data_181010RAL_KL_21_100K_0m_a _audit_creation_method 'SHELXL-2017/1' _shelx_SHELXL_version_number '2017/1' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H38 B2 N2' _chemical_formula_sum 'C34 H38 B2 N2' _chemical_formula_weight 496.28 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' 'B' 'B' 0.0090 0.0039 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.8361(2) _cell_length_b 17.0449(3) _cell_length_c 13.5799(2) _cell_angle_alpha 90 _cell_angle_beta 94.612(1) _cell_angle_gamma 90 _cell_volume 2730.81(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9526 _cell_measurement_theta_min 3.27 _cell_measurement_theta_max 66.64 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.207 _exptl_crystal_F_000 1064 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.524 _exptl_crystal_size_mid 0.322 _exptl_crystal_size_min 0.214 _exptl_absorpt_coefficient_mu 0.514 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.823 _exptl_absorpt_correction_T_max 0.923 _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_special_details ; 'crystal mounted on a Cryoloop using Paratone-N' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD Apex-II area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42701 _diffrn_reflns_av_unetI/netI 0.0250 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.746 _diffrn_reflns_theta_max 66.652 _diffrn_reflns_theta_full 66.652 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measured_fraction_theta_full 0.976 _diffrn_reflns_Laue_measured_fraction_max 0.976 _diffrn_reflns_Laue_measured_fraction_full 0.976 _diffrn_reflns_point_group_measured_fraction_max 0.976 _diffrn_reflns_point_group_measured_fraction_full 0.976 _reflns_number_total 4714 _reflns_number_gt 4162 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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. ; _computing_data_collection 'APEX 2 (Bruker, 2006)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT (Bruker, 2005)' _computing_structure_solution 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics 'SHELXTL' _computing_publication_material 'SHELXTL' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+1.4403P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method 'SHELXL-2017/1 (Sheldrick 2017)' _refine_ls_extinction_coef 0.00135(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4714 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0951 _refine_ls_wR_factor_gt 0.0909 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 N1 N 0.87083(9) 0.15130(6) 0.39542(9) 0.0183(3) Uani 1 1 d . . . . . N2 N 0.58494(9) 0.54192(6) 0.30690(9) 0.0206(3) Uani 1 1 d . . . . . C7 C 0.83835(11) 0.31605(7) 0.34379(9) 0.0156(3) Uani 1 1 d . . . . . C6 C 0.75423(11) 0.26907(7) 0.38325(9) 0.0157(3) Uani 1 1 d . . . . . C12 C 0.81551(11) 0.39786(7) 0.32596(10) 0.0167(3) Uani 1 1 d . . . . . C5 C 0.78729(11) 0.19449(7) 0.43338(10) 0.0171(3) Uani 1 1 d . . . . . C14 C 0.64017(11) 0.29485(7) 0.37398(10) 0.0168(3) Uani 1 1 d . . . . . C13 C 0.70620(11) 0.42791(7) 0.33901(10) 0.0165(3) Uani 1 1 d . . . . . C4 C 0.74112(11) 0.16876(8) 0.52061(10) 0.0207(3) Uani 1 1 d . . . . . C20 C 0.68575(11) 0.51313(8) 0.34803(10) 0.0183(3) Uani 1 1 d . . . . . C9 C 1.02446(11) 0.33031(8) 0.28780(10) 0.0210(3) Uani 1 1 d . . . . . H9 H 1.095787 0.309014 0.274381 0.025 Uiso 1 1 calc R U . . . C8 C 0.94350(11) 0.28110(7) 0.32129(10) 0.0171(3) Uani 1 1 d . . . . . C19 C 0.61547(11) 0.37498(8) 0.34641(10) 0.0173(3) Uani 1 1 d . . . . . C11 C 0.90373(11) 0.44427(8) 0.28993(10) 0.0197(3) Uani 1 1 d . . . . . H11 H 0.891579 0.498639 0.277842 0.024 Uiso 1 1 calc R U . . . C10 C 1.00499(12) 0.41144(8) 0.27274(11) 0.0218(3) Uani 1 1 d . . . . . H10 H 1.063433 0.443429 0.250316 0.026 Uiso 1 1 calc R U . . . C15 C 0.54642(11) 0.24421(8) 0.38599(10) 0.0210(3) Uani 1 1 d . . . . . H15 H 0.559443 0.190864 0.403713 0.025 Uiso 1 1 calc R U . . . C18 C 0.50102(11) 0.40225(8) 0.32596(10) 0.0199(3) Uani 1 1 d . . . . . C21 C 0.76083(11) 0.56372(8) 0.40355(11) 0.0212(3) Uani 1 1 d . . . . . C16 C 0.43829(12) 0.27179(9) 0.37224(11) 0.0255(3) Uani 1 1 d . . . . . H16 H 0.376824 0.237939 0.383328 0.031 Uiso 1 1 calc R U . . . C28 C 0.90039(12) 0.15473(8) 0.20816(11) 0.0232(3) Uani 1 1 d . . . . . H28A H 0.910276 0.097080 0.206494 0.028 Uiso 1 1 calc R U . . . H28B H 0.817948 0.165571 0.202003 0.028 Uiso 1 1 calc R U . . . C17 C 0.41601(11) 0.34994(8) 0.34176(11) 0.0247(3) Uani 1 1 d . . . . . H17 H 0.339491 0.366921 0.331827 0.030 Uiso 1 1 calc R U . . . C26 C 1.08254(11) 0.15707(8) 0.34467(11) 0.0211(3) Uani 1 1 d . . . . . H26A H 1.084437 0.099250 0.338113 0.025 Uiso 1 1 calc R U . . . H26B H 1.132443 0.179171 0.296531 0.025 Uiso 1 1 calc R U . . . C1 C 0.89208(11) 0.07784(8) 0.42889(11) 0.0236(3) Uani 1 1 d . . . . . H1 H 0.945801 0.046904 0.397899 0.028 Uiso 1 1 calc R U . . . C25 C 0.67161(12) 0.21985(9) 0.58356(11) 0.0254(3) Uani 1 1 d . . . . . H25A H 0.591406 0.205602 0.572238 0.038 Uiso 1 1 calc R U . . . H25B H 0.681560 0.275026 0.565897 0.038 Uiso 1 1 calc R U . . . H25C H 0.696757 0.212088 0.653408 0.038 Uiso 1 1 calc R U . . . C24 C 0.56686(12) 0.61968(8) 0.30413(12) 0.0278(3) Uani 1 1 d . . . . . H24 H 0.499171 0.638908 0.270175 0.033 Uiso 1 1 calc R U . . . C2 C 0.83974(12) 0.04618(8) 0.50527(12) 0.0282(3) Uani 1 1 d . . . . . H2 H 0.851856 -0.007025 0.524100 0.034 Uiso 1 1 calc R U . . . C3 C 0.76847(12) 0.09378(8) 0.55456(11) 0.0256(3) Uani 1 1 d . . . . . H3 H 0.737717 0.074917 0.612563 0.031 Uiso 1 1 calc R U . . . C30 C 0.86093(12) 0.53633(8) 0.47008(11) 0.0261(3) Uani 1 1 d . . . . . H30A H 0.930670 0.544393 0.437098 0.039 Uiso 1 1 calc R U . . . H30B H 0.852350 0.480431 0.484644 0.039 Uiso 1 1 calc R U . . . H30C H 0.864934 0.566328 0.531830 0.039 Uiso 1 1 calc R U . . . C31 C 0.48329(12) 0.47582(9) 0.15021(11) 0.0257(3) Uani 1 1 d . . . . . H31A H 0.473651 0.528409 0.119755 0.031 Uiso 1 1 calc R U . . . H31B H 0.559507 0.456533 0.136984 0.031 Uiso 1 1 calc R U . . . C29 C 0.95221(13) 0.18989(9) 0.11940(11) 0.0298(3) Uani 1 1 d . . . . . H29A H 0.937183 0.246423 0.116765 0.045 Uiso 1 1 calc R U . . . H29B H 0.918639 0.165087 0.058845 0.045 Uiso 1 1 calc R U . . . H29C H 1.034242 0.180848 0.125339 0.045 Uiso 1 1 calc R U . . . C33 C 0.36191(12) 0.52659(8) 0.29865(11) 0.0245(3) Uani 1 1 d . . . . . H33A H 0.349745 0.574751 0.258435 0.029 Uiso 1 1 calc R U . . . H33B H 0.297756 0.490740 0.280617 0.029 Uiso 1 1 calc R U . . . C23 C 0.64212(13) 0.67234(8) 0.34832(13) 0.0317(4) Uani 1 1 d . . . . . H23 H 0.629719 0.727233 0.341906 0.038 Uiso 1 1 calc R U . . . C27 C 1.13127(12) 0.17894(9) 0.44863(12) 0.0281(3) Uani 1 1 d . . . . . H27A H 1.128022 0.235988 0.456957 0.042 Uiso 1 1 calc R U . . . H27B H 1.210239 0.161397 0.458205 0.042 Uiso 1 1 calc R U . . . H27C H 1.086814 0.153472 0.497418 0.042 Uiso 1 1 calc R U . . . C22 C 0.73605(12) 0.64341(8) 0.40218(12) 0.0278(3) Uani 1 1 d . . . . . H22 H 0.785097 0.678568 0.439256 0.033 Uiso 1 1 calc R U . . . C34 C 0.35947(13) 0.54863(9) 0.40768(12) 0.0308(4) Uani 1 1 d . . . . . H34A H 0.371340 0.501485 0.448513 0.046 Uiso 1 1 calc R U . . . H34B H 0.285789 0.571834 0.418709 0.046 Uiso 1 1 calc R U . . . H34C H 0.419702 0.586672 0.425641 0.046 Uiso 1 1 calc R U . . . C32 C 0.39482(14) 0.42082(10) 0.09991(12) 0.0338(4) Uani 1 1 d . . . . . H32A H 0.407062 0.367525 0.125663 0.051 Uiso 1 1 calc R U . . . H32B H 0.401724 0.420927 0.028473 0.051 Uiso 1 1 calc R U . . . H32C H 0.318849 0.438677 0.113259 0.051 Uiso 1 1 calc R U . . . B1 B 0.95326(13) 0.18698(9) 0.31515(12) 0.0184(3) Uani 1 1 d . . . . . B2 B 0.47830(13) 0.48480(9) 0.26949(12) 0.0211(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 N1 0.0177(5) 0.0137(5) 0.0228(6) 0.0005(4) -0.0022(5) -0.0003(4) N2 0.0216(6) 0.0177(6) 0.0223(6) 0.0018(5) 0.0010(5) 0.0035(4) C7 0.0180(6) 0.0154(6) 0.0129(6) -0.0005(5) -0.0018(5) -0.0006(5) C6 0.0191(6) 0.0138(6) 0.0140(7) -0.0026(5) -0.0003(5) -0.0006(5) C12 0.0197(6) 0.0150(6) 0.0148(7) -0.0001(5) -0.0019(5) -0.0001(5) C5 0.0160(6) 0.0155(6) 0.0191(7) -0.0012(5) -0.0025(5) -0.0029(5) C14 0.0193(6) 0.0170(6) 0.0141(7) -0.0019(5) 0.0006(5) -0.0014(5) C13 0.0195(6) 0.0163(7) 0.0133(7) 0.0006(5) -0.0019(5) 0.0011(5) C4 0.0182(6) 0.0222(7) 0.0207(7) 0.0023(6) -0.0036(6) -0.0055(5) C20 0.0194(6) 0.0167(7) 0.0188(7) 0.0018(5) 0.0024(5) 0.0018(5) C9 0.0181(6) 0.0204(7) 0.0246(8) 0.0000(6) 0.0030(6) 0.0017(5) C8 0.0178(6) 0.0169(7) 0.0161(7) -0.0006(5) -0.0014(5) 0.0001(5) C19 0.0192(6) 0.0181(7) 0.0145(7) -0.0020(5) 0.0000(5) 0.0007(5) C11 0.0235(7) 0.0136(6) 0.0216(7) 0.0022(5) 0.0001(6) -0.0013(5) C10 0.0212(7) 0.0193(7) 0.0252(8) 0.0036(6) 0.0031(6) -0.0039(5) C15 0.0212(7) 0.0179(7) 0.0235(8) 0.0007(5) 0.0004(6) -0.0024(5) C18 0.0189(7) 0.0219(7) 0.0188(7) -0.0025(5) 0.0005(6) 0.0012(5) C21 0.0220(7) 0.0184(7) 0.0234(8) -0.0016(5) 0.0032(6) -0.0006(5) C16 0.0192(7) 0.0254(7) 0.0319(9) 0.0005(6) 0.0022(6) -0.0054(5) C28 0.0266(7) 0.0173(7) 0.0247(8) -0.0013(6) -0.0037(6) 0.0025(5) C17 0.0172(7) 0.0264(8) 0.0303(8) -0.0002(6) -0.0004(6) 0.0014(5) C26 0.0221(7) 0.0163(7) 0.0251(8) 0.0004(5) 0.0021(6) 0.0031(5) C1 0.0198(7) 0.0149(7) 0.0353(9) 0.0020(6) -0.0038(6) 0.0016(5) C25 0.0276(7) 0.0287(8) 0.0199(8) 0.0016(6) 0.0028(6) -0.0043(6) C24 0.0255(7) 0.0193(7) 0.0384(9) 0.0047(6) 0.0009(7) 0.0058(6) C2 0.0251(7) 0.0187(7) 0.0394(9) 0.0118(6) -0.0061(7) -0.0013(6) C3 0.0217(7) 0.0277(8) 0.0266(8) 0.0099(6) -0.0025(6) -0.0058(6) C30 0.0266(7) 0.0217(7) 0.0289(8) -0.0035(6) -0.0049(6) -0.0029(6) C31 0.0250(7) 0.0268(8) 0.0253(8) 0.0002(6) 0.0019(6) 0.0038(6) C29 0.0341(8) 0.0318(8) 0.0229(8) -0.0015(6) -0.0007(7) 0.0047(6) C33 0.0221(7) 0.0244(7) 0.0269(8) 0.0041(6) 0.0011(6) 0.0050(6) C23 0.0305(8) 0.0157(7) 0.0489(10) -0.0005(7) 0.0041(7) 0.0036(6) C27 0.0246(7) 0.0240(7) 0.0341(9) -0.0020(6) -0.0074(7) 0.0019(6) C22 0.0277(7) 0.0192(7) 0.0367(9) -0.0067(6) 0.0036(7) -0.0022(6) C34 0.0334(8) 0.0304(8) 0.0295(9) 0.0043(7) 0.0080(7) 0.0104(6) C32 0.0415(9) 0.0330(9) 0.0257(9) -0.0027(7) -0.0047(7) 0.0001(7) B1 0.0195(7) 0.0163(7) 0.0196(8) 0.0000(6) 0.0020(6) 0.0008(6) B2 0.0178(7) 0.0223(8) 0.0226(9) 0.0003(6) -0.0019(6) 0.0017(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 N1 C1 1.3488(17) . ? N1 C5 1.3666(17) . ? N1 B1 1.6374(18) . ? N2 C24 1.3427(18) . ? N2 C20 1.3673(17) . ? N2 B2 1.6418(19) . ? C7 C6 1.4161(18) . ? C7 C8 1.4346(18) . ? C7 C12 1.4373(18) . ? C6 C14 1.4156(18) . ? C6 C5 1.4797(18) . ? C12 C13 1.4159(18) . ? C12 C11 1.4274(18) . ? C5 C4 1.4136(19) . ? C14 C15 1.4255(18) . ? C14 C19 1.4400(18) . ? C13 C19 1.4122(18) . ? C13 C20 1.4792(18) . ? C4 C3 1.388(2) . ? C4 C25 1.510(2) . ? C20 C21 1.4121(19) . ? C9 C8 1.3780(19) . ? C9 C10 1.4140(19) . ? C9 H9 0.9500 . ? C8 B1 1.6111(19) . ? C19 C18 1.4380(18) . ? C11 C10 1.3599(19) . ? C11 H11 0.9500 . ? C10 H10 0.9500 . ? C15 C16 1.3622(19) . ? C15 H15 0.9500 . ? C18 C17 1.3741(19) . ? C18 B2 1.615(2) . ? C21 C22 1.389(2) . ? C21 C30 1.505(2) . ? C16 C17 1.413(2) . ? C16 H16 0.9500 . ? C28 C29 1.519(2) . ? C28 B1 1.630(2) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C17 H17 0.9500 . ? C26 C27 1.528(2) . ? C26 B1 1.6320(19) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C1 C2 1.362(2) . ? C1 H1 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C24 C23 1.369(2) . ? C24 H24 0.9500 . ? C2 C3 1.382(2) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.525(2) . ? C31 B2 1.633(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C33 C34 1.530(2) . ? C33 B2 1.6278(19) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C23 C22 1.372(2) . ? C23 H23 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C22 H22 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 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 C1 N1 C5 119.61(12) . . ? C1 N1 B1 117.66(11) . . ? C5 N1 B1 122.61(10) . . ? C24 N2 C20 119.84(12) . . ? C24 N2 B2 117.38(11) . . ? C20 N2 B2 122.52(11) . . ? C6 C7 C8 119.62(11) . . ? C6 C7 C12 118.94(11) . . ? C8 C7 C12 121.44(11) . . ? C14 C6 C7 119.04(12) . . ? C14 C6 C5 121.50(11) . . ? C7 C6 C5 119.46(11) . . ? C13 C12 C11 122.91(12) . . ? C13 C12 C7 119.42(11) . . ? C11 C12 C7 117.56(12) . . ? N1 C5 C4 119.28(12) . . ? N1 C5 C6 117.51(11) . . ? C4 C5 C6 123.11(12) . . ? C6 C14 C15 123.19(12) . . ? C6 C14 C19 119.32(11) . . ? C15 C14 C19 117.41(12) . . ? C19 C13 C12 119.05(12) . . ? C19 C13 C20 119.40(11) . . ? C12 C13 C20 121.52(11) . . ? C3 C4 C5 117.93(13) . . ? C3 C4 C25 117.79(13) . . ? C5 C4 C25 124.09(12) . . ? N2 C20 C21 119.34(12) . . ? N2 C20 C13 117.50(12) . . ? C21 C20 C13 122.94(12) . . ? C8 C9 C10 122.24(12) . . ? C8 C9 H9 118.9 . . ? C10 C9 H9 118.9 . . ? C9 C8 C7 117.11(12) . . ? C9 C8 B1 122.31(12) . . ? C7 C8 B1 119.44(11) . . ? C13 C19 C18 119.32(12) . . ? C13 C19 C14 119.00(12) . . ? C18 C19 C14 121.68(12) . . ? C10 C11 C12 120.65(12) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C11 C10 C9 120.89(12) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C16 C15 C14 120.45(13) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C18 C19 116.77(12) . . ? C17 C18 B2 122.93(12) . . ? C19 C18 B2 119.45(12) . . ? C22 C21 C20 117.82(13) . . ? C22 C21 C30 117.80(13) . . ? C20 C21 C30 124.21(12) . . ? C15 C16 C17 121.10(13) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C29 C28 B1 115.06(12) . . ? C29 C28 H28A 108.5 . . ? B1 C28 H28A 108.5 . . ? C29 C28 H28B 108.5 . . ? B1 C28 H28B 108.5 . . ? H28A C28 H28B 107.5 . . ? C18 C17 C16 122.38(13) . . ? C18 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? C27 C26 B1 115.32(11) . . ? C27 C26 H26A 108.4 . . ? B1 C26 H26A 108.4 . . ? C27 C26 H26B 108.4 . . ? B1 C26 H26B 108.4 . . ? H26A C26 H26B 107.5 . . ? N1 C1 C2 122.72(13) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C4 C25 H25A 109.5 . . ? C4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N2 C24 C23 122.58(14) . . ? N2 C24 H24 118.7 . . ? C23 C24 H24 118.7 . . ? C1 C2 C3 117.98(13) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? C2 C3 C4 121.00(13) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C21 C30 H30A 109.5 . . ? C21 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C21 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 B2 115.07(12) . . ? C32 C31 H31A 108.5 . . ? B2 C31 H31A 108.5 . . ? C32 C31 H31B 108.5 . . ? B2 C31 H31B 108.5 . . ? H31A C31 H31B 107.5 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C34 C33 B2 115.15(12) . . ? C34 C33 H33A 108.5 . . ? B2 C33 H33A 108.5 . . ? C34 C33 H33B 108.5 . . ? B2 C33 H33B 108.5 . . ? H33A C33 H33B 107.5 . . ? C24 C23 C22 117.96(14) . . ? C24 C23 H23 121.0 . . ? C22 C23 H23 121.0 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C22 C21 121.30(14) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C8 B1 C28 110.97(11) . . ? C8 B1 C26 111.59(11) . . ? C28 B1 C26 113.49(11) . . ? C8 B1 N1 106.64(10) . . ? C28 B1 N1 105.16(11) . . ? C26 B1 N1 108.52(11) . . ? C18 B2 C33 112.19(12) . . ? C18 B2 C31 111.81(12) . . ? C33 B2 C31 112.41(12) . . ? C18 B2 N2 105.98(11) . . ? C33 B2 N2 108.05(11) . . ? C31 B2 N2 105.92(11) . . ? _refine_diff_density_max 0.263 _refine_diff_density_min -0.196 _refine_diff_density_rms 0.036 _shelx_res_file ; TITL 181010RAL_KL_21_100K_0m_a.res in P2(1)/c 181010RAL_KL_21_100K_0m_a.res created by SHELXL-2017/1 at 20:11:21 on 10-Oct-2018 CELL 1.54178 11.8361 17.0449 13.5799 90.000 94.612 90.000 ZERR 4.000 0.0002 0.0003 0.0002 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H B N UNIT 136 152 8 8 L.S. 25 ACTA BOND $H FMAP 2 PLAN 4 TEMP -173.270 WGHT 0.037800 1.440300 EXTI 0.001354 FVAR 0.55294 N1 4 0.870825 0.151295 0.395422 11.00000 0.01766 0.01370 = 0.02279 0.00055 -0.00222 -0.00033 N2 4 0.584935 0.541917 0.306900 11.00000 0.02156 0.01767 = 0.02232 0.00177 0.00102 0.00349 C7 1 0.838351 0.316047 0.343790 11.00000 0.01802 0.01542 = 0.01295 -0.00051 -0.00184 -0.00060 C6 1 0.754229 0.269075 0.383253 11.00000 0.01914 0.01382 = 0.01395 -0.00256 -0.00028 -0.00055 C12 1 0.815512 0.397861 0.325956 11.00000 0.01968 0.01503 = 0.01477 -0.00008 -0.00188 -0.00012 C5 1 0.787287 0.194494 0.433379 11.00000 0.01603 0.01553 = 0.01907 -0.00124 -0.00251 -0.00291 C14 1 0.640173 0.294848 0.373979 11.00000 0.01931 0.01703 = 0.01409 -0.00190 0.00061 -0.00140 C13 1 0.706198 0.427912 0.339007 11.00000 0.01949 0.01630 = 0.01327 0.00057 -0.00188 0.00108 C4 1 0.741115 0.168761 0.520608 11.00000 0.01820 0.02225 = 0.02073 0.00235 -0.00363 -0.00549 C20 1 0.685748 0.513128 0.348034 11.00000 0.01936 0.01671 = 0.01883 0.00175 0.00235 0.00181 C9 1 1.024461 0.330314 0.287804 11.00000 0.01809 0.02035 = 0.02465 -0.00005 0.00299 0.00169 AFIX 43 H9 2 1.095787 0.309014 0.274381 11.00000 -1.20000 AFIX 0 C8 1 0.943499 0.281100 0.321290 11.00000 0.01776 0.01694 = 0.01613 -0.00057 -0.00142 0.00013 C19 1 0.615474 0.374985 0.346414 11.00000 0.01922 0.01806 = 0.01447 -0.00203 0.00004 0.00068 C11 1 0.903729 0.444274 0.289930 11.00000 0.02348 0.01355 = 0.02164 0.00222 0.00007 -0.00132 AFIX 43 H11 2 0.891579 0.498639 0.277842 11.00000 -1.20000 AFIX 0 C10 1 1.004990 0.411436 0.272743 11.00000 0.02116 0.01927 = 0.02524 0.00365 0.00311 -0.00386 AFIX 43 H10 2 1.063433 0.443429 0.250316 11.00000 -1.20000 AFIX 0 C15 1 0.546421 0.244211 0.385994 11.00000 0.02119 0.01793 = 0.02355 0.00074 0.00043 -0.00240 AFIX 43 H15 2 0.559443 0.190864 0.403713 11.00000 -1.20000 AFIX 0 C18 1 0.501017 0.402254 0.325959 11.00000 0.01890 0.02186 = 0.01879 -0.00248 0.00047 0.00121 C21 1 0.760833 0.563720 0.403548 11.00000 0.02197 0.01844 = 0.02336 -0.00160 0.00323 -0.00058 C16 1 0.438287 0.271794 0.372242 11.00000 0.01920 0.02544 = 0.03191 0.00051 0.00220 -0.00538 AFIX 43 H16 2 0.376824 0.237939 0.383328 11.00000 -1.20000 AFIX 0 C28 1 0.900385 0.154726 0.208164 11.00000 0.02659 0.01730 = 0.02475 -0.00128 -0.00365 0.00254 AFIX 23 H28A 2 0.910276 0.097080 0.206494 11.00000 -1.20000 H28B 2 0.817948 0.165571 0.202003 11.00000 -1.20000 AFIX 0 C17 1 0.416009 0.349945 0.341756 11.00000 0.01717 0.02641 = 0.03029 -0.00015 -0.00041 0.00145 AFIX 43 H17 2 0.339491 0.366921 0.331827 11.00000 -1.20000 AFIX 0 C26 1 1.082543 0.157072 0.344667 11.00000 0.02207 0.01627 = 0.02512 0.00039 0.00207 0.00309 AFIX 23 H26A 2 1.084437 0.099250 0.338113 11.00000 -1.20000 H26B 2 1.132443 0.179171 0.296531 11.00000 -1.20000 AFIX 0 C1 1 0.892083 0.077838 0.428895 11.00000 0.01983 0.01487 = 0.03527 0.00197 -0.00379 0.00162 AFIX 43 H1 2 0.945801 0.046904 0.397899 11.00000 -1.20000 AFIX 0 C25 1 0.671614 0.219850 0.583559 11.00000 0.02761 0.02869 = 0.01992 0.00159 0.00281 -0.00433 AFIX 137 H25A 2 0.591406 0.205602 0.572238 11.00000 -1.50000 H25B 2 0.681560 0.275026 0.565897 11.00000 -1.50000 H25C 2 0.696757 0.212088 0.653408 11.00000 -1.50000 AFIX 0 C24 1 0.566858 0.619683 0.304135 11.00000 0.02547 0.01928 = 0.03842 0.00472 0.00086 0.00577 AFIX 43 H24 2 0.499171 0.638908 0.270175 11.00000 -1.20000 AFIX 0 C2 1 0.839737 0.046181 0.505274 11.00000 0.02509 0.01871 = 0.03935 0.01176 -0.00613 -0.00130 AFIX 43 H2 2 0.851856 -0.007025 0.524100 11.00000 -1.20000 AFIX 0 C3 1 0.768469 0.093785 0.554558 11.00000 0.02171 0.02768 = 0.02661 0.00994 -0.00250 -0.00583 AFIX 43 H3 2 0.737717 0.074917 0.612563 11.00000 -1.20000 AFIX 0 C30 1 0.860929 0.536328 0.470085 11.00000 0.02659 0.02167 = 0.02895 -0.00353 -0.00490 -0.00288 AFIX 137 H30A 2 0.930670 0.544393 0.437098 11.00000 -1.50000 H30B 2 0.852350 0.480431 0.484644 11.00000 -1.50000 H30C 2 0.864934 0.566328 0.531830 11.00000 -1.50000 AFIX 0 C31 1 0.483295 0.475817 0.150215 11.00000 0.02498 0.02677 = 0.02531 0.00022 0.00187 0.00379 AFIX 23 H31A 2 0.473651 0.528409 0.119755 11.00000 -1.20000 H31B 2 0.559507 0.456533 0.136984 11.00000 -1.20000 AFIX 0 C29 1 0.952210 0.189890 0.119405 11.00000 0.03414 0.03182 = 0.02292 -0.00151 -0.00069 0.00469 AFIX 137 H29A 2 0.937183 0.246423 0.116765 11.00000 -1.50000 H29B 2 0.918639 0.165087 0.058845 11.00000 -1.50000 H29C 2 1.034242 0.180848 0.125339 11.00000 -1.50000 AFIX 0 C33 1 0.361911 0.526593 0.298648 11.00000 0.02206 0.02436 = 0.02685 0.00407 0.00107 0.00499 AFIX 23 H33A 2 0.349745 0.574751 0.258435 11.00000 -1.20000 H33B 2 0.297756 0.490740 0.280617 11.00000 -1.20000 AFIX 0 C23 1 0.642122 0.672341 0.348322 11.00000 0.03055 0.01568 = 0.04889 -0.00047 0.00414 0.00355 AFIX 43 H23 2 0.629719 0.727233 0.341906 11.00000 -1.20000 AFIX 0 C27 1 1.131272 0.178942 0.448629 11.00000 0.02456 0.02403 = 0.03413 -0.00198 -0.00739 0.00188 AFIX 137 H27A 2 1.128022 0.235988 0.456957 11.00000 -1.50000 H27B 2 1.210239 0.161397 0.458205 11.00000 -1.50000 H27C 2 1.086814 0.153472 0.497418 11.00000 -1.50000 AFIX 0 C22 1 0.736052 0.643414 0.402180 11.00000 0.02768 0.01918 = 0.03669 -0.00668 0.00356 -0.00216 AFIX 43 H22 2 0.785097 0.678568 0.439256 11.00000 -1.20000 AFIX 0 C34 1 0.359466 0.548626 0.407676 11.00000 0.03344 0.03043 = 0.02954 0.00430 0.00795 0.01045 AFIX 137 H34A 2 0.371340 0.501485 0.448513 11.00000 -1.50000 H34B 2 0.285789 0.571834 0.418709 11.00000 -1.50000 H34C 2 0.419702 0.586672 0.425641 11.00000 -1.50000 AFIX 0 C32 1 0.394824 0.420820 0.099905 11.00000 0.04150 0.03301 = 0.02569 -0.00272 -0.00472 0.00010 AFIX 137 H32A 2 0.407062 0.367525 0.125663 11.00000 -1.50000 H32B 2 0.401724 0.420927 0.028473 11.00000 -1.50000 H32C 2 0.318849 0.438677 0.113259 11.00000 -1.50000 AFIX 0 B1 3 0.953256 0.186975 0.315153 11.00000 0.01954 0.01627 = 0.01961 -0.00004 0.00203 0.00080 B2 3 0.478302 0.484804 0.269489 11.00000 0.01780 0.02229 = 0.02261 0.00026 -0.00191 0.00173 HKLF 4 REM 181010RAL_KL_21_100K_0m_a.res in P2(1)/c REM R1 = 0.0373 for 4162 Fo > 4sig(Fo) and 0.0434 for all 4714 data REM 350 parameters refined using 0 restraints END WGHT 0.0386 1.4271 REM Highest difference peak 0.263, deepest hole -0.196, 1-sigma level 0.036 Q1 1 0.6307 0.7774 0.3593 11.00000 0.05 0.26 Q2 1 1.0984 0.1593 0.5196 11.00000 0.05 0.26 Q3 1 0.4865 0.4469 0.3064 11.00000 0.05 0.23 Q4 1 1.0213 0.1764 0.3291 11.00000 0.05 0.22 ; _shelx_res_checksum 8548 _shelx_hkl_file ; -1 0 0 61.39 2.40 1 0 0 58.89 2.40 -2 0 0 468.35 17.10 2 0 0 481.45 17.20 -3 0 0 25.60 1.70 3 0 0 25.40 1.70 -4 0 0 1587.64 56.29 4 0 0 1572.64 56.49 -5 0 0 89.49 4.60 5 0 0 79.29 4.40 -5 0 0 84.09 4.30 -5 0 0 80.59 4.50 -5 0 0 78.09 4.30 -6 0 0 278.17 12.40 6 0 0 301.37 12.60 -6 0 0 307.87 12.40 6 0 0 302.17 12.40 -6 0 0 303.67 12.60 7 0 0 5.80 1.40 -7 0 0 5.90 1.80 -7 0 0 4.70 1.60 -7 0 0 9.40 2.10 7 0 0 5.40 1.80 -8 0 0 354.46 15.80 -8 0 0 342.87 14.80 -8 0 0 352.96 15.30 -8 0 0 328.97 15.00 8 0 0 326.07 15.00 -8 0 0 356.66 15.30 8 0 0 355.96 14.90 -9 0 0 10.80 2.40 -9 0 0 9.00 2.30 -9 0 0 9.90 2.50 -9 0 0 10.30 2.80 9 0 0 8.00 2.40 -9 0 0 8.50 2.60 -9 0 0 8.90 2.50 -9 0 0 8.20 2.40 -9 0 0 8.70 2.40 -9 0 0 9.10 2.70 -9 0 0 8.00 3.10 10 0 0 86.89 5.70 -10 0 0 93.29 6.20 -10 0 0 73.99 6.50 10 0 0 91.69 6.20 -10 0 0 81.09 5.50 -10 0 0 91.39 6.20 -10 0 0 89.39 6.10 -10 0 0 83.69 5.50 -10 0 0 87.89 7.20 -10 0 0 80.59 6.50 -11 0 0 22.90 3.60 -11 0 0 26.00 3.70 -11 0 0 21.50 3.10 -11 0 0 21.00 4.30 -11 0 0 29.70 4.00 -11 0 0 24.30 3.30 11 0 0 22.10 3.60 11 0 0 29.90 3.80 -11 0 0 29.60 4.60 -11 0 0 23.20 4.20 -12 0 0 34.30 3.80 -12 0 0 33.70 5.20 -12 0 0 34.40 3.70 -12 0 0 31.60 3.60 -12 0 0 26.50 3.50 -12 0 0 32.40 4.00 -13 0 0 7.00 3.00 -13 0 0 12.00 2.30 -13 0 0 18.80 2.90 -13 0 0 17.90 2.60 -13 0 0 15.40 2.90 -13 0 0 21.00 3.10 -14 0 0 6.40 1.80 -14 0 0 5.30 1.70 -14 0 0 9.70 2.10 14 0 0 4.50 1.60 -14 0 0 7.90 2.10 0 -1 0 1.00 0.20 0 1 0 0.90 0.20 -1 -1 0 3534.75 129.29 1 -1 0 3896.31 129.39 1 1 0 3369.06 129.39 -1 1 0 3986.80 129.49 -2 -1 0 1408.16 50.29 2 -1 0 1423.66 50.39 2 1 0 1454.45 50.19 -2 1 0 1405.06 50.09 3 -1 0 387.16 14.50 -3 -1 0 368.86 14.30 3 1 0 377.06 14.30 -3 1 0 401.46 14.20 4 -1 0 521.45 19.50 -4 -1 0 512.55 19.20 4 1 0 507.05 19.20 -4 1 0 518.75 19.10 -5 -1 0 3.60 1.30 -5 -1 0 2.80 1.20 -5 -1 0 3.00 1.30 5 -1 0 7.20 1.40 -5 1 0 3.40 0.90 -5 1 0 3.20 1.10 5 1 0 3.00 1.10 -5 1 0 3.10 1.30 5 1 0 3.10 1.10 -5 1 0 4.30 1.20 6 -1 0 173.68 8.10 -6 -1 0 163.78 7.80 -6 -1 0 162.08 7.80 -6 -1 0 169.98 7.80 -6 1 0 173.28 8.00 6 1 0 171.28 7.80 -6 1 0 168.38 7.80 -6 1 0 152.88 7.50 6 1 0 165.28 7.60 -6 1 0 163.58 7.80 -7 -1 0 96.49 6.00 7 -1 0 110.89 5.90 -7 -1 0 106.69 6.00 7 -1 0 107.59 6.30 -7 -1 0 106.99 6.10 7 1 0 106.49 5.90 7 1 0 106.09 5.80 -7 1 0 106.09 6.00 -7 1 0 109.69 5.80 -7 1 0 103.69 6.10 8 -1 0 113.99 6.70 -8 -1 0 113.99 7.50 -8 -1 0 119.09 6.90 -8 -1 0 129.59 7.30 8 -1 0 121.89 7.00 -8 -1 0 122.59 7.20 -8 -1 0 123.09 7.20 -8 1 0 117.29 7.00 -8 1 0 118.89 6.70 -8 1 0 124.29 7.20 -8 1 0 115.99 7.70 -8 1 0 123.59 7.00 8 1 0 107.19 6.50 -9 -1 0 60.29 5.70 -9 -1 0 63.39 5.00 -9 -1 0 65.59 4.60 -9 -1 0 60.59 5.00 9 -1 0 62.69 5.00 9 -1 0 58.09 4.40 -9 -1 0 54.89 4.50 -9 -1 0 62.29 5.20 -9 -1 0 65.09 5.40 9 -1 0 53.09 5.40 -9 -1 0 56.39 4.90 -9 -1 0 72.19 5.70 -9 1 0 66.29 4.80 -9 1 0 71.19 6.20 -9 1 0 57.29 5.10 -9 1 0 63.89 5.10 -9 1 0 63.29 4.40 9 1 0 64.29 4.80 -9 1 0 57.89 4.20 -9 1 0 63.69 5.00 -9 1 0 63.79 5.10 10 -1 0 86.49 6.20 -10 -1 0 86.39 6.00 -10 -1 0 86.29 6.70 -10 -1 0 80.69 6.30 -10 -1 0 86.29 6.10 -10 -1 0 81.79 6.30 -10 -1 0 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3 0 104.49 6.60 -7 3 0 115.09 6.20 -7 3 0 113.89 6.20 7 3 0 98.19 5.50 -7 3 0 104.89 6.20 -8 -3 0 39.20 4.60 -8 -3 0 47.30 5.00 -8 -3 0 42.30 3.90 -8 -3 0 41.50 4.10 8 -3 0 39.70 3.70 -8 -3 0 45.20 4.00 8 -3 0 44.90 4.50 -8 3 0 42.40 4.40 -8 3 0 48.10 4.00 -8 3 0 46.80 4.20 -9 -3 0 23.70 3.90 -9 -3 0 37.20 4.60 -9 -3 0 30.60 3.90 9 -3 0 29.00 3.90 -9 -3 0 34.60 4.90 -9 -3 0 29.60 3.40 -9 -3 0 32.50 3.70 -9 -3 0 33.30 4.00 -9 -3 0 33.00 4.30 -9 -3 0 30.50 3.80 -9 -3 0 29.40 3.60 -9 3 0 25.80 3.70 -9 3 0 34.00 4.20 -9 3 0 26.80 4.60 -9 3 0 26.60 4.20 -9 3 0 29.10 3.00 -9 3 0 34.00 3.90 -9 3 0 30.70 4.10 -9 3 0 32.10 3.50 -9 3 0 31.50 3.60 -10 -3 0 75.39 6.40 -10 -3 0 73.19 6.30 -10 -3 0 66.99 5.30 -10 -3 0 68.19 5.40 -10 -3 0 72.59 6.50 -10 -3 0 69.39 5.90 -10 -3 0 71.39 5.50 -10 -3 0 67.09 5.10 -10 -3 0 76.89 5.20 10 -3 0 87.19 6.30 -10 -3 0 74.29 5.50 -10 3 0 76.79 6.20 -10 3 0 76.39 5.20 -10 3 0 70.59 6.10 -10 3 0 73.99 5.30 -10 3 0 80.89 5.70 -10 3 0 76.29 5.60 -10 3 0 64.39 5.00 -10 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0 1483.75 52.89 2 -4 0 16.50 1.50 -2 -4 0 15.50 1.50 2 4 0 15.50 1.00 -2 4 0 15.90 1.00 3 -4 0 68.69 3.70 -3 -4 0 69.49 3.60 -3 4 0 68.19 3.00 3 4 0 64.99 2.90 -4 -4 0 5.80 1.40 -4 -4 0 5.00 1.40 -4 -4 0 3.30 1.20 -4 -4 0 5.90 2.40 4 -4 0 5.40 1.30 -4 4 0 6.20 1.00 4 4 0 5.40 1.00 -4 4 0 4.50 1.20 -4 4 0 5.10 1.30 -4 4 0 5.60 1.30 -5 -4 0 207.68 9.40 -5 -4 0 208.98 9.50 5 -4 0 213.38 9.80 -5 -4 0 226.38 14.10 -5 -4 0 214.98 9.60 -5 4 0 240.68 9.40 -5 4 0 210.38 9.40 -5 4 0 207.78 9.20 -5 4 0 211.88 9.40 -6 -4 0 474.65 18.90 -6 -4 0 464.35 24.20 -6 -4 0 453.75 18.60 -6 -4 0 468.05 18.60 6 -4 0 439.86 18.90 -6 4 0 474.65 18.60 -6 4 0 456.55 18.40 -6 4 0 470.45 18.60 -7 -4 0 63.19 4.50 -7 -4 0 67.69 5.10 -7 -4 0 60.79 5.30 -7 -4 0 67.79 5.00 -7 -4 0 72.99 5.10 7 -4 0 66.29 5.00 -7 4 0 69.69 4.90 -7 4 0 65.29 5.20 -7 4 0 70.39 4.80 -7 4 0 72.19 4.90 8 -4 0 235.38 11.10 -8 -4 0 225.48 11.30 -8 -4 0 229.68 11.90 -8 -4 0 219.28 11.10 -8 -4 0 236.18 11.50 -8 -4 0 250.07 11.70 8 -4 0 224.18 11.70 -8 4 0 217.68 11.10 -8 4 0 222.38 11.00 -8 4 0 229.48 11.00 -8 4 0 240.28 12.20 -9 -4 0 19.40 2.90 -9 -4 0 19.20 2.90 -9 -4 0 15.50 3.00 -9 -4 0 20.80 4.00 -9 -4 0 18.90 3.30 -9 -4 0 15.00 3.00 -9 -4 0 14.30 3.40 -9 -4 0 20.30 3.60 9 -4 0 22.00 3.50 -9 -4 0 15.30 3.00 -9 4 0 13.60 3.40 9 4 0 17.90 3.40 -9 4 0 16.60 2.90 -9 4 0 18.50 2.90 -9 4 0 18.30 3.20 -9 4 0 17.80 3.10 -9 4 0 19.50 3.20 -9 4 0 17.80 3.60 -9 4 0 17.10 3.40 -10 -4 0 351.06 16.10 -10 -4 0 347.07 16.50 10 -4 0 335.37 15.40 -10 -4 0 337.37 14.70 -10 -4 0 347.97 15.80 -10 -4 0 346.27 14.90 -10 -4 0 322.37 14.70 -10 -4 0 333.47 14.40 -10 -4 0 316.27 14.50 -10 4 0 308.87 14.60 -10 4 0 302.07 16.30 10 4 0 344.07 15.60 -10 4 0 313.97 14.10 -10 4 0 334.57 15.60 -10 4 0 334.67 14.80 -10 4 0 314.17 15.40 -10 4 0 333.27 15.60 -10 4 0 332.47 14.90 -11 -4 0 23.50 3.50 -11 -4 0 24.20 3.60 -11 -4 0 20.70 3.90 -11 -4 0 22.70 3.20 -11 -4 0 19.90 3.40 -11 -4 0 20.50 4.00 11 -4 0 28.20 4.20 -11 -4 0 21.60 4.20 -11 -4 0 20.40 3.50 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0 850.11 31.60 -4 -5 0 828.12 37.00 -4 5 0 851.31 30.90 4 5 0 854.11 31.10 -4 5 0 842.62 31.10 -4 5 0 829.22 31.00 -5 -5 0 14.70 4.30 -5 -5 0 13.70 2.00 5 -5 0 15.20 2.50 -5 -5 0 14.10 2.10 -5 5 0 13.20 2.00 -5 5 0 12.40 2.00 -5 5 0 12.90 2.00 5 5 0 13.70 2.10 6 -5 0 33.80 3.30 -6 -5 0 37.10 3.40 -6 -5 0 38.40 3.40 -6 -5 0 40.30 3.40 -6 -5 0 35.60 6.40 -6 5 0 35.20 3.30 -6 5 0 39.80 3.20 -6 5 0 37.10 3.20 6 5 0 31.30 2.90 -7 -5 0 52.79 4.90 -7 -5 0 47.60 4.00 -7 -5 0 57.99 4.60 7 -5 0 50.09 4.60 -7 -5 0 45.10 4.10 -7 5 0 54.99 4.30 7 5 0 49.60 4.10 -7 5 0 48.80 4.10 -7 5 0 54.49 4.80 -7 5 0 44.90 4.10 -8 -5 0 104.49 6.70 -8 -5 0 100.29 6.50 -8 -5 0 98.29 6.90 -8 -5 0 101.49 6.60 8 -5 0 103.09 6.60 8 -5 0 103.79 7.30 -8 5 0 95.89 6.30 -8 5 0 108.79 6.70 -8 5 0 95.39 6.20 8 5 0 112.19 6.80 -8 5 0 88.69 7.20 -9 -5 0 1.00 2.00 -9 -5 0 0.60 1.40 -9 -5 0 2.40 2.60 9 -5 0 2.10 2.10 -9 -5 0 0.10 1.50 -9 -5 0 -2.30 1.70 -9 -5 0 -2.60 1.80 -9 -5 0 2.40 1.80 -9 -5 0 -0.40 1.70 -9 5 0 -1.30 1.90 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209.98 11.00 -12 5 0 200.38 11.90 12 5 0 218.98 10.50 -12 5 0 220.08 10.40 -12 5 0 207.78 10.30 -13 -5 0 8.30 2.00 -13 -5 0 6.00 2.00 -13 -5 0 4.20 2.10 -13 -5 0 1.80 1.60 -13 5 0 3.90 1.90 -13 5 0 4.90 1.80 -13 5 0 3.70 2.40 -13 5 0 6.20 2.10 -13 5 0 1.70 1.80 13 5 0 2.80 1.60 0 -6 0 359.76 13.50 0 6 0 377.36 13.80 -1 -6 0 840.02 29.90 1 -6 0 819.72 30.20 -1 6 0 877.11 29.40 1 6 0 806.02 30.50 1 6 0 791.62 29.50 2 -6 0 18.70 1.80 -2 -6 0 20.70 1.80 -2 -6 0 26.30 4.50 -2 6 0 21.10 2.00 2 6 0 17.20 2.00 -3 -6 0 0.90 0.90 3 -6 0 3.30 1.30 -3 -6 0 2.60 1.00 -3 -6 0 2.40 1.90 -3 6 0 0.70 0.80 -3 6 0 1.20 1.00 -3 6 0 -0.90 0.70 3 6 0 0.90 1.10 4 -6 0 560.14 21.50 -4 -6 0 517.95 21.00 -4 -6 0 542.85 20.90 -4 -6 0 538.45 27.40 4 6 0 559.34 21.00 -4 6 0 542.15 20.90 -4 6 0 542.25 20.80 -4 6 0 557.54 20.70 -5 -6 0 177.18 8.80 -5 -6 0 192.58 14.40 5 -6 0 174.48 9.00 -5 -6 0 191.88 8.70 -5 6 0 188.08 8.60 -5 6 0 195.38 8.50 5 6 0 186.48 8.60 -5 6 0 186.18 8.60 -6 -6 0 93.19 5.90 -6 -6 0 87.09 10.10 -6 -6 0 96.59 5.80 6 -6 0 94.49 6.00 -6 -6 0 89.49 5.70 -6 -6 0 90.99 5.90 6 6 0 101.89 5.80 -6 6 0 100.69 5.80 -6 6 0 94.39 6.30 -6 6 0 103.39 5.60 -6 6 0 100.49 5.80 -7 -6 0 0.30 3.10 -7 -6 0 0.50 1.80 -7 -6 0 0.00 1.50 7 -6 0 1.80 1.90 -7 -6 0 -0.10 1.70 -7 -6 0 1.80 1.70 -7 6 0 0.60 1.50 -7 6 0 0.00 1.10 -7 6 0 1.30 1.60 -7 6 0 2.10 2.10 7 6 0 0.60 1.20 -8 -6 0 19.90 3.40 -8 -6 0 21.20 3.20 -8 -6 0 18.70 3.20 -8 -6 0 17.80 3.00 8 -6 0 16.00 3.10 -8 -6 0 14.10 3.50 -8 -6 0 20.80 2.90 -8 -6 0 18.00 2.90 -8 -6 0 22.30 3.50 -8 6 0 26.60 4.40 -8 6 0 20.10 3.30 -8 6 0 18.70 3.60 -8 6 0 21.30 2.90 -8 6 0 19.30 4.70 -8 6 0 20.90 3.40 -8 6 0 12.30 2.90 -8 6 0 18.80 3.30 -8 6 0 19.20 3.00 -8 6 0 16.30 3.00 8 6 0 20.00 3.30 9 -6 0 78.49 5.90 -9 -6 0 81.79 5.40 -9 -6 0 80.99 6.80 -9 -6 0 74.09 5.40 -9 -6 0 80.29 5.80 -9 -6 0 72.39 5.50 -9 -6 0 76.39 5.60 -9 -6 0 96.69 6.80 -9 -6 0 75.39 6.20 9 6 0 74.39 6.10 -9 6 0 77.29 7.80 -9 6 0 83.59 5.70 -9 6 0 74.79 5.20 -9 6 0 75.99 6.10 -9 6 0 81.79 5.80 -9 6 0 75.89 6.20 -9 6 0 85.09 5.90 -9 6 0 87.19 6.80 -9 6 0 71.69 6.30 -10 -6 0 58.09 4.90 -10 -6 0 52.29 6.00 10 -6 0 53.59 5.30 -10 -6 0 59.09 4.60 -10 -6 0 60.19 5.00 -10 -6 0 63.29 5.80 -10 -6 0 54.99 5.80 -10 -6 0 53.49 4.80 -10 -6 0 53.69 4.90 -10 6 0 65.39 5.70 -10 6 0 53.39 6.10 10 6 0 54.99 5.50 -10 6 0 59.09 4.60 -10 6 0 57.69 5.10 -10 6 0 57.39 4.90 -10 6 0 58.89 5.10 -10 6 0 55.09 5.40 -10 6 0 55.89 5.90 -11 -6 0 24.30 3.20 -11 -6 0 26.50 4.10 -11 -6 0 24.20 3.30 -11 -6 0 29.70 4.60 -11 -6 0 26.80 3.70 -11 -6 0 22.10 3.50 -11 -6 0 24.60 3.60 -11 6 0 21.20 3.10 -11 6 0 23.40 3.30 -11 6 0 22.50 3.40 -11 6 0 28.80 3.80 -11 6 0 24.30 4.00 -11 6 0 20.60 4.70 -12 -6 0 7.00 2.20 -12 -6 0 13.90 2.80 -12 -6 0 13.00 2.80 -12 -6 0 10.00 2.50 -12 -6 0 12.40 3.70 -12 -6 0 16.90 2.70 -12 6 0 11.80 2.40 12 6 0 10.10 2.70 -12 6 0 10.50 2.60 -12 6 0 18.10 3.00 -12 6 0 16.50 3.80 -12 6 0 20.10 3.60 -12 6 0 15.20 2.90 13 -6 0 64.29 3.90 -13 -6 0 63.59 4.00 -13 -6 0 57.69 4.10 -13 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0 82.19 5.10 6 7 0 83.39 5.40 -6 7 0 83.19 5.20 -6 7 0 85.79 5.30 7 -7 0 3.50 2.00 -7 -7 0 0.30 1.80 -7 -7 0 2.30 2.00 -7 -7 0 0.20 3.30 -7 -7 0 1.80 1.60 -7 -7 0 1.00 1.60 7 7 0 2.20 1.40 -7 7 0 1.20 1.70 -7 7 0 1.30 1.70 -7 7 0 3.20 2.70 -7 7 0 2.30 1.50 -8 -7 0 25.70 3.60 -8 -7 0 25.10 3.60 -8 -7 0 29.60 3.60 8 -7 0 24.20 3.50 -8 -7 0 29.10 3.80 -8 -7 0 31.50 4.10 -8 -7 0 30.20 3.40 -8 -7 0 27.80 4.40 -8 -7 0 34.60 4.40 -8 7 0 30.40 3.80 -8 7 0 29.30 5.40 -8 7 0 34.60 3.70 -8 7 0 33.00 4.00 -8 7 0 28.70 3.80 -8 7 0 29.70 4.50 -8 7 0 26.30 3.20 8 7 0 21.60 3.40 -8 7 0 29.20 4.10 -8 7 0 25.10 4.20 -8 7 0 36.90 4.00 9 -7 0 0.10 1.80 -9 -7 0 -1.20 2.20 -9 -7 0 1.90 1.80 -9 -7 0 0.30 2.10 -9 -7 0 -0.40 1.80 -9 -7 0 0.30 2.40 -9 -7 0 0.60 2.10 -9 -7 0 1.50 1.80 -9 -7 0 -0.70 2.10 -9 7 0 0.70 2.50 9 7 0 0.50 2.20 -9 7 0 0.20 2.70 -9 7 0 1.40 2.10 -9 7 0 0.50 1.70 -9 7 0 1.20 2.00 -9 7 0 0.20 2.20 -9 7 0 3.30 2.30 -9 7 0 0.30 2.00 -9 7 0 0.10 3.10 -10 -7 0 48.00 5.70 -10 -7 0 41.00 4.20 -10 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8 0 1821.22 65.69 0 8 0 1852.71 66.19 1 -8 0 2504.55 97.49 1 -8 0 2569.54 92.39 -1 -8 0 2676.63 99.99 1 8 0 2667.03 92.59 1 8 0 2505.05 91.99 -1 8 0 2595.94 91.99 -1 8 0 2692.63 92.49 -2 -8 0 193.58 8.60 -2 -8 0 175.28 8.10 2 -8 0 181.38 8.50 -2 -8 0 207.08 14.30 -2 8 0 199.68 8.20 -2 8 0 185.28 8.00 2 8 0 194.28 8.50 -2 8 0 200.58 8.50 3 -8 0 108.09 5.90 -3 -8 0 103.59 5.60 -3 -8 0 110.09 5.40 -3 -8 0 102.29 10.10 -3 8 0 111.09 5.70 -3 8 0 110.49 5.40 3 8 0 89.39 5.40 -3 8 0 105.99 5.20 4 -8 0 171.18 8.70 -4 -8 0 159.28 8.20 -4 -8 0 181.18 14.60 -4 -8 0 175.98 8.20 4 8 0 174.98 8.30 -4 8 0 202.58 8.40 -4 8 0 169.78 8.20 -4 8 0 166.88 7.90 -5 -8 0 30.60 3.40 -5 -8 0 32.70 7.20 5 -8 0 34.20 3.70 -5 -8 0 27.40 3.10 -5 -8 0 36.60 3.30 -5 -8 0 34.70 3.60 -5 8 0 36.80 3.80 -5 8 0 33.50 3.20 -5 8 0 39.90 3.30 -5 8 0 37.60 3.30 5 8 0 31.20 3.00 6 -8 0 0.90 1.70 -6 -8 0 -3.00 2.10 -6 -8 0 0.60 1.20 -6 -8 0 -2.30 0.80 -6 -8 0 -0.40 1.60 -6 -8 0 0.10 1.60 -6 8 0 1.70 1.60 6 8 0 0.60 1.10 -6 8 0 -0.30 1.50 -6 8 0 -0.90 0.90 -6 8 0 2.20 1.70 -7 -8 0 18.20 6.70 -7 -8 0 26.20 3.90 -7 -8 0 23.30 3.30 -7 -8 0 28.40 3.20 -7 -8 0 22.60 3.50 -7 -8 0 29.60 3.40 -7 -8 0 26.80 3.90 -7 -8 0 29.00 3.70 -7 8 0 26.00 3.60 -7 8 0 25.20 3.40 -7 8 0 25.50 4.90 -7 8 0 26.90 3.60 -7 8 0 23.20 3.50 7 8 0 26.50 3.70 -7 8 0 25.40 4.30 -7 8 0 25.80 3.20 -7 8 0 17.80 3.70 -7 8 0 21.50 3.40 -8 -8 0 43.50 4.20 8 -8 0 38.90 4.70 -8 -8 0 43.10 5.10 -8 -8 0 40.70 4.00 -8 -8 0 43.50 4.30 -8 -8 0 38.10 3.70 -8 -8 0 42.60 5.40 -8 -8 0 41.80 4.40 -8 -8 0 42.30 5.10 -8 8 0 47.50 5.00 -8 8 0 41.00 5.40 8 8 0 38.00 4.60 -8 8 0 38.90 4.60 -8 8 0 39.30 4.20 -8 8 0 38.70 4.10 -8 8 0 42.50 5.50 -8 8 0 38.10 3.80 -8 8 0 41.40 4.40 -8 8 0 42.50 4.60 -8 8 0 39.10 4.30 9 -8 0 17.10 3.40 -9 -8 0 18.00 2.90 -9 -8 0 20.50 3.20 -9 -8 0 20.50 3.10 -9 -8 0 17.60 3.30 -9 -8 0 15.60 3.50 -9 -8 0 12.60 3.40 -9 -8 0 17.70 3.20 -9 -8 0 14.00 3.70 -9 8 0 20.80 3.40 -9 8 0 22.70 3.40 -9 8 0 23.00 3.60 9 8 0 15.20 3.40 -9 8 0 20.30 3.70 -9 8 0 16.30 4.60 -9 8 0 20.20 3.80 -9 8 0 19.70 4.00 -9 8 0 16.30 2.70 -10 -8 0 6.20 2.50 -10 -8 0 9.30 2.40 -10 -8 0 9.50 3.50 10 -8 0 10.70 3.20 -10 -8 0 11.10 3.00 -10 -8 0 7.90 3.30 -10 -8 0 8.60 2.50 -10 -8 0 10.40 2.70 -10 -8 0 5.90 2.80 -10 8 0 10.20 3.30 -10 8 0 6.80 2.60 -10 8 0 7.70 2.90 -10 8 0 6.80 2.40 -10 8 0 10.80 2.90 -10 8 0 10.00 2.70 -10 8 0 12.10 3.20 10 8 0 5.70 2.70 -10 8 0 6.80 3.50 -11 -8 0 12.80 2.60 11 -8 0 6.30 1.90 -11 -8 0 12.00 2.70 -11 -8 0 17.60 2.80 -11 -8 0 12.00 3.30 -11 -8 0 11.00 2.70 -11 -8 0 10.00 2.50 -11 8 0 9.90 3.70 -11 8 0 8.30 3.30 -11 8 0 9.90 2.60 -11 8 0 12.30 3.00 -11 8 0 7.20 2.20 -11 8 0 6.00 2.30 -12 -8 0 7.90 2.30 -12 -8 0 13.60 2.50 -12 -8 0 9.40 1.90 -12 -8 0 8.40 2.10 -12 -8 0 8.50 2.30 12 -8 0 9.10 1.90 -12 -8 0 10.50 3.50 -12 8 0 10.40 2.70 12 8 0 10.20 2.50 -12 8 0 11.10 2.30 -12 8 0 7.40 2.20 -12 8 0 12.10 3.30 -12 8 0 9.50 2.30 0 -9 0 3.60 2.10 0 9 0 0.60 0.90 1 -9 0 688.73 31.90 -1 -9 0 692.33 33.70 1 9 0 728.13 26.70 -1 9 0 714.13 26.60 1 9 0 705.03 26.10 -2 -9 0 7.10 3.20 2 -9 0 7.00 1.70 2 9 0 6.70 1.70 2 9 0 6.60 1.40 -2 9 0 8.70 1.80 -3 -9 0 14.90 2.40 -3 -9 0 12.40 2.00 3 -9 0 16.20 2.50 -3 -9 0 15.10 4.70 -3 9 0 15.70 2.20 -3 9 0 17.90 2.50 3 9 0 12.70 2.00 -4 -9 0 2.80 3.40 4 -9 0 2.60 1.70 -4 -9 0 4.00 1.80 -4 -9 0 3.60 1.50 -4 -9 0 4.50 1.70 4 9 0 3.90 1.80 -4 9 0 3.20 1.40 -4 9 0 4.40 2.40 -4 9 0 5.80 1.60 -5 -9 0 471.65 27.90 5 -9 0 426.66 18.60 -5 -9 0 427.96 17.90 -5 -9 0 423.66 18.20 -5 -9 0 431.66 18.60 -5 -9 0 405.86 17.90 -5 9 0 400.06 17.80 -5 9 0 448.16 19.20 5 9 0 478.55 18.30 -5 9 0 432.46 17.90 -6 -9 0 12.50 2.90 -6 -9 0 13.60 2.70 -6 -9 0 12.20 2.80 -6 -9 0 12.70 2.80 -6 -9 0 8.50 5.20 6 -9 0 15.30 3.30 -6 9 0 9.50 2.40 6 9 0 14.20 2.80 -6 9 0 10.50 3.10 -6 9 0 13.30 2.60 -7 -9 0 165.98 8.40 -7 -9 0 172.28 9.00 -7 -9 0 171.38 10.10 -7 -9 0 182.08 17.50 -7 -9 0 162.58 8.70 7 -9 0 167.18 8.20 -7 -9 0 174.48 8.90 -7 -9 0 161.28 9.40 -7 -9 0 166.48 9.50 -7 -9 0 172.88 8.70 -7 9 0 190.18 9.20 -7 9 0 177.88 9.30 -7 9 0 190.08 9.60 -7 9 0 175.08 10.50 -7 9 0 166.98 8.40 -7 9 0 179.28 14.90 -7 9 0 164.88 9.50 -7 9 0 178.78 11.50 -7 9 0 161.18 8.80 -7 9 0 180.18 8.90 7 9 0 190.18 9.70 -8 -9 0 9.20 6.20 -8 -9 0 11.20 2.50 -8 -9 0 13.30 2.90 8 -9 0 10.20 2.80 -8 -9 0 13.40 3.30 -8 -9 0 13.30 3.30 -8 -9 0 11.30 2.80 -8 -9 0 13.40 2.60 -8 -9 0 16.00 3.00 8 -9 0 11.90 2.40 -8 -9 0 14.90 3.50 -8 9 0 14.10 2.80 -8 9 0 14.80 2.60 8 9 0 16.50 3.30 -8 9 0 11.80 3.00 -8 9 0 13.00 3.00 -8 9 0 14.90 3.00 -8 9 0 14.00 3.70 -8 9 0 17.40 3.40 -8 9 0 16.50 3.30 -8 9 0 11.50 3.90 -9 -9 0 147.29 8.20 9 -9 0 150.98 9.00 -9 -9 0 147.89 9.70 -9 -9 0 165.48 8.50 9 -9 0 145.59 7.50 -9 -9 0 153.18 9.30 -9 -9 0 159.78 9.30 -9 -9 0 144.49 8.40 -9 -9 0 148.99 7.80 -9 -9 0 156.08 8.60 -9 9 0 162.28 8.10 -9 9 0 147.99 11.10 -9 9 0 149.29 8.40 -9 9 0 158.68 10.10 9 9 0 162.18 9.10 -9 9 0 143.39 8.20 -9 9 0 160.78 8.70 -9 9 0 165.18 9.40 -9 9 0 148.39 9.00 -10 -9 0 4.50 2.00 -10 -9 0 -4.30 1.90 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