -8 -8 0 1.88 0.4 -8 8 0 2.09 0.42 -9 8 0 0.7 0.27 -9 8 0 -0.2 0.29 -9 -8 0 0.01 0.38 -9 -8 0 -0.01 0.3 -10 -8 0 4.64 0.68 -10 8 0 5.52 0.61 -10 8 0 5.64 0.66 -10 -8 0 4.9 0.43 -11 8 0 0.19 0.25 0 -9 0 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8.44 0.71 -10 -6 -4 9.12 0.97 -10 -6 4 6.55 0.9 -10 6 -4 9.42 0.89 -10 -6 4 7.1 0.98 -10 6 -4 8.73 0.89 -10 -6 4 8.7 0.71 -11 6 4 7 0.89 -11 -6 -4 8.02 0.68 -11 -6 -4 6.41 0.91 -11 6 -4 9.84 0.88 -11 -6 4 8.38 0.68 -11 6 -4 8.42 0.86 -11 -6 4 7.95 0.87 -12 -6 -4 3.1 0.28 -12 -6 -4 2.55 0.56 -12 -6 4 2.86 0.27 -12 6 -4 3.37 0.42 -12 -6 4 2.09 0.41 0 -7 4 0.16 0.08 0 -7 -4 -0.03 0.06 0 -7 4 0.13 0.07 0 -7 -4 0.04 0.08 0 7 -4 0.02 0.06 0 -7 4 0.04 0.11 -1 -7 -4 21.32 1.79 1 -7 4 24.01 1.71 1 -7 4 20.69 1.69 1 -7 4 18.96 1.73 -1 -7 -4 21.77 1.69 -1 -7 -4 19.17 1.69 1 7 -4 19.37 1.69 -1 -7 4 20.42 1.78 -1 -7 4 19.32 1.69 -1 -7 4 20.25 1.69 1 -7 -4 20.35 1.69 1 -7 -4 23.65 1.71 -2 -7 -4 206.15 15.97 2 7 -4 196.84 15.89 2 -7 4 203.92 15.89 2 -7 4 171.68 15.89 -2 -7 -4 202.18 15.9 2 -7 -4 192.87 15.9 -2 -7 4 200.49 15.91 -2 -7 4 200.96 15.97 2 -7 -4 203.78 15.89 3 7 -4 2.89 0.31 -3 -7 -4 3.2 0.35 3 -7 4 3.06 0.29 -3 -7 -4 3.66 0.44 3 -7 4 2.51 0.32 3 -7 -4 3.35 0.31 3 -7 -4 2.98 0.3 -3 -7 4 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0.35 2 -6 40 0.16 0.27 2 -6 40 -0.01 0.17 -2 -6 40 0.17 0.3 -2 -6 40 0.28 0.21 2 6 40 0.5 0.22 3 -6 40 5.36 0.68 3 -6 40 6.55 0.57 3 6 40 5.91 0.6 -3 -6 40 5.47 0.7 4 -6 40 3.81 0.54 4 6 40 5.23 0.5 -4 -6 40 4.85 0.58 0 -7 -40 0.07 0.14 0 -7 40 -0.18 0.19 0 -7 40 0.36 0.27 0 7 40 -0.09 0.19 -1 -7 -40 0.69 0.16 1 -7 40 0.59 0.29 1 -7 40 1.09 0.24 -1 -7 40 1.01 0.23 1 7 40 0.71 0.23 -1 -7 40 0.86 0.34 2 -7 40 3.36 0.6 -2 -7 -40 4.92 0.47 2 -7 40 4.65 0.47 -2 -7 40 5.4 0.49 -2 -7 40 3.69 0.59 2 7 40 5.36 0.51 3 -7 40 0.54 0.25 3 -7 40 0.83 0.17 3 7 40 0.85 0.21 -3 -7 40 0.35 0.27 -4 -7 40 2.82 0.43 0 -8 -40 5.12 0.5 0 -8 40 5.27 0.53 0 8 40 5.24 0.53 -1 -8 -40 1.58 0.21 1 -8 40 2.16 0.27 1 -8 40 1.4 0.34 1 8 40 1.91 0.26 -1 -8 40 1.07 0.34 -1 -8 40 1.63 0.25 2 -8 40 0.12 0.22 2 -8 40 0.04 0.15 -2 -8 -40 -0.04 0.12 -2 -8 40 0.18 0.25 2 8 40 0.08 0.16 -3 -8 40 2.65 0.42 0 -9 40 0.07 0.22 0 -9 40 -0.05 0.15 1 -9 40 0.19 0.23 -1 -9 40 0.38 0.22 -2 -9 40 1.5 0.33 0 0 41 0.26 0.35 1 0 41 0.06 0.34 2 0 41 -0.16 0.34 3 0 41 0.03 0.3 4 0 41 -0.28 0.19 4 0 41 -0.17 0.25 5 0 41 -0.14 0.24 -5 0 -41 -0.21 0.17 0 -1 41 0.03 0.31 1 -1 41 1.99 0.48 -1 -1 41 2 0.35 -1 -1 41 1.85 0.59 1 1 41 1.69 0.44 2 1 41 23.17 1.86 -2 -1 41 21.29 1.86 -2 -1 41 21.77 1.95 2 1 41 22.02 2 3 -1 41 0.55 0.34 3 1 41 0.08 0.21 3 1 41 0.13 0.32 4 -1 41 0.91 0.32 4 1 41 0.76 0.32 5 -1 41 0.15 0.26 -5 1 -41 0.45 0.2 5 1 41 0.26 0.26 0 -2 41 15.72 1.53 0 -2 41 16.54 1.4 1 -2 41 0.82 0.38 -1 -2 41 1.69 0.31 -1 -2 41 1.37 0.37 -1 -2 41 1.29 0.27 2 -2 41 0.21 0.34 2 -2 41 0.22 0.19 2 2 41 -0.01 0.2 2 2 41 0.17 0.31 -2 -2 41 0.37 0.21 -2 -2 41 0.36 0.32 3 -2 41 -0.37 0.3 3 -2 41 -0.12 0.16 3 2 41 -0.12 0.2 3 2 41 -0.25 0.29 4 -2 41 9.03 0.94 4 2 41 8.66 0.93 5 -2 41 2.64 0.45 5 2 41 2.83 0.48 -5 2 -41 2.64 0.37 0 -3 41 0 0.31 0 -3 41 -0.01 0.2 1 -3 41 0.83 0.24 1 -3 41 0.44 0.36 -1 -3 41 1.22 0.28 -1 -3 41 0.71 0.24 -1 -3 41 0.49 0.34 1 3 41 0.96 0.24 2 -3 41 6.76 0.58 2 -3 41 4.06 0.7 -2 -3 41 6.05 0.57 2 3 41 6.02 0.59 -2 -3 41 4.79 0.7 3 -3 41 3.01 0.35 3 -3 41 2.29 0.44 3 3 41 2.49 0.32 3 3 41 1.94 0.41 4 -3 41 0.12 0.25 4 3 41 0.05 0.19 4 3 41 0 0.26 5 -3 41 -0.1 0.22 -5 3 -41 0.08 0.16 5 3 41 -0.11 0.24 0 -4 41 5.1 0.57 0 -4 41 5.6 0.7 1 -4 41 0.44 0.22 1 -4 41 0.9 0.36 -1 -4 41 0.51 0.32 -1 -4 41 0.88 0.41 -1 -4 41 1.01 0.25 1 4 41 0.63 0.23 2 -4 41 0.79 0.21 2 -4 41 0.57 0.35 -2 -4 41 0.43 0.21 2 4 41 0.63 0.22 -2 -4 41 0.38 0.29 3 -4 41 0.89 0.31 3 -4 41 0.73 0.2 3 4 41 0.84 0.21 -3 -4 41 0.92 0.3 4 -4 41 1.62 0.33 4 4 41 1.23 0.32 0 -5 41 -0.19 0.28 0 -5 41 -0.09 0.19 1 -5 41 0.32 0.3 1 -5 41 0.22 0.21 -1 -5 41 0.43 0.32 1 5 41 0.26 0.2 -1 -5 41 0.72 0.22 2 -5 41 22.83 1.75 2 -5 41 19.96 1.86 -2 -5 41 18.62 1.73 2 5 41 21.63 1.74 3 -5 41 -0.02 0.24 3 -5 41 -0.09 0.15 3 5 41 0.03 0.18 -3 -5 41 0.27 0.26 4 -5 41 3 0.48 4 5 41 4.03 0.44 0 -6 41 11.73 1.31 0 -6 41 16.01 1.2 1 -6 41 -0.11 0.17 1 -6 41 -0.02 0.25 -1 -6 41 0.13 0.2 -1 -6 41 0 0.27 1 6 41 0.14 0.18 2 -6 41 -0.01 0.24 2 -6 41 0.27 0.17 2 6 41 0.04 0.18 -2 -6 41 0.2 0.27 -2 -6 41 0.21 0.15 3 -6 41 0.32 0.25 -3 -6 41 0.48 0.28 3 6 41 0.32 0.18 0 -7 41 0.03 0.16 0 -7 41 -0.04 0.26 0 7 41 -0.03 0.16 1 -7 41 0.35 0.17 1 -7 41 0.17 0.24 -1 -7 41 0.33 0.3 1 7 41 0.4 0.18 -1 -7 41 0.65 0.19 2 -7 41 0.2 0.17 2 -7 41 0 0.22 -2 -7 41 0.31 0.24 2 7 41 0.1 0.16 3 -7 41 0.48 0.23 -3 -7 41 0.22 0.23 0 -8 41 12.72 1.18 1 -8 41 1.16 0.29 -1 -8 41 0.64 0.26 -2 -8 41 0.13 0.23 1 0 42 4.17 0.62 2 0 42 0.76 0.34 3 0 42 10.47 1.05 4 0 42 5.22 0.64 5 0 42 0.71 0.29 0 -1 42 -0.28 0.27 1 -1 42 0.32 0.32 1 1 42 0.72 0.36 -1 -1 42 0.08 0.2 2 -1 42 5.56 0.7 -2 -1 42 6.22 0.56 2 1 42 5.41 0.56 2 1 42 4.24 0.65 3 -1 42 -0.04 0.16 3 -1 42 -0.09 0.27 3 1 42 0.04 0.28 3 1 42 0 0.17 4 -1 42 2.05 0.38 4 1 42 1.99 0.37 0 -2 42 1.06 0.26 0 -2 42 0.89 0.36 1 -2 42 3.01 0.48 1 -2 42 1.94 0.29 -1 -2 42 1.44 0.39 2 -2 42 -0.02 0.16 2 -2 42 0.12 0.27 2 2 42 -0.29 0.19 -2 -2 42 -0.05 0.19 2 2 42 0.01 0.3 3 -2 42 -0.03 0.15 3 -2 42 -0.09 0.25 3 2 42 0.04 0.19 3 2 42 0.05 0.26 4 -2 42 0.37 0.26 4 2 42 0.64 0.28 0 -3 42 -0.02 0.26 0 -3 42 -0.1 0.19 1 -3 42 8.05 0.85 1 -3 42 7.35 0.71 -1 -3 42 7.35 0.71 -1 -3 42 7.05 0.83 2 -3 42 3.76 0.62 2 -3 42 4.79 0.47 2 3 42 4.88 0.5 -2 -3 42 4.79 0.48 -2 -3 42 3.88 0.59 3 -3 42 12.18 1.19 3 -3 42 11.84 1.08 3 3 42 13.59 1.09 4 -3 42 3.21 0.44 4 3 42 1.9 0.41 0 -4 42 5.27 0.69 0 -4 42 6.17 0.58 1 -4 42 11.37 1.23 1 -4 42 14.35 1.12 -1 -4 42 13.68 1.12 1 4 42 12.91 1.11 -1 -4 42 11.5 1.21 2 -4 42 -0.1 0.24 2 -4 42 0.47 0.17 -2 -4 42 0.07 0.28 2 4 42 -0.01 0.17 -2 -4 42 -0.04 0.19 3 -4 42 2.09 0.29 3 -4 42 2.07 0.39 3 4 42 2.73 0.3 -3 -4 42 1.9 0.36 4 -4 42 1.35 0.33 0 -5 42 0.07 0.17 0 -5 42 0.24 0.27 1 -5 42 0.64 0.19 1 -5 42 0.56 0.29 1 5 42 0.39 0.18 -1 -5 42 0.43 0.2 -1 -5 42 0.36 0.27 2 -5 42 0.75 0.18 2 -5 42 0.68 0.27 2 5 42 0.78 0.2 -2 -5 42 0.87 0.31 3 -5 42 1.97 0.36 -3 -5 42 1.78 0.34 0 -6 42 3.68 0.59 0 -6 42 5.78 0.49 1 -6 42 1.57 0.24 1 -6 42 1.48 0.35 -1 -6 42 1.72 0.37 -1 -6 42 1.61 0.28 2 -6 42 -0.03 0.22 -2 -6 42 0.21 0.23 3 -6 42 0.57 0.24 0 -7 42 -0.04 0.24 1 -7 42 7.16 0.76 -1 -7 42 7.38 0.77 2 -7 42 8.99 0.95 -2 -7 42 8.44 0.89 1 0 43 0.03 0.27 -1 0 43 -0.28 0.17 2 0 43 0.18 0.26 3 0 43 -0.25 0.14 3 0 43 0.05 0.23 4 0 43 0.02 0.22 0 -1 43 -0.14 0.17 0 -1 43 0.07 0.26 1 -1 43 3.93 0.48 1 -1 43 4.29 0.6 -1 -1 43 5 0.47 2 -1 43 0.39 0.29 2 -1 43 0.34 0.16 2 1 43 0.66 0.28 3 -1 43 0.85 0.19 3 -1 43 0.42 0.26 3 1 43 0.42 0.26 4 -1 43 1.78 0.32 4 1 43 1.08 0.34 0 -2 43 0.5 0.27 0 -2 43 0.61 0.2 1 -2 43 10.37 0.83 -1 -2 43 9.3 0.82 -1 -2 43 7.76 0.9 2 -2 43 0.15 0.16 2 -2 43 0.26 0.26 2 2 43 0.1 0.2 3 2 43 7.18 0.74 4 -2 43 0.7 0.28 0 -3 43 0.03 0.18 0 -3 43 -0.1 0.25 1 -3 43 0.3 0.26 1 -3 43 0.27 0.17 -1 -3 43 0.33 0.18 -1 -3 43 0.16 0.26 2 -3 43 -0.03 0.14 2 -3 43 0.08 0.24 2 3 43 -0.16 0.19 -2 -3 43 0.05 0.25 3 -3 43 0.05 0.23 0 -4 43 -0.5 0.16 0 -4 43 0.06 0.23 1 -4 43 0.53 0.18 1 -4 43 0.6 0.26 -1 -4 43 0.32 0.19 -1 -4 43 0.33 0.27 2 -4 43 -0.1 0.24 2 -4 43 0.02 0.23 -2 -4 43 0.12 0.22 3 -4 43 1.03 0.27 0 -5 43 -0.1 0.22 0 -5 43 0.02 0.17 1 -5 43 5.45 0.66 -1 -5 43 6.18 0.69 2 -5 43 0.65 0.27 -2 -5 43 0.61 0.25 0 -6 43 1 0.3 1 -6 43 4.38 0.55 -1 -6 43 4.04 0.55 0 0 44 0.84 0.19 -1 0 44 5.32 0.54 1 0 44 5.96 0.53 1 0 44 4.57 0.6 2 0 44 0.04 0.22 2 0 44 -0.01 0.15 3 0 44 12.62 1.18 0 -1 44 -0.02 0.16 0 -1 44 -0.07 0.22 1 -1 44 0.69 0.28 1 -1 44 0.87 0.19 -1 1 44 1.03 0.24 -1 -1 44 1.1 0.3 2 -1 44 2.42 0.44 2 -1 44 4.08 0.39 2 1 44 3.26 0.54 3 -1 44 1.23 0.33 0 -2 44 1.11 0.2 0 -2 44 0.43 0.26 1 -2 44 0.07 0.16 1 -2 44 0.23 0.24 -1 -2 44 0.2 0.22 2 -2 44 0.3 0.23 3 -2 44 0.71 0.3 0 -3 44 0.02 0.22 0 -3 44 0.13 0.24 1 -3 44 4.02 0.41 1 -3 44 2.88 0.46 -1 -3 44 2.61 0.46 2 -3 44 1.63 0.32 0 -4 44 1 0.29 1 -4 44 1.06 0.28 -1 -4 44 1.87 0.46 2 -4 44 0.17 0.23 0 -5 44 -0.01 0.21 1 -5 44 0.18 0.23 _iucr_refine_instructions_details ; v07e.res created by SHELXL-2014/7 TITL v07e in Pbca CELL 1.54178 10.9261 17.1581 37.6908 90 90 90 ZERR 8 0.0006 0.0009 0.002 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O F S Ba UNIT 216 264 24 96 48 16 8 L.S. 50 PLAN 20 SIZE 0.03 0.13 0.135 TEMP -73.16 HTAB BOND $H CONF fmap 2 ACTA 132 REM REM REM WGHT 0.051000 7.991500 FVAR 0.05840 BA 7 0.110524 0.393328 0.360028 11.00000 0.03883 0.02926 = 0.04340 0.00178 0.00799 0.00494 O2 4 -0.038192 0.398441 0.416964 11.00000 0.04293 0.03762 = 0.03776 0.00887 0.00233 0.00501 O1 4 0.010116 0.532020 0.343226 11.00000 0.04503 0.03308 = 0.03150 0.00195 0.00220 0.00514 N3 3 -0.091444 0.639546 0.424885 11.00000 0.04369 0.04809 = 0.03972 -0.00219 0.00341 0.00230 C22 1 -0.107419 0.627474 0.462905 11.00000 0.05846 0.05559 = 0.04082 -0.00851 -0.00309 0.00352 H22A 2 -0.123638 0.672185 0.475275 11.00000 0.04888 H22B 2 -0.020832 0.607808 0.471345 11.00000 0.06622 C21 1 -0.209005 0.569768 0.469900 11.00000 0.05775 0.05571 = 0.04063 0.00149 0.00941 0.00731 H21A 2 -0.228795 0.563358 0.495518 11.00000 0.06093 H21B 2 -0.282548 0.587424 0.455039 11.00000 0.08608 N2 3 -0.170258 0.491435 0.458469 11.00000 0.04841 0.05213 = 0.03297 0.00307 0.00713 0.00449 H2 2 -0.126796 0.489072 0.438121 11.00000 0.04766 C20 1 -0.187021 0.429215 0.477459 11.00000 0.04625 0.06229 = 0.03110 0.00287 0.00283 -0.00557 H20 2 -0.232698 0.436366 0.499343 11.00000 0.04187 C17 1 -0.156876 0.294059 0.494464 11.00000 0.06930 0.06154 = 0.03642 0.00938 -0.00905 -0.02285 H17 2 -0.202901 0.303721 0.513792 11.00000 0.04279 C16 1 -0.099125 0.225187 0.491083 11.00000 0.08360 0.05077 = 0.04645 0.01887 -0.02260 -0.02559 H16 2 -0.106437 0.184574 0.507050 11.00000 0.07358 C15 1 -0.021051 0.211913 0.461601 11.00000 0.06783 0.03981 = 0.05569 0.01375 -0.02386 -0.00923 H15 2 0.019812 0.165610 0.458056 11.00000 0.05760 C14 1 -0.006036 0.268598 0.436244 11.00000 0.04603 0.03821 = 0.04363 0.00836 -0.01434 -0.00770 O3 4 0.059895 0.258983 0.405585 11.00000 0.05192 0.03248 = 0.05689 0.00552 -0.00790 0.00721 C13 1 0.118632 0.184490 0.400175 11.00000 0.06009 0.03563 = 0.08283 0.00928 -0.01103 0.01165 H13A 2 0.061158 0.141797 0.408442 11.00000 0.08035 H13B 2 0.187426 0.189391 0.417827 11.00000 0.06799 C12 1 0.151343 0.177065 0.362336 11.00000 0.06150 0.03728 = 0.08642 -0.00935 -0.00848 0.01061 H12A 2 0.192800 0.126049 0.357744 11.00000 0.07191 H12B 2 0.077461 0.173835 0.347948 11.00000 0.04124 O4 4 0.226546 0.240638 0.352707 11.00000 0.05986 0.03936 = 0.05884 -0.01160 0.00117 0.00807 C11 1 0.279983 0.229710 0.318843 11.00000 0.07826 0.06775 = 0.07555 -0.03099 0.01136 0.01649 H11A 2 0.207419 0.236669 0.301923 11.00000 0.10537 H11B 2 0.311262 0.180865 0.316733 11.00000 0.09972 C10 1 0.373166 0.290888 0.312618 11.00000 0.05690 0.07382 = 0.05953 -0.00980 0.00894 0.02608 H10A 2 0.436745 0.286618 0.331178 11.00000 0.08608 H10B 2 0.405728 0.284376 0.288590 11.00000 0.07550 C18 1 -0.137379 0.355681 0.469638 11.00000 0.04767 0.05038 = 0.03326 0.00683 -0.00332 -0.00969 C19 1 -0.059872 0.344089 0.439507 11.00000 0.03908 0.04026 = 0.03781 0.00628 -0.00953 -0.00509 O5 4 0.314447 0.362618 0.315638 11.00000 0.06436 0.06239 = 0.07426 0.01356 0.02853 0.02782 C9 1 0.378215 0.427511 0.300088 11.00000 0.04630 0.07561 = 0.05569 0.00491 0.01576 0.01073 H9A 2 0.443272 0.406162 0.284604 11.00000 0.06554 H9B 2 0.413462 0.455804 0.318589 11.00000 0.06507 C8 1 0.290110 0.471130 0.278145 11.00000 0.04452 0.05863 = 0.04716 0.00260 0.01615 0.00156 H8A 2 0.332456 0.515400 0.268048 11.00000 0.05599 H8B 2 0.260543 0.438031 0.257893 11.00000 0.05959 O21 4 -0.078344 0.283500 0.331338 11.00000 0.05705 0.06101 = 0.06392 0.01495 -0.00667 0.00955 O22 4 -0.048160 0.393251 0.293420 11.00000 0.05589 0.04711 = 0.06185 -0.00420 0.01300 -0.01725 O23 4 -0.192199 0.292428 0.276303 11.00000 0.06530 0.05572 = 0.05818 -0.01024 -0.00985 -0.01003 O6 4 0.192100 0.494641 0.301053 11.00000 0.04117 0.04378 = 0.03766 -0.00003 0.00637 0.00075 C6 1 0.105534 0.543949 0.287043 11.00000 0.03974 0.03322 = 0.03811 -0.00156 0.00006 -0.00856 C7 1 0.010370 0.562325 0.311880 11.00000 0.04114 0.02684 = 0.03216 -0.00268 -0.00145 -0.00624 C5 1 0.107505 0.575067 0.253833 11.00000 0.05090 0.04540 = 0.03611 -0.00145 0.00670 -0.01206 H5 2 0.166500 0.562386 0.239659 11.00000 0.06256 C4 1 0.018068 0.628684 0.242804 11.00000 0.06268 0.04623 = 0.03610 0.00665 -0.00184 -0.01178 H4 2 0.023823 0.654495 0.218587 11.00000 0.04352 C3 1 -0.073823 0.649417 0.265472 11.00000 0.05456 0.03585 = 0.04178 0.00125 -0.00854 -0.00403 H3 2 -0.133463 0.684546 0.259414 11.00000 0.05343 C2 1 -0.079326 0.616892 0.299875 11.00000 0.04554 0.02750 = 0.03815 -0.00052 -0.00576 -0.00368 C1 1 -0.172614 0.641748 0.323282 11.00000 0.04250 0.03181 = 0.04019 -0.00004 -0.00673 -0.00084 H1 2 -0.232503 0.684514 0.314456 11.00000 0.04685 N1 3 -0.181863 0.616973 0.355630 11.00000 0.04263 0.03947 = 0.04196 0.00123 -0.00048 0.00810 H1A 2 -0.125921 0.585824 0.361871 11.00000 0.06510 C24 1 -0.262336 0.649544 0.382665 11.00000 0.04081 0.05180 = 0.04526 0.00690 0.00534 0.00862 H24A 2 -0.302925 0.609216 0.394988 11.00000 0.06027 H24B 2 -0.322106 0.684168 0.372268 11.00000 0.05400 C23 1 -0.184790 0.691153 0.410066 11.00000 0.05747 0.04006 = 0.04406 -0.00132 0.01086 0.00806 H23A 2 -0.140884 0.732432 0.398641 11.00000 0.05618 H23B 2 -0.230038 0.710475 0.428450 11.00000 0.05382 C25 1 0.033331 0.664518 0.416208 11.00000 0.05028 0.06901 = 0.06452 -0.00790 0.00283 -0.00834 H25A 2 0.039075 0.667182 0.390386 11.00000 0.05417 H25B 2 0.059441 0.714564 0.427388 11.00000 0.06439 H25C 2 0.091805 0.621594 0.427957 11.00000 0.08388 S1 6 0.326641 0.462796 0.424073 11.00000 0.05006 0.04696 = 0.03792 -0.00103 -0.00016 -0.00301 O11 4 0.265022 0.393685 0.434626 11.00000 0.06553 0.06385 = 0.09427 0.01555 0.00770 -0.02122 O12 4 0.293366 0.489057 0.389293 11.00000 0.07140 0.07573 = 0.04524 0.00077 -0.01029 0.00785 O13 4 0.333839 0.524306 0.449523 11.00000 0.10576 0.07203 = 0.05239 -0.02295 0.01390 -0.01119 C26 1 0.484051 0.432888 0.418396 11.00000 0.05206 0.06329 = 0.08867 0.01196 -0.00048 -0.00295 F11 5 0.531971 0.406484 0.447817 11.00000 0.07668 0.15480 = 0.14967 0.07029 -0.04032 -0.00127 F12 5 0.553270 0.491053 0.407587 11.00000 0.06577 0.09761 = 0.15550 0.03192 0.02211 -0.02579 F13 5 0.493648 0.376147 0.394798 11.00000 0.09205 0.08946 = 0.17653 -0.02982 0.02958 0.02475 S2 6 -0.129391 0.332357 0.304030 11.00000 0.04162 0.03688 = 0.04545 0.00254 -0.00376 -0.00501 C27 1 -0.250984 0.382914 0.327909 11.00000 0.04346 0.05148 = 0.05452 0.00788 -0.00432 -0.00077 F21 5 -0.336216 0.332991 0.338449 11.00000 0.05223 0.08970 = 0.09684 0.00034 0.02127 -0.01885 F22 5 -0.208678 0.418464 0.356609 11.00000 0.06607 0.09048 = 0.05822 -0.02093 0.00270 -0.00049 F23 5 -0.305612 0.436372 0.308221 11.00000 0.08510 0.09674 = 0.07296 0.01800 0.00196 0.04596 HKLF 4 REM v07e in Pbca REM R1 = 0.0370 for 5820 Fo > 4sig(Fo) and 0.0408 for all 6423 data REM 592 parameters refined using 0 restraints END WGHT 0.0510 7.9820 REM Instructions for potential hydrogen bonds HTAB N2 O2 EQIV $1 -x, -y+1, -z+1 HTAB C20 O13_$1 EQIV $2 -x+1/2, y-1/2, z HTAB C12 O12_$2 HTAB C12 O21 EQIV $3 x+1, y, z HTAB C10 F21_$3 EQIV $4 x+1/2, y, -z+1/2 HTAB C8 F23_$4 EQIV $5 -x-1/2, y+1/2, z HTAB C1 O23_$5 HTAB C1 S2_$5 HTAB N1 O1 EQIV $6 x-1, y, z HTAB C24 F12_$6 HTAB C24 O21_$5 REM Highest difference peak 0.573, deepest hole -0.949, 1-sigma level 0.083 Q1 1 0.1147 0.3940 0.3336 11.00000 0.05 0.57 Q2 1 0.1122 0.3796 0.3909 11.00000 0.05 0.51 Q3 1 0.1734 0.4053 0.3655 11.00000 0.05 0.43 Q4 1 0.1815 0.3713 0.3606 11.00000 0.05 0.37 Q5 1 0.1641 0.4575 0.3108 11.00000 0.05 0.35 Q6 1 0.5139 0.4673 0.4590 11.00000 0.05 0.35 Q7 1 0.0381 0.4331 0.4100 11.00000 0.05 0.35 Q8 1 0.3294 0.4850 0.4572 11.00000 0.05 0.35 Q9 1 0.5103 0.3835 0.4192 11.00000 0.05 0.34 Q10 1 0.0127 0.3637 0.3097 11.00000 0.05 0.33 Q11 1 0.1933 0.3834 0.2639 11.00000 0.05 0.33 Q12 1 -0.1351 0.3187 0.2708 11.00000 0.05 0.32 Q13 1 0.2937 0.4385 0.3911 11.00000 0.05 0.32 Q14 1 0.3792 0.3684 0.3253 11.00000 0.05 0.31 Q15 1 0.0444 0.4392 0.3128 11.00000 0.05 0.31 Q16 1 0.1232 0.3955 0.4243 11.00000 0.05 0.31 Q17 1 0.1828 0.3629 0.3107 11.00000 0.05 0.30 Q18 1 0.0845 0.3117 0.3113 11.00000 0.05 0.30 Q19 1 0.0590 0.5479 0.2985 11.00000 0.05 0.29 Q20 1 0.0231 0.3912 0.3293 11.00000 0.05 0.29 REM The information below was added by Olex2. REM REM R1 = 0.0370 for 5820 Fo > 4sig(Fo) and 0.0408 for all 41782 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.57, deepest hole -0.95 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0408 REM R1_gt = 0.0370 REM wR_ref = 0.1008 REM GOOF = 1.032 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 41782 REM Reflections_gt = 5820 REM Parameters = n/a REM Hole = -0.95 REM Peak = 0.57 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received' data_L(salben)UO2 _audit_creation_date 2019-08-07 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2014/7' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C25 H31 N3 O8 U' _chemical_formula_sum 'C25 H31 N3 O8 U' _chemical_formula_weight 739.56 _chemical_absolute_configuration ad _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'orthorhombic' _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.8509(3) _cell_length_b 12.0635(4) _cell_length_c 17.8749(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2555.46(13) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9945 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 68.272 _cell_measurement_theta_min 4.421 _shelx_estimated_absorpt_T_max 0.382 _shelx_estimated_absorpt_T_min 0.191 _exptl_absorpt_coefficient_mu 18.348 _exptl_absorpt_correction_T_max 0.7531 _exptl_absorpt_correction_T_min 0.4291 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1291 before and 0.0813 after correction. The Ratio of minimum to maximum transmission is 0.5698. The \l/2 correction factor is 0.00150.' _exptl_absorpt_special_details ? _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.922 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description Chunk _exptl_crystal_F_000 1432 _exptl_crystal_size_max 0.135 _exptl_crystal_size_mid 0.095 _exptl_crystal_size_min 0.065 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_unetI/netI 0.0442 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 21288 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 66.000 _diffrn_reflns_theta_max 68.357 _diffrn_reflns_theta_min 4.422 _diffrn_ambient_temperature 199.99 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker Platinum 135 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'Helios high-brilliance multilayer optics' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.765 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.992 _reflns_number_gt 4390 _reflns_number_total 4586 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _refine_diff_density_max 1.564 _refine_diff_density_min -1.206 _refine_diff_density_rms 0.113 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.012(13) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 364 _refine_ls_number_reflns 4586 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0298 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+4.9947P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.0711 _refine_special_details ; Refined as a 2-component inversion twin. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.988(13) 0.012(13) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 3. Shared sites {N3A, N3} {C24A, C24} {C21A, C21} 4. Restrained distances C23A-C24A = C21A-C22A = C23-C24 = C21-C22 1.51765 with sigma of 0.01 N3A-C23A = N3A-C22A = N3A-C25A = N3-C23 = N3-C22 = N3-C25 1.409138 with sigma of 0.01 N3A-C24A = N3A-C21A = C23A-C22A = C23A-C25A = C22A-C25A 2.478778 with sigma of 0.02 N3-C24 = N3-C21 = C23-C22 = C23-C25 = C22-C25 2.478778 with sigma of 0.02 5. Uiso/Uaniso restraints and constraints Uanis(C23) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C25) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(N3A) = Uanis(N3) Uanis(C24A) = Uanis(C24) Uanis(C21A) = Uanis(C21) 6. Others 1(DFIX)=0.9285*FVAR(2) 1(DFIX)=FVAR(1) 1(DFIX)=1(DFIX)=1.6333*FVAR(2) Sof(N3)=Sof(C23)=Sof(H24C)=Sof(H24D)=Sof(C24)=Sof(H25C)=Sof(H25D)=Sof(C21)= Sof(H21C)=Sof(H21D)=Sof(C22)=Sof(H22C)=Sof(H22D)=Sof(C25)=Sof(H23D)=Sof(H23E)= Sof(H23F)=1-FVAR(2) Sof(N3A)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(C24A)=Sof(H24A)=Sof(H24B)= Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(C25A)= Sof(H25A)=Sof(H25B)=Sof(H25E)=FVAR(2) 7.a Secondary CH2 refined with riding coordinates: C23A(H23A,H23B), C24A(H24A,H24B), C21A(H21A,H21B), C22A(H22A,H22B), C23(H24C, H24D), C24(H25C,H25D), C21(H21C,H21D), C22(H22C,H22D), C8(H8A,H8B), C9(H9A, H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B) 7.b Me refined with riding coordinates: C25A(H25A,H25B,H25E), C25(H23D,H23E,H23F) 7.c Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C20(H20) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U U -0.02501(3) 0.29916(3) 0.15730(2) 0.03618(11) Uani 1 1 d . . . . . O1 O 0.0106(7) 0.4167(7) 0.0625(4) 0.0500(19) Uani 1 1 d . . . . . O2 O 0.1388(6) 0.3436(6) 0.2079(4) 0.0421(17) Uani 1 1 d . . . . . O8 O 0.0410(6) 0.1849(6) 0.1104(4) 0.0429(16) Uani 1 1 d . . . . . O7 O -0.1007(8) 0.4037(7) 0.2068(5) 0.063(2) Uani 1 1 d . . . . . O6 O 0.1370(7) 0.5704(7) -0.0100(4) 0.051(2) Uani 1 1 d . . . . . O5 O 0.3819(7) 0.5974(7) -0.0158(5) 0.0538(19) Uani 1 1 d . . . . . O4 O 0.5384(8) 0.4521(7) 0.0778(5) 0.056(2) Uani 1 1 d . . . . . O3 O 0.3581(8) 0.4207(7) 0.1875(4) 0.052(2) Uani 1 1 d . . . . . N3A N -0.1935(8) 0.1681(8) 0.1977(5) 0.058(3) Uani 0.796(19) 1 d D . P A 1 C23A C -0.2966(10) 0.1983(14) 0.1576(7) 0.061(4) Uani 0.796(19) 1 d D . P A 1 H23A H -0.3244 0.2702 0.1769 0.073 Uiso 0.796(19) 1 calc R . P A 1 H23B H -0.3553 0.1418 0.1678 0.073 Uiso 0.796(19) 1 calc R . P A 1 C24A C -0.2803(10) 0.2073(13) 0.0753(7) 0.068(4) Uani 0.796(19) 1 d D . P A 1 H24A H -0.2597 0.1342 0.0542 0.082 Uiso 0.796(19) 1 calc R . P A 1 H24B H -0.3508 0.2326 0.0512 0.082 Uiso 0.796(19) 1 calc R . P A 1 C21A C -0.0994(12) 0.1513(12) 0.3198(6) 0.072(4) Uani 0.796(19) 1 d D . P A 1 H21A H -0.1019 0.1838 0.3706 0.086 Uiso 0.796(19) 1 calc R . P A 1 H21B H -0.0946 0.0697 0.3249 0.086 Uiso 0.796(19) 1 calc R . P A 1 C22A C -0.2078(11) 0.1819(14) 0.2772(6) 0.061(5) Uani 0.796(19) 1 d D . P A 1 H22A H -0.2706 0.1343 0.2947 0.073 Uiso 0.796(19) 1 calc R . P A 1 H22B H -0.2279 0.2599 0.2881 0.073 Uiso 0.796(19) 1 calc R . P A 1 C25A C -0.1661(14) 0.0513(10) 0.1793(9) 0.057(5) Uani 0.796(19) 1 d D . P A 1 H25A H -0.1567 0.0437 0.1251 0.085 Uiso 0.796(19) 1 calc R . P A 1 H25B H -0.0960 0.0300 0.2045 0.085 Uiso 0.796(19) 1 calc R . P A 1 H25E H -0.2276 0.0031 0.1962 0.085 Uiso 0.796(19) 1 calc R . P A 1 N3 N -0.1935(8) 0.1681(8) 0.1977(5) 0.058(3) Uani 0.204(19) 1 d D . P A 2 C23 C -0.244(5) 0.1223(18) 0.1331(16) 0.062(19) Uani 0.204(19) 1 d D U P A 2 H24C H -0.3112 0.0790 0.1485 0.075 Uiso 0.204(19) 1 calc R . P A 2 H24D H -0.1902 0.0703 0.1096 0.075 Uiso 0.204(19) 1 calc R . P A 2 C24 C -0.2803(10) 0.2073(13) 0.0753(7) 0.068(4) Uani 0.204(19) 1 d D . P A 2 H25C H -0.2995 0.1692 0.0280 0.082 Uiso 0.204(19) 1 calc R . P A 2 H25D H -0.3484 0.2467 0.0932 0.082 Uiso 0.204(19) 1 calc R . P A 2 C21 C -0.0994(12) 0.1513(12) 0.3198(6) 0.072(4) Uani 0.204(19) 1 d D . P A 2 H21C H -0.1492 0.2116 0.3377 0.086 Uiso 0.204(19) 1 calc R . P A 2 H21D H -0.0808 0.1001 0.3613 0.086 Uiso 0.204(19) 1 calc R . P A 2 C22 C -0.146(4) 0.0922(18) 0.2516(15) 0.048(15) Uani 0.204(19) 1 d D U P A 2 H22C H -0.0842 0.0496 0.2275 0.058 Uiso 0.204(19) 1 calc R . P A 2 H22D H -0.2045 0.0390 0.2676 0.058 Uiso 0.204(19) 1 calc R . P A 2 C25 C -0.256(5) 0.255(4) 0.235(3) 0.08(2) Uani 0.204(19) 1 d D U P A 2 H23D H -0.2138 0.2809 0.2787 0.115 Uiso 0.204(19) 1 calc R . P A 2 H23E H -0.2676 0.3171 0.2003 0.115 Uiso 0.204(19) 1 calc R . P A 2 H23F H -0.3296 0.2263 0.2510 0.115 Uiso 0.204(19) 1 calc R . P A 2 N1 N -0.1896(7) 0.2874(9) 0.0619(6) 0.049(2) Uani 1 1 d . . . . . C1 C -0.2031(10) 0.3431(9) 0.0011(7) 0.051(3) Uani 1 1 d . . . . . H1 H -0.2709 0.3282 -0.0254 0.062 Uiso 1 1 calc R . . . . C2 C -0.1307(10) 0.4247(9) -0.0327(6) 0.044(2) Uani 1 1 d . . . . . C7 C -0.0272(11) 0.4573(8) -0.0011(5) 0.041(2) Uani 1 1 d . . . . . C3 C -0.1687(13) 0.4672(11) -0.1010(7) 0.062(3) Uani 1 1 d . . . . . H3 H -0.2386 0.4428 -0.1212 0.075 Uiso 1 1 calc R . . . . C4 C -0.1060(14) 0.5432(12) -0.1384(8) 0.068(4) Uani 1 1 d . . . . . H4 H -0.1319 0.5726 -0.1847 0.082 Uiso 1 1 calc R . . . . C5 C -0.0043(12) 0.5776(10) -0.1088(6) 0.057(4) Uani 1 1 d . . . . . H5 H 0.0392 0.6303 -0.1358 0.069 Uiso 1 1 calc R . . . . C6 C 0.0369(10) 0.5384(9) -0.0411(5) 0.041(2) Uani 1 1 d . . . . . C8 C 0.1967(11) 0.6540(10) -0.0500(7) 0.054(3) Uani 1 1 d . . . . . H8A H 0.1488 0.7208 -0.0549 0.064 Uiso 1 1 calc R . . . . H8B H 0.2148 0.6269 -0.1009 0.064 Uiso 1 1 calc R . . . . C9 C 0.3030(11) 0.6832(10) -0.0101(8) 0.059(3) Uani 1 1 d . . . . . H9A H 0.3350 0.7518 -0.0319 0.071 Uiso 1 1 calc R . . . . H9B H 0.2862 0.6976 0.0432 0.071 Uiso 1 1 calc R . . . . C10 C 0.4887(11) 0.6270(11) 0.0134(7) 0.059(3) Uani 1 1 d . . . . . H10A H 0.4794 0.6592 0.0640 0.071 Uiso 1 1 calc R . . . . H10B H 0.5241 0.6836 -0.0191 0.071 Uiso 1 1 calc R . . . . C11 C 0.5631(10) 0.5264(11) 0.0176(8) 0.060(3) Uani 1 1 d . . . . . H11A H 0.5567 0.4852 -0.0301 0.072 Uiso 1 1 calc R . . . . H11B H 0.6424 0.5512 0.0225 0.072 Uiso 1 1 calc R . . . . C12 C 0.4423(10) 0.3841(11) 0.0654(7) 0.054(3) Uani 1 1 d . . . . . H12A H 0.4605 0.3071 0.0803 0.065 Uiso 1 1 calc R . . . . H12B H 0.4244 0.3837 0.0113 0.065 Uiso 1 1 calc R . . . . C13 C 0.3402(11) 0.4220(11) 0.1081(6) 0.051(3) Uani 1 1 d . . . . . H13A H 0.3205 0.4983 0.0922 0.061 Uiso 1 1 calc R . . . . H13B H 0.2757 0.3733 0.0957 0.061 Uiso 1 1 calc R . . . . C14 C 0.3386(10) 0.3187(10) 0.2204(6) 0.048(3) Uani 1 1 d . . . . . C19 C 0.2248(11) 0.2863(10) 0.2334(6) 0.047(3) Uani 1 1 d . . . . . C15 C 0.4279(12) 0.2528(12) 0.2434(7) 0.062(3) Uani 1 1 d . . . . . H15 H 0.5030 0.2741 0.2319 0.074 Uiso 1 1 calc R . . . . C16 C 0.4082(15) 0.1553(12) 0.2836(8) 0.069(4) Uani 1 1 d . . . . . H16 H 0.4699 0.1102 0.2984 0.083 Uiso 1 1 calc R . . . . C17 C 0.3010(15) 0.1247(12) 0.3016(7) 0.065(4) Uani 1 1 d . . . . . H17 H 0.2889 0.0599 0.3308 0.079 Uiso 1 1 calc R . . . . C18 C 0.2085(12) 0.1872(10) 0.2777(6) 0.056(3) Uani 1 1 d . . . . . C20 C 0.0949(14) 0.1569(10) 0.3025(6) 0.058(4) Uani 1 1 d . . . . . H20 H 0.0913 0.1027 0.3410 0.069 Uiso 1 1 calc R . . . . N2 N 0.0020(9) 0.1926(8) 0.2798(5) 0.055(3) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.03754(16) 0.03070(15) 0.04030(16) 0.00183(15) 0.00959(14) 0.00055(15) O1 0.047(5) 0.055(4) 0.047(4) 0.024(3) -0.009(3) -0.014(4) O2 0.046(4) 0.035(4) 0.046(4) 0.006(3) -0.001(3) 0.001(3) O8 0.037(4) 0.044(4) 0.048(4) -0.006(3) 0.000(3) -0.004(3) O7 0.078(6) 0.038(4) 0.072(5) 0.009(4) 0.027(5) 0.013(4) O6 0.054(5) 0.049(5) 0.050(4) 0.017(4) 0.005(4) -0.007(4) O5 0.042(4) 0.051(5) 0.068(5) -0.003(4) 0.005(4) -0.008(4) O4 0.045(5) 0.062(5) 0.063(5) -0.010(4) -0.001(4) -0.008(4) O3 0.054(5) 0.055(5) 0.047(4) -0.010(4) -0.001(4) -0.007(4) N3A 0.046(6) 0.050(6) 0.078(7) 0.012(5) 0.027(5) 0.014(5) C23A 0.039(7) 0.060(9) 0.083(10) -0.002(12) 0.013(8) -0.010(7) C24A 0.044(7) 0.057(8) 0.103(10) 0.014(8) -0.003(6) -0.017(7) C21A 0.101(12) 0.064(8) 0.050(7) 0.006(6) 0.023(7) -0.018(8) C22A 0.055(10) 0.074(13) 0.054(9) -0.010(8) 0.029(7) -0.018(9) C25A 0.061(10) 0.043(8) 0.066(10) 0.000(7) 0.012(7) -0.007(7) N3 0.046(6) 0.050(6) 0.078(7) 0.012(5) 0.027(5) 0.014(5) C23 0.06(2) 0.06(2) 0.07(2) -0.002(13) 0.003(13) -0.010(13) C24 0.044(7) 0.057(8) 0.103(10) 0.014(8) -0.003(6) -0.017(7) C21 0.101(12) 0.064(8) 0.050(7) 0.006(6) 0.023(7) -0.018(8) C22 0.043(18) 0.044(18) 0.059(19) 0.008(12) 0.003(12) -0.003(12) C25 0.07(3) 0.07(3) 0.08(3) 0.011(13) 0.007(13) -0.005(13) N1 0.026(4) 0.047(5) 0.074(6) 0.000(5) 0.001(4) -0.001(4) C1 0.030(5) 0.044(6) 0.080(9) -0.008(6) -0.009(5) 0.004(5) C2 0.046(6) 0.037(6) 0.048(6) 0.000(5) -0.002(5) 0.005(5) C7 0.048(5) 0.034(5) 0.040(5) -0.001(4) 0.006(5) 0.004(5) C3 0.074(9) 0.056(8) 0.058(7) -0.002(6) -0.018(7) 0.004(7) C4 0.083(11) 0.064(8) 0.058(8) 0.004(6) -0.019(7) 0.014(7) C5 0.075(11) 0.055(7) 0.042(5) 0.009(5) 0.004(5) 0.003(6) C6 0.040(6) 0.044(5) 0.039(5) -0.002(4) 0.005(5) 0.005(5) C8 0.053(7) 0.043(6) 0.064(7) 0.012(5) 0.020(6) -0.007(5) C9 0.053(7) 0.041(7) 0.083(9) 0.005(6) 0.014(6) -0.006(6) C10 0.050(7) 0.065(8) 0.063(7) -0.004(6) 0.007(6) -0.021(6) C11 0.034(6) 0.072(9) 0.073(8) -0.021(7) 0.002(6) -0.008(6) C12 0.048(7) 0.061(7) 0.054(6) -0.011(6) 0.005(5) -0.007(6) C13 0.053(7) 0.057(7) 0.043(6) -0.005(5) 0.001(5) -0.003(6) C14 0.060(7) 0.048(7) 0.037(5) -0.011(5) -0.014(5) 0.006(5) C19 0.069(7) 0.038(6) 0.036(5) -0.017(5) -0.015(5) 0.007(6) C15 0.054(7) 0.078(9) 0.053(7) -0.017(6) -0.020(6) 0.010(7) C16 0.093(12) 0.060(8) 0.055(7) -0.011(6) -0.030(8) 0.033(8) C17 0.098(12) 0.055(8) 0.043(7) 0.001(6) -0.021(7) 0.003(8) C18 0.091(10) 0.038(6) 0.039(6) -0.006(5) -0.021(6) 0.003(6) C20 0.102(12) 0.040(6) 0.032(6) -0.001(5) 0.005(6) -0.008(7) N2 0.082(9) 0.038(5) 0.043(4) 0.004(4) 0.009(4) -0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O1 2.250(7) . ? U O2 2.207(8) . ? U O8 1.792(7) . ? U O7 1.783(8) . ? U N3A 2.647(10) . ? U N3 2.647(10) . ? U N1 2.595(9) . ? U N2 2.559(9) . ? O1 C7 1.317(12) . ? O2 C19 1.313(13) . ? O6 C6 1.366(14) . ? O6 C8 1.425(13) . ? O5 C9 1.399(14) . ? O5 C10 1.415(14) . ? O4 C11 1.430(16) . ? O4 C12 1.421(14) . ? O3 C13 1.436(13) . ? O3 C14 1.383(14) . ? N3A C23A 1.463(11) . ? N3A C22A 1.442(11) . ? N3A C25A 1.483(11) . ? C23A H23A 0.9900 . ? C23A H23B 0.9900 . ? C23A C24A 1.487(12) . ? C24A H24A 0.9900 . ? C24A H24B 0.9900 . ? C24A N1 1.465(15) . ? C21A H21A 0.9900 . ? C21A H21B 0.9900 . ? C21A C22A 1.538(13) . ? C21A N2 1.485(16) . ? C22A H22A 0.9900 . ? C22A H22B 0.9900 . ? C25A H25A 0.9800 . ? C25A H25B 0.9800 . ? C25A H25E 0.9800 . ? N3 C23 1.414(15) . ? N3 C22 1.445(14) . ? N3 C25 1.448(15) . ? C23 H24C 0.9900 . ? C23 H24D 0.9900 . ? C23 C24 1.516(15) . ? C24 H25C 0.9900 . ? C24 H25D 0.9900 . ? C24 N1 1.465(15) . ? C21 H21C 0.9900 . ? C21 H21D 0.9900 . ? C21 C22 1.514(15) . ? C21 N2 1.485(16) . ? C22 H22C 0.9900 . ? C22 H22D 0.9900 . ? C25 H23D 0.9800 . ? C25 H23E 0.9800 . ? C25 H23F 0.9800 . ? N1 C1 1.289(15) . ? C1 H1 0.9500 . ? C1 C2 1.438(16) . ? C2 C7 1.406(17) . ? C2 C3 1.399(17) . ? C7 C6 1.430(15) . ? C3 H3 0.9500 . ? C3 C4 1.36(2) . ? C4 H4 0.9500 . ? C4 C5 1.38(2) . ? C5 H5 0.9500 . ? C5 C6 1.387(15) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C9 1.489(19) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.503(18) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 C13 1.501(17) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C19 1.423(17) . ? C14 C15 1.386(17) . ? C19 C18 1.446(18) . ? C15 H15 0.9500 . ? C15 C16 1.40(2) . ? C16 H16 0.9500 . ? C16 C17 1.36(2) . ? C17 H17 0.9500 . ? C17 C18 1.398(19) . ? C18 C20 1.46(2) . ? C20 H20 0.9500 . ? C20 N2 1.250(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U N3A 136.4(3) . . ? O1 U N3 136.4(3) . . ? O1 U N1 71.4(3) . . ? O1 U N2 159.6(3) . . ? O2 U O1 89.4(3) . . ? O2 U N3A 134.2(3) . . ? O2 U N3 134.2(3) . . ? O2 U N1 160.6(3) . . ? O2 U N2 70.2(3) . . ? O8 U O1 92.9(3) . . ? O8 U O2 89.7(3) . . ? O8 U N3A 89.9(3) . . ? O8 U N3 89.9(3) . . ? O8 U N1 88.8(3) . . ? O8 U N2 87.7(3) . . ? O7 U O1 91.3(3) . . ? O7 U O2 93.9(4) . . ? O7 U O8 174.5(4) . . ? O7 U N3A 84.7(4) . . ? O7 U N3 84.7(4) . . ? O7 U N1 89.2(4) . . ? O7 U N2 89.6(3) . . ? N1 U N3A 65.1(3) . . ? N1 U N3 65.1(3) . . ? N2 U N3A 64.0(3) . . ? N2 U N3 64.0(3) . . ? N2 U N1 129.0(3) . . ? C7 O1 U 145.1(7) . . ? C19 O2 U 134.1(7) . . ? C6 O6 C8 115.3(9) . . ? C9 O5 C10 112.6(10) . . ? C12 O4 C11 114.2(9) . . ? C14 O3 C13 113.9(9) . . ? C23A N3A U 110.4(7) . . ? C23A N3A C25A 108.1(11) . . ? C22A N3A U 106.8(8) . . ? C22A N3A C23A 110.9(9) . . ? C22A N3A C25A 110.7(10) . . ? C25A N3A U 110.0(8) . . ? N3A C23A H23A 108.9 . . ? N3A C23A H23B 108.9 . . ? N3A C23A C24A 113.2(9) . . ? H23A C23A H23B 107.8 . . ? C24A C23A H23A 108.9 . . ? C24A C23A H23B 108.9 . . ? C23A C24A H24A 110.1 . . ? C23A C24A H24B 110.1 . . ? H24A C24A H24B 108.5 . . ? N1 C24A C23A 107.8(11) . . ? N1 C24A H24A 110.1 . . ? N1 C24A H24B 110.1 . . ? H21A C21A H21B 108.0 . . ? C22A C21A H21A 109.4 . . ? C22A C21A H21B 109.4 . . ? N2 C21A H21A 109.4 . . ? N2 C21A H21B 109.4 . . ? N2 C21A C22A 110.9(10) . . ? N3A C22A C21A 111.2(9) . . ? N3A C22A H22A 109.4 . . ? N3A C22A H22B 109.4 . . ? C21A C22A H22A 109.4 . . ? C21A C22A H22B 109.4 . . ? H22A C22A H22B 108.0 . . ? N3A C25A H25A 109.5 . . ? N3A C25A H25B 109.5 . . ? N3A C25A H25E 109.5 . . ? H25A C25A H25B 109.5 . . ? H25A C25A H25E 109.5 . . ? H25B C25A H25E 109.5 . . ? C23 N3 U 109(2) . . ? C23 N3 C22 117.6(12) . . ? C23 N3 C25 116(2) . . ? C22 N3 U 105.3(19) . . ? C22 N3 C25 110.7(18) . . ? C25 N3 U 95(3) . . ? N3 C23 H24C 108.7 . . ? N3 C23 H24D 108.7 . . ? N3 C23 C24 114.3(14) . . ? H24C C23 H24D 107.6 . . ? C24 C23 H24C 108.7 . . ? C24 C23 H24D 108.7 . . ? C23 C24 H25C 109.5 . . ? C23 C24 H25D 109.5 . . ? H25C C24 H25D 108.1 . . ? N1 C24 C23 111(2) . . ? N1 C24 H25C 109.5 . . ? N1 C24 H25D 109.5 . . ? H21C C21 H21D 110.4 . . ? C22 C21 H21C 113.0 . . ? C22 C21 H21D 113.0 . . ? N2 C21 H21C 113.0 . . ? N2 C21 H21D 113.0 . . ? N2 C21 C22 94(2) . . ? N3 C22 C21 112.4(13) . . ? N3 C22 H22C 109.1 . . ? N3 C22 H22D 109.1 . . ? C21 C22 H22C 109.1 . . ? C21 C22 H22D 109.1 . . ? H22C C22 H22D 107.9 . . ? N3 C25 H23D 109.5 . . ? N3 C25 H23E 109.5 . . ? N3 C25 H23F 109.5 . . ? H23D C25 H23E 109.5 . . ? H23D C25 H23F 109.5 . . ? H23E C25 H23F 109.5 . . ? C24A N1 U 118.7(7) . . ? C24 N1 U 118.7(7) . . ? C1 N1 U 128.3(8) . . ? C1 N1 C24A 113.1(10) . . ? C1 N1 C24 113.1(10) . . ? N1 C1 H1 115.2 . . ? N1 C1 C2 129.6(11) . . ? C2 C1 H1 115.2 . . ? C7 C2 C1 122.9(10) . . ? C3 C2 C1 115.1(11) . . ? C3 C2 C7 121.9(11) . . ? O1 C7 C2 122.7(10) . . ? O1 C7 C6 120.3(11) . . ? C2 C7 C6 117.0(9) . . ? C2 C3 H3 119.9 . . ? C4 C3 C2 120.1(13) . . ? C4 C3 H3 119.9 . . ? C3 C4 H4 120.3 . . ? C3 C4 C5 119.5(12) . . ? C5 C4 H4 120.3 . . ? C4 C5 H5 118.7 . . ? C4 C5 C6 122.7(12) . . ? C6 C5 H5 118.7 . . ? O6 C6 C7 116.8(9) . . ? O6 C6 C5 124.4(10) . . ? C5 C6 C7 118.8(11) . . ? O6 C8 H8A 109.6 . . ? O6 C8 H8B 109.6 . . ? O6 C8 C9 110.3(10) . . ? H8A C8 H8B 108.1 . . ? C9 C8 H8A 109.6 . . ? C9 C8 H8B 109.6 . . ? O5 C9 C8 110.9(10) . . ? O5 C9 H9A 109.5 . . ? O5 C9 H9B 109.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? O5 C10 H10A 109.7 . . ? O5 C10 H10B 109.7 . . ? O5 C10 C11 109.9(10) . . ? H10A C10 H10B 108.2 . . ? C11 C10 H10A 109.7 . . ? C11 C10 H10B 109.7 . . ? O4 C11 C10 115.0(10) . . ? O4 C11 H11A 108.5 . . ? O4 C11 H11B 108.5 . . ? C10 C11 H11A 108.5 . . ? C10 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? O4 C12 H12A 109.0 . . ? O4 C12 H12B 109.0 . . ? O4 C12 C13 113.0(10) . . ? H12A C12 H12B 107.8 . . ? C13 C12 H12A 109.0 . . ? C13 C12 H12B 109.0 . . ? O3 C13 C12 112.3(11) . . ? O3 C13 H13A 109.1 . . ? O3 C13 H13B 109.1 . . ? C12 C13 H13A 109.1 . . ? C12 C13 H13B 109.1 . . ? H13A C13 H13B 107.9 . . ? O3 C14 C19 118.2(10) . . ? O3 C14 C15 120.5(12) . . ? C15 C14 C19 121.2(12) . . ? O2 C19 C14 122.3(11) . . ? O2 C19 C18 121.5(12) . . ? C14 C19 C18 116.3(11) . . ? C14 C15 H15 119.7 . . ? C14 C15 C16 120.5(14) . . ? C16 C15 H15 119.7 . . ? C15 C16 H16 119.8 . . ? C17 C16 C15 120.4(13) . . ? C17 C16 H16 119.8 . . ? C16 C17 H17 119.6 . . ? C16 C17 C18 120.9(14) . . ? C18 C17 H17 119.6 . . ? C19 C18 C20 119.7(12) . . ? C17 C18 C19 120.6(14) . . ? C17 C18 C20 119.6(13) . . ? C18 C20 H20 115.7 . . ? N2 C20 C18 128.7(11) . . ? N2 C20 H20 115.7 . . ? C21A N2 U 118.6(8) . . ? C21 N2 U 118.6(8) . . ? C20 N2 U 124.1(8) . . ? C20 N2 C21A 116.2(11) . . ? C20 N2 C21 116.2(11) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C11 H11A O8 0.99 2.51 3.436(14) 155.3 4 C13 H13A O5 0.99 2.38 3.101(15) 128.7 . C13 H13B O2 0.99 2.60 3.126(14) 113.0 . C20 H20 O7 0.95 2.55 3.059(15) 113.7 3_545 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag U O1 C7 C2 0.0(19) . . . . ? U O1 C7 C6 179.6(9) . . . . ? U O2 C19 C14 139.5(9) . . . . ? U O2 C19 C18 -41.7(14) . . . . ? U N3A C23A C24A 50.5(14) . . . . ? U N3A C22A C21A -59.3(13) . . . . ? U N3 C23 C24 -53(4) . . . . ? U N3 C22 C21 61(3) . . . . ? U N1 C1 C2 2.0(18) . . . . ? O1 C7 C6 O6 -0.1(14) . . . . ? O1 C7 C6 C5 178.7(10) . . . . ? O2 C19 C18 C17 177.2(10) . . . . ? O2 C19 C18 C20 -7.5(15) . . . . ? O6 C8 C9 O5 71.5(13) . . . . ? O5 C10 C11 O4 -75.9(13) . . . . ? O4 C12 C13 O3 -60.9(15) . . . . ? O3 C14 C19 O2 7.8(14) . . . . ? O3 C14 C19 C18 -171.1(9) . . . . ? O3 C14 C15 C16 173.3(10) . . . . ? N3A C23A C24A N1 -56.0(16) . . . . ? C23A N3A C22A C21A -179.5(12) . . . . ? C23A C24A N1 U 33.7(14) . . . . ? C23A C24A N1 C1 -147.2(11) . . . . ? C24A N1 C1 C2 -176.9(12) . . . . ? C22A N3A C23A C24A 168.6(13) . . . . ? C22A C21A N2 U 0.1(14) . . . . ? C22A C21A N2 C20 -168.5(12) . . . . ? C25A N3A C23A C24A -69.9(15) . . . . ? C25A N3A C22A C21A 60.5(16) . . . . ? N3 C23 C24 N1 47(4) . . . . ? C23 N3 C22 C21 -177(4) . . . . ? C23 C24 N1 U -16(2) . . . . ? C23 C24 N1 C1 163.3(19) . . . . ? C24 N1 C1 C2 -176.9(12) . . . . ? C22 N3 C23 C24 -173(4) . . . . ? C22 C21 N2 U 52.9(12) . . . . ? C22 C21 N2 C20 -115.8(13) . . . . ? C25 N3 C23 C24 52(5) . . . . ? C25 N3 C22 C21 -40(5) . . . . ? N1 C1 C2 C7 -0.1(19) . . . . ? N1 C1 C2 C3 177.8(12) . . . . ? C1 C2 C7 O1 -1.1(17) . . . . ? C1 C2 C7 C6 179.3(10) . . . . ? C1 C2 C3 C4 -178.8(12) . . . . ? C2 C7 C6 O6 179.5(9) . . . . ? C2 C7 C6 C5 -1.7(15) . . . . ? C2 C3 C4 C5 0(2) . . . . ? C7 C2 C3 C4 -0.9(19) . . . . ? C3 C2 C7 O1 -178.9(11) . . . . ? C3 C2 C7 C6 1.5(16) . . . . ? C3 C4 C5 C6 -1(2) . . . . ? C4 C5 C6 O6 -180.0(12) . . . . ? C4 C5 C6 C7 1.3(18) . . . . ? C6 O6 C8 C9 179.1(10) . . . . ? C8 O6 C6 C7 -177.9(9) . . . . ? C8 O6 C6 C5 3.4(15) . . . . ? C9 O5 C10 C11 170.5(10) . . . . ? C10 O5 C9 C8 172.8(10) . . . . ? C11 O4 C12 C13 -103.5(12) . . . . ? C12 O4 C11 C10 77.1(13) . . . . ? C13 O3 C14 C19 -78.0(12) . . . . ? C13 O3 C14 C15 105.3(12) . . . . ? C14 O3 C13 C12 -85.0(13) . . . . ? C14 C19 C18 C17 -3.9(15) . . . . ? C14 C19 C18 C20 171.4(10) . . . . ? C14 C15 C16 C17 -1.0(18) . . . . ? C19 C14 C15 C16 -3.3(16) . . . . ? C19 C18 C20 N2 15.0(18) . . . . ? C15 C14 C19 O2 -175.5(10) . . . . ? C15 C14 C19 C18 5.6(15) . . . . ? C15 C16 C17 C18 3(2) . . . . ? C16 C17 C18 C19 -0.2(18) . . . . ? C16 C17 C18 C20 -175.5(12) . . . . ? C17 C18 C20 N2 -169.6(12) . . . . ? C18 C20 N2 U 16.1(17) . . . . ? C18 C20 N2 C21A -176.0(12) . . . . ? C18 C20 N2 C21 -176.0(12) . . . . ? N2 C21A C22A N3A 40.7(16) . . . . ? N2 C21 C22 N3 -75(3) . . . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma _refln_scale_group_code -1 0 0 -8.307 0.71692 3 -2 0 0 7390.27 451.27 3 -3 0 0 -3.1449 1.92321 3 4 0 0 3576.01 229.106 4 -4 0 0 3842.62 227.898 3 -5 0 0 1.99456 2.97238 3 5 0 0 -1.446 3.8884 4 5 0 0 -1.5023 5.48776 5 6 0 0 3080.57 197.759 8 -6 0 0 3075.17 196.666 3 6 0 0 3377.4 198.814 5 7 0 0 -3.1529 7.14255 8 7 0 0 8.66746 8.08033 5 8 0 0 253.155 23.0838 8 8 0 0 210.153 23.38 5 9 0 0 -11.705 10.7998 8 9 0 0 -10.65 12.2476 5 -10 0 0 3.30671 12.2726 12 10 0 0 17.6771 15.7992 5 -10 0 0 7.0165 12.3808 11 -10 0 0 35.5895 13.4161 13 10 0 0 15.7992 14.9752 8 -11 0 0 -14.092 14.0304 11 -11 0 0 -13.668 12.6901 13 11 0 0 -8.2779 15.8011 8 -12 0 0 245.331 26.4914 13 13 0 0 -8.1551 8.41073 20 -13 0 0 -0.6436 9.70037 13 14 0 0 97.463 11.6782 20 -14 0 0 97.8104 16.4827 13 0 -1 0 -6.9253 0.63871 2 0 1 0 -5.747 0.78722 2 0 1 0 -7.2678 0.51117 3 -1 1 0 189.904 12.2813 3 -1 -1 0 190.583 12.3111 1 -1 -1 0 196.283 12.2272 3 -2 1 0 2456.77 154.193 3 -2 -1 0 2561.91 153.995 3 -3 -1 0 454.96 29.0139 3 -3 1 0 452.23 29.2713 3 -4 -1 0 1338.96 81.9575 3 4 -1 0 1327.08 83.6999 5 4 -1 0 1239.64 83.7502 4 -4 1 0 1353.59 82.1208 3 -5 1 0 1170.79 71.1992 3 -5 -1 0 1108.66 71.0572 3 5 1 0 1151.04 72.6842 5 5 -1 0 1173.64 73.2057 5 5 -1 0 1025.59 72.8569 4 6 -1 0 1980.72 129.612 4 6 1 0 2191.84 129.274 5 6 -1 0 2162.77 129.66 5 -6 -1 0 1941.38 127.281 3 -6 1 0 1986.09 127.187 3 6 -1 0 2034.83 128.577 8 6 1 0 1970.51 128.647 8 7 -1 0 191.736 20.2906 5 7 -1 0 189.92 19.4281 8 7 1 0 201.711 20.2406 5 7 1 0 199.3 19.6828 8 8 -1 0 1860.49 126.289 5 8 -1 0 1941.96 124.968 8 8 1 0 2056.2 125.792 8 9 -1 0 54.6065 14.0534 8 9 -1 0 66.8187 15.6947 5 9 1 0 45.9358 13.3803 8 10 1 0 794.796 57.2292 8 -10 1 0 748.579 55.5181 13 -10 -1 0 801.752 53.6385 12 -10 -1 0 745.607 55.295 13 -10 -1 0 771.317 53.3025 11 -10 1 0 777.151 53.544 12 10 -1 0 610.607 56.0492 5 10 -1 0 770.186 55.5174 8 -11 -1 0 132.718 16.7404 11 -11 1 0 162.362 23.0759 13 -11 -1 0 122.767 17.6645 13 11 1 0 90.8083 19.8406 8 11 -1 0 92.2843 18.9871 8 -12 -1 0 602.548 45.3917 11 -12 1 0 740.99 48.8937 13 -12 -1 0 664.68 47.9261 13 12 -1 0 622.996 45.0769 20 -13 -1 0 44.498 11.542 13 -13 1 0 46.2293 11.6703 13 13 1 0 45.2199 9.98449 20 13 -1 0 54.8077 9.11611 20 14 1 0 175.593 14.5051 20 14 -1 0 147.595 13.8805 20 0 2 0 6582.82 405.764 2 0 -2 0 6712.81 405.763 2 -1 -2 0 1680.55 103.223 2 1 2 0 1604.99 103.238 2 -1 2 0 1746.74 102.914 3 -2 -2 0 911.994 59.5531 1 -2 2 0 983.208 59.6213 3 -2 -2 0 987.606 59.4473 3 3 -2 0 1467.96 95.8435 4 -3 2 0 1559.59 93.9052 3 -3 -2 0 1531.4 93.5195 3 -3 -2 0 1503.18 93.7051 1 4 -2 0 4118.65 270.033 4 -4 -2 0 4441.65 267.421 3 -4 2 0 4432.3 267.727 3 4 -2 0 4458.5 269.478 5 5 -2 0 812.899 51.6754 5 -5 -2 0 763.8 48.949 3 5 -2 0 741.464 51.8338 4 -5 2 0 731.394 49.0204 3 -6 2 0 623.364 41.835 3 -6 -2 0 616.976 41.8678 3 6 -2 0 642.441 45.2196 4 6 -2 0 641.808 43.7969 8 6 2 0 606.394 43.8598 8 6 -2 0 666.299 44.9719 5 7 -2 0 220.59 21.33 8 7 -2 0 236.585 22.8137 5 7 2 0 227.262 22.3855 8 8 -2 0 18.5877 10.4992 8 8 2 0 34.6561 11.8865 8 8 -2 0 28.343 12.2266 5 9 -2 0 189.204 22.6828 8 9 -2 0 186.458 23.6901 5 9 2 0 190.246 23.9442 8 -10 -2 0 26.9297 13.5803 13 10 -2 0 30.916 15.9452 5 10 -2 0 43.2506 14.2973 8 10 2 0 44.9199 15.5601 8 -10 -2 0 51.0159 13.1694 11 -10 2 0 43.7146 13.204 12 -10 2 0 56.2108 15.8181 13 11 -2 0 -13.083 18.4806 8 -11 -2 0 -4.7551 11.9338 13 -11 2 0 1.1941 13.2417 13 11 2 0 1.86464 15.3214 8 -11 -2 0 11.3871 11.4743 11 11 -2 0 18.2132 10.0356 20 -11 -2 0 21.494 9.02385 11 -12 -2 0 67.4291 13.7071 13 -12 -2 0 99.1704 15.1987 11 -12 2 0 44.5486 14.65 13 12 -2 0 62.3914 11.1333 20 -13 2 0 56.6795 11.6045 13 13 -2 0 37.4695 8.55104 20 -13 -2 0 41.2004 10.0634 11 -13 -2 0 38.2952 11.1459 13 14 2 0 60.3075 8.19283 20 0 3 0 1.05775 1.13981 3 0 -3 0 3.23578 1.7732 2 1 -3 0 210.668 16.9343 4 1 3 0 231.935 14.7987 3 1 -3 0 228.873 15.5854 2 -1 -3 0 226.421 15.3172 2 -1 3 0 231.865 14.8491 3 -2 3 0 242.793 15.9424 3 2 -3 0 235.937 18.1282 4 -3 -3 0 761.319 50.7247 4 3 -3 0 810.526 52.4924 4 -3 -3 0 749.201 50.0542 1 -3 3 0 838.878 49.8967 3 4 -3 0 1393.04 93.7587 4 -4 3 0 1441.47 90.7549 3 4 -3 0 1523.02 92.9695 5 -5 3 0 1434.11 88.8147 3 -5 -3 0 1307.04 88.1731 3 5 -3 0 1524.44 91.4146 5 5 -3 0 1465.83 92.7666 4 5 3 0 1325.19 90.1683 8 6 -3 0 676.147 47.3046 5 6 -3 0 695.784 48.6838 4 6 3 0 638.695 46.4737 8 7 3 0 1198.84 77.6094 8 7 -3 0 1120.63 79.4035 4 7 -3 0 1191.92 78.9519 5 8 3 0 625.799 44.4062 8 8 -3 0 543.497 45.2934 5 -9 -3 0 904.379 60.7437 11 9 -3 0 774.445 63.2269 5 9 3 0 964.302 63.8137 8 -10 -3 0 435.222 35.6118 13 -10 -3 0 397.394 31.7131 11 10 -3 0 369.87 32.5617 20 10 3 0 398.391 37.7146 8 10 -3 0 434.321 43.0725 17 -10 3 0 413.132 36.1175 13 -10 -3 0 393.353 33.9639 11 -10 3 0 417.38 33.3033 12 -11 -3 0 563.143 41.1869 13 -11 3 0 537.772 42.771 13 11 -3 0 492.399 37.9707 20 -11 -3 0 535.916 38.8583 11 -12 3 0 463.088 33.6156 13 -12 -3 0 365.492 29.0565 11 -12 -3 0 359.113 30.9407 13 12 -3 0 328.991 28.4556 20 13 -3 0 230.108 23.3443 20 -13 -3 0 243.083 20.6229 11 -13 -3 0 236.256 21.3198 13 -13 3 0 281.197 23.7514 13 0 -4 0 34.4315 4.54213 2 0 -4 0 30.9667 5.73367 4 0 4 0 30.1075 3.69547 3 1 -4 0 4711.32 289.279 2 -1 4 0 4826.24 288.397 3 1 4 0 4696.28 288.296 3 -1 -4 0 4658.71 290.064 4 1 -4 0 4739.66 290.689 4 -1 -4 0 4639.45 289.035 2 2 -4 0 452.023 30.1188 2 -2 -4 0 431.785 30.4931 4 2 -4 0 465.576 32.0297 4 -2 4 0 458.682 29.0758 3 2 4 0 436.518 28.8187 3 -3 4 0 1922.4 116.576 3 -3 -4 0 1778.19 117.745 4 3 -4 0 2000.68 120.113 4 3 -4 0 1821.57 118.776 5 4 -4 0 860.503 59.3422 4 4 -4 0 871.311 58.2482 5 -4 4 0 868.001 55.534 3 5 -4 0 1804.18 116.852 4 5 -4 0 1857.18 114.854 5 -5 4 0 1705.22 112.256 3 6 -4 0 79.3667 14.8625 5 6 4 0 60.7633 12.8467 8 6 -4 0 101.498 16.2433 4 7 -4 0 495.218 39.5569 5 7 -4 0 498.329 41.1383 4 7 4 0 508.242 38.3503 8 8 4 0 18.0903 11.908 8 8 -4 0 -9.4581 12.9837 5 -9 -4 0 31.7102 12.963 11 9 -4 0 24.8917 9.27206 11 9 -4 0 1.31996 14.1934 5 -9 4 0 17.1776 11.9384 12 -9 -4 0 27.0183 13.5102 13 9 4 0 13.1274 14.274 8 -9 -4 0 23.0253 8.79351 11 10 4 0 -11.469 15.222 8 -10 -4 0 -1.0839 12.7149 13 10 -4 0 1.23568 16.293 17 -10 -4 0 12.1136 8.66712 11 10 -4 0 1.48369 14.7121 11 11 -4 0 51.6629 18.4593 17 -11 -4 0 90.4727 14.6908 11 -11 -4 0 58.7211 13.9581 13 -11 4 0 43.8205 15.5292 13 -12 -4 0 12.133 9.49585 13 -12 4 0 9.46015 11.8059 13 -12 -4 0 10.1216 7.70634 11 12 -4 0 -27.774 16.0358 17 -13 -4 0 77.6819 12.3943 11 -13 4 0 105.29 15.9862 13 0 5 0 3.40065 1.80608 3 0 -5 0 0.538 2.1947 2 0 -5 0 1.24879 3.01179 4 1 5 0 99.9987 7.81927 3 1 -5 0 90.6151 10.4875 4 1 -5 0 97.0997 8.99403 2 -1 -5 0 91.6856 10.439 4 -1 -5 0 92.9121 8.69004 2 -1 5 0 96.8225 7.85514 3 -2 5 0 170.966 12.6078 3 2 -5 0 175.99 16.4615 4 -2 -5 0 157.1 14.7734 4 2 5 0 172.441 12.3379 3 -3 5 0 1944.26 121.9 3 3 -5 0 2091.11 126.426 4 3 5 0 1854.6 121.44 3 4 -5 0 21.0444 8.00316 4 -4 5 0 11.8924 4.37813 3 5 -5 0 1729.88 116.547 4 5 -5 0 1796.25 113.986 5 -6 -5 0 46.4581 15.4734 9 6 -5 0 54.0082 12.4131 5 6 -5 0 55.5848 13.7221 4 7 -5 0 1870.82 121.572 10 7 -5 0 1860.59 124.317 5 7 -5 0 2008.53 128.345 4 8 -5 0 124.785 20.825 5 8 -5 0 147.973 24.9043 4 9 -5 0 1636.68 108.306 17 9 -5 0 1525.98 101.101 11 -9 -5 0 1633 103.88 13 -9 -5 0 1547.71 101.501 11 -10 -5 0 4.41531 8.03425 11 -10 -5 0 -14.919 12.332 13 10 -5 0 -26.314 16.113 17 10 -5 0 13.093 8.44998 11 -11 -5 0 632.327 45.1314 11 11 -5 0 682.247 54.2455 17 -12 -5 0 1.88967 7.54513 11 12 -5 0 -15.174 14.7617 17 -12 5 0 -0.8161 17.9638 13 -13 -5 0 276.782 30.4899 15 13 -5 0 271.047 33.2507 17 0 6 0 408.262 26.4595 3 0 -6 0 387.981 28.2743 6 0 -6 0 390.52 29.7411 4 1 -6 0 2379.95 145.478 4 1 6 0 2330.73 141.59 3 -1 -6 0 2220.59 144.383 4 -1 6 0 2221.19 141.538 3 2 6 0 41.9184 5.53926 3 -2 -6 0 45.0283 9.8208 4 2 -6 0 50.8473 10.0229 4 -2 6 0 47.3057 5.96098 3 3 -6 0 2440.95 156.543 4 4 -6 0 481.541 38.9981 4 -5 -6 0 1305.99 91.772 9 5 -6 0 1477.83 96.5032 4 -6 -6 0 43.7015 14.0605 9 6 -6 0 51.6527 12.4931 10 6 -6 0 69.3693 16.9663 4 7 -6 0 139.971 24.8939 4 7 -6 0 96.8539 15.12 10 7 -6 0 125.071 26.424 5 8 -6 0 25.3943 27.5025 17 -8 -6 0 30.644 9.97413 11 8 -6 0 24.2507 13.8517 5 8 -6 0 27.4875 11.7678 10 8 -6 0 26.1132 9.91305 11 -9 -6 0 32.7675 9.74593 11 9 -6 0 2.23829 17.5482 17 9 -6 0 32.9247 9.31191 11 10 -6 0 16.412 14.8768 17 10 -6 0 9.13282 8.13921 11 -10 -6 0 17.5073 8.58008 11 11 -6 0 13.0969 8.8628 11 11 -6 0 -11.623 13.6852 17 -11 -6 0 8.60049 8.21962 11 -12 -6 0 17.4802 7.00771 11 -12 -6 0 9.12123 14.8961 15 12 -6 0 19.5857 12.6993 17 0 -7 0 7.02751 5.50555 4 1 -7 0 14.564 9.52141 6 -1 -7 0 12.5198 5.94788 4 1 -7 0 7.84951 8.0272 4 2 -7 0 59.9765 12.3843 4 3 -7 0 538.923 41.5359 4 -3 -7 0 483.329 39.7956 9 4 -7 0 129.181 20.8712 4 -4 -7 0 123.988 18.331 9 5 -7 0 891.897 65.1323 10 -5 -7 0 947.369 66.4959 9 5 -7 0 1019.24 72.0144 4 6 -7 0 369.868 38.4429 4 6 -7 0 360.899 32.6912 10 -6 -7 0 369.701 33.1553 9 7 -7 0 968.432 64.5145 11 -7 -7 0 963.542 67.5777 9 -7 -7 0 959.576 64.7625 11 7 -7 0 961.405 65.9691 10 8 -7 0 400.863 44.716 17 8 -7 0 407.388 38.2851 6 -8 -7 0 508.684 42.282 18 8 -7 0 401.253 35.454 10 8 -7 0 450.839 33.417 11 -8 -7 0 414.155 33.9078 11 -8 -7 0 445.662 49.8589 15 -9 -7 0 639.007 62.4333 15 -9 -7 0 684.502 46.9715 11 9 -7 0 665.743 54.5037 17 9 -7 0 641.458 45.4719 11 -9 -7 0 650.778 52.5295 18 -10 -7 0 218.573 22.024 11 -10 -7 0 203.798 37.3193 15 10 -7 0 220.445 20.3907 11 10 -7 0 172.971 31.3423 17 11 -7 0 463.838 37.3343 17 11 -7 0 374.591 29.8782 11 -11 -7 0 414.767 31.3568 11 -11 -7 0 440.653 43.6913 15 12 -7 0 141.46 21.4961 17 -12 -7 0 127.907 25.2284 15 -12 -7 0 149.732 14.8912 11 0 -8 0 3475.17 220.123 4 1 -8 0 1321.92 81.2191 6 -1 -8 0 1116.67 82.1564 4 1 -8 0 1238.67 84.0125 4 -2 -8 0 1396.62 92.1443 9 2 -8 0 1443.55 95.4258 10 2 -8 0 1332.62 95.1835 4 2 -8 0 1408.55 92.6231 6 -3 -8 0 624.718 45.7552 9 3 -8 0 560.567 43.8584 10 3 -8 0 604.615 49.29 4 3 -8 0 622.639 48.6273 6 -4 -8 0 1012.73 68.133 9 4 -8 0 906.508 67.196 10 4 -8 0 960.165 70.2791 6 4 -8 0 976.833 72.9797 4 5 -8 0 377.395 34.953 10 5 -8 0 418.103 39.3654 6 5 -8 0 371.986 40.8209 4 -5 -8 0 422.488 35.9862 9 6 -8 0 730.634 53.4905 6 6 -8 0 702.267 51.8019 10 -6 -8 0 669.155 48.2966 11 6 -8 0 677.784 48.1353 11 -7 -8 0 32.4539 9.93197 11 7 -8 0 38.7614 10.0124 11 7 -8 0 20.7719 32.0145 19 7 -8 0 50.4961 16.1302 6 -7 -8 0 24.6734 16.8078 18 -7 -8 0 42.7037 19.7922 15 7 -8 0 11.6939 20.8557 17 7 -8 0 38.0542 13.4542 10 -8 -8 0 66.5604 11.8752 11 -8 -8 0 67.2735 17.8906 18 -8 -8 0 87.7099 23.7893 15 8 -8 0 49.7539 19.4348 17 8 -8 0 93.9121 15.4045 11 8 -8 0 55.9316 14.8065 10 9 -8 0 47.063 9.32015 11 9 -8 0 61.3134 13.1953 10 -9 -8 0 41.9838 15.0798 18 9 -8 0 33.5989 16.7395 17 -9 -8 0 24.8849 10.2263 11 -9 -8 0 66.2526 21.1672 15 -10 -8 0 -3.0953 16.1256 15 -10 -8 0 -0.6032 13.0234 18 -10 -8 0 7.22333 8.13254 11 10 -8 0 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120.99 5 -4 0 -3 1930.79 119.087 3 -4 0 3 1914.17 119.182 3 5 0 3 5.52067 5.85135 8 -5 0 -3 15.045 3.89396 3 -5 0 3 6.22734 3.4403 3 5 0 -3 12.272 6.47352 5 5 0 -3 -1.4231 6.49036 8 5 0 3 6.14427 5.17163 5 6 0 3 1325.5 95.5066 8 6 0 3 1388.64 96.1215 5 6 0 -3 1541.94 96.699 8 -6 0 3 1564.67 94.5487 3 -6 0 -3 1530.79 94.419 3 6 0 -3 1630.05 97.4227 5 7 0 3 30.5212 9.97812 5 7 0 3 4.52692 8.9346 8 7 0 -3 29.3726 9.67247 5 7 0 -3 22.9685 8.5819 8 8 0 3 2346.66 146.354 8 8 0 -3 2470.79 146.077 8 8 0 3 2110.5 146.202 5 8 0 -3 2208.79 146.474 5 9 0 3 4.00396 13.3293 8 9 0 3 -2.0521 13.6415 5 9 0 -3 11.7948 12.3943 8 9 0 -3 8.8744 12.7094 5 10 0 -3 985.783 68.1014 8 -10 0 -3 987.989 66.2274 12 10 0 -3 810.248 68.5018 5 -10 0 -3 940.022 64.5128 11 -10 0 -3 958.022 65.7382 13 10 0 3 1028.76 69.5279 8 -10 0 3 1010.4 68.0151 13 11 0 3 -16.854 16.6518 8 11 0 -3 -6.2153 16.6241 8 -11 0 3 -8.6132 12.3205 13 -11 0 -3 -9.1251 10.4277 11 11 0 -3 12.3985 10.0364 20 -11 0 -3 -22.467 11.1578 12 -11 0 -3 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35.9872 8 9 -2 -3 483.712 37.4891 5 -10 -2 -3 757.752 59.2202 13 10 2 -3 791.834 61.2151 8 10 -2 3 926.665 65.9326 17 -10 -2 -3 697.891 57.2258 11 10 -2 3 845.823 71.8357 8 -10 2 -3 904.656 60.0366 13 10 2 3 948.054 63.4428 8 10 -2 -3 851.686 57.3254 20 10 -2 -3 852.475 60.4709 8 -10 -2 3 838.461 57.7383 11 -10 2 -3 842.971 58.1087 11 10 -2 -3 807.215 56.869 11 -10 2 -3 960.523 60.1646 12 -10 -2 3 880.855 60.8042 13 -11 -2 -3 228.127 23.2585 11 -11 -2 -3 179.185 24.7528 13 -11 2 -3 198.535 26.0212 13 -11 -2 3 246.845 26.4395 13 11 -2 -3 199.977 20.8425 20 -11 2 -3 209.612 24.1439 12 -12 -2 -3 409.556 34.0893 13 -12 -2 -3 465.73 34.8738 11 -12 2 3 486.972 37.8216 13 -12 -2 3 445.46 36.1394 13 -12 2 -3 513.571 36.5196 13 12 -2 -3 438.315 33.3161 20 13 2 -3 154.119 17.6629 20 -13 -2 -3 182.397 17.3307 11 -13 2 3 161.512 21.4306 13 -13 2 -3 192.239 20.3186 13 13 -2 -3 206.186 18.4055 12 13 -2 -3 168.969 17.3141 20 -13 -2 3 197.12 19.389 13 0 3 -3 1478.93 93.9388 3 0 3 3 1538.53 93.9928 3 0 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999.84 65.1326 5 -5 3 -3 997.028 62.5833 3 5 -3 -3 1004.05 66.4731 5 -5 -3 3 990.722 62.3786 3 5 -3 -3 1024.3 67.0831 4 5 3 3 885.163 63.9629 8 5 -3 -3 1004.93 67.9638 8 6 3 -3 624.754 39.6826 8 6 -3 -3 516.736 41.549 8 6 -3 -3 517.43 40.5841 4 6 -3 -3 489.879 39.879 5 7 -3 3 676.218 48.7611 5 7 3 -3 678.384 47.1191 8 7 3 3 575.458 47.192 8 7 -3 -3 665.526 49.5996 4 7 -3 -3 664.479 48.8763 5 7 -3 -3 676.221 50.2268 8 8 3 -3 96.2107 15.498 8 8 -3 3 66.1005 15.5494 5 8 -3 -3 46.3253 14.8959 4 8 -3 -3 60.392 21.757 8 8 -3 -3 58.9544 15.058 5 8 3 3 31.0897 12.3594 8 9 -3 3 89.8722 19.9117 5 -9 -3 -3 87.9043 13.5009 11 9 3 -3 106.118 17.8396 8 9 -3 -3 77.7371 18.7913 5 -9 -3 3 80.8866 13.1754 11 9 -3 -3 68.8478 11.1344 11 9 3 3 70.8206 16.8092 8 -10 -3 -3 44.3357 14.3351 13 -10 -3 -3 30.5915 11.5542 11 10 3 -3 47.9533 16.0213 8 10 -3 3 17.1808 18.2219 17 -10 -3 3 60.0244 14.1804 13 -10 3 -3 68.9715 14.127 12 10 -3 -3 48.0968 10.1041 11 -10 -3 3 41.512 10.8657 11 -10 3 -3 61.2681 14.7845 13 10 3 3 55.9425 17.8268 8 10 -3 -3 58.7377 10.9863 20 11 -3 3 42.842 16.7268 17 -11 -3 -3 36.4549 11.8985 11 -11 -3 -3 7.6402 20.177 13 -11 -3 3 41.8341 10.0026 11 -11 3 -3 42.4638 12.1264 12 11 -3 -3 39.0078 9.97281 20 11 -3 -3 31.6458 9.55335 11 -11 -3 3 20.8315 12.7036 13 -11 3 -3 28.8663 13.491 13 -12 -3 -3 36.4989 10.9496 11 12 -3 3 32.6611 16.871 17 -12 -3 -3 41.2393 9.0378 11 -12 3 -3 25.5738 12.1773 13 12 -3 -3 34.5365 9.40686 20 -12 -3 3 39.6697 11.8318 13 13 3 -3 47.8598 9.41566 20 -13 -3 -3 59.4499 8.84616 11 -13 3 3 31.3114 12.1906 13 -13 -3 3 42.0269 10.4874 13 -13 3 -3 46.5836 10.6565 13 13 -3 -3 49.9034 8.63879 20 13 -3 -3 66.1622 11.4968 12 0 -4 -3 18.3711 3.69146 2 0 -4 3 9.95886 3.80997 4 0 4 -3 11.2168 2.32985 3 0 4 3 14.3576 2.58546 3 0 -4 -3 7.80292 4.5772 4 1 4 3 91.5663 6.92778 3 1 -4 -3 82.1531 10.4606 4 -1 4 -3 89.0366 7.03624 3 -1 -4 3 89.7296 9.24323 4 1 -4 -3 86.6053 8.29533 2 2 4 3 237.724 15.0765 3 2 -4 -3 228.69 16.9598 2 2 -4 -3 207.109 17.8124 6 -2 4 -3 225.275 15.2333 3 2 -4 -3 207.655 18.9006 4 -2 -4 3 216.681 17.3294 4 3 -4 3 1887.49 121.093 4 -3 4 3 1942.2 118.517 3 3 -4 3 1801.97 119.7 5 -3 -4 -3 1819.17 119.417 1 -3 -4 -3 1775.29 118.852 7 3 -4 -3 2042.14 121.171 5 3 -4 -3 2018.42 123.042 4 -3 -4 3 1982.28 120.929 4 -3 4 -3 1985.58 118.336 3 3 -4 -3 1842.77 120.22 6 -4 -4 -3 299.254 19.451 7 4 -4 3 285.67 20.9363 5 4 -4 -3 222.068 22.5022 5 -4 -4 3 222.449 20.016 4 -4 4 -3 207.813 17.2823 3 4 -4 -3 226.513 22.4275 4 5 -4 3 871.809 67.5447 5 5 -4 3 1022.72 69.8011 4 -5 -4 3 1043.44 69.1856 4 5 4 3 964.368 67.6711 8 -5 4 -3 1030.53 65.7047 3 5 -4 -3 1087.5 70.3731 5 5 -4 -3 1162.96 71.5849 4 6 -4 3 211.529 20.9258 5 6 -4 -3 188.808 21.8345 5 6 -4 -3 186.508 21.8704 4 7 -4 3 1236.61 85.7208 5 7 -4 -3 1263.95 85.8657 5 7 4 3 1205.35 84.1985 8 7 -4 -3 1359.9 88.1479 4 8 -4 3 217.145 22.7198 10 8 4 -3 205.803 24.9891 8 8 -4 3 176.574 27.3268 5 8 -4 -3 190.375 26.1031 4 8 4 3 181.048 24.6419 8 8 -4 -3 181.943 25.0133 5 9 -4 3 1887.33 120.359 17 9 -4 3 1746.5 114.792 10 -9 -4 -3 1774.92 114.951 11 9 -4 3 1563.99 119.3 5 9 4 -3 1743.69 117.391 8 -9 4 -3 1972.83 116.261 12 9 -4 -3 1945.53 125.596 17 -9 4 -3 1894.45 116.812 13 9 4 3 1830.46 118.666 8 9 -4 -3 1512.65 118.367 5 -9 -4 3 1877.03 117.527 13 9 -4 -3 1808.01 114.053 11 -9 -4 3 1831.84 115.198 11 -10 -4 -3 111.002 16.1898 11 10 -4 3 124.532 21.0914 17 10 4 -3 96.1212 20.784 8 -10 -4 3 140.709 19.8153 13 -10 4 -3 166.809 23.5532 13 10 -4 -3 168.756 17.914 11 10 -4 -3 143.12 19.7547 20 10 -4 -3 121.074 22.8148 17 -10 4 -3 190.396 21.0685 12 10 4 3 196.843 27.9531 8 -11 -4 -3 638.871 44.5001 11 11 -4 3 656.529 51.1247 17 -11 -4 -3 643.385 43.2196 11 -11 4 -3 600.816 45.939 13 11 -4 -3 544.79 42.2839 20 -11 4 -3 656.471 44.6493 12 11 -4 -3 582.675 42.7579 11 -11 -4 3 632.46 46.2254 13 -11 -4 3 587.572 43.4611 11 12 -4 3 35.8433 16.8664 17 -12 -4 -3 42.7031 9.01912 11 -12 -4 3 40.9173 12.0572 13 12 -4 -3 46.8115 10.883 12 12 -4 -3 45.7312 8.76307 20 -12 -4 3 48.7575 9.32556 11 -12 4 -3 35.745 12.5792 13 13 4 -3 273.221 21.1563 20 -13 -4 -3 284.372 20.7025 11 13 -4 -3 235.047 20.507 20 -13 -4 3 286.424 20.9979 13 -13 4 -3 241.724 22.7594 13 13 -4 -3 264.09 21.5922 12 0 -5 -3 63.266 8.97762 6 0 5 -3 73.2874 6.5236 3 0 -5 -3 58.5364 10.5342 4 0 5 3 77.176 6.64455 3 0 -5 -3 76.1351 8.31136 7 0 -5 3 78.338 9.63461 4 1 -5 3 4829.3 272.386 4 -1 -5 -3 4213.9 269.323 6 -1 5 3 4428.65 268.898 3 -1 -5 -3 4601.07 269.8 7 1 5 -3 4333.27 268.74 3 -1 5 -3 4370.13 268.786 3 1 -5 -3 3883.12 271.811 4 -1 -5 3 4493.33 271.777 4 1 5 3 4419.4 268.747 3 1 -5 -3 4264.32 270.095 6 2 5 -3 134.404 9.62834 3 2 -5 3 117.464 12.9379 4 -2 -5 -3 127.437 11.6644 7 -2 -5 -3 152.521 12.878 6 -2 5 3 129.435 9.90254 3 -2 -5 3 110.462 12.0978 4 2 -5 -3 99.1989 14.6124 6 2 5 3 107.522 9.24586 3 2 -5 -3 106.178 14.2853 4 -2 5 -3 114.199 9.52856 3 -3 -5 -3 2283.27 148.485 1 3 5 -3 2348.15 146.574 3 -3 -5 -3 2418.64 147.77 7 3 -5 3 2675.44 151.203 4 -3 5 3 2440.8 147.117 3 -3 5 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20 -9 -5 3 41.1351 10.8978 11 -9 -5 3 28.8684 13.9154 13 -9 5 -3 41.5667 14.5714 13 -10 -5 -3 107.181 15.2583 11 10 -5 3 82.2083 18.5517 17 -10 -5 -3 101.746 16.0588 11 10 -5 -3 98.0469 19.8855 17 -10 -5 3 80.3526 13.2901 11 -10 5 -3 102.518 17.4663 12 10 -5 -3 91.5774 13.0168 20 -10 5 -3 57.8006 16.9762 13 -10 -5 3 87.6816 16.0857 13 10 -5 -3 95.2992 15.4692 11 11 -5 3 51.8992 16.3478 17 -11 -5 -3 54.6052 10.0459 11 11 -5 -3 34.9284 9.24832 11 11 -5 -3 41.3175 10.5424 12 11 -5 -3 33.0725 17.2591 17 -11 -5 3 39.9436 9.47854 11 -11 -5 3 21.8554 12.5533 13 11 -5 -3 42.8065 10.2006 20 -11 5 -3 50.6512 13.0022 13 -12 -5 -3 22.0884 15.4479 15 -12 -5 -3 19.3144 8.10403 11 12 -5 3 28.7201 12.7474 17 -12 -5 3 40.6786 8.84161 13 12 -5 -3 4.435 7.73745 20 -12 -5 3 21.6814 7.54004 11 12 -5 -3 21.0897 14.8164 17 12 -5 -3 35.1911 9.30471 12 -12 5 -3 14.9937 10.7704 13 12 -5 -3 21.4702 7.95404 11 13 -5 3 29.4361 16.7245 17 -13 -5 3 46.7486 13.266 15 0 6 -3 97.6817 8.71288 3 0 -6 -3 98.6091 12.1608 6 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4 -7 -3 569.831 49.0515 4 5 -7 3 926.435 67.7013 4 5 -7 3 904.874 62.3789 10 -5 -7 -3 915.794 63.8529 9 5 -7 -3 842.299 64.0307 10 5 -7 -3 943.601 65.8254 6 5 -7 -3 906.924 69.2663 4 6 -7 3 337.969 37.4027 4 6 -7 3 359.752 31.434 10 -6 -7 -3 367.031 33.7483 9 6 -7 -3 333.076 34.4286 10 6 -7 -3 347.108 38.9016 4 6 -7 -3 401.38 35.8074 6 7 -7 3 61.4289 12.1811 11 7 -7 3 55.4512 12.9059 13 7 -7 3 78.4016 13.2017 10 -7 -7 -3 50.4365 25.978 15 7 -7 3 32.0766 24.1018 17 -7 -7 -3 40.0346 15.1186 9 7 -7 -3 82.6736 18.2175 6 7 -7 -3 72.082 11.4076 11 7 -7 -3 49.7383 23.5154 17 -7 -7 3 62.5735 13.1435 13 -7 -7 3 45.6162 11.4481 11 8 -7 3 17.7109 11.1942 10 -8 -7 -3 4.49832 16.7334 18 -8 -7 -3 15.1219 10.2798 21 8 -7 3 18.4804 9.67431 11 -8 -7 -3 26.0291 22.8505 15 8 -7 3 28.6354 16.3064 17 -8 -7 -3 6.16588 14.7433 9 -8 -7 3 26.9459 12.0383 13 -8 -7 3 12.7847 10.092 11 -8 -7 3 45.2293 19.3189 18 8 -7 -3 35.0663 18.7263 17 9 -7 3 80.0945 11.9355 11 9 -7 3 79.4109 13.4766 10 -9 -7 -3 39.2315 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421.35 57.9622 17 6 -8 -3 452.713 42.3187 10 -6 -8 3 484.747 49.1963 15 -6 -8 3 466.194 37.0003 11 -6 -8 3 429.322 36.7813 13 6 -8 -3 494.64 45.1252 6 6 -8 -3 488.996 37.6788 11 7 -8 3 498.426 55.7431 17 7 -8 3 492.135 57.6677 19 -7 -8 -3 509.815 46.7895 18 7 -8 3 462.44 37.7644 13 -7 -8 -3 507.707 36.3315 21 7 -8 3 468.504 36.673 11 -7 -8 -3 410.602 41.0221 9 7 -8 3 484.293 38.1608 10 -7 -8 -3 432.615 50.6698 15 -7 -8 3 590.278 45.5233 18 7 -8 -3 470.844 43.9057 6 7 -8 -3 490.126 53.228 17 7 -8 -3 484.673 41.6462 10 -7 -8 3 466.978 36.6493 13 -7 -8 3 486.929 50.8906 15 7 -8 -3 511.9 36.4229 11 -7 -8 3 493.49 36.9258 11 8 -8 3 488.541 69.9275 19 -8 -8 -3 623.67 51.706 18 -8 -8 -3 560.769 59.2835 15 8 -8 3 649.259 45.023 10 8 -8 3 570.831 53.0697 17 -8 -8 -3 588.374 47.4309 9 -8 -8 -3 664.853 43.8274 21 8 -8 3 628.866 43.8642 11 -8 -8 3 562.315 49.5121 18 -8 -8 3 632.873 57.2566 15 -8 -8 3 629.735 44.4442 11 8 -8 -3 644.962 43.2899 11 8 -8 -3 670.802 56.6224 17 -9 -8 -3 290.16 25.5482 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4 -2 -9 -3 1272.93 84.605 9 -2 -9 -3 1317.47 81.6846 10 -2 -9 3 1118.57 85.4958 4 2 -9 -3 1249.12 83.0462 10 2 -9 -3 1318.85 86.1226 6 3 -9 3 110.875 17.1288 10 3 -9 3 120.639 14.3564 11 -3 -9 -3 95.2123 18.043 9 3 -9 -3 185.295 25.348 10 3 -9 -3 158.471 26.6201 4 4 -9 3 639.173 42.9622 11 -4 -9 -3 622.126 48.4532 9 4 -9 3 621.175 47.4364 10 4 -9 3 616.889 44.6053 13 4 -9 -3 592.938 54.4253 6 -4 -9 3 586.277 42.1726 11 4 -9 -3 581 49.4249 10 -5 -9 -3 149.092 16.7989 21 5 -9 3 131.354 18.1567 10 5 -9 3 124.056 17.4999 11 5 -9 3 130.341 20.7708 13 -5 -9 -3 133.896 21.1652 9 5 -9 3 224.745 45.7486 19 -5 -9 -3 121.29 24.2875 15 -5 -9 -3 88.2686 22.5415 18 5 -9 -3 135.748 20.9506 10 5 -9 -3 118.427 24.3142 6 -5 -9 3 130.375 16.5116 11 5 -9 -3 140.332 36.3562 19 -5 -9 3 154.24 30.4744 18 5 -9 -3 143.135 24.1012 11 -5 -9 3 179.055 30.0304 15 -6 -9 -3 362.49 40.5857 15 6 -9 3 339.507 29.5378 13 6 -9 3 386.854 52.5778 19 -6 -9 -3 308.544 33.3301 9 -6 -9 -3 318.584 27.4237 21 6 -9 3 302.562 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48.8953 5 9 -2 -4 628.717 46.0801 8 9 2 4 631.637 48.1369 8 -9 2 -4 640.872 44.4083 11 9 -2 -4 514.04 47.4219 5 9 -2 -4 553.512 42.4965 11 10 -2 4 265.812 39.7697 17 10 2 -4 290.978 32.3797 8 -10 -2 -4 302.869 27.4405 11 -10 -2 -4 263.312 30.4717 13 10 2 4 322.313 35.0483 8 10 -2 -4 313.683 31.2473 8 10 -2 -4 313.841 27.0979 20 -10 2 -4 354.635 29.0432 11 10 -2 -4 335.454 26.7862 11 -10 2 -4 347.439 30.7755 12 -10 -2 4 359.085 32.796 13 -10 2 -4 397.684 31.2809 13 -11 -2 -4 330.163 29.325 11 11 -2 4 302.675 47.1892 17 -11 -2 -4 320.625 30.5386 13 -11 -2 4 351.102 31.0124 13 11 -2 -4 383.805 27.9834 20 -11 2 -4 391.655 30.1248 11 -11 2 -4 352.463 30.4339 12 11 -2 -4 288.232 33.2145 11 -11 2 -4 360.246 31.8958 13 -12 -2 -4 210.94 22.6624 11 12 2 -4 225.382 22.1856 20 -12 2 -4 279.525 24.9476 13 -12 2 -4 234.428 23.1205 12 -12 -2 4 232.148 24.7348 13 12 -2 -4 245.925 21.5901 20 12 -2 -4 246.414 22.2913 12 -13 -2 -4 120.29 14.9765 11 -13 2 4 136.286 18.6737 13 13 2 -4 140.613 15.2591 20 -13 -2 4 128.17 16.7505 13 -13 2 -4 151.05 17.216 13 13 -2 -4 155.686 15.0683 20 13 -2 -4 135.653 15.9956 12 0 3 -4 6150.41 384.748 3 0 -3 4 6240.37 386.876 4 0 -3 -4 6381.49 386.195 2 0 3 4 6442.68 384.811 3 -1 -3 -4 760.622 48.9052 1 1 3 -4 785.817 47.3387 3 1 -3 4 790.367 49.5128 4 -1 -3 -4 790.204 48.6935 2 -1 3 4 775.358 47.4241 3 1 3 4 749.476 47.2135 3 -1 -3 4 714.495 49.3886 4 1 -3 -4 741.415 48.6463 2 -1 3 -4 728.99 47.2844 3 2 -3 4 1916.99 119.551 4 2 -3 4 1862.55 118.907 5 -2 -3 -4 1774.28 118.899 1 -2 3 4 1825.14 117.626 3 2 3 4 2041.33 117.337 3 -2 -3 4 2009.89 120.021 4 -2 3 -4 1951.03 117.483 3 2 -3 -4 1992.28 119.194 2 2 -3 -4 1793.42 120.945 4 3 -3 4 1928.82 121.521 4 -3 3 4 1840.06 119.614 3 3 -3 4 2012.98 120.927 5 -3 -3 -4 1769.08 120.735 1 3 -3 -4 2221.81 122.327 5 3 -3 -4 1850.43 123.159 4 3 -3 -4 1919.66 121.383 2 -3 3 -4 1912.97 119.408 3 4 -3 4 994.308 64.3072 5 -4 -3 -4 936.779 63.9322 1 -4 -3 -4 908.941 63.2962 7 -4 3 4 929.644 62.451 3 4 -3 4 987.427 65.4554 4 4 3 4 999.102 64.3149 8 -4 3 -4 985.551 62.3336 3 4 -3 -4 930.775 64.0254 6 4 -3 -4 1070 67.0828 4 4 -3 -4 1117.22 66.4694 5 -5 -3 -4 964.714 65.4184 1 5 3 -4 937.322 65.3264 8 -5 -3 -4 948.351 64.4549 7 -5 3 4 1019.84 63.5842 3 5 -3 4 983.073 65.8331 5 5 -3 -4 1095.07 68.392 4 5 -3 -4 984.926 66.4063 8 -5 3 -4 995.144 63.1942 3 5 -3 -4 985.577 67.3758 5 5 3 4 999.038 64.9528 8 6 -3 4 542.012 43.223 5 6 3 -4 549.29 42.8372 8 6 -3 -4 663.545 45.4457 5 6 -3 -4 623.027 44.7861 8 6 -3 -4 665.439 45.968 4 6 3 4 582.489 43.2419 8 7 -3 4 991.326 73.5416 5 7 3 -4 1018.48 72.3334 8 7 -3 -4 1095.63 74.6056 5 7 -3 -4 1188.37 73.9825 8 7 3 4 988.85 72.7444 8 7 -3 -4 1179.24 76.0254 4 8 3 -4 484.401 36.5972 8 8 -3 4 441.316 38.1628 5 8 3 4 396.713 36.6289 8 8 -3 -4 465.783 36.6147 8 8 -3 -4 380.426 36.8702 5 8 -3 -4 424.855 38.7232 4 -9 -3 -4 559.263 43.0867 11 9 -3 4 485.826 48.5144 5 9 3 -4 610.282 47.6308 8 -9 3 -4 629.906 46.4828 12 9 -3 -4 507.435 48.3533 5 9 -3 -4 597.035 42.3841 11 -9 3 -4 646.097 46.0916 13 -9 3 -4 699.062 45.0808 11 -9 -3 4 650.142 47.9645 13 -9 -3 4 629.558 44.1618 11 9 3 4 640.175 48.5141 8 10 3 -4 268.571 31.1622 8 -10 -3 -4 288.009 26.3225 11 10 -3 -4 291.146 25.3218 20 10 -3 -4 271.467 24.7818 11 -10 3 -4 305.494 29.8934 13 -10 -3 4 290.975 29.5525 13 -10 3 -4 307.964 28.5389 12 10 3 4 280.75 33.2374 8 -10 -3 4 304.229 26.2965 11 -11 -3 -4 236.887 24.0512 11 11 -3 4 265.59 31.561 17 -11 3 -4 237.112 24.5158 12 -11 3 -4 238.853 26.3932 13 11 -3 -4 232.114 21.7328 11 -11 -3 4 205.694 26.5974 13 11 -3 -4 229.632 22.5886 20 -12 -3 -4 108.564 15.1366 11 12 -3 4 117.566 23.7672 17 12 3 -4 110.772 13.6536 20 -12 -3 -4 103.37 13.8706 11 -12 3 -4 102.273 14.9897 13 12 -3 -4 116.481 14.6473 20 12 -3 -4 130.883 16.5786 12 -12 -3 4 93.9278 14.3443 13 -13 -3 -4 89.5499 12.0764 11 13 3 -4 87.5942 12.3843 20 13 -3 -4 85.0303 10.5256 20 13 -3 -4 86.2528 13.9487 12 -13 3 -4 97.8517 15.2821 13 -13 -3 4 80.7934 12.1415 13 0 4 -4 631.736 39.5228 3 0 4 4 633.189 39.5771 3 0 -4 4 610.072 42.0097 4 0 -4 -4 632.921 41.2237 2 -1 4 4 3008.47 189.768 3 1 4 -4 2937.65 189.589 3 -1 -4 -4 3060.33 191.594 1 -1 -4 -4 3002.98 191.219 2 1 -4 4 3044.55 192.297 4 -1 -4 4 3255.08 192.507 4 1 -4 -4 3152.9 191.463 2 1 -4 -4 3124.27 190.962 6 1 -4 -4 2869.48 193.113 4 -1 4 -4 3289.81 189.79 3 1 4 4 3269.19 189.69 3 -2 -4 -4 192.703 18.5784 6 2 4 -4 199.716 13.6346 3 -2 -4 -4 203.895 15.5916 1 -2 4 4 198.019 13.9802 3 2 -4 4 195.027 15.5674 5 2 -4 4 197.106 16.2606 4 -2 -4 -4 187.707 14.9852 7 3 -4 4 1455.76 96.3921 5 -3 4 4 1454.36 95.1148 3 3 -4 4 1475.82 97.4885 4 -3 -4 -4 1495.06 95.3696 6 -3 -4 -4 1421.96 96.3255 1 -3 -4 -4 1413.72 95.6357 7 -3 -4 4 1615.63 98.0269 4 3 -4 -4 1580.5 99.8999 4 3 -4 -4 1545.32 97.2552 6 3 4 4 1530.12 94.4289 3 3 -4 -4 1767.22 98.1258 5 -3 4 -4 1546.69 94.8949 3 -4 4 4 450.218 33.4905 3 -4 -4 -4 433.062 34.6584 1 4 -4 4 466.963 36.4576 4 -4 -4 -4 443.156 34.1962 7 4 -4 -4 553.543 36.9955 6 -4 4 -4 618.153 33.9358 3 4 4 4 581.588 35.7278 8 5 -4 -4 749.016 51.614 6 -5 4 -4 705.976 50.4022 3 -5 -4 4 802.584 53.3525 4 5 4 4 686.922 50.689 8 5 -4 -4 816.6 54.476 5 6 -4 4 580.746 41.7703 5 6 -4 -4 602.398 43.7252 4 6 -4 -4 575.991 42.733 5 6 4 4 461.965 39.5444 8 -6 -4 4 515.293 41.974 4 7 -4 4 230.172 26.9718 5 7 -4 -4 261.5 27.4398 4 7 4 4 229.566 25.3249 8 7 -4 -4 255.737 27.3665 5 8 -4 4 533.749 43.4001 5 8 4 4 485.526 40.7572 8 8 -4 -4 454.766 41.9274 5 8 -4 -4 518.569 43.9042 4 -9 -4 -4 131.349 20.2367 11 9 -4 4 134.925 21.0959 10 9 -4 4 115.067 23.4316 5 9 -4 4 158.353 28.9895 17 9 4 -4 131.5 27.2342 8 9 -4 -4 92.2302 20.3124 5 9 -4 -4 112.529 22.523 17 9 4 4 119.753 20.4309 8 -9 -4 4 141.382 19.0662 11 -9 4 -4 191.104 24.1282 13 -9 4 -4 121.553 18.2259 12 9 -4 -4 138.307 16.0488 11 -9 -4 4 106.001 18.9878 13 10 -4 4 312.053 28.1098 10 -10 -4 -4 314.852 27.2676 11 10 4 -4 371.227 47.2998 8 10 -4 4 302.031 37.5358 17 -10 -4 4 257.563 26.4376 11 -10 4 -4 302.255 27.8672 12 10 4 4 290.299 33.8355 8 -10 -4 4 304.926 30.9015 13 10 -4 -4 346.886 38.6914 17 -10 4 -4 251.249 30.2386 13 10 -4 -4 253.809 25.7113 20 10 -4 -4 272.021 24.9227 11 -11 -4 -4 32.9396 12.2013 11 11 -4 4 38.8412 16.1175 17 11 -4 -4 55.0641 11.0767 12 11 -4 -4 44.5716 9.68183 11 -11 -4 4 33.315 12.5444 13 -11 -4 4 50.2185 10.2222 11 -11 4 -4 31.9267 11.0382 12 11 -4 -4 50.1217 10.159 20 -11 4 -4 51.6105 12.8944 13 12 4 -4 231.984 22.2747 20 -12 -4 -4 240.648 21.058 11 12 -4 4 227.394 28.5305 17 12 -4 -4 234.263 20.5386 20 12 -4 -4 211.852 21.263 11 12 -4 -4 264.232 22.4844 12 -12 4 -4 232.556 23.3415 13 -12 -4 4 242.858 24.2122 13 -13 -4 -4 58.0161 8.4589 11 13 -4 4 29.9231 12.9798 17 13 4 -4 66.1089 10.6348 20 -13 -4 4 64.83 9.50708 13 13 -4 -4 50.1063 7.78112 20 -13 4 -4 38.7968 10.3409 13 0 -5 -4 2345.75 155.738 6 0 5 -4 2435.18 154.726 3 0 -5 4 2592.83 158.124 4 0 -5 -4 2608.29 155.759 7 0 5 4 2584.12 154.887 3 -1 -5 -4 121.564 11.6557 6 1 5 -4 126.557 9.66613 3 1 -5 4 130.234 13.2428 4 -1 5 4 136.303 10.1978 3 -1 -5 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724.66 52.507 4 5 -5 -4 648.521 50.9882 5 6 -5 4 549.627 40.1461 10 -6 -5 -4 498.793 41.6385 9 6 -5 4 513.791 41.27 5 6 -5 -4 556.286 41.2496 6 6 -5 -4 590.583 45.3599 4 -6 -5 4 511.611 44.6718 4 6 -5 -4 552.341 43.3514 5 -7 -5 -4 973.53 65.7451 9 7 -5 4 891.328 66.0947 5 7 -5 4 1008.83 63.4459 10 7 -5 -4 934.051 69.0129 4 7 -5 -4 865.351 66.7608 5 8 -5 4 94.3381 18.5712 13 8 -5 4 136.561 22.8462 5 8 -5 4 138.252 20.2256 10 -8 5 -4 119.337 30.27 13 8 -5 -4 103.747 15.5917 11 8 -5 -4 116.363 19.7278 5 -8 -5 4 101.716 17.8254 13 -8 -5 4 83.9114 14.3875 11 -9 -5 -4 545.404 42.8713 11 9 -5 4 557.054 42.1925 10 9 -5 4 576.781 49.9088 17 9 -5 -4 658.797 52.5503 17 9 -5 -4 573.273 40.3028 11 9 -5 -4 539.396 41.9605 20 -9 5 -4 576.11 44.1158 13 -9 -5 4 576.389 45.5649 13 -9 -5 4 552.881 42.4379 11 10 -5 4 1.32376 10.1877 10 -10 -5 -4 3.69706 11.3829 11 10 -5 4 35.362 14.5499 17 -10 -5 -4 9.01563 8.40256 11 -10 5 -4 7.45208 12.373 12 -10 -5 4 3.353 12.4621 13 10 -5 -4 -13.771 15.9183 17 10 -5 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29.4813 4 -2 -6 -4 413.606 29.8844 6 2 -6 -4 371.089 32.5977 4 -2 -6 4 395.741 30.0163 4 2 -6 -4 419.537 30.5639 6 -2 6 -4 343.534 27.7903 3 2 6 4 427.115 27.9421 3 -3 -6 -4 783.222 49.8571 7 3 -6 4 739.162 52.8734 4 -3 -6 4 726.783 52.2332 4 3 -6 -4 717.836 54.7713 4 3 -6 -4 750.599 52.8012 6 -4 -6 -4 804.789 49.837 7 4 -6 4 847.93 54.1169 4 -4 -6 -4 777.451 53.3328 9 -4 -6 4 661.9 51.4418 4 4 -6 -4 666.087 54.8665 4 4 -6 -4 609.432 52.3574 6 5 -6 4 582.447 44.7118 10 -5 -6 -4 538.468 42.6571 7 5 -6 4 663.013 47.9293 4 -5 -6 -4 603.526 46.0754 9 5 -6 -4 609.616 46.9661 6 -5 -6 4 614.592 46.2207 4 5 -6 -4 648.77 50.2993 4 -6 -6 -4 489.092 38.9981 9 6 -6 4 530.552 37.4942 10 6 -6 -4 432.519 38.1284 6 6 -6 -4 404.466 41.5756 4 7 -6 4 257.52 26.5809 11 7 -6 4 255.616 25.3291 10 7 -6 4 207.309 26.8727 5 -7 -6 -4 220.016 26.9412 9 7 -6 -4 215.561 23.3934 11 -7 -6 4 252.299 23.9514 11 7 -6 -4 297.403 40.3424 4 -8 -6 -4 642.651 72.3265 15 8 -6 4 688.585 61.0578 17 8 -6 4 783.662 53.7936 10 8 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404.705 32.6849 5 5 -2 -10 408.941 36.2541 5 -5 2 -10 436.808 36.966 7 5 2 10 473.271 32.9395 8 5 -2 -10 412.946 37.4637 8 -5 2 -10 415.195 35.2698 9 -6 -2 -10 372.469 32.5841 9 6 -2 10 294.698 28.842 5 6 2 -10 312.125 32.7346 8 -6 -2 -10 332.384 30.1273 7 -6 2 -10 339.331 31.0714 7 6 -2 -10 289.948 33.1084 5 6 -2 -10 284.054 37.0686 8 6 2 10 319.251 28.0737 8 -7 -2 -10 178.99 27.1316 12 7 2 -10 205.403 21.7942 11 7 2 -10 184.895 30.949 8 7 -2 10 188.875 25.0902 5 -7 -2 -10 187.979 28.7442 9 -7 -2 -10 252.848 26.8036 7 -7 2 -10 264.212 26.3398 7 -7 2 -10 207.051 26.7782 12 -7 2 -10 209.834 24.4888 11 7 -2 -10 223.761 32.0605 5 7 -2 -10 220.966 21.9686 11 7 -2 -10 230.301 30.1741 12 -7 2 -10 224.301 24.3486 13 7 -2 -10 286.922 36.9744 8 7 2 10 272.765 26.8745 8 -8 -2 -10 39.8335 12.872 21 -8 -2 -10 86.7546 20.7333 18 -8 -2 -10 73.3867 17.6551 7 8 2 -10 70.4728 21.877 8 8 2 -10 70.9221 11.7142 11 -8 -2 -10 38.5196 15.4932 12 8 -2 -10 86.2747 16.8651 20 -8 2 -10 62.6321 17.1865 7 8 -2 -10 114.575 24.9705 8 8 -2 -10 81.9484 11.8336 11 8 -2 -10 62.4041 16.3354 12 -8 2 -10 50.1001 15.287 12 -8 2 -10 79.0568 13.7883 13 8 2 10 62.6192 17.3645 8 -8 2 -10 77.2847 13.1751 11 9 2 -10 97.974 15.9888 11 -9 -2 -10 88.1653 17.2529 12 -9 -2 -10 105.706 17.795 11 -9 2 -10 99.6057 16.6442 12 9 -2 -10 90.8855 15.4549 20 9 -2 -10 94.9576 15.6844 11 -9 2 -10 92.7281 14.4425 13 9 -2 -10 94.6511 16.7651 12 -9 2 -10 102.919 14.9414 11 -10 -2 -10 72.8097 11.5363 11 10 -2 10 62.0583 20.2639 17 -10 -2 -10 71.8897 14.8891 12 -10 2 -10 72.0729 13.2331 12 10 -2 -10 71.3287 14.5373 12 -10 2 -10 73.5284 11.715 11 10 -2 -10 84.6007 14.2205 11 10 -2 -10 57.7293 12.708 20 -10 2 -10 60.756 18.5171 13 11 -2 10 55.1287 15.3852 17 -11 -2 -10 91.9281 13.2814 11 11 -2 -10 82.2717 12.4602 11 11 -2 -10 61.5331 12.75 12 -11 2 -10 63.8097 11.8211 12 11 -2 -10 66.7687 11.0998 20 -11 2 -10 74.2491 10.9586 11 12 -2 10 36.2342 11.8043 17 12 -2 -10 53.8229 9.95123 12 -12 2 -10 36.3535 8.66048 12 12 -2 -10 44.0274 8.28731 20 0 -3 10 95.9901 10.3779 5 0 -3 -10 98.9228 11.602 8 0 3 -10 112.366 18.5668 9 0 -3 -10 92.9265 11.8333 6 1 -3 10 424.412 31.4844 5 -1 -3 -10 403.923 31.3049 7 -1 -3 -10 429.461 31.9182 6 1 3 -10 413.004 40.027 9 -1 3 -10 455.38 36.5329 9 1 -3 -10 488.856 33.1833 8 -1 -3 10 480.097 34.4193 4 1 -3 -10 483.853 32.8289 6 -1 -3 10 497.003 32.0481 5 -2 -3 -10 621.445 54.2421 9 2 -3 10 676.44 49.6506 5 -2 -3 -10 692.057 49.7672 7 -2 -3 -10 701.107 49.9873 6 2 -3 -10 819.89 51.4773 8 2 -3 -10 786.506 51.0567 6 -2 3 -10 765.991 52.9797 9 -2 -3 10 850.966 50.3469 5 -2 -3 10 803.479 53.3047 4 -3 -3 -10 430.21 39.84 9 3 -3 10 458.323 34.1075 5 -3 -3 -10 469.229 34.5224 7 -3 -3 10 508.173 37.9357 4 -3 3 -10 486.527 37.0088 9 3 -3 -10 495.361 36.2134 8 -4 -3 -10 310.262 27.3645 10 4 -3 10 338.112 28.1043 5 -4 -3 -10 341.337 33.4592 9 -4 -3 -10 350.799 29.2374 7 4 -3 -10 380.799 30.8811 5 4 -3 -10 372.835 31.7063 8 -4 3 -10 343.788 30.4273 9 -4 -3 10 355.956 31.7681 4 4 3 10 401.92 28.7029 8 -5 -3 -10 419.25 35.3295 7 5 3 -10 482.676 47.5984 8 5 -3 10 422.389 34.4584 5 -5 -3 -10 436.993 39.2128 9 5 -3 -10 412.713 38.7789 8 5 3 10 482.409 34.0468 8 5 -3 -10 430.567 38.6691 5 -5 -3 10 414.631 38.5929 4 -5 3 -10 440.137 38.0365 7 6 3 -10 359.514 35.5118 8 6 -3 10 283.893 31.5242 5 -6 -3 -10 321.274 34.7662 9 -6 -3 -10 347.663 31.9544 7 6 -3 -10 357.757 38.7222 8 6 3 10 399.443 31.0218 8 -6 -3 10 339.174 36.271 4 6 -3 -10 320.72 36.6572 5 -6 3 -10 409.64 33.3812 7 7 -3 10 537.636 48.1364 5 7 3 -10 650.97 53.2487 8 -7 -3 -10 703.687 51.0972 9 7 3 -10 665.616 44.7996 11 -7 -3 -10 620.292 57.6378 16 -7 -3 -10 699.885 49.394 7 -7 3 -10 630.137 47.2515 12 7 -3 -10 544.831 48.9854 12 -7 3 -10 657.723 45.9851 13 7 -3 -10 503.843 52.5392 5 7 -3 -10 628.995 43.9211 11 -7 3 -10 580.805 46.1115 11 -7 3 -10 729.616 49.295 7 7 -3 -10 583.844 55.2918 8 7 3 10 625.12 48.9655 8 -8 -3 -10 332.184 28.0495 21 -8 -3 -10 328.913 40.9876 16 8 3 -10 270.815 40.413 8 8 3 -10 305.382 28.9224 11 -8 -3 -10 335.351 33.5032 7 -8 -3 -10 311.936 40.0647 18 -8 -3 -10 388.821 51.8792 9 -8 3 -10 358.571 32.971 12 8 3 10 405.689 37.5986 8 -8 3 -10 398.837 33.4566 7 8 -3 -10 367.815 41.5634 8 -8 3 -10 407 31.5069 13 -8 3 -10 358.754 30.9269 11 8 -3 -10 398.202 36.3173 20 8 -3 -10 370.052 28.6616 11 8 -3 -10 378.52 34.8784 12 -9 -3 -10 517.964 36.749 21 -9 -3 -10 519.414 46.8979 18 -9 3 -10 483.072 38.494 11 -9 3 -10 477.223 38.8285 13 9 -3 -10 500.254 36.9506 11 9 -3 -10 535.463 40.9558 12 9 -3 -10 528.451 39.9142 20 -9 3 -10 502.443 39.6432 12 -10 -3 -10 191.874 19.6222 11 10 -3 -10 197.487 24.3872 12 -10 3 -10 210.245 20.788 11 -10 3 -10 195.038 21.8645 12 10 -3 -10 200.367 20.9058 20 -10 -3 10 188.084 25.2956 13 10 -3 -10 181.422 19.0624 11 -10 3 -10 218.011 20.26 13 -11 -3 -10 215.095 20.0767 11 11 -3 10 267.445 25.1106 17 -11 3 -10 238.953 20.142 11 11 -3 -10 198.939 19.5617 11 11 -3 -10 220.323 21.6241 12 -11 -3 10 247.303 23.1449 13 11 -3 -10 219.258 19.9755 20 -11 3 -10 236.798 20.8234 12 -11 3 -10 185.511 25.7481 13 12 -3 10 137.261 18.5174 17 12 -3 -10 117.451 12.8505 20 0 -4 -10 803.175 54.374 8 0 -4 10 785.434 53.12 5 0 4 -10 838.024 58.9139 9 0 -4 -10 805.51 54.0399 6 1 -4 10 2109.34 123.313 5 -1 -4 -10 1870.76 126.635 9 -1 -4 -10 2022.8 122.873 7 -1 -4 -10 2045.28 123.418 6 1 -4 -10 1855.17 123.655 8 -1 4 -10 1965.06 126.682 9 -1 -4 10 1813.93 122.51 5 -1 -4 10 1926.46 125.868 4 1 -4 -10 1942.11 123.796 6 -2 -4 -10 167.2 24.2266 9 -2 -4 -10 163.928 15.53 7 2 -4 10 157.229 15.2456 5 -2 -4 -10 169.411 16.2889 6 -2 -4 10 167.199 18.4589 4 2 -4 -10 158.47 18.4743 8 -2 4 -10 164.119 20.0919 9 2 -4 -10 175.915 18.9121 6 3 -4 10 1504.08 94.5367 5 -3 -4 -10 1438.01 98.718 9 -3 -4 -10 1559.6 94.5413 7 -3 -4 -10 1431.76 93.4208 10 -3 4 -10 1426.55 95.9886 9 3 -4 -10 1406.81 95.4501 8 3 -4 -10 1375.94 95.4478 6 -3 -4 10 1446.7 97.918 4 3 4 10 1554.24 94.2808 8 -4 -4 -10 72.4613 18.2438 9 -4 -4 -10 94.9898 15.5925 7 4 -4 10 94.8833 15.5639 5 -4 -4 -10 67.8618 11.0006 10 -4 -4 10 111.197 18.5547 4 4 4 10 137.065 15.9855 8 4 -4 -10 121.106 20.851 8 -4 4 -10 137.005 18.685 9 -5 -4 -10 597.88 42.1087 7 -5 -4 -10 547.033 39.0926 10 5 -4 10 532.512 42.0032 5 -5 -4 -10 611.998 46.3836 9 5 -4 -10 489.642 44.0119 5 5 4 10 526.168 40.6162 8 -5 -4 10 524.183 45.6059 4 5 -4 -10 505 47.1729 8 6 4 -10 221.75 35.3775 14 -6 -4 -10 220.578 29.3893 9 -6 -4 -10 226.54 24.7575 7 6 -4 10 147.629 25.8383 5 6 4 -10 171.068 20.9321 11 -6 4 -10 223.931 27.2412 7 6 4 10 255.932 25.4262 8 -6 4 -10 175.29 24.601 11 6 -4 -10 212.359 29.9308 5 -6 4 -10 255.349 25.9524 13 6 -4 -10 213.57 33.1311 12 -7 -4 -10 43.134 10.5429 21 7 4 -10 43.1649 18.6192 16 -7 -4 -10 44.8201 19.072 16 7 4 -10 45.0279 16.3595 11 7 4 -10 23.717 18.6905 14 -7 -4 -10 45.3967 16.8057 9 -7 -4 -10 59.3816 16.5929 7 -7 -4 -10 44.9394 19.4897 18 7 -4 -10 34.4777 19.4295 12 -7 4 -10 21.4117 12.6633 11 -7 4 -10 18.1719 15.519 12 7 -4 -10 44.7579 9.91364 11 -7 4 -10 64.899 14.9225 7 -7 4 -10 70.2743 13.7243 13 7 -4 -10 60.2411 24.2976 17 7 4 10 18.85 14.9922 8 7 -4 -10 47.0619 16.8074 20 8 4 -10 113.666 19.9414 16 -8 -4 -10 74.8524 21.3483 16 -8 -4 -10 92.7679 14.2571 21 -8 -4 -10 72.72 19.8359 18 -8 -4 -10 90.6985 19.3522 9 8 -4 -10 76.8594 16.2111 20 -8 -4 10 95.2608 17.959 13 -8 4 -10 73.6398 16.035 12 8 -4 -10 88.3189 14.7469 11 8 4 10 87.7642 20.1279 8 8 -4 -10 86.7663 19.1396 12 -8 4 -10 89.9631 14.7797 13 -8 4 -10 93.175 14.4059 11 -9 -4 -10 20.7108 7.72972 21 -9 -4 -10 6.76377 15.2363 18 9 -4 10 -2.2586 17.1604 17 -9 -4 -10 27.2454 17.7963 16 9 -4 -10 19.2995 11.1978 20 -9 4 -10 13.0251 11.761 12 9 -4 -10 6.32765 14.0224 12 -9 -4 10 18.1408 12.7879 13 -9 4 -10 21.6702 10.9693 13 9 -4 -10 6.72247 8.16836 11 -9 4 -10 3.5512 10.2704 11 -10 -4 -10 108.061 21.6984 18 -10 -4 -10 76.9226 12.3775 21 10 -4 10 107.471 17.2223 17 10 -4 10 96.7519 14.0635 10 10 -4 -10 100.342 13.2898 20 -10 -4 10 86.5076 14.5588 13 10 -4 -10 81.995 12.1706 11 -10 4 -10 61.4975 13.2143 12 -10 4 -10 85.6146 13.6242 13 -10 4 -10 107.461 15.3388 11 10 -4 -10 104.333 16.7297 12 11 -4 10 23.8269 12.4616 17 11 -4 -10 45.2753 8.48798 20 -11 4 -10 32.3984 8.87104 12 -11 4 -10 25.4408 8.92491 11 11 -4 -10 34.1079 8.04821 11 -11 4 -10 31.2531 8.97528 13 11 -4 -10 46.5971 10.3019 12 -11 -4 10 24.1419 9.59979 13 12 -4 -10 75.5573 11.2658 20 0 -5 10 123.775 16.382 4 0 -5 -10 116.6 15.7267 6 0 -5 -10 116.629 13.6193 7 -1 -5 -10 35.9639 9.18185 10 -1 -5 -10 25.6656 7.25148 7 -1 -5 -10 31.389 9.87064 6 -1 -5 10 36.6433 9.80202 4 1 -5 -10 40.235 10.3921 6 -1 5 -10 27.9571 11.4161 9 2 -5 10 502.377 35.6195 5 -2 -5 -10 516.572 35.4172 7 -2 -5 -10 475.516 35.5355 10 -2 -5 -10 479.761 41.4068 9 -2 -5 -10 517.867 35.9958 6 -2 -5 10 451.599 38.1096 4 2 -5 -10 458.981 38.1406 6 -2 5 -10 475.242 38.1394 9 3 -5 10 249.913 22.8708 5 -3 -5 -10 271.295 30.5965 9 -3 -5 -10 271.686 23.0166 10 -3 -5 -10 268.986 23.455 7 -3 -5 -10 272.268 24.082 6 3 -5 -10 235.284 27.5681 6 -3 -5 10 273.655 26.2673 4 -3 5 -10 267.044 25.9069 9 -4 -5 -10 249.112 22.6379 10 -4 -5 -10 238.012 24.4145 7 4 -5 10 242.684 23.9737 5 -4 -5 -10 268.467 30.7849 9 -4 -5 10 250.606 27.4169 4 -4 5 -10 293.672 27.4474 9 -5 -5 -10 691.203 47.2422 10 -5 -5 -10 723.034 49.7935 7 5 -5 10 597.156 49.1816 5 -5 -5 -10 749.463 55.0821 9 -5 5 -10 693.605 47.5914 11 5 5 10 583.573 49.9056 8 6 5 -10 183.329 30.8908 14 -6 -5 -10 156.151 23.7638 9 -6 -5 -10 114.022 19.6172 21 -6 -5 -10 136.029 22.8438 7 -6 -5 -10 94.763 24.3596 16 6 5 -10 130.082 23.332 16 -6 -5 -10 142.049 38.3395 18 6 -5 -10 152.589 29.3491 17 -6 -5 10 141.709 19.2477 13 6 -5 -10 229.359 33.9328 20 -6 5 -10 192.859 22.4861 11 -6 5 -10 179.006 23.9708 13 6 5 10 153.75 24.0758 8 -7 -5 -10 702.528 55.2112 9 -7 -5 -10 720.524 47.2565 21 7 5 -10 648.278 56.2925 16 -7 -5 -10 693.754 53.0891 7 -7 -5 -10 723.928 59.9315 16 7 5 -10 647.547 59.7813 14 -7 -5 -10 738.676 61.2744 18 -7 5 -10 737.139 52.9543 7 -7 5 -10 693.428 50.5062 11 -7 5 -10 709.834 51.1023 13 7 -5 -10 726.282 53.2424 20 7 -5 -10 704.572 65.3246 17 -7 -5 10 743.063 53.8202 13 7 -5 -10 791.526 57.1677 21 7 5 10 589.874 54.3031 8 -8 -5 -10 8.81096 16.5138 16 8 5 -10 38.8928 15.4931 16 8 -5 10 42.3612 14.2409 10 8 -5 10 2.92336 18.8229 17 -8 -5 -10 39.7143 8.60662 21 -8 -5 -10 37.3681 18.5702 18 -8 -5 -10 32.7749 16.0254 9 -8 5 -10 18.857 12.2133 13 8 -5 -10 7.30526 21.3913 12 8 -5 -10 46.3991 13.5881 20 8 -5 -10 25.3815 8.86399 11 8 -5 -10 18.1872 20.3895 17 -8 -5 10 16.6557 13.1786 13 -8 5 -10 22.4825 11.0484 11 -9 -5 -10 419.424 41.3362 18 9 -5 10 460.837 39.7374 17 -9 -5 -10 434.458 31.4625 21 9 -5 10 429.73 35.2377 10 9 5 -10 458.026 40.2943 16 9 -5 -10 480.942 34.7731 20 9 -5 -10 469.935 33.5588 11 -9 5 -10 461.121 35.886 13 -9 -5 10 441.73 37.4247 13 -9 5 -10 421.194 34.7148 11 9 -5 -10 381.579 47.0566 17 9 -5 -10 493.182 36.769 12 -10 -5 -10 9.87886 11.6496 18 -10 -5 -10 7.57899 6.21172 21 10 -5 10 -7.3859 10.1525 10 10 -5 -10 28.5623 10.8261 12 -10 -5 10 14.8011 9.81054 13 10 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-6 -10 48.2035 10.6191 10 -4 6 -10 66.0703 16.8525 13 -4 6 -10 31.2755 11.3649 11 4 -6 -10 24.7133 18.0532 6 5 -6 10 638.945 48.2176 10 -5 -6 -10 550.78 48.2294 9 5 6 -10 535.546 48.2744 14 -5 -6 -10 564.638 39.2794 10 -5 -6 -10 503.591 53.0775 16 5 6 -10 492.956 50.982 16 -5 -6 -10 611.219 42.6591 7 5 -6 -10 426.512 60.7886 17 -5 -6 10 548.21 41.7702 13 -5 6 -10 491.83 41.3547 11 -5 6 -10 520.207 41.2827 13 -6 -6 -10 85.1513 12.718 21 6 6 -10 52.807 19.3974 16 6 6 -10 85.3427 18.7163 14 -6 -6 -10 107.062 18.5953 7 -6 -6 -10 92.875 18.9213 9 -6 -6 -10 87.4395 22.5608 16 6 -6 10 87.6889 17.4549 10 -6 -6 -10 90.2504 23.7236 18 6 -6 -10 71.4349 27.4527 17 6 -6 -10 70.1459 16.7127 20 6 -6 -10 99.2817 12.8686 21 -6 6 -10 95.6004 16.6428 13 -6 6 -10 71.2853 14.8137 11 -6 -6 10 131.812 19.624 13 7 -6 10 125.256 26.5531 17 -7 -6 -10 121.862 23.5896 16 7 6 -10 170.145 31.2623 14 7 -6 10 127.429 16.7698 10 -7 -6 -10 79.6469 22.7867 18 -7 -6 -10 131.679 14.3521 21 7 6 -10 83.0616 19.6638 16 -7 -6 -10 128.733 21.8222 9 -7 6 -10 161.835 22.2839 11 7 -6 -10 109.584 17.6888 20 7 -6 -10 112.149 17.5046 21 -7 -6 10 166.637 22.7594 13 7 -6 -10 102.747 26.6567 17 -7 6 -10 120.569 17.7175 13 -8 -6 -10 82.304 18.7486 16 8 -6 10 59.7339 14.3241 10 8 -6 10 38.2534 17.4254 17 -8 -6 -10 40.1903 18.0606 18 8 6 -10 55.5257 16.055 16 8 6 -10 26.286 19.6781 14 -8 -6 -10 60.8082 8.92702 21 -8 -6 -10 54.2253 16.8426 9 -8 6 -10 71.7539 14.4171 13 8 -6 -10 75.5015 14.2036 20 -8 -6 10 88.5307 14.2988 13 8 -6 -10 99.2084 14.0614 11 8 -6 -10 61.4245 21.9507 17 -9 -6 -10 24.5606 13.8461 18 9 6 -10 31.5862 13.8148 16 -9 -6 -10 28.259 7.23873 21 9 -6 10 34.8671 11.9635 10 9 -6 -10 29.5574 10.9477 20 9 -6 -10 33.9746 8.59407 11 -9 -6 10 32.2936 10.7105 13 9 -6 -10 16.2374 17.6217 17 -9 6 -10 31.3617 11.3822 13 10 6 -10 93.8665 15.6538 16 -10 -6 -10 80.0405 15.3426 18 -10 -6 -10 75.6054 10.9664 21 10 -6 -10 87.0935 13.6296 11 -10 -6 10 106.581 14.2523 13 10 -6 -10 95.4706 11.7165 20 10 -6 -10 129.507 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24.183 7 -4 -7 -10 251.898 33.0414 9 -4 -7 -10 221.244 23.1669 10 -4 -7 -10 206.649 47.8901 18 -4 -7 -10 217.824 17.8131 21 4 -7 -10 156.408 33.0748 17 4 -7 -10 177.796 19.0633 21 -4 -7 10 203.559 31.1337 18 4 -7 -10 218.974 27.0228 20 4 -7 -10 134.718 43.4693 19 -4 7 -10 208.614 24.9637 13 -5 -7 -10 413.919 40.6332 9 -5 -7 -10 431.155 47.5528 18 -5 -7 -10 396.453 26.7002 21 5 7 -10 353.41 41.8219 16 -5 -7 -10 393.162 47.7356 16 -5 -7 -10 422.72 30.625 10 -5 -7 -10 413.356 34.0711 7 5 -7 -10 319.12 28.0478 21 -5 -7 10 304.812 30.3088 13 5 -7 -10 328.282 34.8323 20 -5 7 -10 322.652 31.9086 13 -5 -7 10 376.929 38.1072 18 -6 -7 -10 240.428 38.5809 18 -6 -7 -10 274.839 39.7093 16 6 -7 10 261.89 27.3127 10 -6 -7 -10 282.915 21.5062 21 6 7 -10 257.562 36.9782 16 6 -7 10 243.852 27.8573 13 6 7 -10 270.201 35.0983 14 -6 -7 -10 280.685 34.8371 9 -6 -7 10 306.979 28.0207 13 6 -7 -10 302.463 31.1977 20 6 -7 -10 307.21 24.3033 21 6 -7 -10 277.977 40.1409 17 -6 7 -10 313.717 29.7628 13 -7 -7 -10 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286.714 40.7203 18 -6 -6 -11 291.188 23.9974 21 -6 -6 -11 364.665 35.7968 9 -6 -6 -11 280.831 41.1655 16 6 -6 11 269.528 29.6235 10 6 6 -11 364.325 39.61 14 6 6 -11 261.394 39.2656 16 -6 6 -11 371.163 31.0871 13 -6 -6 11 352.481 30.978 13 6 -6 -11 300.704 50.0022 17 -6 6 -11 317.322 30.1865 11 6 -6 -11 354.701 26.7045 21 6 -6 -11 325.98 33.5884 20 7 -6 11 26.5906 11.3641 10 7 6 -11 -10.924 16.0619 14 7 6 -11 10.6985 15.4772 16 -7 -6 -11 4.12257 17.1279 18 -7 -6 -11 12.5358 15.0698 9 -7 -6 -11 13.6712 17.4711 16 -7 -6 -11 16.4352 7.01481 21 -7 6 -11 41.842 12.8494 13 -7 6 -11 43.8302 11.6605 11 7 -6 -11 22.3928 13.403 20 7 -6 -11 9.5448 21.7703 17 7 -6 -11 34.768 9.81479 21 -7 -6 11 17.984 12.1802 13 -8 -6 -11 75.1077 18.2856 9 -8 -6 -11 59.6149 18.4187 18 -8 -6 -11 84.4775 18.441 16 -8 -6 -11 99.6211 11.2591 21 8 6 -11 76.5386 17.8617 14 8 -6 11 91.1821 15.0423 10 8 -6 11 87.2187 17.3619 17 8 6 -11 78.6128 17.9283 16 8 -6 -11 102.18 21.708 17 -8 -6 11 57.866 13.5344 13 -8 6 -11 83.6275 13.968 13 8 -6 -11 56.744 10.7205 11 8 -6 -11 68.8108 14.0808 20 9 -6 11 11.6468 12 10 -9 -6 -11 7.67296 11.8019 18 -9 -6 -11 16.3054 5.94124 21 9 6 -11 6.78782 12.6765 16 -9 6 -11 32.5631 10.6056 13 9 -6 -11 11.48 7.41975 11 -9 -6 11 22.7395 9.52341 13 9 -6 -11 20.105 16.369 17 9 -6 -11 44.2243 10.4319 20 10 6 -11 6.99498 11.3999 16 -10 -6 -11 -15.625 9.1324 18 10 -6 11 25.1359 9.9584 17 -10 -6 -11 0.56756 4.98961 21 -10 -6 11 1.39123 7.05642 13 10 -6 -11 6.14808 6.73547 11 -10 6 -11 1.28867 8.34259 13 10 -6 -11 -2.9549 7.47795 20 0 -7 11 61.6882 11.8519 13 0 -7 -11 59.7355 15.47 7 0 -7 -11 55.9954 15.064 6 0 -7 -11 63.8211 19.8046 17 0 -7 -11 66.0293 14.4167 10 -1 -7 -11 99.6349 17.3905 6 1 -7 11 115.666 16.5305 13 -1 -7 -11 114.777 15.798 10 -1 -7 -11 97.275 15.9231 7 1 -7 -11 108.661 18.4839 10 1 -7 -11 123.855 20.5359 6 -1 7 -11 90.1991 18.0289 9 -1 -7 11 121.122 15.2204 13 1 -7 -11 109.428 21.3305 17 -2 -7 -11 50.1845 11.8314 10 -2 -7 -11 78.9678 14.5829 20 2 -7 11 40.3261 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28.1027 13 -4 -7 11 221.267 34.9666 18 4 -7 -11 252.229 30.8298 20 4 -7 -11 262.845 23.446 21 -4 -7 11 278.79 26.4136 13 4 -7 -11 358.503 60.0976 19 -5 -7 -11 263.091 21.0088 21 -5 -7 -11 244.235 41.9712 16 5 7 -11 304.688 37.3179 14 -5 -7 -11 248.272 41.4179 18 -5 -7 -11 295.711 37.4583 9 -5 -7 -11 273.546 26.6297 10 5 7 -11 226.187 36.638 16 5 -7 -11 282.111 23.1789 21 -5 -7 11 275.869 33.5114 18 5 -7 -11 295.073 31.5957 20 -5 7 -11 294.787 28.4485 13 5 -7 -11 238.971 49.8474 17 -5 -7 11 328.691 27.2505 13 -6 -7 -11 379.629 44.6211 18 6 7 -11 388.237 42.9501 16 -6 -7 -11 410.801 42.6526 9 -6 -7 -11 446.831 44.9289 16 6 -7 11 375.815 46.0037 13 6 7 -11 462.306 42.4663 14 -6 -7 -11 433.329 28.8861 21 6 -7 -11 362.444 37.0347 20 -6 -7 11 419.038 34.45 13 -6 7 -11 442.677 35.4465 13 6 -7 -11 399.83 31.0011 21 6 -7 -11 353.951 51.6643 17 7 -7 11 190.154 28.6536 13 -7 -7 -11 238.114 33.6714 16 7 -7 11 239.546 24.0604 10 -7 -7 -11 269.421 32.3106 18 -7 -7 -11 247.413 19.3295 21 -7 -7 -11 211.1 29.7318 9 7 7 -11 215.748 32.4098 16 7 7 -11 204.135 35.5731 14 7 -7 -11 238.95 27.1569 20 7 -7 -11 273.934 40.144 17 7 -7 -11 248.967 21.3435 21 -7 -7 11 236.919 25.5176 13 -7 7 -11 264.786 25.6451 13 8 -7 11 302.325 26.7737 13 8 -7 11 270.725 25.8271 10 -8 -7 -11 330.342 32.3701 18 8 7 -11 301.183 32.6155 16 8 7 -11 277.743 31.0999 14 -8 -7 -11 287.568 21.8611 21 -8 -7 11 288.371 26.3138 13 -8 7 -11 287.764 26.0148 13 8 -7 -11 309.55 37.5163 17 8 -7 -11 283.942 23.894 21 8 -7 -11 298.198 26.7135 20 9 -7 11 138.965 25.1817 17 9 7 -11 172.048 23.4139 16 -9 -7 -11 145.638 21.2999 18 -9 -7 -11 137.039 13.5238 21 -9 -7 11 159.912 17.138 13 9 -7 -11 140.524 15.2009 11 -9 7 -11 164.097 16.829 13 9 -7 -11 149.501 17.0209 20 -10 -7 -11 206.997 20.3239 18 -10 -7 -11 226.266 16.5463 21 10 -7 -11 239.015 18.7147 20 0 -8 -11 379.419 61.074 19 0 -8 -11 327.641 33.3036 10 0 -8 -11 342.055 37.3797 6 0 -8 11 319.949 28.3424 13 0 8 -11 348.41 35.9219 9 0 -8 -11 336.298 27.9817 20 -1 -8 -11 557.935 71.3528 19 -1 -8 -11 845.978 62.2014 6 -1 -8 -11 718.222 51.0715 7 1 -8 11 750.914 50.7687 13 -1 -8 -11 711.061 49.8417 20 -1 -8 -11 722.388 52.6628 10 1 -8 -11 906.8 70.3961 6 1 -8 -11 745.167 54.9727 10 -1 -8 11 715.414 50.4324 13 1 -8 -11 766.026 50.733 20 -1 8 -11 737.107 56.3633 9 1 -8 -11 648.944 60.3848 17 1 -8 -11 594.528 81.4184 19 -2 -8 -11 388.345 29.8296 20 -2 -8 -11 364.006 32.2728 7 -2 -8 -11 370.892 50.8155 19 2 8 -11 343.953 45.5779 14 -2 -8 -11 391.007 33.0452 10 2 -8 11 385.409 31.0061 13 -2 8 -11 382.902 32.2694 13 -2 8 -11 357.737 36.0942 9 2 -8 -11 384.709 67.2155 19 2 -8 -11 343.514 27.1878 21 2 -8 -11 352.769 31.2961 20 2 -8 -11 470.156 44.4932 17 -3 -8 -11 491.994 43.734 9 -3 -8 -11 460.318 35.7426 20 3 8 -11 491.805 47.7766 16 3 8 -11 453.999 49.6231 14 3 -8 11 499.605 36.9971 13 -3 -8 -11 466.635 38.215 10 3 -8 -11 492.151 39.0027 20 3 -8 -11 564.895 69.3934 19 3 -8 -11 481.102 50.366 17 -3 8 -11 500.386 39.1055 13 -3 -8 11 435.199 45.597 18 -3 -8 11 513.166 36.8073 13 3 -8 -11 490.599 34.0281 21 -4 -8 -11 327.097 27.0732 20 -4 -8 -11 353.894 38.2722 9 -4 -8 -11 246.125 46.777 16 4 8 -11 344.436 37.3352 16 4 8 -11 336.344 40.7233 14 -4 -8 -11 352.351 29.801 10 4 -8 11 331.395 29.8045 13 -4 8 -11 348.751 30.5449 13 -4 -8 11 323.968 37.661 18 4 -8 -11 317.304 32.2803 20 4 -8 -11 412.233 61.4719 19 -4 -8 11 359.186 29.5164 13 4 -8 -11 263.99 46.9696 17 4 -8 -11 352.261 25.7929 21 -5 -8 -11 177.854 23.2892 10 5 8 -11 229.476 31.8283 14 -5 -8 -11 190.683 15.2362 21 -5 -8 -11 176.761 27.4102 9 5 -8 11 188.42 21.9372 13 -5 -8 -11 190.566 36.862 16 5 8 -11 180.713 31.1248 16 -5 -8 -11 208.369 34.0245 18 5 -8 -11 183.584 17.648 21 -5 -8 11 144.906 27.934 18 -5 8 -11 161.752 23.0199 13 5 -8 -11 186.024 22.226 20 -5 -8 11 149.912 22.1103 13 -6 -8 -11 136.489 23.7284 18 -6 -8 -11 106.007 22.719 9 -6 -8 -11 93.5987 20.5706 16 -6 -8 -11 119.802 12.8763 21 6 8 -11 106.07 20.5994 16 6 8 -11 175.707 28.5338 14 6 -8 11 135.638 19.003 13 -6 -8 11 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33.2152 16 7 -9 11 328.818 37.3737 19 7 -9 -11 413.894 38.7809 17 -7 -9 11 356.593 27.8716 13 -7 9 -11 350.462 28.6719 13 7 -9 -11 385.424 30.11 20 7 -9 -11 368.566 26.347 21 -8 -9 -11 39.5236 13.0269 18 8 9 -11 52.0517 13.03 16 8 -9 11 71.339 16.5618 19 -8 -9 -11 53.3728 7.38767 21 8 -9 -11 51.316 7.66081 21 8 -9 -11 61.4745 10.4536 20 -8 9 -11 64.2216 11.5117 13 8 -9 -11 52.0263 8.3081 21 -8 -9 11 37.6595 11.2709 13 0 -10 11 18.4617 8.85699 13 0 10 -11 -4.6687 15.6198 9 0 -10 -11 29.9899 15.2739 10 0 -10 -11 20.4392 8.61704 20 0 10 -11 22.1646 13.7451 13 0 -10 -11 22.3379 29.8859 19 1 -10 11 718.215 48.8222 13 -1 -10 -11 693.288 53.1827 10 1 10 -11 785.264 57.6714 9 -1 -10 -11 743.209 71.9944 19 -1 -10 -11 702.032 48.4042 20 1 -10 -11 878.992 85.2521 19 -1 -10 11 707.565 49.099 13 -1 10 -11 713.326 54.7823 9 -1 10 -11 695.599 50.876 13 1 -10 -11 640.271 47.3945 21 1 -10 -11 649.557 48.7147 20 1 -10 -11 693.789 55.9693 10 -2 -10 -11 27.5355 13.0766 10 -2 -10 -11 20.6335 8.03727 20 2 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9.90544 18 -10 5 -12 23.8145 8.42329 13 10 -5 -12 12.3538 7.28045 11 10 -5 -12 24.4531 8.33551 20 -10 -5 12 17.783 8.18318 13 10 -5 -12 28.3591 10.0657 12 0 6 -12 14.3314 7.99323 11 0 -6 -12 28.3955 12.4959 6 0 6 -12 23.991 15.4737 9 -1 -6 -12 1007.79 68.383 7 1 6 -12 962.577 66.9125 11 -1 -6 -12 983.641 69.9335 6 1 6 -12 1000.22 76.8391 9 -1 -6 -12 965.736 69.4846 10 -1 6 -12 1099.66 74.9021 9 1 -6 -12 1145.96 83.7054 17 1 -6 -12 1080.91 72.9677 6 2 6 -12 188.662 19.1565 11 -2 -6 -12 180.417 23.3698 6 2 6 -12 238.75 43.8269 14 2 6 -12 131.086 24.7589 9 -2 -6 -12 186.342 32.4087 9 -2 -6 -12 172.057 19.8154 7 2 6 -12 188.783 31.7594 16 -2 -6 -12 188.933 22.3619 10 -2 -6 -12 164.926 28.7494 17 -2 6 -12 165.832 20.2015 11 2 -6 -12 176.483 28.0035 6 2 -6 -12 262.834 34.9306 17 -2 6 -12 221.052 27.6553 9 -2 6 -12 210.131 21.372 13 3 6 -12 627.179 57.9546 14 -3 -6 -12 591.368 50.46 9 -3 -6 -12 620.799 44.2706 7 3 6 -12 605.751 40.962 11 -3 -6 -12 519.496 60.1498 19 -3 -6 -12 477.778 59.6479 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35.9269 13 -5 6 -12 405.024 35.2241 13 -5 6 -12 382.319 34.8339 11 -6 -6 -12 229.66 36.2587 18 6 6 -12 198.113 34.3729 16 6 6 -12 194.373 35.2948 14 -6 -6 -12 239.694 37.559 16 -6 -6 -12 255.485 32.0278 9 -6 -6 -12 232.939 18.8733 21 -6 6 -12 194.872 25.0689 11 6 -6 -12 218.148 30.4 20 -6 -6 12 231.029 27.2861 13 6 -6 -12 247.826 21.6674 21 -6 6 -12 224.684 25.4358 13 -7 -6 -12 115.018 12.9676 21 -7 -6 -12 119.519 22.2536 16 7 -6 12 125.004 16.5293 10 -7 -6 -12 106.875 20.2928 9 7 6 -12 118.062 20.7531 14 7 6 -12 118.79 20.9611 16 -7 -6 -12 96.6098 21.7963 18 7 -6 -12 109.254 17.7679 20 7 -6 -12 77.0846 24.5662 17 -7 6 -12 152.05 20.8284 13 -7 -6 12 141.608 22.0135 13 -7 6 -12 150.775 19.3787 11 7 -6 -12 116.404 15.4593 21 -8 -6 -12 268.84 30.9995 18 8 -6 12 227.006 23.8697 10 -8 -6 -12 270.868 32.0992 16 -8 -6 -12 263.121 19.1361 21 8 6 -12 280.298 29.7907 14 8 -6 12 242.36 28.1313 17 8 6 -12 250.833 32.0002 16 -8 -6 12 250.706 25.199 13 8 -6 -12 247.08 25.2908 20 8 -6 -12 236.304 24.384 21 -8 6 -12 239.505 24.0183 13 8 -6 -12 194.216 28.4951 17 -9 -6 -12 49.2688 6.94285 21 9 6 -12 56.9279 13.9325 16 9 -6 12 46.1084 12.3443 17 -9 -6 -12 24.8916 11.7185 18 -9 6 -12 46.2981 10.6839 13 9 -6 -12 53.4365 11.1418 20 9 -6 -12 58.0502 14.5379 17 9 -6 -12 55.4418 8.38533 11 -9 -6 12 31.0111 10.1199 13 -10 -6 -12 120.823 11.16 21 -10 -6 -12 100.514 16.512 18 10 -6 -12 130.995 13.5518 20 0 -7 -12 642.299 56.5982 17 0 -7 -12 699.252 48.8887 20 0 -7 -12 736.611 53.031 10 0 7 -12 761.866 57.8784 9 0 -7 -12 724.72 54.0087 6 0 -7 -12 674.447 77.5902 19 -1 -7 -12 75.698 18.1998 17 -1 -7 -12 62.2198 13.2187 7 -1 -7 -12 100.252 17.628 6 -1 -7 -12 56.6153 14.3854 10 1 7 -12 64.2602 20.4597 9 -1 -7 -12 94.9669 12.8504 20 -1 -7 -12 32.3856 28.6577 19 1 -7 -12 132.527 14.8976 20 1 -7 -12 127.492 21.5516 6 1 -7 -12 160.14 43.2097 19 -1 7 -12 116.203 19.5236 9 -1 -7 12 146.73 17.2526 13 1 -7 -12 118.02 21.0683 17 2 7 -12 381.474 49.0667 14 -2 -7 -12 397.04 32.8922 7 2 7 -12 453.224 45.4426 16 -2 -7 -12 365.169 52.9127 19 -2 -7 -12 429.849 34.3924 10 -2 -7 -12 376.417 35.8061 6 -2 -7 -12 412.333 31.7243 20 -2 7 -12 421.635 38.764 11 2 -7 -12 344.724 29.5801 21 2 -7 -12 380.496 71.384 19 -2 7 -12 445.716 33.708 13 2 -7 -12 408.202 41.0717 6 2 -7 -12 435.147 34.0108 20 -2 7 -12 403.729 38.3528 9 2 -7 -12 438.394 46.0405 17 -2 -7 12 458.851 32.966 13 3 7 -12 248.536 39.2547 14 -3 -7 -12 201.788 22.5908 10 -3 -7 -12 168.117 33.0814 19 -3 -7 -12 211.869 24.7598 7 -3 -7 -12 233.285 30.2824 9 3 7 -12 165.04 32.4624 16 -3 -7 -12 172.682 20.7805 20 3 -7 -12 209.703 25.3681 20 3 -7 -12 183.288 18.7097 21 3 -7 -12 255.548 39.1716 17 -3 7 -12 191.185 27.7567 9 3 -7 -12 228.914 48.4794 19 -3 -7 12 217.684 23.557 13 -3 7 -12 222.503 27.4807 11 -3 7 -12 189.803 32.5278 18 -3 7 -12 178.713 23.4189 13 -4 -7 -12 296.088 27.2194 10 -4 -7 -12 283.714 44.5222 16 -4 -7 -12 323.742 37.7117 9 4 7 -12 386.496 42.5176 14 4 7 -12 306.956 38.7475 16 -4 -7 -12 341.871 26.5138 20 4 -7 -12 276.438 44.536 17 -4 7 -12 302.224 28.9356 13 4 -7 -12 326.062 25.3638 21 -4 -7 12 282.88 29.3697 13 4 -7 -12 353.479 69.8943 19 4 -7 -12 321.592 31.9903 20 5 7 -12 271.954 38.3309 14 -5 -7 -12 287.24 36.6704 9 -5 -7 -12 281.66 39.8909 18 -5 -7 -12 274.3 40.4439 16 -5 -7 -12 274.538 19.4623 21 5 7 -12 251.984 35.834 16 -5 7 -12 230.245 26.1543 13 5 -7 -12 200.312 29.3191 20 5 -7 -12 240.072 21.5938 21 -5 -7 12 215.442 25.8652 13 -6 -7 -12 102.771 23.5117 18 -6 -7 -12 126.096 23.473 9 6 7 -12 90.8614 21.2476 14 6 7 -12 120.779 21.8685 16 -6 -7 -12 118.818 21.8861 16 -6 -7 -12 123.132 12.3233 21 -6 -7 12 127.706 18.9632 13 6 -7 -12 112.241 14.7761 21 6 -7 -12 80.0824 16.9938 20 -6 7 -12 121.022 16.8637 13 -7 -7 -12 176.229 29.7625 18 7 7 -12 182.732 30.4803 14 -7 -7 -12 201.935 16.2809 21 7 7 -12 160.911 29.2846 16 -7 -7 -12 205.603 31.0033 16 7 -7 -12 140.243 25.3137 17 7 -7 -12 169.68 23.3297 20 7 -7 -12 191.826 18.0156 21 -7 7 -12 217.129 22.0104 13 -7 -7 12 189.303 21.7697 13 8 7 -12 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319.638 26.3348 20 2 8 -12 354.77 43.7574 14 -2 -8 -12 347.951 48.9395 19 -2 8 -12 229.42 41.724 18 2 -8 -12 284.556 43.3222 17 2 -8 -12 277.876 66.1404 19 -2 8 -12 290.887 28.5416 13 2 -8 -12 280.205 28.1791 20 -2 -8 12 316.705 27.4033 13 -2 8 -12 291.41 33.7719 9 -3 -8 -12 248.454 22.1332 20 -3 -8 -12 248.541 25.2093 10 3 -8 12 235.927 25.1824 13 3 8 -12 247.607 32.6799 16 -3 -8 -12 214.125 41.8402 19 3 8 -12 283.913 39.153 14 -3 8 -12 236.243 30.0638 9 3 -8 -12 240.745 20.6555 21 -3 -8 12 236.337 23.2964 13 3 -8 -12 301.312 40.2962 17 3 -8 -12 283.016 61.6139 19 -3 8 -12 244.564 25.729 13 3 -8 -12 234.332 26.0576 20 -4 -8 -12 211.254 42.8836 16 -4 -8 -12 316.173 36.389 9 -4 -8 -12 289.797 27.2316 10 4 8 -12 234.059 35.8653 16 4 8 -12 345.818 39.5836 14 4 -8 12 309.598 27.6748 13 -4 -8 12 345.317 27.3964 13 4 -8 -12 250.521 58.3246 19 4 -8 -12 329.798 45.6959 17 4 -8 -12 326.304 23.987 21 4 -8 -12 298.737 30.5001 20 -4 8 -12 296.279 28.1304 13 5 -8 12 203.149 24.4048 13 -5 -8 -12 168.775 36.7 18 5 8 -12 255.31 34.8885 14 -5 -8 -12 230.336 34.9524 9 -5 -8 -12 238.086 36.1524 16 -5 -8 -12 230.083 16.6031 21 5 8 -12 187.672 32.8566 16 5 -8 -12 196.633 26.3649 20 5 -8 -12 218.916 39.9818 17 -5 -8 12 233.854 23.4805 13 5 -8 -12 231.898 19.2777 21 -5 8 -12 168.597 23.3209 13 6 8 -12 158.567 31.2041 16 -6 -8 -12 249.125 32.4791 18 -6 -8 -12 237.984 17.592 21 6 8 -12 197.372 33.7538 14 6 -8 12 244.433 24.0006 13 -6 -8 -12 278.614 33.6284 16 -6 -8 12 239.561 23.7226 13 6 -8 -12 223.083 25.7074 20 6 -8 -12 253.211 19.7491 21 6 -8 -12 248.378 37.8372 17 -6 8 -12 185.466 24.6044 13 -7 -8 -12 197.947 15.9718 21 -7 -8 -12 197.38 27.2942 18 7 8 -12 186.352 26.8921 14 7 8 -12 150.128 26.9218 16 7 -8 12 204.549 21.263 13 7 -8 -12 180.95 21.9701 20 7 -8 -12 208.213 17.1961 21 -7 -8 12 158.047 19.8603 13 -7 8 -12 212.318 19.9359 13 8 8 -12 116.108 20.774 16 8 -8 12 75.5335 19.357 19 -8 -8 -12 111.055 20.3561 18 8 8 -12 125.952 19.5702 14 -8 -8 -12 110.212 11.2677 21 8 -8 -12 105.207 13.2718 20 -8 -8 12 120.543 14.6087 13 8 -8 -12 124.341 13.1268 21 -8 8 -12 112.774 14.6834 13 8 -8 -12 152.515 22.0022 17 0 -9 12 36.9862 11.0724 13 0 -9 -12 29.4729 16.6435 10 0 -9 -12 54.2306 33.2333 19 0 9 -12 73.3684 18.1244 9 0 -9 -12 40.9171 9.92104 20 -1 -9 -12 288.797 31.5702 10 1 9 -12 235.2 37.4076 9 -1 -9 -12 260.498 49.7461 19 -1 -9 -12 259.3 24.1682 20 1 -9 12 280.629 25.731 13 1 -9 -12 213.576 46.2749 19 -1 -9 12 329.182 25.5595 13 1 -9 -12 296.608 25.1779 20 -1 9 -12 314.046 27.1163 13 1 -9 -12 352.603 35.5832 10 -1 9 -12 308.997 34.4976 9 -2 -9 -12 40.1815 25.0742 19 -2 -9 -12 62.5238 10.3486 20 2 -9 12 73.2646 11.8283 13 -2 -9 -12 63.1007 14.8879 10 2 9 -12 62.0366 23.1793 9 2 9 -12 92.6099 30.975 14 -2 9 -12 58.4172 17.0244 9 2 -9 -12 41.9155 9.03752 21 2 -9 -12 78.3955 38.6836 19 -2 9 -12 45.0564 12.5055 13 2 -9 -12 52.7918 11.9454 20 -2 -9 12 58.9525 11.7591 13 -2 9 -12 49.1085 27.2575 18 2 -9 -12 65.5158 21.8131 17 -3 -9 -12 222.557 20.1599 20 -3 -9 -12 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20.5441 20.77 9 -1 -5 -14 8.37916 4.78934 21 1 5 -14 8.1307 13.6325 16 -1 -5 -14 7.16988 23.713 19 1 5 -14 9.88498 7.08157 11 -1 5 -14 -4.8969 6.60791 11 1 -5 -14 13.7212 15.4834 17 1 -5 -14 5.20477 15.5518 6 1 -5 -14 5.59143 5.49636 21 -1 5 -14 18.0266 15.8569 9 -1 5 -14 -1.4621 8.22371 13 1 -5 -14 2.64765 30.509 19 -1 5 -14 -6.5051 22.141 18 2 5 -14 952.212 60.0427 11 -2 -5 -14 838.312 72.2145 9 2 5 -14 787.542 77.6348 14 -2 -5 -14 1077.66 78.7548 19 -2 -5 -14 902.352 56.6568 21 2 5 -14 803.349 70.9959 9 2 5 -14 956.141 69.7441 16 -2 -5 -14 926.2 66.053 17 -2 -5 -14 869.655 71.9671 16 2 -5 -14 836.608 66.0259 6 2 -5 -14 880.256 70.4223 17 -2 5 -14 1042.79 76.3742 18 2 -5 -14 807.477 58.1884 21 -2 5 -14 943.407 67.4606 9 2 -5 -14 895.39 90.7225 19 -2 5 -14 825.997 60.0607 13 -2 5 -14 899.467 59.4789 11 3 5 -14 62.19 19.6739 16 3 5 -14 76.3109 23.9294 14 -3 -5 -14 63.7447 9.15583 21 -3 -5 -14 77.738 14.9006 7 3 5 -14 77.8539 11.1642 11 -3 -5 -14 70.5637 20.5481 9 -3 -5 -14 54.2057 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15.8016 21 5 -5 -14 100.08 18.9723 20 -6 -5 -14 216.949 35.5792 16 6 5 -14 219.402 33.8583 16 6 5 -14 258.117 33.7987 14 -6 -5 -14 250.72 34.0191 9 -6 -5 -14 237.84 34.7042 18 6 5 -14 210.775 22.1304 11 -6 -5 -14 215.933 19.5166 21 6 -5 -14 239.497 21.8961 21 -6 5 -14 256.326 23.6229 13 -6 5 -14 279.222 24.2403 11 6 -5 -14 241.53 36.9164 17 6 -5 -14 239.44 26.5351 20 -7 -5 -14 54.0572 18.3588 18 7 5 -14 45.2484 17.8405 16 -7 -5 -14 55.183 16.5545 16 -7 -5 -14 70.7626 9.06995 21 7 5 -14 69.6205 16.8951 14 -7 5 -14 53.4877 10.9163 13 -7 5 -14 104.781 16.1852 11 7 -5 -14 52.8038 15.1612 20 7 -5 -14 53.2821 10.2667 21 -8 -5 -14 60.7109 15.1557 18 -8 -5 -14 81.5324 9.729 21 8 5 -14 120.353 20.1849 16 8 5 -14 99.4831 21.2782 14 -8 -5 -14 85.9083 16.5256 16 8 -5 -14 77.775 13.306 20 -8 5 -14 52.053 11.1566 11 8 -5 -14 62.0263 20.6476 12 -9 -5 -14 43.6074 6.20279 21 9 5 -14 53.0283 19.0866 16 -9 -5 -14 43.613 10.8357 18 9 -5 -14 34.9033 9.79657 20 0 6 -14 33.4626 8.61913 11 0 6 -14 28.808 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15.5942 10 3 6 -14 108.019 20.8403 16 3 6 -14 79.3299 21.5898 9 -3 -6 -14 126.27 27.7323 19 3 6 -14 101.775 13.2176 11 -3 -6 -14 123.217 24.8213 17 -3 6 -14 101.928 20.7477 9 -3 6 -14 92.0335 23.4089 18 -3 6 -14 84.3824 13.6428 13 3 -6 -14 65.9315 10.9527 21 3 -6 -14 140.094 41.4872 19 3 -6 -14 91.5852 16.9405 20 3 -6 -14 106.73 22.7005 17 -3 6 -14 101.225 13.7412 11 4 6 -14 292.278 39.836 14 -4 -6 -14 270.562 20.4067 21 4 6 -14 261.47 23.5129 11 -4 -6 -14 234.969 40.8803 16 4 6 -14 255.888 37.1576 16 -4 -6 -14 278.522 32.7994 17 -4 -6 -14 277.283 38.2917 9 -4 6 -14 284.121 25.0872 11 4 -6 -14 225.9 44.7017 17 -4 6 -14 236.815 37.4508 18 4 -6 -14 258.423 30.1774 20 4 -6 -14 247.159 22.3952 21 -4 6 -14 265.669 25.4161 13 -4 6 -14 221.309 33.3531 9 5 6 -14 55.433 17.8006 14 -5 -6 -14 50.1341 21.2176 18 -5 -6 -14 76.854 10.8994 21 5 6 -14 84.5606 20.9691 16 -5 -6 -14 58.315 19.3144 16 -5 -6 -14 96.1204 21.7367 9 5 -6 -14 71.912 23.4653 17 5 -6 -14 41.1443 15.4293 20 -5 6 -14 58.4786 13.5507 11 5 -6 -14 60.2822 10.421 21 -5 6 -14 65.5069 12.8552 13 -6 -6 -14 512.173 54.8355 9 -6 -6 -14 353.4 41 16 6 6 -14 355.338 38.997 14 6 6 -14 350.561 39.3406 16 -6 -6 -14 354.849 26.2407 21 -6 -6 -14 353.383 40.5566 18 6 -6 -14 416.471 28.9547 21 6 -6 -14 410.937 34.5336 20 -6 6 -14 308.798 31.0652 11 -6 6 -14 404.559 30.528 13 6 -6 -14 399.26 43.1212 17 7 6 -14 26.1021 14.891 14 7 6 -14 12.0538 15.6082 16 -7 -6 -14 18.854 14.2411 16 -7 -6 -14 23.9251 6.18322 21 -7 -6 -14 14.0505 16.2789 18 -7 -6 14 13.9792 12.332 13 -7 6 -14 32.848 9.15993 13 7 -6 -14 32.0563 12.7173 20 -7 6 -14 24.0656 9.55508 11 7 -6 -14 31.0257 16.9721 17 7 -6 -14 36.6074 8.34751 21 -8 -6 -14 264.172 29.1217 18 8 6 -14 330.092 29.5062 14 8 6 -14 369.709 31.0872 16 -8 -6 -14 296.631 22.0077 21 8 -6 -14 352.088 32.1246 17 -8 6 -14 277.988 23.1677 13 -8 6 -14 294.916 24.6045 11 8 -6 -14 331.317 23.881 21 -8 -6 14 285.469 26.3903 13 8 -6 -14 355.785 26.4152 20 -9 -6 -14 23.7863 5.12907 21 -9 -6 -14 29.3924 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177.672 25.4861 16 0 3 -20 122.553 15.4445 11 0 -3 -20 149.767 17.5234 12 1 3 -20 77.4739 18.1685 16 -1 -3 -20 98.873 19.121 16 1 3 -20 90.9136 11.9129 11 -1 -3 -20 71.6447 12.0999 12 -1 -3 -20 72.5655 9.9618 21 1 -3 -20 68.8288 17.0364 17 1 -3 -20 75.349 13.5061 12 -1 3 -20 45.3525 10.1568 12 -1 3 -20 60.7045 9.41026 11 1 -3 -20 63.1647 8.75451 21 -1 3 -20 49.3175 14.2635 16 -1 3 -20 61.5584 23.1868 18 2 3 -20 134.871 14.2858 11 -2 -3 -20 115.338 16.0469 12 -2 -3 -20 182.699 29.0057 16 -2 -3 -20 124.391 12.5081 21 2 3 -20 105.403 21.6053 16 2 -3 -20 137.44 14.1983 21 2 -3 -20 114.322 17.9202 12 -2 3 -20 146.185 21.2683 16 -2 3 -20 123.125 15.6631 12 -2 3 -20 118.611 14.6302 11 -2 3 -20 111.813 25.587 18 3 3 -20 84.1668 20.868 16 -3 -3 -20 54.5392 18.3981 16 -3 -3 -20 92.7368 10.9584 21 3 -3 -20 78.5066 10.3579 21 3 -3 -20 99.1177 18.6682 12 -3 3 -20 77.7399 20.3656 18 -4 -3 -20 102.068 19.9786 16 -4 -3 -20 104.131 11.7191 21 -4 3 -20 122.949 22.0302 18 4 -3 -20 89.6359 12.805 21 0 -4 -20 5.70368 5.74499 21 0 4 -20 -11.079 17.8844 18 0 4 -20 13.8786 7.57613 11 0 4 -20 25.3549 13.0044 16 1 4 -20 122.053 19.2237 16 -1 -4 -20 114.403 23.8257 16 -1 -4 -20 120.949 11.3573 21 1 4 -20 111.826 16.6377 11 -1 4 -20 119.114 17.5991 11 1 -4 -20 118.502 12.0291 21 -1 4 -20 117.133 24.1468 18 -1 4 -20 90.3327 16.3781 16 1 -4 -20 114.426 18.7001 17 -2 -4 -20 37.2617 6.29828 21 -2 -4 -20 35.6196 18.6903 16 2 4 -20 32.4352 16.328 16 2 -4 -20 38.0619 7.65228 21 -2 4 -20 33.9897 19.1829 18 3 4 -20 31.4883 21.2704 16 -3 4 -20 46.6945 16.0769 18 3 -4 -20 57.3171 8.37477 21 0 5 -20 164.746 31.6271 18 -1 5 -20 7.35147 18.3394 18 -2 5 -20 139.624 26.2464 18 0 0 -21 2.2975 8.04799 12 0 0 -21 -10.679 6.43347 21 0 0 -21 -19.266 17.8658 16 -1 0 -21 287.049 33.1012 16 -1 0 -21 269.093 22.5864 12 1 0 -21 293.325 23.6169 12 -1 0 -21 262.937 20.6344 21 1 0 -21 278.055 35.574 16 1 0 -21 244.145 20.8152 21 2 0 -21 0.32341 9.26239 21 -2 0 -21 9.09262 12.0441 16 -2 0 -21 8.10581 5.87687 21 0 1 -21 53.6596 16.0578 16 0 -1 -21 26.5561 19.5255 16 0 1 -21 32.2715 10.5761 12 0 -1 -21 24.8147 7.24022 21 0 -1 -21 34.4499 10.9464 12 -1 -1 -21 3.79845 5.73227 21 1 1 -21 -26.888 17.5041 16 -1 -1 -21 -1.9363 10.2621 12 -1 -1 -21 7.03374 16.6563 16 1 -1 -21 17.4348 6.27116 21 1 -1 -21 -19.124 20.32 16 -1 1 -21 5.97901 10.1163 12 1 -1 -21 12.7549 11.1952 12 -1 1 -21 -5.0291 13.6739 16 2 1 -21 40.3685 26.5128 16 -2 -1 -21 39.5963 7.05224 21 -2 -1 -21 68.6185 16.498 16 -2 1 -21 35.0383 17.4203 16 2 -1 -21 34.2334 7.59089 21 0 -2 -21 121.949 12.3969 21 0 2 -21 101.892 18.9381 16 1 2 -21 167.715 25.8506 16 -1 -2 -21 266.59 40.6496 16 -1 -2 -21 167.659 14.6447 21 -1 2 -21 176.349 31.6003 16 1 -2 -21 165.518 15.0501 21 -2 -2 -21 73.1339 9.96439 21 2 -2 -21 77.1279 10.756 21 0 -3 -21 6.45995 6.32694 21 1 -3 -21 49.5763 10.9962 21 _iucr_refine_instructions_details ; v34e.res created by SHELXL-2014/7 TITL v34e in P2(1)2(1)2(1) CELL 1.54178 11.8509 12.0635 17.8749 90 90 90 ZERR 4 0.0003 0.0004 0.0005 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O U UNIT 100 124 12 32 4 EQIV $1 0.5+X,0.5-Y,-Z EQIV $2 -X,-0.5+Y,0.5-Z DFIX 21 0.01 C23A C24A C21A C22A C23 C24 C21 C22 DFIX 20.9285 0.01 N3A C23A N3A C22A N3A C25A N3 C23 N3 C22 N3 C25 DFIX 21.6333 N3A C24A N3A C21A C23A C22A C23A C25A C22A C25A DFIX 21.6333 N3 C24 N3 C21 C23 C22 C23 C25 C22 C25 ISOR 0.01 0.02 C23 C22 ISOR 0.005 0.01 C25 EADP N3A N3 EADP C24A C24 EADP C21A C21 EXYZ N3A N3 EXYZ C24A C24 EXYZ C21A C21 L.S. 50 PLAN 20 SIZE 0.065 0.095 0.135 TEMP -73.16 HTAB C11 O8_$1 HTAB C13 O5 HTAB C13 O2 HTAB C20 O7_$2 BOND $H CONF HTAB fmap -2 acta 132 TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.027700 4.994700 BASF 0.01171 FVAR 0.27062 1.51765 0.79580 U 5 -0.025011 0.299159 0.157303 11.00000 0.03754 0.03070 = 0.04030 0.00183 0.00959 0.00055 O1 4 0.010647 0.416743 0.062518 11.00000 0.04709 0.05542 = 0.04744 0.02406 -0.00922 -0.01380 O2 4 0.138794 0.343616 0.207868 11.00000 0.04569 0.03464 = 0.04604 0.00558 -0.00135 0.00145 O8 4 0.041023 0.184942 0.110444 11.00000 0.03730 0.04383 = 0.04765 -0.00645 -0.00008 -0.00428 O7 4 -0.100724 0.403702 0.206840 11.00000 0.07773 0.03825 = 0.07171 0.00940 0.02727 0.01282 O6 4 0.136994 0.570396 -0.009983 11.00000 0.05388 0.04940 = 0.05018 0.01650 0.00491 -0.00723 O5 4 0.381894 0.597395 -0.015779 11.00000 0.04230 0.05087 = 0.06816 -0.00308 0.00496 -0.00752 O4 4 0.538366 0.452137 0.077771 11.00000 0.04476 0.06180 = 0.06264 -0.01006 -0.00124 -0.00785 O3 4 0.358140 0.420687 0.187529 11.00000 0.05389 0.05532 = 0.04732 -0.00961 -0.00077 -0.00732 PART 1 N3A 3 -0.193490 0.168103 0.197692 31.00000 0.04620 0.04978 = 0.07817 0.01185 0.02721 0.01424 C23A 1 -0.296623 0.198273 0.157587 31.00000 0.03878 0.06049 = 0.08312 -0.00191 0.01306 -0.01005 AFIX 23 H23A 2 -0.324391 0.270173 0.176925 31.00000 -1.20000 H23B 2 -0.355251 0.141815 0.167827 31.00000 -1.20000 AFIX 0 C24A 1 -0.280268 0.207277 0.075344 31.00000 0.04418 0.05720 = 0.10325 0.01359 -0.00301 -0.01681 AFIX 23 H24A 2 -0.259697 0.134163 0.054209 31.00000 -1.20000 H24B 2 -0.350846 0.232624 0.051152 31.00000 -1.20000 AFIX 0 C21A 1 -0.099403 0.151257 0.319776 31.00000 0.10141 0.06440 = 0.04985 0.00637 0.02280 -0.01795 AFIX 23 H21A 2 -0.101937 0.183758 0.370605 31.00000 -1.20000 H21B 2 -0.094631 0.069684 0.324947 31.00000 -1.20000 AFIX 0 C22A 1 -0.207833 0.181933 0.277242 31.00000 0.05523 0.07358 = 0.05402 -0.00968 0.02901 -0.01759 AFIX 23 H22A 2 -0.270579 0.134323 0.294692 31.00000 -1.20000 H22B 2 -0.227892 0.259948 0.288127 31.00000 -1.20000 AFIX 0 C25A 1 -0.166128 0.051300 0.179316 31.00000 0.06122 0.04293 = 0.06568 0.00048 0.01175 -0.00659 AFIX 33 H25A 2 -0.156730 0.043660 0.125090 31.00000 -1.50000 H25B 2 -0.095965 0.029965 0.204508 31.00000 -1.50000 H25E 2 -0.227606 0.003073 0.196204 31.00000 -1.50000 AFIX 0 PART 0 PART 2 N3 3 -0.193490 0.168103 0.197692 -31.00000 0.04620 0.04978 = 0.07817 0.01185 0.02721 0.01424 C23 1 -0.244217 0.122322 0.133128 -31.00000 0.06054 0.05936 = 0.06664 -0.00250 0.00339 -0.01009 AFIX 23 H24C 2 -0.311249 0.079001 0.148542 -31.00000 -1.20000 H24D 2 -0.190242 0.070332 0.109552 -31.00000 -1.20000 AFIX 0 C24 1 -0.280268 0.207277 0.075344 -31.00000 0.04418 0.05720 = 0.10325 0.01359 -0.00301 -0.01681 AFIX 23 H25C 2 -0.299540 0.169241 0.027960 -31.00000 -1.20000 H25D 2 -0.348399 0.246690 0.093222 -31.00000 -1.20000 AFIX 0 C21 1 -0.099403 0.151257 0.319776 -31.00000 0.10141 0.06440 = 0.04985 0.00637 0.02280 -0.01795 AFIX 23 H21C 2 -0.149152 0.211602 0.337693 -31.00000 -1.20000 H21D 2 -0.080836 0.100086 0.361289 -31.00000 -1.20000 AFIX 0 C22 1 -0.145683 0.092220 0.251595 -31.00000 0.04255 0.04364 = 0.05925 0.00826 0.00289 -0.00291 AFIX 23 H22C 2 -0.084220 0.049603 0.227517 -31.00000 -1.20000 H22D 2 -0.204495 0.038977 0.267593 -31.00000 -1.20000 AFIX 0 C25 1 -0.256174 0.255128 0.234935 -31.00000 0.07389 0.07261 = 0.08358 0.01085 0.00742 -0.00499 AFIX 33 H23D 2 -0.213769 0.280853 0.278684 -31.00000 -1.50000 H23E 2 -0.267584 0.317094 0.200298 -31.00000 -1.50000 H23F 2 -0.329590 0.226329 0.251025 -31.00000 -1.50000 AFIX 0 PART 0 N1 3 -0.189591 0.287371 0.061892 11.00000 0.02625 0.04729 = 0.07409 -0.00044 0.00083 -0.00121 C1 1 -0.203081 0.343147 0.001068 11.00000 0.02973 0.04447 = 0.07980 -0.00848 -0.00887 0.00431 AFIX 43 H1 2 -0.270892 0.328152 -0.025408 11.00000 -1.20000 AFIX 0 C2 1 -0.130700 0.424736 -0.032683 11.00000 0.04563 0.03739 = 0.04803 0.00022 -0.00246 0.00470 C7 1 -0.027241 0.457288 -0.001123 11.00000 0.04833 0.03419 = 0.03966 -0.00129 0.00610 0.00370 C3 1 -0.168708 0.467236 -0.100981 11.00000 0.07357 0.05589 = 0.05774 -0.00153 -0.01753 0.00366 AFIX 43 H3 2 -0.238561 0.442839 -0.121197 11.00000 -1.20000 AFIX 0 C4 1 -0.105994 0.543249 -0.138418 11.00000 0.08340 0.06363 = 0.05773 0.00387 -0.01883 0.01356 AFIX 43 H4 2 -0.131861 0.572579 -0.184664 11.00000 -1.20000 AFIX 0 C5 1 -0.004334 0.577599 -0.108767 11.00000 0.07464 0.05497 = 0.04237 0.00942 0.00387 0.00291 AFIX 43 H5 2 0.039187 0.630257 -0.135769 11.00000 -1.20000 AFIX 0 C6 1 0.036897 0.538367 -0.041135 11.00000 0.03966 0.04351 = 0.03880 -0.00181 0.00511 0.00537 C8 1 0.196724 0.654018 -0.050036 11.00000 0.05316 0.04332 = 0.06414 0.01158 0.01950 -0.00676 AFIX 23 H8A 2 0.148761 0.720815 -0.054942 11.00000 -1.20000 H8B 2 0.214772 0.626945 -0.100933 11.00000 -1.20000 AFIX 0 C9 1 0.302962 0.683195 -0.010137 11.00000 0.05306 0.04136 = 0.08289 0.00474 0.01407 -0.00631 AFIX 23 H9A 2 0.335008 0.751758 -0.031930 11.00000 -1.20000 H9B 2 0.286196 0.697569 0.043247 11.00000 -1.20000 AFIX 0 C10 1 0.488673 0.627011 0.013446 11.00000 0.04977 0.06490 = 0.06306 -0.00445 0.00659 -0.02059 AFIX 23 H10A 2 0.479403 0.659245 0.064007 11.00000 -1.20000 H10B 2 0.524129 0.683593 -0.019061 11.00000 -1.20000 AFIX 0 C11 1 0.563133 0.526379 0.017634 11.00000 0.03412 0.07238 = 0.07311 -0.02097 0.00152 -0.00783 AFIX 23 H11A 2 0.556722 0.485186 -0.030079 11.00000 -1.20000 H11B 2 0.642417 0.551188 0.022548 11.00000 -1.20000 AFIX 0 C12 1 0.442254 0.384086 0.065434 11.00000 0.04756 0.06081 = 0.05423 -0.01111 0.00480 -0.00707 AFIX 23 H12A 2 0.460474 0.307103 0.080341 11.00000 -1.20000 H12B 2 0.424419 0.383718 0.011326 11.00000 -1.20000 AFIX 0 C13 1 0.340194 0.422046 0.108065 11.00000 0.05303 0.05690 = 0.04321 -0.00466 0.00108 -0.00307 AFIX 23 H13A 2 0.320534 0.498283 0.092241 11.00000 -1.20000 H13B 2 0.275655 0.373255 0.095722 11.00000 -1.20000 AFIX 0 C14 1 0.338562 0.318659 0.220401 11.00000 0.05955 0.04843 = 0.03713 -0.01099 -0.01422 0.00613 C19 1 0.224771 0.286255 0.233376 11.00000 0.06895 0.03757 = 0.03555 -0.01684 -0.01520 0.00684 C15 1 0.427867 0.252793 0.243441 11.00000 0.05433 0.07787 = 0.05332 -0.01693 -0.02006 0.01006 AFIX 43 H15 2 0.503037 0.274100 0.231862 11.00000 -1.20000 AFIX 0 C16 1 0.408184 0.155320 0.283557 11.00000 0.09324 0.06037 = 0.05450 -0.01089 -0.03002 0.03258 AFIX 43 H16 2 0.469941 0.110156 0.298359 11.00000 -1.20000 AFIX 0 C17 1 0.301006 0.124666 0.301566 11.00000 0.09825 0.05543 = 0.04276 0.00134 -0.02094 0.00321 AFIX 43 H17 2 0.288938 0.059932 0.330754 11.00000 -1.20000 AFIX 0 C18 1 0.208486 0.187221 0.277658 11.00000 0.09066 0.03788 = 0.03852 -0.00636 -0.02106 0.00339 C20 1 0.094929 0.156873 0.302500 11.00000 0.10170 0.03990 = 0.03207 -0.00140 0.00469 -0.00828 AFIX 43 H20 2 0.091343 0.102740 0.341026 11.00000 -1.20000 AFIX 0 N2 3 0.002008 0.192644 0.279811 11.00000 0.08190 0.03843 = 0.04346 0.00351 0.00906 -0.00287 HKLF 4 REM v34e in P2(1)2(1)2(1) REM R1 = 0.0298 for 4390 Fo > 4sig(Fo) and 0.0322 for all 4586 data REM 364 parameters refined using 38 restraints END WGHT 0.0277 4.9952 REM Instructions for potential hydrogen bonds EQIV $3 x-1/2, -y+1/2, -z HTAB C25A O5_$3 HTAB C25A N2 HTAB C22 O2_$2 HTAB C22 O3_$2 HTAB C25 N1 HTAB C11 O8_$1 HTAB C13 O5 HTAB C13 O2 HTAB C20 O7_$2 REM Highest difference peak 1.564, deepest hole -1.206, 1-sigma level 0.113 Q1 1 0.0401 0.3224 0.1689 11.00000 0.05 1.56 Q2 1 -0.1146 0.3051 0.1565 11.00000 0.05 1.41 Q3 1 -0.0718 0.2988 0.1248 11.00000 0.05 -1.21 Q4 1 0.0528 0.2632 0.1566 11.00000 0.05 1.18 Q5 1 -0.0230 0.4157 0.1569 11.00000 0.05 0.90 Q6 1 0.0242 0.1092 0.1791 11.00000 0.05 0.89 Q7 1 -0.0255 0.1840 0.1572 11.00000 0.05 0.88 Q8 1 -0.0211 0.3389 0.1193 11.00000 0.05 0.82 Q9 1 -0.0187 0.3439 0.1991 11.00000 0.05 0.82 Q10 1 -0.0199 0.2575 0.1189 11.00000 0.05 0.77 Q11 1 -0.1618 0.2408 0.1545 11.00000 0.05 -0.73 Q12 1 -0.1643 0.3644 0.1582 11.00000 0.05 -0.72 Q13 1 -0.0220 0.0819 0.1659 11.00000 0.05 -0.71 Q14 1 0.1063 0.2214 0.1536 11.00000 0.05 -0.69 Q15 1 0.0791 0.0953 0.1564 11.00000 0.05 -0.67 Q16 1 0.0576 0.3010 0.0770 11.00000 0.05 -0.65 Q17 1 -0.0185 0.2564 0.1981 11.00000 0.05 0.63 Q18 1 -0.1216 0.3003 0.0788 11.00000 0.05 -0.56 Q19 1 -0.1168 0.2974 0.2358 11.00000 0.05 -0.55 Q20 1 -0.2597 0.2697 0.2634 11.00000 0.05 0.54 REM The information below was added by Olex2. REM REM R1 = 0.0298 for 4390 Fo > 4sig(Fo) and 0.0322 for all 21343 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.56, deepest hole -1.21 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0322 REM R1_gt = 0.0298 REM wR_ref = 0.0711 REM GOOF = 1.043 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 21343 REM Reflections_gt = 4390 REM Parameters = n/a REM Hole = -1.21 REM Peak = 1.56 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.988(13) 2 0.012(13) data_L(salben)UO2K _audit_creation_date 2019-08-15 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2014/7' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C26 H31 F3 K N3 O11 S U' _chemical_formula_sum 'C26 H31 F3 K N3 O11 S U' _chemical_formula_weight 927.73 _chemical_absolute_configuration ? _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'orthorhombic' _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.9299(6) _cell_length_b 13.2222(6) _cell_length_c 18.4887(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3160.9(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8448 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 68.244 _cell_measurement_theta_min 4.111 _shelx_estimated_absorpt_T_max 0.550 _shelx_estimated_absorpt_T_min 0.161 _exptl_absorpt_coefficient_mu 16.968 _exptl_absorpt_correction_T_max 0.7133 _exptl_absorpt_correction_T_min 0.0386 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1271 before and 0.0560 after correction. The Ratio of minimum to maximum transmission is 0.0541. The \l/2 correction factor is 0.00150.' _exptl_absorpt_special_details ? _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.950 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description 'Rectangular parallelepiped' _exptl_crystal_F_000 1800 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.085 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_unetI/netI 0.0456 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 12833 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 66.000 _diffrn_reflns_theta_max 68.426 _diffrn_reflns_theta_min 4.110 _diffrn_ambient_temperature 199.99 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device_type 'Bruker Platinum 135 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'Helios high-brilliance multilayer optics' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.780 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.984 _reflns_number_gt 4839 _reflns_number_total 5277 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _refine_diff_density_max 1.362 _refine_diff_density_min -1.456 _refine_diff_density_rms 0.153 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.526(13) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 496 _refine_ls_number_reflns 5277 _refine_ls_number_restraints 74 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0357 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+3.5456P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0953 _refine_ls_wR_factor_ref 0.0990 _refine_special_details ; Refined as a 2-component inversion twin. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.474(13) 0.526(13) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 3. Shared sites {C9, C9'} 4. Restrained distances S1-O11 = S1-O12 = S1-O13 = S1'-O11' = S1'-O12' = S1'-O13' 1.40954 with sigma of 0.01 C26-F11 = C26-F12 = C26-F13 = C26'-F11' = C26'-F12' = C26'-F13' 1.305234 with sigma of 0.01 S1-C26 = S1'-C26' 1.805621 with sigma of 0.01 F11-F12 = F11-F13 = F12-F13 = F11'-F12' = F11'-F13' = F12'-F13' 2.098805 with sigma of 0.02 O11-O12 = O11-O13 = O12-O13 = O11'-O12' = O11'-O13' = O12'-O13' 2.384942 with sigma of 0.02 C26-O11 = C26-O12 = C26-O13 = C26'-O11' = C26'-O12' = C26'-O13' 2.517438 with sigma of 0.02 S1-F11 = S1-F12 = S1-F13 = S1'-F11' = S1'-F12' = S1'-F13' 2.592144 with sigma of 0.02 5. Uiso/Uaniso restraints and constraints Uanis(C26) \\sim Ueq, Uanis(O12') \\sim Ueq, Uanis(O13') \\sim Ueq, Uanis(F12') \\sim Ueq, Uanis(C26') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(F13') \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(C9) = Uanis(C9') 6. Others Sof(S1')=Sof(O11')=Sof(O12')=Sof(O13')=Sof(F11')=Sof(F12')=Sof(F13')= Sof(C26')=1-FVAR(1) Sof(S1)=Sof(O11)=Sof(O12)=Sof(O13)=Sof(F11)=Sof(F12)=Sof(F13)=Sof(C26)=FVAR(1) Sof(C8')=Sof(H8'A)=Sof(H8'B)=Sof(C9')=Sof(H9'A)=Sof(H9'B)=1-FVAR(2) Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=FVAR(2) 1(DFIX)=0.926*FVAR(4) 1(DFIX)=FVAR(3) 1(DFIX)=1.281*FVAR(4) 1(DFIX)=1.489*FVAR(4) 1(DFIX)=1.692*FVAR(4) 1(DFIX)=1.786*FVAR(4) 1(DFIX)=1.839*FVAR(4) 7.a Riding coordinates: C8'(H8'A,H8'B) 7.b Secondary CH2 refined with riding coordinates: C8(H8A,H8B), C9(H9A,H9B), C9'(H9'A,H9'B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B) 7.c Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C20(H20) 7.d Idealised Me refined as rotating group: C25(H25A,H25B,H25C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary ? _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U U 0.50223(3) 0.20115(2) 0.44409(2) 0.04106(13) Uani 1 1 d . . . . . K K 0.5441(3) 0.4629(4) 0.3830(3) 0.1031(13) Uani 1 1 d . . . . . O1 O 0.4013(6) 0.3271(6) 0.4036(5) 0.045(2) Uani 1 1 d . . . . . O6 O 0.3799(6) 0.4866(7) 0.3170(6) 0.065(2) Uani 1 1 d . . . . . O5 O 0.5187(10) 0.6322(7) 0.3380(7) 0.101(4) Uani 1 1 d . . . . . O4 O 0.7221(8) 0.5684(8) 0.3495(7) 0.082(3) Uani 1 1 d . . . . . O3 O 0.6530(7) 0.4001(8) 0.2766(6) 0.067(2) Uani 1 1 d . . . . . O2 O 0.6310(6) 0.2993(7) 0.3980(5) 0.052(2) Uani 1 1 d . . . . . O7 O 0.5100(8) 0.2622(5) 0.5293(4) 0.0514(17) Uani 1 1 d . . . . . O8 O 0.4909(7) 0.1309(5) 0.3623(4) 0.0516(18) Uani 1 1 d . . . . . N1 N 0.3155(8) 0.1450(8) 0.4563(6) 0.049(3) Uani 1 1 d . . . . . N3 N 0.4817(8) 0.0356(7) 0.5196(6) 0.054(3) Uani 1 1 d . . . . . N2 N 0.6730(8) 0.1095(8) 0.4644(7) 0.052(3) Uani 1 1 d . . . . . C1 C 0.2405(9) 0.1763(10) 0.4168(9) 0.054(3) Uani 1 1 d . . . . . H1 H 0.1765 0.1418 0.4224 0.065 Uiso 1 1 calc R . . . . C2 C 0.2418(9) 0.2586(10) 0.3643(8) 0.052(3) Uani 1 1 d . . . . . C3 C 0.1532(10) 0.2651(11) 0.3201(9) 0.068(4) Uani 1 1 d . . . . . H3 H 0.0987 0.2174 0.3245 0.081 Uiso 1 1 calc R . . . . C4 C 0.1476(11) 0.3431(13) 0.2699(8) 0.065(4) Uani 1 1 d . . . . . H4 H 0.0911 0.3453 0.2372 0.078 Uiso 1 1 calc R . . . . C5 C 0.2212(10) 0.4165(12) 0.2666(8) 0.064(4) Uani 1 1 d . . . . . H5 H 0.2154 0.4698 0.2324 0.077 Uiso 1 1 calc R . . . . C7 C 0.3191(8) 0.3299(10) 0.3623(7) 0.049(3) Uani 1 1 d . . . . . C6 C 0.3055(9) 0.4127(10) 0.3141(7) 0.053(3) Uani 1 1 d . . . . . C8 C 0.362(2) 0.577(2) 0.279(3) 0.102(15) Uani 0.71(5) 1 d . . P A 1 H8A H 0.2876 0.5934 0.2793 0.122 Uiso 0.71(5) 1 calc R . P A 1 H8B H 0.3838 0.5682 0.2275 0.122 Uiso 0.71(5) 1 calc R . P A 1 C9 C 0.4250(11) 0.6631(11) 0.3141(10) 0.070(4) Uani 0.71(5) 1 d . . P A 1 H9A H 0.4348 0.7181 0.2784 0.084 Uiso 0.71(5) 1 calc R . P A 1 H9B H 0.3851 0.6908 0.3553 0.084 Uiso 0.71(5) 1 calc R . P A 1 C8' C 0.352(3) 0.587(3) 0.336(3) 0.037(12) Uiso 0.29(5) 1 d . . P A 2 H8'A H 0.3427 0.5922 0.3875 0.045 Uiso 0.29(5) 1 d R . P A 2 H8'B H 0.2873 0.6037 0.3133 0.045 Uiso 0.29(5) 1 d R . P A 2 C9' C 0.4250(11) 0.6631(11) 0.3141(10) 0.070(4) Uani 0.29(5) 1 d . . P A 2 H9'A H 0.4255 0.6698 0.2608 0.084 Uiso 0.29(5) 1 calc R . P A 2 H9'B H 0.4069 0.7294 0.3355 0.084 Uiso 0.29(5) 1 calc R . P A 2 C10 C 0.6027(13) 0.7034(12) 0.3207(11) 0.083(5) Uani 1 1 d . . . . . H10A H 0.5826 0.7732 0.3339 0.099 Uiso 1 1 calc R . . . . H10B H 0.6185 0.7014 0.2683 0.099 Uiso 1 1 calc R . . . . C11 C 0.6995(15) 0.6690(13) 0.3659(12) 0.095(6) Uani 1 1 d . . . . . H11A H 0.7596 0.7124 0.3540 0.114 Uiso 1 1 calc R . . . . H11B H 0.6848 0.6760 0.4182 0.114 Uiso 1 1 calc R . . . . C12 C 0.7585(13) 0.5470(13) 0.2751(11) 0.082(5) Uani 1 1 d . . . . . H12A H 0.7709 0.6117 0.2496 0.099 Uiso 1 1 calc R . . . . H12B H 0.8249 0.5099 0.2774 0.099 Uiso 1 1 calc R . . . . C13 C 0.6851(12) 0.4883(13) 0.2349(9) 0.075(4) Uani 1 1 d . . . . . H13A H 0.7166 0.4660 0.1887 0.090 Uiso 1 1 calc R . . . . H13B H 0.6240 0.5304 0.2234 0.090 Uiso 1 1 calc R . . . . C14 C 0.7247(9) 0.3288(10) 0.2921(7) 0.053(3) Uani 1 1 d . . . . . C15 C 0.8090(11) 0.3075(13) 0.2466(9) 0.069(4) Uani 1 1 d . . . . . H15 H 0.8198 0.3459 0.2038 0.083 Uiso 1 1 calc R . . . . C16 C 0.8775(11) 0.2284(13) 0.2652(10) 0.072(4) Uani 1 1 d . . . . . H16 H 0.9346 0.2132 0.2348 0.086 Uiso 1 1 calc R . . . . C17 C 0.8612(9) 0.1718(11) 0.3292(9) 0.064(4) Uani 1 1 d . . . . . H17 H 0.9091 0.1211 0.3435 0.077 Uiso 1 1 calc R . . . . C18 C 0.7743(9) 0.1916(10) 0.3706(8) 0.054(3) Uani 1 1 d . . . . . C19 C 0.7072(9) 0.2706(9) 0.3552(7) 0.048(3) Uani 1 1 d . . . . . C20 C 0.7590(9) 0.1244(10) 0.4298(8) 0.055(3) Uani 1 1 d . . . . . H20 H 0.8175 0.0869 0.4456 0.066 Uiso 1 1 calc R . . . . C21 C 0.6729(11) 0.0277(12) 0.5165(9) 0.067(4) Uani 1 1 d . . . . . H21A H 0.6827 0.0549 0.5659 0.081 Uiso 1 1 calc R . . . . H21B H 0.7301 -0.0198 0.5060 0.081 Uiso 1 1 calc R . . . . C22 C 0.5689(12) -0.0272(14) 0.5112(12) 0.086(5) Uani 1 1 d . . . . . H22A H 0.5647 -0.0610 0.4635 0.103 Uiso 1 1 calc R . . . . H22B H 0.5667 -0.0805 0.5488 0.103 Uiso 1 1 calc R . . . . C25 C 0.469(2) 0.0570(15) 0.5985(11) 0.128(11) Uani 1 1 d . . . . . H25A H 0.4242 0.1163 0.6048 0.192 Uiso 1 1 calc GR . . . . H25B H 0.5366 0.0704 0.6202 0.192 Uiso 1 1 calc GR . . . . H25C H 0.4371 -0.0016 0.6222 0.192 Uiso 1 1 calc GR . . . . C23 C 0.3828(13) -0.0146(12) 0.4961(12) 0.084(5) Uani 1 1 d . . . . . H23A H 0.3901 -0.0387 0.4456 0.101 Uiso 1 1 calc R . . . . H23B H 0.3692 -0.0741 0.5272 0.101 Uiso 1 1 calc R . . . . C24 C 0.2945(11) 0.0568(12) 0.5008(11) 0.071(4) Uani 1 1 d . . . . . H24A H 0.2305 0.0231 0.4840 0.085 Uiso 1 1 calc R . . . . H24B H 0.2842 0.0779 0.5517 0.085 Uiso 1 1 calc R . . . . S1 S 0.5415(7) 0.5777(7) 0.5648(5) 0.067(3) Uani 0.719(15) 1 d D . P A 1 O11 O 0.516(2) 0.5125(16) 0.5070(12) 0.170(16) Uani 0.719(15) 1 d D . P A 1 O12 O 0.515(2) 0.5362(14) 0.6336(9) 0.155(13) Uani 0.719(15) 1 d D . P A 1 O13 O 0.6375(11) 0.6280(17) 0.5656(14) 0.138(11) Uani 0.719(15) 1 d D . P A 1 F11 F 0.4565(16) 0.7452(12) 0.6085(10) 0.091(6) Uani 0.719(15) 1 d D . P A 1 F12 F 0.454(3) 0.7250(11) 0.4965(8) 0.20(2) Uani 0.719(15) 1 d D . P A 1 F13 F 0.3539(12) 0.6404(16) 0.5629(18) 0.190(14) Uani 0.719(15) 1 d D . P A 1 C26 C 0.4476(12) 0.6769(10) 0.5578(9) 0.090(8) Uani 0.719(15) 1 d D U P A 1 S1' S 0.5074(14) 0.5635(13) 0.5654(12) 0.062(6) Uani 0.281(15) 1 d D . P A 2 O11' O 0.5270(18) 0.5176(15) 0.4979(13) 0.026(8) Uani 0.281(15) 1 d D . P A 2 O12' O 0.403(2) 0.568(3) 0.587(2) 0.15(3) Uani 0.281(15) 1 d D U P A 2 O13' O 0.575(3) 0.536(3) 0.6216(17) 0.081(15) Uani 0.281(15) 1 d D U P A 2 F11' F 0.520(5) 0.751(2) 0.607(2) 0.13(3) Uani 0.281(15) 1 d D . P A 2 F12' F 0.639(3) 0.706(3) 0.539(3) 0.16(2) Uani 0.281(15) 1 d D U P A 2 F13' F 0.491(5) 0.732(3) 0.496(3) 0.20(4) Uani 0.281(15) 1 d D U P A 2 C26' C 0.540(3) 0.6941(16) 0.5507(18) 0.086(19) Uani 0.281(15) 1 d D U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.03647(19) 0.04754(18) 0.0392(2) -0.00131(12) -0.0024(2) -0.0023(2) K 0.093(3) 0.103(3) 0.113(3) 0.010(3) -0.006(2) -0.002(2) O1 0.041(4) 0.058(5) 0.036(5) 0.004(4) -0.010(4) -0.001(3) O6 0.050(4) 0.065(5) 0.080(7) 0.018(5) -0.011(5) -0.001(4) O5 0.115(10) 0.069(5) 0.119(9) 0.044(6) -0.054(9) -0.027(6) O4 0.078(7) 0.075(6) 0.095(9) 0.019(6) -0.016(6) -0.015(5) O3 0.057(5) 0.076(6) 0.067(6) 0.014(6) 0.001(5) -0.007(5) O2 0.032(4) 0.068(5) 0.056(6) 0.000(5) 0.002(4) -0.013(4) O7 0.062(5) 0.053(3) 0.040(4) -0.001(3) -0.016(5) -0.002(4) O8 0.042(4) 0.063(4) 0.049(4) -0.016(3) -0.020(5) 0.000(4) N1 0.051(6) 0.052(6) 0.044(6) -0.002(5) 0.010(5) 0.003(4) N3 0.047(6) 0.046(4) 0.071(7) 0.002(4) -0.001(6) -0.007(4) N2 0.052(5) 0.048(5) 0.056(7) 0.003(5) -0.004(5) -0.004(5) C1 0.038(5) 0.049(6) 0.075(10) -0.014(7) 0.009(6) -0.003(5) C2 0.033(6) 0.061(7) 0.063(9) -0.016(7) -0.006(6) 0.014(5) C3 0.048(7) 0.079(9) 0.075(11) -0.026(9) -0.001(7) 0.002(6) C4 0.051(7) 0.093(10) 0.050(8) -0.009(8) -0.019(7) 0.002(7) C5 0.054(7) 0.080(9) 0.059(9) -0.001(7) -0.015(7) 0.002(7) C7 0.033(5) 0.067(7) 0.046(7) -0.011(6) 0.003(5) 0.015(5) C6 0.045(6) 0.066(7) 0.049(7) -0.003(6) 0.001(6) 0.012(5) C8 0.069(14) 0.086(16) 0.15(4) 0.06(2) -0.040(18) -0.011(12) C9 0.062(8) 0.058(8) 0.090(12) 0.019(8) 0.001(8) 0.007(6) C9' 0.062(8) 0.058(8) 0.090(12) 0.019(8) 0.001(8) 0.007(6) C10 0.084(10) 0.066(9) 0.098(14) 0.017(10) 0.002(10) -0.027(8) C11 0.097(12) 0.083(11) 0.104(15) 0.021(10) -0.005(11) -0.025(10) C12 0.066(9) 0.089(10) 0.092(12) 0.041(10) 0.013(10) -0.011(8) C13 0.074(9) 0.095(10) 0.057(9) 0.036(8) -0.013(8) 0.001(8) C14 0.039(6) 0.068(7) 0.054(8) 0.007(6) -0.006(6) -0.006(5) C15 0.056(7) 0.083(9) 0.067(10) 0.003(8) 0.010(7) -0.022(8) C16 0.042(7) 0.090(10) 0.084(12) -0.010(9) -0.001(7) -0.004(7) C17 0.042(6) 0.075(8) 0.076(10) -0.017(8) 0.000(7) -0.006(6) C18 0.041(6) 0.060(7) 0.060(9) -0.007(7) -0.005(6) -0.010(6) C19 0.032(5) 0.058(7) 0.054(8) -0.008(6) -0.002(6) -0.013(5) C20 0.046(6) 0.055(7) 0.063(9) -0.008(7) -0.009(6) 0.004(5) C21 0.069(8) 0.066(9) 0.067(10) 0.012(8) -0.021(8) 0.000(7) C22 0.063(9) 0.085(11) 0.109(15) 0.034(11) 0.005(10) 0.006(8) C25 0.21(3) 0.077(9) 0.100(15) 0.003(9) 0.071(18) 0.008(14) C23 0.092(11) 0.062(9) 0.100(14) -0.009(9) 0.006(11) -0.008(8) C24 0.056(8) 0.068(9) 0.087(13) 0.007(9) 0.013(8) 0.000(7) S1 0.074(6) 0.066(4) 0.061(4) -0.010(3) 0.008(4) -0.005(4) O11 0.28(4) 0.14(2) 0.080(16) -0.042(15) -0.03(2) 0.14(2) O12 0.30(4) 0.070(10) 0.091(14) 0.016(9) 0.06(3) 0.03(2) O13 0.099(14) 0.16(2) 0.16(3) -0.09(2) 0.028(15) -0.029(14) F11 0.131(14) 0.062(9) 0.079(13) -0.024(9) 0.012(12) -0.002(9) F12 0.47(6) 0.077(9) 0.058(9) -0.008(7) -0.067(18) 0.11(2) F13 0.098(13) 0.16(2) 0.32(4) -0.10(3) -0.067(18) 0.031(13) C26 0.099(12) 0.080(11) 0.090(13) -0.016(10) -0.007(10) -0.002(10) S1' 0.053(10) 0.046(6) 0.087(12) 0.008(6) -0.008(13) -0.005(8) O11' 0.039(16) 0.011(10) 0.028(15) 0.008(10) -0.010(11) -0.016(11) O12' 0.13(3) 0.16(3) 0.16(3) -0.03(2) 0.00(2) 0.01(2) O13' 0.11(2) 0.08(2) 0.05(2) -0.003(18) -0.027(19) 0.030(19) F11' 0.24(8) 0.07(3) 0.07(3) 0.02(2) -0.02(5) -0.04(4) F12' 0.18(3) 0.15(3) 0.15(3) -0.01(2) 0.03(2) -0.04(2) F13' 0.21(4) 0.20(4) 0.20(4) -0.004(14) 0.009(14) -0.001(14) C26' 0.09(2) 0.08(2) 0.09(2) -0.003(13) 0.000(13) 0.010(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U K 3.681(5) . ? U O1 2.244(8) . ? U O2 2.276(8) . ? U O7 1.773(7) . ? U O8 1.781(7) . ? U N1 2.536(10) . ? U N3 2.610(10) . ? U N2 2.547(11) . ? K O1 2.604(9) . ? K O6 2.468(9) . ? K O5 2.410(10) . ? K O4 2.762(11) . ? K O3 2.558(12) . ? K O2 2.454(11) . ? K C9 3.316(16) . ? K C8' 3.10(4) . ? K C9' 3.316(16) . ? K C13 3.308(17) . ? K O11 2.41(2) . ? K O11' 2.25(2) . ? O1 C7 1.310(14) . ? O6 C6 1.373(15) . ? O6 C8 1.41(2) . ? O6 C8' 1.42(3) . ? O5 C9 1.353(18) . ? O5 C9' 1.353(18) . ? O5 C10 1.473(17) . ? O4 C11 1.40(2) . ? O4 C12 1.48(2) . ? O3 C13 1.458(17) . ? O3 C14 1.353(15) . ? O2 C19 1.320(15) . ? N1 C1 1.283(17) . ? N1 C24 1.453(18) . ? N3 C22 1.409(18) . ? N3 C25 1.50(2) . ? N3 C23 1.505(19) . ? N2 C20 1.298(17) . ? N2 C21 1.447(17) . ? C1 H1 0.9500 . ? C1 C2 1.46(2) . ? C2 C3 1.409(19) . ? C2 C7 1.374(18) . ? C3 H3 0.9500 . ? C3 C4 1.39(2) . ? C4 H4 0.9500 . ? C4 C5 1.36(2) . ? C5 H5 0.9500 . ? C5 C6 1.402(18) . ? C7 C6 1.421(18) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C9 1.55(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C8' H8'A 0.9607 . ? C8' H8'B 0.9596 . ? C8' C9' 1.44(4) . ? C9' H9'A 0.9900 . ? C9' H9'B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.57(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 C13 1.43(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.405(19) . ? C14 C19 1.417(18) . ? C15 H15 0.9500 . ? C15 C16 1.41(2) . ? C16 H16 0.9500 . ? C16 C17 1.42(2) . ? C17 H17 0.9500 . ? C17 C18 1.385(18) . ? C18 C19 1.387(18) . ? C18 C20 1.42(2) . ? C20 H20 0.9500 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 C22 1.53(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.48(2) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? S1 O11 1.413(12) . ? S1 O12 1.427(12) . ? S1 O13 1.409(12) . ? S1 C26 1.792(12) . ? F11 C26 1.307(12) . ? F12 C26 1.303(12) . ? F13 C26 1.307(12) . ? S1' O11' 1.410(13) . ? S1' O12' 1.415(14) . ? S1' O13' 1.410(13) . ? S1' C26' 1.799(14) . ? F11' C26' 1.309(14) . ? F12' C26' 1.307(14) . ? F13' C26' 1.304(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U K 44.4(2) . . ? O1 U O2 83.0(3) . . ? O1 U N1 72.1(3) . . ? O1 U N3 137.9(3) . . ? O1 U N2 155.0(3) . . ? O2 U K 40.7(2) . . ? O2 U N1 153.7(3) . . ? O2 U N3 138.8(3) . . ? O2 U N2 72.1(3) . . ? O7 U K 80.6(2) . . ? O7 U O1 89.6(3) . . ? O7 U O2 91.8(4) . . ? O7 U O8 175.3(3) . . ? O7 U N1 96.2(4) . . ? O7 U N3 84.9(3) . . ? O7 U N2 92.1(4) . . ? O8 U K 104.0(3) . . ? O8 U O1 93.2(3) . . ? O8 U O2 92.3(4) . . ? O8 U N1 81.0(4) . . ? O8 U N3 90.5(3) . . ? O8 U N2 87.0(4) . . ? N1 U K 116.3(3) . . ? N1 U N3 67.1(3) . . ? N1 U N2 132.3(4) . . ? N3 U K 165.4(3) . . ? N2 U K 111.4(3) . . ? N2 U N3 67.0(3) . . ? O1 K O4 166.4(4) . . ? O1 K C9 106.1(3) . . ? O1 K C8' 80.7(7) . . ? O1 K C9' 106.1(3) . . ? O1 K C13 125.6(4) . . ? O6 K O1 63.3(3) . . ? O6 K O4 122.8(4) . . ? O6 K O3 97.7(4) . . ? O6 K C9 46.3(4) . . ? O6 K C8' 26.6(7) . . ? O6 K C9' 46.3(4) . . ? O6 K C13 93.0(4) . . ? O5 K O1 126.5(4) . . ? O5 K O6 66.1(3) . . ? O5 K O4 64.4(4) . . ? O5 K O3 96.4(5) . . ? O5 K O2 157.0(5) . . ? O5 K C9 20.5(4) . . ? O5 K C8' 45.7(7) . . ? O5 K C9' 20.5(4) . . ? O5 K C13 72.3(5) . . ? O5 K O11 93.1(7) . . ? O4 K C9 84.1(4) . . ? O4 K C8' 109.7(8) . . ? O4 K C9' 84.1(4) . . ? O4 K C13 45.9(4) . . ? O3 K O1 106.2(3) . . ? O3 K O4 62.1(4) . . ? O3 K C9 102.7(4) . . ? O3 K C8' 113.4(10) . . ? O3 K C9' 102.7(4) . . ? O3 K C13 24.8(4) . . ? O2 K O1 72.5(3) . . ? O2 K O6 124.2(3) . . ? O2 K O4 95.1(3) . . ? O2 K O3 63.2(3) . . ? O2 K C9 163.7(4) . . ? O2 K C8' 150.0(7) . . ? O2 K C9' 163.7(4) . . ? O2 K C13 86.0(4) . . ? C8' K C9' 25.6(7) . . ? C8' K C13 99.0(10) . . ? C13 K C9 81.8(4) . . ? C13 K C9' 81.8(4) . . ? O11 K O1 86.6(7) . . ? O11 K O6 107.7(7) . . ? O11 K O4 101.7(7) . . ? O11 K O3 154.5(7) . . ? O11 K O2 101.6(6) . . ? O11 K C9 94.5(7) . . ? O11 K C13 147.5(8) . . ? O11' K O1 90.8(5) . . ? O11' K O6 109.9(7) . . ? O11' K O5 90.8(7) . . ? O11' K O4 97.5(6) . . ? O11' K O3 152.0(7) . . ? O11' K O2 102.8(7) . . ? O11' K C8' 90.9(11) . . ? O11' K C9' 93.5(7) . . ? O11' K C13 143.3(6) . . ? U O1 K 98.5(3) . . ? C7 O1 U 133.5(8) . . ? C7 O1 K 118.1(8) . . ? C6 O6 K 122.1(7) . . ? C6 O6 C8 118.0(13) . . ? C6 O6 C8' 119.8(16) . . ? C8 O6 K 119.9(11) . . ? C8' O6 K 102.4(18) . . ? C9 O5 K 121.0(8) . . ? C9 O5 C10 113.3(11) . . ? C9' O5 K 121.0(8) . . ? C9' O5 C10 113.3(11) . . ? C10 O5 K 124.6(10) . . ? C11 O4 K 105.0(10) . . ? C11 O4 C12 116.7(14) . . ? C12 O4 K 112.1(9) . . ? C13 O3 K 107.7(9) . . ? C14 O3 K 116.1(9) . . ? C14 O3 C13 118.3(10) . . ? U O2 K 102.1(3) . . ? C19 O2 U 127.4(8) . . ? C19 O2 K 121.8(9) . . ? C1 N1 U 125.1(9) . . ? C1 N1 C24 116.2(11) . . ? C24 N1 U 117.6(9) . . ? C22 N3 U 110.7(9) . . ? C22 N3 C25 108.0(15) . . ? C22 N3 C23 112.9(12) . . ? C25 N3 U 112.0(9) . . ? C25 N3 C23 105.7(15) . . ? C23 N3 U 107.6(9) . . ? C20 N2 U 126.7(9) . . ? C20 N2 C21 116.2(12) . . ? C21 N2 U 116.9(9) . . ? N1 C1 H1 116.2 . . ? N1 C1 C2 127.7(11) . . ? C2 C1 H1 116.2 . . ? C3 C2 C1 115.0(13) . . ? C7 C2 C1 122.6(12) . . ? C7 C2 C3 122.2(14) . . ? C2 C3 H3 120.8 . . ? C4 C3 C2 118.3(13) . . ? C4 C3 H3 120.8 . . ? C3 C4 H4 119.2 . . ? C5 C4 C3 121.6(13) . . ? C5 C4 H4 119.2 . . ? C4 C5 H5 120.4 . . ? C4 C5 C6 119.3(14) . . ? C6 C5 H5 120.4 . . ? O1 C7 K 42.2(6) . . ? O1 C7 C2 123.7(12) . . ? O1 C7 C6 119.2(11) . . ? C2 C7 K 165.4(9) . . ? C2 C7 C6 117.1(11) . . ? C6 C7 K 77.2(7) . . ? O6 C6 K 37.9(5) . . ? O6 C6 C5 122.9(12) . . ? O6 C6 C7 116.0(10) . . ? C5 C6 K 158.9(10) . . ? C5 C6 C7 121.1(12) . . ? C7 C6 K 78.7(7) . . ? K C8 H8A 139.9 . . ? K C8 H8B 107.3 . . ? O6 C8 K 39.1(8) . . ? O6 C8 H8A 109.9 . . ? O6 C8 H8B 109.9 . . ? O6 C8 C9 109(2) . . ? H8A C8 H8B 108.3 . . ? C9 C8 K 73.8(11) . . ? C9 C8 H8A 109.9 . . ? C9 C8 H8B 109.9 . . ? K C9 H9A 141.6 . . ? K C9 H9B 104.0 . . ? O5 C9 K 38.5(6) . . ? O5 C9 C8 112.7(14) . . ? O5 C9 H9A 109.1 . . ? O5 C9 H9B 109.1 . . ? C8 C9 K 79.5(10) . . ? C8 C9 H9A 109.1 . . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? K C8' H8'A 81.8 . . ? K C8' H8'B 159.8 . . ? O6 C8' K 51.0(14) . . ? O6 C8' H8'A 109.8 . . ? O6 C8' H8'B 108.8 . . ? O6 C8' C9' 114(3) . . ? H8'A C8' H8'B 108.1 . . ? C9' C8' K 85.5(17) . . ? C9' C8' H8'A 108.4 . . ? C9' C8' H8'B 107.0 . . ? K C9' H9'A 116.9 . . ? K C9' H9'B 131.5 . . ? O5 C9' K 38.5(6) . . ? O5 C9' C8' 107(2) . . ? O5 C9' H9'A 110.4 . . ? O5 C9' H9'B 110.4 . . ? C8' C9' K 68.9(17) . . ? C8' C9' H9'A 110.4 . . ? C8' C9' H9'B 110.4 . . ? H9'A C9' H9'B 108.6 . . ? K C10 H10A 135.8 . . ? K C10 H10B 110.3 . . ? O5 C10 K 34.9(6) . . ? O5 C10 H10A 110.4 . . ? O5 C10 H10B 110.4 . . ? O5 C10 C11 106.7(13) . . ? H10A C10 H10B 108.6 . . ? C11 C10 K 74.5(9) . . ? C11 C10 H10A 110.4 . . ? C11 C10 H10B 110.4 . . ? K C11 H11A 161.5 . . ? K C11 H11B 82.5 . . ? O4 C11 K 51.7(8) . . ? O4 C11 C10 109.1(16) . . ? O4 C11 H11A 109.9 . . ? O4 C11 H11B 109.9 . . ? C10 C11 K 79.1(9) . . ? C10 C11 H11A 109.9 . . ? C10 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? O4 C12 H12A 109.2 . . ? O4 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C13 C12 O4 112.0(13) . . ? C13 C12 H12A 109.2 . . ? C13 C12 H12B 109.2 . . ? K C13 H13A 155.5 . . ? K C13 H13B 78.1 . . ? O3 C13 K 47.5(7) . . ? O3 C13 H13A 109.6 . . ? O3 C13 H13B 109.6 . . ? C12 C13 K 89.4(11) . . ? C12 C13 O3 110.3(12) . . ? C12 C13 H13A 109.6 . . ? C12 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? O3 C14 K 42.8(6) . . ? O3 C14 C15 123.0(13) . . ? O3 C14 C19 116.4(11) . . ? C15 C14 K 159.8(10) . . ? C15 C14 C19 120.5(12) . . ? C19 C14 K 76.4(7) . . ? C14 C15 H15 120.4 . . ? C14 C15 C16 119.2(15) . . ? C16 C15 H15 120.4 . . ? C15 C16 H16 119.9 . . ? C15 C16 C17 120.2(14) . . ? C17 C16 H16 119.9 . . ? C16 C17 H17 120.6 . . ? C18 C17 C16 118.8(14) . . ? C18 C17 H17 120.6 . . ? C17 C18 C19 122.4(14) . . ? C17 C18 C20 114.8(13) . . ? C19 C18 C20 122.8(12) . . ? O2 C19 K 38.6(6) . . ? O2 C19 C14 117.2(12) . . ? O2 C19 C18 124.0(13) . . ? C14 C19 K 79.3(8) . . ? C18 C19 K 159.3(10) . . ? C18 C19 C14 118.6(11) . . ? N2 C20 C18 126.3(12) . . ? N2 C20 H20 116.8 . . ? C18 C20 H20 116.8 . . ? N2 C21 H21A 110.1 . . ? N2 C21 H21B 110.1 . . ? N2 C21 C22 108.2(12) . . ? H21A C21 H21B 108.4 . . ? C22 C21 H21A 110.1 . . ? C22 C21 H21B 110.1 . . ? N3 C22 C21 114.6(14) . . ? N3 C22 H22A 108.6 . . ? N3 C22 H22B 108.6 . . ? C21 C22 H22A 108.6 . . ? C21 C22 H22B 108.6 . . ? H22A C22 H22B 107.6 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N3 C23 H23A 109.5 . . ? N3 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? C24 C23 N3 110.8(13) . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? N1 C24 C23 109.5(12) . . ? N1 C24 H24A 109.8 . . ? N1 C24 H24B 109.8 . . ? C23 C24 H24A 109.8 . . ? C23 C24 H24B 109.8 . . ? H24A C24 H24B 108.2 . . ? O11 S1 K 20.2(12) . . ? O11 S1 O12 112.5(14) . . ? O11 S1 C26 103.4(11) . . ? O12 S1 K 131.0(9) . . ? O12 S1 C26 100.5(11) . . ? O13 S1 K 101.3(10) . . ? O13 S1 O11 120.2(14) . . ? O13 S1 O12 112.6(14) . . ? O13 S1 C26 104.6(11) . . ? C26 S1 K 104.0(6) . . ? S1 O11 K 148.1(19) . . ? F11 C26 S1 113.2(12) . . ? F11 C26 F13 106.6(15) . . ? F12 C26 S1 112.1(12) . . ? F12 C26 F11 106.3(13) . . ? F12 C26 F13 107.6(17) . . ? F13 C26 S1 110.6(11) . . ? O11' S1' K 5.2(10) . . ? O11' S1' O12' 116.4(17) . . ? O11' S1' O13' 115.5(16) . . ? O11' S1' C26' 103.7(12) . . ? O12' S1' K 113.9(17) . . ? O12' S1' C26' 103.2(16) . . ? O13' S1' K 120.4(16) . . ? O13' S1' O12' 113.3(18) . . ? O13' S1' C26' 102.2(15) . . ? C26' S1' K 100.3(11) . . ? S1' O11' K 171.5(17) . . ? F11' C26' S1' 112.3(17) . . ? F12' C26' S1' 112.0(17) . . ? F12' C26' F11' 105.1(19) . . ? F13' C26' S1' 112.1(18) . . ? F13' C26' F11' 108(2) . . ? F13' C26' F12' 107(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C11 H11B F12' 0.99 2.34 3.33(6) 174.1 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag U O1 C7 K -137.5(12) . . . . ? U O1 C7 C2 37.8(17) . . . . ? U O1 C7 C6 -144.6(9) . . . . ? U O2 C19 K 141.7(12) . . . . ? U O2 C19 C14 130.3(10) . . . . ? U O2 C19 C18 -53.9(15) . . . . ? U N1 C1 C2 -9.0(19) . . . . ? U N1 C24 C23 -32.4(17) . . . . ? U N3 C22 C21 45.0(18) . . . . ? U N3 C23 C24 -53.4(16) . . . . ? U N2 C20 C18 -3.6(19) . . . . ? U N2 C21 C22 35.8(16) . . . . ? K O1 C7 C2 175.3(9) . . . . ? K O1 C7 C6 -7.1(14) . . . . ? K O6 C6 C5 -167.8(10) . . . . ? K O6 C6 C7 11.7(15) . . . . ? K O6 C8 C9 -27(4) . . . . ? K O6 C8' C9' 61(4) . . . . ? K O5 C9 C8 -33(3) . . . . ? K O5 C9' C8' 12(3) . . . . ? K O5 C10 C11 -23(2) . . . . ? K O4 C11 C10 -58.0(16) . . . . ? K O4 C12 C13 8.2(16) . . . . ? K O3 C13 C12 69.3(15) . . . . ? K O3 C14 C15 -161.1(11) . . . . ? K O3 C14 C19 23.0(13) . . . . ? K O2 C19 C14 -11.3(14) . . . . ? K O2 C19 C18 164.4(9) . . . . ? K C7 C6 O6 -7.3(9) . . . . ? K C7 C6 C5 172.2(13) . . . . ? K C8 C9 O5 19.9(15) . . . . ? K C8' C9' O5 -8.0(17) . . . . ? K C10 C11 O4 42.7(12) . . . . ? K C14 C15 C16 143(2) . . . . ? K C14 C19 O2 7.2(9) . . . . ? K C14 C19 C18 -168.9(10) . . . . ? K S1 C26 F11 -160.8(13) . . . . ? K S1 C26 F12 -40.5(15) . . . . ? K S1 C26 F13 79.7(15) . . . . ? K S1' C26' F11' 172(3) . . . . ? K S1' C26' F12' -70(3) . . . . ? K S1' C26' F13' 50(3) . . . . ? O1 C7 C6 K 4.9(9) . . . . ? O1 C7 C6 O6 -2.4(17) . . . . ? O1 C7 C6 C5 177.1(12) . . . . ? O6 C8 C9 K 18(2) . . . . ? O6 C8 C9 O5 37(4) . . . . ? O6 C8' C9' K -43(3) . . . . ? O6 C8' C9' O5 -51(4) . . . . ? O5 C10 C11 K 13.7(12) . . . . ? O5 C10 C11 O4 56(2) . . . . ? O4 C12 C13 K -6.4(12) . . . . ? O4 C12 C13 O3 -49.9(19) . . . . ? O3 C14 C15 C16 -176.9(13) . . . . ? O3 C14 C19 K -15.8(10) . . . . ? O3 C14 C19 O2 -8.7(16) . . . . ? O3 C14 C19 C18 175.3(11) . . . . ? N1 C1 C2 C3 169.8(13) . . . . ? N1 C1 C2 C7 -16(2) . . . . ? N3 C23 C24 N1 58.0(19) . . . . ? N2 C21 C22 N3 -55(2) . . . . ? C1 N1 C24 C23 135.8(14) . . . . ? C1 C2 C3 C4 178.5(13) . . . . ? C1 C2 C7 K 17(4) . . . . ? C1 C2 C7 O1 4.6(19) . . . . ? C1 C2 C7 C6 -173.1(12) . . . . ? C2 C3 C4 C5 -5(2) . . . . ? C2 C7 C6 K -177.4(11) . . . . ? C2 C7 C6 O6 175.3(11) . . . . ? C2 C7 C6 C5 -5.2(18) . . . . ? C3 C2 C7 K -169(3) . . . . ? C3 C2 C7 O1 178.6(12) . . . . ? C3 C2 C7 C6 1.0(18) . . . . ? C3 C4 C5 C6 1(2) . . . . ? C4 C5 C6 K 163(2) . . . . ? C4 C5 C6 O6 -176.2(13) . . . . ? C4 C5 C6 C7 4(2) . . . . ? C7 C2 C3 C4 4(2) . . . . ? C6 O6 C8 K -178(3) . . . . ? C6 O6 C8 C9 155.1(17) . . . . ? C6 O6 C8' K 139(2) . . . . ? C6 O6 C8' C9' -160(2) . . . . ? C8 O6 C6 K 178(3) . . . . ? C8 O6 C6 C5 10(3) . . . . ? C8 O6 C6 C7 -171(3) . . . . ? C9 O5 C10 K -168(2) . . . . ? C9 O5 C10 C11 168.1(16) . . . . ? C8' O6 C6 K -131(3) . . . . ? C8' O6 C6 C5 62(3) . . . . ? C8' O6 C6 C7 -119(3) . . . . ? C9' O5 C10 K -168(2) . . . . ? C9' O5 C10 C11 168.1(16) . . . . ? C10 O5 C9 K 169(2) . . . . ? C10 O5 C9 C8 136(2) . . . . ? C10 O5 C9' K 169(2) . . . . ? C10 O5 C9' C8' -179(2) . . . . ? C11 O4 C12 C13 -112.8(16) . . . . ? C12 O4 C11 K 124.8(14) . . . . ? C12 O4 C11 C10 66.7(18) . . . . ? C13 O3 C14 K 130.4(15) . . . . ? C13 O3 C14 C15 -31(2) . . . . ? C13 O3 C14 C19 153.4(13) . . . . ? C14 O3 C13 K -134.2(14) . . . . ? C14 O3 C13 C12 -65(2) . . . . ? C14 C15 C16 C17 0(2) . . . . ? C15 C14 C19 K 168.2(13) . . . . ? C15 C14 C19 O2 175.3(12) . . . . ? C15 C14 C19 C18 -0.7(18) . . . . ? C15 C16 C17 C18 4(2) . . . . ? C16 C17 C18 C19 -5.7(19) . . . . ? C16 C17 C18 C20 174.0(12) . . . . ? C17 C18 C19 K -143.2(19) . . . . ? C17 C18 C19 O2 -171.5(12) . . . . ? C17 C18 C19 C14 4.2(17) . . . . ? C17 C18 C20 N2 -160.8(13) . . . . ? C19 C14 C15 C16 -1(2) . . . . ? C19 C18 C20 N2 19(2) . . . . ? C20 N2 C21 C22 -140.2(14) . . . . ? C20 C18 C19 K 37(3) . . . . ? C20 C18 C19 O2 8.8(18) . . . . ? C20 C18 C19 C14 -175.5(12) . . . . ? C21 N2 C20 C18 172.0(13) . . . . ? C22 N3 C23 C24 -175.9(16) . . . . ? C25 N3 C22 C21 -77.8(18) . . . . ? C25 N3 C23 C24 66.4(18) . . . . ? C23 N3 C22 C21 165.7(16) . . . . ? C24 N1 C1 C2 -176.2(13) . . . . ? O11 S1 C26 F11 178.4(18) . . . . ? O11 S1 C26 F12 -61.3(19) . . . . ? O11 S1 C26 F13 59(2) . . . . ? O12 S1 O11 K -158(3) . . . . ? O12 S1 C26 F11 62.0(18) . . . . ? O12 S1 C26 F12 -177.8(18) . . . . ? O12 S1 C26 F13 -57.6(19) . . . . ? O13 S1 O11 K -22(3) . . . . ? O13 S1 C26 F11 -54.9(17) . . . . ? O13 S1 C26 F12 65.4(18) . . . . ? O13 S1 C26 F13 -174.5(16) . . . . ? C26 S1 O11 K 94(3) . . . . ? O11' S1' C26' F11' 176(3) . . . . ? O11' S1' C26' F12' -66(3) . . . . ? O11' S1' C26' F13' 54(3) . . . . ? O12' S1' C26' F11' 54(3) . . . . ? O12' S1' C26' F12' 172(3) . . . . ? O12' S1' C26' F13' -68(4) . . . . ? O13' S1' C26' F11' -64(3) . . . . ? O13' S1' C26' F12' 54(3) . . . . ? O13' S1' C26' F13' 175(3) . . . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma -1 0 0 -0.65 0.03 -2 0 0 483.58 23.43 -3 0 0 -0.43 0.1 -5 0 0 -0.08 0.12 6 0 0 411.33 20.47 6 0 0 424.7 20.48 -6 0 0 430.49 20.65 7 0 0 0.04 0.09 7 0 0 0.42 0.11 -7 0 0 0.2 0.21 -8 0 0 221.81 11.27 8 0 0 227.93 11 8 0 0 226.57 11.01 9 0 0 -0.07 0.11 9 0 0 0.17 0.13 10 0 0 84.53 4.31 10 0 0 87.94 4.31 11 0 0 0.11 0.18 11 0 0 0.09 0.17 12 0 0 48.67 2.56 13 0 0 0.13 0.18 14 0 0 31.33 1.72 15 0 0 0.1 0.17 -1 -1 0 6.03 0.32 -1 1 0 4.98 0.32 -2 -1 0 -0.17 0.06 -2 1 0 -0.13 0.07 -3 1 0 -0.05 0.09 -3 -1 0 -0.12 0.08 -4 1 0 1.59 0.24 -4 -1 0 1.53 0.22 -5 1 0 41.21 2.24 -5 -1 0 43.1 2.23 6 1 0 0.1 0.08 -6 -1 0 0.09 0.16 6 1 0 0.01 0.08 6 -1 0 0.04 0.08 6 -1 0 -0.13 0.11 -6 1 0 0.1 0.21 -7 1 0 15.26 1.06 7 -1 0 14.4 0.82 7 -1 0 14.32 0.84 -7 -1 0 15.14 1 7 1 0 14.71 0.8 7 1 0 15.53 0.81 8 1 0 7.88 0.49 -8 -1 0 7.35 0.69 8 -1 0 8.03 0.51 -8 1 0 7.92 0.77 8 -1 0 8.01 0.52 8 1 0 7.49 0.48 9 -1 0 4.7 0.39 9 1 0 4.52 0.36 9 1 0 4.64 0.35 9 -1 0 4.79 0.41 10 1 0 2.61 0.3 10 -1 0 2.52 0.34 10 1 0 2.52 0.29 10 -1 0 2.5 0.32 11 -1 0 1.85 0.29 11 -1 0 1.57 0.29 11 1 0 1.61 0.26 12 -1 0 0.73 0.25 12 1 0 0.81 0.23 13 1 0 0 0.18 13 -1 0 0.34 0.21 14 1 0 1.89 0.31 14 -1 0 2.78 0.35 15 -1 0 0.12 0.2 15 1 0 0.2 0.2 0 -2 0 320.79 15.57 -1 2 0 630.42 31.16 -1 -2 0 656.5 31.15 -2 -2 0 180.57 8.77 -2 2 0 179.24 8.79 -3 -2 0 214.35 10.31 -3 2 0 208.05 10.34 -4 2 0 148.81 7.53 -4 -2 0 155.39 7.49 5 -2 0 228.46 11.35 -5 2 0 231.88 11.47 -5 -2 0 237.55 11.43 -6 -2 0 136.49 6.74 6 -2 0 141.42 6.64 -6 2 0 134 6.8 6 2 0 137.97 6.57 6 2 0 132.9 6.57 6 -2 0 125.72 6.6 7 -2 0 95.49 4.58 -7 -2 0 92.91 4.72 7 2 0 91.09 4.5 -7 2 0 91.94 4.8 7 -2 0 86.18 4.53 7 2 0 92.78 4.51 8 -2 0 144.68 6.87 -8 -2 0 134.21 7.07 8 -2 0 146.21 6.91 -8 2 0 131.24 7.16 8 2 0 134.44 6.81 8 2 0 145.04 6.83 9 -2 0 31.42 1.68 9 -2 0 30.19 1.64 9 2 0 30.4 1.6 10 2 0 68.06 3.6 10 -2 0 74.21 3.69 10 -2 0 73.6 3.66 11 -2 0 32.71 1.79 11 2 0 30.61 1.7 11 -2 0 29.44 1.98 11 -2 0 32.86 1.76 11 -2 0 33.41 1.84 11 2 0 32.72 1.78 12 -2 0 46.78 2.51 12 2 0 47.62 2.48 13 -2 0 14.05 0.94 14 2 0 28.66 1.51 14 -2 0 25.54 1.52 15 2 0 8.38 0.61 15 -2 0 8.41 0.64 0 -3 0 0 0.08 -1 -3 0 4.3 0.31 -2 3 0 0.33 0.12 -2 -3 0 0.48 0.1 -3 3 0 28.16 1.54 -3 -3 0 29.13 1.49 -4 3 0 15.74 0.97 -4 -3 0 15.79 0.9 5 3 0 16.86 0.93 -5 -3 0 18.12 1.05 5 -3 0 18.24 1.02 -5 3 0 18.36 0.98 -5 3 0 18.54 1.13 6 3 0 34.09 1.68 6 -3 0 35.62 1.78 6 -3 0 30.38 1.71 -6 3 0 31.81 1.73 6 3 0 33.82 1.68 -6 -3 0 33.53 1.84 -6 3 0 34.04 1.94 7 -3 0 4.77 0.38 7 -3 0 4.73 0.44 -7 3 0 5.18 0.63 -7 -3 0 4.7 0.52 7 3 0 5.06 0.34 -8 -3 0 1.06 0.48 8 3 0 1.22 0.18 8 -3 0 0.95 0.25 8 -3 0 1 0.21 9 -3 0 4.6 0.49 9 3 0 4.27 0.35 9 -3 0 4.39 0.46 10 3 0 5.63 0.44 10 -3 0 5.32 0.64 10 -3 0 5.74 0.56 11 -3 0 0.45 0.26 11 -3 0 0.19 0.34 11 -3 0 0.53 0.27 11 -3 0 0.29 0.45 11 3 0 0.47 0.3 11 3 0 0.17 0.19 12 3 0 1.17 0.25 12 -3 0 1.54 0.46 12 -3 0 1.15 0.29 13 -3 0 1.48 0.41 13 3 0 1.29 0.27 13 -3 0 1.51 0.33 14 3 0 0.05 0.22 14 -3 0 0.69 0.26 15 3 0 0.84 0.25 15 -3 0 0.15 0.28 -1 4 0 236.46 11.52 -2 4 0 171.65 8.42 -3 -4 0 266.71 13.51 -3 4 0 281.37 13.42 -4 4 0 51.39 2.65 4 -4 0 49.64 2.59 -4 4 0 48.7 2.5 -4 4 0 50.06 2.54 -4 -4 0 50.91 2.64 5 -4 0 132.85 6.78 -5 4 0 136.77 6.74 -5 4 0 145.77 6.9 5 4 0 131.26 6.66 6 4 0 7.52 0.45 6 -4 0 7.81 0.61 -6 4 0 7.9 0.72 -6 4 0 7.5 0.53 7 -4 0 143.82 6.92 -7 4 0 135.9 7.08 7 -4 0 136.23 6.83 7 4 0 136.43 6.76 -7 4 0 138.65 6.85 8 -4 0 21.03 1.29 8 4 0 21.15 1.13 8 -4 0 20.77 1.21 9 -4 0 47.84 2.42 9 -4 0 44.27 2.48 9 4 0 43.82 2.31 10 -4 0 7.65 0.89 10 -4 0 8.7 0.76 10 -4 0 9.65 0.84 11 4 0 63.95 3.45 11 -4 0 67.92 3.55 11 4 0 69.46 3.46 11 -4 0 67.21 3.61 11 -4 0 71.45 3.54 11 -4 0 64.69 3.66 12 4 0 1.81 0.35 12 4 0 2.61 0.39 12 -4 0 2.13 0.47 12 -4 0 1.79 0.36 13 -4 0 27.95 1.73 13 4 0 27.83 1.53 13 -4 0 26.31 1.59 13 4 0 25.42 1.52 14 4 0 2.82 0.42 14 -4 0 2.56 0.4 14 -4 0 2.31 0.48 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6 0 276.6 12.56 -4 6 0 0.66 0.18 4 6 0 0.42 0.14 -4 6 0 0.56 0.2 5 6 0 154 7.74 -5 6 0 162.11 7.81 6 6 0 3.78 0.34 -6 6 0 4.02 0.44 6 -6 0 3.16 0.49 7 -6 0 91.31 4.77 7 6 0 92.25 4.54 -7 6 0 90.27 4.65 8 -6 0 8.79 0.9 8 -6 0 6.54 0.73 8 6 0 5.93 0.49 -8 6 0 6.52 0.72 9 -6 0 59 3.39 -9 6 0 67.67 3.47 9 -6 0 67.8 3.6 9 -6 0 63.21 3.46 10 -6 0 10.03 1 10 6 0 7.32 0.81 10 -6 0 9.47 1.08 10 6 0 8.14 0.69 10 -6 0 6.92 0.82 10 6 0 8 0.62 11 6 0 53.27 2.72 11 6 0 50.51 2.82 11 6 0 49.49 2.62 11 -6 0 49.79 2.79 11 -6 0 51.82 2.84 12 6 0 3.35 0.44 12 -6 0 2.98 0.52 12 -6 0 3.27 0.46 12 6 0 2.67 0.47 12 6 0 3.49 0.53 13 6 0 24.16 1.5 13 -6 0 22.34 1.59 13 -6 0 27.69 1.52 13 6 0 25.91 1.39 14 -6 0 0.01 0.39 14 6 0 0.6 0.31 14 -6 0 0.61 0.28 14 6 0 0.55 0.2 0 7 0 -0.02 0.1 0 7 0 0 0.1 -1 7 0 1.47 0.18 1 7 0 1.73 0.21 1 7 0 1.58 0.2 -1 7 0 1.66 0.21 -2 7 0 3.98 0.33 -2 7 0 4.44 0.39 2 7 0 4.67 0.34 -3 7 0 1.37 0.2 -3 7 0 0.93 0.23 3 7 0 1.31 0.21 4 7 0 5.32 0.48 -4 7 0 5.23 0.44 -4 7 0 6.73 0.62 -5 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127.37 6.55 6 3 4 135.91 6.52 6 3 4 138.42 6.52 7 -3 4 60.94 2.96 7 -3 4 58.4 3 -7 -3 -4 55.55 3.19 -7 3 4 59.49 3.41 -7 3 -4 56.41 2.95 7 -3 -4 61.08 3.07 7 3 4 61.41 2.92 7 3 4 54.41 2.91 8 -3 4 53.8 2.75 8 -3 4 53.17 2.7 8 -3 -4 55.75 2.81 8 3 4 53.61 2.66 8 3 4 49 2.64 -8 3 -4 51 2.7 9 -3 4 40.19 2.13 9 -3 4 37.89 2.08 9 3 4 39.95 2.03 9 3 4 37.31 2.01 9 -3 -4 40.99 2.19 10 -3 4 40.2 2.14 10 -3 4 36.34 2.19 10 -3 4 39.64 2.1 10 3 4 39.79 2.04 10 3 4 38.47 2.01 10 -3 -4 38.62 2.18 11 -3 4 19.91 1.61 11 3 -4 24 1.44 11 -3 4 22.67 1.55 11 3 -4 22.89 1.33 11 -3 4 24.04 1.43 11 3 -4 24.45 1.37 11 -3 -4 24.99 1.45 11 -3 -4 24.21 1.84 11 -3 -4 25.77 1.63 11 3 4 23.54 1.34 12 -3 4 36.03 2.12 12 3 -4 36.44 1.96 12 3 -4 37.47 2.05 12 3 -4 35.28 1.97 12 -3 -4 36.91 2.05 12 -3 -4 38.19 2.55 13 3 -4 13.8 0.96 13 -3 4 13.36 1.03 13 3 -4 13.07 0.86 13 3 -4 13.94 0.91 13 -3 -4 14.55 0.96 14 3 -4 14.15 0.9 14 3 -4 13.13 1.02 14 3 -4 14.69 0.92 14 -3 -4 15.64 0.97 15 3 -4 6.44 0.58 15 -3 -4 6.91 0.7 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7.68 0.69 10 4 4 8.08 0.6 10 -4 -4 7.69 0.92 11 4 -4 1.92 0.34 11 4 -4 1.68 0.28 11 -4 4 2.48 0.47 11 4 -4 1.93 0.29 11 -4 -4 2.07 0.4 11 4 4 3.02 0.56 11 -4 -4 1.49 0.44 12 -4 4 1.66 0.41 12 4 -4 1.79 0.29 12 4 -4 1.7 0.27 12 4 -4 1.77 0.35 12 -4 -4 1.53 0.37 12 -4 -4 1.45 0.52 13 4 -4 1.45 0.34 13 4 -4 1.22 0.28 13 4 -4 1.43 0.3 13 -4 4 1.71 0.43 13 -4 -4 1.76 0.37 13 -4 -4 0.91 0.46 14 4 -4 1.3 0.33 14 4 -4 1.23 0.27 14 4 -4 1.24 0.24 14 -4 -4 1.09 0.43 14 -4 -4 0.6 0.29 0 5 4 153.9 7.09 0 5 4 135.08 7.09 0 -5 -4 145.14 7.26 -1 -5 -4 4.46 0.51 -1 5 4 3.86 0.33 -1 5 4 3.67 0.34 1 5 4 4.25 0.36 1 -5 -4 4.02 0.46 1 5 4 4.05 0.31 -2 5 4 250.03 12.9 -2 -5 -4 286.97 13.2 -2 5 4 254.94 12.83 2 5 4 260.62 12.83 2 5 4 268.22 12.81 -2 5 -4 256.06 12.8 2 -5 -4 266.91 12.9 -3 5 4 7.95 0.64 -3 5 4 7.55 0.52 -3 -5 -4 6.7 0.73 -3 5 -4 7.63 0.47 3 5 4 7.42 0.47 3 5 4 8.09 0.46 3 -5 -4 7.86 0.6 -4 5 4 186.28 9.59 -4 5 4 205.29 9.43 -4 -5 -4 173.17 9.6 -4 5 4 200.91 9.44 4 5 4 191.35 9.34 -4 5 -4 187.07 9.38 4 -5 -4 193.66 9.52 4 5 4 197.09 9.36 -5 5 4 1.92 0.26 -5 5 4 1.38 0.27 -5 5 4 1.53 0.38 -5 -5 -4 1.86 0.44 -5 5 -4 1.73 0.23 5 5 4 1.72 0.21 5 -5 -4 1.57 0.39 5 5 4 2.13 0.2 -6 -5 -4 96.4 5.45 6 -5 4 103.05 5.22 -6 5 4 97.42 5.49 -6 5 -4 107.01 5.21 6 5 4 108.43 5.16 6 -5 -4 117.18 5.49 6 5 4 103.78 5.14 7 -5 4 0.06 0.23 7 -5 -4 0.59 0.43 -7 5 -4 0.23 0.18 7 5 4 0.33 0.12 7 5 4 0.24 0.13 8 -5 4 106.92 5.22 8 -5 4 101.45 5.28 8 -5 -4 101.64 5.23 8 -5 -4 105.91 5.48 -8 5 -4 106.21 5.21 8 5 4 105.73 5.14 8 5 4 96.25 5.18 9 -5 4 0.16 0.38 9 -5 4 0.3 0.3 9 -5 4 0.69 0.35 -9 5 -4 0.3 0.28 9 -5 -4 0.23 0.5 9 5 4 0.48 0.21 10 5 -4 71.56 3.48 10 5 -4 73.02 3.55 10 -5 4 69.31 3.69 10 -5 4 68.51 3.67 10 -5 4 67.83 3.62 10 5 -4 69.03 3.6 10 5 4 69.55 3.52 10 -5 -4 74.59 3.69 -10 5 -4 64.25 3.59 10 -5 -4 63.58 3.86 11 5 -4 0.46 0.19 11 5 -4 0.48 0.24 11 5 -4 0.49 0.25 11 -5 4 0.69 0.29 11 -5 -4 0.6 0.31 11 -5 -4 0.7 0.38 12 5 -4 38.89 2.21 12 5 -4 39.54 2.07 12 -5 4 39.85 2.23 12 5 -4 42.67 2.15 12 -5 -4 37.42 2.3 12 -5 -4 40.36 2.28 13 -5 4 0.42 0.35 13 5 -4 1.07 0.3 13 5 -4 1.02 0.31 13 5 -4 0.72 0.19 13 -5 -4 0.78 0.36 13 -5 -4 0.23 0.41 14 5 -4 19.8 1.23 14 5 -4 20.74 1.27 14 5 -4 20.27 1.1 14 -5 -4 20.04 1.35 14 -5 -4 20.97 1.33 0 6 4 0.33 0.13 0 6 4 0.11 0.12 -1 6 4 34.79 1.81 -1 6 4 38.08 1.82 1 6 4 34.81 1.8 1 6 4 33.79 1.8 -1 6 -4 34.01 1.77 -2 6 4 0.86 0.17 -2 6 4 0.6 0.21 2 6 4 0.85 0.14 2 6 4 0.73 0.2 -2 6 -4 0.7 0.15 -2 6 -4 0.8 0.18 -3 6 4 15.53 0.91 -3 6 4 13.6 1.06 3 6 4 16.34 0.9 -3 6 -4 14.84 0.89 3 6 4 15.74 0.86 3 -6 -4 16.06 1 -3 6 -4 17.39 0.89 -4 6 4 2.09 0.41 -4 6 4 1.9 0.27 4 6 4 2.26 0.25 4 6 4 2.08 0.23 4 -6 -4 1.79 0.36 -4 6 -4 2.06 0.26 -5 6 4 15.75 1.01 -5 6 4 16.1 1.07 5 6 4 16.68 0.91 -5 6 -4 18.4 1 5 6 4 16.62 0.94 5 -6 -4 16.37 1.15 6 -6 4 3.77 0.48 -6 6 4 4.59 0.49 -6 6 -4 3.44 0.43 6 6 4 3.77 0.36 6 -6 -4 3.62 0.58 6 6 4 3.8 0.34 7 -6 4 6.29 0.67 -7 6 -4 6.79 0.57 7 -6 -4 6.57 0.88 7 6 4 5.7 0.48 8 -6 4 0.11 0.3 -8 6 -4 0.53 0.26 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0.27 10 8 -4 0.66 0.17 10 -8 -4 0.64 0.31 10 8 4 0.68 0.33 10 8 4 0.85 0.23 11 8 -4 1.46 0.38 11 8 -4 1.74 0.23 11 -8 4 1.73 0.33 11 8 -4 1.56 0.48 11 8 4 1.84 0.27 11 -8 -4 1.35 0.33 11 -8 -4 0.1 0.61 11 8 4 1.6 0.32 12 8 -4 0.64 0.3 12 8 -4 0.87 0.29 12 8 -4 0.66 0.17 12 -8 4 0.6 0.23 12 -8 -4 0.26 0.44 12 8 4 0.47 0.27 12 -8 -4 0.5 0.24 13 8 -4 0.48 0.21 13 8 -4 0.6 0.25 13 8 -4 0.58 0.11 13 -8 -4 0.49 0.24 0 9 4 17.44 1 0 9 4 17.04 0.98 -1 9 4 113.01 5.51 -1 9 4 114.43 5.51 1 9 4 104.86 5.49 1 9 4 112.2 5.5 -2 9 4 13.14 0.8 -2 9 4 13.06 0.8 2 9 4 12.53 0.75 2 9 4 11.59 0.76 -3 9 4 98.57 4.67 -3 9 4 95.93 4.65 3 9 4 90.73 4.62 -3 9 -4 85.84 4.62 -4 9 4 5.38 0.52 -4 9 4 5.86 0.59 4 9 4 4.75 0.48 -4 9 -4 4.9 0.44 -5 9 4 57.26 2.98 -5 9 4 57.07 2.9 5 9 4 54.6 2.89 -5 9 -4 54.31 2.85 6 9 -4 12.99 1.08 -6 9 4 15.21 0.95 6 9 4 14.14 0.97 -6 9 -4 13.81 0.9 -7 9 4 48.49 2.6 7 9 -4 45.37 2.43 7 9 -4 49.23 2.68 7 9 -4 46.55 2.66 7 -9 4 45.48 2.75 7 9 4 51.05 2.6 7 9 4 51.63 2.61 7 9 4 50.57 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-4 -3 -20 5.21 0.57 4 3 -20 4.69 0.59 4 3 -20 5.68 0.54 5 3 -20 5.29 0.79 -5 -3 -20 3.8 0.51 5 3 -20 4.21 0.44 6 3 -20 4.75 0.4 0 -4 -20 0.91 0.35 0 4 -20 1.3 0.38 0 4 -20 1.31 0.26 1 4 -20 10.58 0.68 -1 -4 -20 11.18 0.82 1 4 -20 10.85 0.81 1 4 -20 10.9 0.72 -1 4 -20 11.01 0.82 2 4 -20 0.94 0.34 2 4 -20 1.39 0.28 -2 -4 -20 0.95 0.3 -2 4 -20 1.14 0.3 3 4 -20 12.47 0.78 -3 -4 -20 12.43 0.85 3 4 -20 11.74 0.82 -4 -4 -20 0.84 0.29 4 4 -20 0.87 0.23 4 4 -20 1.3 0.3 5 4 -20 8.05 0.75 5 4 -20 8.89 0.59 -5 -4 -20 10.46 0.7 0 5 -20 8.33 0.67 0 -5 -20 6.97 0.7 0 5 -20 7.54 0.53 1 5 -20 0.53 0.2 -1 -5 -20 0.48 0.31 1 5 -20 0.42 0.3 -1 5 -20 0.93 0.26 -1 5 -20 0.45 0.23 2 5 -20 10.16 0.74 2 5 -20 9.9 0.65 -2 -5 -20 9.89 0.74 -2 5 -20 9.59 0.69 3 5 -20 0.56 0.23 3 5 -20 0.43 0.18 -3 -5 -20 0.3 0.24 -4 -5 -20 6.42 0.55 4 5 -20 5.98 0.43 4 5 -20 5.26 0.54 0 6 -20 1.61 0.23 0 6 -20 2.89 0.4 -1 -6 -20 8.55 0.65 1 6 -20 8.22 0.54 1 6 -20 9.71 0.67 -1 6 -20 8.71 0.57 -1 6 -20 9.77 0.63 -2 -6 -20 0.7 0.24 2 6 -20 1.15 0.19 2 6 -20 1.87 0.3 3 6 -20 8.06 0.64 3 6 -20 8.41 0.52 -3 -6 -20 9.31 0.63 0 0 -21 -0.41 0.25 -1 0 -21 15.74 0.99 1 0 -21 15.51 1 2 0 -21 0.46 0.3 -2 0 -21 0.71 0.3 3 0 -21 15.35 1.08 -3 0 -21 17.14 1.01 -4 0 -21 -0.12 0.21 0 -1 -21 5.77 0.57 0 1 -21 6.03 0.59 1 1 -21 1.38 0.31 -1 -1 -21 1.62 0.31 -1 1 -21 1.02 0.3 1 -1 -21 0.92 0.35 -2 -1 -21 2.93 0.4 2 1 -21 3.52 0.51 2 -1 -21 3.12 0.42 -2 1 -21 2.73 0.39 -3 -1 -21 0.84 0.31 3 1 -21 0.7 0.32 -3 1 -21 0.19 0.26 -4 -1 -21 2.52 0.35 4 1 -21 2 0.34 -4 1 -21 2.88 0.39 0 -2 -21 4.27 0.53 0 2 -21 3.62 0.54 1 2 -21 16.56 0.99 -1 -2 -21 16.18 0.98 -1 2 -21 15.37 1 1 -2 -21 16.04 1.03 2 2 -21 3.73 0.53 -2 -2 -21 4.86 0.54 -2 2 -21 4.94 0.54 3 2 -21 10.67 0.74 3 2 -21 9.09 0.71 -3 -2 -21 9.68 0.73 -3 2 -21 10.87 0.69 4 2 -21 3.05 0.54 4 2 -21 3.83 0.42 -4 -2 -21 3.35 0.49 0 3 -21 0.73 0.32 0 -3 -21 0.64 0.29 -1 -3 -21 2.07 0.34 1 3 -21 1.23 0.31 1 3 -21 1.7 0.33 1 -3 -21 1.6 0.38 -1 3 -21 1.93 0.36 2 3 -21 1 0.27 2 3 -21 0.65 0.26 -2 -3 -21 0.97 0.28 -2 3 -21 0.86 0.28 3 3 -21 2.24 0.35 3 3 -21 2.96 0.38 -3 -3 -21 2.4 0.35 -3 3 -21 3.01 0.44 4 3 -21 0.6 0.25 -4 -3 -21 0.36 0.26 0 4 -21 10.55 0.69 0 4 -21 10.87 0.73 0 4 -21 11.95 0.79 0 -4 -21 12.08 0.81 1 4 -21 1.98 0.28 1 4 -21 2.38 0.36 -1 -4 -21 2.29 0.36 -1 4 -21 2.37 0.34 -2 -4 -21 17 0.98 2 4 -21 15.51 0.92 2 4 -21 15.85 0.97 -2 4 -21 15.72 0.97 -3 -4 -21 0.97 0.29 3 4 -21 1.81 0.29 3 4 -21 1.39 0.23 0 5 -21 0.35 0.31 1 5 -21 1.33 0.31 1 5 -21 2.28 0.35 0 0 -22 0.49 0.26 -1 0 -22 -0.02 0.24 1 0 -22 0.02 0.28 -2 0 -22 -0.05 0.27 0 -1 -22 0.83 0.27 0 1 -22 1.05 0.29 -1 -1 -22 18.41 1.07 1 1 -22 18.01 1.08 1 -1 -22 19.41 1.19 -1 1 -22 18.73 1.08 -2 -1 -22 1.5 0.35 -2 1 -22 2.02 0.4 0 2 -22 0.11 0.26 1 2 -22 -0.21 0.28 -1 -2 -22 -0.15 0.28 -1 2 -22 -0.04 0.34 _iucr_refine_instructions_details ; v88e.res created by SHELXL-2014/7 TITL [UO2K(C25H31N3O6)][O3SCF3] CELL 1.54178 12.9299 13.2222 18.4887 90 90 90 ZERR 4 0.0006 0.0006 0.0009 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H F K N O S U UNIT 104 124 12 4 12 44 4 4 DFIX 41 0.01 S1 O11 S1 O12 S1 O13 S1' O11' S1' O12' S1' O13' DFIX 40.926 0.01 C26 F11 C26 F12 C26 F13 C26' F11' C26' F12' C26' F13' DFIX 41.281 0.01 S1 C26 S1' C26' DFIX 41.489 F11 F12 F11 F13 F12 F13 F11' F12' F11' F13' F12' F13' DFIX 41.692 O11 O12 O11 O13 O12 O13 O11' O12' O11' O13' O12' O13' DFIX 41.786 C26 O11 C26 O12 C26 O13 C26' O11' C26' O12' C26' O13' DFIX 41.839 S1 F11 S1 F12 S1 F13 S1' F11' S1' F12' S1' F13' ISOR 0.01 0.02 C26 O12' O13' F12' C26' ISOR 0.005 0.01 F13' EADP C9 C9' EXYZ C9 C9' L.S. 50 PLAN 20 SIZE 0.04 0.085 0.17 TEMP -73.16 HTAB C11 F12' HTAB WPDB -2 BOND $H CONF HTAB fmap -2 acta 132 TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.054700 3.545600 BASF 0.52560 FVAR 0.06534 0.71884 0.70749 1.40954 U 8 0.502228 0.201150 0.444094 11.00000 0.03647 0.04754 = 0.03917 -0.00131 -0.00237 -0.00231 K 4 0.544087 0.462938 0.383003 11.00000 0.09329 0.10285 = 0.11320 0.00998 -0.00637 -0.00188 O1 6 0.401322 0.327090 0.403583 11.00000 0.04092 0.05811 = 0.03621 0.00431 -0.01034 -0.00143 O6 6 0.379938 0.486646 0.316975 11.00000 0.05046 0.06454 = 0.08042 0.01798 -0.01112 -0.00093 O5 6 0.518693 0.632180 0.338048 11.00000 0.11507 0.06854 = 0.11879 0.04360 -0.05354 -0.02729 O4 6 0.722131 0.568369 0.349521 11.00000 0.07823 0.07467 = 0.09457 0.01897 -0.01577 -0.01539 O3 6 0.653010 0.400106 0.276573 11.00000 0.05694 0.07641 = 0.06665 0.01372 0.00077 -0.00671 O2 6 0.631019 0.299260 0.398049 11.00000 0.03200 0.06754 = 0.05590 -0.00041 0.00172 -0.01270 O7 6 0.510032 0.262155 0.529344 11.00000 0.06166 0.05303 = 0.03954 -0.00060 -0.01565 -0.00154 O8 6 0.490922 0.130883 0.362288 11.00000 0.04218 0.06341 = 0.04935 -0.01631 -0.01969 0.00030 N1 5 0.315465 0.144971 0.456252 11.00000 0.05073 0.05237 = 0.04386 -0.00198 0.00989 0.00253 N3 5 0.481690 0.035571 0.519606 11.00000 0.04709 0.04583 = 0.07054 0.00216 -0.00059 -0.00696 N2 5 0.673010 0.109469 0.464429 11.00000 0.05223 0.04808 = 0.05611 0.00325 -0.00411 -0.00371 C1 1 0.240465 0.176321 0.416764 11.00000 0.03780 0.04891 = 0.07510 -0.01374 0.00911 -0.00340 AFIX 43 H1 2 0.176509 0.141833 0.422364 11.00000 -1.20000 AFIX 0 C2 1 0.241776 0.258620 0.364306 11.00000 0.03299 0.06071 = 0.06327 -0.01589 -0.00610 0.01352 C3 1 0.153209 0.265136 0.320122 11.00000 0.04797 0.07932 = 0.07545 -0.02612 -0.00093 0.00238 AFIX 43 H3 2 0.098680 0.217380 0.324545 11.00000 -1.20000 AFIX 0 C4 1 0.147642 0.343142 0.269939 11.00000 0.05147 0.09269 = 0.05030 -0.00950 -0.01888 0.00176 AFIX 43 H4 2 0.091081 0.345279 0.237179 11.00000 -1.20000 AFIX 0 C5 1 0.221175 0.416515 0.266564 11.00000 0.05376 0.08000 = 0.05904 -0.00056 -0.01470 0.00224 AFIX 43 H5 2 0.215436 0.469826 0.232351 11.00000 -1.20000 AFIX 0 C7 1 0.319064 0.329917 0.362267 11.00000 0.03272 0.06740 = 0.04597 -0.01142 0.00337 0.01493 C6 1 0.305535 0.412655 0.314104 11.00000 0.04481 0.06628 = 0.04938 -0.00280 0.00065 0.01182 PART 1 C8 1 0.362205 0.576675 0.278521 31.00000 0.06865 0.08603 = 0.15145 0.06221 -0.03985 -0.01050 AFIX 23 H8A 2 0.287577 0.593381 0.279335 31.00000 -1.20000 H8B 2 0.383758 0.568208 0.227498 31.00000 -1.20000 AFIX 0 C9 1 0.425038 0.663082 0.314079 31.00000 0.06156 0.05848 = 0.08954 0.01893 0.00139 0.00741 AFIX 23 H9A 2 0.434770 0.718126 0.278424 31.00000 -1.20000 H9B 2 0.385143 0.690817 0.355254 31.00000 -1.20000 AFIX 0 PART 0 PART 2 C8' 1 0.351938 0.587386 0.336069 -31.00000 0.03745 AFIX 3 H8'A 2 0.342708 0.592246 0.387509 -31.00000 -1.20000 H8'B 2 0.287348 0.603706 0.313329 -31.00000 -1.20000 AFIX 0 C9' 1 0.425038 0.663082 0.314079 -31.00000 0.06156 0.05848 = 0.08954 0.01893 0.00139 0.00741 AFIX 23 H9'A 2 0.425459 0.669833 0.260752 -31.00000 -1.20000 H9'B 2 0.406914 0.729398 0.335464 -31.00000 -1.20000 AFIX 0 PART 0 C10 1 0.602723 0.703378 0.320696 11.00000 0.08445 0.06568 = 0.09845 0.01720 0.00167 -0.02680 AFIX 23 H10A 2 0.582564 0.773222 0.333870 11.00000 -1.20000 H10B 2 0.618488 0.701438 0.268315 11.00000 -1.20000 AFIX 0 C11 1 0.699510 0.669046 0.365864 11.00000 0.09672 0.08318 = 0.10395 0.02116 -0.00549 -0.02549 AFIX 23 H11A 2 0.759584 0.712398 0.353991 11.00000 -1.20000 H11B 2 0.684819 0.675960 0.418182 11.00000 -1.20000 AFIX 0 C12 1 0.758466 0.546975 0.275052 11.00000 0.06608 0.08890 = 0.09246 0.04091 0.01309 -0.01141 AFIX 23 H12A 2 0.770932 0.611684 0.249563 11.00000 -1.20000 H12B 2 0.824911 0.509914 0.277397 11.00000 -1.20000 AFIX 0 C13 1 0.685128 0.488281 0.234855 11.00000 0.07354 0.09506 = 0.05657 0.03581 -0.01320 0.00075 AFIX 23 H13A 2 0.716645 0.466032 0.188722 11.00000 -1.20000 H13B 2 0.623968 0.530369 0.223373 11.00000 -1.20000 AFIX 0 C14 1 0.724704 0.328830 0.292076 11.00000 0.03897 0.06759 = 0.05380 0.00697 -0.00553 -0.00647 C15 1 0.808986 0.307549 0.246577 11.00000 0.05622 0.08343 = 0.06721 0.00277 0.00969 -0.02150 AFIX 43 H15 2 0.819810 0.345886 0.203784 11.00000 -1.20000 AFIX 0 C16 1 0.877473 0.228418 0.265240 11.00000 0.04168 0.09000 = 0.08373 -0.01022 -0.00050 -0.00394 AFIX 43 H16 2 0.934556 0.213199 0.234775 11.00000 -1.20000 AFIX 0 C17 1 0.861204 0.171781 0.329229 11.00000 0.04216 0.07512 = 0.07564 -0.01653 0.00047 -0.00624 AFIX 43 H17 2 0.909085 0.121078 0.343517 11.00000 -1.20000 AFIX 0 C18 1 0.774268 0.191594 0.370622 11.00000 0.04063 0.06004 = 0.06009 -0.00692 -0.00546 -0.01024 C19 1 0.707198 0.270570 0.355210 11.00000 0.03209 0.05794 = 0.05425 -0.00790 -0.00164 -0.01331 C20 1 0.759026 0.124422 0.429834 11.00000 0.04644 0.05522 = 0.06279 -0.00830 -0.00904 0.00401 AFIX 43 H20 2 0.817493 0.086879 0.445565 11.00000 -1.20000 AFIX 0 C21 1 0.672902 0.027714 0.516480 11.00000 0.06855 0.06635 = 0.06694 0.01218 -0.02145 -0.00041 AFIX 23 H21A 2 0.682699 0.054865 0.565909 11.00000 -1.20000 H21B 2 0.730134 -0.019806 0.505975 11.00000 -1.20000 AFIX 0 C22 1 0.568946 -0.027204 0.511234 11.00000 0.06322 0.08483 = 0.10891 0.03360 0.00529 0.00584 AFIX 23 H22A 2 0.564699 -0.060973 0.463535 11.00000 -1.20000 H22B 2 0.566708 -0.080534 0.548786 11.00000 -1.20000 AFIX 0 C25 1 0.468765 0.057028 0.598499 11.00000 0.20788 0.07684 = 0.09959 0.00252 0.07080 0.00830 AFIX 137 H25A 2 0.424157 0.116300 0.604794 11.00000 -1.50000 H25B 2 0.536558 0.070422 0.620181 11.00000 -1.50000 H25C 2 0.437110 -0.001575 0.622228 11.00000 -1.50000 AFIX 0 C23 1 0.382839 -0.014645 0.496084 11.00000 0.09161 0.06175 = 0.10003 -0.00870 0.00590 -0.00843 AFIX 23 H23A 2 0.390117 -0.038705 0.445633 11.00000 -1.20000 H23B 2 0.369203 -0.074070 0.527232 11.00000 -1.20000 AFIX 0 C24 1 0.294505 0.056793 0.500846 11.00000 0.05644 0.06845 = 0.08714 0.00715 0.01297 -0.00019 AFIX 23 H24A 2 0.230489 0.023120 0.484022 11.00000 -1.20000 H24B 2 0.284238 0.077850 0.551727 11.00000 -1.20000 AFIX 0 PART 1 S1 7 0.541461 0.577703 0.564834 21.00000 0.07444 0.06626 = 0.06064 -0.01034 0.00819 -0.00538 O11 6 0.515734 0.512532 0.507035 21.00000 0.28470 0.14489 = 0.08004 -0.04195 -0.02740 0.13730 O12 6 0.514891 0.536224 0.633639 21.00000 0.30448 0.06980 = 0.09059 0.01632 0.05934 0.03015 O13 6 0.637537 0.628045 0.565640 21.00000 0.09856 0.15708 = 0.15747 -0.09117 0.02822 -0.02865 F11 3 0.456498 0.745239 0.608520 21.00000 0.13144 0.06197 = 0.07907 -0.02437 0.01172 -0.00216 F12 3 0.454140 0.725022 0.496484 21.00000 0.47059 0.07675 = 0.05830 -0.00802 -0.06705 0.11154 F13 3 0.353872 0.640396 0.562885 21.00000 0.09782 0.15787 = 0.31505 -0.10237 -0.06676 0.03123 C26 1 0.447571 0.676894 0.557806 21.00000 0.09946 0.07992 = 0.09014 -0.01623 -0.00688 -0.00171 PART 0 PART 2 S1' 7 0.507426 0.563484 0.565350 -21.00000 0.05308 0.04556 = 0.08708 0.00791 -0.00755 -0.00453 O11' 6 0.526980 0.517591 0.497910 -21.00000 0.03915 0.01137 = 0.02836 0.00773 -0.00970 -0.01616 O12' 6 0.402737 0.567975 0.587346 -21.00000 0.12805 0.16242 = 0.15671 -0.02851 0.00184 0.00759 O13' 6 0.575447 0.535992 0.621623 -21.00000 0.11143 0.08160 = 0.04926 -0.00317 -0.02650 0.02986 F11' 3 0.519944 0.750579 0.607074 -21.00000 0.23649 0.06912 = 0.07417 0.02359 -0.01907 -0.04447 F12' 3 0.639032 0.706323 0.538619 -21.00000 0.17568 0.15097 = 0.15192 -0.01223 0.03097 -0.03599 F13' 3 0.491009 0.732492 0.495548 -21.00000 0.20660 0.19814 = 0.19807 -0.00409 0.00862 -0.00131 C26' 1 0.540210 0.694092 0.550650 -21.00000 0.08913 0.08291 = 0.08680 -0.00262 0.00038 0.01004 HKLF 4 REM [UO2K(C25H31N3O6)][O3SCF3] REM R1 = 0.0357 for 4839 Fo > 4sig(Fo) and 0.0400 for all 5277 data REM 496 parameters refined using 74 restraints END WGHT 0.0547 3.5455 REM Instructions for potential hydrogen bonds EQIV $1 x-1/2, -y+1/2, -z+1 HTAB C1 O7_$1 EQIV $2 -x+1, y+1/2, -z+1/2 HTAB C8 O8_$2 HTAB C9' O8_$2 HTAB C11 F12' HTAB C13 O8_$2 EQIV $3 -x+3/2, -y+1, z-1/2 HTAB C15 O13_$3 HTAB C15 O13'_$3 EQIV $4 x+1/2, -y+1/2, -z+1 HTAB C20 O12'_$4 HTAB C21 F13_$4 EQIV $5 x, y-1, z HTAB C22 F11'_$5 HTAB C24 S1_$1 HTAB C24 O13_$1 REM Highest difference peak 1.362, deepest hole -1.456, 1-sigma level 0.153 Q1 1 0.5023 0.4650 0.3647 11.00000 0.05 -1.46 Q2 1 0.4271 0.2391 0.4402 11.00000 0.05 1.36 Q3 1 0.5002 0.2414 0.4283 11.00000 0.05 1.28 Q4 1 0.4995 0.2106 0.4848 11.00000 0.05 1.28 Q5 1 0.5570 0.2261 0.4423 11.00000 0.05 1.24 Q6 1 0.4275 0.1670 0.4412 11.00000 0.05 1.19 Q7 1 0.5645 0.1888 0.4434 11.00000 0.05 1.17 Q8 1 0.4992 0.1474 0.4257 11.00000 0.05 1.08 Q9 1 0.5891 0.0254 0.5543 11.00000 0.05 1.06 Q10 1 0.5802 0.4508 0.3853 11.00000 0.05 -1.00 Q11 1 0.5024 0.2759 0.4675 11.00000 0.05 0.97 Q12 1 0.4060 0.0293 0.5551 11.00000 0.05 0.92 Q13 1 0.4942 -0.0556 0.4555 11.00000 0.05 0.79 Q14 1 0.4199 0.4422 0.3866 11.00000 0.05 -0.74 Q15 1 0.3377 0.2071 0.4460 11.00000 0.05 0.68 Q16 1 0.5554 0.3341 0.4405 11.00000 0.05 0.64 Q17 1 0.4537 0.3386 0.4428 11.00000 0.05 0.59 Q18 1 0.3995 0.1985 0.3233 11.00000 0.05 -0.55 Q19 1 0.4005 0.7035 0.1773 11.00000 0.05 -0.51 Q20 1 0.4246 0.6932 0.5133 11.00000 0.05 0.49 REM The information below was added by Olex2. REM REM R1 = 0.0357 for 4839 Fo > 4sig(Fo) and 0.0400 for all 12865 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.36, deepest hole -1.46 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0400 REM R1_gt = 0.0357 REM wR_ref = 0.0990 REM GOOF = 1.088 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 12865 REM Reflections_gt = 4839 REM Parameters = n/a REM Hole = -1.46 REM Peak = 1.36 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.474(13) 2 0.526(13) # start Validation Reply Form _vrf_PLAT220_LsalbenUO2K ; PROBLEM: Non-Solvent Resd 1 O Ueq(max)/Ueq(min) Range 6.4 Ratio RESPONSE: The coordinated triflate is disordered. See Supporting Information for further refinement details. ; # end Validation Reply Form data_L(salben)UO2Na _audit_creation_date 2019-08-14 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2014/7' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C26 H31 F3 N3 Na O11 S U' _chemical_formula_sum 'C26 H31 F3 N3 Na O11 S U' _chemical_formula_weight 911.62 _chemical_absolute_configuration ? _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'orthorhombic' _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.9352(2) _cell_length_b 13.2651(2) _cell_length_c 18.4739(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3169.88(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7109 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 70.216 _cell_measurement_theta_min 4.103 _shelx_estimated_absorpt_T_max 0.742 _shelx_estimated_absorpt_T_min 0.232 _exptl_absorpt_coefficient_mu 15.878 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.1621 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0698 before and 0.0480 after correction. The Ratio of minimum to maximum transmission is 0.1621. The \l/2 correction factor is 0.00150.' _exptl_absorpt_special_details ? _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.910 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description 'Rectangular' _exptl_crystal_F_000 1768 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_unetI/netI 0.0390 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.963 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 12908 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.965 _diffrn_reflns_theta_full 66.000 _diffrn_reflns_theta_max 70.244 _diffrn_reflns_theta_min 4.103 _diffrn_ambient_temperature 199.99 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.963 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'Helios Multilayer Optics' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'sealed tube' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.787 _reflns_Friedel_fraction_full 0.995 _reflns_Friedel_fraction_max 0.969 _reflns_number_gt 5097 _reflns_number_total 5437 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _refine_diff_density_max 1.114 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.118 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.494(9) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 496 _refine_ls_number_reflns 5437 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0272 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0354P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.0658 _refine_special_details ; Refined as a 2-component inversion twin. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.506(9) 0.494(9) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 3. Shared sites {C9, C9'} 4. Restrained distances S1-O11 = S1-O12 = S1-O13 = S1'-O11' = S1'-O12' = S1'-O13' 1.41034 with sigma of 0.01 C26-F11 = C26-F12 = C26-F13 = C26'-F11' = C26'-F12' = C26'-F13' 1.305975 with sigma of 0.01 S1-C26 = S1'-C26' 1.806646 with sigma of 0.01 F11-F12 = F11-F13 = F12-F13 = F11'-F12' = F11'-F13' = F12'-F13' 2.099996 with sigma of 0.02 O11-O12 = O11-O13 = O12-O13 = O11'-O12' = O11'-O13' = O12'-O13' 2.386295 with sigma of 0.02 C26-O11 = C26-O12 = C26-O13 = C26'-O11' = C26'-O12' = C26'-O13' 2.518867 with sigma of 0.02 S1-F11 = S1-F12 = S1-F13 = S1'-F11' = S1'-F12' = S1'-F13' 2.593615 with sigma of 0.02 5. Uiso/Uaniso restraints and constraints Uanis(F13') \\sim Ueq, Uanis(C26') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C9) = Uanis(C9') 6. Others Sof(S1')=Sof(O11')=Sof(O12')=Sof(O13')=Sof(F11')=Sof(F12')=Sof(F13')= Sof(C26')=1-FVAR(1) Sof(S1)=Sof(O11)=Sof(O12)=Sof(O13)=Sof(F11)=Sof(F12)=Sof(F13)=Sof(C26)=FVAR(1) Sof(C8')=Sof(H8'A)=Sof(H8'B)=Sof(C9')=Sof(H9'A)=Sof(H9'B)=1-FVAR(2) Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=FVAR(2) 1(DFIX)=0.926*FVAR(4) 1(DFIX)=FVAR(3) 1(DFIX)=1.281*FVAR(4) 1(DFIX)=1.489*FVAR(4) 1(DFIX)=1.692*FVAR(4) 1(DFIX)=1.786*FVAR(4) 1(DFIX)=1.839*FVAR(4) 7.a Riding coordinates: C8'(H8'A,H8'B) 7.b Secondary CH2 refined with riding coordinates: C8(H8A,H8B), C9(H9A,H9B), C9'(H9'A,H9'B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B) 7.c Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C20(H20) 7.d Idealised Me refined as rotating group: C25(H25A,H25B,H25C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary ? _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U U 0.50214(2) 0.20135(2) 0.44421(2) 0.03369(9) Uani 1 1 d . . . . . Na Na 0.5439(3) 0.4607(3) 0.38183(19) 0.0481(7) Uani 1 1 d . . . . . O1 O 0.4016(4) 0.3274(5) 0.4036(3) 0.0426(14) Uani 1 1 d . . . . . O6 O 0.3805(5) 0.4869(6) 0.3156(4) 0.0587(16) Uani 1 1 d . . . . . O5 O 0.5232(6) 0.6306(6) 0.3386(5) 0.076(2) Uani 1 1 d . . . . . O4 O 0.7234(6) 0.5653(6) 0.3482(5) 0.071(2) Uani 1 1 d . . . . . O3 O 0.6510(5) 0.3997(6) 0.2762(4) 0.0568(15) Uani 1 1 d . . . . . O2 O 0.6294(4) 0.2987(6) 0.3977(4) 0.0436(13) Uani 1 1 d . . . . . O7 O 0.5095(7) 0.2628(4) 0.5298(3) 0.0476(13) Uani 1 1 d . . . . . O8 O 0.4949(6) 0.1314(4) 0.3622(3) 0.0489(11) Uani 1 1 d . . . . . N1 N 0.3155(6) 0.1449(6) 0.4564(5) 0.0460(18) Uani 1 1 d . . . . . N3 N 0.4823(6) 0.0356(5) 0.5204(4) 0.0497(18) Uani 1 1 d . . . . . N2 N 0.6738(6) 0.1105(7) 0.4647(5) 0.0465(19) Uani 1 1 d . . . . . C1 C 0.2400(7) 0.1746(7) 0.4163(6) 0.047(2) Uani 1 1 d . . . . . H1 H 0.1771 0.1379 0.4205 0.056 Uiso 1 1 calc R . . . . C2 C 0.2404(7) 0.2580(8) 0.3654(5) 0.0448(19) Uani 1 1 d . . . . . C3 C 0.1530(7) 0.2665(8) 0.3203(6) 0.054(2) Uani 1 1 d . . . . . H3 H 0.0981 0.2193 0.3245 0.064 Uiso 1 1 calc R . . . . C4 C 0.1467(8) 0.3439(10) 0.2694(6) 0.062(3) Uani 1 1 d . . . . . H4 H 0.0902 0.3461 0.2366 0.075 Uiso 1 1 calc R . . . . C5 C 0.2210(7) 0.4164(8) 0.2665(5) 0.055(2) Uani 1 1 d . . . . . H5 H 0.2153 0.4697 0.2324 0.066 Uiso 1 1 calc R . . . . C7 C 0.3193(6) 0.3307(7) 0.3616(4) 0.0399(17) Uani 1 1 d . . . . . C6 C 0.3055(6) 0.4126(7) 0.3133(5) 0.0462(18) Uani 1 1 d . . . . . C8 C 0.3624(14) 0.5741(15) 0.2800(12) 0.063(7) Uani 0.59(4) 1 d . . P A 1 H8A H 0.2879 0.5907 0.2829 0.076 Uiso 0.59(4) 1 calc R . P A 1 H8B H 0.3808 0.5658 0.2283 0.076 Uiso 0.59(4) 1 calc R . P A 1 C9 C 0.4265(10) 0.6615(11) 0.3129(7) 0.068(3) Uani 0.59(4) 1 d . . P A 1 H9A H 0.4366 0.7141 0.2756 0.082 Uiso 0.59(4) 1 calc R . P A 1 H9B H 0.3870 0.6919 0.3533 0.082 Uiso 0.59(4) 1 calc R . P A 1 C8' C 0.3507(17) 0.5863(17) 0.3315(16) 0.050(7) Uiso 0.41(4) 1 d . . P A 2 H8'A H 0.3415 0.5912 0.3830 0.060 Uiso 0.41(4) 1 d R . P A 2 H8'B H 0.2861 0.6026 0.3088 0.060 Uiso 0.41(4) 1 d R . P A 2 C9' C 0.4265(10) 0.6615(11) 0.3129(7) 0.068(3) Uani 0.41(4) 1 d . . P A 2 H9'A H 0.4291 0.6701 0.2597 0.082 Uiso 0.41(4) 1 calc R . P A 2 H9'B H 0.4075 0.7270 0.3349 0.082 Uiso 0.41(4) 1 calc R . P A 2 C10 C 0.6014(10) 0.7019(10) 0.3247(8) 0.072(3) Uani 1 1 d . . . . . H10A H 0.5805 0.7692 0.3427 0.086 Uiso 1 1 calc R . . . . H10B H 0.6147 0.7067 0.2721 0.086 Uiso 1 1 calc R . . . . C11 C 0.6979(11) 0.6657(11) 0.3642(9) 0.083(4) Uani 1 1 d . . . . . H11A H 0.7568 0.7096 0.3508 0.099 Uiso 1 1 calc R . . . . H11B H 0.6868 0.6723 0.4170 0.099 Uiso 1 1 calc R . . . . C12 C 0.7604(9) 0.5460(9) 0.2766(8) 0.074(3) Uani 1 1 d . . . . . H12A H 0.8266 0.5087 0.2792 0.088 Uiso 1 1 calc R . . . . H12B H 0.7735 0.6108 0.2516 0.088 Uiso 1 1 calc R . . . . C13 C 0.6839(9) 0.4861(10) 0.2344(6) 0.069(3) Uani 1 1 d . . . . . H13A H 0.6234 0.5287 0.2226 0.083 Uiso 1 1 calc R . . . . H13B H 0.7156 0.4633 0.1885 0.083 Uiso 1 1 calc R . . . . C14 C 0.7240(6) 0.3279(7) 0.2905(5) 0.0471(19) Uani 1 1 d . . . . . C15 C 0.8075(7) 0.3060(10) 0.2463(5) 0.059(2) Uani 1 1 d . . . . . H15 H 0.8183 0.3437 0.2032 0.071 Uiso 1 1 calc R . . . . C16 C 0.8760(7) 0.2289(9) 0.2649(6) 0.060(3) Uani 1 1 d . . . . . H16 H 0.9336 0.2148 0.2346 0.072 Uiso 1 1 calc R . . . . C17 C 0.8605(7) 0.1732(8) 0.3265(6) 0.056(2) Uani 1 1 d . . . . . H17 H 0.9080 0.1216 0.3393 0.067 Uiso 1 1 calc R . . . . C18 C 0.7747(6) 0.1923(8) 0.3708(5) 0.0448(18) Uani 1 1 d . . . . . C19 C 0.7064(6) 0.2721(7) 0.3540(4) 0.0396(17) Uani 1 1 d . . . . . C20 C 0.7585(7) 0.1236(7) 0.4303(5) 0.048(2) Uani 1 1 d . . . . . H20 H 0.8161 0.0844 0.4453 0.057 Uiso 1 1 calc R . . . . C21 C 0.6729(9) 0.0284(9) 0.5184(7) 0.059(3) Uani 1 1 d . . . . . H21A H 0.6817 0.0563 0.5677 0.071 Uiso 1 1 calc R . . . . H21B H 0.7304 -0.0190 0.5088 0.071 Uiso 1 1 calc R . . . . C22 C 0.5688(9) -0.0270(11) 0.5128(9) 0.078(4) Uani 1 1 d . . . . . H22A H 0.5650 -0.0610 0.4651 0.093 Uiso 1 1 calc R . . . . H22B H 0.5661 -0.0799 0.5506 0.093 Uiso 1 1 calc R . . . . C25 C 0.4682(12) 0.0585(10) 0.6019(6) 0.077(4) Uani 1 1 d . . . . . H25A H 0.4098 0.1047 0.6085 0.116 Uiso 1 1 calc GR . . . . H25B H 0.5313 0.0898 0.6209 0.116 Uiso 1 1 calc GR . . . . H25C H 0.4547 -0.0044 0.6281 0.116 Uiso 1 1 calc GR . . . . C23 C 0.3834(11) -0.0146(9) 0.4987(8) 0.070(3) Uani 1 1 d . . . . . H23A H 0.3898 -0.0400 0.4485 0.084 Uiso 1 1 calc R . . . . H23B H 0.3704 -0.0730 0.5308 0.084 Uiso 1 1 calc R . . . . C24 C 0.2947(8) 0.0568(9) 0.5032(7) 0.058(3) Uani 1 1 d . . . . . H24A H 0.2306 0.0227 0.4872 0.069 Uiso 1 1 calc R . . . . H24B H 0.2852 0.0791 0.5538 0.069 Uiso 1 1 calc R . . . . S1 S 0.5415(6) 0.5783(6) 0.5646(4) 0.0567(19) Uani 0.655(15) 1 d D . P B 1 O11 O 0.522(2) 0.5132(16) 0.5050(11) 0.072(8) Uani 0.655(15) 1 d D . P B 1 O12 O 0.520(2) 0.5356(10) 0.6325(8) 0.111(10) Uani 0.655(15) 1 d D . P B 1 O13 O 0.6372(10) 0.6304(15) 0.5616(13) 0.113(8) Uani 0.655(15) 1 d D . P B 1 F11 F 0.4584(15) 0.7431(13) 0.6083(10) 0.081(5) Uani 0.655(15) 1 d D . P B 1 F12 F 0.442(2) 0.7224(13) 0.4966(8) 0.136(11) Uani 0.655(15) 1 d D . P B 1 F13 F 0.3511(10) 0.6377(15) 0.5656(16) 0.172(13) Uani 0.655(15) 1 d D . P B 1 C26 C 0.4452(11) 0.6752(10) 0.5578(8) 0.091(8) Uani 0.655(15) 1 d D . P B 1 S1' S 0.5089(11) 0.5647(9) 0.5620(9) 0.054(3) Uani 0.345(15) 1 d D . P B 2 O11' O 0.532(3) 0.523(3) 0.4933(15) 0.075(17) Uani 0.345(15) 1 d D . P B 2 O12' O 0.4025(15) 0.571(3) 0.579(2) 0.21(4) Uani 0.345(15) 1 d D . P B 2 O13' O 0.572(2) 0.533(2) 0.6192(13) 0.107(18) Uani 0.345(15) 1 d D . P B 2 F11' F 0.512(4) 0.7524(19) 0.6052(16) 0.15(3) Uani 0.345(15) 1 d D . P B 2 F12' F 0.646(2) 0.706(3) 0.551(2) 0.19(3) Uani 0.345(15) 1 d D . P B 2 F13' F 0.511(3) 0.7343(18) 0.4922(14) 0.094(10) Uani 0.345(15) 1 d D U P B 2 C26' C 0.545(2) 0.6952(13) 0.5524(13) 0.099(14) Uani 0.345(15) 1 d D U P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.03328(12) 0.03708(12) 0.03070(13) -0.00157(7) -0.00243(14) -0.00217(15) Na 0.0481(15) 0.0476(16) 0.0487(17) 0.0047(14) -0.0090(13) -0.0016(14) O1 0.036(3) 0.056(4) 0.036(3) 0.001(3) -0.007(2) 0.001(2) O6 0.046(3) 0.055(4) 0.075(5) 0.013(3) -0.014(3) 0.002(3) O5 0.066(5) 0.069(4) 0.094(5) 0.043(4) -0.020(4) -0.011(3) O4 0.066(4) 0.069(5) 0.079(5) 0.024(4) -0.013(4) -0.011(4) O3 0.044(3) 0.069(4) 0.058(4) 0.015(4) -0.002(3) -0.005(3) O2 0.034(3) 0.052(3) 0.044(3) 0.003(3) -0.001(2) -0.003(3) O7 0.061(4) 0.045(2) 0.037(2) 0.002(2) -0.012(3) -0.010(3) O8 0.040(2) 0.062(3) 0.045(2) -0.009(2) -0.004(3) -0.003(4) N1 0.043(4) 0.049(4) 0.046(4) -0.006(4) 0.010(3) 0.000(3) N3 0.047(5) 0.042(3) 0.060(4) -0.003(3) -0.003(3) -0.005(3) N2 0.042(3) 0.044(4) 0.053(5) 0.000(4) -0.008(3) -0.003(3) C1 0.036(4) 0.042(5) 0.062(6) -0.009(4) 0.009(4) -0.002(3) C2 0.031(4) 0.053(5) 0.050(5) -0.012(4) 0.002(3) 0.005(4) C3 0.035(4) 0.064(5) 0.063(6) -0.016(5) -0.005(4) 0.003(4) C4 0.041(5) 0.082(7) 0.064(6) -0.010(6) -0.014(4) 0.004(5) C5 0.053(5) 0.070(6) 0.042(4) 0.002(4) -0.009(4) 0.013(5) C7 0.034(4) 0.046(4) 0.039(4) -0.008(3) 0.000(3) 0.006(3) C6 0.040(4) 0.057(5) 0.042(4) 0.001(4) -0.001(3) 0.006(4) C8 0.060(10) 0.069(11) 0.061(14) 0.028(10) -0.009(8) -0.005(8) C9 0.068(7) 0.066(7) 0.070(7) 0.016(6) -0.011(5) 0.002(5) C9' 0.068(7) 0.066(7) 0.070(7) 0.016(6) -0.011(5) 0.002(5) C10 0.069(6) 0.062(6) 0.084(8) 0.019(7) -0.001(6) -0.005(6) C11 0.073(7) 0.073(7) 0.102(10) 0.013(7) -0.010(7) -0.018(6) C12 0.065(6) 0.070(6) 0.086(8) 0.036(6) 0.003(6) -0.014(5) C13 0.067(6) 0.082(7) 0.058(6) 0.035(6) -0.001(5) -0.001(6) C14 0.036(4) 0.055(5) 0.050(5) 0.009(4) -0.007(3) -0.009(3) C15 0.045(5) 0.079(7) 0.053(5) 0.009(5) 0.005(4) -0.016(5) C16 0.036(4) 0.074(6) 0.070(7) -0.013(5) 0.007(4) -0.009(4) C17 0.037(4) 0.063(5) 0.067(6) -0.006(5) -0.001(4) -0.005(4) C18 0.033(4) 0.052(5) 0.049(5) -0.004(5) -0.009(3) -0.008(4) C19 0.035(4) 0.045(4) 0.039(4) -0.005(3) -0.002(3) -0.011(3) C20 0.042(4) 0.045(5) 0.056(5) -0.006(4) -0.012(4) -0.001(3) C21 0.059(6) 0.050(5) 0.067(7) 0.015(5) -0.020(5) -0.007(5) C22 0.061(7) 0.069(7) 0.102(10) 0.016(7) 0.006(6) 0.008(6) C25 0.111(12) 0.068(6) 0.052(5) 0.000(5) 0.009(6) -0.004(6) C23 0.082(8) 0.053(6) 0.074(7) -0.009(6) 0.001(6) -0.017(6) C24 0.052(5) 0.054(6) 0.068(6) 0.008(5) 0.011(5) -0.006(4) S1 0.063(4) 0.058(3) 0.049(3) -0.010(2) 0.003(3) -0.004(3) O11 0.12(2) 0.045(9) 0.049(8) -0.013(8) -0.002(10) -0.001(10) O12 0.23(3) 0.044(6) 0.061(9) 0.005(5) 0.018(15) -0.004(14) O13 0.070(9) 0.128(17) 0.141(17) -0.060(17) 0.023(11) -0.026(10) F11 0.105(9) 0.063(9) 0.074(11) -0.021(8) 0.006(7) -0.001(7) F12 0.25(3) 0.090(13) 0.072(10) -0.016(9) -0.051(15) 0.072(17) F13 0.067(9) 0.15(2) 0.29(3) -0.13(2) -0.021(14) 0.015(10) C26 0.135(19) 0.066(11) 0.072(13) -0.029(10) -0.038(13) 0.052(13) S1' 0.060(8) 0.034(4) 0.068(6) -0.002(3) -0.011(8) -0.005(5) O11' 0.14(4) 0.051(19) 0.036(14) 0.005(12) -0.024(18) 0.01(2) O12' 0.09(3) 0.24(7) 0.30(9) -0.21(7) 0.01(4) -0.03(4) O13' 0.17(4) 0.13(3) 0.020(11) -0.017(14) -0.028(18) 0.07(3) F11' 0.35(8) 0.041(12) 0.051(15) 0.002(11) 0.02(4) -0.02(4) F12' 0.23(5) 0.18(4) 0.17(4) -0.06(4) 0.09(4) -0.12(4) F13' 0.17(3) 0.045(9) 0.070(13) 0.002(8) -0.004(17) -0.002(16) C26' 0.115(18) 0.096(18) 0.087(18) 0.000(13) 0.002(13) 0.007(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U Na 3.668(3) . ? U O1 2.247(6) . ? U O2 2.262(6) . ? U O7 1.782(5) . ? U O8 1.780(5) . ? U N1 2.538(8) . ? U N3 2.623(7) . ? U N2 2.555(8) . ? Na O1 2.584(7) . ? Na O6 2.466(7) . ? Na O5 2.406(8) . ? Na O4 2.775(8) . ? Na O3 2.526(8) . ? Na O2 2.435(8) . ? Na O11 2.395(17) . ? Na O11' 2.23(2) . ? O1 C7 1.317(10) . ? O6 C6 1.383(12) . ? O6 C8 1.351(19) . ? O6 C8' 1.40(2) . ? O5 C9 1.399(15) . ? O5 C9' 1.399(15) . ? O5 C10 1.408(14) . ? O4 C11 1.404(18) . ? O4 C12 1.431(17) . ? O3 C13 1.447(13) . ? O3 C14 1.367(12) . ? O2 C19 1.330(11) . ? N1 C1 1.286(14) . ? N1 C24 1.479(14) . ? N3 C22 1.401(14) . ? N3 C25 1.547(14) . ? N3 C23 1.497(14) . ? N2 C20 1.278(13) . ? N2 C21 1.473(13) . ? C1 H1 0.9500 . ? C1 C2 1.452(15) . ? C2 C3 1.410(13) . ? C2 C7 1.406(13) . ? C3 H3 0.9500 . ? C3 C4 1.394(17) . ? C4 H4 0.9500 . ? C4 C5 1.360(16) . ? C5 H5 0.9500 . ? C5 C6 1.395(12) . ? C7 C6 1.419(13) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C9 1.55(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C8' H8'A 0.9600 . ? C8' H8'B 0.9601 . ? C8' C9' 1.44(3) . ? C9' H9'A 0.9900 . ? C9' H9'B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.523(19) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 C13 1.489(19) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.385(14) . ? C14 C19 1.406(13) . ? C15 H15 0.9500 . ? C15 C16 1.396(17) . ? C16 H16 0.9500 . ? C16 C17 1.372(17) . ? C17 H17 0.9500 . ? C17 C18 1.402(13) . ? C18 C19 1.413(14) . ? C18 C20 1.443(15) . ? C20 H20 0.9500 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 C22 1.538(17) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.490(18) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? S1 O11 1.421(10) . ? S1 O12 1.406(11) . ? S1 O13 1.419(11) . ? S1 C26 1.794(11) . ? F11 C26 1.309(11) . ? F12 C26 1.292(12) . ? F13 C26 1.323(12) . ? S1' O11' 1.415(13) . ? S1' O12' 1.413(13) . ? S1' O13' 1.400(13) . ? S1' C26' 1.803(13) . ? F11' C26' 1.308(13) . ? F12' C26' 1.307(13) . ? F13' C26' 1.305(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U Na 44.17(17) . . ? O1 U O2 82.5(3) . . ? O1 U N1 72.4(3) . . ? O1 U N3 138.2(2) . . ? O1 U N2 154.7(2) . . ? O2 U Na 40.37(18) . . ? O2 U N1 153.4(3) . . ? O2 U N3 138.9(2) . . ? O2 U N2 72.1(3) . . ? O7 U Na 80.91(18) . . ? O7 U O1 89.2(3) . . ? O7 U O2 92.1(3) . . ? O7 U N1 96.2(3) . . ? O7 U N3 85.0(2) . . ? O7 U N2 92.2(3) . . ? O8 U Na 103.25(19) . . ? O8 U O1 94.2(3) . . ? O8 U O2 90.7(3) . . ? O8 U O7 175.8(2) . . ? O8 U N1 82.6(3) . . ? O8 U N3 90.9(2) . . ? O8 U N2 85.7(3) . . ? N1 U Na 116.4(2) . . ? N1 U N3 67.2(3) . . ? N1 U N2 132.4(3) . . ? N3 U Na 165.70(17) . . ? N2 U Na 111.2(2) . . ? N2 U N3 67.1(3) . . ? O1 Na U 37.29(14) . . ? O1 Na O4 166.6(3) . . ? O6 Na U 99.3(2) . . ? O6 Na O1 64.1(2) . . ? O6 Na O4 122.4(3) . . ? O6 Na O3 97.6(3) . . ? O5 Na U 165.1(2) . . ? O5 Na O1 127.9(3) . . ? O5 Na O6 66.9(3) . . ? O5 Na O4 63.3(3) . . ? O5 Na O3 96.0(3) . . ? O5 Na O2 156.5(3) . . ? O4 Na U 131.5(2) . . ? O3 Na U 91.3(2) . . ? O3 Na O1 107.0(3) . . ? O3 Na O4 61.9(3) . . ? O2 Na U 36.99(15) . . ? O2 Na O1 72.60(19) . . ? O2 Na O6 125.0(3) . . ? O2 Na O4 95.1(3) . . ? O2 Na O3 64.0(2) . . ? O11 Na U 87.6(6) . . ? O11 Na O1 88.2(7) . . ? O11 Na O6 109.3(7) . . ? O11 Na O5 91.7(6) . . ? O11 Na O4 99.5(7) . . ? O11 Na O3 152.9(7) . . ? O11 Na O2 101.3(6) . . ? O11' Na U 92.7(11) . . ? O11' Na O1 93.4(11) . . ? O11' Na O6 110.2(12) . . ? O11' Na O5 87.2(11) . . ? O11' Na O4 94.7(11) . . ? O11' Na O3 150.8(12) . . ? O11' Na O2 104.4(11) . . ? U O1 Na 98.5(2) . . ? C7 O1 U 133.5(6) . . ? C7 O1 Na 117.4(6) . . ? C6 O6 Na 121.1(5) . . ? C6 O6 C8' 118.8(11) . . ? C8 O6 Na 120.7(9) . . ? C8 O6 C6 118.2(10) . . ? C8' O6 Na 105.3(11) . . ? C9 O5 Na 119.1(7) . . ? C9 O5 C10 112.5(8) . . ? C9' O5 Na 119.1(7) . . ? C9' O5 C10 112.5(8) . . ? C10 O5 Na 127.6(7) . . ? C11 O4 Na 103.4(7) . . ? C11 O4 C12 116.3(10) . . ? C12 O4 Na 113.5(7) . . ? C13 O3 Na 108.7(7) . . ? C14 O3 Na 117.0(6) . . ? C14 O3 C13 116.9(8) . . ? U O2 Na 102.6(2) . . ? C19 O2 U 128.6(6) . . ? C19 O2 Na 120.1(6) . . ? C1 N1 U 125.6(7) . . ? C1 N1 C24 116.1(8) . . ? C24 N1 U 117.2(6) . . ? C22 N3 U 111.4(7) . . ? C22 N3 C25 108.0(10) . . ? C22 N3 C23 113.0(9) . . ? C25 N3 U 111.7(6) . . ? C23 N3 U 108.2(7) . . ? C23 N3 C25 104.4(9) . . ? C20 N2 U 127.3(7) . . ? C20 N2 C21 116.3(9) . . ? C21 N2 U 116.2(6) . . ? N1 C1 H1 116.5 . . ? N1 C1 C2 127.0(8) . . ? C2 C1 H1 116.5 . . ? C3 C2 C1 116.2(9) . . ? C7 C2 C1 123.9(8) . . ? C7 C2 C3 119.8(10) . . ? C2 C3 H3 119.8 . . ? C4 C3 C2 120.3(9) . . ? C4 C3 H3 119.8 . . ? C3 C4 H4 119.8 . . ? C5 C4 C3 120.4(9) . . ? C5 C4 H4 119.8 . . ? C4 C5 H5 119.9 . . ? C4 C5 C6 120.3(10) . . ? C6 C5 H5 119.9 . . ? O1 C7 C2 122.3(9) . . ? O1 C7 C6 119.9(8) . . ? C2 C7 C6 117.7(8) . . ? O6 C6 C5 123.0(9) . . ? O6 C6 C7 116.0(7) . . ? C5 C6 C7 121.1(9) . . ? O6 C8 H8A 109.5 . . ? O6 C8 H8B 109.5 . . ? O6 C8 C9 110.9(13) . . ? H8A C8 H8B 108.0 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? O5 C9 C8 113.1(12) . . ? O5 C9 H9A 109.0 . . ? O5 C9 H9B 109.0 . . ? C8 C9 H9A 109.0 . . ? C8 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? O6 C8' H8'A 107.7 . . ? O6 C8' H8'B 111.0 . . ? O6 C8' C9' 114.4(18) . . ? H8'A C8' H8'B 108.0 . . ? C9' C8' H8'A 105.9 . . ? C9' C8' H8'B 109.4 . . ? O5 C9' C8' 108.9(13) . . ? O5 C9' H9'A 109.9 . . ? O5 C9' H9'B 109.9 . . ? C8' C9' H9'A 109.9 . . ? C8' C9' H9'B 109.9 . . ? H9'A C9' H9'B 108.3 . . ? O5 C10 H10A 110.4 . . ? O5 C10 H10B 110.4 . . ? O5 C10 C11 106.8(10) . . ? H10A C10 H10B 108.6 . . ? C11 C10 H10A 110.4 . . ? C11 C10 H10B 110.4 . . ? O4 C11 C10 113.0(12) . . ? O4 C11 H11A 109.0 . . ? O4 C11 H11B 109.0 . . ? C10 C11 H11A 109.0 . . ? C10 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? O4 C12 H12A 109.5 . . ? O4 C12 H12B 109.5 . . ? O4 C12 C13 110.9(9) . . ? H12A C12 H12B 108.1 . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? O3 C13 C12 109.8(9) . . ? O3 C13 H13A 109.7 . . ? O3 C13 H13B 109.7 . . ? C12 C13 H13A 109.7 . . ? C12 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? O3 C14 C15 124.8(9) . . ? O3 C14 C19 114.5(8) . . ? C15 C14 C19 120.6(9) . . ? C14 C15 H15 119.9 . . ? C14 C15 C16 120.2(9) . . ? C16 C15 H15 119.9 . . ? C15 C16 H16 119.8 . . ? C17 C16 C15 120.4(9) . . ? C17 C16 H16 119.8 . . ? C16 C17 H17 119.9 . . ? C16 C17 C18 120.2(10) . . ? C18 C17 H17 119.9 . . ? C17 C18 C19 120.1(9) . . ? C17 C18 C20 116.5(9) . . ? C19 C18 C20 123.3(8) . . ? O2 C19 C14 119.3(9) . . ? O2 C19 C18 122.2(8) . . ? C14 C19 C18 118.5(8) . . ? N2 C20 C18 126.1(9) . . ? N2 C20 H20 116.9 . . ? C18 C20 H20 116.9 . . ? N2 C21 H21A 110.0 . . ? N2 C21 H21B 110.0 . . ? N2 C21 C22 108.3(9) . . ? H21A C21 H21B 108.4 . . ? C22 C21 H21A 110.0 . . ? C22 C21 H21B 110.0 . . ? N3 C22 C21 114.1(11) . . ? N3 C22 H22A 108.7 . . ? N3 C22 H22B 108.7 . . ? C21 C22 H22A 108.7 . . ? C21 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N3 C23 H23A 109.4 . . ? N3 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C24 C23 N3 111.1(9) . . ? C24 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? N1 C24 C23 109.3(9) . . ? N1 C24 H24A 109.8 . . ? N1 C24 H24B 109.8 . . ? C23 C24 H24A 109.8 . . ? C23 C24 H24B 109.8 . . ? H24A C24 H24B 108.3 . . ? O11 S1 C26 105.0(11) . . ? O12 S1 O11 114.3(13) . . ? O12 S1 O13 114.0(13) . . ? O12 S1 C26 102.2(11) . . ? O13 S1 O11 114.7(13) . . ? O13 S1 C26 104.7(10) . . ? S1 O11 Na 153.2(18) . . ? F11 C26 S1 110.7(11) . . ? F11 C26 F13 107.5(14) . . ? F12 C26 S1 115.4(11) . . ? F12 C26 F11 107.1(13) . . ? F12 C26 F13 104.5(16) . . ? F13 C26 S1 111.2(11) . . ? O11' S1' C26' 103.4(15) . . ? O12' S1' O11' 115.0(17) . . ? O12' S1' C26' 102.6(15) . . ? O13' S1' O11' 116.0(18) . . ? O13' S1' O12' 115.0(18) . . ? O13' S1' C26' 102.1(14) . . ? S1' O11' Na 172(3) . . ? F11' C26' S1' 113.4(15) . . ? F12' C26' S1' 111.4(16) . . ? F12' C26' F11' 106.6(19) . . ? F13' C26' S1' 112.1(15) . . ? F13' C26' F11' 107.1(17) . . ? F13' C26' F12' 105.7(19) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C8 H8B O8 0.99 2.48 3.30(2) 140.1 3_655 C9' H9'A O8 0.99 2.51 3.414(15) 151.7 3_655 C11 H11B F12' 0.99 2.56 3.55(5) 173.9 . C13 H13A O8 0.99 2.58 3.500(13) 154.8 3_655 C15 H15 O13 0.95 2.70 3.59(2) 155.5 2_664 C15 H15 O13' 0.95 2.66 3.54(3) 152.8 2_664 C20 H20 O12' 0.95 2.39 3.19(3) 141.8 4_556 C21 H21B F13 0.99 2.61 3.55(2) 158.0 4_556 C22 H22B F11' 0.99 2.54 3.47(3) 155.5 1_545 C24 H24A S1 0.99 2.95 3.938(14) 178.4 4_456 C24 H24A O13 0.99 2.53 3.43(2) 150.8 4_456 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag U O1 C7 C2 39.3(11) . . . . ? U O1 C7 C6 -144.2(7) . . . . ? U O2 C19 C14 129.2(7) . . . . ? U O2 C19 C18 -53.9(10) . . . . ? U N1 C1 C2 -11.9(14) . . . . ? U N1 C24 C23 -33.3(11) . . . . ? U N3 C22 C21 45.2(14) . . . . ? U N3 C23 C24 -52.5(11) . . . . ? U N2 C20 C18 -1.2(14) . . . . ? U N2 C21 C22 36.5(12) . . . . ? Na O1 C7 C2 175.7(6) . . . . ? Na O1 C7 C6 -7.8(10) . . . . ? Na O6 C6 C5 -168.1(7) . . . . ? Na O6 C6 C7 11.6(11) . . . . ? Na O6 C8 C9 -25(2) . . . . ? Na O6 C8' C9' 57(2) . . . . ? Na O5 C9 C8 -29.1(15) . . . . ? Na O5 C9' C8' 11.4(18) . . . . ? Na O5 C10 C11 -18.0(17) . . . . ? Na O4 C11 C10 -55.2(13) . . . . ? Na O4 C12 C13 8.5(11) . . . . ? Na O3 C13 C12 69.0(10) . . . . ? Na O3 C14 C15 -160.9(8) . . . . ? Na O3 C14 C19 21.7(9) . . . . ? Na O2 C19 C14 -12.7(10) . . . . ? Na O2 C19 C18 164.2(6) . . . . ? O1 C7 C6 O6 -2.0(12) . . . . ? O1 C7 C6 C5 177.8(8) . . . . ? O6 C8 C9 O5 34(2) . . . . ? O6 C8' C9' O5 -47(2) . . . . ? O5 C10 C11 O4 51.9(16) . . . . ? O4 C12 C13 O3 -49.4(13) . . . . ? O3 C14 C15 C16 -178.0(9) . . . . ? O3 C14 C19 O2 -6.6(11) . . . . ? O3 C14 C19 C18 176.4(8) . . . . ? N1 C1 C2 C3 171.1(9) . . . . ? N1 C1 C2 C7 -11.8(15) . . . . ? N3 C23 C24 N1 57.8(13) . . . . ? N2 C21 C22 N3 -55.3(15) . . . . ? C1 N1 C24 C23 135.2(10) . . . . ? C1 C2 C3 C4 -179.7(9) . . . . ? C1 C2 C7 O1 1.6(13) . . . . ? C1 C2 C7 C6 -175.0(8) . . . . ? C2 C3 C4 C5 -5.0(16) . . . . ? C2 C7 C6 O6 174.7(8) . . . . ? C2 C7 C6 C5 -5.6(13) . . . . ? C3 C2 C7 O1 178.6(8) . . . . ? C3 C2 C7 C6 2.1(12) . . . . ? C3 C4 C5 C6 1.5(16) . . . . ? C4 C5 C6 O6 -176.4(10) . . . . ? C4 C5 C6 C7 3.9(15) . . . . ? C7 C2 C3 C4 3.1(14) . . . . ? C6 O6 C8 C9 155.9(11) . . . . ? C6 O6 C8' C9' -163.2(14) . . . . ? C8 O6 C6 C5 11.2(18) . . . . ? C8 O6 C6 C7 -169.0(13) . . . . ? C9 O5 C10 C11 172.4(12) . . . . ? C8' O6 C6 C5 58.8(18) . . . . ? C8' O6 C6 C7 -121.4(16) . . . . ? C9' O5 C10 C11 172.4(12) . . . . ? C10 O5 C9 C8 141.5(14) . . . . ? C10 O5 C9' C8' -178.0(16) . . . . ? C11 O4 C12 C13 -111.2(11) . . . . ? C12 O4 C11 C10 69.8(14) . . . . ? C13 O3 C14 C15 -29.6(14) . . . . ? C13 O3 C14 C19 153.0(9) . . . . ? C14 O3 C13 C12 -66.0(14) . . . . ? C14 C15 C16 C17 0.8(16) . . . . ? C15 C14 C19 O2 175.9(9) . . . . ? C15 C14 C19 C18 -1.2(13) . . . . ? C15 C16 C17 C18 1.1(15) . . . . ? C16 C17 C18 C19 -3.0(13) . . . . ? C16 C17 C18 C20 173.7(9) . . . . ? C17 C18 C19 O2 -173.9(8) . . . . ? C17 C18 C19 C14 3.0(12) . . . . ? C17 C18 C20 N2 -160.4(9) . . . . ? C19 C14 C15 C16 -0.7(15) . . . . ? C19 C18 C20 N2 16.2(14) . . . . ? C20 N2 C21 C22 -139.0(11) . . . . ? C20 C18 C19 O2 9.6(13) . . . . ? C20 C18 C19 C14 -173.5(8) . . . . ? C21 N2 C20 C18 173.7(9) . . . . ? C22 N3 C23 C24 -176.3(11) . . . . ? C25 N3 C22 C21 -77.8(13) . . . . ? C25 N3 C23 C24 66.6(12) . . . . ? C23 N3 C22 C21 167.3(11) . . . . ? C24 N1 C1 C2 -179.4(9) . . . . ? O11 S1 C26 F11 -176.8(17) . . . . ? O11 S1 C26 F12 -55.0(18) . . . . ? O11 S1 C26 F13 63.8(17) . . . . ? O12 S1 O11 Na -160(3) . . . . ? O12 S1 C26 F11 63.5(16) . . . . ? O12 S1 C26 F12 -174.7(16) . . . . ? O12 S1 C26 F13 -55.8(17) . . . . ? O13 S1 O11 Na -26(4) . . . . ? O13 S1 C26 F11 -55.6(16) . . . . ? O13 S1 C26 F12 66.2(16) . . . . ? O13 S1 C26 F13 -175.0(15) . . . . ? C26 S1 O11 Na 89(3) . . . . ? O11' S1' C26' F11' 167(3) . . . . ? O11' S1' C26' F12' -72(3) . . . . ? O11' S1' C26' F13' 46(3) . . . . ? O12' S1' C26' F11' 47(3) . . . . ? O12' S1' C26' F12' 168(3) . . . . ? O12' S1' C26' F13' -74(3) . . . . ? O13' S1' C26' F11' -72(3) . . . . ? O13' S1' C26' F12' 48(2) . . . . ? O13' S1' C26' F13' 167(2) . . . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 1 0 0 0.07 0.16 -1 0 0 0.02 0.15 2 0 0 386.83 14.06 3 0 0 -0.61 0.4 4 0 0 486.12 16.74 6 0 0 483.67 15.01 7 0 0 0.34 0.18 8 0 0 289.94 9.21 9 0 0 0.14 0.2 10 0 0 110.81 3.87 11 0 0 0.23 0.28 11 0 0 0.35 0.29 12 0 0 55.49 2.25 0 -1 0 -0.52 0.23 1 -1 0 7.2 0.44 2 -1 0 -0.02 0.25 -3 -1 0 0.01 0.41 -4 -1 0 1.89 0.98 4 -1 0 2.5 1.2 5 -1 0 38.48 2.88 6 -1 0 -0.04 0.16 6 1 0 0.04 0.16 7 -1 0 19.94 0.88 7 1 0 19.79 0.87 8 1 0 10 0.61 8 -1 0 10.67 0.65 9 1 0 6.11 0.51 9 -1 0 6.74 0.54 10 1 0 2.53 0.41 10 -1 0 2.86 0.46 11 1 0 2.36 0.44 11 -1 0 2.56 0.45 12 -1 0 1.55 0.43 13 -1 0 0.57 0.38 14 -1 0 2.45 0.61 0 -2 0 313.22 10.46 1 -2 0 702.97 22.43 2 -2 0 207.18 6.86 3 -2 0 245.15 8.17 -4 -2 0 117.04 5.4 5 -2 0 289.13 13.22 -5 -2 0 285.86 12.49 6 2 0 153.19 4.98 6 -2 0 157.78 5.02 7 2 0 107.77 3.6 7 -2 0 109.92 3.65 8 -2 0 173.92 5.61 8 2 0 166.81 5.54 9 2 0 39.57 1.6 9 -2 0 39.82 1.65 10 -2 0 86.68 3.22 10 2 0 87.61 3.14 11 -2 0 39.81 1.81 11 -2 0 40.38 1.74 12 -2 0 52.55 1.84 12 -2 0 52.89 2.23 12 -2 0 57.18 2.27 13 -2 0 15.3 0.69 13 -2 0 16.22 1.04 13 -2 0 15.76 1.1 14 -2 0 31.69 1.22 14 -2 0 32.14 1.63 15 -2 0 10.89 0.55 0 -3 0 0.12 0.57 1 -3 0 5.2 0.94 -1 -3 0 4 0.81 2 -3 0 0.32 0.39 3 -3 0 32.04 1.7 4 -3 0 18.87 1.33 6 3 0 39.17 1.39 6 -3 0 35.64 1.43 7 3 0 6.57 0.46 8 3 0 1.27 0.28 9 3 0 5.45 0.5 10 3 0 7.68 1.04 10 -3 0 7.76 0.66 10 -3 0 7.07 0.94 11 -3 0 0.38 0.16 11 -3 0 0.37 0.37 11 -3 0 1.13 0.41 12 -3 0 1.74 0.25 12 -3 0 1.39 0.44 12 -3 0 1.56 0.47 13 -3 0 1.66 0.48 13 -3 0 1.45 0.5 13 -3 0 1.73 0.27 14 -3 0 0.37 0.21 14 -3 0 0.39 0.35 14 -3 0 0.19 0.41 15 -3 0 1.42 0.46 15 -3 0 0.82 0.18 0 -4 0 120.51 5 -1 -4 0 271.67 8.94 1 -4 0 202.26 8.9 2 -4 0 191.51 7.32 -2 -4 0 203.99 7.45 3 -4 0 303.89 10.42 4 -4 0 58.96 2.82 5 4 0 151.48 4.88 6 4 0 9.22 0.54 7 4 0 158.49 5.17 8 4 0 27.78 1.2 9 4 0 52.62 2.04 10 -4 0 11.77 0.87 10 -4 0 12.27 0.88 10 -4 0 11.2 0.82 11 -4 0 81.78 3.12 11 -4 0 86.26 3.19 11 -4 0 82.2 2.83 12 -4 0 2.84 0.36 12 -4 0 3.64 0.63 12 -4 0 3.83 0.58 13 -4 0 33.28 1.73 13 -4 0 34.59 1.58 13 -4 0 33.33 1.38 14 -4 0 2.99 0.45 14 -4 0 3.15 0.38 14 -4 0 3.32 0.57 15 -4 0 24.67 0.92 0 -5 0 0.29 0.61 -1 -5 0 5.65 1.19 1 -5 0 3.91 1.1 -2 -5 0 4.03 1.13 2 -5 0 3.16 1.14 3 -5 0 19.4 1.78 -3 -5 0 21.5 1.94 4 5 0 5.79 0.44 4 -5 0 5.95 1.06 5 5 0 1.53 0.25 6 5 0 0.76 0.23 7 5 0 1.42 0.3 8 5 0 0.22 0.23 9 -5 0 5.89 0.69 10 -5 0 0.22 0.33 10 -5 0 0.1 0.2 10 -5 0 0.19 0.32 11 -5 0 0.27 0.24 11 -5 0 0.5 0.41 11 -5 0 0.49 0.32 12 -5 0 0.32 0.48 12 -5 0 0.05 0.31 12 -5 0 0.07 0.24 13 -5 0 0.98 0.49 13 -5 0 0.9 0.35 13 -5 0 1.12 0.32 14 -5 0 0.09 0.18 14 -5 0 0.06 0.31 14 -5 0 -0.14 0.23 0 -6 0 25.19 2.07 1 -6 0 212.74 8.68 -1 -6 0 231.75 8.79 2 -6 0 3.81 1.33 2 6 0 6.32 0.64 -2 -6 0 6.9 1.47 3 6 0 305.22 9.45 3 -6 0 262.79 11.46 -3 -6 0 297.78 11.39 -4 -6 0 0.84 0.83 4 6 0 0.39 0.25 5 6 0 184.78 6.21 -5 -6 0 195.47 8.45 6 6 0 3.93 0.46 7 6 0 114.42 3.95 9 -6 0 83.49 3.08 9 -6 0 83.6 3.21 9 -6 0 86.26 3.05 10 -6 0 10.64 0.77 10 6 0 10 0.56 10 -6 0 10.1 0.81 10 -6 0 10.77 0.96 11 -6 0 71.47 2.93 11 6 0 69.35 2.38 11 -6 0 68.19 2.64 11 -6 0 71.19 2.63 12 6 0 4.6 0.41 12 -6 0 4.48 0.56 12 -6 0 4.85 0.76 12 -6 0 3.39 0.48 13 -6 0 38.44 1.8 13 6 0 34.85 1.34 13 -6 0 38.19 1.53 13 -6 0 39.99 1.58 14 -6 0 1.17 0.35 14 -6 0 1.04 0.27 14 -6 0 0.96 0.21 0 -7 0 0.2 0.59 -1 -7 0 2.58 0.99 1 -7 0 2.05 0.87 -2 -7 0 6.48 1.44 2 7 0 6.06 0.57 2 -7 0 4.94 1.3 3 7 0 1.28 0.46 -3 -7 0 1.38 0.96 4 7 0 7.87 0.81 -4 -7 0 6.98 1.73 5 7 0 0.22 0.28 6 7 0 0.51 0.35 7 7 0 1.88 0.41 8 -7 0 0.82 0.31 8 -7 0 0.75 0.49 9 7 0 0.03 0.16 9 -7 0 0.26 0.3 9 -7 0 0.16 0.48 9 -7 0 0.38 0.34 10 -7 0 1.15 0.39 10 -7 0 0.65 0.56 10 -7 0 1.24 0.39 10 7 0 1.34 0.24 11 -7 0 0.36 0.32 11 -7 0 0.54 0.49 11 7 0 0.37 0.19 11 -7 0 0.56 0.36 12 -7 0 -0.05 0.26 12 -7 0 -0.07 0.26 12 -7 0 -0.66 0.36 12 7 0 0.11 0.15 13 -7 0 0.56 0.38 13 -7 0 0.76 0.24 13 7 0 0.75 0.17 13 -7 0 0.35 0.26 14 -7 0 0.21 0.14 0 -8 0 148.79 6.78 -1 -8 0 80.57 4.52 -2 -8 0 71.59 4.33 2 8 0 70.08 2.62 3 8 0 72.06 2.82 -3 -8 0 77.38 5.41 4 8 0 93.98 3.56 5 8 0 43.15 2.12 6 8 0 43.64 2.12 7 -8 0 24 1.42 8 8 0 36.91 1.89 8 8 0 38.44 1.44 8 -8 0 38.2 1.74 8 -8 0 38.9 1.61 8 -8 0 37.51 1.91 9 8 0 23.54 0.98 9 -8 0 23.26 1.48 9 -8 0 23.8 1.28 9 -8 0 21.03 1.14 10 -8 0 32.97 1.47 10 8 0 32.97 1.27 10 -8 0 33.59 1.56 10 -8 0 31.49 1.76 11 -8 0 13.34 1.09 11 -8 0 11.96 0.82 11 8 0 12.23 0.63 11 -8 0 13.05 0.86 12 -8 0 13.29 0.79 12 -8 0 13.63 0.78 12 -8 0 12.97 0.98 12 8 0 12.91 0.61 13 8 0 9.75 0.46 13 -8 0 10.27 0.6 13 -8 0 10.57 0.56 1 9 0 2.06 0.38 2 9 0 0.43 0.28 3 9 0 4.69 0.57 4 9 0 -0.09 0.27 5 9 0 5.42 0.66 6 -9 0 1.57 0.48 7 9 0 0.36 0.22 7 -9 0 -0.07 0.41 7 9 0 0.27 0.37 8 -9 0 0.82 0.36 8 -9 0 1.27 0.5 8 9 0 0.51 0.43 8 9 0 0.88 0.25 8 -9 0 0.69 0.47 9 9 0 0.89 0.23 9 -9 0 0.3 0.31 9 -9 0 0.69 0.35 9 -9 0 0.63 0.44 10 -9 0 1.6 0.5 10 -9 0 1.5 0.36 10 9 0 2.09 0.29 10 -9 0 1.34 0.35 11 -9 0 -0.02 0.24 11 -9 0 0.23 0.34 11 9 0 -0.15 0.13 11 -9 0 0.16 0.22 12 9 0 0.71 0.16 12 -9 0 0.74 0.24 12 -9 0 0.81 0.22 1 10 0 0.82 0.35 2 10 0 69.25 2.3 2 10 0 68.6 2.62 3 10 0 0.94 0.35 -3 10 0 0.64 0.37 3 10 0 0.27 0.12 4 10 0 46 1.92 -4 10 0 43.68 1.85 5 10 0 2.33 0.4 -5 10 0 1.27 0.42 5 10 0 1.32 0.29 6 10 0 73.15 2.76 6 10 0 74.91 2.59 7 10 0 2.16 0.44 7 10 0 3.01 0.37 8 10 0 58.17 2.07 8 10 0 57.83 2.32 9 10 0 0.04 0.18 -10 10 0 40.57 1.75 10 10 0 41.43 1.48 10 -10 0 39.57 1.57 -11 10 0 1.77 0.38 11 10 0 1.73 0.22 11 -10 0 1.76 0.29 12 10 0 20.64 0.77 12 10 0 20.57 0.78 -12 10 0 22.18 0.98 0 11 0 -0.2 0.16 0 11 0 0.09 0.24 0 11 0 0.31 0.32 1 11 0 0.97 0.38 1 11 0 0.53 0.28 1 11 0 0.73 0.19 -1 11 0 0.88 0.23 -1 11 0 0.73 0.29 -2 11 0 1.23 0.33 2 11 0 1.13 0.18 2 11 0 1.45 0.39 -3 11 0 0.06 0.28 3 11 0 0.09 0.31 -4 11 0 0.66 0.32 -5 11 0 0.81 0.34 5 11 0 0.61 0.27 5 11 0 0.96 0.34 6 11 0 0.7 0.26 -6 11 0 0.6 0.33 6 11 0 0.77 0.34 7 11 0 1.98 0.31 -7 11 0 1.68 0.39 7 11 0 1.94 0.41 8 11 0 1.65 0.38 8 11 0 1.56 0.28 -8 11 0 1.32 0.38 -9 11 0 0.18 0.3 9 11 0 -0.11 0.16 -10 11 0 0.44 0.26 10 11 0 -0.15 0.13 -11 11 0 1.8 0.28 11 11 0 2.06 0.21 0 12 0 44.85 1.59 0 12 0 44.17 1.89 0 12 0 43.6 1.72 1 12 0 7.59 0.74 -1 12 0 8.68 0.78 1 12 0 7.8 0.44 -1 12 0 8.22 0.66 -1 12 0 7.78 0.5 -2 12 0 60.28 2.11 -2 12 0 59.56 2.21 2 12 0 60.61 1.96 2 12 0 59.36 2.35 -3 12 0 20.75 1.04 4 12 0 47.66 1.87 -4 12 0 48.63 1.9 -5 12 0 13.23 0.86 5 12 0 12.65 0.82 6 12 0 39.46 1.58 6 12 0 36.48 1.47 -6 12 0 37.13 1.58 -7 12 0 11.47 0.79 7 12 0 11.53 0.76 7 12 0 11.56 0.64 8 12 0 28.97 1.22 8 12 0 26.64 1.08 -8 12 0 28.39 1.25 9 12 0 5.5 0.39 -9 12 0 5.03 0.46 10 12 0 16.69 0.67 -10 12 0 17.42 0.78 0 13 0 -0.19 0.3 0 13 0 -0.3 0.13 0 13 0 -0.17 0.21 -1 13 0 0.2 0.18 1 13 0 -0.1 0.27 -1 13 0 -0.21 0.23 -1 13 0 0 0.3 1 13 0 -0.03 0.12 -2 13 0 -0.08 0.39 -2 13 0 -0.34 0.25 -2 13 0 -0.21 0.17 -3 13 0 0.45 0.2 -3 13 0 0.55 0.27 -4 13 0 0.11 0.25 4 13 0 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17.89 0.78 14 -4 -3 16.86 1.04 15 -4 3 2.34 0.27 0 -5 3 0 0.76 0 -5 -3 -0.11 0.23 1 -5 3 90.83 5.36 -1 -5 -3 115.87 4.71 -1 -5 3 112.37 5.18 2 -5 3 5.99 1.5 -2 -5 3 4.03 1.17 2 5 3 3.59 0.48 3 -5 3 53.2 3.4 3 5 3 52.57 2 -3 -5 3 58.3 3.6 4 -5 3 2.56 1.02 4 5 3 2.2 0.35 -4 -5 3 2.1 1.08 5 -5 3 31.62 2.59 -5 -5 3 35.94 3.05 5 5 3 33.62 1.38 6 -5 3 1.9 0.93 6 5 3 2.49 0.35 -6 -5 3 2.24 1.21 7 5 3 33.26 1.45 8 5 3 3.07 0.48 9 -5 3 39.56 1.76 9 -5 3 41.74 1.74 9 5 3 42.43 1.68 9 -5 -3 42.54 2.03 9 5 3 42.28 1.83 9 -5 -3 42.98 1.88 10 -5 3 1.29 0.27 10 -5 3 1.65 0.4 10 -5 3 1.19 0.37 10 5 3 1.69 0.28 10 5 3 1.85 0.46 10 -5 -3 1.23 0.35 10 -5 -3 2.34 0.5 10 5 3 1.85 0.36 10 -5 -3 1.61 0.65 11 -5 3 15.28 1.01 11 -5 3 14.45 0.96 11 -5 3 13.56 0.77 11 -5 -3 15.31 1.01 11 -5 -3 15.12 0.93 11 -5 -3 16.12 1.3 11 5 3 12.85 0.98 11 5 3 13.81 0.71 12 -5 3 2.56 0.37 12 -5 3 2.58 0.48 12 -5 3 3.01 0.57 12 -5 -3 2.15 0.38 12 5 3 2.73 0.31 12 -5 -3 2.05 0.47 12 -5 -3 2.92 0.69 13 -5 3 7.89 0.71 13 -5 3 7.3 0.74 13 -5 3 8.22 0.63 13 5 3 8.18 0.47 13 -5 -3 7.43 0.81 13 -5 -3 8.77 0.58 14 -5 3 1.87 0.32 14 -5 3 1.59 0.33 14 -5 -3 1.93 0.24 14 -5 -3 2.46 0.43 14 5 3 2.07 0.23 0 -6 3 40.33 3.01 1 -6 3 61.29 4.16 -1 -6 -3 72.99 3.81 -1 -6 3 77.88 4.2 -2 -6 -3 114.7 5.37 -2 -6 3 121.47 5.76 2 6 3 115.55 4.15 -3 -6 3 22.52 2.31 3 6 3 23.28 1.18 4 -6 3 108.27 6.32 -4 -6 3 133.6 6.42 4 6 3 128.08 4.29 5 -6 3 10.45 1.83 -5 -6 3 12.92 2.05 5 6 3 12.82 0.82 6 6 3 104.77 3.72 7 6 3 19.68 1.09 8 -6 -3 67.32 3.01 8 6 3 74.03 2.79 9 -6 3 2.28 0.46 9 -6 3 2.96 0.39 9 -6 3 2.63 0.47 9 -6 -3 2.45 0.62 9 6 3 2.9 0.45 9 -6 -3 2.96 0.51 9 6 3 2.6 0.53 9 -6 -3 3.05 0.49 9 6 3 2.4 0.33 10 -6 3 62.57 2.44 10 -6 3 61.58 2.25 10 -6 3 60.38 2.36 10 6 3 61.23 2.33 10 6 3 61.64 2.16 10 -6 -3 59.56 2.38 10 -6 -3 56.21 2.65 10 6 3 60.75 2.55 10 -6 -3 57.1 2.34 11 -6 3 5.58 0.56 11 -6 3 5.82 0.7 11 -6 3 5.03 0.59 11 6 3 5.04 0.72 11 -6 -3 4.38 0.76 11 6 3 5.92 0.49 11 -6 -3 5.8 0.61 11 -6 -3 4.97 0.61 12 -6 3 36.63 1.75 12 -6 3 34.87 1.56 12 -6 3 37.39 1.56 12 6 3 35.31 1.38 12 -6 -3 36.9 1.5 12 -6 -3 35.11 1.81 12 -6 -3 36.54 1.62 13 -6 3 0.49 0.41 13 -6 3 0.56 0.29 13 -6 3 0.35 0.27 13 6 3 0.82 0.2 13 -6 -3 0.47 0.36 14 -6 3 21.13 0.95 14 -6 3 20.34 1.08 14 -6 3 22.78 0.95 14 6 3 22.47 0.87 14 -6 -3 20.17 0.83 0 -7 3 10.07 1.69 1 -7 3 22.18 2.42 -1 -7 3 25.02 2.42 1 7 3 24.49 1.17 -2 -7 -3 4.2 1.24 2 -7 3 3.88 1.43 2 7 3 3.33 0.51 -2 -7 3 4.67 1.29 -3 -7 -3 31.37 2.75 -3 -7 3 33.59 2.91 3 7 3 31.06 1.62 -4 -7 -3 22.25 2.42 4 7 3 24.39 1.39 -4 -7 3 23.37 2.61 5 7 3 34.73 1.71 6 7 3 14.32 1.04 7 7 3 18.52 1.23 8 -7 3 7.55 0.68 8 -7 3 7.9 0.75 8 -7 -3 8.2 0.76 8 -7 -3 7.97 0.72 8 7 3 9.3 0.94 8 7 3 8.4 0.77 8 -7 -3 6 0.82 8 7 3 8.2 0.56 8 7 3 9.38 0.87 9 -7 3 22.85 1.23 9 -7 3 25.2 1.27 9 -7 3 26.21 1.39 9 7 -3 26.63 1.06 9 -7 -3 27.44 1.33 9 7 3 27.47 1.59 9 -7 -3 27.75 1.32 9 7 3 26.26 1.35 9 7 3 24.66 1.09 9 -7 -3 25.49 1.58 10 7 -3 8.92 0.52 10 -7 3 7.97 0.73 10 -7 3 7.07 0.8 10 -7 3 8.67 0.79 10 -7 -3 8.24 0.76 10 -7 -3 9.58 1.04 10 7 3 9.65 0.9 10 7 3 8.72 0.58 10 -7 -3 8.57 0.78 10 7 3 8.5 0.98 11 -7 3 8.28 0.89 11 7 -3 8.54 0.47 11 -7 3 7.28 0.73 11 -7 3 6.86 0.68 11 -7 -3 9 0.96 11 7 3 6.87 0.54 11 -7 -3 9.11 0.72 11 -7 -3 8.13 0.75 12 -7 3 4.75 0.51 12 -7 3 5.76 0.73 12 -7 3 5.56 0.6 12 7 -3 5.08 0.35 12 -7 -3 5.85 0.58 12 -7 -3 4.07 0.61 12 -7 -3 5.52 0.53 12 7 3 5.11 0.43 13 -7 3 6.63 0.57 13 -7 3 6.52 0.54 13 -7 3 3.92 0.54 13 -7 -3 6.87 0.46 13 7 3 5.8 0.42 14 -7 3 2.33 0.29 14 -7 -3 2.71 0.24 0 -8 3 72.18 4.56 1 -8 3 71.22 4.59 -1 -8 3 81.77 4.78 1 8 3 76.85 2.82 2 -8 3 56.96 4.2 2 8 3 67.6 2.49 -3 -8 -3 43.23 3.83 3 8 3 43.36 1.91 4 8 3 50.89 2.28 5 8 3 47.67 2.34 6 8 3 39.65 2.23 7 8 -3 42.28 1.93 7 -8 3 41.42 1.7 7 8 3 51.22 2.46 7 8 3 40.6 1.88 7 -8 -3 38.89 1.96 7 -8 -3 39.21 1.69 8 -8 3 20.36 1.26 8 8 -3 19.88 0.92 8 -8 3 19.74 1.06 8 -8 3 20.34 1.18 8 8 -3 21.63 1.91 8 8 3 20.04 1.27 8 -8 -3 18.13 1.05 8 -8 -3 20.8 1.38 8 8 3 20.74 0.94 8 8 3 27.85 1.51 8 8 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0.9 7 9 -3 7.29 0.55 7 9 3 8.06 0.79 7 -9 -3 7.55 0.96 7 9 3 7.05 0.56 7 9 3 6.61 0.91 7 9 3 6 0.7 8 9 -3 19.63 0.89 8 9 -3 22.14 1.35 8 9 3 19.69 1.14 8 9 3 19.25 1.41 8 -9 -3 18.87 1.02 8 -9 -3 17.92 1 8 9 3 16.72 1.2 8 9 3 18.14 0.9 9 -9 3 2.78 0.43 9 9 -3 3.11 0.35 9 -9 3 2.5 0.55 9 9 3 2.23 0.32 9 -9 -3 3.03 0.43 9 -9 -3 2.88 0.45 9 9 3 3.14 0.49 9 9 3 2.69 0.63 10 -9 3 6.13 0.64 10 -9 3 9.37 0.87 10 9 -3 8.86 0.51 -10 9 3 8.56 0.83 10 -9 3 7.83 0.65 10 9 3 7.78 0.54 10 -9 -3 8.31 0.65 11 9 -3 3.04 0.28 11 -9 3 2.15 0.34 11 -9 3 2.36 0.46 11 -9 3 2.44 0.38 -11 9 3 3.88 0.49 11 9 3 2.31 0.28 11 -9 -3 2.8 0.35 12 -9 3 4.92 0.46 12 9 -3 5.92 0.33 12 -9 3 4.03 0.47 -12 9 3 6.63 0.53 12 -9 3 4.53 0.45 12 -9 -3 6.01 0.42 12 9 3 5.56 0.36 0 10 3 1.69 0.38 0 10 3 1.83 0.41 0 10 -3 1.59 0.24 1 10 -3 89.07 2.92 1 10 3 89.22 3.28 -1 10 -3 89.16 3.02 -2 10 3 6.52 0.59 2 10 -3 6.8 0.38 2 10 3 7.27 0.69 2 10 3 6.7 0.44 2 10 3 8.16 0.84 -3 10 3 83.48 3.06 3 10 3 90.17 2.8 3 10 3 86.03 3.22 3 10 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11 -4 4 2.79 0.48 11 -4 4 2.76 0.52 11 -4 4 2.28 0.31 11 4 4 2.25 0.28 11 -4 -4 2.51 0.42 11 -4 -4 2.15 0.49 11 4 4 1.7 0.42 11 -4 -4 3.92 0.78 12 -4 4 2.07 0.45 12 -4 4 1.7 0.29 12 -4 4 2.51 0.51 12 4 4 1.45 0.23 12 -4 -4 1.41 0.32 12 -4 -4 1.07 0.41 12 -4 -4 1.78 0.58 13 -4 4 1.78 0.41 13 -4 4 1.38 0.4 13 -4 4 1.93 0.31 13 -4 -4 3.02 0.6 13 4 4 1.6 0.23 13 -4 -4 2.38 0.32 14 -4 4 1.4 0.35 14 -4 4 1.33 0.4 14 -4 4 1.57 0.28 14 4 4 1.71 0.21 14 -4 -4 1.28 0.21 15 -4 4 0.8 0.22 0 -5 4 145.92 6.77 1 -5 4 3.72 1.35 1 5 4 5.31 0.58 -1 -5 4 4.99 1.31 2 -5 4 271.05 11.22 -2 -5 4 309.1 11.19 2 5 4 285.14 9.21 3 -5 4 9.29 1.55 -3 -5 4 9.48 1.62 3 5 4 8.8 0.6 4 -5 4 214.77 9.09 -4 -5 4 233.79 9.45 4 5 4 222.29 7.21 5 -5 4 3.74 1.16 -5 -5 4 3.8 1.37 5 5 4 2.98 0.4 -6 -5 4 117.45 6.5 6 5 4 127.78 4.21 7 5 4 0.16 0.25 8 5 4 136.14 4.71 9 -5 4 1.15 0.39 9 -5 4 1.03 0.35 9 5 4 0.94 0.39 9 -5 -4 0.52 0.33 9 5 4 0.63 0.26 9 -5 -4 1.01 0.57 10 -5 4 90.64 3.29 10 -5 4 89.71 3.09 10 -5 4 93.96 3.29 10 5 4 90.91 3.41 10 5 4 89.82 3.06 10 5 4 88.08 3.19 10 -5 -4 89.61 3.63 10 -5 -4 89.7 3.25 10 -5 -4 90.1 3.34 11 -5 4 0.52 0.24 11 -5 4 0.57 0.36 11 -5 4 0.67 0.36 11 5 4 0.51 0.21 11 -5 -4 0.91 0.55 11 5 4 0.61 0.39 11 -5 -4 0.81 0.31 11 -5 -4 0.61 0.37 12 -5 4 54.83 1.95 12 -5 4 50.91 2.07 12 -5 4 49.91 2.13 12 5 4 51.05 1.84 12 -5 -4 49.28 2.33 12 -5 -4 51.15 2.12 12 -5 -4 51.02 1.94 13 -5 4 1.09 0.4 13 -5 4 0.74 0.31 13 -5 4 0.93 0.28 13 5 4 1.03 0.2 13 -5 -4 1.31 0.44 13 -5 -4 0.65 0.21 14 -5 4 29.81 1.22 14 -5 4 29.25 1.23 14 -5 4 30.66 1.43 14 5 4 28.37 1.08 14 -5 -4 28.6 1.08 0 -6 4 0.53 0.86 -1 -6 -4 47.89 3.95 1 -6 4 34.39 3.14 1 6 4 39.68 1.69 -1 -6 4 42.62 3.13 -2 -6 -4 1.21 0.68 2 -6 4 0.58 1.14 2 6 4 1 0.37 -2 -6 4 1.1 0.89 3 -6 4 13.91 2.25 3 6 4 18.39 1.01 -3 -6 4 21.36 2.26 4 -6 4 1.37 1.08 4 6 4 2.29 0.42 -4 -6 4 2.55 1.1 5 -6 4 17.87 2.38 5 6 4 17.69 1.02 -5 -6 4 20.52 2.47 6 6 4 5.33 0.57 7 6 4 7.48 0.71 8 -6 4 1.1 0.35 8 6 4 0.86 0.37 8 6 4 0.59 0.27 8 -6 -4 1.07 0.5 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1.35 8 -6 6 1.69 0.35 8 -6 6 1.25 0.35 8 -6 -6 0.88 0.36 8 6 6 2.03 0.49 8 -6 -6 2.04 0.57 8 -6 -6 1.35 0.34 8 6 6 1.47 0.37 8 6 6 1.26 0.29 9 6 -6 17.55 0.84 9 -6 6 21.18 1.09 9 -6 6 19.85 1.1 9 -6 6 21.43 1.02 9 6 6 20.67 0.98 9 -6 -6 18.85 1.02 9 6 6 21.63 1.14 9 6 6 19.88 1.27 9 -6 -6 19.79 1.15 9 -6 -6 17.48 1.31 10 -6 6 3.56 0.49 10 -6 6 3.57 0.44 10 6 -6 4.12 0.37 10 -6 6 3.77 0.52 10 6 6 4.47 0.45 10 6 6 2.81 0.59 10 -6 -6 3.44 0.44 10 6 6 4.22 0.55 10 -6 -6 3.05 0.64 11 -6 6 17.65 0.96 11 -6 6 17.6 1.05 11 6 -6 15.51 0.73 11 -6 6 18.08 1.02 11 -6 -6 16.64 0.89 11 6 6 18.6 0.89 12 -6 6 1.65 0.41 12 -6 6 1.47 0.34 12 -6 6 2.23 0.42 12 6 6 1.95 0.3 12 -6 -6 2.15 0.31 13 -6 6 8.35 0.73 13 -6 6 8.57 0.6 13 -6 6 7.74 0.61 13 -6 -6 7.26 0.46 13 6 6 8.59 0.53 14 -6 -6 0.28 0.17 14 6 6 0.49 0.2 0 7 6 111.36 3.77 0 -7 6 99.89 5.91 1 -7 6 18.67 2.58 -1 -7 6 20.22 2.5 1 7 6 22.44 1.15 2 7 6 169.14 5.81 3 7 6 51.74 2.23 4 7 6 101.33 3.78 5 7 6 41.75 1.95 6 7 6 59.11 2.5 7 -7 6 18.66 1.01 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0.52 -7 8 6 3.48 0.51 7 8 -6 3.65 0.42 7 8 6 4.55 0.46 -7 8 -6 4.47 0.73 7 -8 -6 3.97 0.5 7 8 6 3.32 0.69 7 8 6 3.21 0.63 -8 8 6 17.66 1.09 8 8 -6 15.79 0.83 8 -8 6 18.96 0.99 8 -8 -6 17.29 0.97 8 8 6 17.55 1.44 -8 8 -6 14.87 1.19 8 8 6 16.28 1.3 8 8 6 18.44 0.9 9 -8 6 8.54 0.71 -9 8 6 9.52 0.89 9 8 -6 8.29 0.57 9 -8 -6 8.72 0.71 9 8 6 7.14 0.85 -9 8 -6 9.31 1.32 9 8 6 9.61 1.21 9 8 6 8.52 0.63 10 8 -6 8.1 0.51 10 -8 6 7.75 0.67 10 -8 -6 7.52 0.6 10 8 6 9.62 0.6 10 8 6 7.04 0.8 11 -8 6 6.78 0.69 11 -8 6 9.1 1.12 11 8 -6 6.35 0.41 11 -8 6 7.53 0.61 11 8 6 7.63 0.52 11 -8 -6 6.74 0.52 12 8 -6 4.38 0.28 12 -8 6 4.12 0.44 12 -8 6 4.91 0.46 12 -8 6 4.16 0.49 12 -8 -6 3.92 0.37 12 8 6 4.57 0.37 13 -8 -6 2.22 0.24 13 8 6 2.85 0.25 0 9 6 7.41 0.71 -1 9 6 139.63 4.77 1 9 6 135.19 4.79 2 9 -6 4.66 0.29 2 9 6 4.48 0.39 2 9 6 3.52 0.58 -3 9 6 115.38 4.35 3 9 6 112.05 3.98 3 9 6 116.19 3.77 3 9 6 119.88 4.23 -4 9 6 11.54 0.82 4 9 6 12.89 0.99 4 9 6 12.35 0.88 -4 9 -6 12.74 1.06 4 9 6 13.68 0.56 5 9 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1.91 0.29 -1 10 -6 2.4 0.42 -2 10 6 17.21 1.06 2 10 -6 17.74 0.65 -2 10 6 16.28 0.94 -2 10 -6 17.25 0.83 2 10 6 17.47 0.95 2 10 6 17.74 1.1 2 10 6 17.66 0.78 -2 10 -6 16.84 1.01 -3 10 6 1.89 0.37 3 10 6 2.05 0.48 -3 10 -6 2.27 0.45 3 10 6 1.66 0.35 3 10 6 1.94 0.23 4 10 -6 26.01 1.17 -4 10 6 25.43 1.22 4 10 6 25.05 1.21 4 10 6 25.11 0.89 -4 10 -6 23.53 1.26 4 10 6 23.7 1.18 4 10 6 26.09 1.41 5 10 -6 1.22 0.32 -5 10 6 1.58 0.37 5 10 6 2.43 0.55 5 10 6 2.31 0.42 5 10 6 1.89 0.41 -5 10 -6 2.07 0.47 -6 10 6 20.56 1.11 6 10 -6 21.86 1.03 -6 10 -6 21.27 1.2 6 10 6 21.93 1.31 6 10 6 20.75 1.14 6 10 6 20.88 1.13 -7 10 6 3.05 0.44 7 10 -6 3.85 0.42 7 10 6 4.21 0.52 7 10 6 3.75 0.59 7 10 6 4.35 0.44 -7 10 -6 4.46 0.58 8 10 -6 10.05 0.63 -8 10 6 10.29 0.77 8 10 6 11 0.65 8 10 6 11.14 0.63 8 10 6 10.17 0.76 -9 10 6 1.44 0.34 9 10 -6 1.27 0.23 9 10 6 1.07 0.23 9 10 6 0.79 0.28 -10 10 6 8.13 0.58 10 10 -6 7.85 0.46 10 10 6 7.31 0.55 10 -10 -6 8.12 0.52 10 10 6 8.89 0.51 11 -10 6 0.2 0.24 11 10 -6 0.61 0.14 -11 10 -6 0.39 0.27 11 10 6 0.47 0.15 11 -10 -6 0.41 0.16 0 11 -6 0.77 0.2 0 11 6 0.67 0.29 0 11 6 1.24 0.42 0 11 6 0.77 0.23 -1 11 6 47.19 1.74 -1 11 6 46.64 1.85 1 11 -6 46.84 1.6 -1 11 6 45.75 2.01 1 11 6 47.5 2.03 -1 11 -6 49.35 1.92 -1 11 -6 47.37 1.71 1 11 6 46.79 1.86 1 11 6 49.41 1.71 -2 11 6 7.14 0.73 -2 11 6 6.35 0.62 2 11 6 6.57 0.42 2 11 6 6.49 0.71 2 11 6 4.44 0.48 -2 11 -6 6.15 0.63 -2 11 -6 6.44 0.48 -3 11 6 36.74 1.74 -3 11 6 38.78 1.62 3 11 6 40.12 1.35 -3 11 -6 39.91 1.67 3 11 6 39.61 1.81 3 11 6 39.97 1.63 -3 11 -6 41.43 1.53 -4 11 6 5.63 0.55 4 11 6 5.02 0.52 4 11 6 4.06 0.6 4 11 6 5.52 0.54 -4 11 -6 3.5 0.47 5 11 -6 32.29 1.4 -5 11 6 34.71 1.46 5 11 -6 35.75 1.4 -5 11 -6 34.51 1.51 5 11 6 32.77 1.62 5 11 6 33.42 1.44 5 11 6 34.51 1.46 -6 11 6 2.39 0.39 6 11 -6 3.14 0.37 -6 11 -6 2.47 0.41 6 11 6 2.56 0.38 6 11 6 2.92 0.44 -7 11 6 35.99 1.47 7 11 -6 35.18 1.38 7 11 6 34.79 1.45 8 11 -6 2.15 0.28 -8 11 6 2.04 0.35 8 11 6 2.18 0.34 8 11 6 1.32 0.33 9 11 -6 21.12 0.86 -9 11 6 21.98 0.94 9 11 6 19.9 0.91 -9 11 -6 22.32 1.36 9 11 6 20.71 0.86 10 11 -6 1.62 0.2 10 11 6 1.42 0.19 0 12 6 8.1 0.75 0 12 6 8.77 0.69 0 12 6 9.08 0.53 0 12 -6 9.77 0.47 -1 12 6 1.64 0.26 -1 12 6 2.16 0.39 1 12 -6 1.72 0.14 -1 12 6 1.46 0.39 1 12 6 1.87 0.35 1 12 6 1.75 0.24 1 12 6 2.15 0.47 -1 12 -6 1.74 0.23 -2 12 6 6.11 0.67 -2 12 6 6.59 0.48 -2 12 6 4.67 0.49 2 12 6 6.53 0.68 2 12 6 6.69 0.37 -2 12 -6 7.42 0.48 2 12 6 7.29 0.62 -3 12 6 1.19 0.32 -3 12 6 1.31 0.38 3 12 6 1.92 0.44 -3 12 -6 1.85 0.35 -3 12 -6 1.48 0.27 3 12 6 1.68 0.35 -4 12 6 6.66 0.59 -4 12 -6 6.77 0.5 4 12 6 6.69 0.62 4 12 6 6.16 0.57 -4 12 -6 7.01 0.62 -5 12 6 1.51 0.33 5 12 -6 1.25 0.28 5 12 6 1.41 0.31 5 12 6 1.76 0.33 -5 12 -6 1.26 0.3 6 12 -6 9.42 0.6 -6 12 6 9.83 0.68 6 12 6 10.24 0.64 7 12 -6 1.11 0.24 -7 12 6 1.13 0.3 7 12 6 1.12 0.26 -8 12 6 7.3 0.52 8 12 -6 6.91 0.44 8 12 6 7.65 0.49 9 12 -6 1.67 0.2 0 13 6 14.13 0.63 0 13 6 14.25 0.8 0 13 -6 13.55 0.51 -1 13 6 18.75 0.91 -1 13 6 16.62 0.74 1 13 6 16.64 0.68 -1 13 -6 17.31 0.69 1 13 6 18.64 0.9 -2 13 6 18.19 0.92 -2 13 6 17.51 0.79 -2 13 -6 17.87 0.74 2 13 6 18.43 0.91 -3 13 6 17.93 0.78 -3 13 6 17.16 0.89 -3 13 -6 16.83 0.73 3 13 6 16.91 0.85 4 13 -6 10.5 0.64 -4 13 6 9.17 0.67 4 13 6 9.69 0.61 -4 13 -6 10.38 0.54 4 13 6 10.07 0.65 5 13 -6 13.47 0.7 -5 13 6 13.96 0.75 -5 13 -6 13.39 0.62 5 13 6 13.04 0.7 5 13 6 12.94 0.7 -6 13 6 13.56 0.7 6 13 6 11.34 0.62 -6 13 -6 12.03 0.57 7 13 -6 9.87 0.51 -7 13 6 10.58 0.56 7 13 6 8.97 0.51 0 14 6 1.55 0.29 0 14 6 1.66 0.16 -1 14 6 6.35 0.36 -1 14 6 7.32 0.53 1 14 6 6.98 0.52 -2 14 6 3.41 0.36 -2 14 6 2.73 0.25 2 14 6 3.19 0.34 -2 14 -6 3.14 0.23 -3 14 6 7.72 0.56 -3 14 6 8.25 0.43 3 14 -6 7.53 0.53 3 14 6 8.38 0.52 -3 14 -6 7.51 0.38 4 14 -6 1.01 0.23 -4 14 6 1.36 0.26 -4 14 6 1.15 0.18 4 14 6 1.45 0.23 -4 14 -6 1.6 0.18 -5 14 6 5.23 0.41 5 14 -6 4.93 0.38 5 14 6 4.86 0.38 -5 14 -6 5.75 0.31 -6 14 6 2.98 0.4 0 15 6 19.38 0.8 -1 15 6 0.82 0.2 1 15 6 0.78 0.2 2 15 -6 19.92 0.8 -2 15 6 19.98 0.8 -2 15 6 18.72 0.72 2 15 6 19.86 0.78 -3 15 6 1.11 0.23 3 15 -6 0.62 0.17 0 0 7 0.1 0.33 -1 0 7 119.35 4.28 1 0 7 117.98 4.55 3 0 -7 80.38 2.71 4 0 7 0.22 0.13 4 0 -7 0.41 0.19 5 0 -7 142.51 4.63 5 0 7 138.98 4.57 6 0 7 0.2 0.18 6 0 -7 0.16 0.2 7 0 7 26.67 1.19 7 0 -7 28.69 1.24 8 0 -7 7.26 0.63 8 0 7 7.3 0.59 9 0 -7 60.54 2.3 9 0 7 58.37 2.27 9 0 7 55.02 2.13 10 0 -7 4.06 0.57 10 0 7 3.75 0.55 10 0 7 2.94 0.32 10 0 7 3.96 0.47 11 0 7 31.58 1.4 11 0 7 31.69 1.53 11 0 7 30.51 1.21 12 0 7 0.25 0.18 12 0 7 0.57 0.32 13 0 7 17.26 0.76 13 0 7 15.94 0.95 14 0 7 1.55 0.22 14 0 7 1.1 0.33 0 -1 7 212.85 7.49 1 -1 7 5.74 0.9 -1 -1 7 6.32 0.81 2 -1 7 165.1 6.36 2 1 -7 155.97 5.38 -2 -1 7 183.77 6.14 3 -1 7 23.87 1.8 3 1 -7 23.28 0.98 4 -1 7 110.37 3.58 4 1 -7 108.52 3.66 4 1 7 111.36 3.6 5 -1 7 24.48 1.01 5 1 -7 24.42 1.06 5 1 7 24.64 1.02 6 -1 7 84.82 2.95 6 1 -7 85.49 3 6 1 7 88.57 2.97 7 1 -7 1.84 0.35 7 -1 7 1.74 0.32 7 1 7 1.98 0.35 8 -1 7 98.25 3.43 8 1 -7 94.58 3.43 8 1 7 98.96 3.43 9 1 -7 3.85 0.51 9 -1 7 3.02 0.46 9 -1 7 4.17 0.47 9 1 7 4.1 0.51 9 -1 -7 3.66 0.5 9 1 7 5.22 0.52 10 -1 7 47.16 2.02 10 -1 7 46.39 1.87 10 -1 7 52.44 2.3 10 -1 7 48.25 1.73 10 1 7 47.33 1.89 10 1 7 47.74 1.71 10 -1 -7 46.83 2.02 11 -1 7 2.5 0.3 11 -1 7 4.38 0.74 11 -1 7 3.12 0.46 11 -1 7 2.33 0.46 11 1 7 2.77 0.31 11 1 7 3.63 0.48 11 1 7 2.52 0.44 11 -1 -7 3.52 0.54 12 -1 7 30.54 1.41 12 -1 7 31.19 1.23 12 1 7 30.89 1.43 12 1 7 32.02 1.22 13 -1 7 1.82 0.36 13 -1 7 2.31 0.28 13 1 7 2.31 0.28 13 1 7 1.69 0.38 14 -1 7 15.95 0.89 14 -1 7 16.94 0.72 14 1 7 15.47 0.95 14 1 7 15.74 0.7 0 -2 7 183.28 6.88 1 2 -7 98.6 3.51 1 -2 7 107.97 4.5 -1 -2 7 110.93 4.51 2 -2 7 56.34 2.96 2 2 -7 51.84 1.98 -2 -2 7 60.6 2.99 3 -2 7 125.54 5.48 3 2 -7 126.13 4.25 -3 -2 7 137.32 5.47 4 -2 7 13.38 1.53 4 -2 7 13.12 0.62 4 2 -7 14.52 0.72 4 2 7 12.59 0.64 5 2 -7 96.29 3.27 5 -2 7 93.8 3.19 5 2 7 96.41 3.21 6 -2 7 33.82 1.38 6 2 -7 35.9 1.45 6 2 7 35.02 1.4 7 -2 7 23.82 1.1 7 2 -7 24.89 1.15 7 2 7 23.32 1.09 8 -2 7 13.82 0.83 8 2 -7 14.34 0.88 8 2 7 14.21 0.84 9 2 -7 20.16 1.09 9 -2 7 18.77 1.07 9 -2 7 18.86 0.96 9 2 7 18.94 0.98 9 2 7 20.31 1.09 10 -2 7 8.9 0.89 10 -2 7 9.66 0.81 10 -2 7 9.77 0.71 10 -2 7 10.39 0.59 10 2 7 9.71 0.56 10 2 7 10.69 0.82 10 -2 -7 11.18 0.86 10 2 7 10.01 0.73 11 -2 7 18.68 1.03 11 -2 7 20.3 0.89 11 -2 7 21.17 1.35 11 2 7 19.97 1.07 11 -2 -7 16.7 1.08 11 2 7 19.23 1.14 11 -2 -7 20.02 1.18 11 2 7 19.92 0.87 12 -2 7 7.64 0.87 12 -2 7 8.46 0.71 12 -2 7 7.76 0.54 12 -2 -7 8 0.5 12 2 7 8.84 0.53 12 2 7 8.9 0.77 13 -2 7 10.75 0.58 13 -2 7 9.98 0.73 13 -2 7 11.58 1.07 13 -2 -7 8.52 0.51 13 2 7 8.95 0.78 13 2 7 9.38 0.54 14 -2 7 4.22 0.37 14 -2 7 4.13 0.48 14 2 7 3.97 0.57 14 2 7 4.13 0.33 0 -3 7 86.85 4.19 1 3 -7 82.98 3.05 1 -3 7 91.62 4.27 -1 -3 7 92.6 4.37 2 -3 7 186.28 7.38 2 3 -7 180.37 5.99 -2 -3 7 188.48 7.52 3 -3 7 69.43 3.69 3 3 -7 65.74 2.41 -3 -3 7 69.64 3.84 3 3 7 67.85 2.33 4 -3 7 49.57 3.16 4 3 -7 47.66 1.85 4 -3 7 48.84 1.77 4 3 7 48.33 1.78 -4 -3 7 56.14 4.32 5 -3 7 88.04 2.98 5 -3 7 86.15 4.65 5 3 -7 85.03 3.04 5 3 7 89.01 3 6 -3 7 56.35 2.08 6 3 -7 56.12 2.13 6 3 7 56.12 2.08 7 3 -7 56.99 2.26 7 -3 7 58.85 2.23 7 3 7 61.75 2.25 8 -3 7 29.7 1.36 8 3 -7 27.8 1.36 8 3 7 29.55 1.36 9 -3 7 34.6 1.44 9 -3 7 33.1 1.57 9 -3 7 34.86 1.59 9 3 7 35.64 1.6 9 3 7 34.75 1.44 9 3 7 33.72 1.48 10 -3 7 18 0.97 10 -3 7 16.89 1.09 10 -3 7 17.44 0.84 10 3 7 17.52 1.02 10 3 7 17.4 0.81 10 -3 -7 18.21 0.91 10 3 7 17.95 1.07 11 -3 7 33.36 1.3 11 -3 7 31.8 1.6 11 -3 7 33.59 1.46 11 3 7 30.74 1.57 11 -3 -7 30.02 1.56 11 3 7 33.49 1.28 11 -3 -7 30.56 1.31 11 3 7 34.87 1.55 12 -3 7 9.83 0.62 12 -3 7 10.28 0.93 12 -3 7 10.75 0.8 12 3 7 10.57 0.6 12 -3 -7 10.41 0.62 12 3 7 11.6 0.91 13 -3 7 10.39 0.6 13 -3 7 11.43 0.93 13 -3 7 10.01 0.74 13 -3 -7 9.49 0.54 13 3 7 11.08 0.93 13 3 7 11.21 0.58 14 -3 7 5.8 0.44 14 -3 7 7.07 0.7 14 -3 7 5.73 0.57 14 -3 -7 4.94 0.3 14 3 7 5.53 0.38 14 3 7 5.71 0.61 0 -4 7 152.38 6.78 1 -4 7 11.19 1.61 1 4 7 9.63 0.57 -1 -4 7 9.29 1.58 2 4 -7 105.9 3.75 2 -4 7 111.71 5.33 2 4 7 104.74 3.62 -2 -4 7 116.28 5.64 3 -4 7 22.75 2.19 3 4 -7 22.98 1.1 3 4 7 24.3 1.04 -3 -4 7 23.59 2.38 4 -4 7 37.65 2.91 4 4 -7 41.32 1.63 -4 -4 7 40.78 3.14 4 4 7 39.25 1.55 5 4 -7 6 0.54 5 -4 7 5.33 1.4 5 4 7 6.34 0.51 6 4 -7 73.55 2.68 6 4 7 70.88 2.62 7 4 -7 6.29 0.61 7 4 7 5.74 0.55 8 4 7 49.54 2.01 8 4 7 45.23 1.88 8 4 7 52.15 2.3 9 -4 7 10.52 0.82 9 -4 7 10.34 0.72 9 -4 7 10.57 0.64 9 4 7 11.51 0.84 9 -4 -7 10.99 0.71 9 4 7 12.29 0.85 9 -4 -7 9.27 1 9 4 7 11.36 0.74 9 4 7 9.98 0.62 10 -4 7 44.55 1.81 10 -4 7 43.33 1.69 10 -4 7 43.04 1.91 10 4 7 46.7 1.95 10 4 7 44 1.67 10 -4 -7 45.85 1.75 10 -4 -7 46.91 2.17 10 4 7 45.09 1.99 11 -4 7 2.42 0.43 11 -4 7 2.43 0.34 11 -4 7 2.22 0.49 11 4 7 1.85 0.43 11 4 7 2.03 0.3 11 -4 -7 2.49 0.36 11 4 7 2.45 0.55 12 -4 7 18.79 0.92 12 -4 7 19.73 1.14 12 -4 7 19.54 1.07 12 4 7 22.77 1.34 12 -4 -7 20.38 0.92 12 4 7 20.25 0.9 13 -4 7 2.52 0.44 13 -4 7 1.7 0.29 13 -4 7 2 0.39 13 4 7 2.32 0.28 13 -4 -7 2.26 0.28 13 4 7 2.08 0.45 14 -4 7 9.71 0.66 14 -4 7 8.87 0.56 14 -4 7 9.92 0.7 14 -4 -7 9.73 0.45 14 4 7 8.87 0.5 0 5 7 3.03 0.43 0 -5 7 2.69 1.2 1 -5 7 215.59 9.58 1 5 7 226.43 7.31 -1 -5 7 235.89 9.89 2 -5 7 7.57 1.7 -2 -5 7 8.39 1.81 2 5 7 7.16 0.55 3 -5 7 134.98 6.78 -3 -5 7 139.44 6.85 3 5 7 142.91 4.67 4 -5 7 7.73 1.7 4 5 -7 8.89 0.69 4 5 7 9.84 0.65 -4 -5 7 8.75 1.82 5 5 -7 139.61 4.73 5 5 7 145.6 4.69 -5 -5 7 125.78 6.91 6 5 -7 1.55 0.4 6 5 7 1.21 0.35 7 5 7 86.22 3.17 8 -5 7 0.7 0.28 8 -5 7 0.98 0.31 8 5 7 1.31 0.4 8 -5 -7 0.35 0.45 8 5 7 0.44 0.27 8 5 7 1.01 0.35 9 -5 7 40.07 1.58 9 -5 7 39.96 1.75 9 -5 7 41.29 1.68 9 -5 -7 39.04 1.99 9 5 7 42.46 1.58 9 -5 -7 38.57 1.63 9 5 7 42.02 1.9 9 5 7 41.59 1.69 9 5 7 40.26 1.86 10 -5 7 2.8 0.37 10 -5 7 2.72 0.48 10 -5 7 4.43 0.55 10 5 7 3.51 0.51 10 5 7 3.51 0.66 10 5 7 3.52 0.61 10 -5 -7 3.42 0.43 10 5 7 3.62 0.41 11 -5 7 31.05 1.5 11 -5 7 34.19 1.39 11 -5 7 31.67 1.48 11 5 7 38.96 1.76 11 -5 -7 32.41 1.36 11 5 7 32.71 1.34 12 -5 7 0.19 0.3 12 -5 7 0.57 0.25 12 -5 7 0.55 0.31 12 5 7 0.7 0.22 12 -5 -7 0.6 0.22 13 -5 7 19.47 1.04 13 -5 7 21.42 0.98 13 -5 7 20.86 1 13 5 7 20.3 0.88 13 -5 -7 19.74 0.85 14 -5 7 0.56 0.21 14 -5 -7 0.24 0.13 14 5 7 0.07 0.15 0 6 7 75.12 2.69 0 -6 7 65.32 4.68 1 -6 7 2.6 1.34 -1 -6 7 2.29 1.2 1 6 7 2.47 0.45 2 -6 7 83.15 5.63 2 6 7 107.22 3.57 -2 -6 7 105.07 5.8 3 -6 7 8.9 2.08 -3 -6 7 13.98 2.05 3 6 7 13.05 0.83 4 6 7 73.59 2.77 5 6 7 5.22 0.63 6 6 7 33.56 1.56 7 6 7 10.13 0.86 7 6 7 12.83 1.09 7 6 7 10.37 0.76 8 -6 7 31.74 1.49 8 6 -7 34 1.29 8 6 7 33.07 1.39 8 -6 -7 34.06 1.44 8 6 7 31.57 1.63 8 6 7 32.15 1.5 8 6 7 42.68 1.94 9 -6 7 3.03 0.44 9 -6 7 3.18 0.44 9 6 -7 3.07 0.34 9 -6 7 3.01 0.47 9 6 7 3.09 0.61 9 6 7 2.96 0.39 9 6 7 2.5 0.45 9 6 7 3.48 0.63 9 -6 -7 3.2 0.43 10 -6 7 24.07 1.16 10 -6 7 24.58 1.24 10 -6 7 22.48 1.22 10 6 -7 25.63 1.02 10 6 7 23.04 1.43 10 6 7 26.74 1.66 10 -6 -7 25.8 1.15 10 6 7 25.25 1.13 10 6 7 24.2 1.3 11 -6 7 3.51 0.52 11 6 -7 3.1 0.3 11 -6 7 3.07 0.42 11 -6 7 2.58 0.44 11 -6 -7 2.45 0.35 11 6 7 3.14 0.39 -11 6 -7 3.63 0.6 12 -6 7 9.34 0.79 12 -6 7 9.51 0.73 12 -6 7 9.28 0.7 12 6 7 10.22 0.63 12 -6 -7 11.52 0.61 13 -6 7 1.99 0.4 13 -6 7 1.7 0.32 13 -6 7 1.8 0.32 13 6 7 1.88 0.28 13 -6 -7 1.69 0.23 0 7 7 29.48 1.39 -1 7 7 60.59 2.25 1 7 7 53.57 2.29 2 7 7 35.02 1.67 3 7 7 57.31 2.38 4 7 7 23.04 1.3 5 7 7 48.26 2.16 6 7 7 10.34 0.96 6 7 7 11.15 0.93 6 7 7 9.29 0.82 7 -7 7 27.78 1.32 7 7 -7 29.57 1.22 7 7 7 29.91 1.27 7 7 7 29.47 1.61 7 -7 -7 28.77 1.31 7 7 7 28.92 1.45 -7 7 -7 29.36 1.57 7 7 7 31.96 1.51 8 7 -7 19.58 0.95 8 -7 7 21.31 1.12 8 -7 -7 21.17 1.07 8 7 7 22.76 1.04 -8 7 -7 19.84 1.3 8 7 7 22.14 1.41 8 7 7 21.83 1.24 9 -7 7 38.31 1.62 9 7 -7 33.66 1.4 9 7 7 36.78 1.92 9 -7 -7 36 1.53 -9 7 -7 36.3 1.81 9 7 7 39.49 1.51 9 7 7 35.97 1.75 10 7 -7 10.09 0.59 10 -7 7 10.98 0.81 10 -7 7 10.59 0.82 10 7 7 10.28 1.01 10 -7 -7 11.12 0.72 10 7 7 11.78 0.71 -10 7 -7 10.4 0.99 11 -7 7 16.45 1.03 11 7 -7 17.01 0.75 11 -7 7 16.94 1 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10.83 0.59 10 8 7 10.39 0.64 10 -8 -7 11.44 0.69 -10 8 -7 10.33 0.97 10 8 7 10.85 0.99 11 8 -7 11.63 0.55 11 -8 7 11.88 0.72 11 -8 -7 11.81 0.65 11 8 7 11.59 0.64 12 -8 7 6.74 0.49 12 8 -7 6.27 0.33 12 8 7 6.28 0.42 12 -8 -7 6.71 0.44 0 9 7 52.23 2.17 0 9 -7 52.12 1.84 -1 9 7 15.69 0.98 1 9 -7 15.02 0.66 -1 9 -7 14.04 0.74 1 9 7 14.95 0.76 1 9 7 15.46 1.02 2 9 -7 33.16 1.12 -2 9 7 32.89 1.53 -2 9 7 32.78 1.4 2 9 7 32.49 1.44 -2 9 -7 32.04 1.32 2 9 7 32.72 1.6 2 9 7 32.42 1.27 -3 9 7 21.2 1.04 3 9 7 19.49 1.21 -3 9 -7 19.98 1.19 3 9 7 21.81 0.88 3 9 7 19.69 1.09 4 9 -7 41.51 1.7 -4 9 7 40.18 1.73 4 9 7 43.73 1.83 -4 9 -7 42.21 1.94 4 9 7 45.98 2.04 4 9 7 45.11 1.48 5 9 -7 10.4 0.73 -5 9 7 10.95 0.77 5 9 7 10.27 0.79 -5 9 -7 10.81 0.98 5 9 7 9.66 0.82 5 9 7 10.65 1 6 9 -7 39.81 1.63 -6 9 7 38.83 1.7 6 9 7 41.44 1.83 6 9 7 42.05 1.78 -6 9 -7 39.75 1.93 6 9 7 45.45 2.09 -7 9 7 4.18 0.5 7 9 -7 4.48 0.47 -7 9 -7 4.83 0.68 7 9 7 5.56 0.66 7 9 7 5.37 0.8 7 9 7 5.77 0.54 7 9 7 5.94 0.5 -8 9 7 27.46 1.34 8 9 -7 30.23 1.24 8 -9 -7 27.95 1.27 -8 9 -7 29.34 1.56 8 9 7 30.61 1.82 8 9 7 30.19 1.24 8 9 7 31.04 1.48 8 9 7 30.57 1.24 9 9 -7 6.64 0.5 9 -9 7 5.83 0.58 9 9 7 6.79 0.53 9 9 7 5.88 0.62 9 -9 -7 6.06 0.55 -9 9 -7 6.54 0.71 10 -9 7 19.5 0.93 10 9 -7 19.27 0.82 10 9 7 19.94 1.02 10 -9 -7 18.7 0.89 10 9 7 19.38 0.87 11 -9 7 3.34 0.35 11 9 -7 3.27 0.28 11 -9 -7 3.18 0.32 11 9 7 3.78 0.35 12 -9 -7 12.07 0.69 12 9 7 14.84 0.59 0 10 -7 0.73 0.21 0 10 -7 0.94 0.35 0 10 7 0.17 0.3 0 10 7 0.69 0.24 0 10 7 1.07 0.31 -1 10 7 39 1.77 -1 10 7 39.94 1.63 1 10 -7 39.27 1.38 -1 10 -7 41.47 1.49 1 10 7 39.18 1.78 1 10 7 38.76 1.61 -1 10 -7 39.76 1.69 1 10 7 39.5 1.5 2 10 -7 2.89 0.25 -2 10 7 3.38 0.45 -2 10 7 2.95 0.54 -2 10 -7 2.65 0.5 2 10 7 2.59 0.47 2 10 7 2.44 0.28 -2 10 -7 2.14 0.31 2 10 7 2.89 0.44 -3 10 7 31.55 1.4 -3 10 7 31.09 1.52 3 10 7 31.19 1.41 -3 10 -7 32.34 1.5 3 10 7 32.27 1.6 3 10 7 32.36 1.18 -4 10 7 4.67 0.49 4 10 -7 4.54 0.49 4 10 7 5.3 0.69 4 10 7 3.22 0.44 4 10 7 3.79 0.25 -4 10 -7 2.87 0.48 -5 10 7 31.6 1.38 5 10 -7 32.3 1.33 -5 10 -7 32.7 1.51 5 10 7 27.58 1.55 5 10 7 28.18 1.38 5 10 7 28.76 1.35 6 10 -7 1.28 0.32 -6 10 7 1.68 0.39 6 10 7 1.77 0.48 -6 10 -7 1.06 0.42 6 10 7 2.1 0.41 6 10 7 1.06 0.35 -7 10 7 23.84 1.13 7 10 -7 22.82 1.03 -7 10 -7 21.54 1.23 7 10 7 21.11 1.13 8 10 -7 0.28 0.21 8 10 7 0.36 0.2 -8 10 -7 0.57 0.34 8 10 7 0.15 0.28 9 10 -7 17.78 0.77 9 10 7 15.79 0.87 9 10 7 16.07 0.77 10 10 -7 0.92 0.18 10 10 7 1.01 0.2 10 10 7 1.2 0.26 10 -10 -7 0.94 0.22 11 10 -7 11.49 0.48 11 10 7 10.8 0.5 0 11 7 54.33 1.96 0 11 -7 56.68 1.88 0 11 7 54.56 2.26 0 11 7 53.79 2.08 -1 11 7 0.68 0.24 1 11 -7 0.76 0.14 -1 11 7 0.32 0.32 -1 11 7 0.85 0.3 1 11 7 0.65 0.29 -1 11 -7 1.03 0.22 -1 11 -7 0.66 0.3 1 11 7 1.02 0.42 1 11 7 0.55 0.21 -2 11 7 55.75 2.13 -2 11 7 55.95 2.3 -2 11 -7 57.75 2.02 2 11 7 55.84 1.94 -2 11 -7 59.07 2.22 2 11 7 56.71 2.15 2 11 7 56.01 2.32 -3 11 7 1.44 0.35 -3 11 7 1.95 0.44 -3 11 -7 1.39 0.38 3 11 7 1.38 0.36 -3 11 -7 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212.73 7.04 -2 -2 8 233.87 8.19 3 2 -8 81.4 2.83 3 -2 8 83.48 4.1 3 2 8 79.44 2.71 4 2 -8 155.4 5.06 4 -2 8 155.83 6.64 4 2 8 148.87 4.94 5 -2 8 37.66 1.42 5 2 -8 36.4 1.5 5 2 8 36.33 1.43 6 -2 8 118.22 3.99 6 2 -8 118.99 4.09 6 2 8 120.38 4.02 7 -2 8 45.79 1.82 7 2 -8 45 1.87 7 2 8 48.46 1.85 8 -2 8 60.53 2.35 8 2 -8 61.99 2.42 8 2 8 62.85 2.38 9 2 -8 15.05 0.99 9 -2 8 15.05 0.95 9 -2 8 15.19 0.84 9 -2 8 14.7 0.74 9 -2 8 15.24 1.05 9 2 8 16.61 0.98 9 2 8 16.58 0.9 9 -2 -8 15.42 0.98 9 2 8 15.18 0.74 10 -2 8 39.89 1.5 10 -2 8 39.89 1.78 10 -2 8 41.54 1.64 10 -2 8 39.71 1.88 10 -2 -8 38.85 1.8 10 2 8 39.12 1.48 10 2 8 37.99 1.65 10 2 8 40.68 1.79 10 -2 -8 35.98 1.48 11 -2 8 16.25 1.21 11 -2 8 17.18 0.8 11 -2 8 16.83 0.94 11 -2 -8 15.2 0.75 11 2 8 16.39 0.97 11 -2 -8 15.17 1.05 11 2 8 13.83 0.97 11 2 8 15.79 0.77 12 -2 8 32.69 1.29 12 -2 8 36.17 1.83 12 -2 8 31.37 1.43 12 2 8 33.31 1.5 12 2 8 33.13 1.27 12 -2 -8 29.8 1.21 13 -2 8 9.55 0.56 13 -2 8 9.36 0.69 13 -2 8 9.16 0.92 13 2 8 8.71 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3.86 0.47 9 -5 -8 4.35 0.47 10 5 -8 7.68 0.46 10 -5 8 6.9 0.71 10 -5 8 5.94 0.6 10 -5 8 7.38 0.59 10 -5 -8 8.47 0.61 10 5 8 7.66 0.7 10 5 8 5.81 0.8 10 5 8 6.5 0.56 10 5 8 6.04 0.72 11 -5 8 3.53 0.54 11 5 -8 2.7 0.34 11 -5 8 2.98 0.39 11 -5 8 3.33 0.47 11 5 8 3.16 0.38 11 5 8 3.93 0.71 11 -5 -8 3.31 0.4 12 -5 8 2.6 0.43 12 -5 8 2.92 0.39 12 -5 8 2.56 0.41 -12 5 -8 2.93 0.52 12 5 8 3.52 0.51 12 -5 -8 3.41 0.35 12 5 8 2.91 0.36 13 -5 8 0.19 0.22 13 -5 8 0.41 0.27 13 -5 8 0.59 0.26 13 5 8 0.34 0.19 13 -5 -8 0.57 0.17 -13 5 -8 0.91 0.34 0 6 8 4.45 0.53 0 -6 8 4.11 1.55 1 -6 8 132.62 7.59 -1 6 8 158.68 5.14 -1 -6 8 143.72 7.58 1 6 8 161.31 5.16 -1 6 -8 155.81 4.9 2 6 8 3.97 0.51 -2 -6 8 3.59 1.4 3 6 8 164.06 5.54 4 6 8 7 0.68 5 6 8 102.53 3.7 6 6 8 1.26 0.39 7 6 -8 75.12 2.98 7 -6 8 76.37 2.79 7 -6 -8 76.23 2.94 7 6 8 75.84 2.8 7 6 8 76.99 2.97 8 6 -8 9.65 0.58 8 -6 8 10.41 0.79 8 6 8 9.43 0.89 8 6 8 9.4 0.74 8 -6 -8 9.9 0.72 8 6 8 10.31 0.69 8 6 8 13.13 1.24 9 -6 8 65.18 2.47 9 -6 8 67.7 2.56 9 6 -8 62.58 2.32 9 6 8 67.72 2.58 9 -6 -8 66.41 2.45 9 6 8 67.01 2.43 9 6 8 63.75 2.74 9 6 8 81.41 2.96 10 -6 8 2.78 0.41 10 -6 8 2.42 0.41 10 -6 8 2.24 0.43 10 6 -8 2.64 0.31 -10 6 -8 3.07 0.58 10 6 8 2.85 0.39 10 -6 -8 2.48 0.37 10 6 8 2.26 0.72 10 6 8 2.56 0.53 10 6 8 3.09 0.51 11 -6 8 33.01 1.45 11 -6 8 33.17 1.41 11 6 -8 31.28 1.21 11 -6 8 32.05 1.45 -11 6 -8 31.74 1.6 11 -6 -8 31.82 1.32 11 6 8 35.42 1.36 11 6 8 31.45 1.45 12 -6 8 1.71 0.35 12 -6 8 1.73 0.35 12 6 -8 1.78 0.2 12 -6 8 2.01 0.4 12 6 8 1.55 0.29 12 -6 -8 1.54 0.26 -12 6 -8 1.62 0.44 13 -6 8 23.89 1.07 13 -6 8 24.23 1.04 13 6 8 26.14 1.01 13 -6 -8 23.49 0.93 0 7 8 11.97 0.83 -1 7 8 5.57 0.62 1 7 8 4.45 0.59 2 7 8 17.53 1.08 3 7 8 13.54 0.98 4 7 8 10.34 0.9 5 7 8 7.98 0.83 5 7 8 7.27 0.39 5 7 8 7.61 0.87 6 -7 8 18.03 0.95 6 7 8 16.95 1.03 6 7 8 17.77 1.16 6 7 8 17.57 1.17 -6 7 -8 17.01 1.2 7 7 -8 8.6 0.6 7 -7 8 8.71 0.71 7 7 8 8.14 0.63 7 7 8 9.4 0.88 7 7 8 9.43 0.65 7 7 8 7.12 0.79 7 7 8 8.24 0.78 7 -7 -8 9.14 0.71 -7 7 -8 8.93 0.94 8 7 -8 8.77 0.6 8 -7 8 8.07 0.71 8 -7 -8 8.92 0.7 8 7 8 7.48 0.89 -8 7 -8 7.8 0.9 8 7 8 8.17 0.64 8 7 8 7.29 0.76 8 7 8 8.48 0.82 9 -7 8 0.47 0.34 9 7 -8 0.68 0.24 9 7 8 0.38 0.25 -9 7 -8 0.78 0.48 9 7 8 0.18 0.32 9 7 8 0.47 0.38 9 -7 -8 0.75 0.3 9 7 8 0.44 0.44 10 -7 8 2.54 0.42 10 7 -8 3.34 0.34 10 -7 -8 2.68 0.37 -10 7 -8 3.61 0.61 10 7 8 3.2 0.41 10 7 8 1.95 0.49 11 7 -8 2.16 0.26 11 -7 8 1.67 0.36 -11 7 -8 0.97 0.44 11 7 8 1.54 0.3 11 -7 -8 1.92 0.3 12 -7 8 2.5 0.35 12 7 -8 3.17 0.24 12 -7 -8 3.73 0.36 12 7 8 2.77 0.33 13 -7 -8 1.7 0.2 13 7 8 1.5 0.21 0 8 8 86.66 3.23 -1 8 8 54.53 2.23 1 8 8 57.07 2.31 -2 8 8 109.42 3.88 2 8 8 108.76 3.99 3 8 8 43.39 1.59 3 8 8 41.53 1.96 -4 8 8 71.59 2.66 4 8 8 73.96 2.46 -4 8 -8 68.85 3.64 4 8 8 79.51 3.07 4 8 8 70.9 2.69 4 8 8 74.06 2.8 5 8 -8 37.29 1.57 5 8 8 41.87 2 -5 8 -8 37.98 1.93 5 8 8 37.45 1.64 5 8 8 41.1 1.83 6 8 -8 48.47 1.92 6 8 8 53.06 2.39 6 -8 -8 52.99 2.02 6 8 8 49.63 2.03 -6 8 -8 48.85 2.3 6 8 8 53.07 2.24 7 -8 8 43.38 1.8 7 8 -8 44.71 1.74 7 8 8 47.48 2.25 7 8 8 49.75 2.1 7 -8 -8 45 1.78 7 8 8 43.89 1.85 -7 8 -8 39.88 2.08 8 8 -8 38.58 1.52 8 -8 8 36.98 1.61 8 8 8 39.13 2.04 8 -8 -8 39.08 1.58 -8 8 -8 35.76 1.89 8 8 8 38.15 1.54 8 8 8 41.67 1.92 9 8 -8 25.6 1.1 9 -8 8 25.82 1.22 -9 8 -8 25.44 1.49 9 -8 -8 26.54 1.17 9 8 8 25.41 1.14 9 8 8 26.38 1.48 10 8 -8 21.32 0.92 10 -8 8 21.75 1.07 10 8 8 21.99 1.27 -10 8 -8 21.15 1.32 10 8 8 22.74 0.98 10 -8 -8 21.7 1 11 -8 8 10.45 0.66 11 8 -8 9.91 0.49 11 8 8 10.04 0.58 11 -8 -8 9.66 0.58 12 8 -8 15.18 0.58 12 -8 8 15.1 0.72 12 8 8 15.39 0.67 12 -8 -8 16.05 0.68 0 9 8 0.89 0.35 0 9 -8 0.49 0.51 0 9 -8 0.64 0.21 0 9 8 0.57 0.28 -1 9 8 15.48 1 -1 9 8 16.23 0.9 1 9 -8 16.91 0.7 1 9 -8 15.91 1.02 -1 9 -8 16.84 0.81 1 9 8 15.86 0.8 1 9 8 16.27 0.93 1 9 8 16.9 1.04 -1 9 -8 15.44 0.96 -2 9 8 0.68 0.35 -2 9 8 1.19 0.33 2 9 -8 1 0.13 2 9 8 1.25 0.42 -2 9 -8 0.78 0.35 2 9 8 1.34 0.35 -2 9 -8 1.29 0.29 2 9 8 1.36 0.26 3 9 -8 24.55 1.45 -3 9 8 23.49 1.24 -3 9 8 23.58 1.12 3 9 8 22.01 1.16 -3 9 -8 23.18 1.3 3 9 8 22.49 1.33 3 9 8 22.96 0.95 4 9 -8 2.04 0.37 -4 9 8 1.97 0.38 4 9 8 2.07 0.43 4 9 8 2.37 0.23 -4 9 -8 2.47 0.54 4 9 8 2.59 0.6 4 9 8 3.12 0.45 -5 9 8 14.08 0.85 5 9 -8 13.94 0.82 5 9 8 11.14 1.05 5 9 8 12.43 0.92 -5 9 -8 11.88 1.04 5 9 8 13.6 0.84 6 9 -8 3.4 0.44 -6 9 8 3.01 0.44 6 9 8 2.84 0.51 6 9 8 3.34 0.66 -6 9 -8 3.65 0.66 7 9 -8 8.09 0.62 7 9 8 5.23 0.77 -7 9 -8 4.73 0.7 7 9 8 6.18 0.67 8 9 -8 0.68 0.26 8 9 8 0.2 0.34 8 -9 -8 0.57 0.26 -8 9 -8 0.47 0.44 8 9 8 0.4 0.22 9 -9 8 4.17 0.45 9 9 -8 5.36 0.45 9 9 8 4.27 0.41 9 -9 -8 5.25 0.52 -9 9 -8 3.65 0.57 9 9 8 4.17 0.54 10 9 -8 1.41 0.23 10 -9 8 1.31 0.29 10 -9 -8 1.42 0.27 10 9 8 0.97 0.23 -10 9 -8 1.68 0.38 10 9 8 1.69 0.35 11 -9 8 2.6 0.31 11 9 -8 2.89 0.25 11 -9 -8 3.61 0.33 11 9 8 2.65 0.27 0 10 8 82.93 3.15 0 10 -8 93.1 2.99 0 10 -8 94.33 3.26 0 10 8 90.45 3.36 0 10 8 90.34 3.06 -1 10 8 0.12 0.26 1 10 -8 0.25 0.13 -1 10 8 0.08 0.31 1 10 8 0.11 0.33 1 10 8 0.05 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7.23 0.33 -1 11 8 6.3 0.7 -1 11 8 6.89 0.63 -1 11 -8 7.34 0.68 1 11 8 6.82 0.71 -1 11 -8 7.89 0.48 1 11 8 7.4 0.48 1 11 8 7.57 0.65 -2 11 8 0.32 0.28 -2 11 8 0.42 0.33 2 11 8 0.1 0.16 -2 11 -8 0.6 0.34 2 11 8 0.27 0.31 2 11 8 0.29 0.29 -2 11 -8 0.29 0.21 -3 11 8 8.42 0.68 -3 11 8 7.32 0.74 3 11 8 8.68 0.77 -3 11 -8 9.08 0.76 -3 11 -8 8.93 0.56 3 11 8 8.47 0.69 3 11 8 8.43 0.4 -4 11 8 0.53 0.29 -4 11 8 0.76 0.42 -4 11 -8 0.81 0.37 4 11 8 0.74 0.31 -4 11 -8 0.63 0.25 4 11 8 0.78 0.37 5 11 -8 7.93 0.61 -5 11 8 7.1 0.63 -5 11 -8 7.95 0.72 5 11 8 8.32 0.7 6 11 -8 1.4 0.3 -6 11 8 1.97 0.35 6 11 8 1.51 0.33 -6 11 -8 1.9 0.41 -7 11 8 2.49 0.36 7 11 -8 2.9 0.34 7 11 8 2.63 0.37 -7 11 -8 1.98 0.38 8 11 -8 1.3 0.24 -8 11 -8 1.16 0.29 8 11 8 0.97 0.24 9 11 -8 4.08 0.33 9 11 8 3.4 0.34 10 11 -8 0.49 0.13 0 12 8 24.56 1.09 0 12 8 22.97 0.93 0 12 -8 21.54 0.8 -1 12 8 8.99 0.69 -1 12 8 9.56 0.56 1 12 8 8.74 0.7 -1 12 -8 9.89 0.48 1 12 8 9.52 0.5 -2 12 8 22.55 0.96 -2 12 8 21.86 1.06 2 12 8 22.26 0.83 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0.56 6 2 14 1.5 0.26 7 2 -14 1.93 0.33 7 2 -14 2.17 0.59 7 -2 14 1.99 0.46 7 -2 -14 2.14 0.54 7 -2 -14 2.48 0.39 7 2 14 2.47 0.4 8 2 -14 0.81 0.25 8 -2 14 0.83 0.43 8 2 14 1.28 0.35 8 -2 -14 0.61 0.27 9 2 -14 1.67 0.29 9 -2 14 2.67 0.54 9 -2 -14 1.85 0.33 9 2 14 2.31 0.41 10 -2 14 0.97 0.35 10 2 -14 0.94 0.22 10 -2 14 1.3 0.42 10 -2 -14 0.53 0.23 10 2 14 0.76 0.28 11 -2 14 1.02 0.23 11 2 -14 0.52 0.17 11 -2 14 0.41 0.34 11 -2 -14 0.95 0.21 11 2 14 1.18 0.28 12 -2 -14 0.42 0.14 -12 2 -14 0.8 0.37 0 -3 -14 91.34 3.04 0 3 -14 89.76 3.02 1 3 -14 24.96 1.02 -1 -3 -14 24.7 1.07 1 -3 -14 26.17 1.03 -1 3 -14 25.66 1.07 2 3 -14 77.12 2.59 -2 3 -14 79.55 2.72 2 3 14 77.4 2.8 2 -3 -14 80.58 2.63 2 3 14 80.24 2.93 3 -3 14 33.55 1.34 3 -3 14 33.32 1.52 3 -3 -14 34.92 1.21 3 3 14 35.15 1.36 3 3 14 34.36 1.46 4 3 -14 48.14 1.88 4 -3 14 47.97 2.01 4 -3 14 49.81 1.82 4 3 -14 51.07 2.32 4 3 14 49.79 1.8 4 3 14 48.41 1.93 4 -3 -14 51.71 1.99 5 -3 14 17.47 1.05 5 3 -14 15.78 1.2 5 -3 14 19.15 0.85 5 3 -14 18.45 0.94 5 3 14 17.74 0.98 5 -3 -14 19.02 1.2 5 3 14 18.44 0.84 5 -3 -14 18.51 1.01 6 3 -14 50.03 2.34 6 -3 14 52.01 2.12 6 3 -14 51.14 1.92 6 3 14 49.91 1.71 6 -3 -14 50.39 2.25 6 3 14 52.28 2.02 6 -3 -14 49.76 2 7 -3 14 32.49 1.51 7 3 -14 31.11 1.29 7 3 -14 28.77 1.67 7 3 14 28.4 1.38 7 -3 -14 30.91 1.38 7 -3 -14 30.94 1.64 8 -3 14 37.69 1.72 8 3 -14 39.19 1.49 8 -3 -14 38.64 1.57 8 3 14 35.91 1.61 9 3 -14 17.58 0.83 9 -3 14 16.58 1.05 9 -3 -14 17.55 0.9 9 3 14 16.24 0.95 10 -3 14 24.86 1.26 10 3 -14 26.18 1.04 10 -3 -14 25.49 1.1 10 3 14 26.06 1.21 11 3 -14 13.34 0.62 11 -3 14 14.17 0.83 -11 3 -14 13.39 0.94 11 3 14 13.7 0.79 11 -3 -14 14.28 0.68 0 4 -14 0.37 0.24 1 -4 14 1.83 0.39 1 4 -14 1.8 0.28 -1 4 -14 1.87 0.32 1 -4 -14 1.5 0.29 2 -4 14 0.4 0.28 2 -4 -14 0.32 0.2 2 4 14 0.4 0.22 -2 4 -14 0.49 0.26 2 4 14 0.22 0.26 3 4 -14 3.19 0.43 3 -4 14 3.28 0.47 3 -4 14 3.3 0.36 3 4 14 3.02 0.49 3 4 14 3.39 0.38 3 -4 -14 2.69 0.27 4 -4 14 4.04 0.4 4 4 -14 2.35 0.38 4 -4 14 2.85 0.45 4 4 14 3.05 0.34 4 4 14 2.86 0.46 5 -4 14 0.2 0.34 5 -4 14 0.19 0.2 5 4 -14 0.04 0.25 -5 4 -14 0.04 0.42 5 -4 -14 0.25 0.3 5 4 14 -0.06 0.31 5 4 14 0.44 0.22 6 4 -14 1.84 0.35 6 -4 14 1.73 0.43 6 -4 -14 2.46 0.54 6 -4 -14 1.54 0.41 6 4 14 2.26 0.46 -6 4 -14 1.85 0.5 7 -4 14 9.67 0.83 7 4 -14 9.07 0.66 7 4 14 9.45 0.8 7 -4 -14 9.48 0.78 -7 4 -14 7.77 0.84 8 -4 14 4.04 0.55 8 4 -14 3.94 0.42 -8 4 -14 3.75 0.66 8 4 14 3.44 0.54 8 -4 -14 3.82 0.48 9 4 -14 1.27 0.28 9 -4 14 1.74 0.39 9 -4 -14 1.37 0.31 -9 4 -14 1.23 0.5 9 4 14 1.5 0.4 10 4 -14 1.27 0.24 10 -4 14 1.65 0.36 -10 4 -14 1.4 0.47 10 4 14 1.61 0.39 10 -4 -14 1.32 0.28 11 -4 14 0.86 0.28 11 4 -14 0.61 0.17 -11 4 -14 1.1 0.4 11 4 14 0.7 0.27 11 -4 -14 0.35 0.2 0 5 -14 79.83 2.73 1 5 -14 5.4 0.42 -1 5 -14 5.65 0.51 2 -5 14 91.94 3.27 -2 5 -14 94.81 3.18 2 5 14 91.58 3.36 2 5 14 92.67 3.19 2 -5 -14 93.14 3.08 3 -5 14 1.47 0.27 3 -5 14 1.71 0.37 3 5 14 1.56 0.42 3 5 14 2.08 0.33 3 -5 -14 2.01 0.25 4 -5 14 72.75 2.71 4 -5 14 74.69 2.56 4 5 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33.25 1.7 6 7 14 31.29 1.64 7 -7 14 13.41 0.81 7 7 -14 15.4 0.84 7 7 14 14.67 0.84 7 7 14 14.98 0.94 -7 7 -14 14.53 1.18 8 7 -14 27.79 1.15 8 -7 14 27.23 1.19 8 7 14 26.55 1.22 8 -7 -14 25.72 1.13 -8 7 -14 26.35 1.42 9 7 -14 6.12 0.46 9 -7 14 5.77 0.5 -9 7 -14 6.35 0.65 9 7 14 5.78 0.53 9 -7 -14 5.45 0.45 10 -7 14 18.61 0.93 10 7 -14 16.87 0.7 -10 7 -14 16.86 0.89 0 8 14 2.28 0.34 0 8 -14 2.07 0.21 -1 8 -14 1.42 0.25 1 8 14 1.05 0.26 -1 8 -14 1.56 0.41 2 8 14 1.27 0.39 -2 8 -14 0.89 0.39 2 8 14 1.34 0.27 -2 8 -14 1.34 0.29 3 8 14 1 0.22 -3 8 -14 0.83 0.3 3 -8 -14 1.32 0.19 3 8 14 1.86 0.45 -3 8 -14 1.32 0.44 4 8 14 2.3 0.44 4 8 14 1.85 0.18 -4 8 -14 1.53 0.36 -4 8 -14 1.61 0.46 5 8 -14 1.17 0.34 5 8 14 2.29 0.44 -5 8 -14 1.47 0.34 -5 8 -14 1.39 0.47 6 8 -14 1.66 0.34 6 8 14 1.91 0.35 6 8 14 2.59 0.43 -6 8 -14 1.16 0.45 -6 8 -14 2 0.43 7 8 -14 0.7 0.26 7 -8 14 0.11 0.22 7 8 14 0.07 0.22 7 8 14 0.04 0.27 -7 8 -14 0.05 0.37 8 8 -14 0.11 0.2 8 -8 14 -0.12 0.19 8 8 14 0.15 0.22 -8 8 -14 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0.73 2 -3 19 13.63 0.88 -2 -3 19 12.91 0.79 2 3 19 14.15 0.93 2 3 19 13.19 0.69 -2 3 -19 12.7 0.7 3 -3 19 25.72 1.05 3 -3 19 25.82 1.24 -3 -3 -19 25.73 1.1 -3 3 -19 23.91 1.06 3 3 19 25.99 1.04 3 3 19 24.73 1.24 4 -3 19 12.49 0.84 4 -3 19 13.08 0.63 4 3 19 12.18 0.8 4 3 19 12.67 0.58 5 -3 19 29.24 1.32 6 -3 19 12.77 0.79 7 -3 19 14.22 0.76 7 3 -19 13.55 0.69 0 4 19 14.74 0.75 0 -4 -19 14.66 0.69 0 -4 19 14.97 0.84 -1 -4 -19 2.15 0.3 1 -4 19 3.06 0.43 1 4 19 2.01 0.3 2 -4 19 7.2 0.66 -2 -4 -19 7.56 0.56 2 -4 19 6.71 0.5 2 4 19 7.92 0.53 2 4 19 7.92 0.7 3 -4 19 1.46 0.36 3 -4 19 1.63 0.26 3 4 19 1.64 0.25 4 -4 19 6.17 0.57 4 4 19 5.1 0.28 5 -4 19 1.33 0.34 6 -4 19 3.61 0.4 6 4 19 3.63 0.52 7 -4 19 0.81 0.23 0 5 19 0.43 0.21 1 -5 19 39.21 1.5 1 5 19 40.57 1.49 2 -5 19 0.04 0.24 2 -5 19 -0.1 0.17 -2 5 -19 0.12 0.11 2 5 19 0.28 0.19 3 -5 19 35.58 1.43 -3 5 -19 35.46 1.26 3 5 19 35.84 1.25 4 -5 19 -0.3 0.21 4 5 19 -0.22 0.2 5 -5 19 29.76 1.18 5 5 19 27.63 1.14 6 -5 19 0.08 0.2 0 6 19 5.93 0.44 -1 6 19 0.03 0.18 1 6 19 0.01 0.17 2 6 19 3.59 0.31 2 6 19 3.46 0.38 3 6 19 0.32 0.23 -3 6 -19 0.51 0.16 3 6 19 0.51 0.1 4 -6 19 2.92 0.32 -4 6 -19 2.5 0.21 4 6 19 2.31 0.33 5 -6 19 0.5 0.27 -5 6 -19 0.68 0.23 0 7 19 14.68 0.65 0 7 19 15.92 0.97 -1 7 19 20.67 0.84 1 7 19 20.66 0.79 1 7 19 20.38 0.88 2 7 19 9.17 0.56 2 7 19 9.45 0.39 3 7 19 21.16 0.93 0 0 20 24.65 1.26 1 0 20 1.46 0.41 -1 0 -20 1.36 0.25 1 0 20 1.14 0.25 -2 0 -20 25.99 1.11 2 0 20 27.18 1.32 2 0 20 26.37 1.08 3 0 20 0.03 0.17 3 0 20 0.14 0.32 4 0 20 21.35 0.84 4 0 20 23.45 1.16 5 0 20 0.88 0.34 6 0 20 15.13 0.85 0 -1 20 1.85 0.42 -1 -1 -20 21.67 0.9 1 -1 20 23.14 1.16 1 -1 20 21.75 0.95 1 1 20 21.32 0.94 -1 1 -20 22.09 0.93 1 1 20 21.87 1.17 2 -1 20 1.22 0.38 -2 -1 -20 1.31 0.35 2 -1 20 1.37 0.26 -2 1 -20 1.55 0.35 2 1 20 1.67 0.27 2 1 20 1.61 0.42 3 -1 20 21.71 0.93 3 -1 20 23.05 1.15 3 1 20 22.1 0.93 3 1 20 24.22 1.23 4 -1 20 1.06 0.36 4 -1 20 1 0.19 4 1 20 1.29 0.38 4 1 20 1.08 0.18 5 -1 20 14.55 0.86 5 1 20 14.65 0.89 6 -1 20 0.8 0.31 6 1 20 0.18 0.24 0 -2 20 20.31 1.04 1 -2 20 7.5 0.52 1 -2 20 7.81 0.72 1 2 20 8.68 0.54 -1 -2 20 8.82 0.67 1 2 20 9.83 0.82 2 -2 20 16.11 0.77 2 -2 20 16.76 0.96 2 2 20 17.68 1.03 2 2 20 16.63 0.77 -2 -2 20 15.93 0.87 3 -2 20 7.94 0.68 3 -2 20 8.39 0.5 3 2 20 7.98 0.75 3 2 20 7.95 0.5 4 -2 20 11.63 0.81 4 2 20 13.87 0.81 4 2 20 12.06 0.49 5 -2 20 10.08 0.69 5 2 20 8.71 0.64 6 -2 20 12.43 0.72 0 3 20 13.96 0.7 0 -3 20 13.28 0.8 1 -3 20 7.5 0.51 1 -3 20 7.91 0.66 -1 -3 20 7.35 0.62 1 3 20 8.26 0.74 1 3 20 7.68 0.51 2 -3 20 11.97 0.62 2 -3 20 11.35 0.75 -2 -3 20 11.85 0.71 2 3 20 12.6 0.63 2 3 20 13.55 0.84 3 -3 20 4.45 0.39 3 -3 20 5.15 0.52 3 3 20 5 0.39 3 3 20 5.03 0.51 4 -3 20 8.69 0.65 4 3 20 9.15 0.64 5 -3 20 6.51 0.56 6 -3 20 8 0.54 0 4 20 2.13 0.27 0 -4 20 2.04 0.33 1 -4 20 18.18 0.82 1 -4 20 17.99 0.9 1 4 20 18.58 0.94 1 4 20 18.36 0.81 2 -4 20 1.45 0.23 2 -4 20 1.7 0.33 2 4 20 1.68 0.33 2 4 20 1.61 0.24 3 -4 20 19.73 0.93 3 4 20 19.29 0.71 -3 4 -20 17.76 0.67 4 -4 20 1.42 0.29 5 -4 20 17.97 0.84 0 5 20 11.98 0.7 0 5 20 12.27 0.62 1 -5 20 1 0.21 -1 5 20 0.86 0.2 1 5 20 0.94 0.2 2 -5 20 14.69 0.74 2 5 20 15.58 0.63 3 -5 20 0.49 0.22 4 -5 20 9.28 0.56 0 6 20 2.47 0.23 1 6 20 16.25 0.65 0 0 21 0.03 0.15 0 0 21 -0.4 0.26 -1 0 21 24.57 1.13 1 0 21 22.84 0.96 1 0 21 24.79 1.15 2 0 21 0.76 0.32 2 0 21 0.73 0.19 3 0 21 28.39 1.24 3 0 21 27.57 1.02 4 0 21 0.07 0.26 5 0 21 21.61 0.99 0 -1 21 10.3 0.73 0 1 21 11.88 0.79 0 1 21 9.69 0.54 0 -1 21 9.35 0.59 -1 1 21 2.32 0.4 1 -1 21 2.41 0.28 1 -1 21 2.95 0.43 1 1 21 1.92 0.25 1 1 21 1.79 0.38 -1 -1 21 1.77 0.35 2 -1 21 6.09 0.59 2 -1 21 5.12 0.4 2 1 21 5.88 0.41 -2 -1 21 5.08 0.48 2 1 21 5.97 0.55 3 -1 21 1.04 0.18 3 -1 21 1.12 0.31 3 1 21 0.98 0.33 3 1 21 0.9 0.17 -3 -1 21 1.21 0.29 4 -1 21 3.97 0.43 -4 -1 21 4.14 0.39 4 1 21 4.49 0.46 5 -1 21 0.73 0.25 0 -2 21 4.93 0.48 0 2 21 5.15 0.56 0 2 21 5.58 0.42 1 -2 21 26.78 1.16 1 -2 21 26.68 1.05 1 2 21 28.4 1.24 -1 -2 21 25.79 1.13 1 2 21 25.79 1.03 2 -2 21 7.26 0.59 2 -2 21 7.1 0.45 2 2 21 8.27 0.68 -2 -2 21 6.9 0.53 2 2 21 7.56 0.44 3 -2 21 17.81 0.88 3 2 21 17.25 0.66 3 2 21 18.43 0.88 -3 -2 21 15.74 0.77 4 -2 21 6.57 0.54 4 2 21 6.28 0.51 5 -2 21 16.54 0.91 0 3 21 1.28 0.21 0 3 21 1.69 0.36 0 -3 21 1.57 0.24 0 -3 21 1.22 0.28 1 -3 21 3.48 0.38 1 -3 21 3.52 0.31 -1 3 21 3.29 0.44 -1 -3 21 3.5 0.36 1 3 21 2.7 0.27 1 3 21 3.01 0.39 2 -3 21 1.5 0.21 2 -3 21 1.59 0.31 2 3 21 1.83 0.32 2 3 21 1.49 0.21 3 -3 21 6.46 0.51 3 3 21 5.59 0.49 4 -3 21 1.21 0.26 0 4 21 20.72 0.91 0 4 21 19.1 0.81 1 -4 21 3.38 0.35 1 -4 21 4.56 0.42 -1 4 21 4.19 0.41 1 4 21 4.6 0.43 1 4 21 4.71 0.33 2 -4 21 26.16 1.08 2 4 21 27.53 1.02 3 -4 21 2.77 0.42 0 0 22 1.39 0.3 -1 0 22 0.15 0.23 -2 0 22 0.12 0.2 2 0 22 0.05 0.22 0 1 22 2.08 0.34 0 -1 22 1.49 0.29 -1 1 22 34.07 1.32 1 -1 22 32.07 1.29 1 1 22 34.41 1.33 -1 -1 22 32 1.28 2 -1 22 3.23 0.37 -2 1 22 3.12 0.36 2 1 22 4.84 0.46 0 2 22 1.09 0.27 0 -2 22 0.61 0.28 -1 2 22 0.13 0.23 1 -2 22 0.16 0.21 1 2 22 0.09 0.23 -2 2 22 0.59 0.3 _iucr_refine_instructions_details ; q43i.res created by SHELXL-2014/7 TITL [UO2(C25H31N3O6)][O3SCF3] CELL 1.54178 12.9352 13.2651 18.4739 90 90 90 ZERR 4 0.0002 0.0002 0.0003 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H F N Na O S U UNIT 104 124 12 12 4 44 4 4 EQIV $1 1-X,0.5+Y,0.5-Z EQIV $2 1.5-X,1-Y,-0.5+Z EQIV $3 0.5+X,0.5-Y,1-Z EQIV $4 +X,-1+Y,+Z EQIV $5 -0.5+X,0.5-Y,1-Z DFIX 41 0.01 S1 O11 S1 O12 S1 O13 S1' O11' S1' O12' S1' O13' DFIX 40.926 0.01 C26 F11 C26 F12 C26 F13 C26' F11' C26' F12' C26' F13' DFIX 41.281 0.01 S1 C26 S1' C26' DFIX 41.489 F11 F12 F11 F13 F12 F13 F11' F12' F11' F13' F12' F13' DFIX 41.692 O11 O12 O11 O13 O12 O13 O11' O12' O11' O13' O12' O13' DFIX 41.786 C26 O11 C26 O12 C26 O13 C26' O11' C26' O12' C26' O13' DFIX 41.839 S1 F11 S1 F12 S1 F13 S1' F11' S1' F12' S1' F13' ISOR 0.01 0.02 F13' C26' EADP C9 C9' EXYZ C9 C9' L.S. 50 PLAN 20 SIZE 0.02 0.04 0.13 TEMP -73.16 HTAB C8 O8_$1 HTAB C9' O8_$1 HTAB C11 F12' HTAB C13 O8_$1 HTAB C15 O13_$2 HTAB C15 O13'_$2 HTAB C20 O12'_$3 HTAB C21 F13_$3 HTAB C22 F11'_$4 HTAB C24 S1_$5 HTAB C24 O13_$5 WPDB -2 BOND $H CONF HTAB HTAB fmap -2 ACTA 132 TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.035400 BASF 0.49354 FVAR 0.06906 0.65499 0.59094 1.41034 U 8 0.502143 0.201352 0.444206 11.00000 0.03328 0.03708 = 0.03070 -0.00157 -0.00243 -0.00217 NA 5 0.543878 0.460688 0.381834 11.00000 0.04809 0.04765 = 0.04870 0.00472 -0.00900 -0.00165 O1 6 0.401561 0.327360 0.403629 11.00000 0.03560 0.05578 = 0.03645 0.00100 -0.00705 0.00134 O6 6 0.380518 0.486888 0.315617 11.00000 0.04634 0.05519 = 0.07472 0.01280 -0.01428 0.00159 O5 6 0.523220 0.630596 0.338641 11.00000 0.06594 0.06903 = 0.09368 0.04305 -0.02009 -0.01136 O4 6 0.723361 0.565276 0.348222 11.00000 0.06625 0.06905 = 0.07881 0.02373 -0.01291 -0.01114 O3 6 0.651018 0.399693 0.276234 11.00000 0.04395 0.06878 = 0.05770 0.01538 -0.00181 -0.00533 O2 6 0.629411 0.298675 0.397688 11.00000 0.03444 0.05239 = 0.04396 0.00285 -0.00109 -0.00288 O7 6 0.509511 0.262792 0.529834 11.00000 0.06109 0.04510 = 0.03659 0.00211 -0.01216 -0.00962 O8 6 0.494943 0.131390 0.362153 11.00000 0.04012 0.06170 = 0.04488 -0.00880 -0.00422 -0.00308 N1 4 0.315458 0.144931 0.456352 11.00000 0.04287 0.04949 = 0.04551 -0.00586 0.01034 0.00012 N3 4 0.482265 0.035642 0.520424 11.00000 0.04700 0.04209 = 0.05988 -0.00253 -0.00323 -0.00477 N2 4 0.673812 0.110460 0.464715 11.00000 0.04213 0.04437 = 0.05296 0.00041 -0.00796 -0.00328 C1 1 0.239963 0.174554 0.416342 11.00000 0.03598 0.04154 = 0.06242 -0.00899 0.00886 -0.00165 AFIX 43 H1 2 0.177149 0.137909 0.420539 11.00000 -1.20000 AFIX 0 C2 1 0.240402 0.257997 0.365434 11.00000 0.03132 0.05294 = 0.05027 -0.01189 0.00248 0.00507 C3 1 0.153010 0.266529 0.320256 11.00000 0.03467 0.06375 = 0.06258 -0.01566 -0.00450 0.00323 AFIX 43 H3 2 0.098129 0.219304 0.324489 11.00000 -1.20000 AFIX 0 C4 1 0.146728 0.343914 0.269407 11.00000 0.04137 0.08198 = 0.06409 -0.01036 -0.01389 0.00439 AFIX 43 H4 2 0.090217 0.346061 0.236599 11.00000 -1.20000 AFIX 0 C5 1 0.220991 0.416355 0.266470 11.00000 0.05320 0.07032 = 0.04157 0.00205 -0.00871 0.01300 AFIX 43 H5 2 0.215278 0.469710 0.232401 11.00000 -1.20000 AFIX 0 C7 1 0.319318 0.330686 0.361641 11.00000 0.03437 0.04615 = 0.03916 -0.00810 -0.00033 0.00586 C6 1 0.305510 0.412645 0.313268 11.00000 0.03984 0.05654 = 0.04228 0.00094 -0.00061 0.00614 PART 1 C8 1 0.362437 0.574085 0.279997 31.00000 0.06006 0.06902 = 0.06078 0.02807 -0.00865 -0.00472 AFIX 23 H8A 2 0.287934 0.590701 0.282853 31.00000 -1.20000 H8B 2 0.380812 0.565805 0.228316 31.00000 -1.20000 AFIX 0 C9 1 0.426513 0.661495 0.312923 31.00000 0.06830 0.06581 = 0.07030 0.01635 -0.01099 0.00213 AFIX 23 H9A 2 0.436624 0.714130 0.275596 31.00000 -1.20000 H9B 2 0.387025 0.691941 0.353289 31.00000 -1.20000 AFIX 0 PART 0 PART 2 C8' 1 0.350706 0.586285 0.331550 -31.00000 0.05009 AFIX 3 H8'A 2 0.341466 0.591155 0.382990 -31.00000 -1.20000 H8'B 2 0.286106 0.602625 0.308800 -31.00000 -1.20000 AFIX 0 C9' 1 0.426513 0.661495 0.312923 -31.00000 0.06830 0.06581 = 0.07030 0.01635 -0.01099 0.00213 AFIX 23 H9'A 2 0.429125 0.670115 0.259724 -31.00000 -1.20000 H9'B 2 0.407462 0.726984 0.334891 -31.00000 -1.20000 AFIX 0 PART 0 C10 1 0.601395 0.701881 0.324720 11.00000 0.06928 0.06237 = 0.08376 0.01889 -0.00075 -0.00473 AFIX 23 H10A 2 0.580458 0.769173 0.342669 11.00000 -1.20000 H10B 2 0.614733 0.706688 0.272063 11.00000 -1.20000 AFIX 0 C11 1 0.697911 0.665707 0.364195 11.00000 0.07281 0.07282 = 0.10204 0.01283 -0.01019 -0.01787 AFIX 23 H11A 2 0.756774 0.709606 0.350799 11.00000 -1.20000 H11B 2 0.686847 0.672333 0.417008 11.00000 -1.20000 AFIX 0 C12 1 0.760442 0.546023 0.276564 11.00000 0.06463 0.06957 = 0.08634 0.03612 0.00319 -0.01351 AFIX 23 H12A 2 0.826593 0.508669 0.279214 11.00000 -1.20000 H12B 2 0.773521 0.610819 0.251599 11.00000 -1.20000 AFIX 0 C13 1 0.683927 0.486123 0.234416 11.00000 0.06743 0.08151 = 0.05804 0.03485 -0.00068 -0.00051 AFIX 23 H13A 2 0.623370 0.528683 0.222583 11.00000 -1.20000 H13B 2 0.715557 0.463282 0.188456 11.00000 -1.20000 AFIX 0 C14 1 0.724039 0.327851 0.290481 11.00000 0.03568 0.05535 = 0.05021 0.00868 -0.00687 -0.00915 C15 1 0.807543 0.306043 0.246284 11.00000 0.04509 0.07868 = 0.05256 0.00937 0.00524 -0.01626 AFIX 43 H15 2 0.818301 0.343687 0.203191 11.00000 -1.20000 AFIX 0 C16 1 0.875974 0.228889 0.264872 11.00000 0.03649 0.07369 = 0.06953 -0.01348 0.00692 -0.00888 AFIX 43 H16 2 0.933617 0.214834 0.234647 11.00000 -1.20000 AFIX 0 C17 1 0.860480 0.173223 0.326542 11.00000 0.03668 0.06327 = 0.06685 -0.00644 -0.00126 -0.00519 AFIX 43 H17 2 0.908048 0.121608 0.339253 11.00000 -1.20000 AFIX 0 C18 1 0.774698 0.192279 0.370835 11.00000 0.03336 0.05234 = 0.04866 -0.00433 -0.00936 -0.00839 C19 1 0.706411 0.272083 0.353993 11.00000 0.03533 0.04490 = 0.03865 -0.00463 -0.00182 -0.01105 C20 1 0.758455 0.123570 0.430306 11.00000 0.04192 0.04467 = 0.05626 -0.00578 -0.01161 -0.00051 AFIX 43 H20 2 0.816096 0.084401 0.445289 11.00000 -1.20000 AFIX 0 C21 1 0.672882 0.028357 0.518432 11.00000 0.05904 0.05008 = 0.06725 0.01477 -0.01959 -0.00670 AFIX 23 H21A 2 0.681730 0.056255 0.567749 11.00000 -1.20000 H21B 2 0.730391 -0.019036 0.508828 11.00000 -1.20000 AFIX 0 C22 1 0.568751 -0.027030 0.512761 11.00000 0.06134 0.06882 = 0.10235 0.01564 0.00581 0.00812 AFIX 23 H22A 2 0.565006 -0.061009 0.465120 11.00000 -1.20000 H22B 2 0.566069 -0.079875 0.550555 11.00000 -1.20000 AFIX 0 C25 1 0.468242 0.058502 0.601932 11.00000 0.11125 0.06812 = 0.05243 0.00036 0.00871 -0.00392 AFIX 137 H25A 2 0.409833 0.104658 0.608494 11.00000 -1.50000 H25B 2 0.531321 0.089760 0.620895 11.00000 -1.50000 H25C 2 0.454688 -0.004427 0.628051 11.00000 -1.50000 AFIX 0 C23 1 0.383444 -0.014597 0.498663 11.00000 0.08186 0.05301 = 0.07396 -0.00897 0.00077 -0.01652 AFIX 23 H23A 2 0.389790 -0.040021 0.448476 11.00000 -1.20000 H23B 2 0.370420 -0.072952 0.530802 11.00000 -1.20000 AFIX 0 C24 1 0.294748 0.056773 0.503152 11.00000 0.05182 0.05414 = 0.06774 0.00845 0.01074 -0.00624 AFIX 23 H24A 2 0.230575 0.022698 0.487210 11.00000 -1.20000 H24B 2 0.285188 0.079107 0.553845 11.00000 -1.20000 AFIX 0 PART 1 S1 7 0.541499 0.578283 0.564577 21.00000 0.06321 0.05786 = 0.04901 -0.01022 0.00265 -0.00368 O11 6 0.522335 0.513217 0.504956 21.00000 0.12297 0.04499 = 0.04851 -0.01274 -0.00197 -0.00146 O12 6 0.519531 0.535611 0.632513 21.00000 0.22779 0.04396 = 0.06126 0.00547 0.01797 -0.00448 O13 6 0.637231 0.630430 0.561641 21.00000 0.07026 0.12766 = 0.14103 -0.06029 0.02324 -0.02580 F11 3 0.458392 0.743097 0.608294 21.00000 0.10543 0.06272 = 0.07431 -0.02083 0.00642 -0.00097 F12 3 0.442269 0.722361 0.496614 21.00000 0.24595 0.09017 = 0.07234 -0.01589 -0.05099 0.07228 F13 3 0.351125 0.637708 0.565628 21.00000 0.06686 0.15442 = 0.29462 -0.12968 -0.02090 0.01462 C26 1 0.445212 0.675177 0.557758 21.00000 0.13474 0.06641 = 0.07203 -0.02944 -0.03763 0.05161 PART 0 PART 2 S1' 7 0.508863 0.564685 0.562020 -21.00000 0.06029 0.03401 = 0.06823 -0.00223 -0.01089 -0.00460 O11' 6 0.531564 0.523068 0.493321 -21.00000 0.13848 0.05108 = 0.03574 0.00542 -0.02368 0.01148 O12' 6 0.402513 0.571231 0.578782 -21.00000 0.09426 0.23818 = 0.29914 -0.20534 0.01327 -0.03152 O13' 6 0.572096 0.532923 0.619161 -21.00000 0.17352 0.12838 = 0.01983 -0.01688 -0.02825 0.07117 F11' 3 0.512129 0.752363 0.605173 -21.00000 0.34640 0.04102 = 0.05097 0.00172 0.01878 -0.02217 F12' 3 0.645830 0.705671 0.550533 -21.00000 0.22520 0.17617 = 0.16999 -0.05684 0.09463 -0.11537 F13' 3 0.511224 0.734275 0.492202 -21.00000 0.16593 0.04497 = 0.07038 0.00215 -0.00397 -0.00163 C26' 1 0.545367 0.695171 0.552421 -21.00000 0.11499 0.09615 = 0.08734 0.00001 0.00225 0.00660 HKLF 4 REM [UO2(C25H31N3O6)][O3SCF3] REM R1 = 0.0272 for 5097 Fo > 4sig(Fo) and 0.0296 for all 5437 data REM 496 parameters refined using 50 restraints END WGHT 0.0354 0.0000 REM Instructions for potential hydrogen bonds HTAB C8 O8_$1 HTAB C9' O8_$1 HTAB C11 F12' HTAB C13 O8_$1 HTAB C20 O12'_$3 HTAB C21 F13_$3 HTAB C22 F11'_$4 HTAB C24 S1_$5 HTAB C24 O13_$5 REM Highest difference peak 1.114, deepest hole -0.582, 1-sigma level 0.118 Q1 1 0.4015 0.0323 0.5539 11.00000 0.05 1.11 Q2 1 0.5897 0.0277 0.5542 11.00000 0.05 1.08 Q3 1 0.5018 0.2603 0.4263 11.00000 0.05 0.95 Q4 1 0.4953 -0.0549 0.4571 11.00000 0.05 0.93 Q5 1 0.5039 0.1174 0.4535 11.00000 0.05 0.81 Q6 1 0.5042 0.1403 0.4203 11.00000 0.05 0.79 Q7 1 0.5389 0.2421 0.4848 11.00000 0.05 0.65 Q8 1 0.3987 0.1831 0.4495 11.00000 0.05 0.61 Q9 1 0.4641 0.2454 0.4886 11.00000 0.05 0.60 Q10 1 0.5022 0.2770 0.3688 11.00000 0.05 -0.58 Q11 1 0.5006 0.3968 0.4717 11.00000 0.05 -0.58 Q12 1 0.4960 0.3996 0.4229 11.00000 0.05 -0.55 Q13 1 0.5008 0.1268 0.5188 11.00000 0.05 -0.53 Q14 1 0.6089 0.1751 0.4538 11.00000 0.05 0.52 Q15 1 0.4969 0.1584 0.6465 11.00000 0.05 -0.47 Q16 1 0.4173 0.5586 0.5576 11.00000 0.05 0.46 Q17 1 0.5962 0.5611 0.5644 11.00000 0.05 0.43 Q18 1 0.3780 0.2069 0.5512 11.00000 0.05 -0.43 Q19 1 0.4985 0.0057 0.4454 11.00000 0.05 -0.42 Q20 1 -0.0049 0.3116 0.3039 11.00000 0.05 -0.42 REM The information below was added by Olex2. REM REM R1 = 0.0272 for 5097 Fo > 4sig(Fo) and 0.0296 for all 12937 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.11, deepest hole -0.58 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0296 REM R1_gt = 0.0272 REM wR_ref = 0.0658 REM GOOF = 1.095 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 12937 REM Reflections_gt = 5097 REM Parameters = n/a REM Hole = -0.58 REM Peak = 1.11 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.506(9) 2 0.494(9) data_L(salben)UO2Ca _audit_creation_date 2019-09-15 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2014/7' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C27.5 H38 Ca F3 N3 O13 S U, C H4 O, C F3 O3 S' _chemical_formula_sum 'C29.50 H42 Ca F6 N3 O17 S2 U' _chemical_formula_weight 1166.89 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7589(9) _cell_length_b 13.2831(9) _cell_length_c 13.7644(10) _cell_angle_alpha 79.402(3) _cell_angle_beta 64.575(3) _cell_angle_gamma 81.805(3) _cell_volume 2065.6(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9758 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 67.933 _cell_measurement_theta_min 3.590 _shelx_estimated_absorpt_T_max 0.487 _shelx_estimated_absorpt_T_min 0.263 _exptl_absorpt_coefficient_mu 14.000 _exptl_absorpt_correction_T_max 0.7530 _exptl_absorpt_correction_T_min 0.4621 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1112 before and 0.0749 after correction. The Ratio of minimum to maximum transmission is 0.6137. The \l/2 correction factor is 0.00150.' _exptl_absorpt_special_details ? _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.876 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description 'Near cube' _exptl_crystal_F_000 1148 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.085 _exptl_crystal_size_min 0.06 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_unetI/netI 0.0515 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 32430 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 66.000 _diffrn_reflns_theta_max 68.453 _diffrn_reflns_theta_min 3.394 _diffrn_ambient_temperature 199.99 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'Helios high-brilliance multilayer optics' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'sealed tube' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6979 _reflns_number_total 7473 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _refine_diff_density_max 1.521 _refine_diff_density_min -1.159 _refine_diff_density_rms 0.128 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 581 _refine_ls_number_reflns 7473 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0370 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+5.7162P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0850 _refine_ls_wR_factor_ref 0.0866 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances C23-C24 = C21-C22 1.52549 with sigma of 0.01 N3-C23 = N3-C22 = N3-C25 1.416417 with sigma of 0.01 C23A-C22A = C23A-C25A = C22A-C25A 2.491583 with sigma of 0.02 N3-C24 = N3-C21 = C23-C22 = C23-C25 = C22-C25 2.491583 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C25A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Others 1(DFIX)=0.9285*FVAR(2) 1(DFIX)=FVAR(1) 1(DFIX)=1(DFIX)=1.6333*FVAR(2) Sof(H21C)=Sof(H21D)=Sof(H24C)=Sof(H24D)=Sof(C22A)=Sof(H22A)=Sof(H22B)= Sof(C23A)=Sof(H23C)=Sof(H23D)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(2) Sof(H21A)=Sof(H21B)=Sof(H24A)=Sof(H24B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C25)= Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C22)=Sof(H22C)=Sof(H22D)=FVAR(2) Fixed Sof: H2SB(0.5) C2S(0.5) H2SC(0.5) H2SD(0.5) H2SE(0.5) 5.a Everything fixed: H2SB 5.b Secondary CH2 refined with riding coordinates: C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C21(H21C,H21D), C21(H21A,H21B), C24(H24A,H24B), C24(H24C,H24D), C23(H23A,H23B), C22A(H22A,H22B), C23A(H23C,H23D), C22(H22C,H22D) 5.c Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C20(H20) 5.d Tetrahedral OH refined with riding coordinates: O1S(H1S) 5.e Idealised Me refined as rotating group: C1S(H1SA,H1SB,H1SC), C2S(H2SC,H2SD,H2SE), C25(H25A,H25B,H25C), C25A(H25D,H25E, H25F), C3S(H3SA,H3SB,H3SC) 5.f Idealised tetrahedral OH refined as rotating group: O3S(H3S) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary ? _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9282(6) 0.3911(5) 0.5300(6) 0.0499(15) Uani 1 1 d . . . . . H1 H 0.9707 0.3707 0.5735 0.060 Uiso 1 1 calc R . . . . C2 C 0.8443(6) 0.4795(4) 0.5569(5) 0.0443(13) Uani 1 1 d . . . . . C3 C 0.8083(8) 0.5071(5) 0.6610(6) 0.0593(19) Uani 1 1 d . . . . . H3 H 0.8392 0.4685 0.7092 0.071 Uiso 1 1 calc R . . . . C4 C 0.7302(9) 0.5881(6) 0.6936(6) 0.067(2) Uani 1 1 d . . . . . H4 H 0.7079 0.6060 0.7639 0.080 Uiso 1 1 calc R . . . . C5 C 0.6825(7) 0.6452(5) 0.6250(6) 0.0547(17) Uani 1 1 d . . . . . H5 H 0.6279 0.7020 0.6480 0.066 Uiso 1 1 calc R . . . . C6 C 0.7151(5) 0.6186(4) 0.5236(5) 0.0356(11) Uani 1 1 d . . . . . C7 C 0.7976(5) 0.5364(4) 0.4845(4) 0.0329(11) Uani 1 1 d . . . . . C8 C 0.5736(6) 0.7427(6) 0.4819(6) 0.0563(17) Uani 1 1 d . . . . . H8A H 0.5490 0.7524 0.5584 0.068 Uiso 1 1 calc R . . . . H8B H 0.5067 0.7209 0.4744 0.068 Uiso 1 1 calc R . . . . C9 C 0.6132(7) 0.8391(5) 0.4095(7) 0.0588(18) Uani 1 1 d . . . . . H9A H 0.5497 0.8943 0.4279 0.071 Uiso 1 1 calc R . . . . H9B H 0.6801 0.8610 0.4169 0.071 Uiso 1 1 calc R . . . . C10 C 0.6897(6) 0.9071(5) 0.2230(7) 0.0599(19) Uani 1 1 d . . . . . H10A H 0.7609 0.9266 0.2246 0.072 Uiso 1 1 calc R . . . . H10B H 0.6305 0.9658 0.2392 0.072 Uiso 1 1 calc R . . . . C11 C 0.7159(6) 0.8796(5) 0.1153(7) 0.062(2) Uani 1 1 d . . . . . H11A H 0.6441 0.8628 0.1127 0.074 Uiso 1 1 calc R . . . . H11B H 0.7488 0.9377 0.0579 0.074 Uiso 1 1 calc R . . . . C12 C 0.8373(7) 0.7613(7) -0.0052(6) 0.066(2) Uani 1 1 d . . . . . H12A H 0.9171 0.7282 -0.0266 0.079 Uiso 1 1 calc R . . . . H12B H 0.8398 0.8224 -0.0595 0.079 Uiso 1 1 calc R . . . . C13 C 0.7584(7) 0.6878(7) -0.0045(6) 0.064(2) Uani 1 1 d . . . . . H13A H 0.6797 0.7215 0.0102 0.077 Uiso 1 1 calc R . . . . H13B H 0.7895 0.6615 -0.0752 0.077 Uiso 1 1 calc R . . . . C14 C 0.7091(7) 0.5178(7) 0.0831(6) 0.0600(18) Uani 1 1 d . . . . . C15 C 0.6564(10) 0.5050(9) 0.0174(9) 0.091(3) Uani 1 1 d . . . . . H15 H 0.6442 0.5617 -0.0307 0.109 Uiso 1 1 calc R . . . . C16 C 0.6211(12) 0.4087(12) 0.0216(13) 0.120(5) Uani 1 1 d . . . . . H16 H 0.5861 0.4011 -0.0250 0.144 Uiso 1 1 calc R . . . . C17 C 0.6349(10) 0.3279(9) 0.0885(11) 0.095(4) Uani 1 1 d . . . . . H17 H 0.6094 0.2636 0.0900 0.115 Uiso 1 1 calc R . . . . C18 C 0.6889(7) 0.3376(7) 0.1592(8) 0.069(2) Uani 1 1 d . . . . . C19 C 0.7212(5) 0.4347(6) 0.1591(6) 0.0492(15) Uani 1 1 d . . . . . C20 C 0.7072(7) 0.2428(6) 0.2216(8) 0.069(2) Uani 1 1 d . . . . . H20 H 0.6715 0.1857 0.2194 0.082 Uiso 1 1 calc R . . . . C21 C 0.7726(8) 0.1170(6) 0.3313(9) 0.080(3) Uani 1 1 d D . . . . H21C H 0.7156 0.1076 0.4082 0.096 Uiso 0.349(13) 1 calc R . P A 2 H21D H 0.7594 0.0683 0.2919 0.096 Uiso 0.349(13) 1 calc R . P A 2 H21A H 0.8247 0.0744 0.2746 0.096 Uiso 0.651(13) 1 calc R . P A 1 H21B H 0.6944 0.0903 0.3637 0.096 Uiso 0.651(13) 1 calc R . P A 1 C24 C 1.0345(6) 0.2489(5) 0.4450(7) 0.062(2) Uani 1 1 d D . . . . H24A H 1.0670 0.2429 0.4997 0.075 Uiso 0.651(13) 1 calc R . P A 1 H24B H 1.0992 0.2534 0.3716 0.075 Uiso 0.651(13) 1 calc R . P A 1 H24C H 1.0170 0.2097 0.5180 0.075 Uiso 0.349(13) 1 calc R . P A 2 H24D H 1.1138 0.2727 0.4164 0.075 Uiso 0.349(13) 1 calc R . P A 2 C26 C 1.0556(6) 0.8731(5) 0.1044(6) 0.0567(17) Uani 1 1 d . . . . . Ca Ca 0.76968(9) 0.64690(8) 0.25373(8) 0.0328(2) Uani 1 1 d . . . . . F11 F 1.1631(5) 0.9021(5) 0.0699(5) 0.099(2) Uani 1 1 d . . . . . F12 F 1.0533(4) 0.8301(4) 0.0265(4) 0.0719(12) Uani 1 1 d . . . . . F13 F 0.9838(5) 0.9578(3) 0.1150(4) 0.0799(15) Uani 1 1 d . . . . . N1 N 0.9502(5) 0.3389(4) 0.4543(5) 0.0472(12) Uani 1 1 d . . . . . N2 N 0.7649(5) 0.2255(4) 0.2793(6) 0.0612(17) Uani 1 1 d . . . . . N3 N 0.9168(5) 0.1672(4) 0.3829(5) 0.0592(16) Uani 1 1 d D . . . . O1 O 0.8296(3) 0.5182(3) 0.3836(3) 0.0344(8) Uani 1 1 d . . . . . O1S O 0.5721(4) 0.6230(3) 0.2992(4) 0.0486(10) Uani 1 1 d . . . . . H1S H 0.5381 0.6690 0.2701 0.07(3) Uiso 1 1 calc R . . . . C1S C 0.5011(6) 0.5389(6) 0.3507(8) 0.068(2) Uani 1 1 d . . . . . H1SA H 0.4251 0.5630 0.4033 0.102 Uiso 1 1 calc GR . . . . H1SB H 0.5386 0.4871 0.3884 0.102 Uiso 1 1 calc GR . . . . H1SC H 0.4907 0.5087 0.2960 0.102 Uiso 1 1 calc GR . . . . O2 O 0.7629(4) 0.4509(3) 0.2267(4) 0.0422(9) Uani 1 1 d . . . . . O2S O 0.9650(4) 0.5933(4) 0.1392(4) 0.0495(10) Uani 1 1 d . . . . . H2SA H 1.030(6) 0.610(6) 0.153(6) 0.048(19) Uiso 1 1 d . . . . . H2SB H 0.9988 0.5656 0.0817 0.059 Uiso 0.5 1 d . . P . . C2S C 1.0183(16) 0.5493(15) 0.0484(12) 0.077(5) Uani 0.5 1 d . . P B 2 H2SC H 1.0997 0.5297 0.0356 0.116 Uiso 0.5 1 calc GR . P B 2 H2SD H 1.0151 0.5980 -0.0132 0.116 Uiso 0.5 1 calc GR . P B 2 H2SE H 0.9792 0.4880 0.0564 0.116 Uiso 0.5 1 calc GR . P B 2 O3 O 0.7547(4) 0.6064(4) 0.0805(4) 0.0538(11) Uani 1 1 d . . . . . O4 O 0.7981(4) 0.7926(4) 0.0992(4) 0.0536(11) Uani 1 1 d . . . . . O5 O 0.6468(4) 0.8191(3) 0.3008(4) 0.0461(10) Uani 1 1 d . . . . . O6 O 0.6702(4) 0.6662(3) 0.4506(3) 0.0432(9) Uani 1 1 d . . . . . O7 O 0.9824(4) 0.3629(3) 0.2243(4) 0.0481(10) Uani 1 1 d . . . . . O8 O 0.7124(4) 0.3363(3) 0.4582(4) 0.0499(10) Uani 1 1 d . . . . . O11 O 0.8971(4) 0.7665(3) 0.2634(4) 0.0460(10) Uani 1 1 d . . . . . O12 O 1.0326(5) 0.8461(5) 0.3012(5) 0.0715(15) Uani 1 1 d . . . . . O13 O 1.0973(4) 0.6985(4) 0.2014(5) 0.0634(14) Uani 1 1 d . . . . . S1 S 1.01670(14) 0.78714(12) 0.23235(14) 0.0491(4) Uani 1 1 d . . . . . U U 0.84327(2) 0.35630(2) 0.33831(2) 0.03483(7) Uani 1 1 d . . . . . C23 C 0.9621(9) 0.1583(6) 0.4661(8) 0.060(3) Uani 0.651(13) 1 d D . P A 1 H23A H 1.0110 0.0932 0.4651 0.072 Uiso 0.651(13) 1 calc R . P A 1 H23B H 0.8965 0.1570 0.5387 0.072 Uiso 0.651(13) 1 calc R . P A 1 C25 C 1.0128(9) 0.1300(8) 0.2848(8) 0.059(3) Uani 0.651(13) 1 d D . P A 1 H25A H 0.9885 0.1423 0.2248 0.089 Uiso 0.651(13) 1 calc GR . P A 1 H25B H 1.0309 0.0563 0.3008 0.089 Uiso 0.651(13) 1 calc GR . P A 1 H25C H 1.0820 0.1671 0.2643 0.089 Uiso 0.651(13) 1 calc GR . P A 1 C22A C 0.891(2) 0.1040(15) 0.322(2) 0.102(13) Uani 0.349(13) 1 d D . P A 2 H22A H 0.9073 0.0311 0.3472 0.122 Uiso 0.349(13) 1 calc R . P A 2 H22B H 0.9441 0.1188 0.2448 0.122 Uiso 0.349(13) 1 calc R . P A 2 C23A C 1.0315(14) 0.1751(13) 0.3668(18) 0.064(7) Uani 0.349(13) 1 d D . P A 2 H23C H 1.0775 0.2029 0.2902 0.077 Uiso 0.349(13) 1 calc R . P A 2 H23D H 1.0670 0.1062 0.3819 0.077 Uiso 0.349(13) 1 calc R . P A 2 C25A C 0.8384(19) 0.1369(16) 0.5112(17) 0.079(8) Uani 0.349(13) 1 d D U P A 2 H25D H 0.8404 0.1901 0.5511 0.119 Uiso 0.349(13) 1 calc GR . P A 2 H25E H 0.8692 0.0709 0.5374 0.119 Uiso 0.349(13) 1 calc GR . P A 2 H25F H 0.7579 0.1314 0.5230 0.119 Uiso 0.349(13) 1 calc GR . P A 2 C3S C 0.3443(10) 0.7564(9) 0.2199(12) 0.102(4) Uani 1 1 d . . . . . H3SA H 0.3391 0.8008 0.1566 0.153 Uiso 1 1 calc GR . . . . H3SB H 0.2756 0.7711 0.2856 0.153 Uiso 1 1 calc GR . . . . H3SC H 0.3482 0.6843 0.2107 0.153 Uiso 1 1 calc GR . . . . O3S O 0.4461(5) 0.7752(4) 0.2296(6) 0.0682(15) Uani 1 1 d . . . . . H3S H 0.4294 0.8194 0.2714 0.102 Uiso 1 1 calc GR . . . . C27 C 0.3932(11) 1.0968(8) 0.1755(10) 0.092(3) Uani 1 1 d . . . . . F21 F 0.3133(8) 1.0520(7) 0.1624(8) 0.141(3) Uani 1 1 d . . . . . F22 F 0.4959(7) 1.0666(6) 0.1045(6) 0.119(2) Uani 1 1 d . . . . . F23 F 0.3762(8) 1.1973(5) 0.1514(7) 0.131(3) Uani 1 1 d . . . . . O21 O 0.4740(5) 1.1150(4) 0.3105(5) 0.0650(13) Uani 1 1 d . . . . . O22 O 0.2660(6) 1.1025(5) 0.3796(7) 0.093(2) Uani 1 1 d . . . . . O23 O 0.3996(5) 0.9531(4) 0.3263(5) 0.0649(14) Uani 1 1 d . . . . . S2 S 0.38086(14) 1.06325(12) 0.31364(16) 0.0540(4) Uani 1 1 d . . . . . C22 C 0.8179(8) 0.1060(7) 0.4195(9) 0.067(4) Uani 0.651(13) 1 d D . P A 1 H22C H 0.7553 0.1289 0.4864 0.081 Uiso 0.651(13) 1 calc R . P A 1 H22D H 0.8413 0.0330 0.4368 0.081 Uiso 0.651(13) 1 calc R . P A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.053(4) 0.043(3) 0.056(4) 0.014(3) -0.032(3) -0.004(3) C2 0.057(4) 0.034(3) 0.048(3) 0.007(2) -0.031(3) -0.008(2) C3 0.100(6) 0.041(3) 0.052(4) 0.001(3) -0.051(4) 0.001(3) C4 0.113(7) 0.053(4) 0.049(4) -0.014(3) -0.048(4) 0.005(4) C5 0.082(5) 0.039(3) 0.043(3) -0.007(3) -0.028(3) 0.002(3) C6 0.048(3) 0.027(2) 0.033(3) 0.001(2) -0.019(2) -0.005(2) C7 0.041(3) 0.023(2) 0.035(3) 0.0005(19) -0.018(2) -0.006(2) C8 0.054(4) 0.059(4) 0.045(4) -0.016(3) -0.015(3) 0.021(3) C9 0.066(4) 0.044(4) 0.075(5) -0.025(3) -0.037(4) 0.016(3) C10 0.054(4) 0.030(3) 0.094(6) 0.006(3) -0.036(4) 0.000(3) C11 0.051(4) 0.049(4) 0.069(5) 0.024(3) -0.023(3) -0.003(3) C12 0.064(4) 0.081(5) 0.040(4) 0.016(3) -0.020(3) -0.002(4) C13 0.068(5) 0.085(5) 0.041(4) 0.001(3) -0.030(3) 0.005(4) C14 0.060(4) 0.078(5) 0.055(4) -0.024(4) -0.034(3) 0.005(4) C15 0.105(7) 0.114(8) 0.090(7) -0.024(6) -0.076(6) 0.008(6) C16 0.131(10) 0.142(12) 0.153(13) -0.066(10) -0.109(10) 0.008(9) C17 0.099(7) 0.096(8) 0.137(10) -0.057(7) -0.078(8) 0.003(6) C18 0.059(4) 0.072(5) 0.095(6) -0.045(5) -0.040(4) 0.005(4) C19 0.039(3) 0.063(4) 0.052(4) -0.022(3) -0.022(3) 0.002(3) C20 0.052(4) 0.059(5) 0.104(7) -0.042(5) -0.029(4) -0.002(3) C21 0.078(5) 0.036(4) 0.123(8) -0.013(4) -0.034(6) -0.014(3) C24 0.060(4) 0.051(4) 0.070(5) 0.001(3) -0.033(4) 0.020(3) C26 0.059(4) 0.048(4) 0.060(4) 0.016(3) -0.027(3) -0.014(3) Ca 0.0344(5) 0.0301(5) 0.0315(5) -0.0002(4) -0.0136(4) 0.0001(4) F11 0.080(3) 0.105(4) 0.103(4) 0.046(3) -0.039(3) -0.051(3) F12 0.076(3) 0.080(3) 0.049(2) 0.007(2) -0.020(2) -0.010(2) F13 0.104(4) 0.046(2) 0.076(3) 0.017(2) -0.036(3) 0.001(2) N1 0.048(3) 0.035(3) 0.054(3) 0.002(2) -0.022(2) 0.006(2) N2 0.055(3) 0.029(3) 0.086(5) -0.025(3) -0.009(3) -0.006(2) N3 0.064(4) 0.035(3) 0.054(3) 0.005(2) -0.007(3) 0.002(2) O1 0.0390(19) 0.0295(18) 0.0331(19) -0.0018(14) -0.0158(16) 0.0028(14) O1S 0.039(2) 0.037(2) 0.066(3) -0.008(2) -0.019(2) -0.0004(17) C1S 0.046(4) 0.044(4) 0.087(6) -0.016(4) 0.001(4) -0.006(3) O2 0.044(2) 0.040(2) 0.048(2) -0.0116(17) -0.0233(19) 0.0027(17) O2S 0.038(2) 0.055(3) 0.046(2) -0.0014(19) -0.0107(19) -0.0032(19) C2S 0.073(10) 0.087(12) 0.039(8) -0.007(7) 0.000(7) 0.013(9) O3 0.058(3) 0.068(3) 0.040(2) 0.001(2) -0.028(2) -0.004(2) O4 0.053(3) 0.051(3) 0.051(3) 0.011(2) -0.025(2) 0.000(2) O5 0.054(2) 0.0300(19) 0.055(3) -0.0047(18) -0.026(2) 0.0037(17) O6 0.048(2) 0.044(2) 0.033(2) -0.0070(16) -0.0160(17) 0.0118(18) O7 0.042(2) 0.037(2) 0.050(2) -0.0017(18) -0.0077(19) 0.0026(17) O8 0.047(2) 0.039(2) 0.056(3) -0.0090(19) -0.014(2) 0.0000(18) O11 0.044(2) 0.041(2) 0.053(3) 0.0022(18) -0.023(2) -0.0046(17) O12 0.089(4) 0.073(4) 0.072(4) 0.009(3) -0.051(3) -0.031(3) O13 0.051(3) 0.049(3) 0.087(4) 0.014(2) -0.036(3) -0.001(2) S1 0.0538(8) 0.0444(8) 0.0544(9) 0.0138(7) -0.0325(7) -0.0137(6) U 0.03358(10) 0.02383(9) 0.03673(11) -0.00257(6) -0.00626(7) 0.00056(6) C23 0.074(8) 0.037(5) 0.049(6) 0.004(4) -0.019(6) 0.017(5) C25 0.065(7) 0.036(5) 0.056(6) -0.013(4) -0.008(5) 0.014(5) C22A 0.086(19) 0.021(10) 0.17(4) -0.017(14) -0.03(2) 0.014(10) C23A 0.046(11) 0.033(9) 0.087(17) 0.006(9) -0.015(11) 0.018(8) C25A 0.076(13) 0.037(9) 0.083(14) 0.025(9) -0.008(10) 0.002(9) C3S 0.091(7) 0.090(7) 0.160(12) -0.040(8) -0.080(8) 0.007(6) O3S 0.068(3) 0.054(3) 0.100(5) -0.020(3) -0.051(3) 0.005(2) C27 0.109(8) 0.080(6) 0.104(8) -0.007(6) -0.070(7) 0.018(6) F21 0.170(7) 0.134(6) 0.186(9) -0.017(6) -0.142(7) 0.002(5) F22 0.141(6) 0.131(6) 0.073(4) -0.011(4) -0.041(4) 0.013(5) F23 0.196(8) 0.080(4) 0.142(6) 0.021(4) -0.115(6) 0.016(4) O21 0.071(3) 0.048(3) 0.079(4) -0.013(2) -0.031(3) -0.004(2) O22 0.066(4) 0.060(3) 0.115(6) -0.015(3) -0.005(4) 0.009(3) O23 0.064(3) 0.033(2) 0.089(4) -0.004(2) -0.028(3) 0.004(2) S2 0.0495(8) 0.0347(7) 0.0677(10) -0.0067(7) -0.0178(8) 0.0064(6) C22 0.062(7) 0.026(5) 0.083(9) 0.012(5) -0.007(7) -0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 H1 0.9500 . ? C1 C2 1.457(9) . ? C1 N1 1.268(9) . ? C2 C3 1.408(10) . ? C2 C7 1.422(8) . ? C3 H3 0.9500 . ? C3 C4 1.356(11) . ? C4 H4 0.9500 . ? C4 C5 1.392(10) . ? C5 H5 0.9500 . ? C5 C6 1.373(9) . ? C6 C7 1.410(8) . ? C6 O6 1.377(7) . ? C7 O1 1.328(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C9 1.473(11) . ? C8 O6 1.445(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 O5 1.434(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.476(12) . ? C10 O5 1.425(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 O4 1.425(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 C13 1.495(12) . ? C12 O4 1.426(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 O3 1.430(9) . ? C14 C15 1.381(11) . ? C14 C19 1.415(11) . ? C14 O3 1.374(10) . ? C15 H15 0.9500 . ? C15 C16 1.399(17) . ? C16 H16 0.9500 . ? C16 C17 1.325(19) . ? C17 H17 0.9500 . ? C17 C18 1.443(12) . ? C18 C19 1.409(11) . ? C18 C20 1.438(14) . ? C19 O2 1.315(8) . ? C20 H20 0.9500 . ? C20 N2 1.270(11) . ? C21 H21C 0.9900 . ? C21 H21D 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 N2 1.497(10) . ? C21 C22A 1.45(2) . ? C21 C22 1.531(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 H24C 0.9900 . ? C24 H24D 0.9900 . ? C24 N1 1.474(8) . ? C24 C23 1.531(9) . ? C24 C23A 1.60(2) . ? C26 F11 1.334(9) . ? C26 F12 1.318(10) . ? C26 F13 1.333(9) . ? C26 S1 1.823(7) . ? Ca O1 2.525(4) . ? Ca O1S 2.376(4) . ? Ca O2 2.715(4) . ? Ca O2S 2.396(4) . ? Ca O3 2.627(5) . ? Ca O4 2.535(4) . ? Ca O5 2.600(4) . ? Ca O6 2.495(4) . ? Ca O11 2.486(5) . ? Ca U 3.9229(10) . ? N1 U 2.471(6) . ? N2 U 2.527(6) . ? N3 U 2.612(5) . ? N3 C23 1.469(8) . ? N3 C25 1.490(8) . ? N3 C22A 1.44(2) . ? N3 C23A 1.399(18) . ? N3 C25A 1.618(19) . ? N3 C22 1.450(8) . ? O1 U 2.310(4) . ? O1S H1S 0.8400 . ? O1S C1S 1.419(8) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? O2 U 2.294(4) . ? O2S H2SA 0.99(8) . ? O2S H2SB 0.8456 . ? O2S C2S 1.338(16) . ? C2S H2SB 0.4923 . ? C2S H2SC 0.9800 . ? C2S H2SD 0.9800 . ? C2S H2SE 0.9800 . ? O7 U 1.795(4) . ? O8 U 1.783(4) . ? O11 S1 1.450(4) . ? O12 S1 1.427(6) . ? O13 S1 1.445(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C22A H22A 0.9900 . ? C22A H22B 0.9900 . ? C23A H23C 0.9900 . ? C23A H23D 0.9900 . ? C25A H25D 0.9800 . ? C25A H25E 0.9800 . ? C25A H25F 0.9800 . ? C3S H3SA 0.9800 . ? C3S H3SB 0.9800 . ? C3S H3SC 0.9800 . ? C3S O3S 1.421(11) . ? O3S H3S 0.8400 . ? C27 F21 1.341(14) . ? C27 F22 1.314(13) . ? C27 F23 1.325(12) . ? C27 S2 1.814(12) . ? O21 S2 1.437(6) . ? O22 S2 1.434(6) . ? O23 S2 1.439(5) . ? C22 H22C 0.9900 . ? C22 H22D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1 116.8 . . ? N1 C1 H1 116.8 . . ? N1 C1 C2 126.3(6) . . ? C3 C2 C1 116.7(6) . . ? C3 C2 C7 119.8(6) . . ? C7 C2 C1 123.5(6) . . ? C2 C3 H3 119.4 . . ? C4 C3 C2 121.1(6) . . ? C4 C3 H3 119.4 . . ? C3 C4 H4 119.7 . . ? C3 C4 C5 120.5(7) . . ? C5 C4 H4 119.7 . . ? C4 C5 H5 120.4 . . ? C6 C5 C4 119.3(6) . . ? C6 C5 H5 120.4 . . ? C5 C6 C7 122.7(5) . . ? C5 C6 O6 124.6(5) . . ? O6 C6 C7 112.7(5) . . ? C6 C7 C2 116.6(5) . . ? O1 C7 C2 123.9(5) . . ? O1 C7 C6 119.5(5) . . ? H8A C8 H8B 108.5 . . ? C9 C8 H8A 110.2 . . ? C9 C8 H8B 110.2 . . ? O6 C8 H8A 110.2 . . ? O6 C8 H8B 110.2 . . ? O6 C8 C9 107.3(6) . . ? C8 C9 H9A 110.3 . . ? C8 C9 H9B 110.3 . . ? H9A C9 H9B 108.6 . . ? O5 C9 C8 106.9(6) . . ? O5 C9 H9A 110.3 . . ? O5 C9 H9B 110.3 . . ? H10A C10 H10B 108.5 . . ? C11 C10 H10A 110.3 . . ? C11 C10 H10B 110.3 . . ? O5 C10 H10A 110.3 . . ? O5 C10 H10B 110.3 . . ? O5 C10 C11 107.2(6) . . ? C10 C11 H11A 110.3 . . ? C10 C11 H11B 110.3 . . ? H11A C11 H11B 108.5 . . ? O4 C11 C10 107.2(6) . . ? O4 C11 H11A 110.3 . . ? O4 C11 H11B 110.3 . . ? H12A C12 H12B 108.1 . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? O4 C12 H12A 109.5 . . ? O4 C12 H12B 109.5 . . ? O4 C12 C13 110.9(6) . . ? C12 C13 H13A 110.7 . . ? C12 C13 H13B 110.7 . . ? H13A C13 H13B 108.8 . . ? O3 C13 C12 105.1(6) . . ? O3 C13 H13A 110.7 . . ? O3 C13 H13B 110.7 . . ? C15 C14 C19 119.8(9) . . ? O3 C14 C15 125.4(9) . . ? O3 C14 C19 114.9(6) . . ? C14 C15 H15 119.9 . . ? C14 C15 C16 120.2(11) . . ? C16 C15 H15 119.9 . . ? C15 C16 H16 119.0 . . ? C17 C16 C15 121.9(10) . . ? C17 C16 H16 119.0 . . ? C16 C17 H17 120.0 . . ? C16 C17 C18 119.9(10) . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 119.0(9) . . ? C19 C18 C20 126.4(7) . . ? C20 C18 C17 114.5(8) . . ? C18 C19 C14 118.9(7) . . ? O2 C19 C14 118.7(6) . . ? O2 C19 C18 122.4(7) . . ? C18 C20 H20 115.8 . . ? N2 C20 C18 128.4(7) . . ? N2 C20 H20 115.8 . . ? H21C C21 H21D 109.2 . . ? H21A C21 H21B 107.8 . . ? N2 C21 H21C 111.3 . . ? N2 C21 H21D 111.3 . . ? N2 C21 H21A 108.9 . . ? N2 C21 H21B 108.9 . . ? N2 C21 C22 113.2(7) . . ? C22A C21 H21C 111.3 . . ? C22A C21 H21D 111.3 . . ? C22A C21 N2 102.4(11) . . ? C22 C21 H21A 108.9 . . ? C22 C21 H21B 108.9 . . ? H24A C24 H24B 109.0 . . ? H24C C24 H24D 107.9 . . ? N1 C24 H24A 111.1 . . ? N1 C24 H24B 111.1 . . ? N1 C24 H24C 109.2 . . ? N1 C24 H24D 109.2 . . ? N1 C24 C23 103.5(6) . . ? N1 C24 C23A 112.1(8) . . ? C23 C24 H24A 111.1 . . ? C23 C24 H24B 111.1 . . ? C23A C24 H24C 109.2 . . ? C23A C24 H24D 109.2 . . ? F11 C26 S1 110.3(5) . . ? F12 C26 F11 107.1(7) . . ? F12 C26 F13 107.2(6) . . ? F12 C26 S1 112.8(5) . . ? F13 C26 F11 107.6(6) . . ? F13 C26 S1 111.6(5) . . ? O1 Ca O2 68.35(13) . . ? O1 Ca O3 125.53(14) . . ? O1 Ca O4 155.52(15) . . ? O1 Ca O5 124.94(14) . . ? O1 Ca U 33.98(9) . . ? O1S Ca O1 106.59(15) . . ? O1S Ca O2 73.31(14) . . ? O1S Ca O2S 142.47(17) . . ? O1S Ca O3 71.64(16) . . ? O1S Ca O4 97.89(16) . . ? O1S Ca O5 71.28(14) . . ? O1S Ca O6 76.57(16) . . ? O1S Ca O11 142.61(15) . . ? O1S Ca U 93.60(11) . . ? O2 Ca U 34.78(9) . . ? O2S Ca O1 77.83(14) . . ? O2S Ca O2 74.17(15) . . ? O2S Ca O3 75.82(16) . . ? O2S Ca O4 83.14(16) . . ? O2S Ca O5 137.34(16) . . ? O2S Ca O6 132.89(16) . . ? O2S Ca O11 73.69(16) . . ? O2S Ca U 69.03(11) . . ? O3 Ca O2 58.96(14) . . ? O3 Ca U 91.80(11) . . ? O4 Ca O2 120.88(16) . . ? O4 Ca O3 62.80(17) . . ? O4 Ca O5 62.57(15) . . ? O4 Ca U 146.59(12) . . ? O5 Ca O2 144.51(14) . . ? O5 Ca O3 106.44(15) . . ? O5 Ca U 150.43(11) . . ? O6 Ca O1 62.39(12) . . ? O6 Ca O2 109.93(14) . . ? O6 Ca O3 148.15(16) . . ? O6 Ca O4 124.90(16) . . ? O6 Ca O5 63.92(14) . . ? O6 Ca U 88.26(10) . . ? O11 Ca O1 87.15(13) . . ? O11 Ca O2 142.91(13) . . ? O11 Ca O3 128.13(16) . . ? O11 Ca O4 72.69(16) . . ? O11 Ca O5 72.40(14) . . ? O11 Ca O6 79.86(16) . . ? O11 Ca U 114.35(10) . . ? C1 N1 C24 117.3(6) . . ? C1 N1 U 126.1(4) . . ? C24 N1 U 115.9(5) . . ? C20 N2 C21 116.1(7) . . ? C20 N2 U 127.4(5) . . ? C21 N2 U 115.9(6) . . ? C23 N3 U 111.2(4) . . ? C23 N3 C25 107.3(7) . . ? C25 N3 U 111.1(5) . . ? C22A N3 U 107.9(10) . . ? C22A N3 C25A 109.2(12) . . ? C23A N3 U 103.8(7) . . ? C23A N3 C22A 121.1(12) . . ? C23A N3 C25A 109.1(13) . . ? C25A N3 U 104.3(8) . . ? C22 N3 U 106.2(5) . . ? C22 N3 C23 111.5(6) . . ? C22 N3 C25 109.6(7) . . ? C7 O1 Ca 119.9(3) . . ? C7 O1 U 123.4(3) . . ? U O1 Ca 108.36(15) . . ? Ca O1S H1S 115.5 . . ? C1S O1S Ca 134.0(4) . . ? C1S O1S H1S 109.5 . . ? O1S C1S H1SA 109.5 . . ? O1S C1S H1SB 109.5 . . ? O1S C1S H1SC 109.5 . . ? H1SA C1S H1SB 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? C19 O2 Ca 119.0(4) . . ? C19 O2 U 138.2(4) . . ? U O2 Ca 102.78(15) . . ? Ca O2S H2SA 119(4) . . ? Ca O2S H2SB 137.0 . . ? H2SA O2S H2SB 103.4 . . ? C2S O2S Ca 136.9(10) . . ? C2S O2S H2SA 103(4) . . ? C2S O2S H2SB 0.1 . . ? O2S C2S H2SB 0.2 . . ? O2S C2S H2SC 109.5 . . ? O2S C2S H2SD 109.5 . . ? O2S C2S H2SE 109.5 . . ? H2SB C2S H2SC 109.4 . . ? H2SB C2S H2SD 109.3 . . ? H2SB C2S H2SE 109.7 . . ? H2SC C2S H2SD 109.5 . . ? H2SC C2S H2SE 109.5 . . ? H2SD C2S H2SE 109.5 . . ? C13 O3 Ca 119.6(5) . . ? C14 O3 C13 116.8(6) . . ? C14 O3 Ca 120.7(4) . . ? C11 O4 C12 113.4(6) . . ? C11 O4 Ca 119.4(4) . . ? C12 O4 Ca 114.9(4) . . ? C9 O5 Ca 115.2(4) . . ? C10 O5 C9 111.8(6) . . ? C10 O5 Ca 115.6(4) . . ? C6 O6 C8 120.5(5) . . ? C6 O6 Ca 122.0(3) . . ? C8 O6 Ca 116.7(4) . . ? S1 O11 Ca 144.6(3) . . ? O11 S1 C26 104.6(3) . . ? O12 S1 C26 103.2(4) . . ? O12 S1 O11 114.8(3) . . ? O12 S1 O13 116.5(4) . . ? O13 S1 C26 102.7(3) . . ? O13 S1 O11 112.9(3) . . ? N1 U Ca 110.49(12) . . ? N1 U N2 132.2(2) . . ? N1 U N3 66.63(18) . . ? N2 U Ca 117.10(16) . . ? N2 U N3 66.4(2) . . ? N3 U Ca 173.57(12) . . ? O1 U Ca 37.66(9) . . ? O1 U N1 74.43(15) . . ? O1 U N2 150.02(18) . . ? O1 U N3 140.77(17) . . ? O2 U Ca 42.45(10) . . ? O2 U N1 152.54(16) . . ? O2 U N2 75.2(2) . . ? O2 U N3 139.60(17) . . ? O2 U O1 79.60(14) . . ? O7 U Ca 89.38(13) . . ? O7 U N1 86.8(2) . . ? O7 U N2 97.1(2) . . ? O7 U N3 84.76(17) . . ? O7 U O1 97.98(17) . . ? O7 U O2 88.07(18) . . ? O8 U Ca 97.12(14) . . ? O8 U N1 88.8(2) . . ? O8 U N2 82.0(2) . . ? O8 U N3 88.65(18) . . ? O8 U O1 85.91(17) . . ? O8 U O2 98.25(19) . . ? O8 U O7 173.12(19) . . ? C24 C23 H23A 109.6 . . ? C24 C23 H23B 109.6 . . ? N3 C23 C24 110.4(6) . . ? N3 C23 H23A 109.6 . . ? N3 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C21 C22A H22A 108.4 . . ? C21 C22A H22B 108.4 . . ? N3 C22A C21 115.6(16) . . ? N3 C22A H22A 108.4 . . ? N3 C22A H22B 108.4 . . ? H22A C22A H22B 107.4 . . ? C24 C23A H23C 109.6 . . ? C24 C23A H23D 109.6 . . ? N3 C23A C24 110.4(12) . . ? N3 C23A H23C 109.6 . . ? N3 C23A H23D 109.6 . . ? H23C C23A H23D 108.1 . . ? N3 C25A H25D 109.5 . . ? N3 C25A H25E 109.5 . . ? N3 C25A H25F 109.5 . . ? H25D C25A H25E 109.5 . . ? H25D C25A H25F 109.5 . . ? H25E C25A H25F 109.5 . . ? H3SA C3S H3SB 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? O3S C3S H3SA 109.5 . . ? O3S C3S H3SB 109.5 . . ? O3S C3S H3SC 109.5 . . ? C3S O3S H3S 109.5 . . ? F21 C27 S2 110.5(9) . . ? F22 C27 F21 107.4(11) . . ? F22 C27 F23 108.3(11) . . ? F22 C27 S2 111.8(7) . . ? F23 C27 F21 107.5(9) . . ? F23 C27 S2 111.1(9) . . ? O21 S2 C27 102.2(5) . . ? O21 S2 O23 113.8(3) . . ? O22 S2 C27 104.6(5) . . ? O22 S2 O21 115.2(4) . . ? O22 S2 O23 115.1(4) . . ? O23 S2 C27 103.7(5) . . ? C21 C22 H22C 109.6 . . ? C21 C22 H22D 109.6 . . ? N3 C22 C21 110.2(7) . . ? N3 C22 H22C 109.6 . . ? N3 C22 H22D 109.6 . . ? H22C C22 H22D 108.1 . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma -1 0 0 164.97 9.37 1 0 0 169.86 9.37 2 0 0 96.28 5.55 -3 0 0 6.76 0.57 3 0 0 8.24 0.74 -4 0 0 3.68 0.45 4 0 0 5.14 0.64 -5 0 0 39.35 2.51 5 0 0 41.39 2.88 -6 0 0 89.31 5.5 -6 0 0 101.04 6.22 -7 0 0 44.7 2.64 -7 0 0 43.77 3.52 -7 0 0 45.28 2.8 -8 0 0 1.14 0.36 -8 0 0 1.01 0.26 -8 0 0 0.31 0.76 -8 0 0 1.34 0.43 -9 0 0 41.44 2.61 -9 0 0 43.88 2.51 -9 0 0 37.77 3.91 -9 0 0 40.45 2.67 -9 0 0 35.25 2.71 -10 0 0 28.14 2.25 -10 0 0 24.67 2.02 -10 0 0 27.81 2.6 -10 0 0 29.15 2.03 -10 0 0 31.38 2.42 -10 0 0 28.08 2.12 -10 0 0 30.49 1.9 -10 0 0 25.83 2.02 -10 0 0 27.89 2.05 -10 0 0 22.2 3.45 -10 0 0 29.07 2.05 -11 0 0 1.07 0.65 -11 0 0 1.18 0.44 -11 0 0 1.42 0.66 -11 0 0 2.16 0.49 -11 0 0 1.03 0.86 -11 0 0 1.86 0.5 -11 0 0 1.17 0.52 -11 0 0 1.8 0.56 -12 0 0 10.53 1.02 -12 0 0 10.89 1.06 -12 0 0 10.97 1.04 -12 0 0 7.87 1.27 -12 0 0 9.71 1.54 -13 0 0 18 1.41 -13 0 0 21.25 1.43 -13 1 0 7.93 0.83 -13 1 0 7.65 0.83 -12 1 0 0.47 0.46 -12 1 0 0.87 0.49 -12 1 0 1.41 0.46 -12 1 0 0.58 0.59 -12 1 0 1.54 0.91 -11 1 0 24.91 2.13 -11 1 0 26.56 1.89 -11 1 0 25.12 1.81 -11 1 0 26.61 1.87 -11 1 0 26.63 2.21 -11 1 0 26.34 1.9 -11 1 0 26.17 1.91 -11 1 0 22.7 2.53 -11 1 0 25.29 1.78 -11 1 0 27.17 1.96 -10 1 0 38.04 4.38 -10 1 0 45.89 2.82 -10 1 0 41.48 2.87 -10 1 0 46.96 2.74 -10 1 0 44.19 2.72 -10 1 0 45.74 2.85 -10 1 0 42.59 3.04 -10 1 0 39.93 2.83 -10 1 0 46.24 3.51 -10 1 0 38.43 2.71 -9 1 0 0.43 1.12 -9 1 0 0.74 0.51 -9 1 0 0.82 0.34 -9 1 0 1.35 0.53 -8 1 0 48.09 2.93 -8 1 0 49.19 2.76 -8 1 0 40.62 3.79 -8 1 0 43.47 3.93 -7 1 0 125.5 7.83 -7 1 0 116.23 6.91 -7 1 0 116.81 6.78 -6 1 0 2.97 0.46 5 -1 0 46.26 3.2 -5 1 0 44.38 3.19 -5 1 0 44.54 2.79 4 -1 0 13.59 0.9 4 -1 0 14.66 1.28 -4 1 0 13.63 1.01 3 -1 0 21.76 1.31 3 -1 0 23.08 1.62 -3 1 0 21.02 1.38 2 -1 0 31.64 1.82 -2 1 0 22.63 1.61 1 -1 0 168.15 9.51 1 -1 0 179.32 9.99 -1 1 0 157.22 9.87 -1 1 0 155.68 9.5 -1 1 0 184.05 9.76 0 -1 0 123 6.89 0 -1 0 121.52 7.36 0 1 0 125.88 7.39 -1 -1 0 11.4 0.68 1 1 0 11.35 0.7 -2 -1 0 920.58 52.91 -2 -1 0 945.64 52.97 2 1 0 1000 52.99 -3 -1 0 303.96 17.99 3 1 0 341.49 18.17 -4 -1 0 1.09 0.3 4 1 0 0.94 0.32 -5 -1 0 48.96 3.5 -5 -1 0 68.51 4.07 -6 -1 0 59.67 3.67 -6 -1 0 63.1 4.33 -6 -1 0 62.31 3.79 -7 -1 0 3.43 0.41 -7 -1 0 3.04 0.53 -8 -1 0 91.07 6.37 -8 -1 0 88.3 5.12 -8 -1 0 88.25 5.24 -8 -1 0 87.7 5.31 -9 -1 0 23.12 3.03 -9 -1 0 29.07 1.93 -9 -1 0 27.77 1.77 -9 -1 0 26.88 2.01 -9 -1 0 25.89 2.41 -10 -1 0 2.39 0.47 -10 -1 0 0.69 1.33 -10 -1 0 3.51 0.49 -10 -1 0 2.31 1.01 -10 -1 0 4.26 0.75 -10 -1 0 1.48 0.75 -10 -1 0 2.88 0.68 -10 -1 0 1.81 0.73 -10 -1 0 1.54 0.78 -10 -1 0 2.17 0.71 -10 -1 0 3.07 0.71 -11 -1 0 5.88 0.7 -11 -1 0 5.73 0.97 -11 -1 0 6.57 1.02 -11 -1 0 7.27 1.19 -11 -1 0 6.93 0.84 -11 -1 0 6.48 0.84 -11 -1 0 5 1.21 -11 -1 0 6.68 0.97 -11 -1 0 8.78 0.94 -11 -1 0 6.61 0.92 -11 -1 0 8.37 1.22 -12 -1 0 19.53 2.01 -12 -1 0 17.52 1.3 -12 -1 0 21.66 1.51 -12 -1 0 18.24 1.47 -12 -1 0 20.39 1.51 -12 -1 0 19.09 1.75 -13 -1 0 0.92 0.67 -13 -1 0 1.48 0.44 -13 -1 0 2.01 0.44 -13 2 0 0.22 0.36 -13 2 0 0.52 0.32 -12 2 0 11.28 1.09 -12 2 0 10.08 1.01 -12 2 0 11.14 1.3 -12 2 0 9.91 1.07 -12 2 0 12.24 1.16 -11 2 0 10.75 1.1 -11 2 0 9.94 1.16 -11 2 0 11.21 1.01 -11 2 0 10.55 1.05 -11 2 0 10.23 1.22 -11 2 0 10.59 1.07 -11 2 0 11.43 1.85 -10 2 0 12.56 1.2 -10 2 0 12.26 1.29 -10 2 0 13.14 1.5 -10 2 0 11.57 0.97 -10 2 0 10.07 1.04 -10 2 0 13.93 1.97 -10 2 0 8.61 1.2 -10 2 0 11.5 1.13 -10 2 0 11.97 1.03 -10 2 0 11.28 1.19 -9 2 0 6.14 0.95 -9 2 0 3.89 1.45 -9 2 0 5.84 0.71 -9 2 0 6.48 0.85 -9 2 0 4.46 1.54 -8 2 0 98.77 6.62 -8 2 0 92.23 5.52 -8 2 0 89.6 6.58 -8 2 0 91.11 5.34 -7 2 0 8.42 0.69 -7 2 0 8.39 0.82 -6 2 0 27.8 2.47 -6 2 0 27.6 1.72 -6 2 0 29.82 1.86 5 -2 0 203.9 11.56 -5 2 0 216.36 12.19 -5 2 0 196.61 11.67 4 -2 0 8.97 0.99 4 -2 0 8.49 0.63 -4 2 0 7.94 0.71 3 -2 0 29.57 1.72 3 -2 0 30.93 2.07 -3 2 0 25.21 1.76 2 -2 0 8 1.27 2 -2 0 7.69 0.54 2 -2 0 7.86 0.74 1 -2 0 16.93 1.12 1 -2 0 15.07 1.73 -1 2 0 15.92 1.99 0 -2 0 52.2 3.18 0 -2 0 53.88 4.01 0 2 0 58.03 5.13 -1 -2 0 304.1 17.95 -1 -2 0 340.21 18.75 -2 -2 0 46.28 2.54 -2 -2 0 44.19 2.6 2 2 0 41.92 2.59 -3 -2 0 59.87 3.68 3 2 0 65.84 3.75 -4 -2 0 49.32 2.98 -5 -2 0 233.9 13.6 -5 -2 0 230.41 13.15 -6 -2 0 26.22 1.78 -6 -2 0 28.25 1.92 -7 -2 0 26.76 1.83 -7 -2 0 26.33 1.64 -7 -2 0 25.74 1.76 -8 -2 0 58.12 3.39 -8 -2 0 52.39 4.45 -8 -2 0 58.32 3.52 -8 -2 0 59.51 3.62 -9 -2 0 25.14 1.64 -9 -2 0 23.57 1.89 -9 -2 0 24.52 1.92 -9 -2 0 24.69 1.8 -10 -2 0 39.69 2.78 -10 -2 0 39.11 2.71 -10 -2 0 43.45 2.8 -10 -2 0 41.8 2.63 -10 -2 0 38.18 2.63 -10 -2 0 48.95 3.2 -10 -2 0 42.8 3.3 -10 -2 0 37.95 2.55 -10 -2 0 49.06 3.48 -10 -2 0 43.7 3.03 -10 -2 0 40.67 2.65 -10 -2 0 47.34 2.79 -10 -2 0 39.96 2.94 -10 -2 0 36.05 4.24 -11 -2 0 13.48 1.29 -11 -2 0 14.19 1.16 -11 -2 0 13.68 1.85 -11 -2 0 14.8 1.4 -11 -2 0 13.48 1.08 -11 -2 0 15.95 1.86 -11 -2 0 14.19 1.28 -11 -2 0 13.83 1.29 -11 -2 0 14.37 1.61 -11 -2 0 14.44 1.59 -11 -2 0 14.51 1.3 -12 -2 0 1.72 0.86 -12 -2 0 2.24 0.73 -12 -2 0 2.36 0.56 -12 -2 0 2.8 0.42 -12 -2 0 2.1 0.53 -12 -2 0 2.64 0.52 -12 -2 0 2.29 0.45 -13 -2 0 2.51 0.43 -13 -2 0 2.28 0.82 -13 3 0 11.94 0.95 -13 3 0 13.07 0.98 -12 3 0 16.55 1.31 -12 3 0 17.41 1.32 -12 3 0 18.3 1.44 -12 3 0 15.42 1.38 -12 3 0 17.14 1.27 -11 3 0 1.02 0.39 -11 3 0 1.12 0.51 -11 3 0 1.17 0.43 -11 3 0 1.75 0.59 -11 3 0 1.52 0.44 -11 3 0 1.57 0.54 -10 3 0 14.32 1.15 -10 3 0 14.23 1.02 -10 3 0 12.76 1.93 -10 3 0 13.64 1.3 -10 3 0 12.81 1.21 -10 3 0 9.26 2.29 -10 3 0 13.76 1.09 -10 3 0 13.34 1.27 -10 3 0 10.34 1.48 -10 3 0 14.22 1.13 -10 3 0 14.34 1.42 -9 3 0 18.22 1.27 -9 3 0 18.41 2.86 -9 3 0 14.88 2.54 -9 3 0 16.21 1.53 -8 3 0 5.59 0.77 -8 3 0 5.75 0.63 -8 3 0 8.59 1.77 -7 3 0 18.8 3.99 -7 3 0 18.46 1.38 -7 3 0 18.62 1.23 -6 3 0 36.06 2.34 -6 3 0 38.73 2.49 -6 3 0 45.6 3.28 5 -3 0 60.8 3.93 -5 3 0 76.56 4.63 -5 3 0 71.76 4.09 -5 3 0 60.68 3.95 4 -3 0 1.13 0.26 4 -3 0 0.9 0.47 -4 3 0 0.62 0.3 -4 3 0 0.4 0.42 3 -3 0 155.27 8.72 3 -3 0 154.09 9.13 2 -3 0 483.87 26.28 2 -3 0 487.7 26.6 -2 3 0 483.72 27.59 -2 3 0 436.57 28.14 1 -3 0 5.51 0.58 1 -3 0 5.44 0.43 1 -3 0 5.81 1.27 -1 3 0 5.67 1.23 0 -3 0 61.56 3.7 0 -3 0 65.19 4.98 -1 -3 0 9.84 0.61 -1 -3 0 8.08 0.7 -1 -3 0 9.98 0.63 -2 -3 0 37.45 2.3 -3 -3 0 11 0.85 -4 -3 0 181.44 10.08 -4 -3 0 173.81 10.13 -5 -3 0 52.77 3.11 -5 -3 0 45.79 3.43 -5 -3 0 49.55 3.01 -6 -3 0 16.12 1.25 -6 -3 0 16.43 1.34 -7 -3 0 74.96 4.41 -7 -3 0 71.39 5.25 -7 -3 0 78.28 4.54 -7 -3 0 72.69 4.28 -8 -3 0 15.1 1.33 -8 -3 0 13.67 1.04 -8 -3 0 13.88 1.19 -9 -3 0 10.99 1.11 -9 -3 0 9.85 1.24 -9 -3 0 10.3 0.92 -9 -3 0 11.76 2.22 -10 -3 0 34.13 2.35 -10 -3 0 37.86 2.52 -10 -3 0 40.27 2.67 -10 -3 0 33.72 3.06 -10 -3 0 41.74 2.47 -10 -3 0 37.66 2.35 -10 -3 0 32.91 2.43 -10 -3 0 37.12 2.35 -10 -3 0 35.88 2.38 -10 -3 0 36.17 2.49 -10 -3 0 31.31 4.93 -10 -3 0 31.34 2.55 -10 -3 0 37.51 2.71 -10 -3 0 35.75 2.26 -11 -3 0 25.73 1.82 -11 -3 0 31.95 2.64 -11 -3 0 24.71 1.9 -11 -3 0 27.69 1.96 -11 -3 0 26.7 1.9 -11 -3 0 25.02 2.18 -11 -3 0 22.58 2.39 -11 -3 0 26.65 1.76 -11 -3 0 26.23 1.9 -11 -3 0 30.58 2.1 -12 -3 0 2.65 0.5 -12 -3 0 2.42 0.51 -12 -3 0 4.14 0.85 -12 -3 0 3.1 0.6 -12 -3 0 1.9 0.4 -12 -3 0 3.16 0.99 -13 -3 0 14.83 1.59 -13 -3 0 17 1.17 -13 4 0 12.94 0.95 -12 4 0 5.38 0.7 -12 4 0 3.98 0.62 -12 4 0 4.63 0.73 -12 4 0 5.75 0.72 -12 4 0 4.86 0.78 -12 4 0 4.27 0.66 -11 4 0 14.35 1.19 -11 4 0 16 1.3 -11 4 0 15.09 1.21 -11 4 0 16.13 1.44 -11 4 0 13.4 1.28 -11 4 0 14.65 1.1 -10 4 0 53.67 3.02 -10 4 0 50.35 3.2 -10 4 0 45.43 3.09 -10 4 0 53.13 3.1 -10 4 0 54.77 3.09 -10 4 0 49.15 3.36 -10 4 0 46.03 3.4 -10 4 0 43.36 4.8 -10 4 0 55.17 3.26 -9 4 0 27.35 1.64 -9 4 0 24.42 3.49 -9 4 0 23.91 2.12 -9 4 0 24.59 1.98 -9 4 0 23.82 1.84 -8 4 0 13.27 1.52 -8 4 0 12.16 2.57 -8 4 0 12.74 3.19 -7 4 0 68.55 5 -7 4 0 68.81 5.3 -7 4 0 63.81 4.05 6 -4 0 8.82 0.89 -6 4 0 11.64 1.02 -6 4 0 9.07 0.9 -6 4 0 12.21 1.59 5 -4 0 57.26 3.12 -5 4 0 51.71 3.09 -5 4 0 44.27 3.25 4 -4 0 68.2 3.89 -4 4 0 63.35 3.81 -4 4 0 66.37 4.16 3 -4 0 20.64 1.4 3 -4 0 19.87 1.78 -3 4 0 25.48 1.77 2 -4 0 1.89 0.44 2 -4 0 1.74 0.25 -2 4 0 1.05 1.16 1 -4 0 115.88 6.98 1 -4 0 115.17 6.73 1 -4 0 123.92 8.96 -1 4 0 122.14 9.66 0 -4 0 387.13 21.31 0 -4 0 391.86 21.47 0 -4 0 370.93 23.39 -1 -4 0 16.25 1.01 -1 -4 0 16.57 1.18 -2 -4 0 182.36 10.37 -3 -4 0 85.62 4.62 -3 -4 0 61.63 4.35 -4 -4 0 17.8 1.42 -5 -4 0 96.96 5.65 -5 -4 0 91.9 5.57 -6 -4 0 58.64 4.35 -6 -4 0 61.21 3.79 -6 -4 0 63.37 3.87 -7 -4 0 8.29 0.94 -7 -4 0 8.61 0.81 -8 -4 0 12.53 1.33 -8 -4 0 13.6 1.18 -8 -4 0 17.35 2.21 -9 -4 0 28.25 1.98 -9 -4 0 26.58 2.21 -10 -4 0 12.24 1.41 -10 -4 0 10.76 1.89 -10 -4 0 14.63 1.86 -10 -4 0 11 1.36 -10 -4 0 15.42 1.34 -10 -4 0 12.52 0.99 -10 -4 0 12.67 1.28 -10 -4 0 10.61 1.15 -10 -4 0 12.39 1.18 -10 -4 0 12.18 1.27 -10 -4 0 14.72 1.61 -10 -4 0 12.31 1.13 -11 -4 0 0.33 0.42 -11 -4 0 0.46 0.66 -11 -4 0 -0.38 0.34 -11 -4 0 0.84 0.37 -11 -4 0 0.49 0.29 -11 -4 0 0.05 0.73 -11 -4 0 0.19 0.43 -11 -4 0 0.26 0.81 -11 -4 0 0.38 0.54 -12 -4 0 9.78 0.91 -12 -4 0 8.04 1.49 -12 -4 0 10.43 1.29 -13 -4 0 9.85 1.29 -13 -4 0 11.7 0.89 -12 5 0 2.18 0.52 -12 5 0 1.45 0.43 -12 5 0 1.35 0.36 -12 5 0 2.02 0.44 -12 5 0 1.95 0.33 -12 5 0 2.51 0.42 -11 5 0 14.06 1.22 -11 5 0 15.28 1.5 -11 5 0 15.9 1.3 -11 5 0 15.93 1.19 -11 5 0 15.37 1.11 -11 5 0 16.56 1.33 -10 5 0 26.03 1.95 -10 5 0 26.66 1.85 -10 5 0 27.89 1.75 -10 5 0 25.37 2.13 -10 5 0 29.77 1.83 -10 5 0 28.99 2.23 -10 5 0 29.25 1.98 -10 5 0 25.35 1.89 -9 5 0 7.42 0.85 -9 5 0 4.78 0.97 -9 5 0 7.37 0.81 -9 5 0 7.9 0.99 -9 5 0 7.32 0.96 -9 5 0 8.61 0.74 -9 5 0 7.58 1.3 -8 5 0 83 6.36 -8 5 0 76.5 4.99 -7 5 0 61.67 5.25 6 -5 0 3.39 0.61 -6 5 0 3.07 0.58 -6 5 0 1.89 1.46 -6 5 0 2.64 0.69 5 -5 0 49.89 3.07 -5 5 0 46.21 2.93 -5 5 0 54.36 3.44 -5 5 0 47.85 3.05 4 -5 0 12.49 0.95 -4 5 0 12.36 0.91 -4 5 0 11.62 0.96 3 -5 0 98.17 6.32 3 -5 0 103.64 5.67 -3 5 0 103.44 6.13 -3 5 0 100.14 5.64 -3 5 0 85.2 6.6 2 -5 0 360.07 19.6 2 -5 0 372.54 20.07 -2 5 0 323.66 23.46 -2 5 0 346.3 19.65 1 -5 0 170.58 9.92 1 -5 0 182.67 10.26 -1 5 0 175.42 13.74 0 -5 0 4.62 0.61 0 -5 0 5.16 0.45 -1 -5 0 17.9 1.13 -1 -5 0 18.25 1.33 -2 -5 0 137.97 8.73 -2 -5 0 165.66 9.14 -3 -5 0 28.58 1.96 -3 -5 0 28.94 1.78 -3 -5 0 28.01 2.19 -4 -5 0 14.19 0.99 -4 -5 0 15.06 1.25 -5 -5 0 174.8 10.62 -5 -5 0 210.63 10.78 -5 -5 0 163.68 10.52 -6 -5 0 3.32 0.65 -6 -5 0 2.99 0.53 -6 -5 0 3.78 0.75 -7 -5 0 23.08 1.83 -7 -5 0 23.05 1.63 -8 -5 0 72.66 4.46 -8 -5 0 74.45 4.7 -9 -5 0 4.68 0.67 -9 -5 0 5.32 0.86 -9 -5 0 6.92 1.16 -10 -5 0 7.86 1.51 -10 -5 0 6.63 0.86 -10 -5 0 5.8 1.23 -10 -5 0 6.67 1.01 -10 -5 0 6.31 0.91 -10 -5 0 6.97 1.11 -10 -5 0 6.36 0.97 -10 -5 0 5.85 0.72 -10 -5 0 7.88 0.98 -11 -5 0 12.67 1.76 -11 -5 0 12.12 1.03 -11 -5 0 13.79 1.1 -11 -5 0 12.5 1.14 -11 -5 0 11.7 1.32 -11 -5 0 12.43 1.47 -12 -5 0 6.77 1.11 -12 -5 0 6.77 0.8 -12 -5 0 7.24 0.76 -12 -5 0 6.46 1.25 -13 -5 0 0.05 0.25 -13 -5 0 0.61 0.54 -12 6 0 12.39 1 -12 6 0 12.47 0.91 -12 6 0 12.2 0.86 -11 6 0 4.14 0.53 -11 6 0 3.45 0.59 -11 6 0 3.82 0.54 -11 6 0 3.82 0.5 -11 6 0 3.55 0.57 -11 6 0 3.7 0.75 -10 6 0 2.63 0.7 -10 6 0 2.6 0.53 -10 6 0 2.43 0.43 -10 6 0 1.47 0.76 -10 6 0 1.3 0.47 -10 6 0 1.63 0.46 -10 6 0 1.81 0.51 -10 6 0 2.83 0.41 -9 6 0 21.25 1.67 -9 6 0 19.85 1.52 -9 6 0 21.93 1.44 -9 6 0 23.3 1.62 -9 6 0 19.01 1.96 -9 6 0 19.85 1.95 -9 6 0 20.01 1.64 -9 6 0 23.15 1.34 -9 6 0 20.96 1.47 -8 6 0 48.97 3.62 -8 6 0 58.4 3.2 -8 6 0 51.65 3.58 -8 6 0 54.45 3.68 -8 6 0 55.64 3.4 -7 6 0 7.79 1.32 6 -6 0 102.05 5.8 -6 6 0 91.55 6.05 5 -6 0 58.85 3.73 -5 6 0 61.46 4.19 -5 6 0 60.63 3.72 -5 6 0 61.99 3.62 4 -6 0 1.29 0.36 -4 6 0 0.95 0.58 -4 6 0 0.96 0.36 -4 6 0 1.38 0.33 3 -6 0 59.45 3.56 -3 6 0 59.8 3.54 -3 6 0 57.71 3.56 2 -6 0 125.2 6.79 -2 6 0 111.01 6.79 1 -6 0 19.75 1.3 -1 6 0 19.12 1.36 0 -6 0 61.27 6.24 0 -6 0 57.43 3.67 0 -6 0 58.34 3.46 -1 -6 0 91.66 5.6 -1 -6 0 96.12 5.47 -1 -6 0 93.77 8.11 -2 -6 0 10.5 0.81 -2 -6 0 8.85 0.94 -3 -6 0 6.15 0.81 -3 -6 0 6.36 0.62 -4 -6 0 86.55 5.58 -4 -6 0 82.72 5.21 -4 -6 0 86.45 5.53 -4 -6 0 85.45 4.96 -5 -6 0 25.83 2.05 -5 -6 0 27.67 2.25 -6 -6 0 4.69 0.64 -6 -6 0 5.98 0.97 -7 -6 0 54.53 3.38 -8 -6 0 31.23 2.17 -9 -6 0 0.39 0.55 -9 -6 0 0.47 0.32 -9 -6 0 0.26 0.46 -9 -6 0 0.81 0.45 -9 -6 0 0.78 0.56 -9 -6 0 0.25 0.76 -9 -6 0 0.49 0.5 -9 -6 0 0.73 0.41 -10 -6 0 27.95 1.91 -10 -6 0 29.44 2.01 -10 -6 0 30.35 2 -10 -6 0 29.71 2.19 -10 -6 0 27.73 1.93 -10 -6 0 29.21 2.13 -10 -6 0 25.7 1.86 -10 -6 0 28.65 2.58 -11 -6 0 12.38 1.79 -11 -6 0 16.56 1.21 -11 -6 0 15.71 1.24 -12 -6 0 0.37 0.31 -12 -6 0 0.78 0.32 -12 -6 0 1.06 0.69 -13 -6 0 9.98 0.78 -11 7 0 1.29 0.4 -11 7 0 0.93 0.38 -11 7 0 1.55 0.56 -11 7 0 0.65 0.34 -11 7 0 1.47 0.3 -10 7 0 13.89 1.33 -10 7 0 15.37 1.6 -10 7 0 15.54 1.51 -10 7 0 15.65 1.25 -10 7 0 16.54 1.29 -10 7 0 16.45 1.1 -10 7 0 14.52 1.26 -10 7 0 16.17 1.15 -9 7 0 17.69 1.15 -9 7 0 16.74 1.09 -9 7 0 16.25 1.79 -9 7 0 17.08 1.39 -9 7 0 16.95 1.24 -9 7 0 14.19 1.69 -9 7 0 16.05 1.39 -9 7 0 16.34 1.45 -8 7 0 5.07 0.76 -8 7 0 3.71 1.01 -8 7 0 4.35 0.56 -8 7 0 4.11 0.75 -8 7 0 5.78 1.7 -8 7 0 3.68 0.87 -8 7 0 5.06 0.58 -8 7 0 4.91 0.77 -7 7 0 24.66 2.12 -7 7 0 22.14 1.98 -6 7 0 36.27 2.94 5 -7 0 62 3.93 -5 7 0 66.5 3.83 -5 7 0 63.6 4.27 -5 7 0 60.99 4.49 4 -7 0 18.8 1.45 -4 7 0 18.99 1.44 -4 7 0 19.4 1.41 3 -7 0 52.55 3.23 -3 7 0 53.66 3.23 -3 7 0 49.78 3.23 2 -7 0 27.88 1.85 -2 7 0 25.38 1.88 -2 7 0 29.51 1.89 1 -7 0 19.87 1.63 1 -7 0 19.49 1.38 -1 7 0 20.31 1.46 0 -7 0 365.1 21.92 0 -7 0 403.56 22.13 0 -7 0 404.14 21.86 -1 -7 0 14.25 1.13 -1 -7 0 15.67 1.35 -2 -7 0 52 3.39 -2 -7 0 51.23 3.17 -3 -7 0 106.88 6.73 -3 -7 0 122.17 7.32 -3 -7 0 106.88 6.49 -4 -7 0 46.96 3.93 -4 -7 0 61.39 3.64 -4 -7 0 60.96 3.33 -4 -7 0 47.22 3.91 -6 -7 0 108.33 6.5 -6 -7 0 115.24 7 -7 -7 0 44.67 2.87 -7 -7 0 44.62 2.8 -8 -7 0 0.82 0.54 -9 -7 0 18.48 1.46 -9 -7 0 15.94 1.3 -9 -7 0 15.88 1.38 -10 -7 0 17.64 1.35 -10 -7 0 19.25 1.42 -10 -7 0 18.58 1.43 -10 -7 0 13.86 1.94 -11 -7 0 0.58 0.76 -11 -7 0 1.47 0.38 -11 -7 0 1.48 0.37 -11 -7 0 0.77 0.39 -12 -7 0 7.4 0.72 -12 -7 0 8.34 0.7 -12 -7 0 7.09 1.14 -11 8 0 11.52 0.82 -11 8 0 12.38 0.94 -11 8 0 10.57 0.95 -11 8 0 11.02 0.92 -10 8 0 18.72 1.65 -10 8 0 19.27 1.67 -10 8 0 20.3 1.41 -10 8 0 17.87 1.4 -10 8 0 18.68 1.3 -10 8 0 19.18 1.26 -10 8 0 19.65 1.45 -9 8 0 2.46 0.34 -9 8 0 2.66 0.37 -9 8 0 1.61 0.66 -9 8 0 2.04 0.53 -9 8 0 1.96 0.51 -9 8 0 0.79 0.74 -8 8 0 24.5 2.21 -8 8 0 27.01 1.91 -8 8 0 24.99 1.87 -8 8 0 25.23 2.71 -8 8 0 24.41 2.15 -8 8 0 25.89 1.63 -7 8 0 75.43 4.51 -7 8 0 68.11 4.7 -7 8 0 74.59 4.46 -7 8 0 78.36 4.31 -7 8 0 76.84 4.25 -7 8 0 63.38 4.72 -6 8 0 1.68 0.78 -6 8 0 2.6 1.01 -5 8 0 28.06 1.87 -5 8 0 24.24 2.55 4 -8 0 28.72 2.07 -4 8 0 29.47 2.02 -4 8 0 28.18 2.08 3 -8 0 36.02 2.49 -3 8 0 37.28 2.52 -3 8 0 39.11 2.51 2 -8 0 8.85 1.19 2 -8 0 8.05 0.83 -2 8 0 9.17 0.92 -2 8 0 8.11 0.95 1 -8 0 91.53 5.34 1 -8 0 89.48 5.6 -1 8 0 89.97 5.41 0 -8 0 41.76 2.88 0 -8 0 40.09 2.66 -1 -8 0 0.54 0.53 -1 -8 0 0.76 0.35 -2 -8 0 90.77 5.25 -2 -8 0 84.18 5.43 -3 -8 0 92.48 5.44 -3 -8 0 89.73 5.69 -4 -8 0 7.73 0.87 -4 -8 0 8.25 1.19 -5 -8 0 43.74 3.68 -6 -8 0 28.24 2.79 -7 -8 0 0.53 0.54 -7 -8 0 0.08 0.22 -8 -8 0 84.2 5.36 -8 -8 0 73.27 4.61 -8 -8 0 68.32 4.51 -8 -8 0 67.4 4.58 -8 -8 0 82.79 4.59 -9 -8 0 34.89 3.07 -9 -8 0 34.55 2.49 -9 -8 0 39.61 2.45 -9 -8 0 38.41 2.44 -10 -8 0 3.15 0.55 -10 -8 0 3.77 0.53 -10 -8 0 2.18 1.34 -10 -8 0 3.17 0.57 -11 -8 0 6.17 0.7 -11 -8 0 5.97 0.71 -11 -8 0 7.31 0.68 -11 -8 0 4.04 1.11 -12 -8 0 9.84 0.71 -12 -8 0 8.05 0.72 -10 9 0 1.99 0.47 -10 9 0 1.48 0.65 -10 9 0 1.84 0.29 -10 9 0 1.68 0.41 -10 9 0 1.88 0.44 -9 9 0 6.52 0.89 -9 9 0 6.9 0.64 -9 9 0 6.68 1 -9 9 0 7.5 1.11 -9 9 0 8.57 0.91 -9 9 0 7.75 0.65 -8 9 0 36.41 2.86 -8 9 0 34.49 2.75 -8 9 0 40.51 2.56 -8 9 0 40.28 2.33 -8 9 0 43.46 2.61 -8 9 0 33.96 3.35 -7 9 0 2.56 0.96 -7 9 0 4.59 0.63 -7 9 0 4.19 0.68 -7 9 0 4.37 0.5 -7 9 0 4.18 0.72 -6 9 0 16.85 1.53 -6 9 0 18.93 1.94 -6 9 0 18.06 1.55 -6 9 0 15.41 1.75 -6 9 0 17.23 1.27 -6 9 0 14.93 1.43 -6 9 0 16.77 1.14 -5 9 0 49.04 4.02 -5 9 0 48.59 3.07 -5 9 0 44.17 3.28 -4 9 0 42.39 2.83 3 -9 0 23.59 2.01 -3 9 0 25.81 1.93 -3 9 0 26.72 1.92 2 -9 0 82.66 4.97 -2 9 0 78.31 4.98 -2 9 0 83.63 5.04 1 -9 0 23.35 2.1 -1 9 0 26.12 1.91 0 -9 0 11.78 1.15 0 -9 0 12.47 1.44 -1 -9 0 66.4 4.47 -1 -9 0 69.5 4.26 -2 -9 0 7.19 1.16 -2 -9 0 6.07 0.88 -3 -9 0 1.82 0.53 -4 -9 0 5.73 0.88 -5 -9 0 50.46 4.59 -5 -9 0 56.41 3.6 -5 -9 0 63.22 3.36 -6 -9 0 0.52 0.23 -6 -9 0 0.19 0.49 -6 -9 0 1 1.23 -7 -9 0 27.83 1.86 -7 -9 0 28.37 2.06 -7 -9 0 32.55 2.85 -7 -9 0 26.72 2.14 -7 -9 0 27.46 1.97 -7 -9 0 32.88 2.16 -7 -9 0 36.25 2.32 -8 -9 0 46.5 3.47 -8 -9 0 43.06 2.71 -8 -9 0 39.75 2.83 -8 -9 0 39.79 2.67 -8 -9 0 40.37 2.77 -8 -9 0 39.1 2.59 -9 -9 0 11.74 1.65 -9 -9 0 12.06 1.18 -9 -9 0 8.3 1.2 -9 -9 0 9.74 0.96 -9 -9 0 12.37 1.05 -9 -9 0 10.16 1.07 -10 -9 0 9.8 0.92 -10 -9 0 9.78 0.95 -10 -9 0 10.38 0.97 -11 -9 0 17.18 1.09 -11 -9 0 16.4 1.15 -11 -9 0 14.58 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1.86 0 -11 3 19.69 1.76 0 -11 3 17.52 1.3 0 -11 3 16.22 1.41 0 -11 3 17.51 1.42 -1 11 -3 10.89 1.64 -1 11 -3 12 1.01 -1 11 -3 11.06 1.29 -1 11 -3 12.41 2.36 1 -11 3 10.93 1.09 1 -11 3 9.78 1.12 1 -11 3 11.13 1.11 1 -11 3 13.56 1.49 1 -11 3 10.79 1.11 -2 11 -3 28.21 2.09 -2 11 -3 28.48 2.01 -2 11 -3 27.19 2.48 -2 11 -3 24.89 2.38 -2 11 -3 31.46 3.61 -2 11 -3 24.74 2.2 2 -11 3 27.69 2.94 2 -11 3 29.26 1.92 -3 11 -3 3.4 0.75 -3 11 -3 3.81 0.86 -3 11 -3 2.76 1.03 -3 11 -3 3.03 0.79 3 -11 3 2.17 1.25 3 -11 3 3.38 0.61 -4 11 -3 48.67 3.35 -4 11 -3 50.53 3.38 -4 11 -3 54.61 3.27 4 -11 3 50.55 3.9 4 -11 3 49.19 3.11 -5 11 -3 12.01 1.25 -5 11 -3 12.22 1.36 -5 11 -3 11.07 0.87 -5 11 -3 10.25 1.06 5 -11 3 10.23 1.72 5 -11 3 11.35 1.03 -6 11 -3 8.55 1.15 -6 11 -3 7.88 0.69 -6 11 -3 7.33 0.83 -6 11 -3 7.01 1.15 6 -11 3 8.42 1.43 -7 11 -3 38.7 2.34 -7 11 -3 34.97 2.58 -7 11 -3 34.41 2.53 -7 11 -3 37.85 2.58 -7 11 -3 38.63 2.23 -8 11 -3 4.87 0.86 -8 11 -3 5.19 0.56 -8 11 -3 5.21 0.77 -8 11 -3 4.95 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3 50.34 3.05 -3 -10 3 54.29 3.52 -3 -10 3 51.44 3.24 2 10 -3 3.42 1.75 -2 -10 3 3.15 0.82 -2 -10 3 2.3 0.51 -2 -10 3 4.01 0.71 -2 -10 3 5.63 1.97 -1 -10 3 33.64 2.51 -1 -10 3 30.14 2.2 0 -10 3 43.12 2.95 0 -10 3 48.51 3.31 0 -10 3 47.38 2.95 1 -10 3 -0.22 0.45 1 -10 3 0.23 0.57 -2 10 -3 43.46 3.25 -2 10 -3 43.98 3.13 -3 10 -3 15.61 1.83 -3 10 -3 16.46 1.64 -3 10 -3 13.62 1.52 -4 10 -3 14.87 1.5 -4 10 -3 13.18 1.46 -4 10 -3 13.7 1.04 -4 10 -3 15.37 1.78 -4 10 -3 16.1 1.53 4 -10 3 14.96 2.09 4 -10 3 13.72 1.22 -5 10 -3 1.26 0.44 -5 10 -3 0.67 0.68 -5 10 -3 0.91 0.3 -5 10 -3 0.66 0.77 -5 10 -3 0.83 0.63 -5 10 -3 0.38 0.62 5 -10 3 0.87 0.94 5 -10 3 0.97 0.4 -6 10 -3 31.53 1.88 -6 10 -3 30.92 2.05 -6 10 -3 29.15 2.22 -6 10 -3 30.15 2.33 -6 10 -3 28.15 2.28 6 -10 3 30.29 2.63 -7 10 -3 6.63 1.03 -7 10 -3 6.14 0.68 -7 10 -3 4.52 0.85 -7 10 -3 5.82 0.6 -7 10 -3 5.16 0.89 -8 10 -3 0.97 0.29 -8 10 -3 1.82 0.36 -8 10 -3 0.38 0.61 -8 10 -3 0.79 0.33 -8 10 -3 1.75 0.6 -8 10 -3 0.71 0.54 -9 10 -3 21.65 1.35 -9 10 -3 19.92 1.36 -9 10 -3 20.39 1.62 -9 10 -3 20.63 1.6 -10 10 -3 14.23 0.88 -10 10 -3 10.9 0.9 -10 10 -3 13.01 1.18 -10 10 -3 12.24 1.08 -10 -9 3 11.63 1.56 -9 -9 3 2.31 0.58 -9 -9 3 2.21 0.69 -8 -9 3 15.7 1.12 -8 -9 3 13.77 1.32 -8 -9 3 15.46 1.08 -8 -9 3 13.52 1.09 -8 -9 3 15.76 1.75 -7 -9 3 2.04 0.43 -7 -9 3 2.55 0.38 -7 -9 3 2.93 0.43 -7 -9 3 3.1 0.76 -7 -9 3 2.77 0.49 -7 -9 3 2.15 0.81 -6 -9 3 0.06 0.36 -6 -9 3 0.39 0.66 -6 -9 3 0.33 0.67 -6 -9 3 0.03 0.42 -6 -9 3 0.4 0.49 -6 -9 3 0.53 0.33 -6 -9 3 0.01 0.34 -5 -9 3 31.46 2.51 -5 -9 3 30.59 2.02 -5 -9 3 33.48 2.13 -5 -9 3 31.23 2.1 -5 -9 3 35.68 3.06 -5 -9 3 29.38 2.06 -5 -9 3 32.4 2.28 -4 -9 3 27.47 1.99 -4 -9 3 29.11 1.86 -4 -9 3 22.86 3.65 -4 -9 3 26.87 1.76 -4 -9 3 26.64 3.95 -3 -9 3 23.58 1.86 -3 -9 3 22.21 1.55 -3 -9 3 22.76 1.74 -2 -9 3 17.01 1.51 -2 -9 3 20.55 1.71 -1 -9 3 84.83 5.32 0 -9 3 0.75 0.55 -2 9 -3 72.86 4.63 -3 9 -3 32.8 2.64 -3 9 -3 35.57 2.5 -4 9 -3 23.09 2.09 -4 9 -3 23.84 1.9 -5 9 -3 25.2 1.51 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51.61 2.99 -6 -8 3 50.3 3.51 -5 -8 3 52.2 3.2 -5 -8 3 44.22 3.87 -5 -8 3 51.43 2.96 -4 -8 3 4.13 0.73 -4 -8 3 3.82 0.55 -4 -8 3 6.2 1.67 -3 -8 3 47.49 2.98 -3 -8 3 41.45 4.12 -2 -8 3 74.82 4.66 -1 -8 3 5.02 0.83 -1 -8 3 3.7 0.88 0 -8 3 5.11 0.86 0 -8 3 5.97 1.1 1 -8 3 43.37 3.12 1 -8 3 42.33 2.94 -2 8 -3 7.35 0.97 2 -8 3 7.64 1.33 -3 8 -3 54.12 3.9 -3 8 -3 65.33 4.16 3 -8 3 69.41 3.99 -4 8 -3 105.46 6.24 -4 8 -3 105.76 6.44 4 -8 3 100.92 6.24 -5 8 -3 78.94 4.96 -5 8 -3 75.11 4.69 -6 8 -3 5.16 0.77 -6 8 -3 4.82 0.99 -6 8 -3 5.45 1.45 -7 8 -3 34.77 2.08 -7 8 -3 33.08 2.09 -7 8 -3 27.31 2.34 -7 8 -3 32.1 2.38 -7 8 -3 32.68 1.97 -7 8 -3 30.72 2.48 -8 8 -3 7.07 1.22 -8 8 -3 6.44 0.63 -8 8 -3 6.96 0.71 -8 8 -3 5.67 1.28 -8 8 -3 6.99 0.78 -8 8 -3 6.26 1.02 -9 8 -3 0.69 0.31 -9 8 -3 0.26 0.3 -9 8 -3 0.58 0.43 -9 8 -3 0 0.56 -10 8 -3 14.94 1.52 -10 8 -3 16.57 1.37 -10 8 -3 16.54 1.13 -10 8 -3 16.84 1.18 -11 8 -3 14.38 1.07 -11 8 -3 15.35 1.33 -11 8 -3 16.07 1.04 -11 8 -3 14.16 1.18 -11 -7 3 0.15 0.41 -11 -7 3 -0.22 0.4 -10 -7 3 7.75 1.16 -10 -7 3 8.04 1.16 -9 -7 3 22.01 2.17 -8 -7 3 3.01 0.77 -8 -7 3 1.84 0.93 -8 -7 3 1.48 0.76 -7 -7 3 7.29 0.92 -7 -7 3 9.71 1.24 -7 -7 3 9.45 1.57 -7 -7 3 6.86 1.29 -7 -7 3 8.34 0.71 -6 -7 3 36.42 2.22 -5 -7 3 11.46 0.93 -5 -7 3 15.1 1.99 -4 -7 3 35.96 3.34 -3 -7 3 147.76 9.76 -3 -7 3 151.52 8.69 -2 -7 3 28.73 2.18 -2 -7 3 27.99 2.01 -1 -7 3 29.62 2.14 -1 -7 3 31.32 2.27 0 -7 3 88.67 5.57 0 -7 3 91.54 5.46 1 -7 3 6.81 1.02 1 -7 3 6.14 0.8 -2 7 -3 20.4 1.57 2 -7 3 20.2 1.5 -3 7 -3 57.81 4.03 -3 7 -3 67.57 3.94 3 -7 3 64.05 3.9 -4 7 -3 88.23 5.61 -4 7 -3 92.43 5.45 4 -7 3 93.23 5.49 -5 7 -3 3.09 0.75 -5 7 -3 2.9 0.58 5 -7 3 2.21 0.61 -6 7 -3 42.45 3.45 -6 7 -3 41.5 2.68 -6 7 -3 43.8 3.01 -7 7 -3 60.43 4.59 -7 7 -3 73.7 4.38 -8 7 -3 2.03 0.39 -8 7 -3 2.52 0.4 -8 7 -3 1.48 0.59 -8 7 -3 2.6 0.46 -8 7 -3 2.49 0.74 -8 7 -3 2.71 0.76 -9 7 -3 26.32 2.25 -9 7 -3 30.83 1.93 -9 7 -3 30.21 2.07 -9 7 -3 33.1 2.22 -9 7 -3 29.99 1.89 -10 7 -3 27.55 2.04 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3.49 -8 7 -4 51.44 3.06 -8 7 -4 48.01 2.98 -9 7 -4 49.22 2.77 -9 7 -4 41.14 3.13 -9 7 -4 51.94 2.99 -9 7 -4 46.74 2.81 -9 7 -4 41.49 3.06 -10 7 -4 2.96 0.76 -10 7 -4 3.15 0.41 -10 7 -4 1.91 0.54 -10 7 -4 2.07 0.58 -10 7 -4 2.77 0.44 -11 7 -4 14.53 1.09 -11 7 -4 13.6 1.01 -11 7 -4 14.98 1.22 -11 7 -4 13.35 1.33 -12 7 -4 10.89 1.04 -12 7 -4 11.97 0.91 -12 7 -4 11.22 0.96 -12 7 -4 11.89 0.87 -12 7 -4 13.12 1.16 -10 -6 4 0.75 0.56 -10 -6 4 0.64 0.5 -9 -6 4 10.35 1.5 -9 -6 4 14.44 1.58 -8 -6 4 14.01 1.53 -8 -6 4 15.73 1.84 -8 -6 4 13.64 1.72 -7 -6 4 1.97 0.69 -7 -6 4 0.51 0.85 -7 -6 4 0.69 0.72 -7 -6 4 0.7 0.26 -7 -6 4 1.42 0.39 -6 -6 4 25.8 1.64 -5 -6 4 102.59 5.87 -4 -6 4 82.67 5.85 -3 -6 4 0.8 0.89 -3 -6 4 1.03 0.41 -2 -6 4 62.47 3.89 -1 -6 4 36.3 2.44 -1 -6 4 34.56 2.38 -1 -6 4 33.83 2.39 0 -6 4 1.54 0.5 0 -6 4 2.02 0.61 1 -6 4 125.52 7.6 1 -6 4 132.69 7.67 -2 6 -4 50.96 3.29 2 -6 4 52.31 3.22 -3 6 -4 1.86 0.57 -3 6 -4 1.66 0.43 3 -6 4 2.63 0.54 -4 6 -4 45.7 3.23 -4 6 -4 52.28 3.12 4 -6 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3.99 1.04 -7 -5 4 10.76 1.54 -7 -5 4 13.21 1.91 -7 -5 4 14.04 1.36 -7 -5 4 14.13 0.96 -7 -5 4 12.99 1.12 -7 -5 4 16.24 1.92 -6 -5 4 38.99 2.63 -6 -5 4 41.14 2.27 -6 -5 4 30.52 4.03 -5 -5 4 3.64 1.6 -4 -5 4 8.72 2.14 -4 -5 4 10.17 1.61 -3 -5 4 58.51 3.41 -3 -5 4 52.33 4.6 -3 -5 4 54.56 4.26 -2 -5 4 103.01 7.08 -2 -5 4 105.55 6.93 -2 -5 4 97.74 5.94 -2 -5 4 97.47 5.93 -1 -5 4 0.98 0.37 -1 -5 4 0.39 0.8 0 -5 4 15.83 1.3 0 -5 4 16.03 3.16 0 -5 4 17.08 1.34 1 -5 4 48.04 3.14 1 -5 4 51.12 3.03 -2 5 -4 0.35 0.29 2 -5 4 0.73 0.31 -3 5 -4 139.99 8.71 -3 5 -4 153.6 8.66 3 -5 4 156.66 8.64 -4 5 -4 92.93 5.87 -4 5 -4 102.72 5.8 4 -5 4 99.65 5.8 -5 5 -4 4.25 0.55 -5 5 -4 4.2 0.76 5 -5 4 4.04 0.59 -6 5 -4 31.31 2.33 -6 5 -4 38.36 2.89 -6 5 -4 32.39 2.14 6 -5 4 32.37 2.28 -7 5 -4 23 2.07 -7 5 -4 22.83 1.82 -7 5 -4 23.21 3.27 7 -5 4 23.16 1.76 -8 5 -4 2.6 0.71 -8 5 -4 1.87 1.57 -9 5 -4 3.17 0.77 -9 5 -4 2.15 0.73 -9 5 -4 1.34 1.76 -9 5 -4 2.77 0.43 -9 5 -4 2.37 0.49 -10 5 -4 13.39 1.53 -10 5 -4 14.13 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-3 -15 6.91 1 -7 -3 -15 7.18 0.71 7 3 15 7.84 1.68 -8 -3 -15 11.35 1.2 -8 -3 -15 10.93 1.02 8 3 15 9.02 1.73 8 3 15 12.74 0.88 -9 -3 -15 0.89 0.45 -9 -3 -15 0.13 0.27 -9 -3 -15 0.68 0.48 9 3 15 0.56 0.85 9 3 15 0.85 0.27 -10 -3 -15 9.57 0.73 -10 -3 -15 9.11 1.01 -10 -3 -15 7.78 0.9 10 3 15 8.67 0.7 -11 -3 -15 1.79 0.5 -11 -3 -15 2.46 0.51 -11 -3 -15 2.12 0.34 11 3 15 3.44 0.42 -1 -4 -15 1.29 0.6 -1 -4 -15 1.84 0.28 1 4 15 3.22 0.42 1 4 15 0.92 0.45 -2 -4 -15 3.17 0.9 -2 -4 -15 3.31 0.4 2 4 15 2.75 0.59 -3 -4 -15 7.9 0.73 -3 -4 -15 7.24 1.42 3 4 15 5.75 0.92 -4 -4 -15 0.6 0.96 -4 -4 -15 2 0.43 4 4 15 0.88 1.29 -5 -4 -15 0.76 0.92 -5 -4 -15 0.14 0.35 5 4 15 0.35 1.16 -6 -4 -15 3.75 0.73 6 4 15 6.2 1.43 -7 -4 -15 2.6 0.47 -7 -4 -15 4.06 0.69 7 4 15 3.3 1.08 -8 -4 -15 0.37 0.4 -8 -4 -15 0.58 0.53 8 4 15 0.32 0.87 8 4 15 0.05 0.28 -9 -4 -15 1.65 0.32 -9 -4 -15 1.33 0.47 -9 -4 -15 2.64 0.61 9 4 15 1.66 0.88 9 4 15 1.81 0.32 -10 -4 -15 8.2 0.94 -10 -4 -15 8.51 1.06 -10 -4 -15 11.85 0.79 10 4 15 9.98 0.76 -11 -4 -15 1.21 0.46 -11 -4 -15 1.7 0.29 -11 -4 -15 0.55 0.46 11 4 15 1.63 0.26 1 5 15 1.64 0.46 -2 -5 -15 10.78 1.34 -2 -5 -15 8.6 0.87 -2 -5 -15 9.42 0.73 2 5 15 9.08 0.98 -3 -5 -15 5.26 1.11 -3 -5 -15 7.3 0.69 -3 -5 -15 7.53 0.79 3 5 15 6.21 0.93 -4 -5 -15 1.22 0.97 -4 -5 -15 0.62 0.32 4 5 15 1.73 1.23 -5 -5 -15 10.31 0.89 -5 -5 -15 8.31 1.76 5 5 15 11.47 2.06 -6 -5 -15 3.87 0.71 6 5 15 6.02 1.37 -7 -5 -15 1.23 0.37 -7 -5 -15 1.24 0.55 7 5 15 1.77 1 -8 -5 -15 2.82 0.55 -8 -5 -15 3.22 0.65 -8 -5 -15 3.13 0.49 8 5 15 2.66 0.97 8 5 15 3.91 0.52 -9 -5 -15 2.29 0.62 -9 -5 -15 3.73 0.55 -9 -5 -15 4.2 0.49 9 5 15 4.52 0.49 -10 -5 -15 0.46 0.24 -10 -5 -15 0.76 0.48 10 5 15 0.58 0.26 -11 -5 -15 0.06 0.43 -11 -5 -15 0.26 0.42 -11 -5 -15 0.56 0.22 11 5 15 0.22 0.21 -2 -6 -15 2.26 0.77 -2 -6 -15 3.43 0.46 -2 -6 -15 3.34 0.53 2 6 15 1.65 0.54 2 6 15 3.52 0.6 -3 -6 -15 0.37 0.29 -3 -6 -15 -0.39 0.79 -3 -6 -15 0.44 0.36 -4 -6 -15 6.08 0.71 -4 -6 -15 6.13 0.8 -4 -6 -15 5.99 1.32 4 6 15 5.57 1.32 -5 -6 -15 10.3 1.04 -5 -6 -15 11.22 0.93 5 6 15 11.84 2.09 -6 -6 -15 0.99 0.49 -6 -6 -15 1.26 0.47 6 6 15 0.98 1.04 -7 -6 -15 6.93 0.62 -7 -6 -15 5.49 0.82 7 6 15 6.71 1.31 -8 -6 -15 6.92 0.6 -8 -6 -15 5.79 0.86 8 6 15 6.98 1.42 8 6 15 7.22 0.63 -9 -6 -15 0.43 0.46 -9 -6 -15 0.44 0.25 9 6 15 0.05 0.25 -10 -6 -15 3.43 0.43 -10 -6 -15 3.75 0.66 10 6 15 3.99 0.46 -11 -6 -15 3.47 0.66 -11 -6 -15 3.74 0.53 11 6 15 4.59 0.43 -2 -7 -15 1.39 0.44 -2 -7 -15 1.6 0.73 -2 -7 -15 0.86 0.32 -3 -7 -15 6.03 0.59 -3 -7 -15 5.12 0.66 -3 -7 -15 4.11 1.03 3 7 15 4.2 1.17 -4 -7 -15 4.39 0.61 -4 -7 -15 2.35 1.07 -4 -7 -15 4.31 0.67 4 7 15 3.63 1.18 -5 -7 -15 0.45 0.36 -5 -7 -15 -0.36 0.97 -5 -7 -15 0.5 0.41 5 7 15 0.88 1.03 -6 -7 -15 0.66 0.55 -6 -7 -15 1.62 0.45 -6 -7 -15 0.81 0.31 6 7 15 1.53 1.1 -7 -7 -15 5.68 0.78 -7 -7 -15 4.68 0.48 -7 -7 -15 4.42 0.5 -7 -7 -15 4.04 0.73 7 7 15 7.52 1.49 -8 -7 -15 0.65 0.53 -8 -7 -15 1.97 0.54 -8 -7 -15 2.11 0.31 8 7 15 1.08 0.78 -9 -7 -15 1.01 0.53 -9 -7 -15 1.09 0.25 -9 -7 -15 1.08 0.46 9 7 15 1.41 0.29 -10 -7 -15 8.98 0.69 -10 -7 -15 9.38 0.99 10 7 15 10.21 0.71 -3 -8 -15 4.9 1.01 -3 -8 -15 7.42 0.64 -3 -8 -15 5.54 0.74 -4 -8 -15 -0.01 0.35 -4 -8 -15 -0.13 0.83 -4 -8 -15 -0.28 0.3 4 8 15 0.75 0.9 -5 -8 -15 5.04 0.65 -5 -8 -15 6.78 0.86 -5 -8 -15 4.81 0.51 -5 -8 -15 4.86 0.68 -5 -8 -15 4.95 1.18 5 8 15 5.9 1.29 -6 -8 -15 3.23 0.43 -6 -8 -15 2.94 0.61 -6 -8 -15 3.83 0.61 6 8 15 2.5 0.99 -7 -8 -15 0.69 0.25 -7 -8 -15 0.33 0.48 -7 -8 -15 0.32 0.46 -7 -8 -15 0.27 0.39 7 8 15 0.44 0.79 -8 -8 -15 0.67 0.22 -8 -8 -15 0.2 0.38 -8 -8 -15 0.68 0.46 8 8 15 0.68 0.74 -9 -8 -15 1.62 0.5 -9 -8 -15 2.29 0.5 -9 -8 -15 2.25 0.31 9 8 15 2.14 0.33 -5 -9 -15 9.14 0.82 5 9 15 8.08 1.58 -6 -9 -15 2.33 0.34 -6 -9 -15 2.33 0.49 6 9 15 2.04 0.81 -7 -9 -15 1.87 0.47 -7 -9 -15 1.51 0.29 7 9 15 2.16 0.77 -8 -9 -15 4.76 0.85 -8 -9 -15 3.91 0.5 -8 -9 -15 4.51 0.92 6 -1 16 7.65 1.47 7 -1 16 4.41 1.14 -4 0 -16 1.74 0.36 -4 0 -16 0.52 0.74 -5 0 -16 1.76 0.81 -5 0 -16 0.72 0.33 5 0 16 1.14 0.91 -6 0 -16 4.5 0.96 -6 0 -16 6.4 0.64 6 0 16 5.01 1.14 -7 0 -16 0.33 0.32 7 0 16 0.79 0.74 -8 0 -16 3.36 0.48 -8 0 -16 3.61 0.74 8 0 16 3.03 0.89 -4 -1 -16 0.93 0.33 -4 -1 -16 0.44 0.69 4 1 16 0.39 1.22 -5 -1 -16 1.81 0.83 -5 -1 -16 1.66 0.37 5 1 16 0.76 1 -6 -1 -16 0.47 0.79 -6 -1 -16 0.48 0.32 6 1 16 0.32 0.93 -7 -1 -16 1.06 0.46 7 1 16 2.72 0.88 -8 -1 -16 3.11 0.53 8 1 16 2.5 0.79 -9 -1 -16 4.91 0.52 -9 -1 -16 4.22 0.68 -3 -2 -16 6.21 1.09 -3 -2 -16 6.37 0.65 -4 -2 -16 11.38 1.44 -4 -2 -16 12.83 0.89 4 2 16 10.66 1.79 -5 -2 -16 1.14 0.79 -5 -2 -16 0.96 0.34 5 2 16 0.16 0.91 -6 -2 -16 2.57 0.94 -6 -2 -16 1.3 0.36 6 2 16 1.83 1.06 -7 -2 -16 5.12 0.71 7 2 16 3.99 1.07 -8 -2 -16 0.24 0.39 8 2 16 1.38 0.72 -9 -2 -16 1.29 0.28 -9 -2 -16 1.61 0.41 -3 -3 -16 4.38 0.54 -3 -3 -16 4.29 0.84 -4 -3 -16 6.05 1.26 -4 -3 -16 6.43 0.6 4 3 16 3.94 1.19 -5 -3 -16 -0.01 0.8 -5 -3 -16 0.64 0.31 5 3 16 -0.21 0.94 -6 -3 -16 7.56 1.32 -6 -3 -16 9.87 0.78 6 3 16 7.77 1.71 -7 -3 -16 2.19 0.49 7 3 16 2.35 0.95 -8 -3 -16 0.86 0.42 8 3 16 0.61 0.75 -9 -3 -16 4.88 0.5 -9 -3 -16 5.56 0.73 -10 -3 -16 1.97 0.54 -10 -3 -16 1.29 0.65 -3 -4 -16 0.23 0.8 -4 -4 -16 0.43 0.3 -4 -4 -16 -0.54 0.74 4 4 16 0.75 1.02 -5 -4 -16 4.35 0.6 -5 -4 -16 4.17 1.07 5 4 16 4.53 1.22 -6 -4 -16 2.64 1.06 -6 -4 -16 4.22 0.57 6 4 16 2.83 1.12 -7 -4 -16 -0.11 0.41 7 4 16 -0.58 0.79 -8 -4 -16 2.64 0.52 8 4 16 1.63 0.8 -9 -4 -16 4.88 0.72 -9 -4 -16 4.43 0.47 -10 -4 -16 0.09 0.5 -4 -5 -16 6.34 0.61 -4 -5 -16 5.62 1.04 -5 -5 -16 2.85 0.38 -5 -5 -16 2.12 0.9 5 5 16 1.07 1.02 -6 -5 -16 -0.54 0.29 -6 -5 -16 0.41 0.85 6 5 16 0.09 0.95 -7 -5 -16 2.77 0.5 7 5 16 3.51 0.99 -8 -5 -16 1.95 0.46 8 5 16 1.19 0.73 -9 -5 -16 0.31 0.38 -9 -5 -16 -0.09 0.23 -5 -6 -16 0.37 0.88 -5 -6 -16 -0.14 0.36 5 6 16 0.65 0.94 -6 -6 -16 7.47 1.55 6 6 16 8.47 1.63 -7 -6 -16 3.22 0.72 7 6 16 3.5 0.94 -8 -6 -16 -0.29 0.4 8 6 16 -0.52 0.79 6 7 16 4.61 1.34 7 7 16 1.58 0.97 _iucr_refine_instructions_details ; v25f.res created by SHELXL-2014/7 TITL v25f in P-1 CELL 1.54178 12.7589 13.2831 13.7644 79.4019 64.575 81.8047 ZERR 2 0.0009 0.0009 0.001 0.0025 0.0025 0.0025 LATT 1 SFAC C H Ca F N O S U UNIT 59 84 2 12 6 34 4 2 DFIX 21 0.01 C23 C24 C21 C22 DFIX 20.9285 0.01 N3 C23 N3 C22 N3 C25 DFIX 21.6333 C23A C22A C23A C25A C22A C25A DFIX 21.6333 N3 C24 N3 C21 C23 C22 C23 C25 C22 C25 ISOR 0.01 0.02 C25A L.S. 50 PLAN 20 SIZE 0.06 0.085 0.13 TEMP -73.16 BOND $H fmap 2 acta 132 REM REM REM WGHT 0.025500 5.716200 FVAR 0.09018 1.52549 0.65124 C1 1 0.928247 0.391118 0.530024 11.00000 0.05268 0.04253 = 0.05575 0.01412 -0.03168 -0.00417 AFIX 43 H1 2 0.970719 0.370671 0.573513 11.00000 -1.20000 AFIX 0 C2 1 0.844286 0.479453 0.556861 11.00000 0.05742 0.03362 = 0.04811 0.00654 -0.03092 -0.00815 C3 1 0.808287 0.507145 0.660993 11.00000 0.10020 0.04143 = 0.05171 0.00054 -0.05063 0.00121 AFIX 43 H3 2 0.839220 0.468463 0.709240 11.00000 -1.20000 AFIX 0 C4 1 0.730172 0.588132 0.693620 11.00000 0.11332 0.05341 = 0.04867 -0.01357 -0.04786 0.00546 AFIX 43 H4 2 0.707854 0.606048 0.763907 11.00000 -1.20000 AFIX 0 C5 1 0.682451 0.645196 0.624975 11.00000 0.08244 0.03859 = 0.04311 -0.00725 -0.02755 0.00242 AFIX 43 H5 2 0.627881 0.701963 0.647991 11.00000 -1.20000 AFIX 0 C6 1 0.715097 0.618558 0.523615 11.00000 0.04797 0.02704 = 0.03328 0.00050 -0.01943 -0.00502 C7 1 0.797580 0.536445 0.484534 11.00000 0.04142 0.02339 = 0.03535 0.00047 -0.01790 -0.00646 C8 1 0.573609 0.742745 0.481858 11.00000 0.05439 0.05854 = 0.04546 -0.01608 -0.01497 0.02109 AFIX 23 H8A 2 0.549003 0.752412 0.558431 11.00000 -1.20000 H8B 2 0.506699 0.720948 0.474380 11.00000 -1.20000 AFIX 0 C9 1 0.613229 0.839128 0.409477 11.00000 0.06612 0.04387 = 0.07538 -0.02457 -0.03735 0.01580 AFIX 23 H9A 2 0.549709 0.894260 0.427939 11.00000 -1.20000 H9B 2 0.680129 0.861040 0.416880 11.00000 -1.20000 AFIX 0 C10 1 0.689677 0.907073 0.222985 11.00000 0.05429 0.02984 = 0.09432 0.00631 -0.03621 -0.00015 AFIX 23 H10A 2 0.760862 0.926620 0.224646 11.00000 -1.20000 H10B 2 0.630496 0.965812 0.239181 11.00000 -1.20000 AFIX 0 C11 1 0.715895 0.879587 0.115339 11.00000 0.05138 0.04939 = 0.06894 0.02415 -0.02252 -0.00251 AFIX 23 H11A 2 0.644098 0.862758 0.112721 11.00000 -1.20000 H11B 2 0.748832 0.937709 0.057923 11.00000 -1.20000 AFIX 0 C12 1 0.837299 0.761322 -0.005248 11.00000 0.06449 0.08106 = 0.04009 0.01613 -0.02025 -0.00159 AFIX 23 H12A 2 0.917113 0.728170 -0.026588 11.00000 -1.20000 H12B 2 0.839764 0.822369 -0.059472 11.00000 -1.20000 AFIX 0 C13 1 0.758432 0.687832 -0.004542 11.00000 0.06831 0.08461 = 0.04088 0.00141 -0.03046 0.00469 AFIX 23 H13A 2 0.679740 0.721538 0.010175 11.00000 -1.20000 H13B 2 0.789539 0.661500 -0.075210 11.00000 -1.20000 AFIX 0 C14 1 0.709055 0.517835 0.083082 11.00000 0.06021 0.07849 = 0.05539 -0.02381 -0.03433 0.00491 C15 1 0.656421 0.504987 0.017430 11.00000 0.10547 0.11364 = 0.09036 -0.02450 -0.07578 0.00774 AFIX 43 H15 2 0.644184 0.561700 -0.030702 11.00000 -1.20000 AFIX 0 C16 1 0.621052 0.408697 0.021572 11.00000 0.13150 0.14239 = 0.15333 -0.06559 -0.10921 0.00825 AFIX 43 H16 2 0.586069 0.401064 -0.024983 11.00000 -1.20000 AFIX 0 C17 1 0.634931 0.327882 0.088521 11.00000 0.09921 0.09552 = 0.13665 -0.05671 -0.07827 0.00332 AFIX 43 H17 2 0.609405 0.263609 0.090007 11.00000 -1.20000 AFIX 0 C18 1 0.688873 0.337584 0.159197 11.00000 0.05910 0.07232 = 0.09517 -0.04529 -0.04025 0.00513 C19 1 0.721208 0.434702 0.159080 11.00000 0.03930 0.06306 = 0.05223 -0.02168 -0.02155 0.00153 C20 1 0.707237 0.242806 0.221608 11.00000 0.05165 0.05917 = 0.10361 -0.04195 -0.02864 -0.00190 AFIX 43 H20 2 0.671543 0.185714 0.219376 11.00000 -1.20000 AFIX 0 C21 1 0.772562 0.117002 0.331312 11.00000 0.07790 0.03611 = 0.12255 -0.01297 -0.03375 -0.01411 PART 2 AFIX 23 H21C 2 0.715607 0.107615 0.408176 -31.00000 -1.20000 H21D 2 0.759439 0.068264 0.291871 -31.00000 -1.20000 AFIX 23 PART 0 PART 1 H21A 2 0.824728 0.074443 0.274646 31.00000 -1.20000 H21B 2 0.694391 0.090303 0.363746 31.00000 -1.20000 AFIX 0 PART 0 C24 1 1.034527 0.248948 0.444970 11.00000 0.06041 0.05061 = 0.07008 0.00139 -0.03325 0.02011 PART 1 AFIX 23 H24A 2 1.066959 0.242859 0.499665 31.00000 -1.20000 H24B 2 1.099155 0.253350 0.371607 31.00000 -1.20000 AFIX 23 PART 0 PART 2 H24C 2 1.017016 0.209716 0.518021 -31.00000 -1.20000 H24D 2 1.113761 0.272707 0.416369 -31.00000 -1.20000 AFIX 0 PART 0 C26 1 1.055593 0.873122 0.104418 11.00000 0.05919 0.04808 = 0.05954 0.01556 -0.02747 -0.01424 CA 3 0.769678 0.646899 0.253728 11.00000 0.03437 0.03011 = 0.03152 -0.00023 -0.01364 0.00007 F11 4 1.163106 0.902123 0.069945 11.00000 0.07954 0.10510 = 0.10251 0.04602 -0.03933 -0.05082 F12 4 1.053265 0.830118 0.026462 11.00000 0.07577 0.07977 = 0.04905 0.00722 -0.02045 -0.01012 F13 4 0.983829 0.957754 0.114954 11.00000 0.10357 0.04587 = 0.07600 0.01673 -0.03578 0.00146 N1 5 0.950153 0.338879 0.454290 11.00000 0.04794 0.03541 = 0.05350 0.00208 -0.02233 0.00557 N2 5 0.764939 0.225514 0.279291 11.00000 0.05495 0.02934 = 0.08608 -0.02470 -0.00909 -0.00618 N3 5 0.916805 0.167194 0.382906 11.00000 0.06391 0.03538 = 0.05382 0.00482 -0.00732 0.00164 O1 6 0.829555 0.518229 0.383587 11.00000 0.03897 0.02946 = 0.03309 -0.00176 -0.01583 0.00276 O1S 6 0.572110 0.622954 0.299231 11.00000 0.03853 0.03747 = 0.06628 -0.00766 -0.01875 -0.00043 AFIX 83 H1S 2 0.538142 0.668951 0.270093 11.00000 0.06630 AFIX 0 C1S 1 0.501133 0.538948 0.350701 11.00000 0.04621 0.04421 = 0.08695 -0.01554 0.00129 -0.00573 AFIX 137 H1SA 2 0.425127 0.563041 0.403251 11.00000 -1.50000 H1SB 2 0.538602 0.487099 0.388436 11.00000 -1.50000 H1SC 2 0.490651 0.508687 0.295961 11.00000 -1.50000 AFIX 0 O2 6 0.762940 0.450914 0.226710 11.00000 0.04385 0.03986 = 0.04811 -0.01165 -0.02334 0.00272 O2S 6 0.965034 0.593290 0.139161 11.00000 0.03846 0.05498 = 0.04562 -0.00143 -0.01067 -0.00322 H2SA 2 1.030192 0.609864 0.152780 11.00000 0.04849 AFIX 1 H2SB 2 0.998800 0.565590 0.081740 10.50000 0.05917 AFIX 0 PART 2 C2S 1 1.018337 0.549285 0.048422 10.50000 0.07296 0.08659 = 0.03943 -0.00680 0.00036 0.01338 AFIX 137 H2SC 2 1.099740 0.529667 0.035642 10.50000 -1.50000 H2SD 2 1.015121 0.597964 -0.013230 10.50000 -1.50000 H2SE 2 0.979193 0.487991 0.056387 10.50000 -1.50000 AFIX 0 PART 0 O3 6 0.754749 0.606391 0.080537 11.00000 0.05760 0.06784 = 0.04021 0.00066 -0.02755 -0.00398 O4 6 0.798068 0.792632 0.099227 11.00000 0.05286 0.05145 = 0.05133 0.01122 -0.02513 0.00024 O5 6 0.646801 0.819075 0.300787 11.00000 0.05440 0.02997 = 0.05498 -0.00471 -0.02602 0.00375 O6 6 0.670234 0.666166 0.450558 11.00000 0.04765 0.04440 = 0.03261 -0.00705 -0.01597 0.01183 O7 6 0.982404 0.362903 0.224298 11.00000 0.04169 0.03705 = 0.04995 -0.00169 -0.00769 0.00260 O8 6 0.712445 0.336255 0.458178 11.00000 0.04682 0.03929 = 0.05613 -0.00901 -0.01421 -0.00004 O11 6 0.897055 0.766512 0.263385 11.00000 0.04397 0.04093 = 0.05341 0.00223 -0.02347 -0.00457 O12 6 1.032608 0.846060 0.301233 11.00000 0.08922 0.07260 = 0.07164 0.00883 -0.05092 -0.03095 O13 6 1.097278 0.698490 0.201427 11.00000 0.05134 0.04887 = 0.08712 0.01440 -0.03618 -0.00120 S1 7 1.016695 0.787136 0.232349 11.00000 0.05378 0.04438 = 0.05442 0.01385 -0.03250 -0.01372 U 8 0.843272 0.356300 0.338311 11.00000 0.03358 0.02383 = 0.03673 -0.00257 -0.00626 0.00056 PART 1 C23 1 0.962125 0.158316 0.466070 31.00000 0.07426 0.03733 = 0.04915 0.00440 -0.01876 0.01722 AFIX 23 H23A 2 1.010997 0.093218 0.465109 31.00000 -1.20000 H23B 2 0.896521 0.156973 0.538731 31.00000 -1.20000 AFIX 0 C25 1 1.012760 0.130035 0.284797 31.00000 0.06512 0.03621 = 0.05574 -0.01265 -0.00824 0.01375 AFIX 137 H25A 2 0.988514 0.142261 0.224775 31.00000 -1.50000 H25B 2 1.030901 0.056333 0.300805 31.00000 -1.50000 H25C 2 1.081986 0.167068 0.264271 31.00000 -1.50000 AFIX 0 PART 0 PART 2 C22A 1 0.890705 0.104010 0.322431 -31.00000 0.08582 0.02116 = 0.17278 -0.01723 -0.03369 0.01418 AFIX 23 H22A 2 0.907272 0.031135 0.347198 -31.00000 -1.20000 H22B 2 0.944091 0.118847 0.244817 -31.00000 -1.20000 AFIX 0 C23A 1 1.031495 0.175141 0.366805 -31.00000 0.04649 0.03264 = 0.08729 0.00620 -0.01544 0.01843 AFIX 23 H23C 2 1.077546 0.202880 0.290177 -31.00000 -1.20000 H23D 2 1.066965 0.106163 0.381919 -31.00000 -1.20000 AFIX 0 C25A 1 0.838355 0.136901 0.511246 -31.00000 0.07622 0.03662 = 0.08252 0.02473 -0.00807 0.00201 AFIX 137 H25D 2 0.840448 0.190073 0.551071 -31.00000 -1.50000 H25E 2 0.869248 0.070898 0.537359 -31.00000 -1.50000 H25F 2 0.757867 0.131389 0.523019 -31.00000 -1.50000 AFIX 0 PART 0 C3S 1 0.344337 0.756402 0.219889 11.00000 0.09077 0.08979 = 0.15985 -0.03951 -0.07968 0.00716 AFIX 137 H3SA 2 0.339059 0.800800 0.156641 11.00000 -1.50000 H3SB 2 0.275589 0.771108 0.285591 11.00000 -1.50000 H3SC 2 0.348190 0.684328 0.210747 11.00000 -1.50000 AFIX 0 O3S 6 0.446061 0.775205 0.229585 11.00000 0.06832 0.05404 = 0.09999 -0.01957 -0.05075 0.00493 AFIX 147 H3S 2 0.429359 0.819417 0.271443 11.00000 -1.50000 AFIX 0 C27 1 0.393246 1.096776 0.175481 11.00000 0.10877 0.07956 = 0.10380 -0.00708 -0.06966 0.01822 F21 4 0.313293 1.051981 0.162371 11.00000 0.16972 0.13446 = 0.18582 -0.01736 -0.14168 0.00163 F22 4 0.495909 1.066578 0.104489 11.00000 0.14084 0.13115 = 0.07335 -0.01061 -0.04141 0.01334 F23 4 0.376186 1.197281 0.151442 11.00000 0.19580 0.07971 = 0.14177 0.02054 -0.11486 0.01593 O21 6 0.474008 1.114985 0.310466 11.00000 0.07054 0.04775 = 0.07874 -0.01350 -0.03102 -0.00394 O22 6 0.265998 1.102456 0.379604 11.00000 0.06603 0.06006 = 0.11473 -0.01546 -0.00545 0.00938 O23 6 0.399567 0.953091 0.326298 11.00000 0.06384 0.03311 = 0.08937 -0.00390 -0.02798 0.00411 S2 7 0.380861 1.063255 0.313640 11.00000 0.04947 0.03466 = 0.06765 -0.00668 -0.01777 0.00636 PART 1 C22 1 0.817900 0.106009 0.419501 31.00000 0.06241 0.02575 = 0.08269 0.01156 -0.00710 -0.00739 AFIX 23 H22C 2 0.755303 0.128866 0.486395 31.00000 -1.20000 H22D 2 0.841290 0.032984 0.436784 31.00000 -1.20000 AFIX 0 HKLF 4 REM v25f in P-1 REM R1 = 0.0370 for 6979 Fo > 4sig(Fo) and 0.0403 for all 7473 data REM 581 parameters refined using 19 restraints END WGHT 0.0255 5.7052 REM Highest difference peak 1.521, deepest hole -1.159, 1-sigma level 0.128 Q1 1 0.8388 0.3960 0.3725 11.00000 0.05 1.52 Q2 1 0.8209 0.3788 0.3944 11.00000 0.05 1.48 Q3 1 0.8196 0.2780 0.2972 11.00000 0.05 1.31 Q4 1 0.7979 0.3478 0.4030 11.00000 0.05 1.21 Q5 1 0.8723 0.3845 0.2372 11.00000 0.05 1.05 Q6 1 0.7958 0.3548 0.3278 11.00000 0.05 0.70 Q7 1 0.7578 0.4134 0.3458 11.00000 0.05 0.65 Q8 1 0.9592 0.2852 0.1809 11.00000 0.05 0.57 Q9 1 0.5381 1.0256 0.0255 11.00000 0.05 0.55 Q10 1 0.5052 1.1219 0.0285 11.00000 0.05 0.55 Q11 1 0.7414 0.3839 0.1364 11.00000 0.05 0.52 Q12 1 0.2783 1.1238 0.3016 11.00000 0.05 0.51 Q13 1 0.8529 0.3301 0.4370 11.00000 0.05 0.48 Q14 1 0.9247 0.5040 0.2639 11.00000 0.05 0.47 Q15 1 0.5382 0.8004 0.4142 11.00000 0.05 0.47 Q16 1 0.9730 0.4397 0.1932 11.00000 0.05 0.47 Q17 1 0.6466 0.3729 0.4683 11.00000 0.05 0.45 Q18 1 0.8795 0.2884 0.5610 11.00000 0.05 0.45 Q19 1 0.8205 0.3997 0.1831 11.00000 0.05 0.44 Q20 1 0.4020 0.6562 0.5817 11.00000 0.05 0.43 REM The information below was added by Olex2. REM REM R1 = 0.0370 for 6979 Fo > 4sig(Fo) and 0.0403 for all 32430 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.52, deepest hole -1.16 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0403 REM R1_gt = 0.0370 REM wR_ref = 0.0866 REM GOOF = 1.093 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 32430 REM Reflections_gt = 6979 REM Parameters = n/a REM Hole = -1.16 REM Peak = 1.52 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received' # start Validation Reply Form _vrf_PLAT410_LsalbenUO2Ca ; PROBLEM: Short Intra H...H Contact H5 ..H8A . 1.88 Ang. RESPONSE: This short H...H contact is attributable to the ruffling of the macrocycle in the presence of the strongly Lewis Acidic Ca2+ ion. The use of idealized H positions for the H atoms involved in this close contact also likely contribute. ; _vrf_PLAT420_LsalbenUO2Ca ; PROBLEM: D-H Without Acceptor O2S --H2SB . Please Check RESPONSE: O2S belongs to a water molecule half the time and to a molecule of methanol half the time. Therefore, H2SB is present only half of the time, and is replaced by a methyl group containing C2S half the time. See the Supporting Information for detailed explanation of this disorder and its consequences. ; # end Validation Reply Form data_L(salben)UO2Y _audit_creation_date 2019-08-07 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2014/7' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C29 H34 F6 N4 O14 S2 U Y, C F3 O3 S' _chemical_formula_sum 'C30 H34 F9 N4 O17 S3 U Y' _chemical_formula_weight 1316.73 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Y' 'Y' -0.2670 2.0244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1814(6) _cell_length_b 13.6032(8) _cell_length_c 18.8769(12) _cell_angle_alpha 102.095(5) _cell_angle_beta 102.738(6) _cell_angle_gamma 103.991(5) _cell_volume 2143.6(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4780 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 69.826 _cell_measurement_theta_min 2.498 _shelx_estimated_absorpt_T_max 0.709 _shelx_estimated_absorpt_T_min 0.666 _exptl_absorpt_coefficient_mu 14.767 _exptl_absorpt_correction_T_max 0.5526 _exptl_absorpt_correction_T_min 0.3888 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _exptl_crystal_colour 'orange' _exptl_crystal_density_diffrn 2.040 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description 'Chunk' _exptl_crystal_F_000 1276 _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.025 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0767 _diffrn_reflns_av_unetI/netI 0.0677 _diffrn_reflns_Laue_measured_fraction_full 0.959 _diffrn_reflns_Laue_measured_fraction_max 0.926 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 28130 _diffrn_reflns_point_group_measured_fraction_full 0.959 _diffrn_reflns_point_group_measured_fraction_max 0.926 _diffrn_reflns_theta_full 66.000 _diffrn_reflns_theta_max 70.433 _diffrn_reflns_theta_min 2.498 _diffrn_ambient_temperature 199.99 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.959 _diffrn_measured_fraction_theta_max 0.926 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'Bruker MicroStar microfocus rotating anode' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6180 _reflns_number_total 7605 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection ? _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution ? _refine_diff_density_max 2.344 _refine_diff_density_min -1.182 _refine_diff_density_rms 0.179 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 587 _refine_ls_number_reflns 7605 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0498 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+5.3038P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1223 _refine_ls_wR_factor_ref 0.1326 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C22(H22A,H22B), C21(H21A,H21B), C13(H13A,H13B), C12(H12A,H12B), C11(H11A, H11B), C10(H10A,H10B), C9(H9A,H9B), C8(H8A,H8B), C24(H24A,H24B), C23(H23A,H23B) 2.b Me refined with riding coordinates: C25(H25A,H25B,H25C) 2.c Aromatic/amide H refined with riding coordinates: C20(H20), C17(H17), C16(H16), C15(H15), C5(H5), C4(H4), C3(H3), C1(H1) 2.d Idealised Me refined as rotating group: C2S(H2SA,H2SB,H2SC) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U U 0.32334(4) 0.03904(2) 0.16143(2) 0.04278(11) Uani 1 1 d . . . . . Y Y 0.53837(9) 0.32612(5) 0.28681(4) 0.04019(18) Uani 1 1 d . . . . . O2 O 0.3920(7) 0.1560(4) 0.2834(3) 0.0400(12) Uani 1 1 d . . . . . O1 O 0.4473(7) 0.2068(4) 0.1547(3) 0.0383(12) Uani 1 1 d . . . . . O7 O 0.1326(7) 0.0507(5) 0.1525(4) 0.0477(14) Uani 1 1 d . . . . . O8 O 0.5057(8) 0.0129(5) 0.1637(4) 0.0512(15) Uani 1 1 d . . . . . N3 N 0.1934(9) -0.1570(6) 0.0876(5) 0.0504(19) Uani 1 1 d . . . . . C22 C 0.2788(15) -0.2129(8) 0.1299(7) 0.060(3) Uani 1 1 d . . . . . H22A H 0.3911 -0.1878 0.1327 0.072 Uiso 1 1 calc R . . . . H22B H 0.2389 -0.2892 0.1034 0.072 Uiso 1 1 calc R . . . . C21 C 0.2613(15) -0.1954(9) 0.2111(7) 0.064(3) Uani 1 1 d . . . . . H21A H 0.1564 -0.2384 0.2097 0.077 Uiso 1 1 calc R . . . . H21B H 0.3411 -0.2177 0.2430 0.077 Uiso 1 1 calc R . . . . N2 N 0.2819(10) -0.0813(6) 0.2438(5) 0.0512(19) Uani 1 1 d . . . . . C20 C 0.2602(13) -0.0574(8) 0.3074(7) 0.058(3) Uani 1 1 d . . . . . H20 H 0.2443 -0.1125 0.3312 0.070 Uiso 1 1 calc R . . . . C18 C 0.2559(12) 0.0454(9) 0.3501(6) 0.053(2) Uani 1 1 d . . . . . C19 C 0.3111(11) 0.1424(8) 0.3344(5) 0.046(2) Uani 1 1 d . . . . . C17 C 0.1839(15) 0.0414(10) 0.4073(7) 0.067(3) Uani 1 1 d . . . . . H17 H 0.1539 -0.0232 0.4198 0.080 Uiso 1 1 calc R . . . . C16 C 0.1545(14) 0.1286(10) 0.4464(6) 0.064(3) Uani 1 1 d . . . . . H16 H 0.1018 0.1237 0.4841 0.077 Uiso 1 1 calc R . . . . C15 C 0.2042(13) 0.2251(10) 0.4295(6) 0.059(3) Uani 1 1 d . . . . . H15 H 0.1854 0.2862 0.4559 0.071 Uiso 1 1 calc R . . . . C14 C 0.2806(10) 0.2306(8) 0.3740(5) 0.0455(19) Uani 1 1 d . . . . . O3 O 0.3323(8) 0.3218(5) 0.3537(4) 0.0473(14) Uani 1 1 d . . . . . C13 C 0.3165(13) 0.4151(8) 0.3984(6) 0.056(2) Uani 1 1 d . . . . . H13A H 0.3708 0.4270 0.4524 0.068 Uiso 1 1 calc R . . . . H13B H 0.2044 0.4079 0.3933 0.068 Uiso 1 1 calc R . . . . C12 C 0.3877(14) 0.5055(9) 0.3710(7) 0.061(3) Uani 1 1 d . . . . . H12A H 0.3197 0.5028 0.3215 0.073 Uiso 1 1 calc R . . . . H12B H 0.4029 0.5735 0.4076 0.073 Uiso 1 1 calc R . . . . O4 O 0.5339(9) 0.4938(5) 0.3641(5) 0.0580(17) Uani 1 1 d . . . . . C11 C 0.6461(15) 0.5874(9) 0.3671(7) 0.066(3) Uani 1 1 d . . . . . H11A H 0.6444 0.6479 0.4062 0.079 Uiso 1 1 calc R . . . . H11B H 0.6264 0.6033 0.3177 0.079 Uiso 1 1 calc R . . . . C10 C 0.8006(14) 0.5644(7) 0.3869(6) 0.059(3) Uani 1 1 d . . . . . H10A H 0.8846 0.6222 0.3827 0.071 Uiso 1 1 calc R . . . . H10B H 0.8265 0.5605 0.4399 0.071 Uiso 1 1 calc R . . . . O5 O 0.7925(8) 0.4677(6) 0.3378(4) 0.0565(17) Uani 1 1 d . . . . . C9 C 0.8894(13) 0.4743(9) 0.2886(7) 0.062(3) Uani 1 1 d . . . . . H9A H 0.9270 0.4116 0.2807 0.074 Uiso 1 1 calc R . . . . H9B H 0.9815 0.5380 0.3110 0.074 Uiso 1 1 calc R . . . . C8 C 0.7933(13) 0.4795(8) 0.2143(7) 0.059(3) Uani 1 1 d . . . . . H8A H 0.7715 0.5481 0.2199 0.071 Uiso 1 1 calc R . . . . H8B H 0.8492 0.4705 0.1753 0.071 Uiso 1 1 calc R . . . . O6 O 0.6492(7) 0.3939(5) 0.1937(4) 0.0471(14) Uani 1 1 d . . . . . C6 C 0.5724(11) 0.3517(8) 0.1171(6) 0.046(2) Uani 1 1 d . . . . . C7 C 0.4665(10) 0.2480(7) 0.0981(5) 0.0435(19) Uani 1 1 d . . . . . C5 C 0.5885(13) 0.4054(9) 0.0647(7) 0.059(3) Uani 1 1 d . . . . . H5 H 0.6555 0.4759 0.0800 0.070 Uiso 1 1 calc R . . . . C4 C 0.5074(14) 0.3576(9) -0.0112(6) 0.059(3) Uani 1 1 d . . . . . H4 H 0.5183 0.3952 -0.0478 0.071 Uiso 1 1 calc R . . . . C3 C 0.4113(14) 0.2555(9) -0.0327(6) 0.057(2) Uani 1 1 d . . . . . H3 H 0.3561 0.2226 -0.0845 0.068 Uiso 1 1 calc R . . . . C2 C 0.3930(11) 0.1982(8) 0.0218(6) 0.047(2) Uani 1 1 d . . . . . C1 C 0.3004(12) 0.0891(8) -0.0112(6) 0.051(2) Uani 1 1 d . . . . . H1 H 0.2596 0.0677 -0.0647 0.061 Uiso 1 1 calc R . . . . N1 N 0.2651(9) 0.0158(6) 0.0224(5) 0.0490(18) Uani 1 1 d . . . . . C24 C 0.1765(15) -0.0896(8) -0.0258(6) 0.062(3) Uani 1 1 d . . . . . H24A H 0.1976 -0.0990 -0.0756 0.074 Uiso 1 1 calc R . . . . H24B H 0.0630 -0.0997 -0.0339 0.074 Uiso 1 1 calc R . . . . C23 C 0.2235(14) -0.1703(9) 0.0113(7) 0.061(3) Uani 1 1 d . . . . . H23A H 0.1630 -0.2422 -0.0214 0.073 Uiso 1 1 calc R . . . . H23B H 0.3361 -0.1618 0.0174 0.073 Uiso 1 1 calc R . . . . C25 C 0.0242(14) -0.1957(11) 0.0775(9) 0.078(4) Uani 1 1 d . . . . . H25A H -0.0295 -0.1562 0.0487 0.116 Uiso 1 1 calc R . . . . H25B H -0.0154 -0.2708 0.0500 0.116 Uiso 1 1 calc R . . . . H25C H 0.0046 -0.1860 0.1271 0.116 Uiso 1 1 calc R . . . . N1S N 0.7270(9) 0.2322(6) 0.2723(5) 0.0469(17) Uani 1 1 d . . . . . C1S C 0.8030(12) 0.1786(8) 0.2623(6) 0.053(2) Uani 1 1 d . . . . . C2S C 0.8979(14) 0.1127(9) 0.2503(8) 0.065(3) Uani 1 1 d . . . . . H2SA H 0.9711 0.1417 0.2238 0.097 Uiso 1 1 calc GR . . . . H2SB H 0.8316 0.0419 0.2197 0.097 Uiso 1 1 calc GR . . . . H2SC H 0.9569 0.1087 0.2991 0.097 Uiso 1 1 calc GR . . . . S1 S 0.1840(3) 0.35120(19) 0.16698(15) 0.0499(5) Uani 1 1 d . . . . . F11 F 0.0504(10) 0.4605(8) 0.0907(5) 0.095(3) Uani 1 1 d . . . . . F12 F 0.2168(15) 0.5512(6) 0.1942(7) 0.125(4) Uani 1 1 d . . . . . F13 F 0.2946(14) 0.4890(11) 0.1014(9) 0.147(6) Uani 1 1 d . . . . . O11 O 0.3452(8) 0.3779(5) 0.2150(4) 0.0473(14) Uani 1 1 d . . . . . O12 O 0.1463(10) 0.2705(8) 0.0994(6) 0.081(3) Uani 1 1 d . . . . . O13 O 0.0715(11) 0.3455(9) 0.2078(7) 0.088(3) Uani 1 1 d . . . . . C26 C 0.1889(14) 0.4680(10) 0.1353(9) 0.070(3) Uani 1 1 d . . . . . S2 S 0.7796(3) 0.32490(19) 0.46747(13) 0.0499(5) Uani 1 1 d . . . . . F21 F 0.8219(17) 0.1985(10) 0.5483(8) 0.166(7) Uani 1 1 d . . . . . F23 F 0.5859(16) 0.2074(11) 0.5204(7) 0.140(5) Uani 1 1 d . . . . . F22 F 0.6669(15) 0.1216(7) 0.4371(9) 0.155(6) Uani 1 1 d . . . . . O21 O 0.6422(8) 0.3182(6) 0.4085(4) 0.0524(15) Uani 1 1 d . . . . . O22 O 0.8121(10) 0.4084(7) 0.5335(5) 0.069(2) Uani 1 1 d . . . . . O23 O 0.9098(10) 0.3116(9) 0.4420(5) 0.080(3) Uani 1 1 d . . . . . C27 C 0.705(2) 0.2058(12) 0.4946(11) 0.103(6) Uani 1 1 d . . . . . S3 S 0.7897(4) -0.2098(2) 0.25518(18) 0.0661(7) Uani 1 1 d . . . . . F31 F 0.6286(12) -0.0811(9) 0.2872(7) 0.113(3) Uani 1 1 d . . . . . F32 F 0.6305(13) -0.1866(8) 0.3551(6) 0.107(3) Uani 1 1 d . . . . . F33 F 0.8317(12) -0.0582(8) 0.3764(5) 0.106(3) Uani 1 1 d . . . . . O31 O 0.9011(14) -0.2428(8) 0.3030(8) 0.101(4) Uani 1 1 d . . . . . O32 O 0.8609(13) -0.1358(7) 0.2203(6) 0.087(3) Uani 1 1 d . . . . . O33 O 0.6509(16) -0.2918(9) 0.2103(6) 0.107(4) Uani 1 1 d . . . . . C28 C 0.7188(16) -0.1300(11) 0.3231(8) 0.074(3) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.04027(17) 0.03191(15) 0.05384(18) 0.00516(12) 0.01360(13) 0.01238(11) Y 0.0375(4) 0.0320(3) 0.0475(4) 0.0032(3) 0.0130(3) 0.0099(3) O2 0.041(3) 0.033(3) 0.044(3) 0.005(2) 0.014(3) 0.010(2) O1 0.032(3) 0.034(3) 0.048(3) 0.010(3) 0.010(3) 0.013(2) O7 0.037(3) 0.039(3) 0.058(4) 0.002(3) 0.012(3) 0.007(3) O8 0.042(3) 0.041(3) 0.065(4) 0.006(3) 0.014(3) 0.011(3) N3 0.038(4) 0.037(4) 0.066(5) 0.000(4) 0.012(4) 0.007(3) C22 0.072(7) 0.043(5) 0.066(6) 0.014(5) 0.015(6) 0.024(5) C21 0.069(7) 0.046(6) 0.077(7) 0.022(5) 0.022(6) 0.013(5) N2 0.050(5) 0.034(4) 0.070(5) 0.013(4) 0.017(4) 0.016(3) C20 0.061(6) 0.041(5) 0.070(7) 0.025(5) 0.015(6) 0.007(4) C18 0.045(5) 0.057(6) 0.058(5) 0.021(5) 0.014(5) 0.016(4) C19 0.034(4) 0.055(5) 0.043(4) 0.011(4) 0.006(4) 0.009(4) C17 0.068(7) 0.062(7) 0.069(7) 0.025(6) 0.021(6) 0.009(5) C16 0.059(6) 0.076(7) 0.055(6) 0.014(6) 0.025(5) 0.012(6) C15 0.057(6) 0.068(7) 0.052(5) 0.010(5) 0.022(5) 0.015(5) C14 0.034(4) 0.054(5) 0.044(4) 0.008(4) 0.009(4) 0.013(4) O3 0.048(4) 0.043(3) 0.050(3) 0.006(3) 0.019(3) 0.015(3) C13 0.056(6) 0.050(5) 0.059(6) -0.003(5) 0.019(5) 0.019(5) C12 0.065(7) 0.046(5) 0.069(7) 0.002(5) 0.019(6) 0.023(5) O4 0.053(4) 0.036(3) 0.078(5) 0.001(3) 0.020(4) 0.013(3) C11 0.081(8) 0.048(6) 0.065(6) 0.005(5) 0.026(6) 0.018(5) C10 0.072(7) 0.028(4) 0.052(5) -0.001(4) -0.003(5) 0.001(4) O5 0.051(4) 0.046(4) 0.067(4) 0.006(3) 0.019(4) 0.012(3) C9 0.048(6) 0.049(5) 0.074(7) 0.001(5) 0.017(5) 0.002(4) C8 0.051(6) 0.044(5) 0.075(7) 0.010(5) 0.025(5) 0.000(4) O6 0.040(3) 0.036(3) 0.060(4) 0.005(3) 0.018(3) 0.004(3) C6 0.037(4) 0.046(5) 0.060(5) 0.014(4) 0.021(4) 0.014(4) C7 0.036(4) 0.044(5) 0.058(5) 0.011(4) 0.023(4) 0.019(4) C5 0.055(6) 0.058(6) 0.072(7) 0.029(6) 0.027(6) 0.016(5) C4 0.066(7) 0.064(6) 0.062(6) 0.030(5) 0.030(6) 0.023(5) C3 0.061(6) 0.070(7) 0.056(6) 0.026(5) 0.027(5) 0.034(5) C2 0.041(5) 0.049(5) 0.062(6) 0.019(5) 0.023(5) 0.022(4) C1 0.045(5) 0.056(6) 0.046(5) 0.002(4) 0.001(4) 0.027(4) N1 0.037(4) 0.041(4) 0.057(5) 0.001(4) 0.003(4) 0.010(3) C24 0.072(7) 0.049(6) 0.045(5) -0.002(4) -0.004(5) 0.016(5) C23 0.064(7) 0.051(6) 0.065(6) 0.005(5) 0.021(6) 0.021(5) C25 0.050(6) 0.073(8) 0.090(9) 0.008(7) 0.017(7) -0.001(6) N1S 0.042(4) 0.040(4) 0.057(4) 0.004(3) 0.013(4) 0.016(3) C1S 0.042(5) 0.052(5) 0.054(5) 0.002(5) 0.006(4) 0.011(4) C2S 0.058(6) 0.058(6) 0.084(8) 0.013(6) 0.027(6) 0.027(5) S1 0.0428(12) 0.0470(12) 0.0649(14) 0.0162(11) 0.0206(11) 0.0171(9) F11 0.081(5) 0.116(7) 0.112(6) 0.057(6) 0.026(5) 0.052(5) F12 0.152(10) 0.045(4) 0.164(10) 0.024(5) 0.013(8) 0.036(5) F13 0.122(8) 0.175(11) 0.253(15) 0.167(12) 0.117(10) 0.088(8) O11 0.045(3) 0.048(3) 0.051(3) 0.009(3) 0.013(3) 0.022(3) O12 0.058(5) 0.074(5) 0.082(6) -0.011(5) -0.010(4) 0.024(4) O13 0.060(5) 0.117(8) 0.126(8) 0.060(7) 0.057(6) 0.045(5) C26 0.057(7) 0.068(8) 0.110(10) 0.056(8) 0.035(7) 0.026(6) S2 0.0507(13) 0.0448(11) 0.0480(11) 0.0018(10) 0.0092(10) 0.0172(10) F21 0.152(11) 0.128(9) 0.179(12) 0.100(10) -0.045(10) 0.005(8) F23 0.122(9) 0.151(11) 0.138(9) 0.088(9) 0.029(8) -0.010(8) F22 0.135(9) 0.039(4) 0.236(15) 0.010(6) -0.012(10) 0.013(5) O21 0.046(4) 0.055(4) 0.053(4) 0.011(3) 0.011(3) 0.015(3) O22 0.062(5) 0.063(5) 0.065(5) -0.015(4) 0.017(4) 0.015(4) O23 0.053(5) 0.112(7) 0.060(5) -0.007(5) 0.004(4) 0.038(5) C27 0.103(12) 0.067(9) 0.122(14) 0.054(10) -0.008(11) 0.012(8) S3 0.0724(18) 0.0514(14) 0.0691(16) 0.0169(13) 0.0199(15) 0.0089(12) F31 0.093(6) 0.133(8) 0.147(9) 0.066(8) 0.041(6) 0.065(6) F32 0.116(7) 0.110(7) 0.100(6) 0.040(6) 0.050(6) 0.018(6) F33 0.101(7) 0.102(7) 0.084(5) -0.012(5) 0.011(5) 0.021(5) O31 0.089(7) 0.074(6) 0.138(10) 0.037(7) 0.010(7) 0.035(5) O32 0.105(7) 0.063(5) 0.106(7) 0.027(5) 0.061(6) 0.018(5) O33 0.134(10) 0.071(6) 0.080(6) 0.015(5) 0.007(7) -0.009(6) C28 0.063(7) 0.073(8) 0.084(8) 0.029(7) 0.020(7) 0.011(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U Y 3.8843(8) . ? U O2 2.361(6) . ? U O1 2.334(6) . ? U O7 1.771(6) . ? U O8 1.788(7) . ? U N3 2.579(8) . ? U N2 2.504(8) . ? U N1 2.495(9) . ? Y O2 2.358(6) . ? Y O1 2.507(6) . ? Y O3 2.491(6) . ? Y O4 2.452(7) . ? Y O5 2.478(7) . ? Y O6 2.448(6) . ? Y N1S 2.416(8) . ? Y O11 2.329(6) . ? Y O21 2.320(7) . ? O2 C19 1.355(11) . ? O1 C7 1.331(11) . ? N3 C22 1.448(14) . ? N3 C23 1.507(14) . ? N3 C25 1.470(14) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C22 C21 1.551(17) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 N2 1.494(14) . ? N2 C20 1.249(15) . ? C20 H20 0.9500 . ? C20 C18 1.475(16) . ? C18 C19 1.411(14) . ? C18 C17 1.389(16) . ? C19 C14 1.399(14) . ? C17 H17 0.9500 . ? C17 C16 1.378(18) . ? C16 H16 0.9500 . ? C16 C15 1.408(17) . ? C15 H15 0.9500 . ? C15 C14 1.388(14) . ? C14 O3 1.381(12) . ? O3 C13 1.428(12) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C12 1.495(16) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 O4 1.419(13) . ? O4 C11 1.412(13) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C10 1.510(18) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 O5 1.416(12) . ? O5 C9 1.423(13) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C8 1.509(17) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 O6 1.448(11) . ? O6 C6 1.387(12) . ? C6 C7 1.427(13) . ? C6 C5 1.360(14) . ? C7 C2 1.389(14) . ? C5 H5 0.9500 . ? C5 C4 1.391(17) . ? C4 H4 0.9500 . ? C4 C3 1.373(17) . ? C3 H3 0.9500 . ? C3 C2 1.428(14) . ? C2 C1 1.443(14) . ? C1 H1 0.9500 . ? C1 N1 1.304(13) . ? N1 C24 1.452(13) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 C23 1.517(16) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? N1S C1S 1.141(13) . ? C1S C2S 1.412(15) . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? S1 O11 1.468(7) . ? S1 O12 1.410(9) . ? S1 O13 1.416(8) . ? S1 C26 1.805(11) . ? F11 C26 1.328(15) . ? F12 C26 1.338(18) . ? F13 C26 1.284(16) . ? S2 O21 1.457(7) . ? S2 O22 1.419(8) . ? S2 O23 1.419(9) . ? S2 C27 1.824(15) . ? F21 C27 1.345(19) . ? F23 C27 1.29(3) . ? F22 C27 1.32(2) . ? S3 O31 1.431(11) . ? S3 O32 1.423(9) . ? S3 O33 1.423(11) . ? S3 C28 1.837(16) . ? F31 C28 1.339(17) . ? F32 C28 1.313(15) . ? F33 C28 1.296(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 U Y 34.58(14) . . ? O2 U N3 141.9(2) . . ? O2 U N2 76.5(2) . . ? O2 U N1 147.5(2) . . ? O1 U Y 38.19(15) . . ? O1 U O2 72.6(2) . . ? O1 U N3 145.5(2) . . ? O1 U N2 146.9(2) . . ? O1 U N1 77.3(2) . . ? O7 U Y 95.1(2) . . ? O7 U O2 85.9(3) . . ? O7 U O1 98.5(2) . . ? O7 U O8 173.7(3) . . ? O7 U N3 87.6(3) . . ? O7 U N2 90.7(3) . . ? O7 U N1 86.7(3) . . ? O8 U Y 91.2(2) . . ? O8 U O2 99.6(3) . . ? O8 U O1 86.3(3) . . ? O8 U N3 86.1(3) . . ? O8 U N2 87.4(3) . . ? O8 U N1 90.4(3) . . ? N3 U Y 175.0(2) . . ? N2 U Y 109.6(2) . . ? N2 U N3 66.1(3) . . ? N1 U Y 115.17(18) . . ? N1 U N3 69.1(3) . . ? N1 U N2 135.2(3) . . ? O2 Y U 34.62(14) . . ? O2 Y O1 69.59(19) . . ? O2 Y O3 65.1(2) . . ? O2 Y O4 126.4(2) . . ? O2 Y O5 147.2(2) . . ? O2 Y O6 132.1(2) . . ? O2 Y N1S 80.0(2) . . ? O1 Y U 35.15(13) . . ? O3 Y U 91.61(15) . . ? O3 Y O1 115.0(2) . . ? O4 Y U 150.53(17) . . ? O4 Y O1 143.3(2) . . ? O4 Y O3 62.0(2) . . ? O4 Y O5 64.2(2) . . ? O5 Y U 145.23(17) . . ? O5 Y O1 123.0(2) . . ? O5 Y O3 120.6(2) . . ? O6 Y U 97.65(15) . . ? O6 Y O1 63.46(19) . . ? O6 Y O3 145.8(2) . . ? O6 Y O4 98.0(2) . . ? O6 Y O5 63.8(2) . . ? N1S Y U 70.26(19) . . ? N1S Y O1 72.0(2) . . ? N1S Y O3 136.6(3) . . ? N1S Y O4 137.8(3) . . ? N1S Y O5 76.8(3) . . ? N1S Y O6 77.2(3) . . ? O11 Y U 87.81(17) . . ? O11 Y O2 100.5(2) . . ? O11 Y O1 71.5(2) . . ? O11 Y O3 73.7(2) . . ? O11 Y O4 72.9(2) . . ? O11 Y O5 112.2(2) . . ? O11 Y O6 73.8(2) . . ? O11 Y N1S 140.7(3) . . ? O21 Y U 107.59(18) . . ? O21 Y O2 78.1(2) . . ? O21 Y O1 138.0(2) . . ? O21 Y O3 71.7(2) . . ? O21 Y O4 78.0(3) . . ? O21 Y O5 74.3(3) . . ? O21 Y O6 134.5(2) . . ? O21 Y N1S 76.7(3) . . ? O21 Y O11 142.3(2) . . ? Y O2 U 110.8(2) . . ? C19 O2 U 123.8(5) . . ? C19 O2 Y 120.7(5) . . ? U O1 Y 106.7(2) . . ? C7 O1 U 134.1(5) . . ? C7 O1 Y 119.0(5) . . ? C22 N3 U 104.6(6) . . ? C22 N3 C23 109.0(8) . . ? C22 N3 C25 111.8(10) . . ? C23 N3 U 107.0(6) . . ? C25 N3 U 114.7(7) . . ? C25 N3 C23 109.5(10) . . ? N3 C22 H22A 109.4 . . ? N3 C22 H22B 109.4 . . ? N3 C22 C21 111.2(9) . . ? H22A C22 H22B 108.0 . . ? C21 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? C22 C21 H21A 109.8 . . ? C22 C21 H21B 109.8 . . ? H21A C21 H21B 108.3 . . ? N2 C21 C22 109.2(8) . . ? N2 C21 H21A 109.8 . . ? N2 C21 H21B 109.8 . . ? C21 N2 U 117.8(7) . . ? C20 N2 U 126.0(7) . . ? C20 N2 C21 115.8(9) . . ? N2 C20 H20 115.9 . . ? N2 C20 C18 128.2(9) . . ? C18 C20 H20 115.9 . . ? C19 C18 C20 125.2(9) . . ? C17 C18 C20 115.0(10) . . ? C17 C18 C19 119.8(10) . . ? O2 C19 C18 124.4(9) . . ? O2 C19 C14 117.5(8) . . ? C14 C19 C18 118.1(9) . . ? C18 C17 H17 119.1 . . ? C16 C17 C18 121.9(11) . . ? C16 C17 H17 119.1 . . ? C17 C16 H16 120.6 . . ? C17 C16 C15 118.8(10) . . ? C15 C16 H16 120.6 . . ? C16 C15 H15 120.1 . . ? C14 C15 C16 119.8(11) . . ? C14 C15 H15 120.1 . . ? C15 C14 C19 121.5(10) . . ? O3 C14 C19 115.0(8) . . ? O3 C14 C15 123.5(9) . . ? C14 O3 Y 115.9(5) . . ? C14 O3 C13 115.9(7) . . ? C13 O3 Y 122.6(6) . . ? O3 C13 H13A 110.2 . . ? O3 C13 H13B 110.2 . . ? O3 C13 C12 107.7(8) . . ? H13A C13 H13B 108.5 . . ? C12 C13 H13A 110.2 . . ? C12 C13 H13B 110.2 . . ? C13 C12 H12A 110.7 . . ? C13 C12 H12B 110.7 . . ? H12A C12 H12B 108.8 . . ? O4 C12 C13 105.5(9) . . ? O4 C12 H12A 110.7 . . ? O4 C12 H12B 110.7 . . ? C12 O4 Y 118.7(6) . . ? C11 O4 Y 118.3(6) . . ? C11 O4 C12 115.1(8) . . ? O4 C11 H11A 110.9 . . ? O4 C11 H11B 110.9 . . ? O4 C11 C10 104.3(9) . . ? H11A C11 H11B 108.9 . . ? C10 C11 H11A 110.9 . . ? C10 C11 H11B 110.9 . . ? C11 C10 H10A 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? O5 C10 C11 110.3(8) . . ? O5 C10 H10A 109.6 . . ? O5 C10 H10B 109.6 . . ? C10 O5 Y 118.8(6) . . ? C10 O5 C9 116.2(8) . . ? C9 O5 Y 115.8(6) . . ? O5 C9 H9A 110.1 . . ? O5 C9 H9B 110.1 . . ? O5 C9 C8 108.0(9) . . ? H9A C9 H9B 108.4 . . ? C8 C9 H9A 110.1 . . ? C8 C9 H9B 110.1 . . ? C9 C8 H8A 110.7 . . ? C9 C8 H8B 110.7 . . ? H8A C8 H8B 108.8 . . ? O6 C8 C9 105.4(9) . . ? O6 C8 H8A 110.7 . . ? O6 C8 H8B 110.7 . . ? C8 O6 Y 123.1(6) . . ? C6 O6 Y 120.3(5) . . ? C6 O6 C8 116.6(8) . . ? O6 C6 C7 113.9(8) . . ? C5 C6 O6 123.7(9) . . ? C5 C6 C7 122.2(10) . . ? O1 C7 C6 117.5(9) . . ? O1 C7 C2 125.5(8) . . ? C2 C7 C6 117.0(9) . . ? C6 C5 H5 119.8 . . ? C6 C5 C4 120.3(10) . . ? C4 C5 H5 119.8 . . ? C5 C4 H4 120.3 . . ? C3 C4 C5 119.3(10) . . ? C3 C4 H4 120.3 . . ? C4 C3 H3 119.5 . . ? C4 C3 C2 121.0(10) . . ? C2 C3 H3 119.5 . . ? C7 C2 C3 119.7(9) . . ? C7 C2 C1 126.6(9) . . ? C3 C2 C1 113.7(9) . . ? C2 C1 H1 115.6 . . ? N1 C1 C2 128.9(9) . . ? N1 C1 H1 115.6 . . ? C1 N1 U 126.8(6) . . ? C1 N1 C24 116.9(9) . . ? C24 N1 U 116.2(7) . . ? N1 C24 H24A 109.8 . . ? N1 C24 H24B 109.8 . . ? N1 C24 C23 109.4(9) . . ? H24A C24 H24B 108.2 . . ? C23 C24 H24A 109.8 . . ? C23 C24 H24B 109.8 . . ? N3 C23 C24 110.8(9) . . ? N3 C23 H23A 109.5 . . ? N3 C23 H23B 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C1S N1S Y 172.9(8) . . ? N1S C1S C2S 179.7(15) . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SB 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? O11 S1 C26 101.8(5) . . ? O12 S1 O11 114.4(5) . . ? O12 S1 O13 116.7(7) . . ? O12 S1 C26 103.6(7) . . ? O13 S1 O11 113.5(5) . . ? O13 S1 C26 104.6(6) . . ? S1 O11 Y 148.9(4) . . ? F11 C26 S1 111.5(8) . . ? F11 C26 F12 104.4(11) . . ? F12 C26 S1 110.1(9) . . ? F13 C26 S1 112.5(9) . . ? F13 C26 F11 109.7(12) . . ? F13 C26 F12 108.3(13) . . ? O21 S2 C27 99.9(6) . . ? O22 S2 O21 112.9(5) . . ? O22 S2 O23 116.6(5) . . ? O22 S2 C27 104.4(8) . . ? O23 S2 O21 115.1(5) . . ? O23 S2 C27 105.5(9) . . ? S2 O21 Y 148.1(4) . . ? F21 C27 S2 107.3(12) . . ? F23 C27 S2 112.5(13) . . ? F23 C27 F21 109.5(18) . . ? F23 C27 F22 109.9(16) . . ? F22 C27 S2 110.5(15) . . ? F22 C27 F21 106.9(17) . . ? O31 S3 C28 102.8(7) . . ? O32 S3 O31 112.9(7) . . ? O32 S3 O33 118.0(7) . . ? O32 S3 C28 103.0(6) . . ? O33 S3 O31 114.8(7) . . ? O33 S3 C28 102.7(8) . . ? F31 C28 S3 109.7(10) . . ? F32 C28 S3 113.0(10) . . ? F32 C28 F31 105.8(12) . . ? F33 C28 S3 112.6(10) . . ? F33 C28 F31 107.6(13) . . ? F33 C28 F32 107.7(12) . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma _refln_scale_group_code 1 0 0 2970.31 166.215 27 2 0 0 6018.57 335.714 27 -3 0 0 152.407 31.3612 16 3 0 0 154.873 14.5704 27 -4 0 0 52.1307 34.727 16 -4 0 0 32.9808 9.0649 12 -4 0 0 35.3356 13.5883 26 4 0 0 26.002 13.9726 11 -5 0 0 194.739 17.5341 12 -5 0 0 202.613 45.4913 16 -5 0 0 204.189 22.4133 26 5 0 0 153.926 22.6285 11 -6 0 0 672.281 45.8872 28 -6 0 0 842.494 83.9117 16 -6 0 0 713.475 46.1192 12 -6 0 0 657.646 51.491 26 6 0 0 692.453 53.1754 11 -7 0 0 -69.417 75.511 16 -7 0 0 42.9563 14.7843 6 -7 0 0 61.3302 13.3556 4 -7 0 0 37.798 14.1592 7 -7 0 0 74.4255 25.0923 26 -7 0 0 48.0987 16.6265 28 -8 0 0 319.89 32.6384 20 -8 0 0 315.294 22.8791 2 -8 0 0 347.812 28.1403 6 -8 0 0 321.179 28.4874 7 -8 0 0 281.996 27.6655 28 -8 0 0 325.442 27.3271 4 -9 0 0 155.489 13.3966 2 -9 0 0 147.71 18.8457 4 -9 0 0 183.506 23.3221 20 -9 0 0 156.211 20.5096 28 -9 0 0 180.157 18.3349 6 -9 0 0 180.71 18.3663 7 -10 0 0 14.0442 10.2829 7 -10 0 0 17.2009 10.6437 6 -10 0 0 20.8939 13.6282 20 -10 1 0 34.4009 14.9851 20 -10 1 0 38.9289 12.0495 6 -10 1 0 35.4719 10.7389 7 -9 1 0 -9.8509 19.2802 20 -9 1 0 8.03557 13.3958 6 -9 1 0 24.4726 13.8156 7 -9 1 0 2.71407 16.0557 28 -9 1 0 1.68676 7.84181 2 -8 1 0 14.6835 14.4417 6 -8 1 0 23.4116 21.972 20 -8 1 0 12.1351 8.81449 2 -8 1 0 -7.2009 14.4076 7 -8 1 0 -12.581 16.3541 28 7 -1 0 76.542 26.5687 11 -7 1 0 76.9448 15.4228 6 -7 1 0 44.6203 15.9318 28 -7 1 0 55.5292 14.8522 7 -7 1 0 88.9169 68.3883 16 -7 1 0 98.2066 23.7097 26 6 -1 0 517.64 44.2614 11 -6 1 0 547.513 71.8815 16 -6 1 0 513.231 35.9909 28 -6 1 0 516.789 43.4705 26 5 -1 0 2314.06 134.404 11 -5 1 0 2154.33 149.829 16 -5 1 0 2422.07 133.813 26 -5 1 0 2276.84 131.089 12 4 -1 0 47.4001 11.6485 27 4 -1 0 57.7686 14.5823 11 -4 1 0 26.8002 9.06943 12 -4 1 0 62.7342 32.1384 16 -4 1 0 33.2045 12.9991 26 3 -1 0 2309.62 131.488 27 2 -1 0 2695.66 149.04 27 -2 1 0 2782.02 150.162 14 -2 1 0 2455.27 148.8 27 1 -1 0 108.502 12.3019 14 1 -1 0 98.1982 8.7974 27 -1 1 0 87.6346 8.52572 27 -1 1 0 84.9822 10.8302 14 0 -1 0 1320.79 71.1385 14 0 1 0 1202.83 70.9216 14 0 1 0 1209.3 69.487 27 -3 -1 0 1049.98 61.2561 12 -4 -1 0 512.904 53.2267 16 -4 -1 0 532.818 33.8626 12 -4 -1 0 592.732 38.3714 26 4 1 0 437.775 38.0035 11 -5 -1 0 4.25371 17.1222 26 -5 -1 0 11.4034 43.9748 16 -5 -1 0 6.93981 11.3331 12 5 1 0 -1.4441 17.6312 11 -6 -1 0 160.803 25.7243 26 -6 -1 0 233.309 62.8854 16 -6 -1 0 163.762 18.951 12 -6 -1 0 127.429 17.4771 28 -7 -1 0 31.4741 8.92329 2 -7 -1 0 0.59493 20.9103 12 -7 -1 0 30.9334 16.0707 28 -7 -1 0 13.0758 13.5554 6 -7 -1 0 4.71187 75.4406 16 -7 -1 0 30.7427 25.6835 26 -7 -1 0 34.8894 12.8892 4 -7 -1 0 40.0075 21.3186 20 -7 -1 0 44.4232 13.238 7 -7 -1 0 46.8237 13.2886 1 -8 -1 0 136.002 21.5797 28 -8 -1 0 114.335 16.0815 4 -8 -1 0 149.66 17.8636 7 -8 -1 0 116.109 16.7771 1 -8 -1 0 109.243 15.9973 6 -8 -1 0 123.42 25.0861 20 -8 -1 0 132.84 12.3334 2 -9 -1 0 106.863 14.3622 7 -9 -1 0 39.264 18.2454 20 -9 -1 0 80.8306 12.9564 4 -9 -1 0 110.238 16.7443 28 -9 -1 0 80.2443 13.6081 6 -10 -1 0 -11.518 11.8679 20 -10 -1 0 -0.7331 12.2166 6 -10 2 0 48.988 11.9977 7 -10 2 0 39.1923 15.4441 20 -10 2 0 64.5849 13.1679 6 -9 2 0 50.1734 15.095 7 -9 2 0 64.0316 17.1508 28 -9 2 0 52.0391 15.4981 6 -9 2 0 45.7863 9.13823 2 -9 2 0 80.4485 22.1382 20 -8 2 0 319.616 23.4381 2 -8 2 0 346.327 27.356 7 -8 2 0 364.572 36.138 20 -8 2 0 314.649 28.7857 6 -8 2 0 309.758 28.925 28 7 -2 0 88.9842 24.3969 11 -7 2 0 65.5622 23.2339 7 -7 2 0 57.1904 15.9458 28 -7 2 0 56.3612 16.9084 6 6 -2 0 99.0586 22.2524 11 -6 2 0 124.813 20.9548 26 -6 2 0 165.871 51.3629 16 -6 2 0 100.101 14.7809 28 5 -2 0 465.08 38.1555 11 -5 2 0 414.625 54.3657 16 -5 2 0 471.379 36.5095 26 4 -2 0 125.556 15.7324 27 4 -2 0 150.598 18.1986 11 -4 2 0 81.5129 34.8823 16 -4 2 0 133.452 17.4375 26 -4 2 0 139.368 13.1294 12 3 -2 0 3133.68 177.614 27 -3 2 0 3142.34 179.687 14 2 -2 0 5668.02 314.602 27 -2 2 0 5576.33 316.66 14 1 -2 0 705.353 43.1483 27 1 -2 0 804.248 48.9218 14 -1 2 0 706.177 43.178 27 -1 2 0 699.744 47.7566 14 0 -2 0 226.919 24.5869 14 0 2 0 213.795 14.8168 27 0 2 0 196.794 23.5201 14 -3 -2 0 383.775 27.5528 12 -3 -2 0 417.734 31.6308 26 -4 -2 0 20.3172 9.98327 12 -4 -2 0 18.8795 15.794 26 4 2 0 28.6455 15.4451 11 -5 -2 0 397.992 56.7568 16 -5 -2 0 351.488 28.3758 28 -5 -2 0 391.218 35.7935 26 -5 -2 0 369.524 29.2848 12 -6 -2 0 753.807 59.9828 26 -6 -2 0 848.756 52.5063 12 -6 -2 0 884.134 108.607 16 -6 -2 0 764.157 51.5013 28 -7 -2 0 108.198 15.4516 6 -7 -2 0 131.382 28.9461 26 -7 -2 0 82.9987 11.052 2 -7 -2 0 104.27 15.0683 1 -7 -2 0 194.263 81.3302 16 -7 -2 0 75.4735 18.1224 12 -7 -2 0 96.3089 14.4988 4 -7 -2 0 106.756 23.2336 20 -7 -2 0 83.4302 15.4857 7 -7 -2 0 116.092 19.8701 28 -8 -2 0 18.9956 9.52788 23 -8 -2 0 17.4894 12.1924 6 -8 -2 0 12.9915 11.6785 1 -8 -2 0 14.5942 13.7918 7 -8 -2 0 11.5568 20.388 20 -8 -2 0 4.20909 12.8345 4 -8 -2 0 39.2681 17.0944 28 -8 -2 0 -2.5884 8.30333 2 -9 -2 0 10.9111 11.4779 6 -9 -2 0 7.36468 11.0717 7 -9 -2 0 -3.6808 10.3419 4 -9 -2 0 11.1202 15.598 20 -10 3 0 6.94871 12.2792 6 -10 3 0 16.1197 11.1456 7 -10 3 0 -3.2096 14.4892 20 -9 3 0 62.2539 15.6939 7 -9 3 0 82.5784 18.4569 28 -9 3 0 66.4695 9.93968 2 -9 3 0 59.6163 15.4106 6 -9 3 0 111.743 22.0618 20 -8 3 0 215.569 17.4175 2 -8 3 0 284.741 28.543 20 -8 3 0 216.772 21.975 6 -8 3 0 257.874 22.4034 7 -8 3 0 193.749 23.4692 28 7 -3 0 126.927 25.2746 11 -7 3 0 91.2132 17.3899 28 6 -3 0 180.892 24.7798 11 -6 3 0 196.387 18.577 28 -6 3 0 196.214 26.7221 26 5 -3 0 2103.18 123.473 11 -5 3 0 2114.09 141.822 16 -5 3 0 2112.2 123.19 26 4 -3 0 1069.82 66.3448 27 4 -3 0 1027.91 66.7594 11 -4 3 0 1202.15 85.2815 16 -4 3 0 1101.61 66.3198 26 3 -3 0 31.9209 12.373 27 -3 3 0 65.6228 20.9497 14 2 -3 0 323.676 26.0562 27 -2 3 0 294.794 37.4262 14 1 -3 0 18.266 8.54443 27 -1 3 0 3.58694 8.45066 27 -1 3 0 18.5212 16.7503 14 0 3 0 568.037 43.1341 14 1 3 0 3396.08 193.179 14 -2 -3 0 478.51 31.7079 12 -2 -3 0 520.606 39.1605 26 -3 -3 0 390.387 28.1076 12 -3 -3 0 410.061 33.4366 26 -4 -3 0 544.63 41.84 26 -4 -3 0 508.274 35.45 12 -5 -3 0 80.2493 14.6201 12 -5 -3 0 83.9632 13.7224 28 -5 -3 0 69.1474 21.3698 26 -5 -3 0 96.5872 47.7601 16 -6 -3 0 700.317 86.4508 16 -6 -3 0 531.275 49.3812 26 -6 -3 0 510.67 36.2622 7 -6 -3 0 542.355 40.2028 4 -6 -3 0 505.673 40.1029 28 -6 -3 0 517.985 35.811 6 -6 -3 0 562.861 40.4968 12 -7 -3 0 223.122 80.3749 16 -7 -3 0 217.079 23.5665 28 -7 -3 0 188.155 17.8945 1 -7 -3 0 227.625 22.9863 12 -7 -3 0 190.366 15.8694 2 -7 -3 0 194.498 19.0174 6 -7 -3 0 207.74 19.5648 4 -7 -3 0 161.118 25.9821 20 -7 -3 0 192.959 19.5826 7 -8 -3 0 32.8429 12.6758 6 -8 -3 0 55.1026 15.8971 28 -8 -3 0 41.7119 13.3919 4 -8 -3 0 -3.063 20.3742 20 -8 -3 0 18.3818 11.2571 1 -8 -3 0 48.9444 9.66962 23 -8 -3 0 36.6898 13.2691 7 -9 -3 0 86.9737 17.5749 20 -9 -3 0 100.732 12.2669 7 -9 -3 0 106.817 12.1198 4 -9 -3 0 124.842 14.4663 6 -10 4 0 106.219 14.264 7 -10 4 0 137.429 16.6672 6 -9 4 0 18.6295 14.0395 6 -9 4 0 22.418 14.8901 7 -9 4 0 11.6773 16.4504 28 -9 4 0 41.4478 20.7671 20 -9 4 0 -4.8465 8.27116 2 -8 4 0 -7.8779 8.96852 2 -8 4 0 8.01049 14.449 6 -8 4 0 -0.5662 16.9509 28 -8 4 0 18.9216 14.7431 7 7 -4 0 271.317 31.6171 11 -7 4 0 245.495 24.5257 28 6 -4 0 39.392 19.8449 11 -6 4 0 18.8645 12.2429 28 5 -4 0 2668.76 154.122 11 4 -4 0 1693.87 107.256 11 4 -4 0 1869.09 107.935 27 -4 4 0 1863.32 114.015 14 -4 4 0 1940.13 106.616 26 3 -4 0 94.0271 14.2837 27 -3 4 0 79.2951 24.7809 14 2 -4 0 456.014 33.6696 13 2 -4 0 606.936 36.3744 27 -2 4 0 559.945 48.6913 14 1 -4 0 1030.25 60.9942 27 -1 4 0 1038.63 70.2064 14 0 4 0 419.526 40.4728 14 -1 -4 0 1507.01 88.8157 12 1 4 0 1615.97 94.5295 14 -2 -4 0 14.8865 8.01181 12 -3 -4 0 686.294 45.7439 26 -3 -4 0 645.121 41.8884 12 -4 -4 0 507.955 36.3738 28 -4 -4 0 553.707 42.7975 26 -4 -4 0 531.292 36.5766 12 -5 -4 0 172.947 52.0921 16 -5 -4 0 221.471 21.9442 12 -5 -4 0 188.298 20.2134 28 -6 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35.1498 6.89183 23 -4 1 21 34.0419 9.39055 20 -4 1 21 42.9649 4.77045 3 -3 1 21 32.5976 4.97448 2 -3 1 21 20.625 9.42271 20 -3 1 21 28.0995 5.09791 22 -3 1 21 28.4812 6.93374 23 -3 1 21 30.4199 4.76485 3 -2 1 21 11.101 8.67243 20 -2 1 21 -7.6082 4.46091 22 -2 1 21 -4.7448 4.18346 2 -1 1 21 32.2102 8.48433 20 -6 2 21 63.2936 6.2361 22 -5 2 21 20.7044 5.98331 23 -5 2 21 26.8021 4.36111 22 -5 2 21 35.6039 4.41964 2 -5 2 21 48.9108 8.34541 20 -5 2 21 25.7959 4.19243 3 -4 2 21 8.72071 8.14871 20 -4 2 21 3.48381 3.96329 2 -4 2 21 -2.0577 4.09929 22 -4 2 21 -3.2965 3.68988 3 -4 2 21 -6.423 5.71749 23 -3 2 21 10.6045 4.2962 22 -3 2 21 10.7219 4.10741 2 -3 2 21 13.1484 8.37502 20 -2 2 21 12.1421 8.01235 20 -1 2 21 41.3386 7.94872 20 -5 3 21 22.0973 7.38389 20 -4 3 21 9.89524 7.2723 20 -3 3 21 72.2887 9.19537 20 -2 3 21 48.2845 9.8455 20 -1 -8 22 22.4269 3.14468 3 -1 -8 22 27.7631 4.21466 23 -3 -7 22 15.6949 3.85943 23 -3 -7 22 18.2185 2.95314 3 -2 -7 22 8.81823 2.67489 3 -2 -7 22 6.91024 3.28972 22 -2 -7 22 10.3907 2.57676 2 -2 -7 22 10.8129 3.7467 23 -1 -7 22 11.865 3.31226 22 -1 -7 22 10.97 2.74198 2 -1 -7 22 13.5127 2.8428 3 -1 -7 22 16.0478 3.9218 23 0 -7 22 18.0196 6.40215 23 0 -7 22 9.22012 2.62458 2 0 -7 22 7.14652 2.85131 22 -3 -6 22 0.97959 2.4809 3 -3 -6 22 1.92942 3.5809 23 -2 -6 22 10.7976 4.24613 23 -2 -6 22 14.1815 2.89883 2 -2 -6 22 12.6275 3.01603 3 -2 -6 22 12.5566 3.58074 22 -1 -6 22 55.1709 4.51275 3 -1 -6 22 46.6224 4.72495 22 -1 -6 22 52.8518 5.50976 23 -1 -6 22 60.3611 5.21543 2 0 -6 22 12.4045 3.00553 3 0 -6 22 12.5607 3.21814 22 0 -6 22 12.2597 3.04689 2 0 -6 22 7.35336 4.24295 23 -4 -5 22 -1.3457 3.74584 23 -4 -5 22 2.57792 2.40084 3 -3 -5 22 12.2675 4.21076 23 -3 -5 22 11.3292 3.592 22 -3 -5 22 6.80448 3.03907 2 -3 -5 22 5.82997 2.9159 3 -2 -5 22 8.90779 3.16237 2 -2 -5 22 10.7029 4.56462 23 -2 -5 22 11.2336 3.15055 3 -2 -5 22 14.7671 3.76968 22 -1 -5 22 89.2979 6.54502 3 -1 -5 22 92.0428 7.74147 23 -1 -5 22 72.9189 6.8518 22 -1 -5 22 81.0483 6.67909 2 0 -5 22 14.3926 3.42914 22 0 -5 22 14.4615 3.31497 2 0 -5 22 12.5177 4.5465 23 0 -5 22 19.7818 3.374 3 -4 -4 22 42.9884 5.47904 23 -4 -4 22 60.4399 4.83197 3 -3 -4 22 39.2736 5.46458 23 -3 -4 22 52.971 4.79823 22 -3 -4 22 43.2633 4.21301 3 -3 -4 22 43.6921 4.27908 2 -2 -4 22 -3.3484 3.19683 3 -2 -4 22 3.09949 4.68411 23 -2 -4 22 -1.8723 3.70295 22 -2 -4 22 0.08734 3.275 2 -1 -4 22 25.5768 3.76426 3 -1 -4 22 25.7691 5.09284 23 -1 -4 22 19.4867 3.76524 2 -1 -4 22 20.7515 3.94183 22 0 -4 22 7.81529 3.28114 2 0 -4 22 8.61026 3.38049 22 -5 -3 22 2.92541 2.42985 3 -5 -3 22 -4.3706 3.69172 23 -4 -3 22 29.7044 3.66202 3 -4 -3 22 34.7277 4.23245 22 -4 -3 22 28.0994 3.58059 2 -4 -3 22 23.5343 5.19326 23 -3 -3 22 14.8777 3.53548 3 -3 -3 22 13.5316 4.2625 22 -3 -3 22 20.7833 3.51029 2 -3 -3 22 18.468 5.13621 23 -2 -3 22 3.43527 3.43979 2 -2 -3 22 0.96331 3.92142 22 -2 -3 22 -2.8767 5.02491 23 -2 -3 22 3.52398 3.37016 3 -1 -3 22 5.65493 3.74348 22 -1 -3 22 1.84471 4.95295 23 -1 -3 22 4.99799 3.31606 3 -1 -3 22 3.67703 3.46627 2 0 -3 22 103.627 9.1801 22 -5 -2 22 36.7554 4.96595 23 -5 -2 22 39.7549 3.73537 3 -4 -2 22 1.32503 3.13444 3 -4 -2 22 -4.8555 3.06538 2 -4 -2 22 0.96231 4.74833 23 -4 -2 22 -2.1751 3.81117 22 -3 -2 22 11.2756 4.13632 22 -3 -2 22 16.1015 5.59621 23 -3 -2 22 20.7836 3.68032 2 -3 -2 22 14.5522 3.59043 3 -2 -2 22 9.13126 3.6135 2 -2 -2 22 -3.987 3.45643 3 -2 -2 22 -2.333 3.85443 22 -2 -2 22 -9.9021 5.52342 23 -1 -2 22 3.10327 6.33599 23 -1 -2 22 30.5142 4.1748 22 -1 -2 22 26.5026 3.95276 2 -1 -2 22 20.3683 5.70279 3 -5 -1 22 21.3573 3.20342 3 -5 -1 22 12.0822 4.47455 23 -5 -1 22 23.4229 3.78323 22 -5 -1 22 21.667 3.41311 2 -4 -1 22 11.1432 3.93134 22 -4 -1 22 8.02815 3.37548 2 -4 -1 22 2.77912 3.31991 3 -4 -1 22 6.62192 5.11697 23 -3 -1 22 66.2254 6.44905 22 -3 -1 22 94.4161 6.92699 3 -3 -1 22 87.3773 6.75437 2 -3 -1 22 80.6185 7.47721 23 -2 -1 22 36.5755 4.18401 3 -2 -1 22 24.7401 4.46759 22 -2 -1 22 34.0765 4.16451 2 -2 -1 22 20.3084 5.80594 23 -1 -1 22 4.48385 4.66828 22 -5 0 22 14.102 3.06054 3 -5 0 22 10.9164 3.24626 2 -5 0 22 8.91211 3.40913 22 -5 0 22 -5.3827 4.34609 23 -4 0 22 0.53329 3.54441 22 -4 0 22 -7.8579 4.89393 23 -4 0 22 -1.6672 3.31764 2 -4 0 22 17.6081 10.088 20 -4 0 22 -0.6039 3.13809 3 -3 0 22 9.23073 3.69765 2 -3 0 22 0.77841 5.42866 23 -3 0 22 5.10525 3.4522 3 -3 0 22 4.98176 3.71275 22 -3 0 22 24.2492 9.76005 20 -2 0 22 24.3198 4.08828 22 -2 0 22 29.2458 4.0085 2 -4 1 22 15.2936 3.60195 22 -4 1 22 21.6822 3.69346 2 -3 1 22 5.78137 5.70313 22 -2 -4 23 37.4115 5.1722 2 -2 -4 23 33.764 3.98083 22 -3 -3 23 -0.2054 5.69397 23 -2 -3 23 4.54237 3.91151 22 _iucr_refine_instructions_details ; q27i.res created by SHELXL-2014/7 TITL q27i in P1 CELL 1.54178 9.1814 13.6032 18.8769 102.0953 102.738 103.9906 ZERR 2 0.0006 0.0008 0.0012 0.0046 0.0055 0.0051 LATT 1 SFAC C H F N O S U Y UNIT 60 68 18 8 34 6 2 2 L.S. 50 PLAN 20 SIZE 0.025 0.03 0.03 TEMP -73.16 BOND $H fmap 2 acta 132 REM REM REM WGHT 0.065800 5.303800 FVAR 0.27260 U 7 0.323339 0.039042 0.161431 11.00000 0.04027 0.03191 = 0.05384 0.00516 0.01360 0.01238 Y 8 0.538367 0.326120 0.286807 11.00000 0.03749 0.03195 = 0.04751 0.00318 0.01302 0.00995 O2 5 0.392009 0.156019 0.283441 11.00000 0.04097 0.03308 = 0.04352 0.00469 0.01400 0.01040 O1 5 0.447270 0.206760 0.154650 11.00000 0.03228 0.03411 = 0.04831 0.00972 0.00979 0.01268 O7 5 0.132564 0.050678 0.152499 11.00000 0.03724 0.03900 = 0.05817 0.00197 0.01209 0.00743 O8 5 0.505746 0.012903 0.163673 11.00000 0.04215 0.04112 = 0.06481 0.00579 0.01422 0.01138 N3 4 0.193445 -0.157018 0.087584 11.00000 0.03754 0.03704 = 0.06623 0.00015 0.01227 0.00725 C22 1 0.278815 -0.212862 0.129911 11.00000 0.07153 0.04348 = 0.06635 0.01389 0.01498 0.02360 AFIX 23 H22A 2 0.391060 -0.187831 0.132654 11.00000 -1.20000 H22B 2 0.238927 -0.289177 0.103375 11.00000 -1.20000 AFIX 0 C21 1 0.261290 -0.195444 0.211107 11.00000 0.06887 0.04620 = 0.07704 0.02211 0.02182 0.01293 AFIX 23 H21A 2 0.156376 -0.238425 0.209682 11.00000 -1.20000 H21B 2 0.341069 -0.217688 0.243027 11.00000 -1.20000 AFIX 0 N2 4 0.281930 -0.081319 0.243780 11.00000 0.05028 0.03427 = 0.06994 0.01281 0.01695 0.01623 C20 1 0.260161 -0.057450 0.307360 11.00000 0.06141 0.04134 = 0.06970 0.02526 0.01518 0.00723 AFIX 43 H20 2 0.244318 -0.112491 0.331233 11.00000 -1.20000 AFIX 0 C18 1 0.255928 0.045393 0.350094 11.00000 0.04520 0.05746 = 0.05813 0.02114 0.01410 0.01557 C19 1 0.311102 0.142397 0.334422 11.00000 0.03406 0.05513 = 0.04270 0.01135 0.00603 0.00949 C17 1 0.183864 0.041442 0.407295 11.00000 0.06761 0.06157 = 0.06919 0.02517 0.02100 0.00922 AFIX 43 H17 2 0.153945 -0.023168 0.419803 11.00000 -1.20000 AFIX 0 C16 1 0.154537 0.128607 0.446419 11.00000 0.05913 0.07607 = 0.05541 0.01409 0.02453 0.01199 AFIX 43 H16 2 0.101786 0.123702 0.484142 11.00000 -1.20000 AFIX 0 C15 1 0.204165 0.225096 0.429480 11.00000 0.05657 0.06758 = 0.05154 0.01038 0.02235 0.01462 AFIX 43 H15 2 0.185372 0.286163 0.455922 11.00000 -1.20000 AFIX 0 C14 1 0.280641 0.230644 0.374006 11.00000 0.03441 0.05367 = 0.04424 0.00753 0.00918 0.01296 O3 5 0.332312 0.321844 0.353660 11.00000 0.04849 0.04320 = 0.05012 0.00597 0.01933 0.01519 C13 1 0.316459 0.415104 0.398441 11.00000 0.05562 0.04983 = 0.05852 -0.00324 0.01926 0.01932 AFIX 23 H13A 2 0.370821 0.427048 0.452395 11.00000 -1.20000 H13B 2 0.204438 0.407921 0.393280 11.00000 -1.20000 AFIX 0 C12 1 0.387678 0.505473 0.371004 11.00000 0.06513 0.04604 = 0.06900 0.00151 0.01930 0.02272 AFIX 23 H12A 2 0.319725 0.502799 0.321547 11.00000 -1.20000 H12B 2 0.402942 0.573492 0.407620 11.00000 -1.20000 AFIX 0 O4 5 0.533858 0.493848 0.364098 11.00000 0.05299 0.03645 = 0.07796 0.00134 0.01993 0.01292 C11 1 0.646088 0.587365 0.367116 11.00000 0.08113 0.04819 = 0.06471 0.00508 0.02589 0.01838 AFIX 23 H11A 2 0.644362 0.647874 0.406248 11.00000 -1.20000 H11B 2 0.626390 0.603292 0.317670 11.00000 -1.20000 AFIX 0 C10 1 0.800570 0.564369 0.386937 11.00000 0.07215 0.02771 = 0.05235 -0.00147 -0.00316 0.00067 AFIX 23 H10A 2 0.884555 0.622156 0.382654 11.00000 -1.20000 H10B 2 0.826484 0.560526 0.439850 11.00000 -1.20000 AFIX 0 O5 5 0.792493 0.467730 0.337847 11.00000 0.05069 0.04577 = 0.06732 0.00560 0.01855 0.01155 C9 1 0.889354 0.474285 0.288603 11.00000 0.04777 0.04877 = 0.07420 0.00086 0.01667 0.00171 AFIX 23 H9A 2 0.927018 0.411639 0.280653 11.00000 -1.20000 H9B 2 0.981467 0.538041 0.310966 11.00000 -1.20000 AFIX 0 C8 1 0.793309 0.479538 0.214278 11.00000 0.05131 0.04407 = 0.07488 0.01018 0.02519 0.00025 AFIX 23 H8A 2 0.771539 0.548142 0.219944 11.00000 -1.20000 H8B 2 0.849243 0.470530 0.175278 11.00000 -1.20000 AFIX 0 O6 5 0.649241 0.393947 0.193690 11.00000 0.03958 0.03605 = 0.05953 0.00466 0.01781 0.00449 C6 1 0.572442 0.351718 0.117088 11.00000 0.03685 0.04610 = 0.05954 0.01403 0.02110 0.01353 C7 1 0.466463 0.247969 0.098068 11.00000 0.03605 0.04442 = 0.05763 0.01125 0.02313 0.01942 C5 1 0.588519 0.405420 0.064702 11.00000 0.05544 0.05824 = 0.07163 0.02911 0.02749 0.01572 AFIX 43 H5 2 0.655530 0.475947 0.080002 11.00000 -1.20000 AFIX 0 C4 1 0.507356 0.357626 -0.011175 11.00000 0.06576 0.06363 = 0.06166 0.03015 0.02957 0.02348 AFIX 43 H4 2 0.518301 0.395222 -0.047764 11.00000 -1.20000 AFIX 0 C3 1 0.411254 0.255547 -0.032651 11.00000 0.06078 0.07012 = 0.05648 0.02635 0.02705 0.03431 AFIX 43 H3 2 0.356086 0.222565 -0.084474 11.00000 -1.20000 AFIX 0 C2 1 0.392984 0.198208 0.021754 11.00000 0.04107 0.04936 = 0.06164 0.01948 0.02344 0.02237 C1 1 0.300411 0.089097 -0.011213 11.00000 0.04468 0.05649 = 0.04634 0.00183 0.00081 0.02671 AFIX 43 H1 2 0.259606 0.067739 -0.064721 11.00000 -1.20000 AFIX 0 N1 4 0.265067 0.015764 0.022374 11.00000 0.03687 0.04052 = 0.05731 0.00103 0.00259 0.01035 C24 1 0.176478 -0.089608 -0.025806 11.00000 0.07169 0.04923 = 0.04520 -0.00184 -0.00397 0.01560 AFIX 23 H24A 2 0.197564 -0.099022 -0.075625 11.00000 -1.20000 H24B 2 0.062972 -0.099680 -0.033912 11.00000 -1.20000 AFIX 0 C23 1 0.223500 -0.170273 0.011340 11.00000 0.06381 0.05142 = 0.06502 0.00529 0.02067 0.02104 AFIX 23 H23A 2 0.163040 -0.242181 -0.021432 11.00000 -1.20000 H23B 2 0.336109 -0.161806 0.017391 11.00000 -1.20000 AFIX 0 C25 1 0.024204 -0.195731 0.077485 11.00000 0.05037 0.07312 = 0.08973 0.00826 0.01691 -0.00092 AFIX 33 H25A 2 -0.029480 -0.156191 0.048684 11.00000 -1.50000 H25B 2 -0.015367 -0.270826 0.049954 11.00000 -1.50000 H25C 2 0.004602 -0.185991 0.127084 11.00000 -1.50000 AFIX 0 N1S 4 0.726978 0.232237 0.272263 11.00000 0.04186 0.03951 = 0.05684 0.00429 0.01346 0.01612 C1S 1 0.803027 0.178596 0.262320 11.00000 0.04150 0.05215 = 0.05352 0.00193 0.00589 0.01123 C2S 1 0.897919 0.112700 0.250321 11.00000 0.05842 0.05770 = 0.08367 0.01343 0.02670 0.02730 AFIX 137 H2SA 2 0.971058 0.141731 0.223800 11.00000 -1.50000 H2SB 2 0.831614 0.041895 0.219701 11.00000 -1.50000 H2SC 2 0.956950 0.108735 0.299133 11.00000 -1.50000 AFIX 0 S1 6 0.184001 0.351196 0.166978 11.00000 0.04283 0.04696 = 0.06490 0.01625 0.02056 0.01707 F11 3 0.050412 0.460481 0.090739 11.00000 0.08088 0.11595 = 0.11182 0.05665 0.02577 0.05189 F12 3 0.216789 0.551233 0.194236 11.00000 0.15151 0.04539 = 0.16381 0.02395 0.01310 0.03648 F13 3 0.294560 0.489022 0.101390 11.00000 0.12187 0.17510 = 0.25302 0.16723 0.11714 0.08827 O11 5 0.345206 0.377893 0.215005 11.00000 0.04536 0.04798 = 0.05050 0.00911 0.01293 0.02222 O12 5 0.146286 0.270496 0.099392 11.00000 0.05843 0.07357 = 0.08214 -0.01120 -0.00973 0.02420 O13 5 0.071486 0.345505 0.207816 11.00000 0.06015 0.11666 = 0.12635 0.06001 0.05676 0.04508 C26 1 0.188898 0.468018 0.135327 11.00000 0.05680 0.06843 = 0.10983 0.05618 0.03495 0.02597 S2 6 0.779634 0.324903 0.467473 11.00000 0.05068 0.04481 = 0.04803 0.00181 0.00925 0.01721 F21 3 0.821876 0.198550 0.548319 11.00000 0.15190 0.12835 = 0.17922 0.10037 -0.04451 0.00519 F23 3 0.585931 0.207438 0.520382 11.00000 0.12234 0.15052 = 0.13848 0.08817 0.02949 -0.00961 F22 3 0.666947 0.121555 0.437071 11.00000 0.13511 0.03908 = 0.23578 0.01014 -0.01249 0.01310 O21 5 0.642178 0.318152 0.408459 11.00000 0.04583 0.05452 = 0.05337 0.01102 0.01102 0.01513 O22 5 0.812052 0.408449 0.533518 11.00000 0.06205 0.06321 = 0.06487 -0.01465 0.01724 0.01502 O23 5 0.909818 0.311608 0.441971 11.00000 0.05341 0.11216 = 0.06026 -0.00685 0.00426 0.03821 C27 1 0.704615 0.205761 0.494588 11.00000 0.10342 0.06742 = 0.12248 0.05446 -0.00826 0.01214 S3 6 0.789739 -0.209828 0.255181 11.00000 0.07242 0.05140 = 0.06908 0.01686 0.01994 0.00890 F31 3 0.628596 -0.081124 0.287223 11.00000 0.09264 0.13343 = 0.14716 0.06600 0.04084 0.06493 F32 3 0.630545 -0.186578 0.355120 11.00000 0.11593 0.10960 = 0.10004 0.03961 0.05034 0.01818 F33 3 0.831729 -0.058211 0.376391 11.00000 0.10090 0.10153 = 0.08449 -0.01178 0.01069 0.02129 O31 5 0.901114 -0.242805 0.303012 11.00000 0.08943 0.07407 = 0.13817 0.03664 0.01035 0.03531 O32 5 0.860886 -0.135765 0.220313 11.00000 0.10508 0.06340 = 0.10586 0.02678 0.06074 0.01830 O33 5 0.650949 -0.291784 0.210327 11.00000 0.13371 0.07120 = 0.08009 0.01456 0.00749 -0.00883 C28 1 0.718750 -0.129973 0.323080 11.00000 0.06343 0.07350 = 0.08392 0.02943 0.02003 0.01053 HKLF 4 REM q27i in P1 REM R1 = 0.0498 for 6180 Fo > 4sig(Fo) and 0.0669 for all 7605 data REM 587 parameters refined using 0 restraints END WGHT 0.0658 5.3109 REM Highest difference peak 2.344, deepest hole -1.182, 1-sigma level 0.179 Q1 1 0.3653 0.0988 0.1419 11.00000 0.05 2.34 Q2 1 0.2932 -0.0084 0.1919 11.00000 0.05 2.25 Q3 1 0.3734 0.0600 0.2160 11.00000 0.05 2.01 Q4 1 0.2604 0.0013 0.1035 11.00000 0.05 1.92 Q5 1 0.4703 0.2878 0.2407 11.00000 0.05 1.45 Q6 1 0.1152 -0.2453 0.0362 11.00000 0.05 1.34 Q7 1 0.4921 0.2559 0.3027 11.00000 0.05 1.07 Q8 1 0.5560 0.2642 0.2627 11.00000 0.05 0.98 Q9 1 0.3608 -0.0066 0.1430 11.00000 0.05 0.93 Q10 1 0.4354 0.0661 0.1791 11.00000 0.05 0.92 Q11 1 0.1868 -0.1158 0.1794 11.00000 0.05 0.84 Q12 1 0.3380 0.1263 0.2098 11.00000 0.05 0.82 Q13 1 0.3241 -0.0060 0.2481 11.00000 0.05 0.81 Q14 1 0.0825 -0.1578 0.0391 11.00000 0.05 0.81 Q15 1 0.1352 -0.2082 0.1477 11.00000 0.05 0.79 Q16 1 0.3153 0.0980 0.0787 11.00000 0.05 0.75 Q17 1 0.8695 0.6556 0.3817 11.00000 0.05 0.72 Q18 1 0.5773 0.3776 0.2639 11.00000 0.05 0.68 Q19 1 0.2085 0.0612 0.1076 11.00000 0.05 0.66 Q20 1 0.7284 0.2594 0.4824 11.00000 0.05 0.65 REM The information below was added by Olex2. REM REM R1 = 0.0498 for 6180 Fo > 4sig(Fo) and 0.0669 for all 28130 data REM n/a parameters refined using n/a restraints REM Highest difference peak 2.34, deepest hole -1.18 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0669 REM R1_gt = 0.0498 REM wR_ref = 0.1326 REM GOOF = 1.067 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 28130 REM Reflections_gt = 6180 REM Parameters = n/a REM Hole = -1.18 REM Peak = 2.34 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received' # start Validation Reply Form _vrf_PLAT029_LsalbenUO2Y ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.959 Why? RESPONSE: The completeness could not be increased beyond 0.959 without remounting the crystal, since copper radiation was used for this triclinic structure. (Note the threshold for an alert in this case is the arbitrary value of 0.96.) ; # end Validation Reply Form