data_mo_dhng157 _audit_creation_date 2016-07-12 _audit_creation_method ; Olex2 1.2 (compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _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. (2015a). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015b). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C19 H41 N O3 P2 Ru' _chemical_formula_sum 'C19 H41 N O3 P2 Ru' _chemical_formula_weight 494.54 _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' 0.0033 0.0016 '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' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 '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 14.1700(5) _cell_length_b 15.3918(6) _cell_length_c 21.7410(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4741.8(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9989 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 30.39 _cell_measurement_theta_min 2.17 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.813 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6931 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0797 before and 0.0492 after correction. The Ratio of minimum to maximum transmission is 0.9290. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 2080 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_unetI/netI 0.0210 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 81145 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 30.453 _diffrn_reflns_theta_min 1.873 _diffrn_ambient_temperature 100.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6139 _reflns_number_total 7191 _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, 2015b)' _computing_structure_solution 'XT (Sheldrick, 2015a)' _refine_diff_density_max 0.416 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.064 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 252 _refine_ls_number_reflns 7191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0208 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+2.2661P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.0506 _refine_special_details ; H atoms were positioned geometrically and allowed to ride on their parent atoms except for H atoms bonded to N and Ru ; those H atoms were located from a difference Fourier map and refined freely. ; _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 Ternary CH refined with riding coordinates: C1(H1A), C11(H11), C14(H14), C4(H4) 2.b Secondary CH2 refined with riding coordinates: C9(H9A,H9B), C7(H7A,H7B), C10(H10A,H10B), C8(H8A,H8B) 2.c Idealised Me refined as rotating group: C19(H19A,H19B,H19C), C15(H15A,H15B,H15C), C5(H5A,H5B,H5C), C16(H16A,H16B, H16C), C12(H12A,H12B,H12C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C13(H13A,H13B, H13C), C2(H2A,H2B,H2C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _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 Ru1 Ru 0.68309(2) 0.42052(2) 0.35773(2) 0.00972(3) Uani 1 1 d . . . . . P2 P 0.70036(2) 0.37447(2) 0.45875(2) 0.01221(6) Uani 1 1 d . . . . . P1 P 0.63792(2) 0.49256(2) 0.26843(2) 0.01307(7) Uani 1 1 d . . . . . O2 O 0.55728(6) 0.33598(6) 0.34488(4) 0.01522(19) Uani 1 1 d . . . . . O3 O 0.44731(7) 0.39730(7) 0.40514(5) 0.0198(2) Uani 1 1 d . . . . . O1 O 0.83336(7) 0.30668(7) 0.30415(5) 0.0240(2) Uani 1 1 d . . . . . N1 N 0.59531(8) 0.52006(7) 0.40143(5) 0.0124(2) Uani 1 1 d . . . . . C17 C 0.77161(9) 0.34800(9) 0.32402(6) 0.0151(2) Uani 1 1 d . . . . . C1 C 0.55602(10) 0.43240(10) 0.21726(6) 0.0197(3) Uani 1 1 d . . . . . H1A H 0.4980 0.4220 0.2424 0.024 Uiso 1 1 calc R . . . . C18 C 0.47588(9) 0.34004(9) 0.36904(6) 0.0134(2) Uani 1 1 d . . . . . C9 C 0.62781(9) 0.53995(9) 0.46471(6) 0.0151(2) Uani 1 1 d . . . . . H9A H 0.5832 0.5809 0.4845 0.018 Uiso 1 1 calc R . . . . H9B H 0.6906 0.5680 0.4631 0.018 Uiso 1 1 calc R . . . . C7 C 0.56037(10) 0.57975(9) 0.29824(6) 0.0172(3) Uani 1 1 d . . . . . H7A H 0.5675 0.6325 0.2726 0.021 Uiso 1 1 calc R . . . . H7B H 0.4937 0.5608 0.2960 0.021 Uiso 1 1 calc R . . . . C10 C 0.63386(9) 0.45708(9) 0.50253(6) 0.0158(3) Uani 1 1 d . . . . . H10A H 0.5696 0.4353 0.5116 0.019 Uiso 1 1 calc R . . . . H10B H 0.6661 0.4690 0.5420 0.019 Uiso 1 1 calc R . . . . C11 C 0.63770(9) 0.27282(9) 0.47943(6) 0.0180(3) Uani 1 1 d . . . . . H11 H 0.5690 0.2865 0.4756 0.022 Uiso 1 1 calc R . . . . C8 C 0.58596(10) 0.60075(9) 0.36459(6) 0.0168(3) Uani 1 1 d . . . . . H8A H 0.6463 0.6332 0.3656 0.020 Uiso 1 1 calc R . . . . H8B H 0.5364 0.6381 0.3828 0.020 Uiso 1 1 calc R . . . . C14 C 0.81561(9) 0.37108(9) 0.49895(6) 0.0170(3) Uani 1 1 d . . . . . H14 H 0.8034 0.3563 0.5430 0.020 Uiso 1 1 calc R . . . . C19 C 0.40939(10) 0.26643(10) 0.35117(7) 0.0209(3) Uani 1 1 d . . . . . H19A H 0.4014 0.2657 0.3064 0.031 Uiso 1 1 calc GR . . . . H19B H 0.3480 0.2754 0.3709 0.031 Uiso 1 1 calc GR . . . . H19C H 0.4361 0.2109 0.3648 0.031 Uiso 1 1 calc GR . . . . C4 C 0.72263(10) 0.55039(10) 0.21818(6) 0.0191(3) Uani 1 1 d . . . . . H4 H 0.6856 0.5836 0.1869 0.023 Uiso 1 1 calc R . . . . C15 C 0.86354(10) 0.46011(10) 0.49712(7) 0.0218(3) Uani 1 1 d . . . . . H15A H 0.8724 0.4780 0.4542 0.033 Uiso 1 1 calc GR . . . . H15B H 0.9251 0.4566 0.5175 0.033 Uiso 1 1 calc GR . . . . H15C H 0.8239 0.5028 0.5184 0.033 Uiso 1 1 calc GR . . . . C5 C 0.78685(11) 0.48710(11) 0.18392(7) 0.0261(3) Uani 1 1 d . . . . . H5A H 0.8204 0.4506 0.2137 0.039 Uiso 1 1 calc GR . . . . H5B H 0.8327 0.5198 0.1593 0.039 Uiso 1 1 calc GR . . . . H5C H 0.7487 0.4503 0.1568 0.039 Uiso 1 1 calc GR . . . . C16 C 0.88046(10) 0.30134(11) 0.47239(8) 0.0256(3) Uani 1 1 d . . . . . H16A H 0.8519 0.2440 0.4785 0.038 Uiso 1 1 calc GR . . . . H16B H 0.9416 0.3035 0.4933 0.038 Uiso 1 1 calc GR . . . . H16C H 0.8895 0.3118 0.4283 0.038 Uiso 1 1 calc GR . . . . C12 C 0.65608(11) 0.19913(10) 0.43365(8) 0.0258(3) Uani 1 1 d . . . . . H12A H 0.6414 0.2191 0.3919 0.039 Uiso 1 1 calc GR . . . . H12B H 0.6160 0.1493 0.4439 0.039 Uiso 1 1 calc GR . . . . H12C H 0.7226 0.1819 0.4358 0.039 Uiso 1 1 calc GR . . . . C3 C 0.59226(12) 0.34208(11) 0.19962(7) 0.0272(3) Uani 1 1 d . . . . . H3A H 0.6466 0.3479 0.1721 0.041 Uiso 1 1 calc GR . . . . H3B H 0.5420 0.3098 0.1787 0.041 Uiso 1 1 calc GR . . . . H3C H 0.6113 0.3107 0.2368 0.041 Uiso 1 1 calc GR . . . . C6 C 0.78133(11) 0.61542(10) 0.25489(8) 0.0269(3) Uani 1 1 d . . . . . H6A H 0.7393 0.6574 0.2749 0.040 Uiso 1 1 calc GR . . . . H6B H 0.8244 0.6461 0.2271 0.040 Uiso 1 1 calc GR . . . . H6C H 0.8179 0.5845 0.2863 0.040 Uiso 1 1 calc GR . . . . C13 C 0.65181(11) 0.24339(12) 0.54609(7) 0.0298(4) Uani 1 1 d . . . . . H13A H 0.7167 0.2227 0.5516 0.045 Uiso 1 1 calc GR . . . . H13B H 0.6076 0.1962 0.5555 0.045 Uiso 1 1 calc GR . . . . H13C H 0.6401 0.2924 0.5739 0.045 Uiso 1 1 calc GR . . . . C2 C 0.52275(12) 0.48421(13) 0.16111(8) 0.0332(4) Uani 1 1 d . . . . . H2A H 0.5017 0.5419 0.1743 0.050 Uiso 1 1 calc GR . . . . H2B H 0.4703 0.4536 0.1413 0.050 Uiso 1 1 calc GR . . . . H2C H 0.5750 0.4903 0.1319 0.050 Uiso 1 1 calc GR . . . . H1 H 0.5398(12) 0.4943(11) 0.4029(7) 0.017(4) Uiso 1 1 d . . . . . H H 0.7648(13) 0.4849(12) 0.3662(8) 0.028(5) Uiso 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 Ru1 0.00941(5) 0.01105(5) 0.00872(5) -0.00022(4) 0.00121(3) 0.00099(4) P2 0.01040(14) 0.01565(16) 0.01057(14) 0.00192(12) 0.00074(11) 0.00017(12) P1 0.01235(15) 0.01649(16) 0.01036(14) 0.00154(12) 0.00073(12) 0.00144(12) O2 0.0138(4) 0.0159(5) 0.0160(4) -0.0030(4) 0.0022(3) -0.0017(4) O3 0.0158(5) 0.0237(5) 0.0198(5) -0.0071(4) 0.0036(4) -0.0012(4) O1 0.0213(5) 0.0247(6) 0.0259(5) -0.0039(4) 0.0063(4) 0.0081(4) N1 0.0118(5) 0.0132(5) 0.0123(5) -0.0011(4) 0.0007(4) 0.0000(4) C17 0.0158(6) 0.0158(6) 0.0138(6) -0.0002(5) 0.0002(5) -0.0011(5) C1 0.0185(6) 0.0283(8) 0.0123(6) 0.0000(5) -0.0034(5) -0.0019(6) C18 0.0143(6) 0.0160(6) 0.0097(5) 0.0016(4) -0.0017(4) -0.0010(5) C9 0.0139(6) 0.0174(6) 0.0142(6) -0.0052(5) 0.0008(5) 0.0006(5) C7 0.0159(6) 0.0181(6) 0.0175(6) 0.0033(5) 0.0009(5) 0.0050(5) C10 0.0139(6) 0.0225(7) 0.0109(6) -0.0008(5) 0.0021(5) 0.0010(5) C11 0.0142(6) 0.0206(7) 0.0192(6) 0.0075(5) -0.0004(5) -0.0032(5) C8 0.0189(6) 0.0128(6) 0.0187(6) 0.0001(5) 0.0018(5) 0.0027(5) C14 0.0127(6) 0.0247(7) 0.0137(6) 0.0039(5) -0.0017(5) -0.0002(5) C19 0.0190(6) 0.0218(7) 0.0218(7) -0.0026(6) 0.0008(5) -0.0057(6) C4 0.0174(6) 0.0236(7) 0.0163(6) 0.0070(5) 0.0034(5) 0.0014(6) C15 0.0165(6) 0.0293(8) 0.0195(7) -0.0001(6) -0.0033(5) -0.0057(6) C5 0.0233(7) 0.0345(9) 0.0204(7) 0.0004(6) 0.0092(6) -0.0003(6) C16 0.0143(6) 0.0305(8) 0.0320(8) 0.0010(7) -0.0015(6) 0.0057(6) C12 0.0250(7) 0.0161(7) 0.0365(9) 0.0040(6) -0.0016(6) 0.0017(6) C3 0.0297(8) 0.0322(9) 0.0198(7) -0.0104(6) -0.0001(6) -0.0035(7) C6 0.0259(8) 0.0229(8) 0.0321(8) 0.0019(7) 0.0087(6) -0.0044(6) C13 0.0249(7) 0.0401(10) 0.0244(8) 0.0194(7) -0.0039(6) -0.0096(7) C2 0.0309(9) 0.0485(11) 0.0203(7) 0.0085(7) -0.0108(6) -0.0050(8) _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 Ru1 P2 2.3208(3) . ? Ru1 P1 2.3256(3) . ? Ru1 O2 2.2246(9) . ? Ru1 N1 2.1902(11) . ? Ru1 C17 1.8321(13) . ? Ru1 H 1.535(18) . ? P2 C10 1.8468(14) . ? P2 C11 1.8543(14) . ? P2 C14 1.8529(13) . ? P1 C1 1.8552(14) . ? P1 C7 1.8516(14) . ? P1 C4 1.8511(14) . ? O2 C18 1.2689(16) . ? O3 C18 1.2477(16) . ? O1 C17 1.1648(16) . ? N1 C9 1.4829(16) . ? N1 C8 1.4837(17) . ? N1 H1 0.881(17) . ? C1 H1A 1.0000 . ? C1 C3 1.531(2) . ? C1 C2 1.532(2) . ? C18 C19 1.5238(19) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.5200(19) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.5221(19) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11 1.0000 . ? C11 C12 1.531(2) . ? C11 C13 1.531(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C14 H14 1.0000 . ? C14 C15 1.530(2) . ? C14 C16 1.526(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C4 H4 1.0000 . ? C4 C5 1.527(2) . ? C4 C6 1.527(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? 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 P2 Ru1 P1 164.725(13) . . ? P2 Ru1 H 90.2(6) . . ? P1 Ru1 H 90.0(6) . . ? O2 Ru1 P2 91.42(3) . . ? O2 Ru1 P1 87.34(3) . . ? O2 Ru1 H 175.6(7) . . ? N1 Ru1 P2 82.13(3) . . ? N1 Ru1 P1 82.66(3) . . ? N1 Ru1 O2 90.49(4) . . ? N1 Ru1 H 85.7(7) . . ? C17 Ru1 P2 96.91(4) . . ? C17 Ru1 P1 98.34(4) . . ? C17 Ru1 O2 98.17(5) . . ? C17 Ru1 N1 171.32(5) . . ? C17 Ru1 H 85.7(7) . . ? C10 P2 Ru1 102.93(4) . . ? C10 P2 C11 102.22(6) . . ? C10 P2 C14 103.06(6) . . ? C11 P2 Ru1 115.89(5) . . ? C14 P2 Ru1 123.23(4) . . ? C14 P2 C11 106.49(6) . . ? C1 P1 Ru1 115.77(5) . . ? C7 P1 Ru1 102.51(4) . . ? C7 P1 C1 101.56(7) . . ? C4 P1 Ru1 122.92(5) . . ? C4 P1 C1 106.96(7) . . ? C4 P1 C7 104.06(6) . . ? C18 O2 Ru1 130.37(8) . . ? Ru1 N1 H1 102.0(11) . . ? C9 N1 Ru1 111.75(8) . . ? C9 N1 C8 110.84(10) . . ? C9 N1 H1 109.6(11) . . ? C8 N1 Ru1 113.71(8) . . ? C8 N1 H1 108.5(11) . . ? O1 C17 Ru1 174.48(12) . . ? P1 C1 H1A 105.5 . . ? C3 C1 P1 113.18(10) . . ? C3 C1 H1A 105.5 . . ? C3 C1 C2 112.09(13) . . ? C2 C1 P1 114.23(11) . . ? C2 C1 H1A 105.5 . . ? O2 C18 C19 114.83(12) . . ? O3 C18 O2 126.16(12) . . ? O3 C18 C19 119.00(12) . . ? N1 C9 H9A 109.6 . . ? N1 C9 H9B 109.6 . . ? N1 C9 C10 110.26(11) . . ? H9A C9 H9B 108.1 . . ? C10 C9 H9A 109.6 . . ? C10 C9 H9B 109.6 . . ? P1 C7 H7A 109.6 . . ? P1 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C8 C7 P1 110.14(9) . . ? C8 C7 H7A 109.6 . . ? C8 C7 H7B 109.6 . . ? P2 C10 H10A 109.9 . . ? P2 C10 H10B 109.9 . . ? C9 C10 P2 109.13(9) . . ? C9 C10 H10A 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? P2 C11 H11 105.6 . . ? C12 C11 P2 112.70(10) . . ? C12 C11 H11 105.6 . . ? C12 C11 C13 111.95(13) . . ? C13 C11 P2 114.61(10) . . ? C13 C11 H11 105.6 . . ? N1 C8 C7 110.79(11) . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? P2 C14 H14 107.8 . . ? C15 C14 P2 110.72(9) . . ? C15 C14 H14 107.8 . . ? C16 C14 P2 111.83(10) . . ? C16 C14 H14 107.8 . . ? C16 C14 C15 110.65(11) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? P1 C4 H4 107.9 . . ? C5 C4 P1 111.57(10) . . ? C5 C4 H4 107.9 . . ? C6 C4 P1 111.10(10) . . ? C6 C4 H4 107.9 . . ? C6 C4 C5 110.40(12) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? 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 Ru1 P2 C10 C9 -23.03(10) . . . . ? Ru1 P2 C11 C12 49.46(11) . . . . ? Ru1 P2 C11 C13 179.05(10) . . . . ? Ru1 P2 C14 C15 55.32(11) . . . . ? Ru1 P2 C14 C16 -68.58(11) . . . . ? Ru1 P1 C1 C3 -53.94(11) . . . . ? Ru1 P1 C1 C2 176.16(10) . . . . ? Ru1 P1 C7 C8 25.10(10) . . . . ? Ru1 P1 C4 C5 70.49(11) . . . . ? Ru1 P1 C4 C6 -53.17(12) . . . . ? Ru1 O2 C18 O3 3.0(2) . . . . ? Ru1 O2 C18 C19 -176.68(9) . . . . ? Ru1 N1 C9 C10 -53.96(12) . . . . ? Ru1 N1 C8 C7 48.51(13) . . . . ? P1 C7 C8 N1 -47.51(13) . . . . ? N1 C9 C10 P2 49.52(12) . . . . ? C1 P1 C7 C8 145.10(10) . . . . ? C1 P1 C4 C5 -67.16(12) . . . . ? C1 P1 C4 C6 169.18(10) . . . . ? C9 N1 C8 C7 175.39(11) . . . . ? C7 P1 C1 C3 -164.08(11) . . . . ? C7 P1 C1 C2 66.03(12) . . . . ? C7 P1 C4 C5 -174.16(10) . . . . ? C7 P1 C4 C6 62.19(11) . . . . ? C10 P2 C11 C12 160.53(10) . . . . ? C10 P2 C11 C13 -69.88(12) . . . . ? C10 P2 C14 C15 -59.93(11) . . . . ? C10 P2 C14 C16 176.17(10) . . . . ? C11 P2 C10 C9 -143.56(9) . . . . ? C11 P2 C14 C15 -167.10(10) . . . . ? C11 P2 C14 C16 69.00(11) . . . . ? C8 N1 C9 C10 178.08(10) . . . . ? C14 P2 C10 C9 106.05(10) . . . . ? C14 P2 C11 C12 -91.70(11) . . . . ? C14 P2 C11 C13 37.89(13) . . . . ? C4 P1 C1 C3 87.16(11) . . . . ? C4 P1 C1 C2 -42.74(13) . . . . ? C4 P1 C7 C8 -103.91(10) . . . . ? _shelx_res_file ; mo_dhng157.res created by SHELXL-2014/7 TITL mo_dhng157_a.res in Pbca REM Old TITL mo_DHNG157 in Pbca #61 REM SHELXT solution in Pbca REM R1 0.228, Rweak 0.003, Alpha 0.031, Orientation as input REM Formula found by SHELXT: C19 N O5 Ru CELL 0.71073 14.17 15.3918 21.741 90 90 90 ZERR 8 0.0005 0.0006 0.0008 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 P Ru UNIT 152 328 8 24 16 8 L.S. 10 PLAN 20 TEMP -173.15 BOND $H LIST 4 MORE -1 CONF fmap 2 acta 52 REM REM REM WGHT 0.020400 2.266100 FVAR 0.22751 RU1 6 0.683088 0.420517 0.357727 11.00000 0.00941 0.01105 = 0.00872 -0.00022 0.00121 0.00099 P2 5 0.700362 0.374471 0.458751 11.00000 0.01040 0.01565 = 0.01057 0.00192 0.00074 0.00017 P1 5 0.637919 0.492561 0.268430 11.00000 0.01235 0.01649 = 0.01036 0.00154 0.00073 0.00144 O2 4 0.557280 0.335981 0.344882 11.00000 0.01378 0.01587 = 0.01601 -0.00296 0.00216 -0.00165 O3 4 0.447309 0.397303 0.405137 11.00000 0.01582 0.02375 = 0.01983 -0.00712 0.00362 -0.00123 O1 4 0.833364 0.306678 0.304147 11.00000 0.02134 0.02468 = 0.02590 -0.00394 0.00632 0.00807 N1 3 0.595311 0.520061 0.401426 11.00000 0.01184 0.01319 = 0.01232 -0.00105 0.00067 -0.00002 C17 1 0.771612 0.347996 0.324016 11.00000 0.01581 0.01584 = 0.01376 -0.00015 0.00020 -0.00114 C1 1 0.556016 0.432404 0.217265 11.00000 0.01849 0.02829 = 0.01227 -0.00001 -0.00343 -0.00193 AFIX 13 H1A 2 0.498027 0.421951 0.242413 11.00000 -1.20000 AFIX 0 C18 1 0.475881 0.340040 0.369035 11.00000 0.01428 0.01605 = 0.00973 0.00163 -0.00167 -0.00099 C9 1 0.627811 0.539946 0.464714 11.00000 0.01390 0.01735 = 0.01418 -0.00518 0.00078 0.00062 AFIX 23 H9A 2 0.583240 0.580882 0.484456 11.00000 -1.20000 H9B 2 0.690609 0.568039 0.463057 11.00000 -1.20000 AFIX 0 C7 1 0.560365 0.579746 0.298245 11.00000 0.01588 0.01813 = 0.01753 0.00329 0.00093 0.00504 AFIX 23 H7A 2 0.567495 0.632457 0.272567 11.00000 -1.20000 H7B 2 0.493685 0.560798 0.296037 11.00000 -1.20000 AFIX 0 C10 1 0.633859 0.457079 0.502534 11.00000 0.01387 0.02251 = 0.01089 -0.00081 0.00208 0.00100 AFIX 23 H10A 2 0.569598 0.435349 0.511626 11.00000 -1.20000 H10B 2 0.666083 0.469016 0.542044 11.00000 -1.20000 AFIX 0 C11 1 0.637699 0.272818 0.479428 11.00000 0.01418 0.02061 = 0.01924 0.00751 -0.00036 -0.00322 AFIX 13 H11 2 0.568967 0.286534 0.475610 11.00000 -1.20000 AFIX 0 C8 1 0.585962 0.600754 0.364591 11.00000 0.01886 0.01284 = 0.01869 0.00008 0.00179 0.00266 AFIX 23 H8A 2 0.646261 0.633211 0.365586 11.00000 -1.20000 H8B 2 0.536430 0.638112 0.382808 11.00000 -1.20000 AFIX 0 C14 1 0.815608 0.371084 0.498951 11.00000 0.01273 0.02471 = 0.01368 0.00392 -0.00168 -0.00024 AFIX 13 H14 2 0.803412 0.356261 0.543023 11.00000 -1.20000 AFIX 0 C19 1 0.409392 0.266432 0.351175 11.00000 0.01900 0.02181 = 0.02184 -0.00260 0.00081 -0.00574 AFIX 137 H19A 2 0.401408 0.265674 0.306403 11.00000 -1.50000 H19B 2 0.347954 0.275382 0.370880 11.00000 -1.50000 H19C 2 0.436052 0.210902 0.364754 11.00000 -1.50000 AFIX 0 C4 1 0.722627 0.550391 0.218181 11.00000 0.01737 0.02357 = 0.01630 0.00695 0.00338 0.00143 AFIX 13 H4 2 0.685571 0.583588 0.186876 11.00000 -1.20000 AFIX 0 C15 1 0.863541 0.460110 0.497116 11.00000 0.01654 0.02932 = 0.01951 -0.00010 -0.00328 -0.00570 AFIX 137 H15A 2 0.872357 0.478020 0.454244 11.00000 -1.50000 H15B 2 0.925069 0.456569 0.517547 11.00000 -1.50000 H15C 2 0.823901 0.502769 0.518383 11.00000 -1.50000 AFIX 0 C5 1 0.786852 0.487101 0.183920 11.00000 0.02332 0.03452 = 0.02036 0.00041 0.00920 -0.00030 AFIX 137 H5A 2 0.820389 0.450552 0.213661 11.00000 -1.50000 H5B 2 0.832671 0.519791 0.159334 11.00000 -1.50000 H5C 2 0.748712 0.450343 0.156777 11.00000 -1.50000 AFIX 0 C16 1 0.880458 0.301343 0.472390 11.00000 0.01429 0.03047 = 0.03201 0.00102 -0.00147 0.00566 AFIX 137 H16A 2 0.851858 0.244010 0.478461 11.00000 -1.50000 H16B 2 0.941650 0.303468 0.493341 11.00000 -1.50000 H16C 2 0.889498 0.311779 0.428315 11.00000 -1.50000 AFIX 0 C12 1 0.656082 0.199128 0.433652 11.00000 0.02496 0.01606 = 0.03648 0.00398 -0.00159 0.00170 AFIX 137 H12A 2 0.641398 0.219080 0.391930 11.00000 -1.50000 H12B 2 0.616046 0.149280 0.443924 11.00000 -1.50000 H12C 2 0.722569 0.181863 0.435807 11.00000 -1.50000 AFIX 0 C3 1 0.592257 0.342075 0.199620 11.00000 0.02967 0.03223 = 0.01983 -0.01037 -0.00010 -0.00348 AFIX 137 H3A 2 0.646621 0.347930 0.172065 11.00000 -1.50000 H3B 2 0.542046 0.309792 0.178679 11.00000 -1.50000 H3C 2 0.611305 0.310683 0.236819 11.00000 -1.50000 AFIX 0 C6 1 0.781326 0.615420 0.254892 11.00000 0.02587 0.02288 = 0.03208 0.00186 0.00869 -0.00437 AFIX 137 H6A 2 0.739337 0.657411 0.274871 11.00000 -1.50000 H6B 2 0.824407 0.646114 0.227121 11.00000 -1.50000 H6C 2 0.817914 0.584479 0.286251 11.00000 -1.50000 AFIX 0 C13 1 0.651806 0.243391 0.546086 11.00000 0.02494 0.04007 = 0.02443 0.01942 -0.00386 -0.00964 AFIX 137 H13A 2 0.716681 0.222727 0.551560 11.00000 -1.50000 H13B 2 0.607638 0.196236 0.555501 11.00000 -1.50000 H13C 2 0.640127 0.292381 0.573854 11.00000 -1.50000 AFIX 0 C2 1 0.522751 0.484210 0.161115 11.00000 0.03086 0.04852 = 0.02033 0.00852 -0.01079 -0.00497 AFIX 137 H2A 2 0.501659 0.541936 0.174256 11.00000 -1.50000 H2B 2 0.470315 0.453572 0.141281 11.00000 -1.50000 H2C 2 0.575006 0.490254 0.131898 11.00000 -1.50000 AFIX 0 H1 2 0.539850 0.494278 0.402948 11.00000 0.01749 H 2 0.764776 0.484934 0.366217 11.00000 0.02787 HKLF 4 REM mo_dhng157_a.res in Pbca REM R1 = 0.0208 for 6139 Fo > 4sig(Fo) and 0.0291 for all 7191 data REM 252 parameters refined using 0 restraints END WGHT 0.0204 2.2660 REM Highest difference peak 0.416, deepest hole -0.354, 1-sigma level 0.064 Q1 1 0.8309 0.4172 0.4997 11.00000 0.05 0.42 Q2 1 0.4374 0.3041 0.3583 11.00000 0.05 0.42 Q3 1 0.6834 0.5182 0.2437 11.00000 0.05 0.39 Q4 1 0.6651 0.4223 0.4835 11.00000 0.05 0.39 Q5 1 0.6509 0.2330 0.4582 11.00000 0.05 0.35 Q6 1 0.6380 0.4979 0.4821 11.00000 0.05 0.34 Q7 1 0.7606 0.3759 0.4739 11.00000 0.05 0.34 Q8 1 0.7374 0.4035 0.3229 11.00000 0.05 0.34 Q9 1 0.5736 0.5881 0.3303 11.00000 0.05 0.33 Q10 1 0.6453 0.2623 0.5098 11.00000 0.05 0.33 Q11 1 0.7543 0.5773 0.2354 11.00000 0.05 0.32 Q12 1 0.5439 0.4621 0.1904 11.00000 0.05 0.32 Q13 1 0.5933 0.5419 0.2840 11.00000 0.05 0.31 Q14 1 0.5882 0.5586 0.3806 11.00000 0.05 0.31 Q15 1 0.6015 0.4615 0.2366 11.00000 0.05 0.30 Q16 1 0.6756 0.3132 0.4800 11.00000 0.05 0.30 Q17 1 0.6977 0.4002 0.4195 11.00000 0.05 0.30 Q18 1 0.6098 0.5311 0.4320 11.00000 0.05 0.29 Q19 1 0.6397 0.4951 0.3895 11.00000 0.05 0.28 Q20 1 0.6545 0.4601 0.2958 11.00000 0.05 0.27 ; _shelx_res_checksum 20687 _shelx_hkl_file ; 1 0 0 0.20 0.30 1 0 0 0.50 0.50 -1 0 0 0.60 0.40 -1 0 0 0.30 0.40 -1 0 0 0.50 0.50 -2 0 0 4038.40 98.09 -2 0 0 4158.78 101.19 -2 0 0 4133.99 98.69 2 0 0 4102.99 96.89 -2 0 0 4021.60 99.39 2 0 0 4016.00 99.39 2 0 0 3969.30 97.39 2 0 0 3866.01 100.79 2 0 0 4104.19 97.79 2 0 0 3979.00 99.09 -2 0 0 4007.30 97.49 -3 0 0 -0.30 1.10 3 0 0 0.50 0.70 3 0 0 2.50 1.50 3 0 0 -0.80 1.30 3 0 0 -0.50 1.50 3 0 0 0.20 0.60 -3 0 0 8.00 1.80 -3 0 0 -0.50 1.40 -3 0 0 2.30 1.30 -3 0 0 0.40 1.20 3 0 0 0.70 1.30 3 0 0 -1.40 1.40 -4 0 0 4052.19 99.49 4 0 0 4104.09 100.19 4 0 0 4036.80 99.79 -4 0 0 4161.98 98.89 4 0 0 4049.69 99.69 -4 0 0 3960.10 99.89 -4 0 0 4101.69 100.09 4 0 0 4042.70 100.79 4 0 0 4198.58 100.19 -4 0 0 4093.09 99.79 -5 0 0 4.80 2.10 5 0 0 4.40 2.30 -5 0 0 3.60 1.80 5 0 0 1.80 1.80 5 0 0 7.10 2.90 -5 0 0 4.20 1.90 5 0 0 4.00 2.10 5 0 0 1.70 2.10 -5 0 0 3.50 1.80 6 0 0 2508.35 66.09 6 0 0 2591.94 67.79 -6 0 0 2596.64 66.69 -6 0 0 2630.74 65.19 6 0 0 2663.43 66.39 6 0 0 2585.64 66.59 -6 0 0 2696.83 67.99 -6 0 0 2593.64 65.69 -7 0 0 2.90 2.20 7 0 0 4.30 2.50 7 0 0 4.50 2.70 7 0 0 4.00 2.40 7 0 0 6.90 3.20 -7 0 0 5.20 2.50 -7 0 0 3.20 2.60 8 0 0 3272.47 87.49 -8 0 0 3341.77 85.89 8 0 0 3327.47 85.89 8 0 0 3404.76 85.39 8 0 0 3448.16 86.29 -8 0 0 3308.27 84.19 -9 0 0 1.10 2.60 9 0 0 2.70 3.20 9 0 0 0.70 2.40 -9 0 0 2.40 2.40 9 0 0 -0.20 2.40 9 0 0 3.90 3.10 10 0 0 111.99 8.40 10 0 0 106.99 7.70 10 0 0 101.99 7.90 -10 0 0 103.69 7.90 10 0 0 104.29 9.70 -10 0 0 115.89 7.50 -11 0 0 4.30 3.30 11 0 0 5.20 3.40 11 0 0 18.10 5.10 11 0 0 7.00 3.30 11 0 0 11.80 4.20 -11 0 0 6.70 3.70 12 0 0 89.19 10.10 -12 0 0 98.89 8.70 -12 0 0 109.99 10.20 12 0 0 107.09 10.00 12 0 0 107.59 8.40 13 0 0 6.00 4.60 13 0 0 3.40 3.70 13 0 0 0.70 3.20 -13 0 0 3.80 4.00 -13 0 0 7.10 4.00 14 0 0 89.29 11.20 14 0 0 89.49 9.30 14 0 0 91.99 10.20 -14 0 0 104.19 10.20 15 0 0 14.60 6.40 15 0 0 3.60 4.50 -15 0 0 1.40 4.10 -16 0 0 727.93 28.00 16 0 0 747.43 29.20 16 0 0 787.62 33.50 17 0 0 2.70 5.90 -17 0 0 9.60 5.20 17 0 0 14.50 6.10 18 0 0 315.47 21.80 18 0 0 292.67 17.70 19 0 0 8.60 6.40 19 0 0 5.30 5.30 20 0 0 81.09 14.20 0 -1 0 0.80 0.40 0 -1 0 -0.20 0.40 0 1 0 0.00 0.50 -1 -1 0 -0.60 0.80 -1 1 0 0.70 0.50 1 -1 0 -0.20 0.50 1 -1 0 0.40 0.60 -1 -1 0 0.10 0.70 1 1 0 -0.20 0.60 1 -1 0 0.30 0.40 -1 1 0 -0.20 0.60 -1 -1 0 2.60 0.90 -1 1 0 0.00 0.50 1 1 0 0.30 0.80 1 -1 0 1.00 0.70 -2 1 0 827.72 20.70 2 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6.50 19 -4 0 -12.40 4.70 19 4 0 -6.30 5.20 0 5 0 7.40 2.20 0 -5 0 9.10 2.60 0 5 0 8.30 2.20 0 5 0 6.40 2.70 0 5 0 11.60 2.60 0 -5 0 2.60 1.80 1 5 0 -1.10 1.40 -1 -5 0 -3.50 1.90 1 -5 0 -0.40 2.00 -1 5 0 -1.80 1.40 -1 5 0 -0.70 1.70 1 -5 0 0.10 1.50 1 5 0 -0.70 2.10 1 5 0 3.40 2.20 -1 -5 0 1.20 1.50 -1 -5 0 -0.60 1.70 1 5 0 1.70 2.90 1 -5 0 -1.80 1.70 1 -5 0 1.70 2.10 -1 5 0 -0.30 2.10 -1 5 0 0.70 1.70 2 5 0 106.09 6.60 -2 5 0 115.89 5.70 2 -5 0 110.89 6.70 2 5 0 103.09 7.20 2 -5 0 107.99 5.50 -2 -5 0 112.59 7.30 2 -5 0 111.59 4.70 -2 5 0 110.59 4.90 2 5 0 120.29 6.80 2 -5 0 108.89 5.60 -2 5 0 103.19 7.50 -2 -5 0 105.99 4.50 -2 5 0 113.89 6.30 2 -5 0 112.59 6.10 -2 -5 0 106.79 7.10 3 -5 0 -0.80 2.00 3 -5 0 1.20 2.50 -3 -5 0 0.30 2.80 3 5 0 -0.60 2.90 3 5 0 -0.10 3.40 3 -5 0 -1.00 1.80 3 -5 0 -2.10 1.60 -3 5 0 2.00 1.90 3 5 0 0.10 2.80 -3 5 0 -2.70 1.90 3 -5 0 -0.10 1.10 -3 -5 0 2.00 2.70 -4 -5 0 1688.83 46.80 4 -5 0 1764.32 46.70 4 5 0 1655.53 47.60 4 5 0 1695.83 45.00 4 -5 0 1642.64 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4 -6 0 -0.40 0.90 4 6 0 -0.30 3.60 -4 6 0 0.90 2.30 4 6 0 7.40 3.70 4 -6 0 -0.10 2.80 -4 6 0 3.20 2.70 4 -6 0 0.10 2.30 4 -6 0 -0.70 1.00 4 -6 0 -0.90 1.90 -4 -6 0 1.80 3.00 5 -6 0 6.20 2.80 -5 -6 0 -4.20 2.80 5 -6 0 -2.10 2.50 -5 6 0 2.60 2.10 5 -6 0 0.70 1.10 5 -6 0 -1.20 1.80 -5 6 0 -0.30 0.70 5 6 0 -0.50 0.90 5 6 0 1.70 3.30 -6 6 0 850.81 24.30 -6 -6 0 881.21 28.40 6 -6 0 812.82 27.40 6 -6 0 709.33 22.40 6 6 0 883.01 29.40 6 -6 0 856.71 26.20 6 6 0 837.42 28.00 6 -6 0 832.52 23.40 7 -6 0 -1.30 1.60 7 6 0 -1.50 3.20 -7 6 0 0.20 2.10 7 -6 0 1.10 2.90 7 -6 0 0.00 2.80 7 6 0 -6.90 2.50 -7 -6 0 -1.60 3.60 7 -6 0 0.60 1.50 8 -6 0 3468.25 85.99 -8 6 0 3469.45 87.19 8 6 0 3367.36 92.69 8 -6 0 3485.85 90.99 -8 -6 0 3399.16 92.49 8 -6 0 3441.56 92.09 8 -6 0 3495.85 85.49 9 -6 0 -0.40 1.90 9 -6 0 -2.00 3.60 -9 6 0 2.50 1.60 9 -6 0 -1.70 1.70 9 6 0 -0.80 3.40 -9 -6 0 2.60 3.90 -9 6 0 -0.10 2.20 9 -6 0 -1.80 3.40 9 6 0 -5.10 3.70 10 6 0 409.26 18.80 -10 -6 0 430.46 19.60 -10 6 0 384.46 12.80 10 6 0 361.86 18.90 10 -6 0 401.36 18.70 10 -6 0 393.16 13.50 -10 6 0 380.66 14.70 10 -6 0 386.96 18.30 10 -6 0 431.16 13.40 10 6 0 409.96 20.50 11 -6 0 1.60 2.10 11 6 0 -1.00 4.20 11 6 0 -1.90 4.30 -11 6 0 2.90 3.00 -11 6 0 -1.30 2.20 11 -6 0 -0.50 4.00 -11 -6 0 5.50 5.00 11 6 0 4.00 3.20 11 -6 0 0.40 1.90 11 -6 0 0.50 3.90 12 -6 0 278.57 16.60 12 -6 0 287.67 16.70 12 6 0 271.97 16.60 12 -6 0 276.77 10.40 -12 -6 0 280.77 16.80 12 6 0 291.37 18.30 12 6 0 293.27 12.80 -12 6 0 291.07 11.80 13 -6 0 0.60 2.00 13 6 0 -0.10 2.50 13 -6 0 0.00 4.00 13 6 0 6.70 5.10 13 6 0 3.50 5.20 13 -6 0 -0.10 4.70 -13 -6 0 1.20 4.90 -14 -6 0 817.12 33.20 14 -6 0 818.32 33.10 14 -6 0 813.32 23.00 14 6 0 808.52 33.30 14 6 0 788.52 34.40 14 -6 0 875.51 33.70 -15 -6 0 -8.10 4.70 15 6 0 2.10 5.90 15 6 0 -8.80 4.30 15 -6 0 -2.10 4.90 15 -6 0 0.40 4.90 16 6 0 771.12 35.00 16 6 0 720.63 33.00 16 -6 0 701.23 32.60 17 6 0 5.30 7.20 17 6 0 0.70 5.60 17 -6 0 -6.30 4.90 18 -6 0 -8.50 5.70 18 6 0 4.30 6.70 18 6 0 -15.00 5.30 19 6 0 0.20 6.70 19 -6 0 5.00 7.70 19 6 0 6.60 7.50 0 7 0 9.80 3.10 0 -7 0 7.30 3.30 0 7 0 15.40 4.00 -1 -7 0 3.10 2.10 1 -7 0 2.80 2.50 1 7 0 3.30 3.40 1 7 0 -2.20 2.60 -1 7 0 -0.50 1.40 -1 -7 0 0.30 1.50 -1 -7 0 -4.20 2.20 1 -7 0 0.30 2.60 1 -7 0 -2.60 1.80 1 -7 0 -2.50 2.30 -1 7 0 0.00 2.30 -1 7 0 -3.20 2.50 2 -7 0 257.57 11.00 -2 7 0 246.38 11.20 -2 -7 0 272.47 12.70 2 -7 0 277.57 9.40 -2 -7 0 238.08 11.60 2 7 0 258.57 12.00 -2 -7 0 248.48 9.20 2 7 0 275.17 13.50 2 -7 0 257.27 10.50 -2 7 0 251.67 9.50 2 -7 0 242.88 11.30 -2 7 0 259.57 11.50 -3 -7 0 2.30 2.90 3 7 0 0.60 3.10 3 -7 0 -0.80 1.40 3 7 0 4.10 3.30 3 -7 0 2.60 2.10 3 -7 0 -0.90 2.10 -3 7 0 2.30 3.00 3 -7 0 -3.10 2.30 3 -7 0 2.70 2.30 -3 7 0 2.10 2.70 4 -7 0 3420.96 85.89 4 7 0 3503.75 91.69 4 -7 0 3470.45 83.59 4 7 0 3495.95 90.19 4 -7 0 3539.05 86.89 -4 -7 0 3340.57 90.09 -4 7 0 3382.86 87.39 4 -7 0 3467.45 87.29 4 -7 0 3457.05 85.99 4 -7 0 3335.77 89.39 5 7 0 -2.00 2.80 -5 7 0 -0.50 2.10 5 -7 0 -4.90 2.70 -5 -7 0 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0 83.99 9.10 5 -11 0 -2.40 1.50 -5 -11 0 0.30 4.20 5 11 0 2.50 4.80 -5 11 0 -1.90 3.10 5 -11 0 4.20 2.90 5 11 0 -2.50 3.80 5 -11 0 -1.90 2.40 5 -11 0 -3.60 2.30 5 -11 0 1.50 4.20 6 -11 0 64.19 8.70 6 -11 0 64.59 3.30 -6 -11 0 65.79 9.90 6 -11 0 72.79 7.70 6 -11 0 72.09 6.40 6 -11 0 65.39 6.60 6 11 0 73.19 10.00 6 11 0 46.80 9.20 -6 11 0 62.59 7.50 7 11 0 -7.30 4.40 7 -11 0 1.60 2.40 7 -11 0 -0.20 2.40 7 -11 0 -1.40 3.40 7 -11 0 -2.60 3.40 -7 -11 0 0.20 4.40 7 11 0 -0.20 4.80 -7 11 0 -2.30 2.90 8 11 0 16.40 7.00 -8 -11 0 20.50 6.50 8 11 0 21.30 6.50 8 -11 0 18.20 6.50 8 -11 0 22.30 3.50 8 -11 0 20.20 5.60 9 -11 0 -1.60 3.80 9 -11 0 -0.50 1.80 9 11 0 -0.90 5.20 -9 -11 0 -1.10 5.30 9 -11 0 -1.10 3.70 -10 -11 0 1038.50 39.70 10 -11 0 1006.20 38.40 10 -11 0 1006.30 27.00 10 11 0 1064.99 42.10 10 -11 0 1078.19 36.10 11 11 0 3.00 5.10 -11 -11 0 8.50 6.40 11 11 0 6.00 6.80 11 -11 0 8.30 5.30 12 11 0 345.67 23.60 -12 -11 0 371.06 22.60 12 11 0 388.16 19.30 12 11 0 380.06 20.70 12 -11 0 370.46 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356.96 22.30 11 11 -12 435.66 26.30 11 11 -12 357.26 23.00 -11 11 12 370.56 21.40 -11 -11 12 331.67 22.80 11 11 12 382.06 25.10 11 11 12 384.66 18.90 11 11 12 365.16 17.90 11 -11 -12 396.86 20.80 -12 11 12 -0.10 5.70 12 -11 12 3.30 6.30 12 11 -12 -10.30 6.50 -12 -11 -12 7.50 6.50 12 11 -12 4.10 7.90 12 11 12 -9.40 5.50 12 11 12 -0.80 4.80 12 -11 -12 -0.70 4.80 -12 -11 12 -4.70 6.20 13 11 -12 117.39 16.00 13 -11 12 140.29 16.00 -13 11 12 134.79 15.20 13 11 -12 144.99 18.90 -13 -11 12 119.59 16.50 13 -11 -12 153.48 14.60 13 11 12 199.48 22.30 13 11 12 138.79 18.40 14 11 -12 16.80 9.00 14 11 -12 22.30 10.30 14 -11 12 31.70 9.60 -14 11 12 26.90 8.80 14 11 12 18.90 8.70 -14 -11 12 24.70 9.20 14 -11 -12 16.70 7.00 15 11 -12 5.20 7.60 -15 11 12 8.60 7.40 15 -11 12 -0.80 7.10 15 11 -12 9.00 9.00 -15 -11 12 2.80 8.90 15 -11 -12 3.00 5.90 15 11 12 -1.80 8.20 0 12 12 26.10 8.10 0 12 -12 11.10 5.40 0 -12 -12 16.50 6.60 0 -12 12 11.20 4.90 0 12 -12 16.20 5.60 0 12 12 19.10 6.40 1 -12 12 1365.06 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389.16 22.50 -6 1 29 399.36 27.60 -6 -1 -29 385.06 25.70 -6 1 29 395.56 22.10 -6 -1 29 393.56 28.20 -6 1 -29 419.76 25.90 6 -1 -29 413.36 25.60 6 1 29 329.27 22.40 6 -1 -29 351.56 26.00 -7 1 29 14.90 14.50 7 1 -29 17.60 9.00 7 -1 29 20.30 7.30 -7 1 29 10.80 7.30 7 1 -29 16.10 8.80 -7 -1 29 13.30 6.80 7 -1 -29 17.50 9.00 7 -1 -29 13.30 9.00 7 1 29 19.00 8.00 0 2 29 318.97 23.80 0 2 -29 273.67 21.60 0 -2 29 320.57 22.40 0 -2 -29 325.97 22.30 -1 -2 -29 249.88 19.60 1 2 -29 235.78 22.10 1 -2 29 215.78 21.00 -1 2 29 215.58 22.10 -1 -2 29 185.08 19.80 -1 2 -29 194.28 19.90 1 -2 -29 245.48 23.10 1 2 29 183.38 20.70 1 -2 -29 227.78 21.10 -2 2 29 252.07 24.50 -2 -2 -29 218.08 20.70 2 2 -29 205.08 20.60 2 -2 29 231.18 19.00 2 -2 -29 206.78 20.90 -2 -2 29 230.98 22.90 -2 2 -29 249.38 22.40 2 2 29 213.98 21.70 2 -2 -29 243.18 19.50 -3 -2 -29 114.79 15.50 3 2 -29 87.89 14.60 3 -2 29 83.19 12.80 -3 2 29 103.49 16.20 3 -2 -29 104.09 14.50 -3 -2 29 77.69 14.20 3 2 29 91.09 14.50 3 -2 -29 88.39 14.60 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29 308.97 23.80 0 4 -29 316.07 22.20 0 -4 -29 318.17 22.50 -1 -4 -29 160.08 18.40 1 -4 29 231.88 21.00 -1 4 29 234.28 24.00 1 4 -29 188.08 20.00 -1 4 -29 209.18 20.70 1 -4 -29 196.58 20.40 1 4 29 216.18 23.00 -1 -4 29 184.98 19.50 1 -4 -29 185.88 19.90 -2 4 29 22.20 9.60 2 4 -29 20.50 9.50 2 -4 29 28.30 8.80 -2 -4 -29 42.50 10.70 2 4 29 18.20 9.20 2 -4 -29 27.60 9.80 2 -4 -29 32.00 10.30 -2 4 -29 27.50 8.90 -2 -4 29 22.50 9.80 3 4 -29 4.90 7.10 3 -4 29 9.80 6.90 -3 4 29 11.70 6.90 -3 4 29 7.70 8.20 -3 -4 -29 8.30 8.10 -3 -4 29 7.30 8.70 3 4 29 4.50 7.40 3 -4 -29 8.40 8.50 3 -4 -29 3.30 7.70 -3 4 -29 2.10 6.40 -4 4 29 -3.90 6.10 -4 -4 -29 16.90 9.00 4 4 -29 0.80 7.60 -4 4 29 4.20 8.10 4 -4 29 -5.70 5.10 -4 4 -29 11.40 8.10 4 4 29 -0.90 7.40 4 -4 -29 15.90 8.30 4 -4 -29 7.00 7.30 -4 -4 29 -2.20 6.90 5 4 -29 74.79 13.60 5 -4 29 99.99 12.10 -5 4 29 78.79 12.10 -5 -4 -29 119.99 16.90 -5 4 29 79.19 16.80 -5 -4 29 106.19 16.50 5 -4 -29 70.99 13.70 -5 4 -29 80.49 13.50 5 -4 -29 59.29 12.20 5 4 29 71.29 14.00 6 4 -29 118.59 16.10 -6 4 29 125.49 17.30 -6 4 29 90.59 16.60 6 4 -29 69.19 13.90 6 -4 -29 116.69 15.70 6 -4 -29 122.89 18.30 6 4 29 106.89 15.90 -6 4 -29 131.99 17.20 0 -5 29 11.70 7.30 0 -5 -29 2.30 6.60 0 5 29 2.80 7.70 0 -5 -29 -11.80 5.60 0 5 -29 2.00 6.80 -1 -5 -29 63.19 13.20 1 -5 29 48.70 10.50 -1 5 29 53.09 13.00 -1 -5 -29 64.99 16.10 1 5 -29 53.69 12.50 1 -5 -29 56.99 11.90 1 5 29 77.99 14.30 1 -5 -29 92.09 14.60 -1 5 -29 75.39 13.80 -1 -5 29 70.19 12.60 -2 5 29 377.46 27.70 2 5 -29 432.06 26.10 2 -5 29 319.87 21.10 -2 -5 -29 360.36 23.90 -2 5 29 322.87 20.30 2 -5 -29 328.87 23.20 -2 -5 29 347.57 23.70 2 -5 -29 407.66 25.30 -2 5 -29 346.27 23.60 2 5 29 324.67 25.30 -3 5 29 182.88 16.50 -3 -5 -29 210.28 21.60 3 -5 29 215.88 16.60 3 5 -29 220.08 21.60 -3 5 29 209.18 24.00 -3 5 -29 196.28 19.90 -3 -5 29 184.98 20.30 3 5 29 246.48 24.00 3 -5 -29 216.38 21.20 3 -5 -29 178.78 19.80 -4 5 29 226.28 19.20 -4 5 29 251.47 24.70 4 5 -29 229.38 21.90 4 -5 29 239.38 16.80 -4 -5 -29 241.68 22.30 4 -5 -29 238.58 21.80 -4 5 -29 235.28 22.20 4 5 29 218.38 22.10 4 -5 -29 242.28 23.50 -4 -5 29 251.27 23.80 5 5 -29 95.09 14.90 -5 5 29 89.89 12.70 -5 5 29 101.59 18.00 -5 -5 29 119.79 23.70 5 5 29 119.49 16.80 5 -5 -29 123.99 17.80 5 -5 -29 111.59 15.60 -5 5 -29 93.59 14.20 0 -6 -29 25.40 10.10 0 6 -29 23.20 8.50 0 -6 -29 36.30 10.30 0 -6 29 30.30 9.50 0 6 29 16.60 9.20 1 6 -29 -2.60 7.20 -1 -6 -29 14.50 8.10 -1 -6 -29 11.50 7.20 -1 6 29 -3.70 7.20 1 -6 29 1.10 6.10 1 6 29 1.50 7.50 1 -6 -29 13.80 8.30 -1 -6 29 17.20 8.40 -1 6 -29 10.50 8.00 1 -6 -29 -5.80 7.20 2 -6 29 36.90 9.70 -2 6 29 42.80 13.80 -2 6 29 56.09 10.20 -2 -6 -29 29.30 10.00 2 6 -29 34.20 10.40 2 6 29 26.10 10.30 2 -6 -29 39.50 11.70 -2 -6 29 25.00 9.60 -2 6 -29 57.69 12.20 2 -6 -29 58.79 12.30 -3 6 29 -9.10 5.70 -3 6 29 -8.20 7.10 3 6 -29 12.50 7.70 -3 -6 -29 5.80 8.10 3 -6 29 -0.10 5.80 3 -6 -29 -2.10 6.60 3 6 29 1.20 7.30 -3 -6 29 7.60 8.30 3 -6 -29 4.80 7.60 -3 6 -29 15.80 8.10 4 6 -29 -1.80 7.20 -4 6 29 -4.00 7.30 -4 6 29 0.90 6.90 4 -6 29 3.00 5.60 4 -6 -29 3.60 7.00 -4 -6 29 6.40 8.90 4 6 29 2.10 9.30 4 -6 -29 -2.30 7.20 -4 6 -29 -4.80 5.90 0 -7 29 -1.50 6.60 0 -7 -29 -2.40 6.70 0 -7 -29 0.40 6.30 0 7 -29 -13.50 5.10 0 7 29 12.80 8.50 -1 7 29 56.39 15.00 -1 -7 -29 75.49 13.10 1 -7 29 42.30 9.80 -1 7 29 78.89 15.70 1 7 -29 80.89 14.20 -1 -7 -29 83.49 13.70 1 -7 -29 45.60 12.00 1 -7 -29 52.29 11.70 -1 7 -29 72.39 13.00 -1 -7 29 56.29 11.80 1 7 29 58.39 15.40 -2 7 29 283.27 31.20 -2 7 29 305.37 19.90 -2 -7 -29 240.68 22.70 2 7 -29 311.47 22.40 2 -7 29 323.67 20.20 -2 -7 29 317.67 22.90 2 -7 -29 291.97 23.50 -2 7 -29 288.77 21.40 3 -7 29 211.68 16.00 3 -7 -29 172.88 20.50 -3 -7 29 200.68 21.10 0 0 -30 113.39 15.80 0 0 30 116.69 16.80 1 0 -30 601.34 32.10 -1 0 30 705.83 35.70 -1 0 -30 643.14 33.20 1 0 30 695.93 34.80 -2 0 30 15.60 8.70 -2 0 -30 11.00 8.60 2 0 -30 33.00 10.50 2 0 30 16.30 9.00 3 0 -30 149.29 17.50 -3 0 30 155.68 19.20 3 0 30 174.98 18.70 3 0 -30 181.58 23.60 -3 0 -30 204.48 20.80 4 0 -30 83.69 14.80 4 0 -30 123.19 16.40 -4 0 -30 121.19 16.90 4 0 30 154.18 17.30 -4 0 30 126.09 18.90 5 0 -30 10.60 7.60 5 0 30 16.80 8.00 5 0 -30 6.30 7.60 0 -1 30 1.90 7.20 0 1 30 -0.70 7.40 0 1 -30 -1.00 5.90 0 -1 -30 -0.70 6.50 -1 -1 -30 7.10 7.60 1 -1 30 1.10 6.90 -1 1 30 2.70 7.60 1 1 -30 1.70 7.00 -1 -1 30 8.60 8.30 1 -1 -30 18.20 9.10 -1 1 -30 18.70 9.60 1 1 30 10.60 8.50 2 1 -30 21.70 9.20 2 -1 30 28.90 9.40 -2 -1 -30 25.70 9.50 -2 1 30 23.20 10.00 2 -1 -30 14.00 9.30 -2 -1 30 22.90 9.80 2 1 30 39.60 11.00 -2 1 -30 14.10 8.00 -3 -1 -30 247.58 23.20 3 -1 30 220.68 20.70 3 1 -30 188.18 19.60 -3 1 30 204.38 22.80 3 1 30 230.58 21.90 -3 1 -30 259.87 23.20 3 -1 -30 186.38 20.10 -3 -1 30 186.38 20.60 3 -1 -30 184.68 21.10 4 1 -30 22.70 9.30 4 1 -30 -1.60 5.80 4 -1 30 -0.60 5.90 -4 -1 -30 4.30 7.00 -4 1 30 -13.70 6.20 4 -1 -30 -2.80 7.20 4 -1 -30 15.90 8.80 4 1 30 -0.20 7.20 -4 -1 30 -5.30 6.70 -4 1 -30 0.50 6.30 0 2 30 49.70 13.00 0 2 -30 80.79 13.70 0 -2 30 84.99 13.70 0 -2 -30 82.49 13.70 1 2 -30 147.59 17.80 -1 2 30 163.38 20.30 1 -2 30 135.49 17.00 -1 -2 -30 157.28 18.70 -1 2 -30 139.59 17.50 1 2 30 171.78 20.10 1 -2 -30 194.78 20.30 -1 -2 30 144.09 17.80 2 2 -30 -5.90 6.90 -2 -2 -30 10.70 8.00 2 -2 30 -4.60 6.60 -2 2 30 7.00 8.20 2 -2 -30 6.40 8.50 -2 2 -30 9.40 8.20 2 -2 -30 5.00 6.70 2 2 30 5.40 8.20 -2 -2 30 30.80 10.90 3 2 -30 -1.00 6.10 -3 2 30 14.50 9.40 -3 -2 -30 0.40 7.50 3 -2 30 4.40 6.90 3 -2 -30 13.30 8.30 -3 2 -30 -12.60 5.70 -3 -2 30 0.60 8.20 3 -2 -30 -3.40 7.10 3 2 30 6.70 8.20 -4 2 30 146.99 27.50 4 2 -30 126.79 17.30 -4 -2 -30 157.78 18.90 4 -2 30 128.79 15.50 4 -2 -30 145.99 17.60 -4 -2 30 155.78 23.10 4 2 30 132.59 17.20 -4 2 -30 146.99 18.10 4 -2 -30 174.08 20.60 0 3 -30 2.20 6.50 0 -3 -30 16.40 8.10 0 3 30 -1.80 7.20 0 -3 30 -4.40 6.70 -1 -3 -30 61.29 12.30 1 3 -30 46.00 11.70 1 -3 30 55.59 12.60 -1 3 30 65.79 13.90 1 -3 -30 62.19 12.60 1 3 30 70.49 13.70 -1 -3 30 67.49 13.50 1 -3 -30 76.49 16.80 -1 3 -30 80.69 14.10 -2 3 30 37.10 11.80 -2 -3 -30 20.20 9.20 2 -3 30 13.70 8.70 2 3 -30 28.00 9.90 -2 -3 30 18.70 8.90 2 -3 -30 17.60 9.10 2 -3 -30 34.60 10.80 2 3 30 9.00 8.00 -2 3 -30 21.60 9.10 3 -3 30 571.14 29.20 -3 -3 -30 586.14 31.60 3 3 -30 600.44 31.80 -3 3 30 550.94 34.10 3 -3 -30 598.74 31.60 -3 3 -30 599.54 31.30 3 -3 -30 617.74 32.80 -3 -3 30 584.54 32.90 3 3 30 638.74 34.10 -4 -3 -30 12.10 8.50 4 3 -30 20.00 10.00 4 -3 30 17.50 8.00 -4 3 -30 3.20 7.50 4 -3 -30 22.50 9.60 4 -3 -30 14.50 8.40 4 3 30 -0.60 7.30 0 -4 30 8.30 7.50 0 4 30 7.20 8.10 0 4 -30 -4.70 7.20 0 -4 -30 8.50 8.10 -1 4 30 400.46 28.10 -1 -4 -30 403.86 26.10 1 4 -30 367.36 25.00 1 -4 30 393.96 24.70 1 -4 -30 407.96 26.50 -1 -4 30 393.16 25.50 1 4 30 391.56 27.70 1 -4 -30 417.56 25.70 -1 4 -30 356.46 24.30 -2 -4 -30 5.30 7.50 -2 4 30 1.90 6.80 2 -4 30 -3.60 6.40 2 4 -30 -1.80 6.00 2 -4 -30 1.10 7.50 -2 -4 30 -1.50 7.50 2 4 30 2.50 7.30 -2 4 -30 -9.80 6.50 2 -4 -30 2.60 6.90 -3 -4 -30 40.30 11.50 3 4 -30 28.70 9.60 3 -4 30 19.20 7.90 3 -4 -30 37.50 10.90 3 4 30 39.70 11.30 3 -4 -30 31.30 9.90 -3 4 -30 24.80 9.30 -3 -4 30 25.90 11.20 0 5 -30 5.60 7.90 0 -5 30 -4.00 6.10 0 -5 -30 -2.40 7.40 0 -5 -30 7.10 8.00 -1 -5 -30 35.50 10.90 1 5 -30 14.90 8.60 1 -5 30 21.90 8.80 1 -5 -30 16.20 7.80 1 -5 -30 17.30 8.90 -1 -5 30 19.90 8.80 -1 5 -30 29.00 10.10 2 5 -30 -1.00 7.40 2 -5 30 1.80 6.40 2 -5 -30 5.90 8.00 -2 -5 30 4.40 7.60 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 88219 _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received'