# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_kla0026a _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59.50 H86 Cr2 N4' _chemical_formula_weight 961.32 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' Cr Cr 0.3209 0.6236 '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' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _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, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.960(7) _cell_length_b 12.029(3) _cell_length_c 37.245(8) _cell_angle_alpha 90 _cell_angle_beta 110.265(9) _cell_angle_gamma 90 _cell_volume 10911(5) _cell_formula_units_Z 8 _cell_measurement_temperature 195(2) _cell_measurement_reflns_used 952 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_F_000 4152 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 0.438 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.777278 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'APEX2 (Bruker, 2007)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 195(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 58708 _diffrn_reflns_av_unetI/netI 0.1169 _diffrn_reflns_av_R_equivalents 0.1248 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.675 _diffrn_reflns_theta_max 28.359 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 13590 _reflns_number_gt 7571 _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 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ? ; _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^)+(0.0960P)^2^+0.4633P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 13590 _refine_ls_number_parameters 590 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1397 _refine_ls_R_factor_gt 0.0703 _refine_ls_wR_factor_ref 0.2083 _refine_ls_wR_factor_gt 0.1727 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Cr1 Cr 0.10726(2) 0.33181(5) 0.12639(2) 0.02442(16) Uani 1 1 d . . . . . Cr2 Cr 0.15731(2) 0.39580(5) 0.10337(2) 0.02452(15) Uani 1 1 d . . . . . N1 N 0.14755(11) 0.3124(2) 0.17962(8) 0.0249(6) Uani 1 1 d . . . . . N2 N 0.22605(11) 0.3582(2) 0.14051(8) 0.0263(6) Uani 1 1 d . . . . . N3 N 0.03856(11) 0.3912(2) 0.09459(8) 0.0258(6) Uani 1 1 d . . . . . N4 N 0.12143(11) 0.5231(2) 0.07529(8) 0.0257(6) Uani 1 1 d . . . . . C1 C 0.20308(13) 0.2908(3) 0.19413(10) 0.0288(8) Uani 1 1 d . . . . . H1 H 0.2173 0.2603 0.2192 0.035 Uiso 1 1 calc R U . . . C2 C 0.23866(14) 0.3089(3) 0.17601(10) 0.0291(8) Uani 1 1 d . . . . . H2 H 0.2756 0.2860 0.1886 0.035 Uiso 1 1 calc R U . . . C3 C 0.13971(15) 0.3861(3) 0.23922(10) 0.0323(8) Uani 1 1 d . . . . . C4 C 0.11749(16) 0.3782(3) 0.26831(11) 0.0385(9) Uani 1 1 d . . . . . H4 H 0.1294 0.4286 0.2892 0.046 Uiso 1 1 calc R U . . . C5 C 0.07882(16) 0.2992(3) 0.26754(11) 0.0405(10) Uani 1 1 d . . . . . H5 H 0.0643 0.2950 0.2877 0.049 Uiso 1 1 calc R U . . . C6 C 0.06139(14) 0.2264(3) 0.23736(10) 0.0350(9) Uani 1 1 d . . . . . H6 H 0.0344 0.1725 0.2369 0.042 Uiso 1 1 calc R U . . . C7 C 0.08178(13) 0.2286(3) 0.20727(10) 0.0271(8) Uani 1 1 d . . . . . C8 C 0.12206(13) 0.3093(3) 0.20894(10) 0.0281(8) Uani 1 1 d . . . . . C9 C 0.18200(16) 0.4777(3) 0.24218(11) 0.0387(9) Uani 1 1 d . . . . . H9 H 0.1916 0.4755 0.2184 0.046 Uiso 1 1 calc R U . . . C10 C 0.23469(17) 0.4593(4) 0.27640(12) 0.0561(12) Uani 1 1 d . . . . . H10A H 0.2262 0.4599 0.3001 0.084 Uiso 1 1 calc R U . . . H10B H 0.2609 0.5187 0.2773 0.084 Uiso 1 1 calc R U . . . H10C H 0.2508 0.3873 0.2738 0.084 Uiso 1 1 calc R U . . . C11 C 0.1584(2) 0.5915(4) 0.24480(13) 0.0575(13) Uani 1 1 d . . . . . H11A H 0.1242 0.6020 0.2231 0.086 Uiso 1 1 calc R U . . . H11B H 0.1849 0.6490 0.2443 0.086 Uiso 1 1 calc R U . . . H11C H 0.1508 0.5971 0.2688 0.086 Uiso 1 1 calc R U . . . C12 C 0.06413(14) 0.1431(3) 0.17581(10) 0.0324(8) Uani 1 1 d . . . . . H12 H 0.0626 0.1808 0.1516 0.039 Uiso 1 1 calc R U . . . C13 C 0.10632(18) 0.0496(3) 0.18320(12) 0.0491(11) Uani 1 1 d . . . . . H13A H 0.1425 0.0812 0.1864 0.074 Uiso 1 1 calc R U . . . H13B H 0.0955 -0.0018 0.1614 0.074 Uiso 1 1 calc R U . . . H13C H 0.1081 0.0094 0.2065 0.074 Uiso 1 1 calc R U . . . C14 C 0.00643(17) 0.0968(4) 0.16965(13) 0.0508(12) Uani 1 1 d . . . . . H14A H 0.0066 0.0583 0.1929 0.076 Uiso 1 1 calc R U . . . H14B H -0.0040 0.0445 0.1481 0.076 Uiso 1 1 calc R U . . . H14C H -0.0200 0.1581 0.1640 0.076 Uiso 1 1 calc R U . . . C15 C 0.29606(15) 0.3077(3) 0.11237(11) 0.0350(9) Uani 1 1 d . . . . . C16 C 0.34496(16) 0.3331(4) 0.10625(12) 0.0450(10) Uani 1 1 d . . . . . H16 H 0.3601 0.2808 0.0936 0.054 Uiso 1 1 calc R U . . . C17 C 0.37146(16) 0.4327(4) 0.11829(13) 0.0503(11) Uani 1 1 d . . . . . H17 H 0.4045 0.4488 0.1137 0.060 Uiso 1 1 calc R U . . . C18 C 0.35004(15) 0.5092(4) 0.13700(12) 0.0449(11) Uani 1 1 d . . . . . H18 H 0.3689 0.5773 0.1454 0.054 Uiso 1 1 calc R U . . . C19 C 0.30087(14) 0.4882(3) 0.14390(10) 0.0333(9) Uani 1 1 d . . . . . C20 C 0.27446(13) 0.3860(3) 0.13129(10) 0.0295(8) Uani 1 1 d . . . . . C21 C 0.26861(17) 0.1953(3) 0.09936(12) 0.0437(10) Uani 1 1 d . . . . . H21 H 0.2322 0.1969 0.1030 0.052 Uiso 1 1 calc R U . . . C22 C 0.2578(2) 0.1743(4) 0.05720(15) 0.0720(16) Uani 1 1 d . . . . . H22A H 0.2388 0.2385 0.0422 0.108 Uiso 1 1 calc R U . . . H22B H 0.2348 0.1079 0.0490 0.108 Uiso 1 1 calc R U . . . H22C H 0.2927 0.1628 0.0531 0.108 Uiso 1 1 calc R U . . . C23 C 0.3024(2) 0.0998(4) 0.12429(17) 0.0783(17) Uani 1 1 d . . . . . H23A H 0.3370 0.0913 0.1195 0.117 Uiso 1 1 calc R U . . . H23B H 0.2814 0.0305 0.1178 0.117 Uiso 1 1 calc R U . . . H23C H 0.3102 0.1171 0.1514 0.117 Uiso 1 1 calc R U . . . C24 C 0.27903(16) 0.5730(3) 0.16550(11) 0.0417(10) Uani 1 1 d . . . . . H24 H 0.2388 0.5589 0.1589 0.050 Uiso 1 1 calc R U . . . C25 C 0.28591(18) 0.6921(4) 0.15468(13) 0.0499(11) Uani 1 1 d . . . . . H25A H 0.3250 0.7113 0.1639 0.075 Uiso 1 1 calc R U . . . H25B H 0.2664 0.7419 0.1664 0.075 Uiso 1 1 calc R U . . . H25C H 0.2708 0.7000 0.1268 0.075 Uiso 1 1 calc R U . . . C26 C 0.3064(2) 0.5602(4) 0.20897(12) 0.0654(14) Uani 1 1 d . . . . . H26A H 0.3024 0.4833 0.2163 0.098 Uiso 1 1 calc R U . . . H26B H 0.2888 0.6105 0.2219 0.098 Uiso 1 1 calc R U . . . H26C H 0.3455 0.5787 0.2165 0.098 Uiso 1 1 calc R U . . . C27 C 0.02708(14) 0.4719(3) 0.06692(10) 0.0309(8) Uani 1 1 d . . . . . H27 H -0.0104 0.4848 0.0522 0.037 Uiso 1 1 calc R U . . . C28 C 0.06530(14) 0.5349(3) 0.05894(10) 0.0310(8) Uani 1 1 d . . . . . H28 H 0.0521 0.5922 0.0404 0.037 Uiso 1 1 calc R U . . . C29 C -0.03890(14) 0.2580(3) 0.08002(10) 0.0334(9) Uani 1 1 d . . . . . C30 C -0.08900(15) 0.2293(4) 0.08351(12) 0.0434(10) Uani 1 1 d . . . . . H30 H -0.1089 0.1676 0.0695 0.052 Uiso 1 1 calc R U . . . C31 C -0.11030(16) 0.2885(4) 0.10682(13) 0.0494(12) Uani 1 1 d . . . . . H31 H -0.1448 0.2680 0.1084 0.059 Uiso 1 1 calc R U . . . C32 C -0.08155(16) 0.3780(4) 0.12804(12) 0.0430(10) Uani 1 1 d . . . . . H32 H -0.0962 0.4172 0.1445 0.052 Uiso 1 1 calc R U . . . C33 C -0.03122(14) 0.4111(3) 0.12536(11) 0.0352(9) Uani 1 1 d . . . . . C34 C -0.01071(13) 0.3512(3) 0.10077(10) 0.0310(8) Uani 1 1 d . . . . . C35 C -0.01814(15) 0.1923(3) 0.05289(11) 0.0374(9) Uani 1 1 d . . . . . H35 H 0.0198 0.2186 0.0564 0.045 Uiso 1 1 calc R U . . . C36 C -0.01526(19) 0.0684(4) 0.06158(12) 0.0523(12) Uani 1 1 d . . . . . H36A H -0.0522 0.0405 0.0581 0.078 Uiso 1 1 calc R U . . . H36B H 0.0088 0.0558 0.0881 0.078 Uiso 1 1 calc R U . . . H36C H -0.0006 0.0291 0.0442 0.078 Uiso 1 1 calc R U . . . C37 C -0.0536(2) 0.2115(4) 0.01134(12) 0.0626(13) Uani 1 1 d . . . . . H37A H -0.0914 0.1882 0.0073 0.094 Uiso 1 1 calc R U . . . H37B H -0.0392 0.1680 -0.0053 0.094 Uiso 1 1 calc R U . . . H37C H -0.0533 0.2906 0.0052 0.094 Uiso 1 1 calc R U . . . C38 C -0.00244(16) 0.5116(3) 0.14780(12) 0.0446(10) Uani 1 1 d . . . . . H38 H 0.0361 0.5120 0.1477 0.053 Uiso 1 1 calc R U . . . C39 C -0.0299(2) 0.6181(4) 0.12893(16) 0.0667(15) Uani 1 1 d . . . . . H39A H -0.0280 0.6233 0.1031 0.100 Uiso 1 1 calc R U . . . H39B H -0.0109 0.6820 0.1442 0.100 Uiso 1 1 calc R U . . . H39C H -0.0684 0.6180 0.1273 0.100 Uiso 1 1 calc R U . . . C40 C 0.0004(2) 0.5086(4) 0.18935(13) 0.0592(13) Uani 1 1 d . . . . . H40A H -0.0367 0.5144 0.1903 0.089 Uiso 1 1 calc R U . . . H40B H 0.0227 0.5710 0.2033 0.089 Uiso 1 1 calc R U . . . H40C H 0.0172 0.4385 0.2011 0.089 Uiso 1 1 calc R U . . . C41 C 0.18600(14) 0.6245(3) 0.05030(10) 0.0321(8) Uani 1 1 d . . . . . C42 C 0.21058(17) 0.7253(4) 0.04694(12) 0.0448(10) Uani 1 1 d . . . . . H42 H 0.2340 0.7276 0.0322 0.054 Uiso 1 1 calc R U . . . C43 C 0.20212(18) 0.8210(4) 0.06406(12) 0.0487(11) Uani 1 1 d . . . . . H43 H 0.2187 0.8888 0.0608 0.058 Uiso 1 1 calc R U . . . C44 C 0.16919(17) 0.8173(3) 0.08607(12) 0.0424(10) Uani 1 1 d . . . . . H44 H 0.1639 0.8833 0.0984 0.051 Uiso 1 1 calc R U . . . C45 C 0.14348(15) 0.7207(3) 0.09082(10) 0.0335(8) Uani 1 1 d . . . . . C46 C 0.15132(14) 0.6227(3) 0.07203(10) 0.0282(8) Uani 1 1 d . . . . . C47 C 0.19406(15) 0.5250(3) 0.02747(10) 0.0358(9) Uani 1 1 d . . . . . H47 H 0.1817 0.4568 0.0375 0.043 Uiso 1 1 calc R U . . . C48 C 0.25409(17) 0.5087(4) 0.03120(13) 0.0525(12) Uani 1 1 d . . . . . H48A H 0.2653 0.5687 0.0177 0.079 Uiso 1 1 calc R U . . . H48B H 0.2582 0.4370 0.0200 0.079 Uiso 1 1 calc R U . . . H48C H 0.2772 0.5098 0.0583 0.079 Uiso 1 1 calc R U . . . C49 C 0.15736(18) 0.5397(4) -0.01469(11) 0.0503(11) Uani 1 1 d . . . . . H49A H 0.1190 0.5478 -0.0164 0.075 Uiso 1 1 calc R U . . . H49B H 0.1609 0.4744 -0.0294 0.075 Uiso 1 1 calc R U . . . H49C H 0.1688 0.6063 -0.0251 0.075 Uiso 1 1 calc R U . . . C50 C 0.10848(16) 0.7259(3) 0.11616(11) 0.0400(9) Uani 1 1 d . . . . . H50 H 0.0928 0.6501 0.1165 0.048 Uiso 1 1 calc R U . . . C51 C 0.14303(19) 0.7562(4) 0.15758(12) 0.0558(12) Uani 1 1 d . . . . . H51A H 0.1727 0.7019 0.1676 0.084 Uiso 1 1 calc R U . . . H51B H 0.1197 0.7555 0.1734 0.084 Uiso 1 1 calc R U . . . H51C H 0.1588 0.8305 0.1582 0.084 Uiso 1 1 calc R U . . . C52 C 0.06064(18) 0.8060(4) 0.10015(13) 0.0513(11) Uani 1 1 d . . . . . H52A H 0.0747 0.8806 0.0984 0.077 Uiso 1 1 calc R U . . . H52B H 0.0390 0.8078 0.1171 0.077 Uiso 1 1 calc R U . . . H52C H 0.0373 0.7812 0.0746 0.077 Uiso 1 1 calc R U . . . C53 C 0.12856(15) 0.1858(3) 0.10594(10) 0.0317(8) Uani 1 1 d . . . . . H53A H 0.1639 0.1538 0.1226 0.038 Uiso 1 1 calc R U . . . H53B H 0.0991 0.1290 0.0986 0.038 Uiso 1 1 calc R U . . . C54 C 0.13239(14) 0.2510(3) 0.07372(10) 0.0305(8) Uani 1 1 d . . . . . C55 C 0.11344(16) 0.2207(3) 0.03663(11) 0.0377(9) Uani 1 1 d . . . . . C56 C 0.1026(2) 0.0994(4) 0.02480(13) 0.0585(13) Uani 1 1 d . . . . . H56A H 0.1154 0.0520 0.0476 0.088 Uiso 1 1 calc R U . . . H56B H 0.1222 0.0799 0.0074 0.088 Uiso 1 1 calc R U . . . H56C H 0.0631 0.0881 0.0118 0.088 Uiso 1 1 calc R U . . . C57 C 0.10308(19) 0.2979(4) 0.00347(11) 0.0546(12) Uani 1 1 d . . . . . H57A H 0.0910 0.2551 -0.0204 0.082 Uiso 1 1 calc R U . . . H57B H 0.1370 0.3379 0.0058 0.082 Uiso 1 1 calc R U . . . H57C H 0.0744 0.3512 0.0032 0.082 Uiso 1 1 calc R U . . . C58 C 0.39829(19) 0.2894(4) 0.20762(11) 0.164(9) Uiso 0.5 1 d R U P A -1 H58A H 0.3668 0.3384 0.1958 0.245 Uiso 0.5 1 calc R U P B -1 H58B H 0.3908 0.2417 0.2265 0.245 Uiso 0.5 1 calc R U P C -1 H58C H 0.4046 0.2432 0.1879 0.245 Uiso 0.5 1 calc R U P D -1 C59 C 0.44938(19) 0.3599(4) 0.22744(11) 0.36(3) Uiso 0.5 1 d R U P A -1 H59A H 0.4423 0.4077 0.2469 0.431 Uiso 0.5 1 calc R U P E -1 H59B H 0.4561 0.4092 0.2082 0.431 Uiso 0.5 1 calc R U P F -1 C60 C 0.50102(19) 0.2904(4) 0.24693(11) 0.382(14) Uiso 0.5 1 d R U P A -1 H60A H 0.4942 0.2410 0.2661 0.458 Uiso 0.5 1 calc R U P G -1 H60B H 0.5080 0.2426 0.2275 0.458 Uiso 0.5 1 calc R U P H -1 C61 C 0.55250(19) 0.3599(4) 0.26689(11) 0.34(3) Uiso 0.5 1 d R U P A -1 H61A H 0.5595 0.4092 0.2478 0.414 Uiso 0.5 1 calc R U P I -1 H61B H 0.5456 0.4077 0.2864 0.414 Uiso 0.5 1 calc R U P J -1 C62 C 0.60375(19) 0.2894(4) 0.28622(11) 0.51(4) Uiso 0.5 1 d R . P A -1 H62A H 0.6352 0.3383 0.2984 0.760 Uiso 0.5 1 calc R U P K -1 H62B H 0.6114 0.2432 0.2670 0.760 Uiso 0.5 1 calc R U P L -1 H62C H 0.5975 0.2416 0.3056 0.760 Uiso 0.5 1 calc R U P M -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 Cr1 0.0226(3) 0.0232(3) 0.0256(3) 0.0013(2) 0.0059(2) 0.0008(2) Cr2 0.0246(3) 0.0223(3) 0.0260(3) -0.0003(2) 0.0080(2) 0.0014(2) N1 0.0236(14) 0.0268(17) 0.0239(15) 0.0006(12) 0.0079(11) 0.0001(12) N2 0.0216(14) 0.0258(16) 0.0300(16) -0.0025(13) 0.0072(12) 0.0000(12) N3 0.0231(14) 0.0224(16) 0.0311(16) 0.0038(13) 0.0084(12) 0.0028(12) N4 0.0283(15) 0.0241(16) 0.0254(15) 0.0018(12) 0.0102(12) 0.0005(12) C1 0.0266(17) 0.032(2) 0.0240(18) 0.0013(15) 0.0041(14) -0.0010(15) C2 0.0233(16) 0.030(2) 0.0305(19) 0.0018(16) 0.0054(14) 0.0013(14) C3 0.0334(19) 0.032(2) 0.031(2) -0.0003(17) 0.0108(16) 0.0023(16) C4 0.044(2) 0.045(3) 0.028(2) -0.0026(18) 0.0135(17) 0.0028(19) C5 0.044(2) 0.048(3) 0.034(2) 0.0058(19) 0.0194(18) 0.0056(19) C6 0.0301(19) 0.041(2) 0.038(2) 0.0065(18) 0.0167(17) 0.0006(17) C7 0.0225(16) 0.025(2) 0.034(2) 0.0059(15) 0.0093(14) 0.0044(14) C8 0.0247(17) 0.033(2) 0.0255(18) 0.0055(16) 0.0079(14) 0.0055(15) C9 0.047(2) 0.036(2) 0.034(2) -0.0048(18) 0.0140(18) -0.0107(18) C10 0.051(3) 0.066(3) 0.046(3) -0.007(2) 0.010(2) -0.019(2) C11 0.078(3) 0.042(3) 0.052(3) -0.004(2) 0.022(3) -0.006(2) C12 0.0282(18) 0.035(2) 0.031(2) 0.0011(16) 0.0062(15) -0.0037(16) C13 0.060(3) 0.034(3) 0.050(3) -0.006(2) 0.015(2) 0.007(2) C14 0.045(2) 0.055(3) 0.051(3) 0.003(2) 0.014(2) -0.022(2) C15 0.0309(19) 0.034(2) 0.042(2) 0.0069(18) 0.0147(17) 0.0037(16) C16 0.038(2) 0.050(3) 0.055(3) 0.007(2) 0.025(2) 0.008(2) C17 0.032(2) 0.057(3) 0.070(3) 0.013(2) 0.027(2) 0.001(2) C18 0.030(2) 0.045(3) 0.058(3) 0.009(2) 0.0144(19) -0.0093(18) C19 0.0239(17) 0.038(2) 0.035(2) 0.0054(17) 0.0063(15) -0.0014(16) C20 0.0226(16) 0.033(2) 0.032(2) 0.0031(16) 0.0090(15) 0.0016(15) C21 0.042(2) 0.037(2) 0.060(3) -0.001(2) 0.027(2) 0.0090(18) C22 0.090(4) 0.061(4) 0.081(4) -0.029(3) 0.050(3) -0.015(3) C23 0.064(3) 0.043(3) 0.116(5) 0.018(3) 0.017(3) 0.009(3) C24 0.038(2) 0.043(3) 0.044(2) -0.010(2) 0.0146(19) -0.0129(18) C25 0.049(3) 0.042(3) 0.058(3) -0.009(2) 0.019(2) -0.005(2) C26 0.095(4) 0.059(3) 0.041(3) -0.007(2) 0.022(3) -0.028(3) C27 0.0261(17) 0.031(2) 0.034(2) 0.0053(17) 0.0081(15) 0.0046(15) C28 0.0322(19) 0.028(2) 0.031(2) 0.0086(16) 0.0091(16) 0.0061(15) C29 0.0269(18) 0.034(2) 0.032(2) 0.0141(17) 0.0018(15) 0.0017(16) C30 0.033(2) 0.041(3) 0.052(3) 0.013(2) 0.0083(19) -0.0093(18) C31 0.028(2) 0.061(3) 0.060(3) 0.027(2) 0.015(2) 0.001(2) C32 0.034(2) 0.050(3) 0.050(3) 0.014(2) 0.0203(19) 0.0092(19) C33 0.0298(19) 0.034(2) 0.043(2) 0.0092(18) 0.0146(17) 0.0065(16) C34 0.0209(16) 0.035(2) 0.034(2) 0.0123(17) 0.0053(15) 0.0029(15) C35 0.036(2) 0.032(2) 0.039(2) 0.0009(17) 0.0057(17) -0.0065(17) C36 0.068(3) 0.039(3) 0.044(3) -0.003(2) 0.011(2) -0.010(2) C37 0.068(3) 0.071(4) 0.040(3) 0.015(2) 0.009(2) 0.011(3) C38 0.036(2) 0.041(3) 0.065(3) -0.006(2) 0.028(2) 0.0039(18) C39 0.086(4) 0.043(3) 0.090(4) 0.005(3) 0.055(3) 0.005(3) C40 0.064(3) 0.057(3) 0.062(3) -0.005(2) 0.029(3) 0.012(2) C41 0.0348(19) 0.034(2) 0.0279(19) 0.0029(16) 0.0108(16) -0.0017(16) C42 0.049(2) 0.045(3) 0.045(2) 0.004(2) 0.023(2) -0.007(2) C43 0.060(3) 0.032(3) 0.053(3) 0.005(2) 0.019(2) -0.014(2) C44 0.053(2) 0.026(2) 0.045(2) -0.0024(18) 0.013(2) -0.0025(18) C45 0.040(2) 0.029(2) 0.0288(19) 0.0027(16) 0.0076(16) 0.0015(16) C46 0.0367(19) 0.0214(19) 0.0256(18) 0.0040(15) 0.0096(15) -0.0001(15) C47 0.039(2) 0.038(2) 0.034(2) 0.0021(18) 0.0176(17) 0.0044(17) C48 0.052(3) 0.058(3) 0.054(3) 0.007(2) 0.027(2) 0.010(2) C49 0.060(3) 0.054(3) 0.035(2) 0.003(2) 0.014(2) 0.013(2) C50 0.053(2) 0.024(2) 0.044(2) 0.0007(18) 0.019(2) 0.0054(18) C51 0.069(3) 0.057(3) 0.042(3) 0.002(2) 0.021(2) 0.015(2) C52 0.056(3) 0.046(3) 0.054(3) 0.002(2) 0.022(2) 0.012(2) C53 0.0336(19) 0.027(2) 0.035(2) -0.0049(16) 0.0116(16) -0.0001(15) C54 0.0288(18) 0.027(2) 0.035(2) -0.0050(16) 0.0112(15) 0.0008(15) C55 0.045(2) 0.036(2) 0.032(2) -0.0090(18) 0.0124(17) -0.0053(18) C56 0.083(3) 0.044(3) 0.049(3) -0.019(2) 0.023(3) -0.008(2) C57 0.071(3) 0.055(3) 0.031(2) -0.005(2) 0.009(2) -0.011(2) _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 Cr1 N3 1.905(3) . ? Cr1 N1 1.909(3) . ? Cr1 Cr2 1.9462(8) . ? Cr1 C53 2.065(3) . ? Cr1 C54 2.471(4) . ? Cr2 N2 1.895(3) . ? Cr2 N4 1.906(3) . ? Cr2 C54 2.044(4) . ? N1 C1 1.378(4) . ? N1 C8 1.460(4) . ? N2 C2 1.381(4) . ? N2 C20 1.452(4) . ? N3 C27 1.371(4) . ? N3 C34 1.458(4) . ? N4 C28 1.378(4) . ? N4 C46 1.454(4) . ? C1 C2 1.337(5) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 C4 1.396(5) . ? C3 C8 1.406(5) . ? C3 C9 1.532(5) . ? C4 C5 1.375(5) . ? C4 H4 0.9500 . ? C5 C6 1.372(5) . ? C5 H5 0.9500 . ? C6 C7 1.396(5) . ? C6 H6 0.9500 . ? C7 C8 1.412(5) . ? C7 C12 1.507(5) . ? C9 C11 1.518(6) . ? C9 C10 1.529(6) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.527(5) . ? C12 C14 1.539(5) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.399(5) . ? C15 C20 1.404(5) . ? C15 C21 1.527(5) . ? C16 C17 1.377(6) . ? C16 H16 0.9500 . ? C17 C18 1.382(6) . ? C17 H17 0.9500 . ? C18 C19 1.409(5) . ? C18 H18 0.9500 . ? C19 C20 1.407(5) . ? C19 C24 1.525(5) . ? C21 C22 1.518(6) . ? C21 C23 1.545(6) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.515(6) . ? C24 C26 1.534(6) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.361(5) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.394(5) . ? C29 C34 1.414(5) . ? C29 C35 1.521(5) . ? C30 C31 1.378(6) . ? C30 H30 0.9500 . ? C31 C32 1.390(6) . ? C31 H31 0.9500 . ? C32 C33 1.402(5) . ? C32 H32 0.9500 . ? C33 C34 1.407(5) . ? C33 C38 1.512(6) . ? C35 C37 1.520(5) . ? C35 C36 1.522(5) . ? C35 H35 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.515(6) . ? C38 C40 1.524(6) . ? C38 H38 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.396(5) . ? C41 C46 1.404(5) . ? C41 C47 1.524(5) . ? C42 C43 1.370(6) . ? C42 H42 0.9500 . ? C43 C44 1.375(6) . ? C43 H43 0.9500 . ? C44 C45 1.382(5) . ? C44 H44 0.9500 . ? C45 C46 1.421(5) . ? C45 C50 1.521(5) . ? C47 C48 1.529(5) . ? C47 C49 1.539(5) . ? C47 H47 1.0000 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C52 1.521(5) . ? C50 C51 1.536(6) . ? C50 H50 1.0000 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.466(5) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.346(5) . ? C55 C57 1.493(5) . ? C55 C56 1.523(6) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.5311 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.5331 . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.5331 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.5311 . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 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 N3 Cr1 N1 138.58(12) . . ? N3 Cr1 Cr2 101.64(9) . . ? N1 Cr1 Cr2 107.25(9) . . ? N3 Cr1 C53 113.72(13) . . ? N1 Cr1 C53 99.12(13) . . ? Cr2 Cr1 C53 82.47(10) . . ? N3 Cr1 C54 95.83(12) . . ? N1 Cr1 C54 125.18(12) . . ? Cr2 Cr1 C54 53.53(9) . . ? C53 Cr1 C54 36.34(13) . . ? N2 Cr2 N4 138.58(12) . . ? N2 Cr2 Cr1 100.81(9) . . ? N4 Cr2 Cr1 106.60(9) . . ? N2 Cr2 C54 103.46(13) . . ? N4 Cr2 C54 112.65(13) . . ? Cr1 Cr2 C54 76.49(10) . . ? C1 N1 C8 112.7(3) . . ? C1 N1 Cr1 123.6(2) . . ? C8 N1 Cr1 123.5(2) . . ? C2 N2 C20 112.8(3) . . ? C2 N2 Cr2 130.7(2) . . ? C20 N2 Cr2 116.5(2) . . ? C27 N3 C34 112.2(3) . . ? C27 N3 Cr1 130.2(2) . . ? C34 N3 Cr1 117.5(2) . . ? C28 N4 C46 113.0(3) . . ? C28 N4 Cr2 124.5(2) . . ? C46 N4 Cr2 122.3(2) . . ? C2 C1 N1 125.7(3) . . ? C2 C1 H1 117.2 . . ? N1 C1 H1 117.2 . . ? C1 C2 N2 125.2(3) . . ? C1 C2 H2 117.4 . . ? N2 C2 H2 117.4 . . ? C4 C3 C8 118.0(3) . . ? C4 C3 C9 118.2(3) . . ? C8 C3 C9 123.8(3) . . ? C5 C4 C3 121.7(4) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C6 C5 C4 119.3(4) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C5 C6 C7 122.4(4) . . ? C5 C6 H6 118.8 . . ? C7 C6 H6 118.8 . . ? C6 C7 C8 117.3(3) . . ? C6 C7 C12 120.9(3) . . ? C8 C7 C12 121.7(3) . . ? C3 C8 C7 121.2(3) . . ? C3 C8 N1 118.5(3) . . ? C7 C8 N1 120.3(3) . . ? C11 C9 C10 110.0(4) . . ? C11 C9 C3 111.0(3) . . ? C10 C9 C3 111.6(3) . . ? C11 C9 H9 108.0 . . ? C10 C9 H9 108.0 . . ? C3 C9 H9 108.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 C13 110.9(3) . . ? C7 C12 C14 112.4(3) . . ? C13 C12 C14 111.2(3) . . ? C7 C12 H12 107.4 . . ? C13 C12 H12 107.4 . . ? C14 C12 H12 107.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 118.5(4) . . ? C16 C15 C21 119.5(4) . . ? C20 C15 C21 122.0(3) . . ? C17 C16 C15 121.1(4) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 120.0(4) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C19 121.4(4) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C20 C19 C18 117.6(4) . . ? C20 C19 C24 122.2(3) . . ? C18 C19 C24 120.1(4) . . ? C15 C20 C19 121.4(3) . . ? C15 C20 N2 119.5(3) . . ? C19 C20 N2 118.9(3) . . ? C22 C21 C15 112.0(4) . . ? C22 C21 C23 111.2(4) . . ? C15 C21 C23 111.2(4) . . ? C22 C21 H21 107.4 . . ? C15 C21 H21 107.4 . . ? C23 C21 H21 107.4 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C19 113.1(3) . . ? C25 C24 C26 108.8(3) . . ? C19 C24 C26 111.7(4) . . ? C25 C24 H24 107.7 . . ? C19 C24 H24 107.7 . . ? C26 C24 H24 107.7 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 N3 125.0(3) . . ? C28 C27 H27 117.5 . . ? N3 C27 H27 117.5 . . ? C27 C28 N4 125.8(3) . . ? C27 C28 H28 117.1 . . ? N4 C28 H28 117.1 . . ? C30 C29 C34 117.9(4) . . ? C30 C29 C35 119.4(4) . . ? C34 C29 C35 122.7(3) . . ? C31 C30 C29 121.4(4) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C30 C31 C32 120.3(4) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C33 120.6(4) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C32 C33 C34 118.2(4) . . ? C32 C33 C38 118.8(3) . . ? C34 C33 C38 122.9(3) . . ? C33 C34 C29 121.4(3) . . ? C33 C34 N3 118.9(3) . . ? C29 C34 N3 119.5(3) . . ? C37 C35 C29 111.6(3) . . ? C37 C35 C36 109.5(3) . . ? C29 C35 C36 111.7(3) . . ? C37 C35 H35 108.0 . . ? C29 C35 H35 108.0 . . ? C36 C35 H35 108.0 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 C39 110.9(4) . . ? C33 C38 C40 112.5(4) . . ? C39 C38 C40 109.9(4) . . ? C33 C38 H38 107.7 . . ? C39 C38 H38 107.7 . . ? C40 C38 H38 107.7 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C46 118.0(4) . . ? C42 C41 C47 118.5(3) . . ? C46 C41 C47 123.3(3) . . ? C43 C42 C41 122.4(4) . . ? C43 C42 H42 118.8 . . ? C41 C42 H42 118.8 . . ? C42 C43 C44 118.9(4) . . ? C42 C43 H43 120.5 . . ? C44 C43 H43 120.5 . . ? C43 C44 C45 122.1(4) . . ? C43 C44 H44 119.0 . . ? C45 C44 H44 119.0 . . ? C44 C45 C46 118.5(3) . . ? C44 C45 C50 117.6(4) . . ? C46 C45 C50 123.9(3) . . ? C41 C46 C45 120.1(3) . . ? C41 C46 N4 121.8(3) . . ? C45 C46 N4 118.1(3) . . ? C41 C47 C48 112.5(3) . . ? C41 C47 C49 108.8(3) . . ? C48 C47 C49 111.0(3) . . ? C41 C47 H47 108.1 . . ? C48 C47 H47 108.1 . . ? C49 C47 H47 108.1 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C52 C50 C45 111.4(3) . . ? C52 C50 C51 110.9(3) . . ? C45 C50 C51 111.5(3) . . ? C52 C50 H50 107.6 . . ? C45 C50 H50 107.6 . . ? C51 C50 H50 107.6 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 Cr1 87.1(2) . . ? C54 C53 H53A 114.1 . . ? Cr1 C53 H53A 114.1 . . ? C54 C53 H53B 114.1 . . ? Cr1 C53 H53B 114.1 . . ? H53A C53 H53B 111.3 . . ? C55 C54 C53 126.2(3) . . ? C55 C54 Cr2 136.1(3) . . ? C53 C54 Cr2 96.5(2) . . ? C55 C54 Cr1 144.9(3) . . ? C53 C54 Cr1 56.57(18) . . ? Cr2 C54 Cr1 49.98(8) . . ? C54 C55 C57 125.3(4) . . ? C54 C55 C56 121.5(4) . . ? C57 C55 C56 113.2(3) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C59 C58 H58A 109.5 . . ? C59 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C59 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C58 C59 C60 113.3 . . ? C58 C59 H59A 108.9 . . ? C60 C59 H59A 108.9 . . ? C58 C59 H59B 108.9 . . ? C60 C59 H59B 108.9 . . ? H59A C59 H59B 107.7 . . ? C61 C60 C59 113.8 . . ? C61 C60 H60A 108.8 . . ? C59 C60 H60A 108.8 . . ? C61 C60 H60B 108.8 . . ? C59 C60 H60B 108.8 . . ? H60A C60 H60B 107.7 . . ? C62 C61 C60 113.3 . . ? C62 C61 H61A 108.9 . . ? C60 C61 H61A 108.9 . . ? C62 C61 H61B 108.9 . . ? C60 C61 H61B 108.9 . . ? H61A C61 H61B 107.7 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? _refine_diff_density_max 1.116 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.086 _shelxl_version_number 2013-2 _shelx_res_file ; TITL kla0026a in C2/c CELL 0.71073 25.9600 12.0290 37.2450 90.000 110.265 90.000 ZERR 8 0.0070 0.0030 0.0080 0.000 0.009 0.000 LATT 7 SYMM - X , Y , 0.50000 - Z SFAC C H Cr N UNIT 476 688 16 32 L.S. 20 ACTA 50 BOND $H FMAP 2 PLAN 20 TEMP -78 OMIT 0 0 2 OMIT 2 0 0 WGHT 0.096000 0.463300 FVAR 0.13722 CR1 3 0.107256 0.331808 0.126393 11.00000 0.02259 0.02319 = 0.02558 0.00129 0.00593 0.00079 CR2 3 0.157313 0.395798 0.103375 11.00000 0.02460 0.02231 = 0.02604 -0.00034 0.00799 0.00137 N1 4 0.147552 0.312386 0.179622 11.00000 0.02365 0.02678 = 0.02391 0.00058 0.00787 0.00012 N2 4 0.226045 0.358197 0.140512 11.00000 0.02164 0.02577 = 0.02998 -0.00245 0.00720 -0.00003 N3 4 0.038561 0.391211 0.094591 11.00000 0.02306 0.02240 = 0.03113 0.00380 0.00843 0.00282 N4 4 0.121430 0.523147 0.075288 11.00000 0.02826 0.02407 = 0.02545 0.00177 0.01024 0.00050 C1 1 0.203075 0.290761 0.194126 11.00000 0.02659 0.03206 = 0.02398 0.00129 0.00409 -0.00099 AFIX 43 H1 2 0.217325 0.260332 0.219181 11.00000 -1.20000 AFIX 0 C2 1 0.238656 0.308873 0.176008 11.00000 0.02326 0.03040 = 0.03053 0.00177 0.00535 0.00133 AFIX 43 H2 2 0.275573 0.285974 0.188560 11.00000 -1.20000 AFIX 0 C3 1 0.139714 0.386106 0.239219 11.00000 0.03344 0.03177 = 0.03139 -0.00028 0.01085 0.00229 C4 1 0.117486 0.378157 0.268305 11.00000 0.04421 0.04464 = 0.02760 -0.00261 0.01348 0.00279 AFIX 43 H4 2 0.129385 0.428646 0.289183 11.00000 -1.20000 AFIX 0 C5 1 0.078818 0.299170 0.267536 11.00000 0.04360 0.04804 = 0.03445 0.00578 0.01945 0.00555 AFIX 43 H5 2 0.064333 0.295044 0.287685 11.00000 -1.20000 AFIX 0 C6 1 0.061391 0.226410 0.237362 11.00000 0.03011 0.04058 = 0.03821 0.00651 0.01667 0.00059 AFIX 43 H6 2 0.034440 0.172502 0.236929 11.00000 -1.20000 AFIX 0 C7 1 0.081782 0.228629 0.207270 11.00000 0.02250 0.02494 = 0.03358 0.00588 0.00929 0.00440 C8 1 0.122056 0.309304 0.208942 11.00000 0.02475 0.03349 = 0.02551 0.00547 0.00794 0.00552 C9 1 0.181997 0.477657 0.242176 11.00000 0.04672 0.03590 = 0.03352 -0.00483 0.01398 -0.01072 AFIX 13 H9 2 0.191571 0.475541 0.218387 11.00000 -1.20000 AFIX 0 C10 1 0.234693 0.459263 0.276401 11.00000 0.05093 0.06574 = 0.04628 -0.00738 0.01018 -0.01883 AFIX 137 H10A 2 0.226185 0.459933 0.300063 11.00000 -1.50000 H10B 2 0.260917 0.518731 0.277305 11.00000 -1.50000 H10C 2 0.250757 0.387333 0.273773 11.00000 -1.50000 AFIX 0 C11 1 0.158383 0.591531 0.244795 11.00000 0.07789 0.04198 = 0.05246 -0.00420 0.02224 -0.00562 AFIX 137 H11A 2 0.124208 0.602008 0.223071 11.00000 -1.50000 H11B 2 0.184869 0.648986 0.244256 11.00000 -1.50000 H11C 2 0.150823 0.597134 0.268750 11.00000 -1.50000 AFIX 0 C12 1 0.064135 0.143052 0.175810 11.00000 0.02823 0.03530 = 0.03067 0.00109 0.00621 -0.00370 AFIX 13 H12 2 0.062637 0.180824 0.151551 11.00000 -1.20000 AFIX 0 C13 1 0.106322 0.049594 0.183197 11.00000 0.06031 0.03400 = 0.04962 -0.00590 0.01463 0.00688 AFIX 137 H13A 2 0.142456 0.081152 0.186421 11.00000 -1.50000 H13B 2 0.095512 -0.001782 0.161429 11.00000 -1.50000 H13C 2 0.108082 0.009414 0.206482 11.00000 -1.50000 AFIX 0 C14 1 0.006433 0.096769 0.169648 11.00000 0.04500 0.05459 = 0.05084 0.00306 0.01410 -0.02171 AFIX 137 H14A 2 0.006580 0.058264 0.192871 11.00000 -1.50000 H14B 2 -0.003998 0.044462 0.148145 11.00000 -1.50000 H14C 2 -0.020026 0.158108 0.164004 11.00000 -1.50000 AFIX 0 C15 1 0.296062 0.307711 0.112375 11.00000 0.03092 0.03397 = 0.04172 0.00695 0.01466 0.00374 C16 1 0.344955 0.333141 0.106250 11.00000 0.03802 0.04954 = 0.05484 0.00702 0.02531 0.00766 AFIX 43 H16 2 0.360115 0.280832 0.093572 11.00000 -1.20000 AFIX 0 C17 1 0.371464 0.432698 0.118286 11.00000 0.03151 0.05673 = 0.06982 0.01275 0.02670 0.00051 AFIX 43 H17 2 0.404494 0.448826 0.113729 11.00000 -1.20000 AFIX 0 C18 1 0.350043 0.509204 0.137000 11.00000 0.03042 0.04511 = 0.05843 0.00875 0.01445 -0.00933 AFIX 43 H18 2 0.368863 0.577349 0.145391 11.00000 -1.20000 AFIX 0 C19 1 0.300870 0.488243 0.143895 11.00000 0.02394 0.03847 = 0.03460 0.00537 0.00633 -0.00137 C20 1 0.274457 0.386006 0.131288 11.00000 0.02259 0.03340 = 0.03215 0.00309 0.00904 0.00158 C21 1 0.268609 0.195319 0.099361 11.00000 0.04164 0.03705 = 0.05987 -0.00118 0.02715 0.00895 AFIX 13 H21 2 0.232223 0.196927 0.103010 11.00000 -1.20000 AFIX 0 C22 1 0.257783 0.174267 0.057195 11.00000 0.08999 0.06114 = 0.08116 -0.02910 0.05040 -0.01526 AFIX 137 H22A 2 0.238796 0.238505 0.042230 11.00000 -1.50000 H22B 2 0.234818 0.107877 0.048988 11.00000 -1.50000 H22C 2 0.292746 0.162828 0.053143 11.00000 -1.50000 AFIX 0 C23 1 0.302372 0.099835 0.124290 11.00000 0.06433 0.04324 = 0.11625 0.01780 0.01708 0.00921 AFIX 137 H23A 2 0.336974 0.091315 0.119496 11.00000 -1.50000 H23B 2 0.281358 0.030492 0.117812 11.00000 -1.50000 H23C 2 0.310205 0.117117 0.151380 11.00000 -1.50000 AFIX 0 C24 1 0.279032 0.573034 0.165498 11.00000 0.03787 0.04339 = 0.04408 -0.00997 0.01458 -0.01288 AFIX 13 H24 2 0.238846 0.558938 0.158913 11.00000 -1.20000 AFIX 0 C25 1 0.285911 0.692085 0.154681 11.00000 0.04903 0.04236 = 0.05831 -0.00866 0.01856 -0.00528 AFIX 137 H25A 2 0.325014 0.711306 0.163878 11.00000 -1.50000 H25B 2 0.266366 0.741942 0.166387 11.00000 -1.50000 H25C 2 0.270801 0.700022 0.126782 11.00000 -1.50000 AFIX 0 C26 1 0.306388 0.560234 0.208965 11.00000 0.09528 0.05892 = 0.04116 -0.00681 0.02249 -0.02824 AFIX 137 H26A 2 0.302395 0.483327 0.216281 11.00000 -1.50000 H26B 2 0.288776 0.610509 0.221920 11.00000 -1.50000 H26C 2 0.345471 0.578689 0.216467 11.00000 -1.50000 AFIX 0 C27 1 0.027081 0.471909 0.066916 11.00000 0.02610 0.03074 = 0.03408 0.00533 0.00805 0.00464 AFIX 43 H27 2 -0.010415 0.484795 0.052191 11.00000 -1.20000 AFIX 0 C28 1 0.065301 0.534933 0.058938 11.00000 0.03221 0.02837 = 0.03089 0.00863 0.00911 0.00607 AFIX 43 H28 2 0.052114 0.592178 0.040443 11.00000 -1.20000 AFIX 0 C29 1 -0.038904 0.257964 0.080025 11.00000 0.02689 0.03405 = 0.03249 0.01407 0.00179 0.00168 C30 1 -0.089002 0.229300 0.083508 11.00000 0.03275 0.04079 = 0.05176 0.01280 0.00827 -0.00932 AFIX 43 H30 2 -0.108887 0.167614 0.069508 11.00000 -1.20000 AFIX 0 C31 1 -0.110302 0.288496 0.106815 11.00000 0.02806 0.06050 = 0.05985 0.02689 0.01546 0.00088 AFIX 43 H31 2 -0.144798 0.268025 0.108393 11.00000 -1.20000 AFIX 0 C32 1 -0.081553 0.378040 0.128035 11.00000 0.03420 0.04957 = 0.04961 0.01354 0.02025 0.00923 AFIX 43 H32 2 -0.096151 0.417186 0.144502 11.00000 -1.20000 AFIX 0 C33 1 -0.031217 0.411104 0.125357 11.00000 0.02981 0.03435 = 0.04299 0.00921 0.01456 0.00647 C34 1 -0.010715 0.351176 0.100773 11.00000 0.02093 0.03459 = 0.03421 0.01235 0.00529 0.00294 C35 1 -0.018137 0.192309 0.052890 11.00000 0.03609 0.03155 = 0.03895 0.00090 0.00573 -0.00650 AFIX 13 H35 2 0.019848 0.218622 0.056420 11.00000 -1.20000 AFIX 0 C36 1 -0.015261 0.068378 0.061584 11.00000 0.06798 0.03895 = 0.04358 -0.00280 0.01136 -0.01024 AFIX 137 H36A 2 -0.052158 0.040485 0.058074 11.00000 -1.50000 H36B 2 0.008780 0.055754 0.088091 11.00000 -1.50000 H36C 2 -0.000552 0.029089 0.044187 11.00000 -1.50000 AFIX 0 C37 1 -0.053648 0.211475 0.011338 11.00000 0.06826 0.07105 = 0.04028 0.01460 0.00852 0.01054 AFIX 137 H37A 2 -0.091404 0.188157 0.007340 11.00000 -1.50000 H37B 2 -0.039187 0.168007 -0.005316 11.00000 -1.50000 H37C 2 -0.053253 0.290619 0.005198 11.00000 -1.50000 AFIX 0 C38 1 -0.002437 0.511627 0.147805 11.00000 0.03645 0.04067 = 0.06502 -0.00568 0.02833 0.00385 AFIX 13 H38 2 0.036056 0.511964 0.147749 11.00000 -1.20000 AFIX 0 C39 1 -0.029858 0.618142 0.128930 11.00000 0.08617 0.04321 = 0.08969 0.00513 0.05455 0.00533 AFIX 137 H39A 2 -0.027989 0.623296 0.103150 11.00000 -1.50000 H39B 2 -0.010945 0.681996 0.144178 11.00000 -1.50000 H39C 2 -0.068373 0.618025 0.127254 11.00000 -1.50000 AFIX 0 C40 1 0.000432 0.508610 0.189350 11.00000 0.06381 0.05725 = 0.06238 -0.00492 0.02937 0.01239 AFIX 137 H40A 2 -0.036717 0.514356 0.190323 11.00000 -1.50000 H40B 2 0.022698 0.571037 0.203320 11.00000 -1.50000 H40C 2 0.017161 0.438497 0.201128 11.00000 -1.50000 AFIX 0 C41 1 0.185999 0.624461 0.050297 11.00000 0.03482 0.03354 = 0.02792 0.00286 0.01082 -0.00169 C42 1 0.210583 0.725289 0.046935 11.00000 0.04934 0.04546 = 0.04484 0.00404 0.02296 -0.00718 AFIX 43 H42 2 0.234043 0.727619 0.032234 11.00000 -1.20000 AFIX 0 C43 1 0.202122 0.821016 0.064058 11.00000 0.06044 0.03231 = 0.05274 0.00527 0.01893 -0.01430 AFIX 43 H43 2 0.218736 0.888807 0.060774 11.00000 -1.20000 AFIX 0 C44 1 0.169189 0.817326 0.086069 11.00000 0.05337 0.02564 = 0.04503 -0.00240 0.01313 -0.00250 AFIX 43 H44 2 0.163939 0.883291 0.098400 11.00000 -1.20000 AFIX 0 C45 1 0.143478 0.720661 0.090821 11.00000 0.03966 0.02879 = 0.02882 0.00272 0.00759 0.00147 C46 1 0.151316 0.622684 0.072035 11.00000 0.03667 0.02138 = 0.02555 0.00401 0.00955 -0.00009 C47 1 0.194060 0.524986 0.027469 11.00000 0.03916 0.03825 = 0.03377 0.00209 0.01758 0.00437 AFIX 13 H47 2 0.181667 0.456804 0.037528 11.00000 -1.20000 AFIX 0 C48 1 0.254092 0.508678 0.031200 11.00000 0.05234 0.05757 = 0.05391 0.00742 0.02660 0.01001 AFIX 137 H48A 2 0.265302 0.568721 0.017703 11.00000 -1.50000 H48B 2 0.258242 0.437027 0.019977 11.00000 -1.50000 H48C 2 0.277221 0.509830 0.058313 11.00000 -1.50000 AFIX 0 C49 1 0.157361 0.539718 -0.014688 11.00000 0.06025 0.05363 = 0.03522 0.00291 0.01419 0.01282 AFIX 137 H49A 2 0.119022 0.547812 -0.016388 11.00000 -1.50000 H49B 2 0.160902 0.474424 -0.029398 11.00000 -1.50000 H49C 2 0.168788 0.606299 -0.025124 11.00000 -1.50000 AFIX 0 C50 1 0.108476 0.725915 0.116162 11.00000 0.05343 0.02354 = 0.04428 0.00066 0.01851 0.00541 AFIX 13 H50 2 0.092824 0.650120 0.116495 11.00000 -1.20000 AFIX 0 C51 1 0.143033 0.756209 0.157581 11.00000 0.06921 0.05743 = 0.04225 0.00196 0.02112 0.01488 AFIX 137 H51A 2 0.172701 0.701889 0.167615 11.00000 -1.50000 H51B 2 0.119684 0.755531 0.173373 11.00000 -1.50000 H51C 2 0.158766 0.830539 0.158185 11.00000 -1.50000 AFIX 0 C52 1 0.060643 0.806006 0.100146 11.00000 0.05579 0.04599 = 0.05428 0.00186 0.02165 0.01182 AFIX 137 H52A 2 0.074740 0.880612 0.098372 11.00000 -1.50000 H52B 2 0.039034 0.807846 0.117117 11.00000 -1.50000 H52C 2 0.037333 0.781172 0.074626 11.00000 -1.50000 AFIX 0 C53 1 0.128556 0.185768 0.105943 11.00000 0.03356 0.02680 = 0.03455 -0.00492 0.01155 -0.00010 AFIX 23 H53A 2 0.163907 0.153758 0.122562 11.00000 -1.20000 H53B 2 0.099136 0.128975 0.098629 11.00000 -1.20000 AFIX 0 C54 1 0.132395 0.251028 0.073721 11.00000 0.02885 0.02734 = 0.03542 -0.00498 0.01117 0.00079 C55 1 0.113443 0.220717 0.036634 11.00000 0.04467 0.03592 = 0.03176 -0.00905 0.01240 -0.00535 C56 1 0.102561 0.099359 0.024799 11.00000 0.08276 0.04414 = 0.04896 -0.01922 0.02344 -0.00847 AFIX 137 H56A 2 0.115434 0.051984 0.047588 11.00000 -1.50000 H56B 2 0.122177 0.079896 0.007436 11.00000 -1.50000 H56C 2 0.063069 0.088098 0.011755 11.00000 -1.50000 AFIX 0 C57 1 0.103083 0.297863 0.003468 11.00000 0.07081 0.05499 = 0.03128 -0.00546 0.00919 -0.01147 AFIX 33 H57A 2 0.091041 0.255062 -0.020398 11.00000 -1.50000 H57B 2 0.136963 0.337926 0.005801 11.00000 -1.50000 H57C 2 0.074446 0.351237 0.003231 11.00000 -1.50000 AFIX 3 SIMU C58 C59 C60 C61 C61 RIGU C58 C59 C60 C61 C61 PART -1 C58 1 0.398288 0.289439 0.207624 10.50000 0.16353 AFIX 33 H58A 2 0.366774 0.338354 0.195756 10.50000 -1.50000 H58B 2 0.390764 0.241652 0.226542 10.50000 -1.50000 H58C 2 0.404628 0.243197 0.187891 10.50000 -1.50000 AFIX 3 C59 1 0.449375 0.359921 0.227438 10.50000 0.35940 AFIX 23 H59A 2 0.442279 0.407670 0.246871 10.50000 -1.20000 H59B 2 0.456132 0.409217 0.208247 10.50000 -1.20000 AFIX 3 C60 1 0.501020 0.290353 0.246927 10.50000 0.38186 AFIX 23 H60A 2 0.494155 0.241016 0.266065 10.50000 -1.20000 H60B 2 0.508002 0.242562 0.227459 10.50000 -1.20000 AFIX 3 C61 1 0.552498 0.359912 0.266887 10.50000 0.34460 AFIX 23 H61A 2 0.559479 0.409209 0.247782 10.50000 -1.20000 H61B 2 0.545626 0.407661 0.286406 10.50000 -1.20000 AFIX 3 C62 1 0.603753 0.289421 0.286223 10.50000 0.50663 AFIX 33 H62A 2 0.635151 0.338331 0.298421 10.50000 -1.50000 H62B 2 0.611389 0.243180 0.266986 10.50000 -1.50000 H62C 2 0.597526 0.241632 0.305637 10.50000 -1.50000 AFIX 0 HKLF 4 1 1.0000 -2.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 REM kla0026a in C2/c REM R1 = 0.0703 for 7571 Fo > 4sig(Fo) and 0.1397 for all 13590 data REM 590 parameters refined using 3 restraints END WGHT 0.0952 0.1212 REM Highest difference peak 1.116, deepest hole -0.587, 1-sigma level 0.086 Q1 1 0.4225 0.2815 0.2100 11.00000 0.05 1.12 Q2 1 0.5962 0.3355 0.2720 11.00000 0.05 1.00 Q3 1 0.5000 0.3844 0.2500 10.50000 0.05 0.95 Q4 1 0.5028 0.3242 0.2252 11.00000 0.05 0.90 Q5 1 0.4554 0.2810 0.2281 11.00000 0.05 0.84 Q6 1 0.1199 0.3839 0.1079 11.00000 0.05 0.61 Q7 1 0.1389 0.3436 0.1175 11.00000 0.05 0.59 Q8 1 0.1990 0.3912 0.1217 11.00000 0.05 0.48 Q9 1 0.5525 0.3341 0.2535 11.00000 0.05 0.47 Q10 1 0.1015 0.3860 0.0069 11.00000 0.05 0.45 Q11 1 0.0524 0.2746 -0.0160 11.00000 0.05 0.41 Q12 1 0.0687 0.3438 0.1228 11.00000 0.05 0.41 Q13 1 0.1307 0.3241 0.1599 11.00000 0.05 0.37 Q14 1 0.1897 0.5673 0.0395 11.00000 0.05 0.35 Q15 1 0.0186 0.3657 0.1002 11.00000 0.05 0.35 Q16 1 0.1305 0.3206 0.0826 11.00000 0.05 0.34 Q17 1 0.5514 0.2778 0.2359 11.00000 0.05 0.34 Q18 1 0.1341 0.2752 -0.0116 11.00000 0.05 0.33 Q19 1 0.0895 0.2914 0.2038 11.00000 0.05 0.32 Q20 1 -0.0287 0.3834 0.1141 11.00000 0.05 0.32 ; _shelx_res_checksum 60442 _shelx_hkl_file ; -1 -1 0 607.04 32.93 1 1 0 604.51 32.89 1 1 0 610.20 35.74 1 1 0 588.96 35.77 -2 -2 0 708.78 38.45 2 2 0 676.21 42.47 2 2 0 689.64 42.49 3 3 0 161.53 14.29 -3 -3 0 163.61 11.02 3 3 0 148.93 13.61 4 4 0 305.72 23.03 4 4 0 310.36 23.67 -4 -4 0 267.79 18.28 -5 -5 0 12.77 3.90 5 5 0 21.98 6.94 5 5 0 25.47 7.29 6 6 0 322.09 25.59 -6 -6 0 275.42 19.09 6 6 0 218.71 25.55 7 7 0 375.04 34.47 -7 -7 0 437.39 27.70 7 7 0 419.04 34.37 8 8 0 29.97 10.84 8 8 0 32.53 10.29 -8 -8 0 61.92 8.95 9 9 0 5.35 9.30 9 9 0 0.22 8.23 10 10 0 211.12 29.44 10 10 0 173.24 29.01 11 11 0 15.58 12.11 11 11 0 21.75 13.76 12 12 0 -0.95 12.50 12 12 0 4.05 12.80 13 13 0 84.31 23.78 14 14 0 19.44 18.81 13 14 0 -0.18 16.28 12 13 0 75.95 21.25 12 13 0 74.20 20.61 11 12 0 82.29 20.01 11 12 0 84.68 19.92 10 11 0 25.74 12.67 10 11 0 22.60 10.92 9 10 0 390.59 40.61 9 10 0 380.97 38.65 8 9 0 2.75 7.22 8 9 0 3.21 7.60 -8 -9 0 5.55 4.92 -7 -8 0 22.15 5.88 7 8 0 4.22 6.56 7 8 0 14.33 7.68 6 7 0 247.81 25.95 -6 -7 0 250.97 18.89 6 7 0 238.30 24.99 5 6 0 504.58 36.09 -5 -6 0 484.46 30.17 5 6 0 419.08 34.47 4 5 0 290.08 24.15 4 5 0 295.05 24.49 -4 -5 0 325.68 20.75 3 4 0 97.00 11.71 -3 -4 0 96.65 8.93 3 4 0 88.15 11.23 2 3 0 3264.11 188.80 2 3 0 3360.14 187.81 -2 -3 0 3216.85 176.21 1 2 0 97.87 8.48 -1 -2 0 110.82 7.90 1 2 0 118.57 9.00 0 1 0 -0.26 0.56 0 -1 0 -0.75 0.45 0 1 0 1.97 0.99 1 0 0 2274.44 138.92 -1 0 0 2433.95 140.25 1 0 0 2586.94 132.17 -1 0 0 2533.35 131.88 -2 -1 0 2254.21 127.17 -2 -1 0 2071.88 118.16 2 1 0 2307.14 126.47 2 1 0 2196.32 118.37 -3 -2 0 50.11 7.68 -3 -2 0 58.28 4.50 3 2 0 45.10 7.73 4 3 0 26.37 6.04 -4 -3 0 26.16 3.65 4 3 0 24.02 6.31 5 4 0 234.27 20.41 5 4 0 217.66 22.41 -5 -4 0 247.10 15.57 -6 -5 0 205.67 14.41 6 5 0 226.27 23.76 6 5 0 207.94 21.70 7 6 0 9.46 6.49 -7 -6 0 -2.06 2.74 7 6 0 -5.68 5.23 8 7 0 427.94 38.01 -8 -7 0 430.12 27.72 8 7 0 422.23 36.08 9 8 0 7.18 8.74 9 8 0 -2.30 7.02 10 9 0 120.26 22.45 10 9 0 135.13 22.76 11 10 0 35.59 15.29 11 10 0 -0.29 10.30 12 11 0 -0.34 12.34 12 11 0 11.15 12.11 13 12 0 22.68 15.93 14 13 0 18.53 17.74 12 14 0 35.35 16.88 12 14 0 35.95 18.21 11 13 0 12.47 11.66 11 13 0 23.98 12.65 10 12 0 34.84 14.24 10 12 0 44.81 15.21 9 11 0 96.49 19.23 -9 -11 0 65.31 12.68 9 11 0 97.65 18.85 -8 -10 0 15.03 6.14 8 10 0 2.25 8.22 8 10 0 6.37 8.31 7 9 0 593.56 47.71 -7 -9 0 659.19 41.82 7 9 0 608.56 47.38 6 8 0 290.34 26.38 -6 -8 0 306.38 22.70 6 8 0 267.10 28.10 5 7 0 466.25 35.89 -5 -7 0 491.50 31.74 5 7 0 462.13 36.21 4 6 0 5.80 4.33 -4 -6 0 2.69 2.93 4 6 0 3.64 4.95 -3 -5 0 78.59 8.98 3 5 0 86.27 11.57 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19.38 -6 2 -5 225.13 26.23 -7 1 -5 17.71 7.88 7 -1 5 13.70 4.95 7 -1 5 10.86 6.55 8 0 5 423.14 29.43 8 0 5 444.50 37.24 -8 0 -5 426.21 36.65 -9 -1 -5 14.92 7.98 9 1 5 -6.43 5.21 10 2 5 33.56 13.70 -10 -2 -5 48.86 13.17 -11 -3 -5 11.45 10.66 11 3 5 23.14 12.14 -12 -4 -5 27.02 12.14 12 4 5 0.09 9.73 -13 -5 -5 29.14 15.16 13 5 5 78.60 22.39 14 6 5 -1.14 13.30 15 7 5 10.77 14.36 16 8 5 41.63 23.87 9 18 -5 -4.78 18.50 8 17 -5 7.19 15.56 -8 -17 5 11.12 11.53 -7 -16 5 44.34 15.39 7 16 -5 50.81 18.64 -6 -15 5 51.51 14.96 6 15 -5 22.05 14.67 -5 -14 5 12.59 8.79 5 14 -5 -12.10 9.78 -4 -13 5 24.20 9.12 -4 -13 5 11.87 8.78 4 13 -5 3.39 10.25 -3 -12 5 -1.71 5.44 3 12 -5 8.92 6.14 3 12 -5 8.66 11.00 -3 -12 5 -7.77 5.40 2 11 -5 238.16 32.29 -2 -11 5 197.15 25.76 -2 -11 5 236.27 23.62 2 11 -5 244.81 21.37 1 10 -5 127.34 22.70 -1 -10 5 139.04 20.93 1 10 -5 156.84 16.43 -1 -10 5 152.64 17.45 0 9 -5 30.75 7.26 0 -9 5 26.74 9.09 0 9 -5 50.99 13.11 1 -8 5 252.46 25.52 -1 8 -5 259.19 30.92 1 -8 5 263.46 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14.76 2 -8 9 44.98 11.76 3 -7 9 3.27 4.53 3 -7 9 1.03 3.80 -3 7 -9 -1.29 7.51 4 -6 9 210.85 20.74 -4 6 -9 209.65 27.61 4 -6 9 171.17 20.55 -5 5 -9 81.78 17.13 5 -5 9 108.70 15.63 5 -5 9 147.29 17.38 -6 4 -9 1.82 6.40 6 -4 9 2.24 4.99 6 -4 9 1.72 4.03 -7 3 -9 79.12 16.59 7 -3 9 63.26 11.47 7 -3 9 44.39 12.38 -8 2 -9 2.98 7.85 8 -2 9 -3.77 4.23 8 -2 9 9.03 7.57 9 -1 9 381.53 39.07 9 -1 9 322.66 27.28 -9 1 -9 358.25 36.71 -10 0 -9 46.55 14.09 10 0 9 34.74 14.22 -11 -1 -9 18.63 9.86 11 1 9 10.13 9.75 12 2 9 30.66 15.03 -12 -2 -9 29.72 12.36 13 3 9 14.70 15.11 14 4 9 12.69 15.16 15 5 9 27.37 18.12 7 18 -9 -7.47 20.78 -7 -18 9 -16.44 12.72 6 17 -9 -1.70 15.37 -6 -17 9 2.58 10.82 -5 -16 9 17.10 12.48 5 16 -9 1.05 14.19 -4 -15 9 19.01 11.74 4 15 -9 7.56 13.75 3 14 -9 24.43 15.08 -3 -14 9 15.24 9.77 2 13 -9 -13.88 9.81 -2 -13 9 -5.50 7.12 -1 -12 9 40.64 13.06 1 12 -9 67.08 18.44 0 11 -9 39.66 15.45 0 -11 9 37.23 11.41 1 -10 9 116.30 20.04 -1 10 -9 153.12 27.23 2 -9 9 175.68 23.98 -2 9 -9 162.04 26.86 2 -9 9 209.04 20.43 3 -8 9 242.22 22.78 -3 8 -9 176.58 28.07 3 -8 9 251.85 26.72 4 -7 9 63.24 13.43 4 -7 9 58.60 11.96 -4 7 -9 55.03 15.36 5 -6 9 55.15 11.09 5 -6 9 43.46 10.90 -5 6 -9 61.97 15.83 6 -5 9 24.33 8.43 -6 5 -9 28.63 11.54 6 -5 9 9.35 6.77 7 -4 9 64.17 12.29 -7 4 -9 73.48 17.59 7 -4 9 62.51 14.13 -8 3 -9 15.86 10.94 8 -3 9 12.89 7.74 8 -3 9 23.88 7.67 9 -2 9 74.51 14.27 9 -2 9 116.39 21.70 -9 2 -9 120.08 21.99 10 -1 9 9.95 9.47 -10 1 -9 17.95 10.29 -11 0 -9 18.63 10.54 11 0 9 14.33 11.33 -12 -1 -9 45.72 16.00 12 1 9 71.33 20.97 13 2 9 71.55 22.96 14 3 9 8.60 16.45 15 4 9 9.91 18.17 -6 -18 9 -9.67 12.84 6 18 -9 -5.76 21.51 5 17 -9 2.07 16.62 -5 -17 9 9.85 11.23 4 16 -9 -9.75 14.31 -4 -16 9 3.38 9.23 -3 -15 9 21.55 12.54 3 15 -9 -7.28 12.66 2 14 -9 137.76 28.81 -2 -14 9 134.69 23.69 1 13 -9 4.77 11.01 -1 -13 9 -7.64 5.91 0 12 -9 0.53 10.92 0 -12 9 -9.39 6.33 1 -11 9 -2.57 6.15 -1 11 -9 8.38 11.09 2 -10 9 10.16 7.95 -2 10 -9 -2.49 10.04 3 -9 9 192.24 20.61 3 -9 9 128.47 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14 207.34 28.11 -1 -12 14 164.00 25.07 1 12 -14 175.65 33.09 0 11 -14 -1.62 11.38 0 -11 14 1.99 5.77 1 -10 14 0.85 5.71 -1 10 -14 -5.84 10.14 -2 9 -14 -1.73 9.93 2 -9 14 18.56 8.25 3 -8 14 22.34 9.44 -3 8 -14 26.74 13.04 -4 7 -14 21.93 12.25 4 -7 14 33.85 10.61 4 -7 14 56.82 11.28 -5 6 -14 -12.14 7.09 5 -6 14 4.58 6.21 5 -6 14 2.13 5.98 6 -5 14 85.11 15.65 -6 5 -14 44.96 14.84 6 -5 14 60.94 12.72 7 -4 14 64.62 13.59 7 -4 14 80.89 16.79 -7 4 -14 46.49 15.31 8 -3 14 19.06 8.46 -8 3 -14 11.21 9.26 8 -3 14 2.62 8.47 -9 2 -14 24.88 10.61 9 -2 14 25.99 12.11 9 -2 14 29.29 10.90 10 -1 14 -0.76 9.37 -10 1 -14 13.80 10.57 11 0 14 9.56 12.69 12 1 14 168.58 33.30 13 2 14 10.36 14.24 14 3 14 -8.03 13.19 15 4 14 9.42 20.75 5 17 -14 1.38 22.20 -5 -17 14 18.91 12.55 4 16 -14 -15.82 14.29 -4 -16 14 1.47 10.16 3 15 -14 37.54 20.24 -3 -15 14 19.66 10.56 -2 -14 14 -1.66 7.71 2 14 -14 3.90 12.69 1 13 -14 48.16 19.48 -1 -13 14 34.11 11.97 0 -12 14 250.34 30.84 0 12 -14 190.36 35.87 -1 11 -14 66.76 20.19 1 -11 14 77.38 17.39 -2 10 -14 21.90 14.17 2 -10 14 13.98 9.13 3 -9 14 3.30 7.24 -3 9 -14 8.08 10.06 -4 8 -14 126.45 24.38 4 -8 14 106.10 18.94 -5 7 -14 -6.35 9.07 5 -7 14 -0.10 5.73 5 -7 14 7.22 6.08 -6 6 -14 5.92 9.60 6 -6 14 17.06 8.23 6 -6 14 6.26 7.30 7 -5 14 287.56 30.53 7 -5 14 231.84 26.77 -7 5 -14 264.85 34.37 -8 4 -14 27.71 12.73 8 -4 14 21.38 10.56 8 -4 14 17.31 10.89 9 -3 14 16.70 9.72 9 -3 14 18.75 10.27 -9 3 -14 8.22 10.65 10 -2 14 17.34 10.25 -10 2 -14 10.37 11.29 11 -1 14 1.83 10.43 -11 1 -14 -4.67 10.84 12 0 14 91.73 23.55 13 1 14 -3.87 12.19 14 2 14 21.79 18.62 15 3 14 49.96 26.74 4 17 -14 85.56 32.66 -4 -17 14 50.21 18.01 3 16 -14 -3.76 15.03 -3 -16 14 14.22 10.83 -2 -15 14 41.42 15.46 2 15 -14 80.75 24.39 -1 -14 14 8.07 9.92 1 14 -14 22.89 16.62 0 -13 14 10.80 9.17 0 13 -14 -4.89 13.65 1 -12 14 10.32 7.63 -1 12 -14 1.39 12.71 2 -11 14 113.76 21.95 -2 11 -14 137.94 27.97 -3 10 -14 1.99 12.51 3 -10 14 10.83 9.46 -4 9 -14 -0.03 10.60 4 -9 14 -1.86 6.49 5 -8 14 44.10 13.27 -5 8 -14 38.72 15.60 6 -7 14 -9.96 5.53 -6 7 -14 3.92 10.42 6 -7 14 -4.67 6.76 7 -6 14 113.51 20.86 -7 6 -14 132.18 25.28 7 -6 14 136.89 20.72 -8 5 -14 -11.85 10.20 8 -5 14 15.35 9.20 8 -5 14 -3.76 8.64 9 -4 14 21.49 9.73 -9 4 -14 32.51 13.96 9 -4 14 45.11 15.69 10 -3 14 4.73 11.11 -10 3 -14 32.40 13.72 11 -2 14 62.44 19.67 -11 2 -14 57.17 18.80 12 -1 14 15.38 13.30 13 0 14 11.90 13.86 14 1 14 12.70 18.30 15 2 14 43.77 25.95 -3 -17 14 73.46 20.80 3 17 -14 37.75 23.35 2 16 -14 15.97 17.12 -2 -16 14 2.71 11.47 1 15 -14 16.88 19.35 -1 -15 14 -2.75 9.44 0 -14 14 84.82 20.35 0 14 -14 94.96 30.58 -1 13 -14 9.90 14.65 1 -13 14 1.99 8.00 2 -12 14 27.83 14.19 -2 12 -14 64.99 21.09 -3 11 -14 32.35 16.97 3 -11 14 16.23 11.51 4 -10 14 63.52 17.04 -4 10 -14 84.14 23.61 5 -9 14 15.55 9.31 -5 9 -14 16.59 12.76 6 -8 14 31.22 12.37 -6 8 -14 34.86 14.53 7 -7 14 27.69 11.53 -7 7 -14 -2.87 11.32 7 -7 14 13.09 9.89 8 -6 14 84.78 19.55 8 -6 14 95.95 18.37 -8 6 -14 113.58 23.28 9 -5 14 11.30 11.20 9 -5 14 10.03 12.33 -9 5 -14 22.57 14.24 10 -4 14 28.46 14.45 -10 4 -14 13.76 12.18 11 -3 14 -1.07 9.34 -11 3 -14 3.94 14.57 12 -2 14 16.99 14.77 13 -1 14 64.53 23.08 14 0 14 -9.38 17.12 -2 -17 14 6.29 14.34 2 17 -14 8.72 19.23 -1 -16 14 -13.60 12.16 1 16 -14 16.23 21.23 0 15 -14 -22.05 12.96 0 -15 14 -12.98 7.85 1 -14 14 52.58 16.38 -1 14 -14 58.69 25.04 -2 13 -14 29.46 19.52 2 -13 14 23.07 12.72 -3 12 -14 50.06 22.13 3 -12 14 51.51 16.05 -4 11 -14 -19.99 11.29 4 -11 14 -12.19 7.14 -5 10 -14 -10.39 10.90 5 -10 14 20.91 10.42 6 -9 14 9.88 10.26 -6 9 -14 6.57 14.71 7 -8 14 -7.16 8.94 -7 8 -14 0.36 12.53 8 -7 14 97.73 21.47 8 -7 14 98.81 20.01 -8 7 -14 87.95 23.15 -9 6 -14 44.69 17.23 9 -6 14 41.90 15.24 9 -6 14 18.27 13.61 10 -5 14 86.55 21.46 -10 5 -14 95.50 23.94 11 -4 14 7.34 11.98 -11 4 -14 14.58 15.20 12 -3 14 8.09 12.84 13 -2 14 -17.05 14.59 14 -1 14 9.03 18.93 0 -16 14 3.00 12.78 0 16 -14 -24.43 15.18 1 -15 14 64.26 19.94 -1 15 -14 89.53 28.63 2 -14 14 1.45 10.65 -2 14 -14 4.78 18.97 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14.66 9.68 4 -9 -15 53.42 16.32 -4 9 15 54.26 18.63 4 -9 -15 75.95 15.56 -3 10 15 40.27 14.97 3 -10 -15 52.10 12.53 -3 10 15 28.44 15.00 -2 11 15 6.72 10.58 -2 11 15 2.02 7.82 2 -11 -15 14.23 8.74 -1 12 15 29.63 14.62 -1 12 15 29.01 13.31 1 -12 -15 44.06 13.39 0 13 15 15.19 12.42 0 -13 -15 47.14 13.80 0 13 15 37.02 13.24 -1 -14 -15 34.29 13.26 1 14 15 31.11 16.75 1 14 15 13.04 12.43 2 15 15 -11.04 11.95 -2 -15 -15 11.58 9.80 2 15 15 12.59 14.63 3 16 15 12.86 13.34 3 16 15 -2.66 12.41 -3 -16 -15 15.98 9.37 4 17 15 3.19 13.90 -4 -17 -15 4.73 14.62 -5 -18 -15 4.08 17.57 5 18 15 -13.91 13.77 -13 -1 15 -11.05 14.96 13 1 -15 9.09 14.95 -12 0 15 22.08 16.57 12 0 -15 24.92 14.68 -11 1 15 8.46 13.67 11 -1 -15 6.41 9.67 10 -2 -15 15.54 12.93 -10 2 15 10.34 12.70 -9 3 15 111.72 26.25 9 -3 -15 146.00 27.63 -8 4 15 178.51 31.32 8 -4 -15 178.14 30.02 -7 5 15 -1.29 11.09 7 -5 -15 -3.15 9.44 -6 6 15 20.57 14.02 6 -6 -15 10.09 11.32 -5 7 15 2.82 10.59 5 -7 -15 4.81 7.15 5 -7 -15 3.89 8.05 4 -8 -15 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12.28 10.45 6 -4 -15 8.82 7.97 5 -5 -15 241.93 30.44 -5 5 15 271.05 35.66 5 -5 -15 225.90 22.43 -4 6 15 407.21 42.12 4 -6 -15 361.66 29.02 4 -6 -15 295.67 35.31 -3 7 15 4.51 7.70 3 -7 -15 -8.78 4.87 -3 7 15 6.76 9.18 -2 8 15 201.32 27.33 -2 8 15 252.08 31.39 2 -8 -15 213.35 23.93 -1 9 15 4.27 6.50 -1 9 15 -0.45 7.56 1 -9 -15 -1.53 5.63 0 -10 -15 1.27 6.18 0 10 15 2.19 7.85 0 10 15 -3.24 8.35 1 11 15 9.88 9.62 -1 -11 -15 19.16 8.81 1 11 15 10.36 8.91 -2 -12 -15 205.86 27.09 2 12 15 348.37 38.84 2 12 15 238.80 30.01 -3 -13 -15 -9.45 8.38 3 13 15 -5.48 8.16 3 13 15 -10.16 8.99 -4 -14 -15 -1.22 7.50 4 14 15 6.06 10.95 4 14 15 4.89 11.15 5 15 15 20.40 14.81 -5 -15 -15 38.07 14.54 -6 -16 -15 -6.87 10.60 6 16 15 -16.61 12.02 7 17 15 11.33 17.60 -7 -17 -15 3.41 12.37 8 18 15 38.15 19.66 -8 -18 -15 53.60 21.71 14 5 -15 -10.91 15.58 14 5 -15 5.53 21.75 13 4 -15 25.47 15.26 -13 -4 15 4.46 15.32 12 3 -15 52.79 17.39 -12 -3 15 17.06 15.77 -11 -2 15 21.78 15.21 11 2 -15 10.01 10.13 -10 -1 15 39.92 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9 -15 94.21 21.09 6 8 -15 277.89 36.75 -6 -8 15 318.68 25.58 6 8 -15 367.37 28.01 -5 -7 15 194.03 18.74 5 7 -15 181.48 18.01 5 7 -15 165.99 26.05 4 6 -15 31.18 10.18 4 6 -15 25.79 6.55 -4 -6 15 22.58 8.02 -4 -6 15 27.41 6.92 3 5 -15 9.26 3.99 3 5 -15 5.75 6.27 -3 -5 15 1.11 4.45 -3 -5 15 7.23 4.44 -2 -4 15 237.21 25.02 2 4 -15 266.93 27.10 -2 -4 15 228.43 20.78 2 4 -15 283.55 17.32 1 3 -15 130.08 9.66 -1 -3 15 171.88 16.52 1 3 -15 140.27 17.99 -1 -3 15 143.75 18.18 0 2 -15 7.25 4.69 0 -2 15 1.40 4.07 0 -2 15 -0.37 2.14 0 -2 15 7.21 3.93 1 -1 15 5.96 4.08 -1 1 -15 0.89 3.48 1 -1 15 -0.11 3.59 2 0 15 17.52 6.78 -2 0 -15 21.75 5.00 2 0 15 13.09 5.65 -3 -1 -15 280.13 19.38 3 1 15 307.19 24.31 3 1 15 310.86 24.54 4 2 15 114.18 15.68 4 2 15 125.50 16.96 5 3 15 42.59 9.99 5 3 15 43.45 10.15 6 4 15 3.18 5.81 6 4 15 0.85 4.43 7 5 15 5.90 7.58 7 5 15 36.03 9.50 8 6 15 1.63 8.52 8 6 15 3.81 6.62 9 7 15 87.11 21.14 -9 -7 -15 83.11 14.42 -10 -8 -15 1.30 7.18 10 8 15 10.13 10.64 11 9 15 25.67 12.40 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25.78 12.43 9 6 15 77.67 14.46 -10 -7 -15 128.38 17.59 10 7 15 80.23 20.97 11 8 15 23.72 13.41 12 9 15 25.33 14.40 13 10 15 4.49 13.33 14 11 15 24.12 17.83 15 12 15 -6.17 15.20 11 15 -15 7.84 18.70 10 14 -15 2.35 14.73 9 13 -15 16.49 15.23 8 12 -15 28.99 15.16 7 11 -15 -17.10 9.20 -7 -11 15 -7.56 5.20 -6 -10 15 176.34 20.02 6 10 -15 167.27 27.44 -5 -9 15 12.87 7.13 5 9 -15 19.81 11.88 -5 -9 15 2.57 5.22 -4 -8 15 22.76 7.43 -4 -8 15 5.87 6.02 4 8 -15 14.83 10.44 -3 -7 15 200.67 24.11 -3 -7 15 218.75 21.09 3 7 -15 196.76 26.53 2 6 -15 121.09 18.31 -2 -6 15 115.43 18.07 -2 -6 15 114.05 14.97 -1 -5 15 141.86 16.41 1 5 -15 169.84 20.92 -1 -5 15 134.04 18.92 0 -4 15 0.23 4.60 0 -4 15 0.13 2.83 0 4 -15 0.55 4.19 1 -3 15 548.69 36.79 1 -3 15 531.10 32.11 -1 3 -15 453.24 37.14 -2 2 -15 301.57 23.47 2 -2 15 243.15 23.38 2 -2 15 273.36 20.79 3 -1 15 85.21 13.69 3 -1 15 104.83 13.30 -3 1 -15 131.65 13.09 4 0 15 5.11 4.31 4 0 15 6.46 5.19 -4 0 -15 14.97 4.49 -5 -1 -15 429.65 29.10 5 1 15 435.45 33.17 5 1 15 470.62 35.33 -6 -2 -15 85.53 8.83 6 2 15 60.49 11.84 6 2 15 58.88 13.45 -7 -3 -15 198.68 15.09 7 3 15 186.76 21.34 7 3 15 145.53 23.03 8 4 15 -3.89 6.68 8 4 15 1.82 5.39 -8 -4 -15 5.19 4.63 9 5 15 241.92 33.87 9 5 15 264.99 26.64 10 6 15 14.06 11.88 10 6 15 46.30 10.75 11 7 15 -0.59 9.55 12 8 15 38.50 16.76 13 9 15 8.25 12.87 14 10 15 70.71 23.57 15 11 15 3.57 18.58 10 15 -15 38.40 21.68 9 14 -15 0.76 13.58 8 13 -15 25.94 15.26 -7 -12 15 57.92 12.82 7 12 -15 23.37 14.94 -6 -11 15 261.19 32.79 6 11 -15 268.80 37.13 -6 -11 15 288.04 27.07 -5 -10 15 -3.23 3.95 -5 -10 15 4.12 7.59 5 10 -15 1.68 9.26 -4 -9 15 93.25 14.99 4 9 -15 76.64 18.62 -4 -9 15 105.20 18.10 -3 -8 15 137.15 19.68 -3 -8 15 109.07 15.56 3 8 -15 139.50 22.97 2 7 -15 15.02 7.74 -2 -7 15 23.20 7.86 -2 -7 15 25.04 6.68 -1 -6 15 78.66 12.57 -1 -6 15 59.98 12.87 1 6 -15 83.98 15.66 0 -5 15 378.94 29.27 0 -5 15 371.51 32.83 0 5 -15 409.20 33.61 1 -4 15 3.73 4.09 -1 4 -15 17.82 6.59 2 -3 15 56.38 10.05 2 -3 15 85.49 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16.77 -4 6 -15 23.04 11.75 4 -6 15 37.33 9.07 4 -6 15 7.65 6.70 -5 5 -15 9.80 8.92 5 -5 15 4.71 6.67 5 -5 15 11.64 6.78 -6 4 -15 250.90 29.95 6 -4 15 290.07 28.00 6 -4 15 292.67 28.90 7 -3 15 -7.29 5.34 -7 3 -15 0.97 5.99 7 -3 15 0.04 5.88 8 -2 15 16.86 8.45 8 -2 15 28.84 11.39 -8 2 -15 31.53 9.82 9 -1 15 21.96 11.48 9 -1 15 39.85 10.88 -9 1 -15 33.13 10.79 -10 0 -15 2.90 7.84 10 0 15 10.84 11.09 10 0 15 5.04 7.04 11 1 15 79.52 21.92 12 2 15 -7.13 9.31 13 3 15 2.27 10.87 14 4 15 -2.95 15.93 15 5 15 19.73 19.27 6 17 -15 4.79 20.91 -6 -17 15 24.26 13.97 -5 -16 15 -0.17 9.65 5 16 -15 0.74 16.44 -4 -15 15 76.08 18.50 4 15 -15 48.34 20.97 -3 -14 15 21.25 10.50 3 14 -15 -2.79 11.27 -2 -13 15 4.61 7.14 -2 -13 15 -4.15 10.78 2 13 -15 -6.24 11.84 -1 -12 15 -2.34 9.79 -1 -12 15 -0.75 6.47 1 12 -15 -5.66 11.55 0 -11 15 135.02 22.38 0 11 -15 175.34 30.60 -1 10 -15 26.90 13.76 1 -10 15 4.09 7.07 2 -9 15 45.54 11.53 -2 9 -15 49.66 16.74 3 -8 15 -2.43 4.70 -3 8 -15 9.70 10.13 4 -7 15 50.22 13.09 -4 7 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66.69 15.66 -7 5 -15 18.75 12.27 7 -5 15 17.06 10.04 7 -5 15 9.67 7.93 8 -4 15 186.78 27.33 -8 4 -15 145.69 25.23 8 -4 15 191.20 23.79 -9 3 -15 11.32 11.46 9 -3 15 17.39 10.88 9 -3 15 21.11 11.93 -10 2 -15 61.88 17.06 10 -2 15 37.65 15.11 11 -1 15 37.04 14.78 12 0 15 44.94 18.96 13 1 15 49.72 21.04 14 2 15 -3.77 14.34 15 3 15 6.30 18.75 4 17 -15 -3.29 21.59 -4 -17 15 -3.16 11.79 3 16 -15 23.21 18.59 -3 -16 15 20.65 12.33 2 15 -15 -25.67 13.03 -2 -15 15 -1.60 9.39 1 14 -15 79.38 26.57 -1 -14 15 66.98 18.58 0 -13 15 2.78 8.44 0 13 -15 3.63 13.33 1 -12 15 50.18 15.43 -1 12 -15 21.20 15.72 2 -11 15 31.92 12.20 -2 11 -15 40.49 17.50 3 -10 15 -6.14 6.76 -3 10 -15 -4.58 11.57 -4 9 -15 18.03 13.46 4 -9 15 22.36 9.79 5 -8 15 0.89 6.79 -5 8 -15 17.50 11.98 -6 7 -15 59.97 16.97 6 -7 15 57.99 14.20 7 -6 15 160.49 23.82 -7 6 -15 136.84 25.31 7 -6 15 110.73 19.94 -8 5 -15 11.35 10.95 8 -5 15 1.62 8.29 8 -5 15 7.32 9.30 9 -4 15 18.25 10.69 -9 4 -15 10.79 12.13 9 -4 15 14.49 10.49 10 -3 15 7.99 10.56 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23 67.22 16.27 9 6 23 1.33 8.29 9 6 23 1.18 9.90 10 7 23 0.34 7.81 10 7 23 0.87 10.76 11 8 23 26.32 15.60 -11 -8 -23 37.01 14.41 12 9 23 20.98 14.75 13 10 23 -23.64 13.58 14 11 23 17.21 21.13 9 13 -23 -6.68 17.52 -9 -13 23 38.92 17.15 -8 -12 23 5.28 11.07 8 12 -23 22.71 17.38 -7 -11 23 -0.99 9.72 7 11 -23 25.45 17.83 -6 -10 23 18.03 12.57 -6 -10 23 44.59 12.59 6 10 -23 29.22 15.61 -5 -9 23 -0.27 5.46 -5 -9 23 13.29 9.82 5 9 -23 18.10 13.39 -4 -8 23 106.41 21.56 4 8 -23 140.48 25.36 -4 -8 23 90.43 15.83 -3 -7 23 148.32 23.65 -3 -7 23 127.75 19.75 3 7 -23 143.04 24.48 -2 -6 23 17.16 8.13 2 6 -23 3.85 8.93 -2 -6 23 13.41 8.17 -1 -5 23 143.32 20.77 1 5 -23 130.59 20.95 -1 -5 23 131.10 22.02 0 4 -23 9.11 5.76 0 -4 23 -0.84 6.35 0 -4 23 -2.83 4.39 1 -3 23 308.12 30.88 1 -3 23 324.53 22.61 -1 3 -23 301.38 28.02 2 -2 23 82.90 11.73 2 -2 23 81.60 15.59 -2 2 -23 68.84 12.32 -3 1 -23 160.73 17.38 3 -1 23 168.07 18.17 3 -1 23 81.34 17.89 4 0 23 3.26 5.77 4 0 23 8.35 6.97 -4 0 -23 6.62 4.70 5 1 23 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1 3 28 38.34 12.76 1 3 28 37.38 11.26 2 4 28 5.96 8.70 2 4 28 -5.18 6.38 3 5 28 84.86 18.70 3 5 28 113.07 22.06 4 6 28 93.06 21.41 4 6 28 71.85 17.79 5 7 28 5.59 10.34 5 7 28 1.38 10.18 -6 -8 -28 -0.87 10.63 6 8 28 3.33 9.61 7 9 28 6.41 10.55 -7 -9 -28 6.49 11.85 -8 -10 -28 52.72 16.66 8 10 28 31.43 16.62 -9 -11 -28 -0.13 12.20 9 11 28 14.31 13.65 -10 -12 -28 90.13 21.66 10 12 28 85.19 25.56 -11 -13 -28 13.60 14.74 11 13 28 -23.26 15.15 -12 -14 -28 -13.35 16.99 12 14 28 10.30 19.11 -10 -9 28 18.86 20.64 10 9 -28 -4.33 18.97 9 8 -28 44.35 22.86 -9 -8 28 23.53 16.37 8 7 -28 29.11 18.36 -8 -7 28 20.74 12.38 7 6 -28 1.98 13.12 -7 -6 28 21.98 12.94 -6 -5 28 34.82 14.37 6 5 -28 68.31 19.31 -5 -4 28 50.53 15.39 5 4 -28 12.82 13.07 -4 -3 28 7.96 8.33 4 3 -28 44.12 16.26 -4 -3 28 29.74 11.40 -3 -2 28 23.20 9.99 3 2 -28 7.92 9.74 3 2 -28 15.15 6.43 -3 -2 28 4.87 8.75 2 1 -28 92.84 19.50 -2 -1 28 97.98 20.56 -2 -1 28 117.23 15.21 -2 -1 28 68.43 15.55 1 0 -28 68.08 14.42 -1 0 28 52.08 15.71 -1 0 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12.77 -2 -2 28 10.82 8.51 -2 -2 28 -3.51 5.61 2 2 -28 -0.72 4.35 2 2 -28 -1.63 9.24 -1 -1 28 365.94 40.81 -1 -1 28 374.64 37.01 -1 -1 28 400.76 30.01 1 1 -28 426.06 36.04 0 0 -28 -6.04 5.79 0 0 28 -2.91 6.02 0 0 28 -3.54 5.16 1 1 28 -4.40 5.77 -1 -1 -28 -0.52 5.77 1 1 28 -1.51 6.87 2 2 28 69.84 16.85 2 2 28 102.84 16.74 -2 -2 -28 121.40 14.85 3 3 28 0.58 7.33 3 3 28 14.81 8.41 4 4 28 97.79 20.42 4 4 28 77.14 17.62 5 5 28 172.29 26.45 5 5 28 158.01 25.53 6 6 28 -3.73 9.10 6 6 28 12.05 10.76 7 7 28 10.31 10.62 7 7 28 15.30 11.62 8 8 28 -4.13 9.53 -8 -8 -28 -2.93 10.42 9 9 28 -6.89 10.39 -9 -9 -28 -0.78 10.24 10 10 28 12.06 14.00 -10 -10 -28 12.55 12.24 -11 -11 -28 -18.40 11.74 11 11 28 -7.41 13.45 -12 -12 -28 24.37 15.89 12 12 28 11.67 15.41 -9 -10 28 28.00 18.57 9 10 -28 6.05 20.18 8 9 -28 16.49 17.97 -8 -9 28 34.35 15.66 -7 -8 28 8.87 10.85 7 8 -28 0.69 18.41 6 7 -28 20.87 15.53 -6 -7 28 -0.43 10.63 -5 -6 28 45.35 13.73 -5 -6 28 35.98 13.34 5 6 -28 20.04 13.94 -4 -5 28 4.88 8.34 4 5 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26.67 5 7 -28 15.84 13.54 -5 -7 28 6.47 8.34 -5 -7 28 6.60 10.67 -4 -6 28 4.52 8.80 4 6 -28 -2.45 10.99 -4 -6 28 5.21 9.26 3 5 -28 58.07 17.54 -3 -5 28 40.62 14.99 -3 -5 28 43.87 13.27 2 4 -28 45.71 14.49 -2 -4 28 29.62 11.59 -2 -4 28 27.32 10.93 -1 -3 28 7.36 7.96 -1 -3 28 -0.50 6.63 1 3 -28 -2.46 6.83 0 2 -28 92.94 16.47 0 -2 28 70.67 16.61 1 -1 28 30.12 11.06 -1 1 -28 14.11 7.92 1 -1 28 19.50 7.34 2 0 28 5.25 6.62 2 0 28 14.13 7.90 -2 0 -28 1.16 5.76 3 1 28 59.67 15.41 3 1 28 82.58 15.47 4 2 28 304.32 30.33 4 2 28 184.77 27.59 5 3 28 7.83 8.82 5 3 28 1.52 7.93 6 4 28 17.81 10.73 6 4 28 18.11 10.80 7 5 28 266.17 35.21 7 5 28 297.62 35.85 8 6 28 23.19 12.03 8 6 28 38.51 14.46 9 7 28 6.07 9.84 9 7 28 -5.51 8.25 10 8 28 13.76 13.29 10 8 28 40.92 16.86 -10 -8 -28 38.46 16.44 -11 -9 -28 70.16 19.71 11 9 28 53.84 19.90 12 10 28 -2.26 13.66 -12 -10 -28 13.99 16.34 13 11 28 21.31 22.64 -9 -12 28 17.94 18.38 9 12 -28 11.70 21.61 -8 -11 28 12.28 12.85 8 11 -28 -24.16 14.52 -7 -10 28 25.58 14.70 7 10 -28 42.38 20.97 -6 -9 28 1.28 9.31 6 9 -28 29.98 18.18 5 8 -28 83.86 24.21 -5 -8 28 98.57 22.12 -5 -8 28 142.60 22.10 4 7 -28 28.43 15.36 -4 -7 28 25.09 10.91 -4 -7 28 20.51 10.88 3 6 -28 58.24 17.23 -3 -6 28 13.87 10.08 -3 -6 28 37.57 12.25 2 5 -28 38.60 13.56 -2 -5 28 23.49 10.54 -2 -5 28 11.40 9.53 -1 -4 28 39.66 14.07 1 4 -28 28.94 12.80 -1 -4 28 12.60 9.20 0 -3 28 -3.09 6.88 0 3 -28 -7.89 5.24 -1 2 -28 191.85 22.51 1 -2 28 139.00 23.56 -2 1 -28 392.55 33.66 2 -1 28 505.60 34.83 2 -1 28 358.76 38.86 -3 0 -28 16.42 7.43 3 0 28 13.02 8.55 3 0 28 14.81 9.19 4 1 28 45.51 14.28 4 1 28 71.00 14.64 5 2 28 107.06 20.34 5 2 28 124.64 22.86 6 3 28 3.08 8.63 6 3 28 5.14 7.42 7 4 28 7.32 9.07 7 4 28 3.50 8.81 8 5 28 66.73 17.98 8 5 28 45.12 15.13 9 6 28 6.69 10.76 9 6 28 10.27 10.62 10 7 28 69.70 18.33 10 7 28 36.53 15.56 11 8 28 13.16 12.88 -11 -8 -28 28.92 15.89 -12 -9 -28 14.23 16.31 12 9 28 -1.45 14.41 13 10 28 15.55 20.08 8 12 -28 43.42 23.79 -8 -12 28 17.06 15.44 7 11 -28 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-18.73 15.05 -2 1 42 -5.40 13.21 -1 2 42 7.46 13.57 0 3 42 -10.83 13.29 1 4 42 -15.80 11.75 2 5 42 15.46 14.38 3 6 42 48.26 19.56 3 6 42 53.88 22.24 -4 -7 -42 0.22 16.35 4 7 42 2.45 14.87 -5 -8 -42 17.25 17.87 5 8 42 3.56 15.56 -6 -9 -42 11.96 20.15 6 9 42 21.98 19.71 -4 -2 42 16.97 18.78 -2 0 42 12.63 14.53 -1 1 42 3.29 12.91 0 2 42 -1.68 12.79 1 3 42 42.23 17.49 2 4 42 -2.74 14.08 3 5 42 15.69 16.98 4 6 42 22.36 16.78 4 6 42 -0.53 14.65 5 7 42 -6.59 14.51 5 7 42 14.75 17.43 6 8 42 63.43 23.62 -6 -8 -42 52.64 24.98 7 9 42 -16.86 15.36 -7 -9 -42 0.90 22.77 -4 -3 42 0.57 17.50 4 3 -42 6.24 18.34 -2 -1 42 -13.12 11.45 -1 0 42 53.74 18.58 0 1 42 15.15 13.03 1 2 42 20.50 13.56 2 3 42 21.14 13.57 3 4 42 48.63 19.59 4 5 42 49.01 21.50 5 6 42 53.97 22.21 5 6 42 9.10 16.22 6 7 42 62.51 21.49 6 7 42 23.38 20.17 7 8 42 -2.06 16.82 -7 -8 -42 -2.82 23.22 8 9 42 -17.49 17.05 -8 -9 -42 9.52 23.73 4 4 -42 -12.86 16.14 -4 -4 42 6.41 20.86 -2 -2 42 18.02 15.50 -1 -1 42 126.15 27.86 0 0 42 24.23 16.42 1 1 42 110.09 24.57 2 2 42 -1.78 10.55 3 3 42 19.01 16.84 4 4 42 22.80 17.10 5 5 42 6.84 14.80 6 6 42 -17.03 13.36 6 6 42 -11.06 14.40 7 7 42 36.51 19.81 7 7 42 94.67 25.58 8 8 42 56.64 21.26 8 8 42 29.01 22.84 -4 -5 42 31.06 21.84 4 5 -42 3.96 17.19 -2 -3 42 13.88 13.11 -1 -2 42 17.54 14.73 0 -1 42 8.23 12.41 1 0 42 31.39 14.36 2 1 42 67.65 19.58 3 2 42 1.08 11.60 4 3 42 -6.41 14.12 5 4 42 51.67 20.93 6 5 42 3.08 15.42 7 6 42 9.86 15.87 7 6 42 -8.31 13.69 8 7 42 7.85 17.28 8 7 42 7.18 17.50 3 5 -42 15.18 16.80 -2 -4 42 19.99 15.11 -1 -3 42 15.37 13.19 0 -2 42 26.77 14.34 1 -1 42 7.76 13.18 2 0 42 0.09 11.73 3 1 42 10.84 13.49 4 2 42 76.54 22.45 5 3 42 16.85 15.37 6 4 42 41.74 20.43 7 5 42 -14.88 12.93 8 6 42 42.92 21.54 8 6 42 82.72 26.09 9 7 42 -31.93 14.22 9 7 42 5.00 16.27 3 6 -42 12.72 19.61 -2 -5 42 -18.69 13.25 -1 -4 42 -11.82 11.18 0 -3 42 -28.60 9.54 1 -2 42 11.62 11.76 2 -1 42 51.71 19.53 3 0 42 -8.95 12.63 4 1 42 -15.70 11.33 5 2 42 -4.68 12.92 6 3 42 50.12 21.24 7 4 42 -2.44 14.04 8 5 42 43.10 20.47 9 6 42 10.14 16.33 9 6 42 2.63 15.41 -2 -6 42 -1.72 15.65 -1 -5 42 -0.93 13.76 0 -4 42 -22.56 11.05 1 -3 42 23.67 15.18 2 -2 42 24.43 16.12 3 -1 42 25.79 15.17 4 0 42 -3.72 11.94 5 1 42 -14.66 12.87 6 2 42 29.65 16.85 7 3 42 11.21 17.36 8 4 42 25.73 17.43 9 5 42 -2.64 16.79 -2 -7 42 3.41 15.28 -1 -6 42 27.42 16.78 0 -5 42 0.33 14.83 1 -4 42 15.50 14.35 2 -3 42 -7.92 13.11 3 -2 42 4.52 14.83 4 -1 42 -13.37 13.21 5 0 42 91.22 25.08 6 1 42 25.85 17.04 7 2 42 -1.04 14.29 8 3 42 29.55 16.76 9 4 42 -10.29 17.15 -1 -7 42 6.83 15.95 0 -6 42 74.49 24.44 1 -5 42 -18.62 14.52 2 -4 42 18.42 16.26 3 -3 42 58.09 22.01 4 -2 42 8.64 13.97 5 -1 42 25.42 18.72 6 0 42 1.84 15.15 7 1 42 15.43 17.73 8 2 42 2.67 16.83 9 3 42 -0.39 18.50 0 -7 42 -0.89 18.92 1 -6 42 18.17 17.79 2 -5 42 42.15 21.35 3 -4 42 -4.05 15.57 4 -3 42 13.91 17.00 5 -2 42 21.35 17.91 6 -1 42 52.21 24.52 7 0 42 13.71 16.50 8 1 42 31.75 18.89 9 2 42 28.67 20.58 1 -7 42 21.95 20.22 2 -6 42 77.68 27.90 3 -5 42 52.46 24.94 4 -4 42 1.79 15.46 5 -3 42 -8.68 15.80 6 -2 42 80.21 24.70 7 -1 42 -6.17 15.72 8 0 42 53.79 22.57 3 -6 42 1.57 20.56 4 -5 42 -14.53 17.49 5 -4 42 -24.07 14.74 6 -3 42 45.54 22.46 7 -2 42 24.50 21.92 8 -1 42 65.59 25.82 1 -5 -43 26.37 19.57 0 -6 -43 -15.68 14.43 0 6 43 11.61 14.80 -1 -7 -43 -4.59 16.29 1 7 43 -0.41 14.98 2 8 43 3.68 17.32 -2 -8 -43 25.48 21.35 2 -3 -43 23.53 22.21 1 -4 -43 36.35 20.30 0 -5 -43 23.04 17.81 1 6 43 9.16 17.53 -1 -6 -43 34.80 18.72 2 7 43 2.12 16.28 -2 -7 -43 17.45 19.11 3 8 43 27.93 20.44 -3 -8 -43 85.57 27.47 4 9 43 -0.77 17.06 -4 -9 -43 -1.94 20.12 -2 2 43 -4.04 15.90 -1 3 43 -15.12 13.77 0 4 43 1.19 13.92 -1 -5 -43 4.61 16.23 1 5 43 16.74 17.10 -2 -6 -43 -4.34 16.31 2 6 43 -12.46 15.64 -3 -7 -43 13.49 16.40 3 7 43 29.33 18.71 4 8 43 -41.13 15.72 -4 -8 -43 -20.78 16.48 5 9 43 18.79 18.97 -5 -9 -43 11.89 21.64 -2 1 43 -9.40 15.43 -1 2 43 16.20 13.99 0 3 43 50.29 18.25 1 4 43 6.96 15.19 2 5 43 -3.23 13.26 3 6 43 41.02 21.46 3 6 43 57.56 21.64 4 7 43 -9.30 14.54 -4 -7 -43 36.38 18.14 5 8 43 10.64 19.88 -5 -8 -43 5.72 18.42 -6 -9 -43 42.50 24.38 6 9 43 27.59 19.89 -4 -2 43 0.44 17.92 -2 0 43 23.34 15.72 -1 1 43 7.18 12.89 0 2 43 15.35 13.65 1 3 43 -21.18 10.58 2 4 43 28.41 17.68 3 5 43 -4.08 13.91 4 6 43 7.70 18.43 4 6 43 72.40 25.44 5 7 43 108.26 28.09 5 7 43 65.53 27.01 6 8 43 -2.14 16.91 -6 -8 -43 63.23 26.27 -4 -3 43 31.76 22.10 -2 -1 43 29.67 15.51 -1 0 43 20.76 14.78 0 1 43 144.52 28.95 1 2 43 7.31 13.27 2 3 43 -6.69 13.45 3 4 43 35.36 17.74 4 5 43 9.19 14.95 5 6 43 -9.38 14.94 5 6 43 1.22 16.33 6 7 43 138.50 32.57 6 7 43 152.15 33.45 -7 -8 -43 23.70 26.55 7 8 43 18.56 20.02 -2 -2 43 60.96 20.83 -1 -1 43 -7.85 11.97 0 0 43 23.41 14.66 1 1 43 20.19 14.69 2 2 43 14.06 14.43 3 3 43 -2.51 13.80 4 4 43 13.13 16.82 5 5 43 0.25 14.64 6 6 43 4.99 16.63 6 6 43 11.45 16.80 7 7 43 -3.24 17.04 7 7 43 46.57 21.57 -2 -3 43 11.94 15.32 -1 -2 43 10.15 14.32 0 -1 43 28.21 16.60 1 0 43 122.55 26.90 2 1 43 7.28 13.45 3 2 43 -11.86 12.53 4 3 43 17.80 17.98 5 4 43 -6.36 17.33 6 5 43 2.75 16.12 7 6 43 21.41 17.56 8 7 43 8.28 18.67 8 7 43 18.09 19.34 -2 -4 43 -9.72 13.63 -1 -3 43 -6.78 11.88 0 -2 43 13.34 15.02 1 -1 43 13.37 13.69 2 0 43 72.39 22.00 3 1 43 18.32 16.80 4 2 43 35.87 17.84 5 3 43 16.54 16.63 6 4 43 -8.42 16.57 7 5 43 -12.01 14.29 8 6 43 16.31 19.62 -2 -5 43 4.85 15.60 -1 -4 43 -1.70 15.29 0 -3 43 8.76 15.39 1 -2 43 9.62 14.75 2 -1 43 -7.79 11.49 3 0 43 -15.44 11.33 4 1 43 57.88 21.55 5 2 43 26.32 17.16 6 3 43 19.46 18.88 7 4 43 -25.43 14.11 8 5 43 -14.90 16.07 -2 -6 43 21.91 17.04 -1 -5 43 -5.90 12.97 0 -4 43 -5.56 12.95 1 -3 43 9.05 14.53 2 -2 43 -6.18 13.56 3 -1 43 16.57 15.75 4 0 43 6.40 16.50 5 1 43 -21.18 12.37 6 2 43 -10.16 13.54 7 3 43 -3.15 14.47 8 4 43 8.07 21.07 9 5 43 -4.70 16.20 -1 -6 43 20.31 19.14 0 -5 43 82.00 25.90 1 -4 43 26.20 16.60 2 -3 43 16.66 16.65 3 -2 43 29.94 19.91 4 -1 43 1.52 15.19 5 0 43 16.95 17.31 6 1 43 58.73 22.70 7 2 43 1.05 15.84 8 3 43 21.02 19.15 0 -6 43 -0.47 15.01 1 -5 43 -15.51 14.10 2 -4 43 19.59 18.22 3 -3 43 14.99 17.82 4 -2 43 19.57 18.87 5 -1 43 34.38 17.84 6 0 43 9.10 16.48 7 1 43 -8.60 15.48 8 2 43 -10.19 14.42 1 -6 43 13.60 18.98 2 -5 43 10.06 19.45 3 -4 43 13.28 19.74 4 -3 43 14.62 18.12 5 -2 43 -17.25 14.51 6 -1 43 12.14 17.38 7 0 43 75.11 23.29 8 1 43 5.82 16.00 2 -6 43 61.78 25.78 3 -5 43 11.72 19.87 4 -4 43 17.50 19.57 5 -3 43 14.87 19.73 6 -2 43 14.93 16.88 7 -1 43 34.32 21.44 5 -4 43 -12.70 16.67 6 -3 43 32.00 23.80 1 -4 -44 7.22 17.95 0 -5 -44 -0.63 16.59 -1 -6 -44 15.15 18.65 -2 -7 -44 36.27 24.32 2 7 44 62.93 23.63 -1 3 44 -6.12 17.71 0 4 44 3.33 16.58 -1 -5 -44 22.57 19.12 -2 -6 -44 26.17 20.29 -3 -7 -44 16.51 21.21 3 7 44 13.33 17.85 4 8 44 -11.77 17.48 -4 -8 -44 19.70 21.55 -1 2 44 57.94 21.46 0 3 44 -17.05 13.47 1 4 44 13.17 15.52 2 5 44 -3.01 14.71 3 6 44 -6.83 15.60 4 7 44 29.03 21.89 -4 -7 -44 4.86 20.75 -5 -8 -44 32.79 24.30 5 8 44 13.12 18.98 -2 0 44 16.15 18.27 -1 1 44 3.78 14.89 0 2 44 48.60 19.99 1 3 44 3.80 14.44 2 4 44 -1.97 12.30 3 5 44 59.62 21.51 4 6 44 7.62 19.15 5 7 44 2.12 19.47 5 7 44 8.68 20.21 6 8 44 0.01 17.03 -6 -8 -44 28.40 25.81 -2 -1 44 56.78 19.53 -1 0 44 16.55 18.03 0 1 44 15.75 15.10 1 2 44 -1.18 13.48 2 3 44 -1.93 15.54 3 4 44 -7.01 13.28 4 5 44 -4.87 16.38 5 6 44 96.61 28.67 6 7 44 -28.36 16.33 6 7 44 2.87 18.23 -2 -2 44 52.84 19.62 -1 -1 44 21.29 16.58 0 0 44 108.11 25.97 1 1 44 12.96 14.27 2 2 44 16.50 15.73 3 3 44 -4.32 15.35 4 4 44 7.98 16.01 5 5 44 -27.68 14.62 6 6 44 47.10 23.49 7 7 44 36.39 19.71 7 7 44 37.84 20.29 -2 -3 44 40.70 21.28 -1 -2 44 5.31 14.74 0 -1 44 -19.10 12.40 1 0 44 -13.23 12.13 2 1 44 -2.24 15.02 3 2 44 19.91 18.51 4 3 44 12.61 17.66 5 4 44 17.39 18.14 6 5 44 1.14 16.32 7 6 44 -15.12 15.17 -2 -4 44 12.34 17.02 -1 -3 44 -8.80 13.79 0 -2 44 7.41 13.02 1 -1 44 42.44 19.72 2 0 44 17.03 16.45 3 1 44 -11.58 12.43 4 2 44 10.89 15.71 5 3 44 9.97 15.44 6 4 44 -11.91 18.27 7 5 44 68.14 23.06 8 6 44 9.54 20.12 -1 -4 44 -27.52 13.01 0 -3 44 5.06 14.61 1 -2 44 2.94 12.69 2 -1 44 4.72 12.93 3 0 44 -5.25 14.93 4 1 44 -0.61 14.20 5 2 44 -6.84 13.34 6 3 44 -21.36 16.04 7 4 44 6.80 18.07 8 5 44 -1.94 19.43 -1 -5 44 27.03 18.27 0 -4 44 5.09 13.60 1 -3 44 -2.05 14.69 2 -2 44 -25.63 13.25 3 -1 44 -8.12 14.02 4 0 44 9.58 16.04 5 1 44 20.96 16.78 6 2 44 -19.93 13.84 7 3 44 3.67 17.31 8 4 44 2.47 19.36 0 -5 44 -14.29 14.46 1 -4 44 5.99 16.60 2 -3 44 9.08 16.83 3 -2 44 7.78 17.25 4 -1 44 34.89 20.59 5 0 44 23.78 20.03 6 1 44 -19.72 13.66 7 2 44 -1.29 16.46 8 3 44 24.97 19.65 1 -5 44 28.15 20.17 2 -4 44 1.29 18.76 3 -3 44 17.56 20.68 4 -2 44 7.15 18.98 5 -1 44 17.84 18.59 6 0 44 11.29 16.53 7 1 44 -13.87 16.63 2 -5 44 25.08 21.60 3 -4 44 2.45 19.59 4 -3 44 38.97 22.27 5 -2 44 13.61 17.92 6 -1 44 -13.26 17.37 7 0 44 -22.62 16.21 4 -4 44 8.64 21.47 5 -3 44 10.32 17.64 6 -2 44 -27.88 15.99 -1 3 45 21.04 19.81 0 4 45 11.29 17.04 -1 -5 -45 7.14 21.48 -2 -6 -45 12.59 22.94 -1 2 45 34.78 19.69 0 3 45 45.27 20.84 1 4 45 -3.13 17.64 2 5 45 -14.89 16.31 3 6 45 -36.03 16.31 4 7 45 8.30 18.33 -4 -7 -45 3.85 21.02 -1 1 45 32.12 18.21 0 2 45 -2.96 15.21 1 3 45 48.07 22.02 2 4 45 46.59 22.40 3 5 45 17.25 18.19 4 6 45 52.22 26.46 -5 -7 -45 67.75 28.01 5 7 45 32.52 24.51 -1 0 45 58.36 22.95 0 1 45 7.00 15.20 1 2 45 32.82 17.23 2 3 45 -4.88 14.92 3 4 45 7.92 18.46 4 5 45 -0.51 19.67 5 6 45 12.41 20.67 -2 -2 45 28.74 20.54 -1 -1 45 1.90 14.25 0 0 45 -14.72 14.52 1 1 45 23.00 16.93 2 2 45 56.63 22.45 3 3 45 -13.58 16.12 4 4 45 16.11 17.55 5 5 45 7.75 19.91 6 6 45 18.14 20.44 -1 -2 45 3.11 15.03 0 -1 45 31.92 18.25 1 0 45 12.35 15.35 2 1 45 -8.89 14.81 3 2 45 10.31 18.80 4 3 45 -23.48 15.29 5 4 45 16.70 20.52 6 5 45 15.21 20.08 -1 -3 45 21.64 18.58 0 -2 45 23.80 17.78 1 -1 45 -5.60 14.13 2 0 45 50.85 21.84 3 1 45 3.32 16.27 4 2 45 -5.03 16.92 5 3 45 -16.50 17.27 6 4 45 10.29 18.60 7 5 45 2.82 18.09 -1 -4 45 -2.75 16.63 0 -3 45 6.10 16.70 1 -2 45 -8.78 14.83 2 -1 45 -8.95 15.90 3 0 45 12.20 19.64 4 1 45 -9.17 16.83 5 2 45 35.28 21.99 6 3 45 16.19 20.59 7 4 45 -10.50 18.42 0 -4 45 -17.17 15.40 1 -3 45 5.41 16.63 2 -2 45 -4.05 15.98 3 -1 45 -5.95 17.68 4 0 45 34.85 22.74 5 1 45 5.91 18.12 6 2 45 20.15 20.33 7 3 45 2.19 19.40 1 -4 45 13.32 19.26 2 -3 45 20.67 19.70 3 -2 45 -0.57 19.64 4 -1 45 13.47 19.12 5 0 45 0.00 16.52 6 1 45 13.87 18.25 7 2 45 -10.26 16.57 2 -4 45 25.49 20.79 3 -3 45 -10.10 19.11 4 -2 45 26.76 22.81 5 -1 45 16.81 18.57 6 0 45 22.69 19.70 4 -3 45 33.37 23.32 5 -2 45 -14.21 15.91 1 4 46 13.78 17.08 0 2 46 -3.81 13.47 1 3 46 21.36 18.86 2 4 46 -4.25 17.62 3 5 46 -27.95 16.28 0 1 46 3.30 16.06 1 2 46 49.16 21.39 2 3 46 0.70 17.55 3 4 46 -8.04 17.96 4 5 46 45.67 26.58 0 0 46 3.03 15.29 1 1 46 66.38 24.83 2 2 46 2.80 17.08 3 3 46 2.01 18.81 4 4 46 -3.91 18.47 5 5 46 -4.85 17.75 0 -1 46 -13.13 13.74 1 0 46 13.95 16.74 2 1 46 97.45 28.33 3 2 46 6.39 19.44 4 3 46 13.63 22.28 5 4 46 14.06 22.66 0 -2 46 7.56 17.32 1 -1 46 10.74 16.74 2 0 46 37.07 21.67 3 1 46 17.44 20.57 4 2 46 16.90 20.53 5 3 46 -12.27 18.79 6 4 46 -20.20 19.82 1 -2 46 39.44 25.85 2 -1 46 72.61 28.37 3 0 46 17.41 19.58 4 1 46 0.21 18.78 5 2 46 -8.09 19.39 6 3 46 -15.85 19.01 1 -3 46 -1.75 17.86 2 -2 46 -4.13 18.02 3 -1 46 -14.48 16.82 4 0 46 0.08 17.51 5 1 46 8.35 19.14 6 2 46 23.96 20.67 3 -2 46 0.67 19.60 4 -1 46 9.74 19.55 5 0 46 12.52 20.00 2 2 47 7.26 17.24 3 3 47 -8.64 20.53 2 1 47 1.61 17.77 3 2 47 3.19 20.78 4 3 47 15.87 21.64 2 0 47 6.86 18.94 3 1 47 26.46 22.49 4 2 47 -13.82 18.34 3 0 47 0.07 18.48 4 1 47 23.35 21.89 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 80826 _database_code_depnum_ccdc_archive 'CCDC 971178' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_kla0119 # start Validation Reply Form _vrf_PLAT220_kla0119 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.1 Ratio RESPONSE: Slight but unresolvable disorder in the isopropyl groups leads to larger C Ueq range. ; # end Validation Reply Form _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H72 Cr2 N4 S2' _chemical_formula_weight 921.25 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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/n' _space_group_name_Hall '-P 2yn' _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+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.703(5) _cell_length_b 19.311(7) _cell_length_c 19.558(7) _cell_angle_alpha 90 _cell_angle_beta 99.039(6) _cell_angle_gamma 90 _cell_volume 5111(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 987 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 21.87 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.197 _exptl_crystal_F_000 1968 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.298 _exptl_crystal_size_mid 0.277 _exptl_crystal_size_min 0.085 _exptl_absorpt_coefficient_mu 0.544 _shelx_estimated_absorpt_T_min 0.855 _shelx_estimated_absorpt_T_max 0.955 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8534 _exptl_absorpt_correction_T_max 0.9548 _exptl_absorpt_process_details 'APEX2 (Bruker, 2007)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 69278 _diffrn_reflns_av_unetI/netI 0.0565 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.696 _diffrn_reflns_theta_max 28.307 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 12708 _reflns_number_gt 8732 _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 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _refine_special_details ; ? ; _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^)+(0.0665P)^2^+0.6071P] 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 none _refine_ls_extinction_coef . _refine_ls_number_reflns 12708 _refine_ls_number_parameters 557 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1333 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Cr1 Cr 0.11459(2) 0.17723(2) 0.21161(2) 0.02589(9) Uani 1 1 d . . . . . Cr2 Cr -0.02405(2) 0.16545(2) 0.21649(2) 0.02669(9) Uani 1 1 d . . . . . S1 S 0.08549(4) 0.15999(3) 0.09582(3) 0.03540(14) Uani 1 1 d . . . . . S2 S -0.06059(4) 0.17978(3) 0.09979(3) 0.03575(14) Uani 1 1 d . . . . . N1 N 0.13237(12) 0.27548(9) 0.22439(8) 0.0273(4) Uani 1 1 d . . . . . N2 N -0.05914(12) 0.24670(9) 0.26435(9) 0.0299(4) Uani 1 1 d . . . . . N3 N 0.17633(11) 0.09505(9) 0.25392(8) 0.0279(4) Uani 1 1 d . . . . . N4 N -0.03461(12) 0.06767(9) 0.23092(9) 0.0289(4) Uani 1 1 d . . . . . C1 C 0.07323(16) 0.32402(11) 0.24724(11) 0.0330(5) Uani 1 1 d . . . . . H1 H 0.0949 0.3708 0.2486 0.040 Uiso 1 1 calc R U . . . C2 C -0.01512(16) 0.31022(11) 0.26838(11) 0.0330(5) Uani 1 1 d . . . . . H2 H -0.0481 0.3473 0.2871 0.040 Uiso 1 1 calc R U . . . C3 C 0.30975(15) 0.30695(11) 0.24222(12) 0.0349(5) Uani 1 1 d . . . . . C4 C 0.39112(17) 0.33045(12) 0.21329(15) 0.0445(6) Uani 1 1 d . . . . . H4 H 0.4546 0.3313 0.2410 0.053 Uiso 1 1 calc R U . . . C5 C 0.38089(19) 0.35217(14) 0.14596(15) 0.0506(7) Uani 1 1 d . . . . . H5 H 0.4375 0.3663 0.1270 0.061 Uiso 1 1 calc R U . . . C6 C 0.28860(18) 0.35373(13) 0.10523(13) 0.0451(6) Uani 1 1 d . . . . . H6 H 0.2822 0.3705 0.0591 0.054 Uiso 1 1 calc R U . . . C7 C 0.20497(16) 0.33096(11) 0.13105(12) 0.0339(5) Uani 1 1 d . . . . . C8 C 0.21766(15) 0.30474(11) 0.19881(11) 0.0304(5) Uani 1 1 d . . . . . C9 C 0.32042(16) 0.28820(12) 0.31852(12) 0.0412(6) Uani 1 1 d . . . . . H9 H 0.2745 0.2489 0.3235 0.049 Uiso 1 1 calc R U . . . C10 C 0.42466(19) 0.26575(14) 0.34932(16) 0.0578(7) Uani 1 1 d . . . . . H10A H 0.4474 0.2300 0.3200 0.087 Uiso 1 1 calc R U . . . H10B H 0.4245 0.2471 0.3959 0.087 Uiso 1 1 calc R U . . . H10C H 0.4692 0.3057 0.3519 0.087 Uiso 1 1 calc R U . . . C11 C 0.2903(2) 0.35010(16) 0.36049(14) 0.0618(8) Uani 1 1 d . . . . . H11A H 0.3291 0.3909 0.3518 0.093 Uiso 1 1 calc R U . . . H11B H 0.3028 0.3388 0.4100 0.093 Uiso 1 1 calc R U . . . H11C H 0.2198 0.3599 0.3463 0.093 Uiso 1 1 calc R U . . . C12 C 0.10373(17) 0.33763(12) 0.08668(12) 0.0373(5) Uani 1 1 d . . . . . H12 H 0.0575 0.3059 0.1063 0.045 Uiso 1 1 calc R U . . . C13 C 0.1040(2) 0.31690(14) 0.01187(13) 0.0512(7) Uani 1 1 d . . . . . H13A H 0.1369 0.3529 -0.0115 0.077 Uiso 1 1 calc R U . . . H13B H 0.0358 0.3115 -0.0116 0.077 Uiso 1 1 calc R U . . . H13C H 0.1394 0.2730 0.0104 0.077 Uiso 1 1 calc R U . . . C14 C 0.0645(2) 0.41192(13) 0.09068(15) 0.0541(7) Uani 1 1 d . . . . . H14A H 0.0673 0.4252 0.1393 0.081 Uiso 1 1 calc R U . . . H14B H -0.0040 0.4141 0.0671 0.081 Uiso 1 1 calc R U . . . H14C H 0.1053 0.4437 0.0682 0.081 Uiso 1 1 calc R U . . . C15 C -0.12882(16) 0.25562(13) 0.37262(12) 0.0397(5) Uani 1 1 d . . . . . C16 C -0.21181(18) 0.26232(14) 0.40512(13) 0.0499(7) Uani 1 1 d . . . . . H16 H -0.2033 0.2696 0.4537 0.060 Uiso 1 1 calc R U . . . C17 C -0.30557(18) 0.25855(14) 0.36832(14) 0.0503(7) Uani 1 1 d . . . . . H17 H -0.3611 0.2634 0.3915 0.060 Uiso 1 1 calc R U . . . C18 C -0.31934(17) 0.24782(14) 0.29834(13) 0.0476(6) Uani 1 1 d . . . . . H18 H -0.3847 0.2440 0.2739 0.057 Uiso 1 1 calc R U . . . C19 C -0.24008(16) 0.24235(13) 0.26208(12) 0.0397(5) Uani 1 1 d . . . . . C20 C -0.14409(15) 0.24648(11) 0.30054(11) 0.0330(5) Uani 1 1 d . . . . . C21 C -0.25828(18) 0.23788(19) 0.18438(13) 0.0626(9) Uani 1 1 d . . . . . H21 H -0.1952 0.2226 0.1694 0.075 Uiso 1 1 calc R U . . . C22 C -0.3375(3) 0.18684(19) 0.15513(18) 0.0841(11) Uani 1 1 d . . . . . H22A H -0.3247 0.1421 0.1784 0.126 Uiso 1 1 calc R U . . . H22B H -0.3371 0.1811 0.1054 0.126 Uiso 1 1 calc R U . . . H22C H -0.4022 0.2042 0.1626 0.126 Uiso 1 1 calc R U . . . C23 C -0.2825(4) 0.3091(3) 0.1539(2) 0.149(2) Uani 1 1 d . . . . . H23A H -0.3524 0.3193 0.1544 0.223 Uiso 1 1 calc R U . . . H23B H -0.2691 0.3102 0.1061 0.223 Uiso 1 1 calc R U . . . H23C H -0.2415 0.3438 0.1815 0.223 Uiso 1 1 calc R U . . . C24 C -0.02689(18) 0.25927(16) 0.41676(13) 0.0526(7) Uani 1 1 d . . . . . H24 H 0.0229 0.2482 0.3861 0.063 Uiso 1 1 calc R U . . . C25 C -0.0042(3) 0.33206(19) 0.44578(17) 0.0766(10) Uani 1 1 d . . . . . H25A H -0.0117 0.3656 0.4077 0.115 Uiso 1 1 calc R U . . . H25B H 0.0638 0.3336 0.4705 0.115 Uiso 1 1 calc R U . . . H25C H -0.0500 0.3436 0.4778 0.115 Uiso 1 1 calc R U . . . C26 C -0.0155(2) 0.2051(2) 0.47509(15) 0.0725(10) Uani 1 1 d . . . . . H26A H 0.0503 0.2092 0.5029 0.109 Uiso 1 1 calc R U . . . H26B H -0.0236 0.1586 0.4549 0.109 Uiso 1 1 calc R U . . . H26C H -0.0660 0.2129 0.5046 0.109 Uiso 1 1 calc R U . . . C27 C 0.13559(15) 0.03212(11) 0.26084(11) 0.0321(5) Uani 1 1 d . . . . . H27 H 0.1788 -0.0051 0.2762 0.038 Uiso 1 1 calc R U . . . C28 C 0.03655(15) 0.01846(11) 0.24727(11) 0.0325(5) Uani 1 1 d . . . . . H28 H 0.0160 -0.0284 0.2494 0.039 Uiso 1 1 calc R U . . . C29 C 0.30682(15) 0.10062(11) 0.35534(11) 0.0323(5) Uani 1 1 d . . . . . C30 C 0.40607(16) 0.09474(12) 0.38359(12) 0.0384(5) Uani 1 1 d . . . . . H30 H 0.4249 0.0961 0.4324 0.046 Uiso 1 1 calc R U . . . C31 C 0.47755(16) 0.08693(12) 0.34185(12) 0.0406(6) Uani 1 1 d . . . . . H31 H 0.5451 0.0834 0.3621 0.049 Uiso 1 1 calc R U . . . C32 C 0.45144(15) 0.08426(13) 0.27095(12) 0.0399(5) Uani 1 1 d . . . . . H32 H 0.5016 0.0799 0.2428 0.048 Uiso 1 1 calc R U . . . C33 C 0.35251(15) 0.08786(11) 0.23955(11) 0.0334(5) Uani 1 1 d . . . . . C34 C 0.28071(14) 0.09620(11) 0.28316(11) 0.0291(4) Uani 1 1 d . . . . . C35 C 0.23014(17) 0.11025(13) 0.40378(12) 0.0420(6) Uani 1 1 d . . . . . H35 H 0.1661 0.1230 0.3746 0.050 Uiso 1 1 calc R U . . . C36 C 0.2576(2) 0.16843(16) 0.45566(15) 0.0595(8) Uani 1 1 d . . . . . H36A H 0.2059 0.1734 0.4847 0.089 Uiso 1 1 calc R U . . . H36B H 0.2642 0.2118 0.4308 0.089 Uiso 1 1 calc R U . . . H36C H 0.3206 0.1575 0.4849 0.089 Uiso 1 1 calc R U . . . C37 C 0.2136(2) 0.04354(16) 0.44143(16) 0.0655(8) Uani 1 1 d . . . . . H37A H 0.1956 0.0065 0.4076 0.098 Uiso 1 1 calc R U . . . H37B H 0.1601 0.0502 0.4687 0.098 Uiso 1 1 calc R U . . . H37C H 0.2743 0.0309 0.4723 0.098 Uiso 1 1 calc R U . . . C38 C 0.32604(16) 0.08019(13) 0.16185(12) 0.0398(5) Uani 1 1 d . . . . . H38 H 0.2532 0.0719 0.1509 0.048 Uiso 1 1 calc R U . . . C39 C 0.3488(2) 0.14651(15) 0.12486(14) 0.0592(7) Uani 1 1 d . . . . . H39A H 0.3147 0.1856 0.1427 0.089 Uiso 1 1 calc R U . . . H39B H 0.3261 0.1416 0.0750 0.089 Uiso 1 1 calc R U . . . H39C H 0.4202 0.1549 0.1331 0.089 Uiso 1 1 calc R U . . . C40 C 0.3782(2) 0.01845(16) 0.13394(15) 0.0632(8) Uani 1 1 d . . . . . H40A H 0.4497 0.0266 0.1414 0.095 Uiso 1 1 calc R U . . . H40B H 0.3544 0.0131 0.0843 0.095 Uiso 1 1 calc R U . . . H40C H 0.3638 -0.0238 0.1583 0.095 Uiso 1 1 calc R U . . . C41 C -0.18709(16) 0.03599(12) 0.27685(13) 0.0400(5) Uani 1 1 d . . . . . C42 C -0.28192(18) 0.00783(14) 0.26461(16) 0.0543(7) Uani 1 1 d . . . . . H42 H -0.3197 0.0062 0.3013 0.065 Uiso 1 1 calc R U . . . C43 C -0.32211(19) -0.01761(15) 0.20052(18) 0.0622(8) Uani 1 1 d . . . . . H43 H -0.3874 -0.0357 0.1933 0.075 Uiso 1 1 calc R U . . . C44 C -0.26793(19) -0.01684(14) 0.14695(16) 0.0563(7) Uani 1 1 d . . . . . H44 H -0.2961 -0.0355 0.1033 0.068 Uiso 1 1 calc R U . . . C45 C -0.17265(16) 0.01060(12) 0.15514(13) 0.0400(5) Uani 1 1 d . . . . . C46 C -0.13427(15) 0.03853(11) 0.22045(12) 0.0334(5) Uani 1 1 d . . . . . C47 C -0.14258(17) 0.05867(14) 0.34907(13) 0.0452(6) Uani 1 1 d . . . . . H47 H -0.0977 0.0987 0.3446 0.054 Uiso 1 1 calc R U . . . C48 C -0.2197(2) 0.08229(16) 0.39322(16) 0.0639(8) Uani 1 1 d . . . . . H48A H -0.2632 0.1169 0.3676 0.096 Uiso 1 1 calc R U . . . H48B H -0.1861 0.1026 0.4365 0.096 Uiso 1 1 calc R U . . . H48C H -0.2590 0.0424 0.4037 0.096 Uiso 1 1 calc R U . . . C49 C -0.0798(2) -0.00012(16) 0.38776(14) 0.0634(8) Uani 1 1 d . . . . . H49A H -0.1219 -0.0405 0.3918 0.095 Uiso 1 1 calc R U . . . H49B H -0.0510 0.0159 0.4341 0.095 Uiso 1 1 calc R U . . . H49C H -0.0268 -0.0129 0.3619 0.095 Uiso 1 1 calc R U . . . C50 C -0.11243(19) 0.00460(13) 0.09603(12) 0.0460(6) Uani 1 1 d . . . . . H50 H -0.0546 0.0366 0.1063 0.055 Uiso 1 1 calc R U . . . C51 C -0.1705(3) 0.02483(17) 0.02569(15) 0.0749(10) Uani 1 1 d . . . . . H51A H -0.1257 0.0270 -0.0086 0.112 Uiso 1 1 calc R U . . . H51B H -0.2013 0.0702 0.0293 0.112 Uiso 1 1 calc R U . . . H51C H -0.2220 -0.0098 0.0113 0.112 Uiso 1 1 calc R U . . . C52 C -0.0727(2) -0.06890(15) 0.09297(16) 0.0687(9) Uani 1 1 d . . . . . H52A H -0.0337 -0.0809 0.1378 0.103 Uiso 1 1 calc R U . . . H52B H -0.0309 -0.0717 0.0568 0.103 Uiso 1 1 calc R U . . . H52C H -0.1281 -0.1013 0.0824 0.103 Uiso 1 1 calc R U . . . 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 Cr1 0.02226(17) 0.03033(18) 0.02527(18) 0.00038(13) 0.00433(13) 0.00016(13) Cr2 0.02161(16) 0.03139(19) 0.02688(18) 0.00116(13) 0.00326(13) 0.00042(13) S1 0.0368(3) 0.0420(3) 0.0280(3) -0.0032(2) 0.0071(2) 0.0013(2) S2 0.0328(3) 0.0431(3) 0.0295(3) 0.0013(2) -0.0008(2) -0.0006(2) N1 0.0242(8) 0.0319(9) 0.0254(9) -0.0011(7) 0.0030(7) -0.0032(7) N2 0.0239(9) 0.0391(10) 0.0273(9) 0.0015(8) 0.0063(7) 0.0027(7) N3 0.0217(8) 0.0350(10) 0.0274(9) 0.0013(7) 0.0049(7) 0.0018(7) N4 0.0232(8) 0.0338(9) 0.0294(9) 0.0023(7) 0.0033(7) -0.0025(7) C1 0.0340(11) 0.0334(12) 0.0321(12) -0.0031(9) 0.0064(9) -0.0017(9) C2 0.0349(12) 0.0340(12) 0.0311(11) -0.0033(9) 0.0088(9) 0.0025(9) C3 0.0282(11) 0.0322(12) 0.0438(13) -0.0045(10) 0.0041(9) -0.0015(9) C4 0.0253(11) 0.0442(14) 0.0642(18) -0.0054(12) 0.0074(11) -0.0064(10) C5 0.0369(14) 0.0525(16) 0.0672(19) 0.0005(14) 0.0231(13) -0.0109(11) C6 0.0479(15) 0.0444(14) 0.0468(15) 0.0025(11) 0.0192(12) -0.0085(11) C7 0.0353(12) 0.0330(12) 0.0348(12) -0.0019(9) 0.0102(10) -0.0026(9) C8 0.0280(11) 0.0317(11) 0.0329(12) -0.0029(9) 0.0091(9) -0.0028(8) C9 0.0325(12) 0.0422(13) 0.0449(14) -0.0025(11) -0.0063(10) -0.0058(10) C10 0.0423(15) 0.0504(16) 0.073(2) 0.0091(14) -0.0141(13) -0.0051(12) C11 0.0653(19) 0.072(2) 0.0424(16) -0.0152(14) -0.0079(13) 0.0129(15) C12 0.0413(13) 0.0389(13) 0.0315(12) 0.0051(9) 0.0047(10) -0.0002(10) C13 0.0606(17) 0.0573(17) 0.0346(14) 0.0068(12) 0.0046(12) -0.0003(13) C14 0.0557(16) 0.0465(15) 0.0576(17) 0.0060(13) 0.0013(13) 0.0078(12) C15 0.0307(12) 0.0557(15) 0.0341(13) 0.0018(11) 0.0091(10) 0.0061(10) C16 0.0433(14) 0.0738(19) 0.0360(14) 0.0048(12) 0.0175(11) 0.0138(13) C17 0.0357(13) 0.0717(18) 0.0486(16) 0.0153(13) 0.0223(12) 0.0193(12) C18 0.0271(12) 0.0654(17) 0.0513(16) 0.0145(13) 0.0087(11) 0.0102(11) C19 0.0263(11) 0.0540(15) 0.0397(13) 0.0057(11) 0.0081(10) 0.0054(10) C20 0.0270(11) 0.0401(12) 0.0340(12) 0.0034(9) 0.0110(9) 0.0060(9) C21 0.0236(12) 0.126(3) 0.0371(15) -0.0027(16) 0.0017(10) 0.0082(14) C22 0.091(3) 0.086(3) 0.065(2) -0.0086(18) -0.0208(19) 0.004(2) C23 0.218(6) 0.157(4) 0.052(2) 0.053(3) -0.039(3) -0.097(4) C24 0.0361(13) 0.092(2) 0.0303(13) -0.0055(13) 0.0070(10) 0.0010(13) C25 0.070(2) 0.107(3) 0.0523(19) -0.0195(18) 0.0095(16) -0.0197(19) C26 0.0433(16) 0.131(3) 0.0426(16) 0.0175(18) 0.0045(13) 0.0137(17) C27 0.0271(11) 0.0331(12) 0.0356(12) 0.0047(9) 0.0037(9) 0.0042(9) C28 0.0277(11) 0.0317(11) 0.0381(12) 0.0029(9) 0.0051(9) 0.0003(9) C29 0.0278(11) 0.0345(11) 0.0345(12) 0.0025(9) 0.0043(9) 0.0021(9) C30 0.0330(12) 0.0450(13) 0.0347(12) 0.0017(10) -0.0024(10) 0.0025(10) C31 0.0236(11) 0.0471(14) 0.0486(15) -0.0022(11) -0.0023(10) 0.0021(10) C32 0.0237(11) 0.0515(15) 0.0455(14) -0.0029(11) 0.0089(10) -0.0002(10) C33 0.0246(10) 0.0403(13) 0.0359(12) -0.0016(10) 0.0068(9) -0.0002(9) C34 0.0215(10) 0.0313(11) 0.0339(12) 0.0008(9) 0.0021(8) 0.0014(8) C35 0.0324(12) 0.0615(16) 0.0320(12) 0.0025(11) 0.0046(10) 0.0065(11) C36 0.0609(18) 0.077(2) 0.0444(16) -0.0081(14) 0.0197(14) 0.0051(15) C37 0.069(2) 0.075(2) 0.0591(18) 0.0157(16) 0.0304(15) -0.0028(16) C38 0.0263(11) 0.0583(15) 0.0356(13) -0.0032(11) 0.0079(9) -0.0001(10) C39 0.0628(18) 0.073(2) 0.0431(16) 0.0077(14) 0.0138(14) -0.0005(15) C40 0.0603(18) 0.074(2) 0.0525(17) -0.0209(15) -0.0010(14) 0.0114(15) C41 0.0300(12) 0.0373(13) 0.0536(15) 0.0097(11) 0.0092(10) 0.0002(9) C42 0.0316(13) 0.0525(16) 0.082(2) 0.0131(14) 0.0177(13) -0.0013(11) C43 0.0286(13) 0.0567(18) 0.099(2) 0.0059(16) 0.0021(15) -0.0124(12) C44 0.0411(15) 0.0479(16) 0.072(2) -0.0007(14) -0.0144(14) -0.0096(12) C45 0.0320(12) 0.0336(12) 0.0508(15) 0.0040(10) -0.0045(10) -0.0036(9) C46 0.0228(10) 0.0334(12) 0.0425(13) 0.0058(10) 0.0005(9) -0.0022(8) C47 0.0385(13) 0.0534(15) 0.0473(15) 0.0109(12) 0.0178(11) 0.0035(11) C48 0.0608(18) 0.074(2) 0.0651(19) 0.0116(16) 0.0359(15) 0.0105(15) C49 0.0612(18) 0.084(2) 0.0477(17) 0.0159(15) 0.0156(14) 0.0199(16) C50 0.0523(15) 0.0418(14) 0.0400(14) -0.0030(11) -0.0048(11) -0.0089(11) C51 0.088(2) 0.079(2) 0.0485(18) 0.0021(16) -0.0186(16) -0.0237(18) C52 0.090(2) 0.0518(17) 0.067(2) -0.0148(15) 0.0185(17) -0.0009(16) _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 Cr1 N3 1.9234(17) . ? Cr1 N1 1.9242(18) . ? Cr1 Cr2 1.9305(8) . ? Cr1 S1 2.2614(10) . ? Cr2 N4 1.9179(18) . ? Cr2 N2 1.9263(18) . ? Cr2 S2 2.2753(10) . ? S1 S2 2.0513(10) . ? N1 C1 1.360(3) . ? N1 C8 1.456(3) . ? N2 C2 1.364(3) . ? N2 C20 1.454(3) . ? N3 C27 1.353(3) . ? N3 C34 1.455(2) . ? N4 C28 1.363(3) . ? N4 C46 1.461(3) . ? C1 C2 1.366(3) . ? C3 C4 1.403(3) . ? C3 C8 1.407(3) . ? C3 C9 1.520(3) . ? C4 C5 1.368(4) . ? C5 C6 1.385(4) . ? C6 C7 1.394(3) . ? C7 C8 1.404(3) . ? C7 C12 1.522(3) . ? C9 C10 1.523(3) . ? C9 C11 1.543(4) . ? C12 C13 1.517(3) . ? C12 C14 1.538(3) . ? C15 C16 1.393(3) . ? C15 C20 1.403(3) . ? C15 C24 1.524(3) . ? C16 C17 1.372(4) . ? C17 C18 1.368(4) . ? C18 C19 1.391(3) . ? C19 C20 1.411(3) . ? C19 C21 1.503(3) . ? C21 C22 1.511(4) . ? C21 C23 1.515(5) . ? C24 C25 1.530(4) . ? C24 C26 1.538(4) . ? C27 C28 1.367(3) . ? C29 C30 1.390(3) . ? C29 C34 1.403(3) . ? C29 C35 1.533(3) . ? C30 C31 1.378(3) . ? C31 C32 1.377(3) . ? C32 C33 1.399(3) . ? C33 C34 1.409(3) . ? C33 C38 1.513(3) . ? C35 C37 1.518(4) . ? C35 C36 1.521(4) . ? C38 C39 1.527(4) . ? C38 C40 1.534(4) . ? C41 C42 1.394(3) . ? C41 C46 1.412(3) . ? C41 C47 1.513(4) . ? C42 C43 1.378(4) . ? C43 C44 1.376(4) . ? C44 C45 1.395(3) . ? C45 C46 1.410(3) . ? C45 C50 1.526(4) . ? C47 C48 1.535(3) . ? C47 C49 1.548(4) . ? C50 C52 1.525(4) . ? C50 C51 1.528(4) . ? 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 N3 Cr1 N1 136.02(7) . . ? N3 Cr1 Cr2 104.55(5) . . ? N1 Cr1 Cr2 102.44(5) . . ? N3 Cr1 S1 107.80(6) . . ? N1 Cr1 S1 105.91(5) . . ? Cr2 Cr1 S1 90.69(2) . . ? N4 Cr2 N2 134.42(7) . . ? N4 Cr2 Cr1 102.77(5) . . ? N2 Cr2 Cr1 104.52(5) . . ? N4 Cr2 S2 104.93(5) . . ? N2 Cr2 S2 110.86(6) . . ? Cr1 Cr2 S2 89.96(2) . . ? S2 S1 Cr1 87.38(3) . . ? S1 S2 Cr2 87.31(3) . . ? C1 N1 C8 113.43(17) . . ? C1 N1 Cr1 130.73(14) . . ? C8 N1 Cr1 115.47(13) . . ? C2 N2 C20 110.80(17) . . ? C2 N2 Cr2 128.23(14) . . ? C20 N2 Cr2 120.94(14) . . ? C27 N3 C34 111.72(16) . . ? C27 N3 Cr1 128.58(14) . . ? C34 N3 Cr1 119.70(13) . . ? C28 N4 C46 112.49(17) . . ? C28 N4 Cr2 130.78(14) . . ? C46 N4 Cr2 116.68(13) . . ? N1 C1 C2 124.6(2) . . ? N2 C2 C1 124.27(19) . . ? C4 C3 C8 117.4(2) . . ? C4 C3 C9 120.9(2) . . ? C8 C3 C9 121.62(19) . . ? C5 C4 C3 121.3(2) . . ? C4 C5 C6 120.4(2) . . ? C5 C6 C7 120.9(2) . . ? C6 C7 C8 118.0(2) . . ? C6 C7 C12 119.6(2) . . ? C8 C7 C12 122.38(19) . . ? C7 C8 C3 121.69(19) . . ? C7 C8 N1 118.52(18) . . ? C3 C8 N1 119.79(19) . . ? C3 C9 C10 113.3(2) . . ? C3 C9 C11 110.2(2) . . ? C10 C9 C11 108.8(2) . . ? C13 C12 C7 112.8(2) . . ? C13 C12 C14 110.4(2) . . ? C7 C12 C14 110.14(19) . . ? C16 C15 C20 117.8(2) . . ? C16 C15 C24 118.6(2) . . ? C20 C15 C24 123.62(19) . . ? C17 C16 C15 121.3(2) . . ? C18 C17 C16 120.2(2) . . ? C17 C18 C19 121.7(2) . . ? C18 C19 C20 117.4(2) . . ? C18 C19 C21 120.1(2) . . ? C20 C19 C21 122.33(19) . . ? C15 C20 C19 121.47(19) . . ? C15 C20 N2 118.95(19) . . ? C19 C20 N2 119.4(2) . . ? C19 C21 C22 114.6(3) . . ? C19 C21 C23 109.7(3) . . ? C22 C21 C23 110.1(3) . . ? C15 C24 C25 111.6(2) . . ? C15 C24 C26 111.5(2) . . ? C25 C24 C26 111.1(2) . . ? N3 C27 C28 124.51(19) . . ? N4 C28 C27 124.2(2) . . ? C30 C29 C34 118.3(2) . . ? C30 C29 C35 119.2(2) . . ? C34 C29 C35 122.55(18) . . ? C31 C30 C29 121.0(2) . . ? C30 C31 C32 120.3(2) . . ? C31 C32 C33 121.4(2) . . ? C32 C33 C34 117.4(2) . . ? C32 C33 C38 119.92(19) . . ? C34 C33 C38 122.62(18) . . ? C29 C34 C33 121.60(18) . . ? C29 C34 N3 118.42(18) . . ? C33 C34 N3 119.82(19) . . ? C37 C35 C36 110.1(2) . . ? C37 C35 C29 111.5(2) . . ? C36 C35 C29 112.3(2) . . ? C33 C38 C39 111.0(2) . . ? C33 C38 C40 112.4(2) . . ? C39 C38 C40 110.0(2) . . ? C42 C41 C46 117.2(2) . . ? C42 C41 C47 120.1(2) . . ? C46 C41 C47 122.6(2) . . ? C43 C42 C41 121.6(3) . . ? C42 C43 C44 120.2(2) . . ? C43 C44 C45 121.6(3) . . ? C44 C45 C46 117.3(2) . . ? C44 C45 C50 119.5(2) . . ? C46 C45 C50 123.1(2) . . ? C45 C46 C41 122.0(2) . . ? C45 C46 N4 118.79(19) . . ? C41 C46 N4 119.10(19) . . ? C41 C47 C48 113.5(2) . . ? C41 C47 C49 110.8(2) . . ? C48 C47 C49 108.8(2) . . ? C52 C50 C51 110.0(2) . . ? C52 C50 C45 109.8(2) . . ? C51 C50 C45 113.3(2) . . ? 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 C8 N1 C1 C2 174.4(2) . . . . ? Cr1 N1 C1 C2 1.8(3) . . . . ? C20 N2 C2 C1 171.2(2) . . . . ? Cr2 N2 C2 C1 -10.9(3) . . . . ? N1 C1 C2 N2 -5.2(4) . . . . ? C8 C3 C4 C5 1.7(3) . . . . ? C9 C3 C4 C5 -175.2(2) . . . . ? C3 C4 C5 C6 2.3(4) . . . . ? C4 C5 C6 C7 -2.3(4) . . . . ? C5 C6 C7 C8 -1.7(3) . . . . ? C5 C6 C7 C12 176.1(2) . . . . ? C6 C7 C8 C3 5.9(3) . . . . ? C12 C7 C8 C3 -171.8(2) . . . . ? C6 C7 C8 N1 -174.96(19) . . . . ? C12 C7 C8 N1 7.3(3) . . . . ? C4 C3 C8 C7 -5.9(3) . . . . ? C9 C3 C8 C7 171.1(2) . . . . ? C4 C3 C8 N1 174.96(19) . . . . ? C9 C3 C8 N1 -8.1(3) . . . . ? C1 N1 C8 C7 -81.4(2) . . . . ? Cr1 N1 C8 C7 92.4(2) . . . . ? C1 N1 C8 C3 97.8(2) . . . . ? Cr1 N1 C8 C3 -88.4(2) . . . . ? C4 C3 C9 C10 -26.3(3) . . . . ? C8 C3 C9 C10 156.9(2) . . . . ? C4 C3 C9 C11 95.9(3) . . . . ? C8 C3 C9 C11 -80.9(3) . . . . ? C6 C7 C12 C13 43.2(3) . . . . ? C8 C7 C12 C13 -139.1(2) . . . . ? C6 C7 C12 C14 -80.7(3) . . . . ? C8 C7 C12 C14 97.0(2) . . . . ? C20 C15 C16 C17 1.5(4) . . . . ? C24 C15 C16 C17 -179.1(3) . . . . ? C15 C16 C17 C18 0.2(4) . . . . ? C16 C17 C18 C19 -1.8(4) . . . . ? C17 C18 C19 C20 1.6(4) . . . . ? C17 C18 C19 C21 -173.7(3) . . . . ? C16 C15 C20 C19 -1.6(4) . . . . ? C24 C15 C20 C19 179.0(2) . . . . ? C16 C15 C20 N2 173.6(2) . . . . ? C24 C15 C20 N2 -5.8(4) . . . . ? C18 C19 C20 C15 0.1(4) . . . . ? C21 C19 C20 C15 175.4(2) . . . . ? C18 C19 C20 N2 -175.0(2) . . . . ? C21 C19 C20 N2 0.2(4) . . . . ? C2 N2 C20 C15 -65.6(3) . . . . ? Cr2 N2 C20 C15 116.3(2) . . . . ? C2 N2 C20 C19 109.7(2) . . . . ? Cr2 N2 C20 C19 -68.4(2) . . . . ? C18 C19 C21 C22 -46.9(4) . . . . ? C20 C19 C21 C22 138.0(3) . . . . ? C18 C19 C21 C23 77.4(4) . . . . ? C20 C19 C21 C23 -97.7(3) . . . . ? C16 C15 C24 C25 -68.6(3) . . . . ? C20 C15 C24 C25 110.8(3) . . . . ? C16 C15 C24 C26 56.1(3) . . . . ? C20 C15 C24 C26 -124.5(3) . . . . ? C34 N3 C27 C28 170.2(2) . . . . ? Cr1 N3 C27 C28 -10.3(3) . . . . ? C46 N4 C28 C27 -178.8(2) . . . . ? Cr2 N4 C28 C27 3.9(3) . . . . ? N3 C27 C28 N4 -6.1(4) . . . . ? C34 C29 C30 C31 2.0(3) . . . . ? C35 C29 C30 C31 -179.1(2) . . . . ? C29 C30 C31 C32 -0.5(4) . . . . ? C30 C31 C32 C33 -1.4(4) . . . . ? C31 C32 C33 C34 1.7(3) . . . . ? C31 C32 C33 C38 -176.1(2) . . . . ? C30 C29 C34 C33 -1.7(3) . . . . ? C35 C29 C34 C33 179.5(2) . . . . ? C30 C29 C34 N3 173.67(19) . . . . ? C35 C29 C34 N3 -5.2(3) . . . . ? C32 C33 C34 C29 -0.1(3) . . . . ? C38 C33 C34 C29 177.6(2) . . . . ? C32 C33 C34 N3 -175.39(19) . . . . ? C38 C33 C34 N3 2.3(3) . . . . ? C27 N3 C34 C29 -77.4(2) . . . . ? Cr1 N3 C34 C29 103.03(19) . . . . ? C27 N3 C34 C33 98.0(2) . . . . ? Cr1 N3 C34 C33 -81.6(2) . . . . ? C30 C29 C35 C37 -73.6(3) . . . . ? C34 C29 C35 C37 105.2(3) . . . . ? C30 C29 C35 C36 50.5(3) . . . . ? C34 C29 C35 C36 -130.7(2) . . . . ? C32 C33 C38 C39 -76.8(3) . . . . ? C34 C33 C38 C39 105.6(2) . . . . ? C32 C33 C38 C40 47.0(3) . . . . ? C34 C33 C38 C40 -130.6(2) . . . . ? C46 C41 C42 C43 1.1(4) . . . . ? C47 C41 C42 C43 -175.6(2) . . . . ? C41 C42 C43 C44 1.2(4) . . . . ? C42 C43 C44 C45 -1.3(4) . . . . ? C43 C44 C45 C46 -0.9(4) . . . . ? C43 C44 C45 C50 174.8(2) . . . . ? C44 C45 C46 C41 3.2(3) . . . . ? C50 C45 C46 C41 -172.2(2) . . . . ? C44 C45 C46 N4 179.9(2) . . . . ? C50 C45 C46 N4 4.5(3) . . . . ? C42 C41 C46 C45 -3.3(3) . . . . ? C47 C41 C46 C45 173.2(2) . . . . ? C42 C41 C46 N4 180.0(2) . . . . ? C47 C41 C46 N4 -3.5(3) . . . . ? C28 N4 C46 C45 -83.8(2) . . . . ? Cr2 N4 C46 C45 93.9(2) . . . . ? C28 N4 C46 C41 93.0(2) . . . . ? Cr2 N4 C46 C41 -89.3(2) . . . . ? C42 C41 C47 C48 -29.1(3) . . . . ? C46 C41 C47 C48 154.4(2) . . . . ? C42 C41 C47 C49 93.6(3) . . . . ? C46 C41 C47 C49 -82.9(3) . . . . ? C44 C45 C50 C52 -76.5(3) . . . . ? C46 C45 C50 C52 98.9(3) . . . . ? C44 C45 C50 C51 46.9(3) . . . . ? C46 C45 C50 C51 -137.7(2) . . . . ? _refine_diff_density_max 0.581 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.072 _shelxl_version_number 2013-2 _shelx_res_file ; TITL kla0119 in P2(1)/n CELL 0.71073 13.7027 19.3110 19.5576 90.000 99.039 90.000 ZERR 4.00 0.0046 0.0065 0.0065 0.000 0.006 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N S Cr UNIT 208 288 16 8 8 L.S. 10 ACTA CONF WPDB BOND FMAP 2 PLAN 20 SIZE 0.085 0.277 0.298 TEMP -73 OMIT 0 1 1 WGHT 0.066500 0.607100 FVAR 0.18773 MOLE 1 CR1 5 0.114588 0.177235 0.211606 11.00000 0.02226 0.03033 = 0.02527 0.00038 0.00433 0.00016 CR2 5 -0.024047 0.165449 0.216487 11.00000 0.02161 0.03139 = 0.02688 0.00116 0.00326 0.00042 S1 4 0.085493 0.159987 0.095821 11.00000 0.03676 0.04204 = 0.02804 -0.00317 0.00710 0.00135 S2 4 -0.060589 0.179779 0.099789 11.00000 0.03281 0.04311 = 0.02949 0.00134 -0.00081 -0.00058 N1 3 0.132373 0.275483 0.224392 11.00000 0.02416 0.03193 = 0.02541 -0.00109 0.00300 -0.00315 N2 3 -0.059140 0.246696 0.264352 11.00000 0.02393 0.03914 = 0.02728 0.00149 0.00634 0.00266 N3 3 0.176331 0.095050 0.253918 11.00000 0.02166 0.03500 = 0.02739 0.00134 0.00492 0.00177 N4 3 -0.034614 0.067675 0.230921 11.00000 0.02318 0.03377 = 0.02936 0.00232 0.00334 -0.00247 C1 1 0.073227 0.324021 0.247237 11.00000 0.03403 0.03341 = 0.03211 -0.00309 0.00644 -0.00175 AFIX 43 H1 2 0.094879 0.370805 0.248585 11.00000 -1.20000 AFIX 0 C2 1 -0.015125 0.310221 0.268380 11.00000 0.03489 0.03404 = 0.03110 -0.00332 0.00882 0.00248 AFIX 43 H2 2 -0.048073 0.347290 0.287115 11.00000 -1.20000 AFIX 0 C3 1 0.309747 0.306953 0.242224 11.00000 0.02821 0.03215 = 0.04381 -0.00454 0.00410 -0.00151 C4 1 0.391122 0.330452 0.213290 11.00000 0.02528 0.04425 = 0.06417 -0.00537 0.00742 -0.00637 AFIX 43 H4 2 0.454602 0.331300 0.241001 11.00000 -1.20000 AFIX 0 C5 1 0.380886 0.352173 0.145956 11.00000 0.03689 0.05250 = 0.06725 0.00050 0.02314 -0.01089 AFIX 43 H5 2 0.437453 0.366283 0.127015 11.00000 -1.20000 AFIX 0 C6 1 0.288605 0.353726 0.105229 11.00000 0.04791 0.04443 = 0.04678 0.00251 0.01916 -0.00848 AFIX 43 H6 2 0.282206 0.370529 0.059087 11.00000 -1.20000 AFIX 0 C7 1 0.204974 0.330956 0.131053 11.00000 0.03527 0.03300 = 0.03481 -0.00187 0.01017 -0.00259 C8 1 0.217663 0.304735 0.198806 11.00000 0.02798 0.03166 = 0.03294 -0.00291 0.00909 -0.00280 C9 1 0.320423 0.288198 0.318517 11.00000 0.03245 0.04220 = 0.04493 -0.00253 -0.00627 -0.00580 AFIX 13 H9 2 0.274498 0.248918 0.323479 11.00000 -1.20000 AFIX 0 C10 1 0.424659 0.265751 0.349316 11.00000 0.04228 0.05042 = 0.07313 0.00907 -0.01408 -0.00508 AFIX 137 H10A 2 0.447370 0.229960 0.319957 11.00000 -1.50000 H10B 2 0.424510 0.247131 0.395913 11.00000 -1.50000 H10C 2 0.469154 0.305721 0.351893 11.00000 -1.50000 AFIX 0 C11 1 0.290286 0.350105 0.360488 11.00000 0.06527 0.07239 = 0.04240 -0.01517 -0.00791 0.01294 AFIX 137 H11A 2 0.329085 0.390907 0.351836 11.00000 -1.50000 H11B 2 0.302798 0.338843 0.409951 11.00000 -1.50000 H11C 2 0.219830 0.359889 0.346339 11.00000 -1.50000 AFIX 0 C12 1 0.103735 0.337627 0.086684 11.00000 0.04128 0.03893 = 0.03147 0.00514 0.00468 -0.00025 AFIX 13 H12 2 0.057518 0.305875 0.106270 11.00000 -1.20000 AFIX 0 C13 1 0.103982 0.316899 0.011873 11.00000 0.06060 0.05734 = 0.03463 0.00680 0.00455 -0.00034 AFIX 137 H13A 2 0.136946 0.352885 -0.011481 11.00000 -1.50000 H13B 2 0.035773 0.311456 -0.011590 11.00000 -1.50000 H13C 2 0.139386 0.272967 0.010372 11.00000 -1.50000 AFIX 0 C14 1 0.064518 0.411923 0.090682 11.00000 0.05569 0.04654 = 0.05763 0.00602 0.00131 0.00784 AFIX 137 H14A 2 0.067339 0.425246 0.139304 11.00000 -1.50000 H14B 2 -0.004037 0.414127 0.067136 11.00000 -1.50000 H14C 2 0.105268 0.443725 0.068154 11.00000 -1.50000 AFIX 0 C15 1 -0.128817 0.255624 0.372618 11.00000 0.03065 0.05574 = 0.03406 0.00183 0.00910 0.00609 C16 1 -0.211814 0.262317 0.405117 11.00000 0.04333 0.07385 = 0.03600 0.00476 0.01748 0.01381 AFIX 43 H16 2 -0.203330 0.269633 0.453725 11.00000 -1.20000 AFIX 0 C17 1 -0.305571 0.258554 0.368318 11.00000 0.03575 0.07167 = 0.04860 0.01527 0.02234 0.01926 AFIX 43 H17 2 -0.361102 0.263420 0.391531 11.00000 -1.20000 AFIX 0 C18 1 -0.319337 0.247822 0.298343 11.00000 0.02708 0.06540 = 0.05126 0.01451 0.00867 0.01020 AFIX 43 H18 2 -0.384716 0.244004 0.273860 11.00000 -1.20000 AFIX 0 C19 1 -0.240078 0.242350 0.262078 11.00000 0.02628 0.05400 = 0.03966 0.00565 0.00809 0.00542 C20 1 -0.144094 0.246479 0.300538 11.00000 0.02696 0.04005 = 0.03397 0.00340 0.01095 0.00597 C21 1 -0.258279 0.237877 0.184383 11.00000 0.02356 0.12614 = 0.03711 -0.00272 0.00168 0.00821 AFIX 13 H21 2 -0.195192 0.222556 0.169416 11.00000 -1.20000 AFIX 0 C22 1 -0.337530 0.186842 0.155129 11.00000 0.09125 0.08553 = 0.06481 -0.00864 -0.02076 0.00427 AFIX 137 H22A 2 -0.324705 0.142092 0.178442 11.00000 -1.50000 H22B 2 -0.337067 0.181099 0.105395 11.00000 -1.50000 H22C 2 -0.402223 0.204233 0.162575 11.00000 -1.50000 AFIX 0 C23 1 -0.282467 0.309101 0.153897 11.00000 0.21770 0.15652 = 0.05241 0.05285 -0.03906 -0.09695 AFIX 137 H23A 2 -0.352409 0.319339 0.154358 11.00000 -1.50000 H23B 2 -0.269136 0.310227 0.106125 11.00000 -1.50000 H23C 2 -0.241503 0.343813 0.181487 11.00000 -1.50000 AFIX 0 C24 1 -0.026893 0.259266 0.416756 11.00000 0.03615 0.09192 = 0.03031 -0.00551 0.00699 0.00100 AFIX 13 H24 2 0.022879 0.248201 0.386054 11.00000 -1.20000 AFIX 0 C25 1 -0.004157 0.332057 0.445782 11.00000 0.07017 0.10744 = 0.05228 -0.01951 0.00950 -0.01971 AFIX 137 H25A 2 -0.011719 0.365556 0.407674 11.00000 -1.50000 H25B 2 0.063820 0.333606 0.470473 11.00000 -1.50000 H25C 2 -0.050007 0.343646 0.477795 11.00000 -1.50000 AFIX 0 C26 1 -0.015532 0.205051 0.475093 11.00000 0.04330 0.13092 = 0.04256 0.01746 0.00449 0.01367 AFIX 137 H26A 2 0.050256 0.209159 0.502883 11.00000 -1.50000 H26B 2 -0.023620 0.158550 0.454932 11.00000 -1.50000 H26C 2 -0.065996 0.212905 0.504631 11.00000 -1.50000 AFIX 0 C27 1 0.135592 0.032125 0.260839 11.00000 0.02711 0.03308 = 0.03558 0.00474 0.00375 0.00418 AFIX 43 H27 2 0.178795 -0.005138 0.276187 11.00000 -1.20000 AFIX 0 C28 1 0.036547 0.018461 0.247272 11.00000 0.02770 0.03166 = 0.03814 0.00291 0.00511 0.00028 AFIX 43 H28 2 0.015976 -0.028366 0.249375 11.00000 -1.20000 AFIX 0 C29 1 0.306822 0.100619 0.355343 11.00000 0.02776 0.03453 = 0.03455 0.00254 0.00429 0.00213 C30 1 0.406070 0.094742 0.383591 11.00000 0.03296 0.04496 = 0.03474 0.00167 -0.00238 0.00252 AFIX 43 H30 2 0.424941 0.096131 0.432435 11.00000 -1.20000 AFIX 0 C31 1 0.477552 0.086928 0.341846 11.00000 0.02361 0.04712 = 0.04855 -0.00222 -0.00230 0.00209 AFIX 43 H31 2 0.545093 0.083370 0.362052 11.00000 -1.20000 AFIX 0 C32 1 0.451443 0.084256 0.270951 11.00000 0.02369 0.05149 = 0.04554 -0.00286 0.00889 -0.00025 AFIX 43 H32 2 0.501635 0.079874 0.242791 11.00000 -1.20000 AFIX 0 C33 1 0.352514 0.087865 0.239550 11.00000 0.02460 0.04028 = 0.03588 -0.00156 0.00683 -0.00021 C34 1 0.280709 0.096200 0.283162 11.00000 0.02146 0.03127 = 0.03393 0.00077 0.00210 0.00140 C35 1 0.230143 0.110249 0.403785 11.00000 0.03242 0.06146 = 0.03205 0.00254 0.00464 0.00651 AFIX 13 H35 2 0.166106 0.123039 0.374564 11.00000 -1.20000 AFIX 0 C36 1 0.257639 0.168434 0.455664 11.00000 0.06089 0.07684 = 0.04443 -0.00815 0.01972 0.00506 AFIX 137 H36A 2 0.205906 0.173446 0.484682 11.00000 -1.50000 H36B 2 0.264161 0.211839 0.430814 11.00000 -1.50000 H36C 2 0.320566 0.157502 0.484918 11.00000 -1.50000 AFIX 0 C37 1 0.213563 0.043537 0.441426 11.00000 0.06900 0.07498 = 0.05913 0.01575 0.03039 -0.00280 AFIX 137 H37A 2 0.195595 0.006454 0.407581 11.00000 -1.50000 H37B 2 0.160062 0.050224 0.468656 11.00000 -1.50000 H37C 2 0.274332 0.030878 0.472335 11.00000 -1.50000 AFIX 0 C38 1 0.326039 0.080194 0.161846 11.00000 0.02629 0.05832 = 0.03565 -0.00317 0.00789 -0.00008 AFIX 13 H38 2 0.253221 0.071894 0.150908 11.00000 -1.20000 AFIX 0 C39 1 0.348799 0.146514 0.124857 11.00000 0.06284 0.07341 = 0.04308 0.00766 0.01384 -0.00051 AFIX 137 H39A 2 0.314699 0.185599 0.142662 11.00000 -1.50000 H39B 2 0.326087 0.141598 0.075024 11.00000 -1.50000 H39C 2 0.420217 0.154907 0.133144 11.00000 -1.50000 AFIX 0 C40 1 0.378184 0.018453 0.133941 11.00000 0.06031 0.07351 = 0.05249 -0.02086 -0.00101 0.01142 AFIX 137 H40A 2 0.449664 0.026582 0.141375 11.00000 -1.50000 H40B 2 0.354370 0.013101 0.084294 11.00000 -1.50000 H40C 2 0.363834 -0.023771 0.158324 11.00000 -1.50000 AFIX 0 C41 1 -0.187091 0.035992 0.276853 11.00000 0.03002 0.03726 = 0.05365 0.00970 0.00923 0.00023 C42 1 -0.281921 0.007834 0.264608 11.00000 0.03163 0.05251 = 0.08168 0.01309 0.01766 -0.00128 AFIX 43 H42 2 -0.319745 0.006153 0.301332 11.00000 -1.20000 AFIX 0 C43 1 -0.322107 -0.017614 0.200525 11.00000 0.02862 0.05669 = 0.09868 0.00593 0.00214 -0.01235 AFIX 43 H43 2 -0.387373 -0.035735 0.193310 11.00000 -1.20000 AFIX 0 C44 1 -0.267926 -0.016843 0.146952 11.00000 0.04110 0.04790 = 0.07232 -0.00070 -0.01441 -0.00959 AFIX 43 H44 2 -0.296104 -0.035453 0.103332 11.00000 -1.20000 AFIX 0 C45 1 -0.172650 0.010595 0.155138 11.00000 0.03203 0.03364 = 0.05084 0.00400 -0.00448 -0.00359 C46 1 -0.134270 0.038527 0.220453 11.00000 0.02277 0.03344 = 0.04247 0.00579 0.00053 -0.00218 C47 1 -0.142576 0.058674 0.349067 11.00000 0.03847 0.05338 = 0.04728 0.01086 0.01779 0.00353 AFIX 13 H47 2 -0.097657 0.098684 0.344647 11.00000 -1.20000 AFIX 0 C48 1 -0.219679 0.082294 0.393218 11.00000 0.06081 0.07427 = 0.06510 0.01164 0.03595 0.01054 AFIX 137 H48A 2 -0.263237 0.116937 0.367628 11.00000 -1.50000 H48B 2 -0.186067 0.102637 0.436497 11.00000 -1.50000 H48C 2 -0.258956 0.042387 0.403715 11.00000 -1.50000 AFIX 0 C49 1 -0.079779 -0.000116 0.387760 11.00000 0.06117 0.08351 = 0.04773 0.01588 0.01559 0.01988 AFIX 137 H49A 2 -0.121867 -0.040477 0.391759 11.00000 -1.50000 H49B 2 -0.050965 0.015869 0.434109 11.00000 -1.50000 H49C 2 -0.026759 -0.012948 0.361904 11.00000 -1.50000 AFIX 0 C50 1 -0.112434 0.004597 0.096034 11.00000 0.05230 0.04182 = 0.03997 -0.00296 -0.00478 -0.00888 AFIX 13 H50 2 -0.054609 0.036598 0.106285 11.00000 -1.20000 AFIX 0 C51 1 -0.170545 0.024834 0.025693 11.00000 0.08827 0.07855 = 0.04845 0.00214 -0.01860 -0.02375 AFIX 137 H51A 2 -0.125657 0.027033 -0.008627 11.00000 -1.50000 H51B 2 -0.201281 0.070239 0.029283 11.00000 -1.50000 H51C 2 -0.221966 -0.009792 0.011312 11.00000 -1.50000 AFIX 0 C52 1 -0.072737 -0.068902 0.092965 11.00000 0.08961 0.05178 = 0.06660 -0.01476 0.01848 -0.00089 AFIX 137 H52A 2 -0.033674 -0.080915 0.137757 11.00000 -1.50000 H52B 2 -0.030911 -0.071742 0.056760 11.00000 -1.50000 H52C 2 -0.128108 -0.101296 0.082407 11.00000 -1.50000 AFIX 0 HKLF 4 REM kla0119 in P2(1)/n REM R1 = 0.0475 for 8732 Fo > 4sig(Fo) and 0.0772 for all 12708 data REM 557 parameters refined using 0 restraints END WGHT 0.0623 0.8765 REM Highest difference peak 0.581, deepest hole -0.239, 1-sigma level 0.072 Q1 1 0.0474 0.2410 0.2490 11.00000 0.05 0.58 Q2 1 0.0603 0.1650 0.2357 11.00000 0.05 0.56 Q3 1 -0.3107 0.3180 0.1580 11.00000 0.05 0.56 Q4 1 0.0443 0.1773 0.2136 11.00000 0.05 0.53 Q5 1 0.0754 0.1076 0.2483 11.00000 0.05 0.48 Q6 1 -0.1945 0.2437 0.2815 11.00000 0.05 0.43 Q7 1 -0.0410 0.1167 0.2338 11.00000 0.05 0.40 Q8 1 -0.0385 0.2815 0.2588 11.00000 0.05 0.40 Q9 1 -0.2429 0.2778 0.1547 11.00000 0.05 0.37 Q10 1 0.1309 0.2352 0.2206 11.00000 0.05 0.36 Q11 1 0.2555 0.3219 0.2261 11.00000 0.05 0.35 Q12 1 -0.2710 0.2502 0.2764 11.00000 0.05 0.35 Q13 1 0.3202 0.0831 0.2636 11.00000 0.05 0.35 Q14 1 -0.0799 0.2576 0.3934 11.00000 0.05 0.35 Q15 1 0.1494 0.3398 0.1134 11.00000 0.05 0.35 Q16 1 0.0063 0.1156 0.2149 11.00000 0.05 0.35 Q17 1 0.0810 0.2255 0.2228 11.00000 0.05 0.34 Q18 1 -0.0576 0.2177 0.2297 11.00000 0.05 0.34 Q19 1 0.1183 0.2983 0.2445 11.00000 0.05 0.33 Q20 1 0.0381 0.3021 0.2626 11.00000 0.05 0.33 ; _shelx_res_checksum 14059 _shelx_hkl_file ; -1 0 0 -0.17 0.12 -1 0 0 0.06 0.14 1 0 0 -0.03 0.15 -1 0 0 0.10 0.13 1 0 0 -0.11 0.14 -2 0 0 74.43 5.70 2 0 0 84.08 5.72 -2 0 0 81.74 5.73 2 0 0 75.59 5.65 -3 0 0 -0.54 0.43 3 0 0 -0.32 0.52 -3 0 0 0.35 0.36 3 0 0 0.00 0.45 -4 0 0 25.36 1.92 -4 0 0 19.65 2.03 4 0 0 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4.83 1.44 4 -11 5 2.43 1.18 4 11 5 4.09 1.39 4 11 5 1.10 1.10 -4 11 -5 3.25 1.31 5 -11 5 64.55 5.78 5 11 5 69.18 5.96 -5 11 -5 67.77 6.02 5 11 5 73.12 6.03 -5 -11 -5 70.27 5.79 5 -11 5 63.88 5.82 6 11 5 24.52 3.15 -6 11 -5 22.61 2.99 6 -11 5 24.19 3.05 -6 -11 -5 20.92 2.87 6 -11 5 28.76 3.15 6 11 5 25.93 3.01 -7 11 -5 47.78 4.58 7 11 5 42.92 4.64 7 -11 5 36.26 4.38 -7 -11 -5 44.86 4.45 7 11 5 51.68 4.54 7 -11 5 48.22 4.63 -8 11 -5 73.47 6.94 8 -11 5 75.91 6.99 -8 -11 -5 82.73 7.02 8 11 5 92.07 7.02 8 -11 5 84.24 7.05 8 11 5 80.56 7.10 -8 11 -5 73.41 7.00 -9 -11 -5 1.43 1.60 9 11 5 -0.05 1.80 9 -11 5 -0.33 1.61 -9 11 -5 -0.61 1.37 9 11 5 -0.11 1.65 -9 11 -5 -0.33 1.57 -10 11 -5 17.26 3.21 -10 11 -5 17.65 3.01 10 -11 5 25.05 3.54 -10 -11 -5 19.25 3.23 10 11 5 25.59 3.56 11 11 5 14.20 3.18 11 -11 5 14.14 2.82 -11 11 -5 9.09 2.56 -11 -11 -5 14.57 2.84 -11 11 -5 11.76 3.15 12 -11 5 22.78 4.35 -12 11 -5 36.40 4.34 12 11 5 27.70 4.37 -12 11 -5 25.20 4.48 -12 -11 -5 26.26 4.08 -13 -11 -5 19.46 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8 -12 -5 43.70 3.83 -8 -12 5 31.50 4.10 -8 12 5 37.26 4.01 -7 12 5 10.11 2.02 7 -12 -5 13.89 2.21 7 12 -5 7.33 1.97 7 12 -5 12.63 1.96 7 -12 -5 9.48 1.81 -7 -12 5 11.19 2.24 -7 12 5 10.32 2.06 -7 -12 5 11.40 1.85 -6 -12 5 -1.08 1.20 -6 12 5 -0.98 1.03 6 -12 -5 0.56 1.10 -6 12 5 1.57 1.30 6 -12 -5 1.47 1.12 -6 -12 5 0.63 1.11 6 12 -5 1.45 1.21 6 12 -5 0.68 1.25 -5 -12 5 4.82 1.27 5 12 -5 6.22 1.62 5 -12 -5 5.31 1.44 5 -12 -5 4.71 1.49 -5 12 5 5.19 1.55 -5 12 5 9.02 1.64 5 12 -5 5.40 1.58 -5 -12 5 4.54 1.51 4 -12 -5 102.82 8.69 -4 12 5 117.78 8.55 -4 -12 5 108.46 8.41 4 12 -5 125.05 8.97 4 12 -5 108.50 8.78 -4 12 5 105.48 8.96 -4 -12 5 119.05 8.90 4 -12 -5 112.02 8.62 -3 -12 5 90.11 6.97 3 12 -5 81.99 6.64 -3 -12 5 81.01 6.47 -3 12 5 87.39 7.07 3 -12 -5 83.59 6.76 -3 12 5 88.45 6.50 3 12 -5 79.10 6.92 3 -12 -5 84.31 6.71 2 -12 -5 141.03 11.20 2 12 -5 154.42 11.14 2 -12 -5 148.86 11.31 -2 12 5 149.33 10.93 -2 -12 5 161.53 11.09 -2 -12 5 135.63 11.36 2 12 -5 157.53 11.66 1 -12 -5 12.75 2.03 -1 12 5 14.99 2.24 -1 -12 5 12.38 1.75 1 12 -5 17.90 2.35 1 -12 -5 13.32 2.06 -1 12 5 13.68 1.58 1 12 -5 13.60 1.83 -1 -12 5 18.54 2.38 0 -12 -5 -0.39 0.91 0 12 5 0.08 1.04 0 -12 5 0.87 1.13 0 -12 5 -0.38 0.85 0 12 -5 -0.56 1.14 0 12 -5 0.35 0.86 0 -12 -5 0.65 1.16 -1 -12 -5 0.92 1.03 -1 12 -5 0.29 1.22 -1 12 -5 -0.89 0.79 -1 -12 -5 0.43 1.15 1 -12 5 0.95 1.16 1 -12 5 0.21 0.89 1 12 5 -0.14 1.12 -2 12 -5 32.07 3.61 -2 -12 -5 35.49 3.43 2 12 5 30.64 3.53 2 -12 5 32.75 3.46 2 12 5 32.75 3.50 2 -12 5 36.10 3.32 -2 12 -5 34.09 2.84 3 -12 5 22.15 2.68 -3 12 -5 26.59 2.97 3 -12 5 20.50 2.45 -3 -12 -5 13.98 2.39 3 12 5 20.83 2.72 3 12 5 21.04 2.76 -4 12 -5 25.14 3.02 4 12 5 17.09 2.69 4 12 5 17.89 2.74 -4 -12 -5 31.72 2.97 4 -12 5 28.88 2.86 4 -12 5 18.39 2.69 -5 12 -5 173.42 13.62 5 12 5 179.70 13.40 5 -12 5 158.40 13.16 -5 -12 -5 183.44 13.27 5 -12 5 188.62 13.43 -6 -12 -5 1.55 1.17 6 -12 5 0.90 1.23 6 -12 5 -0.40 1.38 -6 12 -5 0.86 1.22 6 12 5 0.71 1.31 6 12 5 0.10 1.42 7 12 5 108.54 9.12 -7 -12 -5 110.70 9.03 7 -12 5 109.02 9.09 7 -12 5 119.84 9.13 7 12 5 126.90 9.37 -7 12 -5 103.50 9.15 -8 -12 -5 0.99 1.41 8 -12 5 1.13 1.64 8 12 5 -1.93 1.43 -8 12 -5 0.86 1.44 8 12 5 -1.15 1.55 -8 12 -5 0.05 1.56 -9 12 -5 52.60 5.65 9 12 5 56.08 5.93 9 -12 5 52.38 5.65 -9 12 -5 65.27 6.01 9 12 5 67.81 5.90 -9 -12 -5 64.24 5.85 10 -12 5 0.46 2.03 -10 -12 -5 -0.13 1.78 -10 12 -5 -0.39 1.68 10 12 5 1.48 2.07 -10 12 -5 0.35 2.07 11 12 5 3.02 2.39 -11 12 -5 -0.26 2.26 11 -12 5 1.90 2.21 -11 -12 -5 2.21 2.27 -11 12 -5 0.45 2.14 -12 12 -5 2.76 2.80 -12 -12 -5 4.42 2.55 -12 12 -5 2.90 2.95 12 12 5 2.94 2.73 12 -12 5 2.33 2.63 13 -12 5 16.59 4.46 -13 -12 -5 24.20 4.22 13 12 5 20.98 4.51 -13 12 -5 16.48 4.46 -14 -12 -5 1.32 3.21 14 12 5 10.22 4.00 -14 12 -5 3.52 3.46 14 -12 5 2.03 3.53 15 -12 5 1.84 3.88 15 12 5 -4.38 3.19 -15 12 -5 -3.91 2.82 15 -13 -5 41.69 5.60 15 13 -5 27.02 5.21 -15 -13 5 26.47 5.26 -15 13 5 32.42 5.32 14 -13 -5 -0.20 2.89 -14 -13 5 -1.56 3.51 -14 13 5 -3.25 2.83 14 13 -5 0.50 3.42 -13 13 5 1.28 3.02 13 13 -5 1.49 2.73 -13 -13 5 2.72 2.92 13 -13 -5 -2.34 2.21 12 -13 -5 1.05 2.13 12 13 -5 0.02 2.30 -12 -13 5 2.48 2.67 -12 13 5 2.80 2.59 11 -13 -5 9.91 2.69 11 13 -5 16.34 3.29 -11 13 5 11.75 2.90 -11 -13 5 13.45 3.15 -10 13 5 30.02 4.04 10 13 -5 30.40 4.19 -10 -13 5 30.31 4.21 10 -13 -5 33.65 4.12 -10 13 5 37.85 4.01 -9 13 5 7.43 2.13 -9 -13 5 3.23 2.00 9 -13 -5 4.10 1.87 9 13 -5 4.38 2.01 -9 13 5 6.73 1.95 8 13 -5 16.36 2.47 8 13 -5 16.67 2.80 -8 13 5 16.03 2.55 8 -13 -5 7.94 2.15 -8 13 5 13.92 2.54 -8 -13 5 12.28 2.50 7 13 -5 38.12 4.19 7 -13 -5 42.46 4.26 7 -13 -5 46.88 3.95 7 13 -5 45.09 4.05 -7 13 5 39.83 4.16 -7 13 5 36.46 4.06 -7 -13 5 32.65 4.14 -6 13 5 9.11 1.89 6 -13 -5 8.63 1.85 6 -13 -5 8.47 1.76 6 13 -5 7.37 1.83 -6 13 5 7.78 1.82 6 13 -5 3.59 1.61 -6 -13 5 9.99 1.71 -6 -13 5 5.73 1.80 5 13 -5 24.64 2.85 5 -13 -5 25.47 2.66 -5 -13 5 22.76 2.35 -5 13 5 14.20 2.52 -5 13 5 18.41 2.45 -5 -13 5 21.54 2.89 5 13 -5 21.62 2.78 5 -13 -5 22.53 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28.73 3.61 -4 5 14 34.06 3.61 -4 5 14 38.60 3.73 4 5 -14 36.61 3.59 4 5 -14 38.37 3.68 3 5 -14 67.28 5.76 3 -5 -14 56.05 5.57 -3 -5 14 62.63 5.72 3 5 -14 61.68 5.45 -3 5 14 62.22 5.67 -3 5 14 75.67 5.69 -2 5 14 20.19 2.86 -2 5 14 19.13 2.68 2 5 -14 25.90 3.06 2 5 -14 23.85 2.70 -2 -5 14 23.80 2.97 2 -5 -14 25.86 2.94 -1 5 14 0.03 1.16 1 5 -14 0.32 1.29 1 5 -14 -0.04 1.14 1 -5 -14 -0.03 0.93 -1 -5 14 1.47 1.23 -1 5 14 0.48 1.13 0 -5 -14 27.06 3.44 0 -5 14 37.18 3.81 0 5 14 37.99 3.64 0 5 -14 36.03 3.36 0 5 14 33.16 3.76 0 5 -14 33.61 3.81 -1 -5 -14 8.78 1.81 -1 5 -14 10.47 2.13 -1 5 -14 12.38 1.80 1 5 14 14.52 2.24 1 -5 14 4.80 1.82 1 5 14 10.55 2.10 2 5 14 71.67 5.70 -2 5 -14 60.56 5.94 -2 5 -14 69.61 5.31 -2 -5 -14 59.47 5.60 2 5 14 53.68 5.77 2 -5 14 66.07 5.95 -3 5 -14 27.79 3.49 -3 -5 -14 23.65 3.08 3 -5 14 26.17 3.40 -3 5 -14 23.62 2.72 3 5 14 27.73 3.12 3 5 14 28.86 3.46 4 5 14 3.02 1.60 4 5 14 3.80 1.82 -4 -5 -14 0.13 1.26 -4 5 -14 6.25 1.85 4 -5 14 5.05 1.82 5 -5 14 15.80 2.77 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10.79 4.54 -6 4 25 10.92 4.35 6 -4 -25 13.98 4.67 -5 -4 25 8.00 3.93 5 -4 -25 13.57 4.51 5 4 -25 2.91 4.56 5 4 -25 6.15 3.94 -5 4 25 17.95 4.57 -5 4 25 12.60 4.01 -4 4 25 1.44 3.35 4 4 -25 4.23 3.83 4 -4 -25 -1.87 3.47 -4 4 25 2.73 3.70 4 4 -25 4.89 4.51 -4 -4 25 4.97 3.87 3 -4 -25 -4.23 3.28 3 4 -25 0.44 4.42 -3 4 25 0.87 3.17 -3 4 25 5.07 3.60 3 4 -25 -0.64 4.24 -3 -4 25 -3.79 3.18 2 -4 -25 -3.97 3.13 -2 4 25 0.26 3.89 2 4 -25 3.40 4.66 -2 -4 25 2.76 3.54 -2 4 25 2.36 3.25 -1 -4 25 2.66 4.71 1 -4 -25 2.07 3.48 -1 4 25 0.46 3.75 1 4 -25 -1.41 4.31 -1 4 25 0.14 3.32 0 4 -25 20.04 5.68 0 4 25 18.55 4.88 0 4 25 25.74 5.18 0 -4 -25 26.02 4.97 0 -4 25 20.14 5.03 1 -4 25 2.72 4.00 1 4 25 3.58 4.08 1 4 25 1.43 3.69 -1 4 -25 3.89 4.54 -1 -4 -25 6.71 4.08 -6 -5 25 1.39 4.31 6 5 -25 -0.19 3.72 6 -5 -25 2.82 4.39 -6 5 25 5.11 4.00 -6 5 25 0.74 4.12 -5 5 25 6.31 4.07 -5 5 25 9.07 3.74 5 -5 -25 16.21 4.70 5 5 -25 4.72 4.08 5 5 -25 8.47 5.24 -5 -5 25 11.94 4.45 4 5 -25 4.59 4.58 -4 -5 25 -3.44 3.34 4 -5 -25 -2.86 3.60 4 5 -25 -0.01 4.43 -4 5 25 0.09 3.44 -4 5 25 -1.41 3.02 -3 -5 25 2.48 3.63 -3 5 25 3.01 3.85 -3 5 25 -0.35 3.23 3 -5 -25 4.82 3.82 3 5 -25 -1.04 4.10 -2 -5 25 2.15 3.67 2 5 -25 3.57 4.25 -2 5 25 2.97 3.97 2 -5 -25 -0.57 3.66 -2 5 25 3.93 3.56 -1 5 25 38.06 5.94 -1 5 25 32.46 5.65 1 -5 -25 29.49 5.40 -1 -5 25 46.12 6.35 1 5 -25 39.59 6.32 0 5 25 31.22 5.30 0 -5 -25 22.47 5.15 0 5 -25 26.83 5.66 0 5 25 22.71 5.20 0 -5 25 28.15 5.28 -1 -5 -25 8.95 4.42 1 5 25 9.71 4.48 -5 -6 25 -0.89 4.03 -5 6 25 1.66 3.68 5 -6 -25 0.11 4.08 -5 6 25 -1.01 3.87 5 6 -25 -3.51 4.42 4 6 -25 -2.14 4.09 4 -6 -25 -0.46 3.89 -4 -6 25 -1.55 4.13 -4 6 25 5.11 3.55 -4 6 25 3.22 3.78 -3 -6 25 -6.14 3.55 -3 6 25 5.46 3.86 -3 6 25 -4.46 3.08 3 -6 -25 -0.79 3.81 3 6 -25 -1.45 3.89 2 -6 -25 -2.60 3.85 -2 -6 25 0.79 3.79 -2 6 25 2.47 3.65 2 6 -25 1.13 4.11 -2 6 25 4.48 3.90 1 -6 -25 0.27 3.92 -1 6 25 4.45 4.14 -1 6 25 4.03 3.81 -1 -6 25 -0.25 3.75 1 6 -25 -1.77 4.10 0 6 25 3.08 4.03 0 -6 -25 -1.10 4.04 0 6 -25 1.77 4.43 0 -6 25 0.66 4.13 -4 -7 25 2.87 4.61 4 7 -25 -0.74 4.28 -4 7 25 -4.63 3.26 -4 7 25 3.03 3.97 4 -7 -25 -1.96 3.98 -3 -7 25 -0.75 4.19 3 -7 -25 2.33 4.32 -3 7 25 5.23 3.89 -3 7 25 4.21 4.20 3 7 -25 -0.84 4.12 2 -7 -25 8.18 4.65 -2 7 25 4.86 4.38 -2 -7 25 9.43 4.79 2 7 -25 6.73 4.45 4 0 -26 50.96 6.68 -4 0 26 40.00 6.46 4 0 -26 49.95 7.42 3 0 -26 3.63 4.39 -3 0 26 1.02 3.80 3 0 -26 -3.03 4.89 -2 0 26 -1.18 3.63 2 0 -26 4.82 4.21 2 0 -26 -3.84 4.76 4 1 -26 -3.55 3.95 4 -1 -26 7.06 4.44 3 -1 -26 -2.19 5.02 3 1 -26 0.94 4.16 3 1 -26 -2.47 4.92 -3 1 26 3.46 3.71 3 -1 -26 -1.16 3.92 -3 -1 26 -1.82 3.67 -2 1 26 0.25 3.38 2 -1 -26 1.71 5.03 2 1 -26 -0.05 4.42 2 1 -26 -5.80 4.82 2 -1 -26 0.19 3.93 -2 -1 26 -2.62 3.48 3 -2 -26 -5.08 3.93 3 2 -26 3.33 4.48 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 14243 _database_code_depnum_ccdc_archive 'CCDC 971179' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_klat762d-sr # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.072 0.500 0.500 505 113 2(pentane) _platon_squeeze_details ; PLATON Reference : Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13. Spek, A.L. (2009). Acta Cryst. D65, 148-155. Void space analysis consistent with initial solutions showing two severely disordered pentane molecules in the unit cell. ; # start Validation Reply Form _vrf_CHEMW03_klat762d-sr ; PROBLEM: WARNING: The ratio of given/expected molecular weight as RESPONSE: see _platon_squeeze_details ; _vrf_PLAT220_klat762d-sr ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.4 Ratio RESPONSE: Isopropyl groups have unresolvable disorder leading to large C Ueq range. ; _vrf_PLAT230_klat762d-sr ; PROBLEM: Hirshfeld Test Diff for C24 -- C26 .. 7.4 su RESPONSE: Atom identities consistent with synthesis and spectroscopy. ; # end Validation Reply Form _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H94 Cr2 N6' _chemical_formula_weight 1111.50 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -z' _cell_length_a 10.073(2) _cell_length_b 13.461(3) _cell_length_c 13.590(3) _cell_angle_alpha 79.66(3) _cell_angle_beta 81.58(3) _cell_angle_gamma 80.96(3) _cell_volume 1777.0(7) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 984 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 25.73 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.039 _exptl_crystal_F_000 598 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.481 _exptl_crystal_size_mid 0.317 _exptl_crystal_size_min 0.117 _exptl_absorpt_coefficient_mu 0.345 _shelx_estimated_absorpt_T_min 0.852 _shelx_estimated_absorpt_T_max 0.961 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.852 _exptl_absorpt_correction_T_max 0.961 _exptl_absorpt_process_details 'APEX2 (Bruker, 2007)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 13916 _diffrn_reflns_av_unetI/netI 0.0117 _diffrn_reflns_av_R_equivalents 0.0008 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.535 _diffrn_reflns_theta_max 26.019 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 6958 _reflns_number_gt 6597 _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 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ? ; _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^)+(0.0761P)^2^+11.1738P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 6958 _refine_ls_number_parameters 333 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0866 _refine_ls_wR_factor_ref 0.2365 _refine_ls_wR_factor_gt 0.2346 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 Cr1 Cr 0.89769(6) 0.01837(5) 0.06134(5) 0.0215(2) Uani 1 1 d . . . . . N1 N 0.8299(4) 0.1306(3) 0.1303(3) 0.0337(9) Uani 1 1 d . . . . . N2 N 0.7653(3) -0.0575(3) 0.1388(3) 0.0337(9) Uani 1 1 d . . . . . N3 N 0.9255(3) 0.0419(3) -0.0740(3) 0.0250(7) Uani 1 1 d . . . . . C1 C 0.6980(4) 0.1221(3) 0.1234(4) 0.0306(10) Uani 1 1 d . . . . . H1A H 0.6315 0.1802 0.1131 0.037 Uiso 1 1 calc R U . . . C2 C 0.6671(4) 0.0246(3) 0.1320(3) 0.0246(8) Uani 1 1 d . . . . . H2A H 0.5756 0.0145 0.1333 0.030 Uiso 1 1 calc R U . . . C3 C 0.9187(5) 0.2275(4) 0.2333(4) 0.0394(11) Uani 1 1 d . . . . . C4 C 0.9348(6) 0.3272(4) 0.2498(5) 0.0500(14) Uani 1 1 d . . . . . H4A H 0.9720 0.3322 0.3088 0.060 Uiso 1 1 calc R U . . . C5 C 0.9016(6) 0.4114(4) 0.1886(5) 0.0467(13) Uani 1 1 d . . . . . H5A H 0.9122 0.4744 0.2068 0.056 Uiso 1 1 calc R U . . . C6 C 0.8506(5) 0.4128(4) 0.0964(5) 0.0453(13) Uani 1 1 d . . . . . H6A H 0.8309 0.4741 0.0510 0.054 Uiso 1 1 calc R U . . . C7 C 0.8308(5) 0.3151(3) 0.0765(4) 0.0355(10) Uani 1 1 d . . . . . C8 C 0.8599(4) 0.2266(3) 0.1435(4) 0.0291(9) Uani 1 1 d . . . . . C9 C 0.9560(6) 0.1335(4) 0.3037(4) 0.0482(13) Uani 1 1 d . . . . . H9A H 0.9288 0.0758 0.2775 0.058 Uiso 1 1 calc R U . . . C10 C 1.1084(7) 0.1103(6) 0.3093(8) 0.084(2) Uani 1 1 d . . . . . H10A H 1.1572 0.1312 0.2427 0.126 Uiso 1 1 calc R U . . . H10B H 1.1331 0.0370 0.3306 0.126 Uiso 1 1 calc R U . . . H10C H 1.1327 0.1478 0.3580 0.126 Uiso 1 1 calc R U . . . C11 C 0.8781(13) 0.1374(7) 0.4067(5) 0.109(4) Uani 1 1 d . . . . . H11A H 0.9058 0.1910 0.4363 0.164 Uiso 1 1 calc R U . . . H11B H 0.8970 0.0715 0.4500 0.164 Uiso 1 1 calc R U . . . H11C H 0.7809 0.1522 0.4009 0.164 Uiso 1 1 calc R U . . . C12 C 0.7791(5) 0.3152(4) -0.0211(4) 0.0386(11) Uani 1 1 d . . . . . H12 H 0.7699 0.2435 -0.0261 0.046 Uiso 1 1 calc R U . . . C13 C 0.8740(6) 0.3564(5) -0.1119(5) 0.0550(14) Uani 1 1 d . . . . . H13A H 0.9274 0.4028 -0.0921 0.082 Uiso 1 1 calc R U . . . H13B H 0.8208 0.3932 -0.1653 0.082 Uiso 1 1 calc R U . . . H13C H 0.9350 0.2996 -0.1368 0.082 Uiso 1 1 calc R U . . . C14 C 0.6376(6) 0.3808(5) -0.0283(5) 0.0563(15) Uani 1 1 d . . . . . H14A H 0.6482 0.4533 -0.0394 0.084 Uiso 1 1 calc R U . . . H14B H 0.5783 0.3645 0.0346 0.084 Uiso 1 1 calc R U . . . H14C H 0.5975 0.3659 -0.0846 0.084 Uiso 1 1 calc R U . . . C15 C 0.7338(4) -0.2336(3) 0.1269(4) 0.0317(10) Uani 1 1 d . . . . . C16 C 0.7029(5) -0.3278(4) 0.1771(4) 0.0418(12) Uani 1 1 d . . . . . H16 H 0.7055 -0.3814 0.1396 0.050 Uiso 1 1 calc R U . . . C17 C 0.6698(6) -0.3450(4) 0.2760(5) 0.0486(13) Uani 1 1 d . . . . . H17 H 0.6452 -0.4095 0.3075 0.058 Uiso 1 1 calc R U . . . C18 C 0.6704(5) -0.2712(4) 0.3340(5) 0.0495(13) Uani 1 1 d . . . . . H18 H 0.6507 -0.2861 0.4052 0.059 Uiso 1 1 calc R U . . . C19 C 0.6999(4) -0.1743(4) 0.2883(4) 0.0350(10) Uani 1 1 d . . . . . C20 C 0.7343(4) -0.1557(3) 0.1847(3) 0.0267(9) Uani 1 1 d . . . . . C21 C 0.7571(4) -0.2111(3) 0.0138(4) 0.0344(10) Uani 1 1 d . . . . . H21 H 0.8305 -0.1665 -0.0050 0.041 Uiso 1 1 calc R U . . . C22 C 0.8011(5) -0.3034(4) -0.0384(5) 0.0523(15) Uani 1 1 d . . . . . H22A H 0.7407 -0.3549 -0.0114 0.078 Uiso 1 1 calc R U . . . H22B H 0.8942 -0.3320 -0.0266 0.078 Uiso 1 1 calc R U . . . H22C H 0.7969 -0.2832 -0.1110 0.078 Uiso 1 1 calc R U . . . C23 C 0.6328(5) -0.1525(4) -0.0265(4) 0.0424(12) Uani 1 1 d . . . . . H23A H 0.5541 -0.1865 0.0041 0.064 Uiso 1 1 calc R U . . . H23B H 0.6428 -0.1491 -0.0998 0.064 Uiso 1 1 calc R U . . . H23C H 0.6199 -0.0833 -0.0102 0.064 Uiso 1 1 calc R U . . . C24 C 0.6922(6) -0.0870(5) 0.3520(5) 0.0610(17) Uani 1 1 d . . . . . H24 H 0.7446 -0.0335 0.3107 0.073 Uiso 1 1 calc R U . . . C25 C 0.5460(6) -0.0379(6) 0.3739(7) 0.080(2) Uani 1 1 d . . . . . H25A H 0.4918 -0.0892 0.4134 0.120 Uiso 1 1 calc R U . . . H25B H 0.5088 -0.0108 0.3102 0.120 Uiso 1 1 calc R U . . . H25C H 0.5434 0.0176 0.4121 0.120 Uiso 1 1 calc R U . . . C26 C 0.7604(7) -0.1284(6) 0.4471(4) 0.0613(17) Uani 1 1 d . . . . . H26A H 0.7860 -0.0718 0.4734 0.092 Uiso 1 1 calc R U . . . H26B H 0.8416 -0.1759 0.4309 0.092 Uiso 1 1 calc R U . . . H26C H 0.6973 -0.1640 0.4981 0.092 Uiso 1 1 calc R U . . . C27 C 0.9269(4) 0.1372(4) -0.2458(3) 0.0361(10) Uani 1 1 d . . . . . H27 H 1.0230 0.1302 -0.2555 0.043 Uiso 1 1 calc R U . . . C28 C 0.8591(6) 0.1862(5) -0.3159(5) 0.0574(16) Uani 1 1 d . . . . . H28 H 0.9084 0.2127 -0.3776 0.069 Uiso 1 1 calc R U . . . C29 C 0.7149(5) 0.2042(6) -0.3083(4) 0.0599(17) Uani 1 1 d . . . . . H29 H 0.6684 0.2418 -0.3621 0.072 Uiso 1 1 calc R U . . . C30 C 0.6498(5) 0.1653(5) -0.2215(4) 0.0478(13) Uani 1 1 d . . . . . H30 H 0.5536 0.1763 -0.2125 0.057 Uiso 1 1 calc R U . . . C31 C 0.7158(4) 0.1104(4) -0.1452(4) 0.0359(10) Uani 1 1 d . . . . . H31 H 0.6648 0.0829 -0.0848 0.043 Uiso 1 1 calc R U . . . C32 C 0.8584(4) 0.0932(3) -0.1536(3) 0.0268(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 Cr1 0.0112(3) 0.0232(3) 0.0324(4) -0.0089(3) -0.0023(2) -0.0043(2) N1 0.0171(17) 0.035(2) 0.055(2) -0.0169(18) -0.0060(16) -0.0085(15) N2 0.0163(16) 0.0315(19) 0.057(2) -0.0172(18) -0.0025(16) -0.0039(14) N3 0.0139(15) 0.0266(17) 0.0361(19) -0.0110(14) -0.0055(13) 0.0020(13) C1 0.0098(17) 0.035(2) 0.053(3) -0.025(2) 0.0012(17) -0.0038(16) C2 0.0124(17) 0.029(2) 0.034(2) -0.0048(17) -0.0083(15) -0.0036(15) C3 0.044(3) 0.034(2) 0.048(3) -0.023(2) 0.002(2) -0.016(2) C4 0.048(3) 0.044(3) 0.071(4) -0.039(3) -0.005(3) -0.015(2) C5 0.044(3) 0.033(3) 0.067(4) -0.021(2) -0.010(3) -0.002(2) C6 0.036(3) 0.029(2) 0.077(4) -0.029(2) -0.002(2) -0.003(2) C7 0.030(2) 0.022(2) 0.058(3) -0.014(2) -0.005(2) -0.0066(17) C8 0.0215(19) 0.025(2) 0.045(3) -0.0193(18) -0.0080(18) 0.0020(16) C9 0.059(3) 0.048(3) 0.044(3) -0.008(2) -0.018(3) -0.017(3) C10 0.055(4) 0.069(5) 0.142(8) -0.035(5) -0.032(5) -0.015(3) C11 0.208(12) 0.087(6) 0.040(4) -0.010(4) -0.026(5) -0.034(7) C12 0.031(2) 0.029(2) 0.056(3) -0.009(2) -0.009(2) 0.0018(18) C13 0.048(3) 0.062(4) 0.059(4) -0.015(3) -0.004(3) -0.017(3) C14 0.039(3) 0.055(3) 0.080(4) -0.016(3) -0.027(3) 0.005(3) C15 0.0137(18) 0.033(2) 0.052(3) -0.017(2) -0.0058(18) -0.0007(16) C16 0.033(2) 0.034(2) 0.061(3) -0.009(2) -0.007(2) -0.010(2) C17 0.041(3) 0.039(3) 0.067(4) -0.001(3) -0.011(3) -0.012(2) C18 0.030(3) 0.049(3) 0.066(4) -0.004(3) 0.001(2) -0.009(2) C19 0.022(2) 0.046(3) 0.042(3) -0.011(2) -0.0061(18) -0.0115(19) C20 0.0103(16) 0.025(2) 0.045(2) -0.0060(17) 0.0006(16) -0.0067(14) C21 0.019(2) 0.030(2) 0.059(3) -0.019(2) -0.0002(19) -0.0087(17) C22 0.030(3) 0.046(3) 0.088(4) -0.035(3) 0.003(3) -0.009(2) C23 0.042(3) 0.037(3) 0.050(3) -0.015(2) -0.015(2) 0.007(2) C24 0.033(3) 0.082(4) 0.079(4) -0.041(4) 0.002(3) -0.018(3) C25 0.041(3) 0.100(6) 0.108(6) -0.066(5) 0.017(4) -0.003(3) C26 0.061(4) 0.095(5) 0.037(3) -0.014(3) -0.008(3) -0.033(4) C27 0.020(2) 0.058(3) 0.032(2) -0.010(2) -0.0005(17) -0.008(2) C28 0.031(3) 0.063(4) 0.068(4) 0.004(3) -0.001(3) 0.001(3) C29 0.025(3) 0.108(5) 0.047(3) -0.002(3) -0.011(2) -0.015(3) C30 0.017(2) 0.068(4) 0.060(3) -0.008(3) -0.014(2) -0.004(2) C31 0.0133(19) 0.046(3) 0.049(3) -0.006(2) -0.0049(18) -0.0071(18) C32 0.0143(18) 0.034(2) 0.035(2) -0.0090(18) -0.0032(16) -0.0065(16) _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 Cr1 N3 1.797(4) . ? Cr1 N3 1.856(3) 2_755 ? Cr1 N2 1.887(4) . ? Cr1 N1 1.904(4) . ? Cr1 C2 2.375(4) . ? Cr1 C1 2.398(4) . ? Cr1 Cr1 2.4982(15) 2_755 ? N1 C1 1.370(5) . ? N1 C8 1.420(5) . ? N2 C2 1.362(5) . ? N2 C20 1.418(5) . ? N3 C32 1.380(5) . ? N3 Cr1 1.856(3) 2_755 ? C1 C2 1.376(6) . ? C3 C8 1.435(7) . ? C3 C4 1.437(6) . ? C3 C9 1.476(8) . ? C4 C5 1.308(8) . ? C5 C6 1.418(8) . ? C6 C7 1.438(6) . ? C7 C8 1.383(7) . ? C7 C12 1.495(7) . ? C9 C11 1.507(10) . ? C9 C10 1.529(9) . ? C12 C13 1.523(8) . ? C12 C14 1.560(7) . ? C15 C16 1.386(7) . ? C15 C20 1.420(6) . ? C15 C21 1.504(7) . ? C16 C17 1.323(8) . ? C17 C18 1.375(8) . ? C18 C19 1.397(7) . ? C19 C20 1.387(7) . ? C19 C24 1.565(7) . ? C21 C23 1.492(6) . ? C21 C22 1.515(6) . ? C24 C25 1.527(8) . ? C24 C26 1.528(9) . ? C27 C28 1.278(8) . ? C27 C32 1.416(6) . ? C28 C29 1.426(7) . ? C29 C30 1.324(8) . ? C30 C31 1.355(7) . ? C31 C32 1.409(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 N3 Cr1 N3 93.72(15) . 2_755 ? N3 Cr1 N2 125.02(17) . . ? N3 Cr1 N2 114.01(16) 2_755 . ? N3 Cr1 N1 118.40(17) . . ? N3 Cr1 N1 117.53(15) 2_755 . ? N2 Cr1 N1 90.43(16) . . ? N3 Cr1 C2 115.11(15) . . ? N3 Cr1 C2 146.26(15) 2_755 . ? N2 Cr1 C2 34.96(15) . . ? N1 Cr1 C2 64.97(15) . . ? N3 Cr1 C1 111.04(16) . . ? N3 Cr1 C1 149.48(15) 2_755 . ? N2 Cr1 C1 66.42(16) . . ? N1 Cr1 C1 34.81(14) . . ? C2 Cr1 C1 33.50(14) . . ? N3 Cr1 Cr1 47.85(10) . 2_755 ? N3 Cr1 Cr1 45.87(11) 2_755 2_755 ? N2 Cr1 Cr1 135.65(12) . 2_755 ? N1 Cr1 Cr1 133.27(12) . 2_755 ? C2 Cr1 Cr1 157.39(11) . 2_755 ? C1 Cr1 Cr1 153.93(13) . 2_755 ? C1 N1 C8 117.8(4) . . ? C1 N1 Cr1 92.7(3) . . ? C8 N1 Cr1 142.2(3) . . ? C2 N2 C20 121.1(3) . . ? C2 N2 Cr1 92.5(3) . . ? C20 N2 Cr1 145.9(3) . . ? C32 N3 Cr1 138.8(3) . . ? C32 N3 Cr1 134.4(3) . 2_755 ? Cr1 N3 Cr1 86.28(15) . 2_755 ? N1 C1 C2 116.3(4) . . ? N1 C1 Cr1 52.5(2) . . ? C2 C1 Cr1 72.3(2) . . ? N2 C2 C1 121.2(3) . . ? N2 C2 Cr1 52.5(2) . . ? C1 C2 Cr1 74.2(2) . . ? C8 C3 C4 114.5(5) . . ? C8 C3 C9 122.4(4) . . ? C4 C3 C9 123.1(5) . . ? C5 C4 C3 124.1(5) . . ? C4 C5 C6 122.9(5) . . ? C5 C6 C7 115.4(5) . . ? C8 C7 C6 121.6(5) . . ? C8 C7 C12 122.4(4) . . ? C6 C7 C12 116.0(5) . . ? C7 C8 N1 122.8(4) . . ? C7 C8 C3 121.3(4) . . ? N1 C8 C3 115.8(4) . . ? C3 C9 C11 111.0(6) . . ? C3 C9 C10 112.7(5) . . ? C11 C9 C10 111.3(7) . . ? C7 C12 C13 112.5(4) . . ? C7 C12 C14 112.0(4) . . ? C13 C12 C14 107.3(5) . . ? C16 C15 C20 118.3(5) . . ? C16 C15 C21 121.5(4) . . ? C20 C15 C21 120.1(4) . . ? C17 C16 C15 121.6(5) . . ? C16 C17 C18 121.3(5) . . ? C17 C18 C19 120.1(6) . . ? C20 C19 C18 118.8(5) . . ? C20 C19 C24 120.1(5) . . ? C18 C19 C24 121.1(5) . . ? C19 C20 N2 118.7(4) . . ? C19 C20 C15 119.7(4) . . ? N2 C20 C15 121.6(4) . . ? C23 C21 C15 110.1(4) . . ? C23 C21 C22 108.9(4) . . ? C15 C21 C22 115.3(4) . . ? C25 C24 C26 113.2(6) . . ? C25 C24 C19 110.7(5) . . ? C26 C24 C19 109.6(6) . . ? C28 C27 C32 119.9(5) . . ? C27 C28 C29 124.8(6) . . ? C30 C29 C28 115.8(5) . . ? C29 C30 C31 122.2(5) . . ? C30 C31 C32 121.4(5) . . ? N3 C32 C31 121.4(4) . . ? N3 C32 C27 122.6(4) . . ? C31 C32 C27 115.8(4) . . ? _refine_diff_density_max 1.014 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.161 _shelxl_version_number 2013-2 _shelx_res_file ; TITL klat762b in P-1 CELL 0.71073 10.0732 13.4606 13.5905 79.6553 81.5778 80.9562 ZERR 1 0.0020 0.0027 0.0032 0.0280 0.0340 0.0300 LATT 1 SFAC C H N Cr UNIT 69 94 6 2 L.S. 20 OMIT 0 1 0 OMIT 1 1 1 OMIT 1 2 0 OMIT 0 -2 1 OMIT -2 -1 1 OMIT 1 4 2 OMIT 0 -5 3 OMIT -2 0 1 ACTA SIZE 0.481 0.317 0.117 BOND FMAP 2 PLAN 20 TEMP -73 WGHT 0.076100 11.173800 FVAR 6.13357 CR1 4 0.897690 0.018366 0.061336 11.00000 0.01123 0.02317 = 0.03244 -0.00892 -0.00226 -0.00433 N1 3 0.829923 0.130611 0.130339 11.00000 0.01714 0.03521 = 0.05458 -0.01686 -0.00603 -0.00852 N2 3 0.765301 -0.057486 0.138802 11.00000 0.01626 0.03148 = 0.05669 -0.01717 -0.00254 -0.00388 N3 3 0.925508 0.041939 -0.073980 11.00000 0.01387 0.02658 = 0.03607 -0.01096 -0.00551 0.00197 C1 1 0.697969 0.122066 0.123373 11.00000 0.00975 0.03454 = 0.05321 -0.02541 0.00116 -0.00377 AFIX 43 H1A 2 0.631544 0.180173 0.113134 11.00000 -1.20000 AFIX 0 C2 1 0.667053 0.024644 0.132033 11.00000 0.01238 0.02911 = 0.03419 -0.00484 -0.00830 -0.00357 AFIX 43 H2A 2 0.575569 0.014457 0.133317 11.00000 -1.20000 AFIX 0 C3 1 0.918653 0.227490 0.233288 11.00000 0.04398 0.03414 = 0.04775 -0.02331 0.00184 -0.01607 C4 1 0.934836 0.327163 0.249790 11.00000 0.04804 0.04426 = 0.07083 -0.03865 -0.00477 -0.01491 AFIX 43 H4A 2 0.971958 0.332226 0.308774 11.00000 -1.20000 AFIX 0 C5 1 0.901632 0.411365 0.188647 11.00000 0.04438 0.03299 = 0.06747 -0.02085 -0.01014 -0.00202 AFIX 43 H5A 2 0.912156 0.474365 0.206818 11.00000 -1.20000 AFIX 0 C6 1 0.850629 0.412820 0.096448 11.00000 0.03574 0.02890 = 0.07724 -0.02881 -0.00208 -0.00342 AFIX 43 H6A 2 0.830919 0.474081 0.050995 11.00000 -1.20000 AFIX 0 C7 1 0.830807 0.315145 0.076515 11.00000 0.02952 0.02217 = 0.05848 -0.01379 -0.00529 -0.00662 C8 1 0.859942 0.226617 0.143493 11.00000 0.02146 0.02517 = 0.04544 -0.01930 -0.00797 0.00202 C9 1 0.955952 0.133516 0.303714 11.00000 0.05890 0.04828 = 0.04427 -0.00836 -0.01784 -0.01656 AFIX 13 H9A 2 0.928791 0.075809 0.277492 11.00000 -1.20000 AFIX 0 C10 1 1.108435 0.110305 0.309270 11.00000 0.05515 0.06882 = 0.14210 -0.03473 -0.03174 -0.01511 AFIX 137 H10A 2 1.157246 0.131224 0.242742 11.00000 -1.50000 H10B 2 1.133085 0.037009 0.330589 11.00000 -1.50000 H10C 2 1.132718 0.147804 0.358040 11.00000 -1.50000 AFIX 0 C11 1 0.878132 0.137417 0.406749 11.00000 0.20791 0.08728 = 0.04003 -0.00962 -0.02560 -0.03358 AFIX 137 H11A 2 0.905821 0.191010 0.436350 11.00000 -1.50000 H11B 2 0.897026 0.071544 0.449993 11.00000 -1.50000 H11C 2 0.780929 0.152234 0.400924 11.00000 -1.50000 AFIX 0 C12 1 0.779076 0.315243 -0.021118 11.00000 0.03107 0.02903 = 0.05609 -0.00920 -0.00948 0.00175 AFIX 13 H12 2 0.769919 0.243465 -0.026113 11.00000 -1.20000 AFIX 0 C13 1 0.874026 0.356366 -0.111898 11.00000 0.04825 0.06211 = 0.05922 -0.01546 -0.00410 -0.01738 AFIX 137 H13A 2 0.927368 0.402808 -0.092089 11.00000 -1.50000 H13B 2 0.820792 0.393179 -0.165262 11.00000 -1.50000 H13C 2 0.935026 0.299577 -0.136766 11.00000 -1.50000 AFIX 0 C14 1 0.637627 0.380834 -0.028278 11.00000 0.03863 0.05463 = 0.08022 -0.01612 -0.02740 0.00491 AFIX 137 H14A 2 0.648186 0.453292 -0.039382 11.00000 -1.50000 H14B 2 0.578326 0.364492 0.034634 11.00000 -1.50000 H14C 2 0.597508 0.365923 -0.084583 11.00000 -1.50000 AFIX 0 C15 1 0.733812 -0.233631 0.126945 11.00000 0.01372 0.03277 = 0.05209 -0.01701 -0.00581 -0.00067 C16 1 0.702905 -0.327797 0.177128 11.00000 0.03258 0.03401 = 0.06148 -0.00856 -0.00736 -0.01044 AFIX 43 H16 2 0.705519 -0.381370 0.139629 11.00000 -1.20000 AFIX 0 C17 1 0.669841 -0.344952 0.275983 11.00000 0.04115 0.03854 = 0.06659 -0.00052 -0.01078 -0.01208 AFIX 43 H17 2 0.645221 -0.409480 0.307518 11.00000 -1.20000 AFIX 0 C18 1 0.670431 -0.271170 0.333955 11.00000 0.03025 0.04933 = 0.06583 -0.00355 0.00106 -0.00879 AFIX 43 H18 2 0.650733 -0.286122 0.405151 11.00000 -1.20000 AFIX 0 C19 1 0.699948 -0.174271 0.288322 11.00000 0.02181 0.04554 = 0.04197 -0.01053 -0.00613 -0.01153 C20 1 0.734285 -0.155682 0.184725 11.00000 0.01030 0.02475 = 0.04546 -0.00598 0.00063 -0.00669 C21 1 0.757136 -0.211096 0.013775 11.00000 0.01899 0.02964 = 0.05924 -0.01855 -0.00017 -0.00867 AFIX 13 H21 2 0.830472 -0.166517 -0.004963 11.00000 -1.20000 AFIX 0 C22 1 0.801135 -0.303442 -0.038410 11.00000 0.03034 0.04618 = 0.08759 -0.03490 0.00269 -0.00874 AFIX 137 H22A 2 0.740730 -0.354897 -0.011410 11.00000 -1.50000 H22B 2 0.894184 -0.331955 -0.026607 11.00000 -1.50000 H22C 2 0.796948 -0.283202 -0.110965 11.00000 -1.50000 AFIX 0 C23 1 0.632833 -0.152474 -0.026473 11.00000 0.04201 0.03736 = 0.04963 -0.01494 -0.01534 0.00743 AFIX 137 H23A 2 0.554117 -0.186501 0.004087 11.00000 -1.50000 H23B 2 0.642827 -0.149100 -0.099773 11.00000 -1.50000 H23C 2 0.619883 -0.083302 -0.010177 11.00000 -1.50000 AFIX 0 C24 1 0.692228 -0.087004 0.351965 11.00000 0.03312 0.08188 = 0.07943 -0.04148 0.00232 -0.01827 AFIX 13 H24 2 0.744624 -0.033460 0.310727 11.00000 -1.20000 AFIX 0 C25 1 0.545953 -0.037947 0.373889 11.00000 0.04054 0.09989 = 0.10841 -0.06559 0.01713 -0.00340 AFIX 137 H25A 2 0.491779 -0.089158 0.413356 11.00000 -1.50000 H25B 2 0.508785 -0.010827 0.310231 11.00000 -1.50000 H25C 2 0.543425 0.017626 0.412148 11.00000 -1.50000 AFIX 0 C26 1 0.760395 -0.128374 0.447123 11.00000 0.06074 0.09542 = 0.03719 -0.01366 -0.00834 -0.03327 AFIX 137 H26A 2 0.785967 -0.071758 0.473354 11.00000 -1.50000 H26B 2 0.841594 -0.175930 0.430943 11.00000 -1.50000 H26C 2 0.697339 -0.163964 0.498094 11.00000 -1.50000 AFIX 0 C27 1 0.926851 0.137180 -0.245815 11.00000 0.01979 0.05783 = 0.03162 -0.00974 -0.00054 -0.00795 AFIX 43 H27 2 1.022989 0.130216 -0.255531 11.00000 -1.20000 AFIX 0 C28 1 0.859089 0.186248 -0.315910 11.00000 0.03147 0.06314 = 0.06807 0.00444 -0.00136 0.00124 AFIX 43 H28 2 0.908360 0.212676 -0.377611 11.00000 -1.20000 AFIX 0 C29 1 0.714926 0.204231 -0.308280 11.00000 0.02493 0.10770 = 0.04684 -0.00201 -0.01062 -0.01469 AFIX 43 H29 2 0.668449 0.241782 -0.362084 11.00000 -1.20000 AFIX 0 C30 1 0.649831 0.165339 -0.221538 11.00000 0.01746 0.06829 = 0.05950 -0.00845 -0.01428 -0.00438 AFIX 43 H30 2 0.553637 0.176329 -0.212511 11.00000 -1.20000 AFIX 0 C31 1 0.715787 0.110400 -0.145225 11.00000 0.01329 0.04607 = 0.04895 -0.00586 -0.00495 -0.00705 AFIX 43 H31 2 0.664827 0.082891 -0.084776 11.00000 -1.20000 AFIX 0 C32 1 0.858351 0.093188 -0.153593 11.00000 0.01434 0.03362 = 0.03480 -0.00902 -0.00321 -0.00645 HKLF 4 REM klat762b in P-1 REM R1 = 0.0866 for 6597 Fo > 4sig(Fo) and 0.0897 for all 6958 data REM 333 parameters refined using 0 restraints END WGHT 0.1766 2.2727 REM Highest difference peak 1.014, deepest hole -0.829, 1-sigma level 0.161 Q1 1 0.8709 0.1187 0.0114 11.00000 0.05 1.01 Q2 1 0.6624 0.1770 0.0629 11.00000 0.05 0.83 Q3 1 0.9671 -0.0025 -0.0154 11.00000 0.05 0.79 Q4 1 0.9689 -0.0440 -0.0370 11.00000 0.05 0.79 Q5 1 0.8603 0.1753 0.0459 11.00000 0.05 0.60 Q6 1 0.7876 0.3902 0.1945 11.00000 0.05 0.58 Q7 1 0.6571 0.1382 0.1417 11.00000 0.05 0.56 Q8 1 0.7910 0.1672 0.0434 11.00000 0.05 0.56 Q9 1 0.9511 -0.0614 0.1140 11.00000 0.05 0.55 Q10 1 0.8617 0.0560 0.1677 11.00000 0.05 0.55 Q11 1 0.8168 0.2639 -0.1450 11.00000 0.05 0.54 Q12 1 1.0523 0.0499 0.3478 11.00000 0.05 0.53 Q13 1 0.8909 -0.3593 -0.1602 11.00000 0.05 0.53 Q14 1 1.0281 0.0224 0.3222 11.00000 0.05 0.52 Q15 1 0.6931 -0.1438 0.1099 11.00000 0.05 0.52 Q16 1 0.8507 0.3764 0.2147 11.00000 0.05 0.52 Q17 1 0.9184 -0.0657 -0.0765 11.00000 0.05 0.52 Q18 1 0.9004 0.4320 0.1620 11.00000 0.05 0.52 Q19 1 0.5317 0.0735 0.2002 11.00000 0.05 0.51 Q20 1 0.9202 0.3414 0.1618 11.00000 0.05 0.50 ; _shelx_res_checksum 29241 _shelx_hkl_file ; -1 0 0 456291 2184 311995 -18.24 1.24 1.0000 1 0 0 456570 2184 311995 -18.24 -1.24 1.0000 -2 0 0 387788 829 134532 39.87 0.58 1.0000 2 0 0 387829 829 134532 39.87 -0.58 1.0000 -3 0 0 276 44 2792 -5.68 0.44 1.0000 3 0 0 269 44 2792 -5.68 -0.44 1.0000 -4 0 0 166126 894 152641 2.64 -0.34 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0.07 1.0000 -1 -4 -16 1989 63 2177 0.31 0.14 1.0000 1 4 16 1999 63 2177 0.31 -0.14 1.0000 -2 -4 -16 4 21 -218 0.29 -0.10 1.0000 2 4 16 4 21 -218 0.29 0.10 1.0000 -3 -4 -16 0 21 -49 -0.07 0.03 1.0000 3 4 16 0 21 -49 -0.07 -0.03 1.0000 -4 -4 -16 232 162 142 0.52 0.06 1.0000 4 4 16 231 162 142 0.52 -0.06 1.0000 -5 -4 -16 3204 303 4060 -1.10 -0.11 1.0000 5 4 16 3211 303 4060 -1.10 0.11 1.0000 1 -5 -16 1343 169 1331 -0.03 0.03 1.0000 -1 5 16 1344 169 1331 -0.03 -0.03 1.0000 0 -5 -16 3634 216 3960 0.41 0.01 1.0000 0 5 16 3634 216 3960 0.41 -0.01 1.0000 -1 -5 -16 2243 190 1843 -0.69 -0.09 1.0000 1 5 16 2236 190 1843 -0.69 0.09 1.0000 -2 -5 -16 171 24 263 0.50 0.00 1.0000 2 5 16 171 24 263 0.50 0.00 1.0000 -3 -5 -16 177 154 295 -0.60 -0.02 1.0000 3 5 16 177 154 295 -0.60 0.02 1.0000 -4 -5 -16 93 166 130 -0.27 -0.04 1.0000 4 5 16 94 166 130 -0.27 0.04 1.0000 -5 -5 -16 1848 176 1514 0.63 0.06 1.0000 5 5 16 1846 176 1514 0.63 -0.06 1.0000 0 -6 -16 1762 167 1671 -0.17 0.02 1.0000 0 6 16 1764 167 1671 -0.17 -0.02 1.0000 -1 -6 -16 2471 142 2688 0.33 0.01 1.0000 1 6 16 2471 142 2688 0.33 -0.01 1.0000 -2 -6 -16 2168 195 1921 -0.43 0.03 1.0000 2 6 16 2170 195 1921 -0.43 -0.03 1.0000 -3 -6 -16 84 149 137 0.39 0.06 1.0000 3 6 16 86 149 137 0.39 -0.06 1.0000 -4 -6 -16 4 143 -210 0.31 -0.02 1.0000 4 6 16 4 143 -210 0.31 0.02 1.0000 -1 -7 -16 4675 161 4716 0.04 0.06 1.0000 1 7 16 4680 161 4716 0.04 -0.06 1.0000 -2 -7 -16 2716 139 2646 -0.10 -0.04 1.0000 2 7 16 2713 139 2646 -0.10 0.04 1.0000 -3 -7 -16 197 100 212 0.09 -0.06 1.0000 3 7 16 196 100 212 0.09 0.06 1.0000 -4 -7 -16 4 95 15 -0.40 0.06 1.0000 4 7 16 4 95 15 -0.40 -0.06 1.0000 0 0 0 7 0 0 -0.40 -0.06 1.0000 ; _shelx_hkl_checksum 50650 _database_code_depnum_ccdc_archive 'CCDC 971180' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_klat946 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67.50 H95 Cr2 N5 O0.50' _chemical_formula_weight 1088.48 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' Cr Cr 0.3209 0.6236 '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -z' _cell_length_a 13.946(3) _cell_length_b 21.212(4) _cell_length_c 22.202(4) _cell_angle_alpha 70.368(4) _cell_angle_beta 87.412(4) _cell_angle_gamma 80.550(4) _cell_volume 6102(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 1010 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.185 _exptl_crystal_F_000 2348 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.269 _exptl_crystal_size_mid 0.125 _exptl_crystal_size_min 0.035 _exptl_absorpt_coefficient_mu 0.401 _shelx_estimated_absorpt_T_min 0.900 _shelx_estimated_absorpt_T_max 0.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8994 _exptl_absorpt_correction_T_max 0.9860 _exptl_absorpt_process_details 'APEX2 (Bruker, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 74140 _diffrn_reflns_av_unetI/netI 0.1924 _diffrn_reflns_av_R_equivalents 0.1242 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.480 _diffrn_reflns_theta_max 28.328 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 30190 _reflns_number_gt 13347 _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 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ? ; _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^)+(0.0501P)^2^] 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 none _refine_ls_extinction_coef . _refine_ls_number_reflns 30190 _refine_ls_number_parameters 1362 _refine_ls_number_restraints 315 _refine_ls_R_factor_all 0.2006 _refine_ls_R_factor_gt 0.0918 _refine_ls_wR_factor_ref 0.2128 _refine_ls_wR_factor_gt 0.1651 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.002 _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 Cr1 Cr 0.19886(5) 0.18773(4) 0.80323(4) 0.02748(19) Uani 1 1 d . . . . . Cr2 Cr 0.12269(5) 0.26494(4) 0.73936(4) 0.02905(19) Uani 1 1 d . . . . . Cr3 Cr 0.37419(5) 0.24381(4) 0.27139(4) 0.02868(19) Uani 1 1 d . . . . . Cr4 Cr 0.32910(5) 0.31026(4) 0.18850(4) 0.02610(18) Uani 1 1 d . . . . . N1 N 0.2722(3) 0.22930(18) 0.84768(17) 0.0272(9) Uani 1 1 d . . . . . N2 N 0.1308(3) 0.34355(19) 0.76140(18) 0.0301(9) Uani 1 1 d . . . . . N3 N 0.2650(3) 0.1279(2) 0.76122(18) 0.0325(10) Uani 1 1 d . . . . . N4 N 0.1425(3) 0.2416(2) 0.66441(18) 0.0338(10) Uani 1 1 d . . . . . N5 N 0.0698(3) 0.20487(19) 0.81447(18) 0.0294(9) Uani 1 1 d . . . . . N6 N 0.3766(3) 0.15712(19) 0.26358(18) 0.0302(9) Uani 1 1 d . . . . . N7 N 0.2788(3) 0.25804(19) 0.14390(18) 0.0299(9) Uani 1 1 d . . . . . N8 N 0.3181(3) 0.28516(19) 0.33084(18) 0.0305(9) Uani 1 1 d . . . . . N9 N 0.2466(3) 0.38450(19) 0.20351(18) 0.0274(9) Uani 1 1 d . . . . . N10 N 0.4580(3) 0.28766(19) 0.20356(18) 0.0305(9) Uani 1 1 d . . . . . C1 C 0.2314(3) 0.2886(2) 0.8579(2) 0.0292(11) Uani 1 1 d . . . . . H1 H 0.2494 0.2937 0.8965 0.035 Uiso 1 1 calc R U . . . C2 C 0.1684(3) 0.3403(2) 0.8189(2) 0.0298(11) Uani 1 1 d . . . . . H2 H 0.1482 0.3783 0.8326 0.036 Uiso 1 1 calc R U . . . C3 C 0.4434(3) 0.2255(3) 0.8724(2) 0.0360(12) Uani 1 1 d . . . . . C4 C 0.5228(4) 0.1956(3) 0.9129(3) 0.0468(14) Uani 1 1 d . . . . . H4 H 0.5803 0.2156 0.9046 0.056 Uiso 1 1 calc R U . . . C5 C 0.5213(4) 0.1373(3) 0.9651(3) 0.0485(15) Uani 1 1 d . . . . . H5 H 0.5772 0.1179 0.9920 0.058 Uiso 1 1 calc R U . . . C6 C 0.4390(4) 0.1077(3) 0.9779(3) 0.0451(14) Uani 1 1 d . . . . . H6 H 0.4383 0.0675 1.0135 0.054 Uiso 1 1 calc R U . . . C7 C 0.3557(3) 0.1364(2) 0.9390(2) 0.0327(11) Uani 1 1 d . . . . . C8 C 0.3580(3) 0.1960(2) 0.8869(2) 0.0297(11) Uani 1 1 d . . . . . C9 C 0.4472(4) 0.2894(3) 0.8154(3) 0.0453(14) Uani 1 1 d . . . . . H9 H 0.3855 0.3209 0.8158 0.054 Uiso 1 1 calc R U . . . C10 C 0.5304(5) 0.3270(3) 0.8184(3) 0.075(2) Uani 1 1 d . . . . . H10A H 0.5293 0.3347 0.8595 0.112 Uiso 1 1 calc R U . . . H10B H 0.5228 0.3706 0.7836 0.112 Uiso 1 1 calc R U . . . H10C H 0.5925 0.2997 0.8140 0.112 Uiso 1 1 calc R U . . . C11 C 0.4485(5) 0.2763(3) 0.7522(3) 0.0649(19) Uani 1 1 d . . . . . H11A H 0.5081 0.2456 0.7496 0.097 Uiso 1 1 calc R U . . . H11B H 0.4463 0.3192 0.7168 0.097 Uiso 1 1 calc R U . . . H11C H 0.3918 0.2554 0.7494 0.097 Uiso 1 1 calc R U . . . C12 C 0.2634(4) 0.1051(3) 0.9590(2) 0.0381(12) Uani 1 1 d . . . . . H12 H 0.2180 0.1233 0.9213 0.046 Uiso 1 1 calc R U . . . C13 C 0.2141(4) 0.1278(3) 1.0125(3) 0.0576(17) Uani 1 1 d . . . . . H13A H 0.2598 0.1154 1.0484 0.086 Uiso 1 1 calc R U . . . H13B H 0.1569 0.1055 1.0267 0.086 Uiso 1 1 calc R U . . . H13C H 0.1940 0.1770 0.9967 0.086 Uiso 1 1 calc R U . . . C14 C 0.2800(4) 0.0287(3) 0.9779(3) 0.0537(16) Uani 1 1 d . . . . . H14A H 0.3165 0.0151 0.9443 0.080 Uiso 1 1 calc R U . . . H14B H 0.2172 0.0125 0.9834 0.080 Uiso 1 1 calc R U . . . H14C H 0.3171 0.0089 1.0181 0.080 Uiso 1 1 calc R U . . . C15 C 0.0005(4) 0.4324(2) 0.6997(2) 0.0336(12) Uani 1 1 d . . . . . C16 C -0.0304(4) 0.5003(3) 0.6620(2) 0.0441(14) Uani 1 1 d . . . . . H16 H -0.0957 0.5141 0.6469 0.053 Uiso 1 1 calc R U . . . C17 C 0.0320(4) 0.5469(3) 0.6465(2) 0.0448(14) Uani 1 1 d . . . . . H17 H 0.0094 0.5929 0.6221 0.054 Uiso 1 1 calc R U . . . C18 C 0.1273(4) 0.5268(3) 0.6666(2) 0.0433(14) Uani 1 1 d . . . . . H18 H 0.1703 0.5593 0.6555 0.052 Uiso 1 1 calc R U . . . C19 C 0.1624(4) 0.4600(3) 0.7027(2) 0.0350(12) Uani 1 1 d . . . . . C20 C 0.0975(3) 0.4123(2) 0.7200(2) 0.0297(11) Uani 1 1 d . . . . . C21 C -0.0751(4) 0.3864(3) 0.7207(3) 0.0442(14) Uani 1 1 d . . . . . H21 H -0.0406 0.3391 0.7411 0.053 Uiso 1 1 calc R U . . . C22 C -0.1377(5) 0.4066(3) 0.7717(3) 0.074(2) Uani 1 1 d . . . . . H22A H -0.0957 0.4068 0.8059 0.110 Uiso 1 1 calc R U . . . H22B H -0.1823 0.3739 0.7897 0.110 Uiso 1 1 calc R U . . . H22C H -0.1751 0.4519 0.7524 0.110 Uiso 1 1 calc R U . . . C23 C -0.1379(4) 0.3869(4) 0.6663(3) 0.073(2) Uani 1 1 d . . . . . H23A H -0.1781 0.4315 0.6487 0.109 Uiso 1 1 calc R U . . . H23B H -0.1800 0.3522 0.6825 0.109 Uiso 1 1 calc R U . . . H23C H -0.0962 0.3773 0.6327 0.109 Uiso 1 1 calc R U . . . C24 C 0.2702(4) 0.4416(3) 0.7224(3) 0.0437(14) Uani 1 1 d . . . . . H24 H 0.2849 0.3915 0.7442 0.052 Uiso 1 1 calc R U . . . C25 C 0.2931(4) 0.4763(3) 0.7698(3) 0.0576(17) Uani 1 1 d . . . . . H25A H 0.2814 0.5256 0.7488 0.086 Uiso 1 1 calc R U . . . H25B H 0.3614 0.4615 0.7834 0.086 Uiso 1 1 calc R U . . . H25C H 0.2512 0.4639 0.8071 0.086 Uiso 1 1 calc R U . . . C26 C 0.3372(4) 0.4607(3) 0.6636(3) 0.0575(17) Uani 1 1 d . . . . . H26A H 0.3300 0.4333 0.6368 0.086 Uiso 1 1 calc R U . . . H26B H 0.4050 0.4521 0.6781 0.086 Uiso 1 1 calc R U . . . H26C H 0.3191 0.5089 0.6388 0.086 Uiso 1 1 calc R U . . . C27 C 0.2619(4) 0.1389(3) 0.6964(2) 0.0391(13) Uani 1 1 d . . . . . H27 H 0.3025 0.1069 0.6814 0.047 Uiso 1 1 calc R U . . . C28 C 0.2070(4) 0.1905(3) 0.6525(2) 0.0402(13) Uani 1 1 d . . . . . H28 H 0.2133 0.1919 0.6093 0.048 Uiso 1 1 calc R U . . . C29 C 0.2513(5) 0.0071(3) 0.8195(3) 0.0483(15) Uani 1 1 d . . . . . C30 C 0.2974(6) -0.0584(3) 0.8543(3) 0.0640(19) Uani 1 1 d . . . . . H30 H 0.2601 -0.0942 0.8695 0.077 Uiso 1 1 calc R U . . . C31 C 0.3952(6) -0.0714(3) 0.8666(3) 0.071(2) Uani 1 1 d . . . . . H31 H 0.4248 -0.1160 0.8906 0.086 Uiso 1 1 calc R U . . . C32 C 0.4512(5) -0.0208(3) 0.8446(3) 0.0640(19) Uani 1 1 d . . . . . H32 H 0.5190 -0.0311 0.8537 0.077 Uiso 1 1 calc R U . . . C33 C 0.4109(4) 0.0446(3) 0.8098(3) 0.0458(15) Uani 1 1 d . . . . . C34 C 0.3095(4) 0.0592(3) 0.7980(2) 0.0379(13) Uani 1 1 d . . . . . C35 C 0.1450(4) 0.0189(3) 0.8033(3) 0.0505(15) Uani 1 1 d . . . . . H35 H 0.1191 0.0680 0.7945 0.061 Uiso 1 1 calc R U . . . C36 C 0.0860(5) -0.0232(3) 0.8579(3) 0.070(2) Uani 1 1 d . . . . . H36A H 0.1031 -0.0713 0.8625 0.104 Uiso 1 1 calc R U . . . H36B H 0.0164 -0.0085 0.8481 0.104 Uiso 1 1 calc R U . . . H36C H 0.1008 -0.0166 0.8980 0.104 Uiso 1 1 calc R U . . . C37 C 0.1303(5) 0.0014(3) 0.7428(3) 0.0653(18) Uani 1 1 d . . . . . H37A H 0.1664 0.0287 0.7073 0.098 Uiso 1 1 calc R U . . . H37B H 0.0610 0.0112 0.7316 0.098 Uiso 1 1 calc R U . . . H37C H 0.1543 -0.0468 0.7508 0.098 Uiso 1 1 calc R U . . . C38 C 0.4757(4) 0.0972(3) 0.7837(3) 0.0578(17) Uani 1 1 d . . . . . H38 H 0.4365 0.1421 0.7806 0.069 Uiso 1 1 calc R U . . . C39 C 0.5645(4) 0.0865(4) 0.8266(3) 0.073(2) Uani 1 1 d . . . . . H39A H 0.5431 0.0805 0.8706 0.109 Uiso 1 1 calc R U . . . H39B H 0.5977 0.1262 0.8109 0.109 Uiso 1 1 calc R U . . . H39C H 0.6092 0.0461 0.8257 0.109 Uiso 1 1 calc R U . . . C40 C 0.5104(5) 0.1011(4) 0.7161(3) 0.082(2) Uani 1 1 d . . . . . H40A H 0.5396 0.0558 0.7162 0.123 Uiso 1 1 calc R U . . . H40B H 0.5588 0.1317 0.7027 0.123 Uiso 1 1 calc R U . . . H40C H 0.4549 0.1184 0.6864 0.123 Uiso 1 1 calc R U . . . C41 C -0.0043(4) 0.2490(3) 0.6030(3) 0.0520(15) Uani 1 1 d . . . . . C42 C -0.0695(5) 0.2861(4) 0.5532(3) 0.069(2) Uani 1 1 d . . . . . H42 H -0.1244 0.2674 0.5473 0.083 Uiso 1 1 calc R U . . . C43 C -0.0561(5) 0.3487(4) 0.5125(3) 0.067(2) Uani 1 1 d . . . . . H43 H -0.1005 0.3723 0.4781 0.081 Uiso 1 1 calc R U . . . C44 C 0.0215(4) 0.3776(3) 0.5213(3) 0.0565(17) Uani 1 1 d . . . . . H44 H 0.0287 0.4216 0.4935 0.068 Uiso 1 1 calc R U . . . C45 C 0.0895(4) 0.3436(3) 0.5701(2) 0.0404(13) Uani 1 1 d . . . . . C46 C 0.0744(4) 0.2787(3) 0.6122(2) 0.0385(13) Uani 1 1 d . . . . . C47 C -0.0202(5) 0.1778(3) 0.6432(3) 0.0627(19) Uani 1 1 d . . . . . H47 H 0.0219 0.1623 0.6824 0.075 Uiso 1 1 calc R U . . . C48 C -0.1255(5) 0.1755(4) 0.6639(3) 0.084(2) Uani 1 1 d . . . . . H48A H -0.1468 0.2103 0.6837 0.125 Uiso 1 1 calc R U . . . H48B H -0.1310 0.1307 0.6948 0.125 Uiso 1 1 calc R U . . . H48C H -0.1666 0.1840 0.6264 0.125 Uiso 1 1 calc R U . . . C49 C 0.0105(5) 0.1290(4) 0.6047(3) 0.084(2) Uani 1 1 d . . . . . H49A H -0.0210 0.1482 0.5624 0.126 Uiso 1 1 calc R U . . . H49B H -0.0093 0.0850 0.6276 0.126 Uiso 1 1 calc R U . . . H49C H 0.0813 0.1231 0.5997 0.126 Uiso 1 1 calc R U . . . C50 C 0.1778(4) 0.3739(3) 0.5751(2) 0.0405(13) Uani 1 1 d . . . . . H50 H 0.1909 0.3639 0.6216 0.049 Uiso 1 1 calc R U . . . C51 C 0.1633(4) 0.4512(3) 0.5430(3) 0.0540(16) Uani 1 1 d . . . . . H51A H 0.1563 0.4625 0.4967 0.081 Uiso 1 1 calc R U . . . H51B H 0.2197 0.4687 0.5521 0.081 Uiso 1 1 calc R U . . . H51C H 0.1046 0.4717 0.5597 0.081 Uiso 1 1 calc R U . . . C52 C 0.2671(4) 0.3411(3) 0.5477(3) 0.069(2) Uani 1 1 d . . . . . H52A H 0.2808 0.2926 0.5721 0.104 Uiso 1 1 calc R U . . . H52B H 0.3232 0.3624 0.5505 0.104 Uiso 1 1 calc R U . . . H52C H 0.2546 0.3473 0.5028 0.104 Uiso 1 1 calc R U . . . C53 C -0.0143(3) 0.1919(2) 0.8564(2) 0.0333(12) Uani 1 1 d . . . . . C54 C -0.1084(3) 0.2049(3) 0.8173(2) 0.0400(13) Uani 1 1 d . . . . . H54A H -0.1190 0.2523 0.7877 0.048 Uiso 1 1 calc R U . . . H54B H -0.1020 0.1745 0.7915 0.048 Uiso 1 1 calc R U . . . C55 C -0.1951(4) 0.1925(3) 0.8616(3) 0.0495(15) Uani 1 1 d . . . . . H55 H -0.2553 0.2013 0.8353 0.059 Uiso 1 1 calc R U . . . C56 C -0.1801(4) 0.1191(3) 0.9065(3) 0.0530(16) Uani 1 1 d . . . . . H56A H -0.1735 0.0880 0.8813 0.064 Uiso 1 1 calc R U . . . H56B H -0.2368 0.1108 0.9348 0.064 Uiso 1 1 calc R U . . . C57 C -0.0881(4) 0.1062(3) 0.9465(3) 0.0516(16) Uani 1 1 d . . . . . H57 H -0.0773 0.0583 0.9763 0.062 Uiso 1 1 calc R U . . . C58 C -0.0004(4) 0.1193(3) 0.9018(2) 0.0431(14) Uani 1 1 d . . . . . H58A H 0.0595 0.1102 0.9276 0.052 Uiso 1 1 calc R U . . . H58B H 0.0075 0.0879 0.8768 0.052 Uiso 1 1 calc R U . . . C59 C -0.0262(3) 0.2402(3) 0.8959(2) 0.0382(13) Uani 1 1 d . . . . . H59A H 0.0334 0.2324 0.9216 0.046 Uiso 1 1 calc R U . . . H59B H -0.0363 0.2878 0.8669 0.046 Uiso 1 1 calc R U . . . C60 C -0.1140(4) 0.2273(3) 0.9403(3) 0.0475(15) Uani 1 1 d . . . . . H60 H -0.1212 0.2585 0.9660 0.057 Uiso 1 1 calc R U . . . C61 C -0.2067(4) 0.2403(3) 0.9008(3) 0.0533(16) Uani 1 1 d . . . . . H61A H -0.2631 0.2322 0.9296 0.064 Uiso 1 1 calc R U . . . H61B H -0.2183 0.2880 0.8720 0.064 Uiso 1 1 calc R U . . . C62 C -0.0988(4) 0.1550(3) 0.9850(3) 0.0572(17) Uani 1 1 d . . . . . H62A H -0.1549 0.1473 1.0140 0.069 Uiso 1 1 calc R U . . . H62B H -0.0396 0.1464 1.0114 0.069 Uiso 1 1 calc R U . . . C63 C 0.3663(3) 0.1464(3) 0.2059(2) 0.0334(12) Uani 1 1 d . . . . . H63 H 0.3919 0.1026 0.2042 0.040 Uiso 1 1 calc R U . . . C64 C 0.3236(3) 0.1918(2) 0.1524(2) 0.0305(11) Uani 1 1 d . . . . . H64 H 0.3239 0.1773 0.1163 0.037 Uiso 1 1 calc R U . . . C65 C 0.4745(4) 0.0754(3) 0.3560(3) 0.0440(14) Uani 1 1 d . . . . . C66 C 0.4850(5) 0.0132(3) 0.4064(3) 0.0585(18) Uani 1 1 d . . . . . H66 H 0.5419 -0.0003 0.4325 0.070 Uiso 1 1 calc R U . . . C67 C 0.4163(5) -0.0284(3) 0.4191(3) 0.0600(18) Uani 1 1 d . . . . . H67 H 0.4252 -0.0703 0.4534 0.072 Uiso 1 1 calc R U . . . C68 C 0.3338(5) -0.0087(3) 0.3813(3) 0.0577(17) Uani 1 1 d . . . . . H68 H 0.2866 -0.0381 0.3897 0.069 Uiso 1 1 calc R U . . . C69 C 0.3171(4) 0.0521(3) 0.3316(3) 0.0437(14) Uani 1 1 d . . . . . C70 C 0.3892(4) 0.0943(3) 0.3183(2) 0.0389(13) Uani 1 1 d . . . . . C71 C 0.5585(4) 0.1150(3) 0.3410(3) 0.0493(15) Uani 1 1 d . . . . . H71 H 0.5370 0.1585 0.3057 0.059 Uiso 1 1 calc R U . . . C72 C 0.5900(4) 0.1323(4) 0.3973(3) 0.068(2) Uani 1 1 d . . . . . H72A H 0.5337 0.1552 0.4140 0.102 Uiso 1 1 calc R U . . . H72B H 0.6392 0.1622 0.3834 0.102 Uiso 1 1 calc R U . . . H72C H 0.6177 0.0905 0.4310 0.102 Uiso 1 1 calc R U . . . C73 C 0.6446(4) 0.0751(3) 0.3164(3) 0.071(2) Uani 1 1 d . . . . . H73A H 0.6653 0.0312 0.3495 0.106 Uiso 1 1 calc R U . . . H73B H 0.6987 0.1010 0.3061 0.106 Uiso 1 1 calc R U . . . H73C H 0.6244 0.0677 0.2779 0.106 Uiso 1 1 calc R U . . . C74 C 0.2224(4) 0.0692(3) 0.2935(3) 0.0500(15) Uani 1 1 d . . . . . H74 H 0.2176 0.1170 0.2639 0.060 Uiso 1 1 calc R U . . . C75 C 0.1325(4) 0.0649(3) 0.3365(3) 0.0660(19) Uani 1 1 d . . . . . H75A H 0.1370 0.0191 0.3677 0.099 Uiso 1 1 calc R U . . . H75B H 0.0738 0.0752 0.3102 0.099 Uiso 1 1 calc R U . . . H75C H 0.1296 0.0977 0.3591 0.099 Uiso 1 1 calc R U . . . C76 C 0.2213(5) 0.0237(3) 0.2522(3) 0.0656(19) Uani 1 1 d . . . . . H76A H 0.2767 0.0286 0.2232 0.098 Uiso 1 1 calc R U . . . H76B H 0.1607 0.0373 0.2273 0.098 Uiso 1 1 calc R U . . . H76C H 0.2258 -0.0236 0.2800 0.098 Uiso 1 1 calc R U . . . C77 C 0.2333(3) 0.3359(2) 0.0347(2) 0.0323(11) Uani 1 1 d . . . . . C78 C 0.1680(4) 0.3573(3) -0.0172(2) 0.0380(13) Uani 1 1 d . . . . . H78 H 0.1810 0.3923 -0.0550 0.046 Uiso 1 1 calc R U . . . C79 C 0.0858(4) 0.3288(3) -0.0145(3) 0.0393(13) Uani 1 1 d . . . . . H79 H 0.0439 0.3424 -0.0507 0.047 Uiso 1 1 calc R U . . . C80 C 0.0649(4) 0.2803(3) 0.0414(3) 0.0399(13) Uani 1 1 d . . . . . H80 H 0.0069 0.2616 0.0433 0.048 Uiso 1 1 calc R U . . . C81 C 0.1251(3) 0.2574(3) 0.0954(2) 0.0344(12) Uani 1 1 d . . . . . C82 C 0.2114(3) 0.2849(2) 0.0908(2) 0.0285(11) Uani 1 1 d . . . . . C83 C 0.3286(4) 0.3630(3) 0.0257(2) 0.0388(13) Uani 1 1 d . . . . . H83 H 0.3557 0.3540 0.0693 0.047 Uiso 1 1 calc R U . . . C84 C 0.3179(4) 0.4391(3) -0.0090(3) 0.0555(16) Uani 1 1 d . . . . . H84A H 0.3032 0.4490 -0.0543 0.083 Uiso 1 1 calc R U . . . H84B H 0.3787 0.4550 -0.0051 0.083 Uiso 1 1 calc R U . . . H84C H 0.2649 0.4624 0.0100 0.083 Uiso 1 1 calc R U . . . C85 C 0.4010(4) 0.3243(3) -0.0078(3) 0.0555(17) Uani 1 1 d . . . . . H85A H 0.4103 0.2759 0.0173 0.083 Uiso 1 1 calc R U . . . H85B H 0.4634 0.3409 -0.0116 0.083 Uiso 1 1 calc R U . . . H85C H 0.3761 0.3312 -0.0505 0.083 Uiso 1 1 calc R U . . . C86 C 0.0983(3) 0.2058(3) 0.1565(2) 0.0377(12) Uani 1 1 d . . . . . H86 H 0.1587 0.1725 0.1730 0.045 Uiso 1 1 calc R U . . . C87 C 0.0656(4) 0.2372(3) 0.2081(3) 0.0494(15) Uani 1 1 d . . . . . H87A H 0.1167 0.2604 0.2157 0.074 Uiso 1 1 calc R U . . . H87B H 0.0532 0.2015 0.2478 0.074 Uiso 1 1 calc R U . . . H87C H 0.0059 0.2699 0.1940 0.074 Uiso 1 1 calc R U . . . C88 C 0.0214(4) 0.1650(3) 0.1480(3) 0.0570(17) Uani 1 1 d . . . . . H88A H -0.0404 0.1954 0.1343 0.085 Uiso 1 1 calc R U . . . H88B H 0.0126 0.1296 0.1887 0.085 Uiso 1 1 calc R U . . . H88C H 0.0430 0.1440 0.1155 0.085 Uiso 1 1 calc R U . . . C89 C 0.2465(4) 0.3418(2) 0.3203(2) 0.0362(12) Uani 1 1 d . . . . . H89 H 0.2169 0.3497 0.3570 0.043 Uiso 1 1 calc R U . . . C90 C 0.2155(3) 0.3862(2) 0.2633(2) 0.0327(12) Uani 1 1 d . . . . . H90 H 0.1667 0.4230 0.2638 0.039 Uiso 1 1 calc R U . . . C91 C 0.4292(4) 0.2897(3) 0.4117(3) 0.0438(14) Uani 1 1 d . . . . . C92 C 0.4698(4) 0.2621(3) 0.4737(3) 0.0527(16) Uani 1 1 d . . . . . H92 H 0.5186 0.2825 0.4852 0.063 Uiso 1 1 calc R U . . . C93 C 0.4404(5) 0.2065(3) 0.5176(3) 0.0577(18) Uani 1 1 d . . . . . H93 H 0.4692 0.1881 0.5590 0.069 Uiso 1 1 calc R U . . . C94 C 0.3683(5) 0.1770(3) 0.5016(3) 0.0516(16) Uani 1 1 d . . . . . H94 H 0.3484 0.1383 0.5327 0.062 Uiso 1 1 calc R U . . . C95 C 0.3241(4) 0.2023(3) 0.4412(3) 0.0428(14) Uani 1 1 d . . . . . C96 C 0.3584(4) 0.2585(3) 0.3953(2) 0.0352(12) Uani 1 1 d . . . . . C97 C 0.4614(4) 0.3536(3) 0.3672(3) 0.0493(15) Uani 1 1 d . . . . . H97 H 0.4392 0.3607 0.3229 0.059 Uiso 1 1 calc R U . . . C98 C 0.4130(5) 0.4145(3) 0.3866(3) 0.0659(19) Uani 1 1 d . . . . . H98A H 0.3421 0.4185 0.3839 0.099 Uiso 1 1 calc R U . . . H98B H 0.4337 0.4561 0.3576 0.099 Uiso 1 1 calc R U . . . H98C H 0.4322 0.4077 0.4305 0.099 Uiso 1 1 calc R U . . . C99 C 0.5722(5) 0.3512(4) 0.3665(3) 0.075(2) Uani 1 1 d . . . . . H99A H 0.5939 0.3522 0.4075 0.113 Uiso 1 1 calc R U . . . H99B H 0.5893 0.3904 0.3318 0.113 Uiso 1 1 calc R U . . . H99C H 0.6040 0.3094 0.3597 0.113 Uiso 1 1 calc R U . . . C100 C 0.2401(4) 0.1717(3) 0.4275(3) 0.0489(15) Uani 1 1 d . . . . . H100 H 0.2450 0.1721 0.3824 0.059 Uiso 1 1 calc R U . . . C101 C 0.1430(4) 0.2153(3) 0.4350(3) 0.073(2) Uani 1 1 d . . . . . H10G H 0.1398 0.2189 0.4779 0.109 Uiso 1 1 calc R U . . . H10H H 0.0887 0.1940 0.4287 0.109 Uiso 1 1 calc R U . . . H10I H 0.1388 0.2607 0.4030 0.109 Uiso 1 1 calc R U . . . C102 C 0.2391(5) 0.0990(3) 0.4716(3) 0.068(2) Uani 1 1 d . . . . . H10D H 0.3030 0.0718 0.4712 0.103 Uiso 1 1 calc R U . . . H10E H 0.1895 0.0797 0.4567 0.103 Uiso 1 1 calc R U . . . H10F H 0.2243 0.0987 0.5153 0.103 Uiso 1 1 calc R U . . . C103 C 0.2859(4) 0.4961(3) 0.1325(2) 0.0359(12) Uani 1 1 d . . . . . C104 C 0.2553(4) 0.5581(3) 0.0854(3) 0.0450(14) Uani 1 1 d . . . . . H104 H 0.2992 0.5898 0.0711 0.054 Uiso 1 1 calc R U . . . C105 C 0.1632(4) 0.5750(3) 0.0587(3) 0.0496(15) Uani 1 1 d . . . . . H105 H 0.1442 0.6177 0.0266 0.060 Uiso 1 1 calc R U . . . C106 C 0.0995(4) 0.5296(3) 0.0791(2) 0.0437(14) Uani 1 1 d . . . . . H106 H 0.0361 0.5414 0.0608 0.052 Uiso 1 1 calc R U . . . C107 C 0.1252(3) 0.4667(2) 0.1259(2) 0.0333(12) Uani 1 1 d . . . . . C108 C 0.2190(3) 0.4494(2) 0.1525(2) 0.0288(11) Uani 1 1 d . . . . . C109 C 0.3866(3) 0.4812(3) 0.1620(3) 0.0396(13) Uani 1 1 d . . . . . H109 H 0.4091 0.4313 0.1746 0.048 Uiso 1 1 calc R U . . . C110 C 0.3842(4) 0.5005(3) 0.2217(3) 0.0555(16) Uani 1 1 d . . . . . H11G H 0.3611 0.5493 0.2107 0.083 Uiso 1 1 calc R U . . . H11H H 0.4497 0.4896 0.2403 0.083 Uiso 1 1 calc R U . . . H11I H 0.3402 0.4753 0.2527 0.083 Uiso 1 1 calc R U . . . C111 C 0.4610(4) 0.5168(3) 0.1158(3) 0.0572(17) Uani 1 1 d . . . . . H11J H 0.4457 0.5658 0.1074 0.086 Uiso 1 1 calc R U . . . H11K H 0.4588 0.5075 0.0755 0.086 Uiso 1 1 calc R U . . . H11L H 0.5262 0.4999 0.1348 0.086 Uiso 1 1 calc R U . . . C112 C 0.0484(3) 0.4206(3) 0.1474(2) 0.0395(13) Uani 1 1 d . . . . . H112 H 0.0823 0.3738 0.1705 0.047 Uiso 1 1 calc R U . . . C113 C -0.0228(5) 0.4426(4) 0.1939(3) 0.084(2) Uani 1 1 d . . . . . H11M H 0.0125 0.4388 0.2325 0.127 Uiso 1 1 calc R U . . . H11N H -0.0730 0.4134 0.2056 0.127 Uiso 1 1 calc R U . . . H11O H -0.0533 0.4898 0.1734 0.127 Uiso 1 1 calc R U . . . C114 C -0.0085(4) 0.4178(3) 0.0919(3) 0.0460(14) Uani 1 1 d . . . . . H11D H -0.0507 0.4613 0.0726 0.069 Uiso 1 1 calc R U . . . H11E H -0.0483 0.3816 0.1074 0.069 Uiso 1 1 calc R U . . . H11F H 0.0368 0.4085 0.0597 0.069 Uiso 1 1 calc R U . . . C115 C 0.6119(4) 0.3173(4) 0.2241(3) 0.074(2) Uani 1 1 d . U . . . H11T H 0.6154 0.2830 0.2674 0.089 Uiso 1 1 calc R U . . . H11U H 0.5768 0.3606 0.2271 0.089 Uiso 1 1 calc R U . . . C116 C 0.7152(5) 0.3265(4) 0.1998(4) 0.090(2) Uani 1 1 d . U . . . H116 H 0.7497 0.3422 0.2294 0.108 Uiso 1 1 calc R U . . . C117 C 0.7660(5) 0.2617(4) 0.1990(4) 0.091(2) Uani 1 1 d . U . . . H11R H 0.7673 0.2285 0.2428 0.110 Uiso 1 1 calc R U . . . H11S H 0.8341 0.2663 0.1861 0.110 Uiso 1 1 calc R U . . . C118 C 0.7195(5) 0.2346(4) 0.1535(4) 0.086(2) Uani 1 1 d . U . . . H118 H 0.7567 0.1905 0.1524 0.103 Uiso 1 1 calc R U . . . C119 C 0.6093(5) 0.2283(3) 0.1762(4) 0.088(2) Uani 1 1 d . U . . . H11P H 0.5752 0.2142 0.1459 0.106 Uiso 1 1 calc R U . . . H11Q H 0.6093 0.1930 0.2189 0.106 Uiso 1 1 calc R U . . . C120 C 0.5561(3) 0.2947(3) 0.1794(3) 0.0365(12) Uani 1 1 d . U . . . C121 C 0.7137(5) 0.3759(4) 0.1346(4) 0.096(2) Uani 1 1 d . U . . . H12E H 0.6838 0.4213 0.1355 0.115 Uiso 1 1 calc R U . . . H12F H 0.7813 0.3786 0.1196 0.115 Uiso 1 1 calc R U . . . C122 C 0.6594(4) 0.3577(4) 0.0896(4) 0.077(2) Uani 1 1 d . U . . . H122 H 0.6569 0.3934 0.0465 0.092 Uiso 1 1 calc R U . . . C123 C 0.5553(4) 0.3488(3) 0.1141(3) 0.0665(19) Uani 1 1 d . U . . . H12A H 0.5203 0.3924 0.1165 0.080 Uiso 1 1 calc R U . . . H12B H 0.5199 0.3361 0.0833 0.080 Uiso 1 1 calc R U . . . C124 C 0.7079(6) 0.2900(4) 0.0854(4) 0.108(3) Uani 1 1 d . U . . . H12C H 0.7727 0.2946 0.0659 0.130 Uiso 1 1 calc R U . . . H12D H 0.6684 0.2759 0.0577 0.130 Uiso 1 1 calc R U . . . C125 C 0.8956(4) 0.1647(5) 0.3810(3) 0.143(4) Uani 1 1 d DG U . . . H12G H 0.9340 0.1682 0.3439 0.171 Uiso 1 1 calc R U . . . C126 C 0.8810(5) 0.1014(4) 0.4223(4) 0.168(4) Uani 1 1 d G U . . . H12H H 0.9095 0.0616 0.4135 0.201 Uiso 1 1 calc R U . . . C127 C 0.8248(6) 0.0963(4) 0.4766(4) 0.190(5) Uani 1 1 d G U . . . H12I H 0.8149 0.0530 0.5049 0.227 Uiso 1 1 calc R U . . . C128 C 0.7832(5) 0.1545(6) 0.4895(3) 0.193(5) Uani 1 1 d G U . . . H12J H 0.7448 0.1511 0.5266 0.231 Uiso 1 1 calc R U . . . C129 C 0.7978(5) 0.2179(4) 0.4482(4) 0.157(4) Uani 1 1 d DG U . . . H12K H 0.7693 0.2577 0.4570 0.189 Uiso 1 1 calc R U . . . C130 C 0.8539(5) 0.2229(4) 0.3939(4) 0.157(4) Uani 1 1 d DG U . . . C131 C 0.8718(10) 0.2889(5) 0.3546(6) 0.248(7) Uani 1 1 d D U . . . H13D H 0.9123 0.2851 0.3184 0.372 Uiso 1 1 calc R U . . . H13E H 0.9055 0.3087 0.3799 0.372 Uiso 1 1 calc R U . . . H13F H 0.8098 0.3181 0.3387 0.372 Uiso 1 1 calc R U . . . O1 O 0.6557(5) 0.3277(3) 0.5365(3) 0.146(3) Uani 1 1 d G U . . . C132 C 0.6747(6) 0.3965(4) 0.5096(3) 0.153(4) Uani 1 1 d G U . . . H13G H 0.6617 0.4142 0.4629 0.183 Uiso 1 1 calc R U . . . H13H H 0.7433 0.3986 0.5172 0.183 Uiso 1 1 calc R U . . . C133 C 0.6062(7) 0.4382(3) 0.5433(5) 0.223(6) Uani 1 1 d G U . . . H13I H 0.5421 0.4551 0.5214 0.268 Uiso 1 1 calc R U . . . H13J H 0.6346 0.4770 0.5459 0.268 Uiso 1 1 calc R U . . . C134 C 0.5980(7) 0.3853(5) 0.6098(4) 0.200(5) Uani 1 1 d G U . . . H13K H 0.6544 0.3804 0.6375 0.240 Uiso 1 1 calc R U . . . H13L H 0.5373 0.3970 0.6313 0.240 Uiso 1 1 calc R U . . . C135 C 0.5972(6) 0.3209(4) 0.5929(3) 0.166(4) Uani 1 1 d G U . . . H13M H 0.6249 0.2802 0.6286 0.200 Uiso 1 1 calc R U . . . H13N H 0.5299 0.3167 0.5843 0.200 Uiso 1 1 calc R U . . . 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 Cr1 0.0279(4) 0.0252(4) 0.0289(4) -0.0082(3) -0.0003(3) -0.0045(3) Cr2 0.0290(4) 0.0280(4) 0.0294(4) -0.0080(4) -0.0018(3) -0.0052(3) Cr3 0.0252(4) 0.0293(5) 0.0310(4) -0.0103(4) -0.0007(3) -0.0019(3) Cr4 0.0222(4) 0.0274(4) 0.0294(4) -0.0098(3) 0.0005(3) -0.0050(3) N1 0.024(2) 0.024(2) 0.031(2) -0.0055(17) -0.0031(16) -0.0033(16) N2 0.029(2) 0.027(2) 0.033(2) -0.0094(18) -0.0011(17) -0.0011(17) N3 0.034(2) 0.030(2) 0.030(2) -0.0073(19) -0.0005(18) -0.0006(18) N4 0.038(2) 0.033(2) 0.029(2) -0.0072(19) -0.0050(18) -0.0044(19) N5 0.024(2) 0.032(2) 0.034(2) -0.0123(19) -0.0012(17) -0.0071(17) N6 0.030(2) 0.026(2) 0.033(2) -0.0080(18) -0.0009(17) -0.0024(17) N7 0.026(2) 0.031(2) 0.033(2) -0.0107(19) 0.0003(17) -0.0039(17) N8 0.032(2) 0.030(2) 0.028(2) -0.0085(18) 0.0006(17) -0.0019(18) N9 0.025(2) 0.027(2) 0.030(2) -0.0085(18) 0.0029(16) -0.0082(16) N10 0.023(2) 0.034(2) 0.038(2) -0.0168(19) 0.0007(17) -0.0049(17) C1 0.028(2) 0.029(3) 0.036(3) -0.015(2) -0.001(2) -0.008(2) C2 0.032(3) 0.027(3) 0.035(3) -0.017(2) -0.003(2) -0.004(2) C3 0.029(3) 0.036(3) 0.045(3) -0.015(3) -0.001(2) -0.004(2) C4 0.027(3) 0.061(4) 0.059(4) -0.027(3) -0.007(3) -0.007(3) C5 0.037(3) 0.059(4) 0.048(4) -0.020(3) -0.014(3) 0.006(3) C6 0.041(3) 0.043(3) 0.043(3) -0.004(3) -0.007(3) -0.006(3) C7 0.034(3) 0.031(3) 0.033(3) -0.011(2) -0.007(2) -0.003(2) C8 0.028(3) 0.030(3) 0.033(3) -0.016(2) -0.004(2) 0.001(2) C9 0.030(3) 0.040(3) 0.064(4) -0.013(3) 0.005(3) -0.010(2) C10 0.061(4) 0.058(5) 0.100(6) -0.014(4) -0.003(4) -0.025(4) C11 0.081(5) 0.048(4) 0.062(4) -0.012(3) 0.015(4) -0.018(3) C12 0.041(3) 0.033(3) 0.036(3) -0.006(2) -0.006(2) -0.003(2) C13 0.046(4) 0.069(5) 0.068(4) -0.037(4) 0.013(3) -0.011(3) C14 0.067(4) 0.040(4) 0.049(4) -0.007(3) 0.004(3) -0.010(3) C15 0.038(3) 0.030(3) 0.029(3) -0.009(2) 0.003(2) 0.002(2) C16 0.043(3) 0.046(4) 0.035(3) -0.010(3) 0.000(2) 0.007(3) C17 0.057(4) 0.029(3) 0.036(3) 0.002(2) 0.000(3) 0.004(3) C18 0.056(4) 0.027(3) 0.044(3) -0.008(2) 0.003(3) -0.009(3) C19 0.044(3) 0.033(3) 0.027(3) -0.009(2) 0.001(2) -0.007(2) C20 0.035(3) 0.025(3) 0.028(3) -0.009(2) 0.000(2) -0.002(2) C21 0.033(3) 0.043(3) 0.051(4) -0.014(3) 0.005(3) 0.003(2) C22 0.074(5) 0.050(4) 0.083(5) -0.011(4) 0.036(4) -0.003(3) C23 0.054(4) 0.079(5) 0.076(5) -0.013(4) -0.024(4) -0.010(4) C24 0.040(3) 0.043(3) 0.045(3) -0.008(3) 0.003(3) -0.015(3) C25 0.057(4) 0.056(4) 0.065(4) -0.022(3) 0.001(3) -0.020(3) C26 0.047(4) 0.056(4) 0.065(4) -0.010(3) 0.008(3) -0.019(3) C27 0.048(3) 0.036(3) 0.037(3) -0.019(3) 0.002(2) -0.003(2) C28 0.054(3) 0.038(3) 0.032(3) -0.015(3) 0.001(2) -0.009(3) C29 0.071(4) 0.030(3) 0.044(3) -0.016(3) 0.000(3) 0.001(3) C30 0.107(6) 0.036(4) 0.047(4) -0.015(3) -0.002(4) -0.001(4) C31 0.118(7) 0.038(4) 0.051(4) -0.021(3) -0.022(4) 0.024(4) C32 0.085(5) 0.047(4) 0.060(4) -0.030(4) -0.024(4) 0.021(4) C33 0.063(4) 0.036(3) 0.040(3) -0.024(3) -0.011(3) 0.012(3) C34 0.051(3) 0.030(3) 0.033(3) -0.015(2) -0.006(2) 0.003(2) C35 0.068(4) 0.035(3) 0.051(4) -0.016(3) 0.006(3) -0.013(3) C36 0.105(6) 0.044(4) 0.070(5) -0.024(4) 0.023(4) -0.035(4) C37 0.071(5) 0.067(5) 0.064(4) -0.024(4) 0.006(4) -0.025(4) C38 0.044(4) 0.050(4) 0.080(5) -0.027(4) -0.011(3) 0.009(3) C39 0.046(4) 0.090(6) 0.098(6) -0.060(5) -0.016(4) 0.011(4) C40 0.059(4) 0.116(7) 0.067(5) -0.026(5) -0.002(4) -0.014(4) C41 0.059(4) 0.056(4) 0.038(3) -0.008(3) -0.012(3) -0.017(3) C42 0.066(4) 0.096(6) 0.046(4) -0.010(4) -0.019(3) -0.036(4) C43 0.063(4) 0.081(5) 0.041(4) 0.005(3) -0.024(3) -0.010(4) C44 0.057(4) 0.053(4) 0.045(4) 0.006(3) -0.008(3) -0.014(3) C45 0.045(3) 0.040(3) 0.032(3) -0.007(2) -0.001(2) -0.006(3) C46 0.048(3) 0.039(3) 0.026(3) -0.005(2) -0.011(2) -0.008(3) C47 0.084(5) 0.069(5) 0.041(4) -0.009(3) -0.016(3) -0.044(4) C48 0.090(5) 0.114(7) 0.046(4) -0.001(4) -0.011(4) -0.069(5) C49 0.111(6) 0.073(5) 0.072(5) -0.016(4) -0.032(4) -0.037(5) C50 0.047(3) 0.035(3) 0.036(3) -0.006(2) 0.004(2) -0.008(2) C51 0.072(4) 0.043(4) 0.042(3) -0.005(3) -0.002(3) -0.015(3) C52 0.054(4) 0.059(4) 0.101(6) -0.035(4) 0.032(4) -0.019(3) C53 0.024(2) 0.032(3) 0.044(3) -0.011(2) 0.001(2) -0.012(2) C54 0.035(3) 0.048(3) 0.038(3) -0.011(3) -0.002(2) -0.016(2) C55 0.029(3) 0.059(4) 0.059(4) -0.013(3) -0.003(3) -0.015(3) C56 0.041(3) 0.051(4) 0.066(4) -0.010(3) 0.012(3) -0.026(3) C57 0.043(3) 0.044(4) 0.054(4) 0.006(3) 0.008(3) -0.017(3) C58 0.038(3) 0.045(3) 0.043(3) -0.008(3) 0.014(2) -0.013(3) C59 0.028(3) 0.044(3) 0.047(3) -0.018(3) 0.002(2) -0.011(2) C60 0.034(3) 0.066(4) 0.049(4) -0.026(3) 0.012(3) -0.018(3) C61 0.031(3) 0.061(4) 0.061(4) -0.012(3) 0.008(3) -0.007(3) C62 0.037(3) 0.079(5) 0.048(4) -0.010(3) 0.011(3) -0.014(3) C63 0.028(3) 0.034(3) 0.041(3) -0.017(2) 0.001(2) -0.003(2) C64 0.023(2) 0.036(3) 0.037(3) -0.018(2) 0.000(2) -0.007(2) C65 0.048(3) 0.041(3) 0.036(3) -0.012(3) -0.006(3) 0.012(3) C66 0.063(4) 0.059(4) 0.038(3) -0.007(3) -0.005(3) 0.016(3) C67 0.068(4) 0.043(4) 0.048(4) 0.003(3) 0.003(3) 0.011(3) C68 0.073(5) 0.031(3) 0.056(4) -0.001(3) 0.005(3) -0.001(3) C69 0.048(3) 0.031(3) 0.046(3) -0.009(3) 0.008(3) -0.001(3) C70 0.042(3) 0.031(3) 0.037(3) -0.010(2) -0.001(2) 0.008(2) C71 0.046(3) 0.052(4) 0.039(3) -0.007(3) -0.008(3) 0.007(3) C72 0.056(4) 0.089(6) 0.063(4) -0.034(4) -0.015(3) 0.002(4) C73 0.047(4) 0.085(5) 0.071(5) -0.026(4) 0.000(3) 0.016(3) C74 0.047(3) 0.039(3) 0.060(4) -0.009(3) 0.006(3) -0.012(3) C75 0.056(4) 0.062(5) 0.073(5) -0.012(4) 0.011(3) -0.015(3) C76 0.067(4) 0.044(4) 0.088(5) -0.021(4) -0.006(4) -0.018(3) C77 0.032(3) 0.031(3) 0.037(3) -0.018(2) 0.005(2) -0.003(2) C78 0.042(3) 0.037(3) 0.032(3) -0.012(2) -0.001(2) 0.002(2) C79 0.037(3) 0.041(3) 0.045(3) -0.024(3) -0.016(2) 0.006(2) C80 0.030(3) 0.042(3) 0.050(3) -0.020(3) -0.004(2) -0.002(2) C81 0.029(3) 0.035(3) 0.041(3) -0.015(2) -0.003(2) -0.003(2) C82 0.025(2) 0.031(3) 0.032(3) -0.015(2) -0.005(2) 0.000(2) C83 0.043(3) 0.045(3) 0.029(3) -0.011(2) 0.000(2) -0.012(3) C84 0.062(4) 0.054(4) 0.049(4) -0.009(3) 0.005(3) -0.024(3) C85 0.039(3) 0.079(5) 0.061(4) -0.037(4) 0.010(3) -0.016(3) C86 0.028(3) 0.040(3) 0.044(3) -0.013(3) 0.001(2) -0.005(2) C87 0.053(4) 0.050(4) 0.045(3) -0.013(3) 0.011(3) -0.017(3) C88 0.048(4) 0.062(4) 0.066(4) -0.019(3) 0.006(3) -0.030(3) C89 0.041(3) 0.032(3) 0.031(3) -0.009(2) 0.008(2) -0.002(2) C90 0.030(3) 0.028(3) 0.038(3) -0.011(2) 0.006(2) -0.001(2) C91 0.047(3) 0.046(4) 0.038(3) -0.018(3) -0.002(3) 0.002(3) C92 0.050(4) 0.070(5) 0.041(3) -0.027(3) -0.011(3) 0.000(3) C93 0.078(5) 0.052(4) 0.037(3) -0.017(3) -0.014(3) 0.015(3) C94 0.076(4) 0.040(4) 0.033(3) -0.010(3) 0.002(3) 0.005(3) C95 0.049(3) 0.043(3) 0.036(3) -0.017(3) 0.004(3) 0.002(3) C96 0.038(3) 0.035(3) 0.031(3) -0.012(2) -0.001(2) 0.002(2) C97 0.053(4) 0.063(4) 0.042(3) -0.025(3) 0.004(3) -0.023(3) C98 0.093(5) 0.058(4) 0.053(4) -0.020(3) 0.004(4) -0.026(4) C99 0.071(5) 0.108(6) 0.067(5) -0.043(4) 0.008(4) -0.043(4) C100 0.062(4) 0.045(4) 0.035(3) -0.007(3) 0.007(3) -0.012(3) C101 0.051(4) 0.066(5) 0.086(5) -0.006(4) 0.006(4) -0.012(3) C102 0.091(5) 0.048(4) 0.062(4) -0.007(3) 0.016(4) -0.025(4) C103 0.035(3) 0.035(3) 0.036(3) -0.012(2) 0.006(2) -0.003(2) C104 0.054(4) 0.033(3) 0.043(3) -0.005(3) 0.009(3) -0.012(3) C105 0.066(4) 0.029(3) 0.040(3) 0.003(2) 0.003(3) 0.000(3) C106 0.040(3) 0.043(3) 0.039(3) -0.008(3) -0.004(2) 0.004(3) C107 0.034(3) 0.031(3) 0.035(3) -0.012(2) 0.001(2) -0.003(2) C108 0.029(3) 0.029(3) 0.027(3) -0.007(2) 0.005(2) -0.007(2) C109 0.031(3) 0.031(3) 0.056(4) -0.011(3) 0.002(2) -0.012(2) C110 0.043(3) 0.056(4) 0.064(4) -0.009(3) -0.005(3) -0.020(3) C111 0.043(3) 0.049(4) 0.081(5) -0.018(3) 0.021(3) -0.024(3) C112 0.031(3) 0.042(3) 0.043(3) -0.013(3) -0.004(2) 0.001(2) C113 0.063(5) 0.149(8) 0.069(5) -0.058(5) 0.025(4) -0.053(5) C114 0.038(3) 0.058(4) 0.049(4) -0.028(3) -0.009(3) -0.002(3) C115 0.037(3) 0.106(5) 0.089(5) -0.041(4) -0.001(3) -0.019(3) C116 0.042(4) 0.103(5) 0.137(6) -0.050(4) 0.003(4) -0.020(3) C117 0.043(4) 0.093(5) 0.136(6) -0.035(4) 0.029(4) -0.017(3) C118 0.054(4) 0.063(4) 0.152(6) -0.051(4) 0.054(4) -0.023(3) C119 0.059(4) 0.062(4) 0.151(6) -0.049(4) 0.054(4) -0.019(3) C120 0.022(2) 0.042(3) 0.050(3) -0.019(2) 0.008(2) -0.011(2) C121 0.046(4) 0.093(5) 0.144(6) -0.029(4) 0.024(4) -0.026(4) C122 0.042(3) 0.090(5) 0.086(5) -0.013(4) 0.030(3) -0.012(3) C123 0.033(3) 0.092(5) 0.063(4) -0.012(3) 0.014(3) -0.013(3) C124 0.078(5) 0.126(6) 0.135(6) -0.061(4) 0.067(4) -0.039(4) C125 0.082(6) 0.205(9) 0.144(8) -0.054(7) 0.018(6) -0.042(7) C126 0.085(7) 0.263(10) 0.146(9) -0.034(7) 0.002(6) -0.075(7) C127 0.136(10) 0.288(12) 0.149(9) -0.048(8) -0.008(6) -0.095(9) C128 0.152(9) 0.296(12) 0.145(9) -0.071(9) -0.041(7) -0.068(9) C129 0.112(8) 0.272(11) 0.123(8) -0.096(7) -0.043(6) -0.054(7) C130 0.106(8) 0.237(10) 0.138(8) -0.061(7) -0.047(6) -0.041(7) C131 0.244(15) 0.244(12) 0.238(13) -0.029(9) -0.072(11) -0.077(10) O1 0.176(7) 0.159(6) 0.134(6) -0.073(5) 0.042(5) -0.068(5) C132 0.194(10) 0.162(8) 0.124(8) -0.052(6) 0.038(7) -0.091(7) C133 0.318(15) 0.173(9) 0.185(11) -0.077(7) 0.064(10) -0.040(9) C134 0.247(13) 0.221(11) 0.170(9) -0.097(8) 0.076(9) -0.092(10) C135 0.223(11) 0.207(10) 0.102(7) -0.064(7) 0.049(7) -0.108(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 Cr1 N5 1.800(4) . ? Cr1 N3 1.914(4) . ? Cr1 N1 1.942(4) . ? Cr1 Cr2 1.9560(11) . ? Cr2 N4 1.886(4) . ? Cr2 N2 1.910(4) . ? Cr2 N5 1.929(4) . ? Cr3 N8 1.893(4) . ? Cr3 N6 1.899(4) . ? Cr3 N10 1.938(4) . ? Cr3 Cr4 1.9594(11) . ? Cr4 N10 1.799(4) . ? Cr4 N9 1.907(4) . ? Cr4 N7 1.938(4) . ? N1 C1 1.378(5) . ? N1 C8 1.445(5) . ? N2 C2 1.379(6) . ? N2 C20 1.451(6) . ? N3 C27 1.379(6) . ? N3 C34 1.459(6) . ? N4 C28 1.380(6) . ? N4 C46 1.451(6) . ? N5 C53 1.467(5) . ? N6 C63 1.392(6) . ? N6 C70 1.462(6) . ? N7 C64 1.393(6) . ? N7 C82 1.440(6) . ? N8 C89 1.391(6) . ? N8 C96 1.452(6) . ? N9 C90 1.389(5) . ? N9 C108 1.464(5) . ? N10 C120 1.459(5) . ? C1 C2 1.356(6) . ? C3 C4 1.384(7) . ? C3 C8 1.411(6) . ? C3 C9 1.518(7) . ? C4 C5 1.383(7) . ? C5 C6 1.371(7) . ? C6 C7 1.405(7) . ? C7 C8 1.402(6) . ? C7 C12 1.525(7) . ? C9 C11 1.519(8) . ? C9 C10 1.526(7) . ? C12 C14 1.512(7) . ? C12 C13 1.522(7) . ? C15 C20 1.396(6) . ? C15 C16 1.406(7) . ? C15 C21 1.506(7) . ? C16 C17 1.372(7) . ? C17 C18 1.373(7) . ? C18 C19 1.391(7) . ? C19 C20 1.413(7) . ? C19 C24 1.534(7) . ? C21 C23 1.521(8) . ? C21 C22 1.530(7) . ? C24 C25 1.542(7) . ? C24 C26 1.549(7) . ? C27 C28 1.346(7) . ? C29 C30 1.403(7) . ? C29 C34 1.418(8) . ? C29 C35 1.502(8) . ? C30 C31 1.368(9) . ? C31 C32 1.374(9) . ? C32 C33 1.378(7) . ? C33 C34 1.414(7) . ? C33 C38 1.499(8) . ? C35 C37 1.539(8) . ? C35 C36 1.540(7) . ? C38 C40 1.535(8) . ? C38 C39 1.537(8) . ? C41 C42 1.393(8) . ? C41 C46 1.406(7) . ? C41 C47 1.521(8) . ? C42 C43 1.369(8) . ? C43 C44 1.380(8) . ? C44 C45 1.391(7) . ? C45 C46 1.423(7) . ? C45 C50 1.504(7) . ? C47 C48 1.523(8) . ? C47 C49 1.550(9) . ? C50 C52 1.530(7) . ? C50 C51 1.535(7) . ? C53 C58 1.518(7) . ? C53 C54 1.540(6) . ? C53 C59 1.542(7) . ? C54 C55 1.523(7) . ? C55 C56 1.527(7) . ? C55 C61 1.530(8) . ? C56 C57 1.528(8) . ? C57 C62 1.536(8) . ? C57 C58 1.541(6) . ? C59 C60 1.538(6) . ? C60 C62 1.506(8) . ? C60 C61 1.529(7) . ? C63 C64 1.342(6) . ? C65 C66 1.404(7) . ? C65 C70 1.408(7) . ? C65 C71 1.513(8) . ? C66 C67 1.366(8) . ? C67 C68 1.377(8) . ? C68 C69 1.379(7) . ? C69 C70 1.411(7) . ? C69 C74 1.526(8) . ? C71 C72 1.517(8) . ? C71 C73 1.542(7) . ? C74 C75 1.537(7) . ? C74 C76 1.539(8) . ? C77 C78 1.405(7) . ? C77 C82 1.407(6) . ? C77 C83 1.512(7) . ? C78 C79 1.370(7) . ? C79 C80 1.377(7) . ? C80 C81 1.393(7) . ? C81 C82 1.407(6) . ? C81 C86 1.507(7) . ? C83 C85 1.522(7) . ? C83 C84 1.524(7) . ? C86 C87 1.528(7) . ? C86 C88 1.538(7) . ? C89 C90 1.338(6) . ? C91 C96 1.398(7) . ? C91 C92 1.406(7) . ? C91 C97 1.509(8) . ? C92 C93 1.363(8) . ? C93 C94 1.384(8) . ? C94 C95 1.397(7) . ? C95 C96 1.420(7) . ? C95 C100 1.516(8) . ? C97 C98 1.539(8) . ? C97 C99 1.537(8) . ? C100 C102 1.527(7) . ? C100 C101 1.546(7) . ? C103 C104 1.391(7) . ? C103 C108 1.422(6) . ? C103 C109 1.516(7) . ? C104 C105 1.379(7) . ? C105 C106 1.368(7) . ? C106 C107 1.391(7) . ? C107 C108 1.400(6) . ? C107 C112 1.521(7) . ? C109 C110 1.510(7) . ? C109 C111 1.530(6) . ? C112 C114 1.520(7) . ? C112 C113 1.532(7) . ? C115 C120 1.525(8) . ? C115 C116 1.535(8) . ? C116 C117 1.445(9) . ? C116 C121 1.474(10) . ? C117 C118 1.532(10) . ? C118 C124 1.568(11) . ? C118 C119 1.608(8) . ? C119 C120 1.504(7) . ? C120 C123 1.517(7) . ? C121 C122 1.464(10) . ? C122 C124 1.514(10) . ? C122 C123 1.545(7) . ? C125 C126 1.3900 . ? C125 C130 1.3900 . ? C126 C127 1.3900 . ? C127 C128 1.3900 . ? C128 C129 1.3900 . ? C129 C130 1.3900 . ? C130 C131 1.434(8) . ? O1 C135 1.4432 . ? O1 C132 1.4433 . ? C132 C133 1.5349 . ? C133 C134 1.5387 . ? C134 C135 1.5349 . ? 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 N5 Cr1 N3 126.68(18) . . ? N5 Cr1 N1 112.71(16) . . ? N3 Cr1 N1 120.27(16) . . ? N5 Cr1 Cr2 61.62(12) . . ? N3 Cr1 Cr2 108.51(12) . . ? N1 Cr1 Cr2 103.88(11) . . ? N4 Cr2 N2 135.26(17) . . ? N4 Cr2 N5 120.27(17) . . ? N2 Cr2 N5 104.16(16) . . ? N4 Cr2 Cr1 102.49(13) . . ? N2 Cr2 Cr1 107.13(12) . . ? N5 Cr2 Cr1 55.22(11) . . ? N8 Cr3 N6 133.74(17) . . ? N8 Cr3 N10 122.05(17) . . ? N6 Cr3 N10 104.04(16) . . ? N8 Cr3 Cr4 103.44(12) . . ? N6 Cr3 Cr4 106.22(13) . . ? N10 Cr3 Cr4 54.97(11) . . ? N10 Cr4 N9 126.14(17) . . ? N10 Cr4 N7 113.46(17) . . ? N9 Cr4 N7 119.99(16) . . ? N10 Cr4 Cr3 61.90(13) . . ? N9 Cr4 Cr3 108.27(12) . . ? N7 Cr4 Cr3 104.59(12) . . ? C1 N1 C8 112.2(4) . . ? C1 N1 Cr1 120.2(3) . . ? C8 N1 Cr1 125.6(3) . . ? C2 N2 C20 113.2(4) . . ? C2 N2 Cr2 123.0(3) . . ? C20 N2 Cr2 123.8(3) . . ? C27 N3 C34 112.8(4) . . ? C27 N3 Cr1 125.5(3) . . ? C34 N3 Cr1 120.8(3) . . ? C28 N4 C46 113.5(4) . . ? C28 N4 Cr2 130.3(3) . . ? C46 N4 Cr2 116.0(3) . . ? C53 N5 Cr1 148.7(3) . . ? C53 N5 Cr2 147.1(3) . . ? Cr1 N5 Cr2 63.16(12) . . ? C63 N6 C70 112.9(4) . . ? C63 N6 Cr3 124.1(3) . . ? C70 N6 Cr3 123.0(3) . . ? C64 N7 C82 113.0(4) . . ? C64 N7 Cr4 119.8(3) . . ? C82 N7 Cr4 125.7(3) . . ? C89 N8 C96 113.9(4) . . ? C89 N8 Cr3 128.6(3) . . ? C96 N8 Cr3 117.3(3) . . ? C90 N9 C108 112.8(4) . . ? C90 N9 Cr4 124.8(3) . . ? C108 N9 Cr4 122.1(3) . . ? C120 N10 Cr4 148.0(3) . . ? C120 N10 Cr3 148.8(3) . . ? Cr4 N10 Cr3 63.13(12) . . ? C2 C1 N1 127.3(4) . . ? C1 C2 N2 126.6(4) . . ? C4 C3 C8 117.8(5) . . ? C4 C3 C9 121.0(5) . . ? C8 C3 C9 121.1(4) . . ? C5 C4 C3 122.2(5) . . ? C6 C5 C4 119.8(5) . . ? C5 C6 C7 120.6(5) . . ? C8 C7 C6 118.9(5) . . ? C8 C7 C12 122.5(4) . . ? C6 C7 C12 118.3(4) . . ? C7 C8 C3 120.7(4) . . ? C7 C8 N1 120.7(4) . . ? C3 C8 N1 118.6(4) . . ? C11 C9 C3 112.3(5) . . ? C11 C9 C10 110.2(5) . . ? C3 C9 C10 114.1(5) . . ? C14 C12 C13 110.9(4) . . ? C14 C12 C7 113.7(4) . . ? C13 C12 C7 109.9(4) . . ? C20 C15 C16 118.8(5) . . ? C20 C15 C21 123.1(4) . . ? C16 C15 C21 117.9(5) . . ? C17 C16 C15 121.3(5) . . ? C16 C17 C18 119.6(5) . . ? C17 C18 C19 121.6(5) . . ? C18 C19 C20 118.8(5) . . ? C18 C19 C24 118.2(5) . . ? C20 C19 C24 123.0(5) . . ? C15 C20 C19 119.9(5) . . ? C15 C20 N2 120.3(4) . . ? C19 C20 N2 119.8(4) . . ? C15 C21 C23 113.8(5) . . ? C15 C21 C22 108.3(5) . . ? C23 C21 C22 110.8(5) . . ? C19 C24 C25 111.4(4) . . ? C19 C24 C26 111.7(5) . . ? C25 C24 C26 109.4(5) . . ? C28 C27 N3 126.4(5) . . ? C27 C28 N4 126.0(5) . . ? C30 C29 C34 117.7(6) . . ? C30 C29 C35 119.6(6) . . ? C34 C29 C35 122.5(5) . . ? C31 C30 C29 121.0(7) . . ? C30 C31 C32 120.8(6) . . ? C31 C32 C33 121.3(7) . . ? C32 C33 C34 118.5(6) . . ? C32 C33 C38 119.4(6) . . ? C34 C33 C38 122.1(5) . . ? C33 C34 C29 120.6(5) . . ? C33 C34 N3 119.6(5) . . ? C29 C34 N3 119.7(5) . . ? C29 C35 C37 110.3(5) . . ? C29 C35 C36 112.5(5) . . ? C37 C35 C36 108.7(5) . . ? C33 C38 C40 111.7(5) . . ? C33 C38 C39 113.4(6) . . ? C40 C38 C39 109.1(5) . . ? C42 C41 C46 118.1(5) . . ? C42 C41 C47 118.3(5) . . ? C46 C41 C47 123.5(5) . . ? C43 C42 C41 121.5(6) . . ? C42 C43 C44 120.3(6) . . ? C43 C44 C45 121.4(6) . . ? C44 C45 C46 117.6(5) . . ? C44 C45 C50 120.1(5) . . ? C46 C45 C50 122.2(5) . . ? C41 C46 C45 121.0(5) . . ? C41 C46 N4 119.2(5) . . ? C45 C46 N4 119.8(5) . . ? C41 C47 C48 111.8(6) . . ? C41 C47 C49 109.5(5) . . ? C48 C47 C49 109.9(5) . . ? C45 C50 C52 111.0(5) . . ? C45 C50 C51 113.1(4) . . ? C52 C50 C51 110.0(4) . . ? N5 C53 C58 111.1(4) . . ? N5 C53 C54 111.2(4) . . ? C58 C53 C54 108.4(4) . . ? N5 C53 C59 108.7(4) . . ? C58 C53 C59 108.9(4) . . ? C54 C53 C59 108.4(4) . . ? C55 C54 C53 110.5(4) . . ? C54 C55 C56 109.8(4) . . ? C54 C55 C61 109.9(5) . . ? C56 C55 C61 109.6(5) . . ? C55 C56 C57 108.8(5) . . ? C56 C57 C62 109.5(5) . . ? C56 C57 C58 109.3(5) . . ? C62 C57 C58 108.6(5) . . ? C53 C58 C57 110.9(4) . . ? C60 C59 C53 109.5(4) . . ? C62 C60 C61 109.1(5) . . ? C62 C60 C59 110.0(4) . . ? C61 C60 C59 110.1(5) . . ? C55 C61 C60 109.0(5) . . ? C60 C62 C57 110.0(5) . . ? C64 C63 N6 126.2(5) . . ? C63 C64 N7 127.2(5) . . ? C66 C65 C70 117.6(6) . . ? C66 C65 C71 118.8(5) . . ? C70 C65 C71 123.4(5) . . ? C67 C66 C65 122.2(6) . . ? C66 C67 C68 118.8(6) . . ? C67 C68 C69 122.5(6) . . ? C68 C69 C70 118.1(5) . . ? C68 C69 C74 118.0(5) . . ? C70 C69 C74 123.9(5) . . ? C65 C70 C69 120.6(5) . . ? C65 C70 N6 119.8(5) . . ? C69 C70 N6 119.6(5) . . ? C65 C71 C72 113.4(5) . . ? C65 C71 C73 109.3(5) . . ? C72 C71 C73 110.5(5) . . ? C69 C74 C75 112.4(5) . . ? C69 C74 C76 111.8(5) . . ? C75 C74 C76 109.8(5) . . ? C78 C77 C82 118.2(5) . . ? C78 C77 C83 118.7(4) . . ? C82 C77 C83 122.7(4) . . ? C79 C78 C77 121.6(5) . . ? C78 C79 C80 119.0(5) . . ? C79 C80 C81 122.7(5) . . ? C80 C81 C82 117.4(5) . . ? C80 C81 C86 121.3(5) . . ? C82 C81 C86 121.3(4) . . ? C81 C82 C77 121.0(4) . . ? C81 C82 N7 118.5(4) . . ? C77 C82 N7 120.5(4) . . ? C77 C83 C85 110.2(4) . . ? C77 C83 C84 113.5(4) . . ? C85 C83 C84 111.1(4) . . ? C81 C86 C87 112.2(4) . . ? C81 C86 C88 114.2(5) . . ? C87 C86 C88 109.5(4) . . ? C90 C89 N8 126.1(4) . . ? C89 C90 N9 127.2(4) . . ? C96 C91 C92 118.7(5) . . ? C96 C91 C97 123.4(5) . . ? C92 C91 C97 117.9(5) . . ? C93 C92 C91 121.1(6) . . ? C92 C93 C94 119.9(6) . . ? C93 C94 C95 121.9(6) . . ? C94 C95 C96 117.4(5) . . ? C94 C95 C100 120.0(5) . . ? C96 C95 C100 122.6(5) . . ? C91 C96 C95 120.9(5) . . ? C91 C96 N8 119.3(5) . . ? C95 C96 N8 119.8(5) . . ? C91 C97 C98 109.5(5) . . ? C91 C97 C99 113.4(5) . . ? C98 C97 C99 109.0(5) . . ? C95 C100 C102 113.2(5) . . ? C95 C100 C101 109.5(5) . . ? C102 C100 C101 108.5(5) . . ? C104 C103 C108 117.8(5) . . ? C104 C103 C109 120.0(5) . . ? C108 C103 C109 122.2(4) . . ? C105 C104 C103 122.2(5) . . ? C106 C105 C104 119.2(5) . . ? C105 C106 C107 121.8(5) . . ? C106 C107 C108 118.9(5) . . ? C106 C107 C112 118.1(5) . . ? C108 C107 C112 123.0(4) . . ? C107 C108 C103 120.2(4) . . ? C107 C108 N9 119.9(4) . . ? C103 C108 N9 119.8(4) . . ? C110 C109 C103 111.0(4) . . ? C110 C109 C111 109.2(5) . . ? C103 C109 C111 113.0(5) . . ? C114 C112 C107 112.8(4) . . ? C114 C112 C113 109.1(4) . . ? C107 C112 C113 111.2(5) . . ? C120 C115 C116 111.2(6) . . ? C117 C116 C121 108.8(8) . . ? C117 C116 C115 108.1(7) . . ? C121 C116 C115 111.3(6) . . ? C116 C117 C118 113.1(7) . . ? C117 C118 C124 109.1(6) . . ? C117 C118 C119 107.1(6) . . ? C124 C118 C119 103.7(6) . . ? C120 C119 C118 110.9(5) . . ? N10 C120 C119 110.6(4) . . ? N10 C120 C123 111.8(4) . . ? C119 C120 C123 109.7(5) . . ? N10 C120 C115 109.4(4) . . ? C119 C120 C115 108.8(5) . . ? C123 C120 C115 106.5(5) . . ? C122 C121 C116 112.2(7) . . ? C121 C122 C124 109.4(7) . . ? C121 C122 C123 110.4(6) . . ? C124 C122 C123 106.7(6) . . ? C120 C123 C122 111.7(5) . . ? C122 C124 C118 110.8(6) . . ? C126 C125 C130 120.0 . . ? C125 C126 C127 120.0 . . ? C128 C127 C126 120.0 . . ? C127 C128 C129 120.0 . . ? C130 C129 C128 120.0 . . ? C131 C130 C129 118.1(6) . . ? C131 C130 C125 121.8(6) . . ? C129 C130 C125 120.0 . . ? C135 O1 C132 109.5 . . ? O1 C132 C133 106.4 . . ? C132 C133 C134 101.5 . . ? C135 C134 C133 101.5 . . ? O1 C135 C134 106.4 . . ? _refine_diff_density_max 0.748 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.079 _shelxl_version_number 2013-2 _shelx_res_file ; TITL klat946 in P-1 CELL 0.71073 13.9457 21.2120 22.2021 70.368 87.412 80.550 ZERR 4.00 0.0027 0.0042 0.0043 0.004 0.004 0.004 LATT 1 SFAC C H N Cr O UNIT 270 380 20 8 2 L.S. 10 ACTA BOND FMAP 2 PLAN 20 SIZE 0.035 0.125 0.269 TEMP -73 SIMU C115 C116 C117 C118 C119 C120 C121 C122 C123 C124 RIGU C115 C116 C117 C118 C119 C120 C121 C122 C123 C124 SIMU C125 C126 C127 C128 C129 C130 C131 SIMU O1 C132 C133 C134 C135 RIGU C125 C126 C127 C128 C129 C130 C131 RIGU O1 C132 C133 C134 C135 FLAT C125 C126 C127 C128 C129 C130 C131 SADI C125 C131 C129 C131 DFIX 1.52 0.01 C130 C131 OMIT 0 1 0 OMIT 0 0 1 OMIT 0 1 1 OMIT 0 2 1 OMIT 0 1 2 OMIT -1 1 3 OMIT 2 2 1 OMIT -1 0 1 OMIT 1 2 2 OMIT 0 -1 1 OMIT 0 1 3 OMIT 1 0 1 OMIT 1 2 0 OMIT 2 1 2 WGHT 0.050100 FVAR 0.27445 CR1 4 0.198855 0.187730 0.803232 11.00000 0.02786 0.02523 = 0.02891 -0.00822 -0.00030 -0.00449 CR2 4 0.122694 0.264941 0.739356 11.00000 0.02900 0.02799 = 0.02938 -0.00797 -0.00183 -0.00518 CR3 4 0.374193 0.243815 0.271385 11.00000 0.02516 0.02929 = 0.03102 -0.01030 -0.00069 -0.00193 CR4 4 0.329096 0.310262 0.188500 11.00000 0.02220 0.02739 = 0.02937 -0.00984 0.00049 -0.00504 N1 3 0.272240 0.229296 0.847685 11.00000 0.02446 0.02369 = 0.03085 -0.00554 -0.00309 -0.00327 N2 3 0.130805 0.343553 0.761397 11.00000 0.02880 0.02699 = 0.03296 -0.00942 -0.00107 -0.00108 N3 3 0.264985 0.127937 0.761223 11.00000 0.03422 0.02983 = 0.03000 -0.00734 -0.00047 -0.00065 N4 3 0.142494 0.241573 0.664405 11.00000 0.03767 0.03293 = 0.02866 -0.00717 -0.00499 -0.00444 N5 3 0.069757 0.204869 0.814466 11.00000 0.02396 0.03243 = 0.03386 -0.01235 -0.00121 -0.00710 N6 3 0.376615 0.157118 0.263579 11.00000 0.02973 0.02631 = 0.03267 -0.00798 -0.00086 -0.00243 N7 3 0.278813 0.258037 0.143897 11.00000 0.02601 0.03091 = 0.03250 -0.01070 0.00029 -0.00387 N8 3 0.318088 0.285156 0.330837 11.00000 0.03235 0.02951 = 0.02786 -0.00851 0.00063 -0.00190 N9 3 0.246618 0.384496 0.203507 11.00000 0.02526 0.02719 = 0.03012 -0.00852 0.00294 -0.00820 N10 3 0.457971 0.287655 0.203562 11.00000 0.02254 0.03424 = 0.03833 -0.01677 0.00071 -0.00492 C1 1 0.231422 0.288556 0.857867 11.00000 0.02784 0.02856 = 0.03591 -0.01484 -0.00055 -0.00839 AFIX 43 H1 2 0.249419 0.293708 0.896510 11.00000 -1.20000 AFIX 0 C2 1 0.168449 0.340340 0.818910 11.00000 0.03226 0.02685 = 0.03532 -0.01691 -0.00277 -0.00402 AFIX 43 H2 2 0.148211 0.378267 0.832650 11.00000 -1.20000 AFIX 0 C3 1 0.443419 0.225539 0.872361 11.00000 0.02887 0.03580 = 0.04457 -0.01525 -0.00094 -0.00431 C4 1 0.522842 0.195554 0.912882 11.00000 0.02721 0.06080 = 0.05866 -0.02729 -0.00693 -0.00672 AFIX 43 H4 2 0.580282 0.215609 0.904571 11.00000 -1.20000 AFIX 0 C5 1 0.521347 0.137338 0.965089 11.00000 0.03662 0.05941 = 0.04764 -0.01968 -0.01360 0.00555 AFIX 43 H5 2 0.577150 0.117942 0.991952 11.00000 -1.20000 AFIX 0 C6 1 0.439039 0.107718 0.977939 11.00000 0.04116 0.04350 = 0.04297 -0.00362 -0.00688 -0.00611 AFIX 43 H6 2 0.438347 0.067451 1.013528 11.00000 -1.20000 AFIX 0 C7 1 0.355734 0.136372 0.938960 11.00000 0.03433 0.03079 = 0.03342 -0.01147 -0.00666 -0.00260 C8 1 0.357958 0.196046 0.886875 11.00000 0.02831 0.03047 = 0.03259 -0.01553 -0.00440 0.00081 C9 1 0.447180 0.289448 0.815383 11.00000 0.03042 0.03965 = 0.06370 -0.01254 0.00468 -0.01040 AFIX 13 H9 2 0.385525 0.320937 0.815756 11.00000 -1.20000 AFIX 0 C10 1 0.530364 0.326960 0.818386 11.00000 0.06121 0.05809 = 0.10048 -0.01352 -0.00317 -0.02524 AFIX 137 H10A 2 0.529255 0.334699 0.859533 11.00000 -1.50000 H10B 2 0.522795 0.370609 0.783564 11.00000 -1.50000 H10C 2 0.592458 0.299661 0.813990 11.00000 -1.50000 AFIX 0 C11 1 0.448457 0.276267 0.752175 11.00000 0.08143 0.04782 = 0.06210 -0.01240 0.01504 -0.01769 AFIX 137 H11A 2 0.508098 0.245649 0.749574 11.00000 -1.50000 H11B 2 0.446251 0.319233 0.716801 11.00000 -1.50000 H11C 2 0.391845 0.255415 0.749373 11.00000 -1.50000 AFIX 0 C12 1 0.263393 0.105091 0.958970 11.00000 0.04127 0.03263 = 0.03604 -0.00641 -0.00605 -0.00277 AFIX 13 H12 2 0.217957 0.123311 0.921318 11.00000 -1.20000 AFIX 0 C13 1 0.214136 0.127771 1.012471 11.00000 0.04573 0.06914 = 0.06790 -0.03670 0.01313 -0.01054 AFIX 137 H13A 2 0.259784 0.115399 1.048388 11.00000 -1.50000 H13B 2 0.156948 0.105480 1.026747 11.00000 -1.50000 H13C 2 0.193958 0.177039 0.996728 11.00000 -1.50000 AFIX 0 C14 1 0.279987 0.028671 0.977860 11.00000 0.06652 0.03977 = 0.04901 -0.00698 0.00402 -0.01022 AFIX 137 H14A 2 0.316482 0.015060 0.944278 11.00000 -1.50000 H14B 2 0.217173 0.012513 0.983437 11.00000 -1.50000 H14C 2 0.317060 0.008905 1.018108 11.00000 -1.50000 AFIX 0 C15 1 0.000547 0.432403 0.699657 11.00000 0.03828 0.03041 = 0.02853 -0.00909 0.00316 0.00239 C16 1 -0.030358 0.500278 0.661969 11.00000 0.04342 0.04635 = 0.03513 -0.01012 -0.00034 0.00658 AFIX 43 H16 2 -0.095716 0.514082 0.646902 11.00000 -1.20000 AFIX 0 C17 1 0.032020 0.546937 0.646541 11.00000 0.05671 0.02875 = 0.03560 0.00188 -0.00002 0.00364 AFIX 43 H17 2 0.009438 0.592889 0.622147 11.00000 -1.20000 AFIX 0 C18 1 0.127267 0.526813 0.666570 11.00000 0.05605 0.02741 = 0.04428 -0.00798 0.00270 -0.00949 AFIX 43 H18 2 0.170253 0.559278 0.655456 11.00000 -1.20000 AFIX 0 C19 1 0.162370 0.460030 0.702750 11.00000 0.04393 0.03316 = 0.02688 -0.00869 0.00086 -0.00654 C20 1 0.097473 0.412346 0.720041 11.00000 0.03465 0.02547 = 0.02842 -0.00932 -0.00038 -0.00193 C21 1 -0.075057 0.386410 0.720744 11.00000 0.03339 0.04315 = 0.05103 -0.01388 0.00476 0.00275 AFIX 13 H21 2 -0.040550 0.339075 0.741092 11.00000 -1.20000 AFIX 0 C22 1 -0.137667 0.406551 0.771736 11.00000 0.07412 0.04952 = 0.08313 -0.01108 0.03569 -0.00337 AFIX 137 H22A 2 -0.095683 0.406774 0.805865 11.00000 -1.50000 H22B 2 -0.182321 0.373880 0.789653 11.00000 -1.50000 H22C 2 -0.175109 0.451902 0.752357 11.00000 -1.50000 AFIX 0 C23 1 -0.137948 0.386881 0.666343 11.00000 0.05375 0.07950 = 0.07640 -0.01258 -0.02440 -0.00966 AFIX 137 H23A 2 -0.178149 0.431517 0.648728 11.00000 -1.50000 H23B 2 -0.179998 0.352156 0.682496 11.00000 -1.50000 H23C 2 -0.096225 0.377274 0.632749 11.00000 -1.50000 AFIX 0 C24 1 0.270168 0.441650 0.722370 11.00000 0.03998 0.04343 = 0.04544 -0.00819 0.00323 -0.01524 AFIX 13 H24 2 0.284862 0.391484 0.744191 11.00000 -1.20000 AFIX 0 C25 1 0.293131 0.476327 0.769751 11.00000 0.05721 0.05570 = 0.06516 -0.02189 0.00134 -0.02036 AFIX 137 H25A 2 0.281420 0.525626 0.748825 11.00000 -1.50000 H25B 2 0.361380 0.461488 0.783402 11.00000 -1.50000 H25C 2 0.251186 0.463903 0.807138 11.00000 -1.50000 AFIX 0 C26 1 0.337221 0.460750 0.663593 11.00000 0.04653 0.05637 = 0.06476 -0.00975 0.00805 -0.01900 AFIX 137 H26A 2 0.329977 0.433349 0.636759 11.00000 -1.50000 H26B 2 0.404963 0.452079 0.678079 11.00000 -1.50000 H26C 2 0.319135 0.508902 0.638764 11.00000 -1.50000 AFIX 0 C27 1 0.261924 0.138923 0.696449 11.00000 0.04798 0.03574 = 0.03732 -0.01902 0.00234 -0.00262 AFIX 43 H27 2 0.302539 0.106931 0.681380 11.00000 -1.20000 AFIX 0 C28 1 0.207027 0.190536 0.652476 11.00000 0.05359 0.03779 = 0.03230 -0.01503 0.00076 -0.00860 AFIX 43 H28 2 0.213294 0.191947 0.609275 11.00000 -1.20000 AFIX 0 C29 1 0.251323 0.007107 0.819484 11.00000 0.07111 0.02952 = 0.04407 -0.01606 0.00050 0.00082 C30 1 0.297401 -0.058356 0.854263 11.00000 0.10695 0.03585 = 0.04667 -0.01485 -0.00188 -0.00110 AFIX 43 H30 2 0.260125 -0.094159 0.869468 11.00000 -1.20000 AFIX 0 C31 1 0.395188 -0.071371 0.866593 11.00000 0.11792 0.03794 = 0.05139 -0.02063 -0.02173 0.02446 AFIX 43 H31 2 0.424795 -0.115964 0.890633 11.00000 -1.20000 AFIX 0 C32 1 0.451174 -0.020766 0.844649 11.00000 0.08538 0.04746 = 0.05975 -0.03027 -0.02381 0.02147 AFIX 43 H32 2 0.519005 -0.031053 0.853671 11.00000 -1.20000 AFIX 0 C33 1 0.410903 0.044589 0.809829 11.00000 0.06312 0.03632 = 0.04047 -0.02415 -0.01073 0.01222 C34 1 0.309540 0.059168 0.797966 11.00000 0.05141 0.02971 = 0.03306 -0.01466 -0.00618 0.00264 C35 1 0.145018 0.018885 0.803274 11.00000 0.06833 0.03458 = 0.05148 -0.01645 0.00604 -0.01341 AFIX 13 H35 2 0.119111 0.067993 0.794497 11.00000 -1.20000 AFIX 0 C36 1 0.085966 -0.023210 0.857950 11.00000 0.10462 0.04403 = 0.06985 -0.02372 0.02285 -0.03465 AFIX 137 H36A 2 0.103127 -0.071300 0.862544 11.00000 -1.50000 H36B 2 0.016389 -0.008465 0.848137 11.00000 -1.50000 H36C 2 0.100804 -0.016650 0.897960 11.00000 -1.50000 AFIX 0 C37 1 0.130343 0.001390 0.742759 11.00000 0.07116 0.06703 = 0.06374 -0.02379 0.00550 -0.02511 AFIX 137 H37A 2 0.166421 0.028653 0.707333 11.00000 -1.50000 H37B 2 0.061011 0.011222 0.731603 11.00000 -1.50000 H37C 2 0.154254 -0.046845 0.750816 11.00000 -1.50000 AFIX 0 C38 1 0.475705 0.097192 0.783705 11.00000 0.04408 0.04963 = 0.07962 -0.02743 -0.01071 0.00861 AFIX 13 H38 2 0.436478 0.142107 0.780616 11.00000 -1.20000 AFIX 0 C39 1 0.564471 0.086543 0.826613 11.00000 0.04606 0.09032 = 0.09843 -0.06042 -0.01574 0.01117 AFIX 137 H39A 2 0.543115 0.080508 0.870583 11.00000 -1.50000 H39B 2 0.597686 0.126212 0.810943 11.00000 -1.50000 H39C 2 0.609227 0.046115 0.825679 11.00000 -1.50000 AFIX 0 C40 1 0.510386 0.101134 0.716127 11.00000 0.05893 0.11649 = 0.06673 -0.02649 -0.00157 -0.01389 AFIX 137 H40A 2 0.539645 0.055834 0.716179 11.00000 -1.50000 H40B 2 0.558769 0.131709 0.702691 11.00000 -1.50000 H40C 2 0.454887 0.118377 0.686359 11.00000 -1.50000 AFIX 0 C41 1 -0.004329 0.249006 0.603049 11.00000 0.05945 0.05627 = 0.03798 -0.00750 -0.01159 -0.01723 C42 1 -0.069465 0.286054 0.553183 11.00000 0.06555 0.09560 = 0.04571 -0.00952 -0.01865 -0.03563 AFIX 43 H42 2 -0.124371 0.267450 0.547260 11.00000 -1.20000 AFIX 0 C43 1 -0.056137 0.348678 0.512515 11.00000 0.06276 0.08065 = 0.04068 0.00547 -0.02447 -0.01010 AFIX 43 H43 2 -0.100532 0.372346 0.478084 11.00000 -1.20000 AFIX 0 C44 1 0.021528 0.377557 0.521336 11.00000 0.05689 0.05341 = 0.04473 0.00580 -0.00765 -0.01384 AFIX 43 H44 2 0.028722 0.421611 0.493490 11.00000 -1.20000 AFIX 0 C45 1 0.089505 0.343573 0.570105 11.00000 0.04509 0.03976 = 0.03237 -0.00696 -0.00123 -0.00597 C46 1 0.074372 0.278694 0.612227 11.00000 0.04794 0.03935 = 0.02551 -0.00524 -0.01129 -0.00794 C47 1 -0.020163 0.177775 0.643250 11.00000 0.08442 0.06879 = 0.04064 -0.00865 -0.01609 -0.04441 AFIX 13 H47 2 0.021899 0.162346 0.682441 11.00000 -1.20000 AFIX 0 C48 1 -0.125515 0.175486 0.663866 11.00000 0.09024 0.11429 = 0.04618 -0.00068 -0.01126 -0.06884 AFIX 137 H48A 2 -0.146824 0.210274 0.683669 11.00000 -1.50000 H48B 2 -0.130961 0.130702 0.694797 11.00000 -1.50000 H48C 2 -0.166571 0.184007 0.626400 11.00000 -1.50000 AFIX 0 C49 1 0.010521 0.129016 0.604682 11.00000 0.11147 0.07342 = 0.07205 -0.01592 -0.03175 -0.03683 AFIX 137 H49A 2 -0.020962 0.148166 0.562429 11.00000 -1.50000 H49B 2 -0.009345 0.084991 0.627566 11.00000 -1.50000 H49C 2 0.081270 0.123065 0.599669 11.00000 -1.50000 AFIX 0 C50 1 0.177759 0.373924 0.575114 11.00000 0.04655 0.03492 = 0.03559 -0.00574 0.00443 -0.00769 AFIX 13 H50 2 0.190921 0.363862 0.621584 11.00000 -1.20000 AFIX 0 C51 1 0.163299 0.451208 0.542989 11.00000 0.07223 0.04345 = 0.04157 -0.00519 -0.00212 -0.01467 AFIX 137 H51A 2 0.156332 0.462535 0.496662 11.00000 -1.50000 H51B 2 0.219747 0.468744 0.552120 11.00000 -1.50000 H51C 2 0.104585 0.471693 0.559673 11.00000 -1.50000 AFIX 0 C52 1 0.267123 0.341091 0.547662 11.00000 0.05439 0.05910 = 0.10134 -0.03466 0.03159 -0.01940 AFIX 137 H52A 2 0.280765 0.292554 0.572120 11.00000 -1.50000 H52B 2 0.323237 0.362403 0.550492 11.00000 -1.50000 H52C 2 0.254603 0.347287 0.502792 11.00000 -1.50000 AFIX 0 C53 1 -0.014335 0.191921 0.856395 11.00000 0.02413 0.03245 = 0.04409 -0.01065 0.00127 -0.01176 C54 1 -0.108387 0.204947 0.817312 11.00000 0.03489 0.04785 = 0.03835 -0.01089 -0.00190 -0.01608 AFIX 23 H54A 2 -0.119030 0.252323 0.787696 11.00000 -1.20000 H54B 2 -0.101960 0.174487 0.791471 11.00000 -1.20000 AFIX 0 C55 1 -0.195101 0.192543 0.861564 11.00000 0.02859 0.05947 = 0.05865 -0.01320 -0.00286 -0.01480 AFIX 13 H55 2 -0.255310 0.201297 0.835292 11.00000 -1.20000 AFIX 0 C56 1 -0.180072 0.119108 0.906480 11.00000 0.04139 0.05065 = 0.06569 -0.01040 0.01240 -0.02638 AFIX 23 H56A 2 -0.173523 0.087960 0.881332 11.00000 -1.20000 H56B 2 -0.236817 0.110782 0.934841 11.00000 -1.20000 AFIX 0 C57 1 -0.088062 0.106186 0.946481 11.00000 0.04298 0.04369 = 0.05415 0.00578 0.00843 -0.01732 AFIX 13 H57 2 -0.077312 0.058271 0.976260 11.00000 -1.20000 AFIX 0 C58 1 -0.000413 0.119256 0.901751 11.00000 0.03783 0.04458 = 0.04278 -0.00812 0.01408 -0.01288 AFIX 23 H58A 2 0.059450 0.110172 0.927622 11.00000 -1.20000 H58B 2 0.007500 0.087928 0.876751 11.00000 -1.20000 AFIX 0 C59 1 -0.026250 0.240160 0.895897 11.00000 0.02800 0.04375 = 0.04671 -0.01829 0.00234 -0.01054 AFIX 23 H59A 2 0.033380 0.232434 0.921633 11.00000 -1.20000 H59B 2 -0.036252 0.287795 0.866863 11.00000 -1.20000 AFIX 0 C60 1 -0.113983 0.227267 0.940327 11.00000 0.03446 0.06636 = 0.04932 -0.02605 0.01211 -0.01786 AFIX 13 H60 2 -0.121181 0.258520 0.965961 11.00000 -1.20000 AFIX 0 C61 1 -0.206687 0.240290 0.900843 11.00000 0.03063 0.06107 = 0.06077 -0.01170 0.00833 -0.00741 AFIX 23 H61A 2 -0.263103 0.232249 0.929552 11.00000 -1.20000 H61B 2 -0.218327 0.287983 0.871994 11.00000 -1.20000 AFIX 0 C62 1 -0.098820 0.155041 0.984998 11.00000 0.03732 0.07862 = 0.04772 -0.00957 0.01075 -0.01440 AFIX 23 H62A 2 -0.154912 0.147284 1.014038 11.00000 -1.20000 H62B 2 -0.039622 0.146425 1.011375 11.00000 -1.20000 AFIX 0 C63 1 0.366261 0.146367 0.205862 11.00000 0.02754 0.03352 = 0.04149 -0.01668 0.00141 -0.00286 AFIX 43 H63 2 0.391890 0.102644 0.204184 11.00000 -1.20000 AFIX 0 C64 1 0.323551 0.191847 0.152382 11.00000 0.02335 0.03585 = 0.03702 -0.01757 0.00021 -0.00663 AFIX 43 H64 2 0.323852 0.177297 0.116298 11.00000 -1.20000 AFIX 0 C65 1 0.474524 0.075357 0.355980 11.00000 0.04834 0.04077 = 0.03627 -0.01222 -0.00629 0.01236 C66 1 0.485027 0.013224 0.406372 11.00000 0.06340 0.05874 = 0.03797 -0.00741 -0.00526 0.01579 AFIX 43 H66 2 0.541870 -0.000304 0.432512 11.00000 -1.20000 AFIX 0 C67 1 0.416303 -0.028430 0.419090 11.00000 0.06798 0.04284 = 0.04805 0.00297 0.00289 0.01077 AFIX 43 H67 2 0.425235 -0.070284 0.453432 11.00000 -1.20000 AFIX 0 C68 1 0.333839 -0.008702 0.381266 11.00000 0.07332 0.03117 = 0.05553 -0.00149 0.00531 -0.00053 AFIX 43 H68 2 0.286624 -0.038094 0.389716 11.00000 -1.20000 AFIX 0 C69 1 0.317138 0.052091 0.331579 11.00000 0.04803 0.03130 = 0.04628 -0.00928 0.00775 -0.00110 C70 1 0.389235 0.094276 0.318308 11.00000 0.04228 0.03139 = 0.03712 -0.00995 -0.00055 0.00783 C71 1 0.558466 0.114996 0.341005 11.00000 0.04565 0.05212 = 0.03915 -0.00684 -0.00812 0.00707 AFIX 13 H71 2 0.537041 0.158546 0.305746 11.00000 -1.20000 AFIX 0 C72 1 0.590049 0.132276 0.397317 11.00000 0.05626 0.08879 = 0.06263 -0.03362 -0.01504 0.00204 AFIX 137 H72A 2 0.533701 0.155228 0.413973 11.00000 -1.50000 H72B 2 0.639173 0.162226 0.383363 11.00000 -1.50000 H72C 2 0.617672 0.090535 0.430986 11.00000 -1.50000 AFIX 0 C73 1 0.644565 0.075079 0.316359 11.00000 0.04691 0.08482 = 0.07127 -0.02614 -0.00028 0.01616 AFIX 137 H73A 2 0.665324 0.031244 0.349473 11.00000 -1.50000 H73B 2 0.698724 0.100962 0.306050 11.00000 -1.50000 H73C 2 0.624384 0.067654 0.277883 11.00000 -1.50000 AFIX 0 C74 1 0.222421 0.069155 0.293514 11.00000 0.04680 0.03906 = 0.05981 -0.00924 0.00617 -0.01208 AFIX 13 H74 2 0.217640 0.117011 0.263934 11.00000 -1.20000 AFIX 0 C75 1 0.132530 0.064891 0.336531 11.00000 0.05581 0.06213 = 0.07305 -0.01209 0.01132 -0.01508 AFIX 137 H75A 2 0.136951 0.019068 0.367746 11.00000 -1.50000 H75B 2 0.073751 0.075162 0.310193 11.00000 -1.50000 H75C 2 0.129581 0.097724 0.359081 11.00000 -1.50000 AFIX 0 C76 1 0.221299 0.023740 0.252240 11.00000 0.06748 0.04388 = 0.08821 -0.02060 -0.00585 -0.01755 AFIX 137 H76A 2 0.276718 0.028600 0.223190 11.00000 -1.50000 H76B 2 0.160673 0.037340 0.227259 11.00000 -1.50000 H76C 2 0.225791 -0.023645 0.279983 11.00000 -1.50000 AFIX 0 C77 1 0.233328 0.335860 0.034738 11.00000 0.03246 0.03057 = 0.03728 -0.01763 0.00527 -0.00270 C78 1 0.167961 0.357273 -0.017179 11.00000 0.04182 0.03721 = 0.03230 -0.01186 -0.00150 0.00214 AFIX 43 H78 2 0.181025 0.392303 -0.055027 11.00000 -1.20000 AFIX 0 C79 1 0.085801 0.328828 -0.014519 11.00000 0.03669 0.04102 = 0.04477 -0.02356 -0.01577 0.00553 AFIX 43 H79 2 0.043907 0.342415 -0.050740 11.00000 -1.20000 AFIX 0 C80 1 0.064856 0.280262 0.041426 11.00000 0.03012 0.04244 = 0.04957 -0.01954 -0.00439 -0.00220 AFIX 43 H80 2 0.006933 0.261561 0.043336 11.00000 -1.20000 AFIX 0 C81 1 0.125082 0.257406 0.095352 11.00000 0.02874 0.03481 = 0.04101 -0.01512 -0.00323 -0.00292 C82 1 0.211403 0.284950 0.090766 11.00000 0.02492 0.03102 = 0.03227 -0.01542 -0.00516 -0.00021 C83 1 0.328594 0.362958 0.025718 11.00000 0.04261 0.04534 = 0.02913 -0.01119 0.00050 -0.01162 AFIX 13 H83 2 0.355705 0.353962 0.069278 11.00000 -1.20000 AFIX 0 C84 1 0.317866 0.439128 -0.009005 11.00000 0.06199 0.05420 = 0.04922 -0.00919 0.00550 -0.02434 AFIX 137 H84A 2 0.303176 0.448970 -0.054301 11.00000 -1.50000 H84B 2 0.378654 0.455038 -0.005091 11.00000 -1.50000 H84C 2 0.264866 0.462371 0.010042 11.00000 -1.50000 AFIX 0 C85 1 0.401044 0.324296 -0.007754 11.00000 0.03902 0.07872 = 0.06063 -0.03682 0.01022 -0.01591 AFIX 137 H85A 2 0.410291 0.275853 0.017257 11.00000 -1.50000 H85B 2 0.463367 0.340905 -0.011622 11.00000 -1.50000 H85C 2 0.376135 0.331228 -0.050455 11.00000 -1.50000 AFIX 0 C86 1 0.098306 0.205755 0.156478 11.00000 0.02807 0.03982 = 0.04432 -0.01291 0.00122 -0.00542 AFIX 13 H86 2 0.158698 0.172519 0.172995 11.00000 -1.20000 AFIX 0 C87 1 0.065581 0.237203 0.208131 11.00000 0.05268 0.05039 = 0.04523 -0.01334 0.01101 -0.01719 AFIX 137 H87A 2 0.116652 0.260431 0.215728 11.00000 -1.50000 H87B 2 0.053244 0.201470 0.247801 11.00000 -1.50000 H87C 2 0.005860 0.269875 0.193989 11.00000 -1.50000 AFIX 0 C88 1 0.021398 0.165011 0.147995 11.00000 0.04839 0.06169 = 0.06579 -0.01870 0.00638 -0.02977 AFIX 137 H88A 2 -0.040413 0.195408 0.134345 11.00000 -1.50000 H88B 2 0.012586 0.129614 0.188717 11.00000 -1.50000 H88C 2 0.043009 0.144046 0.115516 11.00000 -1.50000 AFIX 0 C89 1 0.246502 0.341820 0.320324 11.00000 0.04130 0.03248 = 0.03107 -0.00850 0.00767 -0.00190 AFIX 43 H89 2 0.216857 0.349745 0.357040 11.00000 -1.20000 AFIX 0 C90 1 0.215485 0.386220 0.263316 11.00000 0.03025 0.02801 = 0.03768 -0.01065 0.00624 -0.00110 AFIX 43 H90 2 0.166737 0.423020 0.263817 11.00000 -1.20000 AFIX 0 C91 1 0.429231 0.289702 0.411668 11.00000 0.04727 0.04637 = 0.03799 -0.01802 -0.00220 0.00151 C92 1 0.469814 0.262081 0.473672 11.00000 0.05034 0.07048 = 0.04115 -0.02658 -0.01069 0.00007 AFIX 43 H92 2 0.518605 0.282500 0.485171 11.00000 -1.20000 AFIX 0 C93 1 0.440354 0.206521 0.517557 11.00000 0.07755 0.05190 = 0.03733 -0.01664 -0.01400 0.01513 AFIX 43 H93 2 0.469243 0.188113 0.559019 11.00000 -1.20000 AFIX 0 C94 1 0.368297 0.176958 0.501632 11.00000 0.07590 0.03953 = 0.03264 -0.01002 0.00184 0.00473 AFIX 43 H94 2 0.348355 0.138317 0.532696 11.00000 -1.20000 AFIX 0 C95 1 0.324059 0.202319 0.441185 11.00000 0.04921 0.04288 = 0.03562 -0.01732 0.00443 0.00226 C96 1 0.358420 0.258504 0.395309 11.00000 0.03775 0.03495 = 0.03103 -0.01185 -0.00140 0.00210 C97 1 0.461437 0.353650 0.367219 11.00000 0.05343 0.06261 = 0.04233 -0.02511 0.00403 -0.02293 AFIX 13 H97 2 0.439212 0.360731 0.322894 11.00000 -1.20000 AFIX 0 C98 1 0.412953 0.414520 0.386571 11.00000 0.09290 0.05753 = 0.05316 -0.02002 0.00397 -0.02619 AFIX 137 H98A 2 0.342134 0.418510 0.383943 11.00000 -1.50000 H98B 2 0.433699 0.456070 0.357589 11.00000 -1.50000 H98C 2 0.432154 0.407737 0.430502 11.00000 -1.50000 AFIX 0 C99 1 0.572212 0.351197 0.366496 11.00000 0.07093 0.10781 = 0.06665 -0.04260 0.00823 -0.04287 AFIX 137 H99A 2 0.593915 0.352222 0.407481 11.00000 -1.50000 H99B 2 0.589332 0.390423 0.331812 11.00000 -1.50000 H99C 2 0.604035 0.309383 0.359735 11.00000 -1.50000 AFIX 0 C100 1 0.240112 0.171721 0.427535 11.00000 0.06246 0.04491 = 0.03533 -0.00735 0.00745 -0.01250 AFIX 13 H100 2 0.244966 0.172066 0.382353 11.00000 -1.20000 AFIX 0 C101 1 0.142958 0.215320 0.434956 11.00000 0.05115 0.06644 = 0.08563 -0.00589 0.00648 -0.01203 AFIX 137 H10G 2 0.139802 0.218880 0.477905 11.00000 -1.50000 H10H 2 0.088686 0.194018 0.428692 11.00000 -1.50000 H10I 2 0.138787 0.260707 0.402976 11.00000 -1.50000 AFIX 0 C102 1 0.239128 0.098968 0.471612 11.00000 0.09084 0.04809 = 0.06151 -0.00744 0.01642 -0.02452 AFIX 137 H10D 2 0.303013 0.071787 0.471197 11.00000 -1.50000 H10E 2 0.189483 0.079723 0.456679 11.00000 -1.50000 H10F 2 0.224258 0.098689 0.515257 11.00000 -1.50000 AFIX 0 C103 1 0.285916 0.496131 0.132458 11.00000 0.03521 0.03513 = 0.03606 -0.01224 0.00619 -0.00300 C104 1 0.255274 0.558080 0.085363 11.00000 0.05386 0.03296 = 0.04325 -0.00512 0.00858 -0.01152 AFIX 43 H104 2 0.299215 0.589773 0.071090 11.00000 -1.20000 AFIX 0 C105 1 0.163208 0.574997 0.058714 11.00000 0.06573 0.02884 = 0.03989 0.00341 0.00271 0.00024 AFIX 43 H105 2 0.144240 0.617654 0.026573 11.00000 -1.20000 AFIX 0 C106 1 0.099516 0.529633 0.079105 11.00000 0.04046 0.04339 = 0.03932 -0.00793 -0.00399 0.00394 AFIX 43 H106 2 0.036055 0.541419 0.060798 11.00000 -1.20000 AFIX 0 C107 1 0.125201 0.466703 0.125935 11.00000 0.03417 0.03081 = 0.03505 -0.01236 0.00129 -0.00274 C108 1 0.219013 0.449389 0.152505 11.00000 0.02915 0.02888 = 0.02655 -0.00657 0.00467 -0.00680 C109 1 0.386550 0.481227 0.161968 11.00000 0.03131 0.03102 = 0.05590 -0.01090 0.00229 -0.01156 AFIX 13 H109 2 0.409097 0.431254 0.174583 11.00000 -1.20000 AFIX 0 C110 1 0.384196 0.500546 0.221651 11.00000 0.04337 0.05574 = 0.06351 -0.00873 -0.00473 -0.01972 AFIX 137 H11G 2 0.361150 0.549285 0.210719 11.00000 -1.50000 H11H 2 0.449740 0.489604 0.240280 11.00000 -1.50000 H11I 2 0.340172 0.475282 0.252677 11.00000 -1.50000 AFIX 0 C111 1 0.461008 0.516802 0.115789 11.00000 0.04289 0.04921 = 0.08081 -0.01801 0.02114 -0.02401 AFIX 137 H11J 2 0.445687 0.565780 0.107405 11.00000 -1.50000 H11K 2 0.458818 0.507550 0.075538 11.00000 -1.50000 H11L 2 0.526221 0.499868 0.134842 11.00000 -1.50000 AFIX 0 C112 1 0.048408 0.420621 0.147421 11.00000 0.03073 0.04159 = 0.04342 -0.01295 -0.00422 0.00077 AFIX 13 H112 2 0.082303 0.373753 0.170544 11.00000 -1.20000 AFIX 0 C113 1 -0.022777 0.442619 0.193917 11.00000 0.06256 0.14904 = 0.06870 -0.05797 0.02489 -0.05279 AFIX 137 H11M 2 0.012455 0.438809 0.232506 11.00000 -1.50000 H11N 2 -0.072965 0.413359 0.205556 11.00000 -1.50000 H11O 2 -0.053349 0.489757 0.173427 11.00000 -1.50000 AFIX 0 C114 1 -0.008495 0.417758 0.091853 11.00000 0.03760 0.05785 = 0.04929 -0.02796 -0.00884 -0.00209 AFIX 137 H11D 2 -0.050663 0.461298 0.072633 11.00000 -1.50000 H11E 2 -0.048348 0.381621 0.107398 11.00000 -1.50000 H11F 2 0.036836 0.408509 0.059699 11.00000 -1.50000 AFIX 0 C115 1 0.611884 0.317286 0.224061 11.00000 0.03661 0.10613 = 0.08911 -0.04097 -0.00136 -0.01912 AFIX 23 H11T 2 0.615353 0.282963 0.267397 11.00000 -1.20000 H11U 2 0.576787 0.360632 0.227078 11.00000 -1.20000 AFIX 0 C116 1 0.715187 0.326524 0.199841 11.00000 0.04234 0.10258 = 0.13658 -0.05048 0.00331 -0.02044 AFIX 13 H116 2 0.749652 0.342224 0.229385 11.00000 -1.20000 AFIX 0 C117 1 0.765996 0.261737 0.199018 11.00000 0.04300 0.09254 = 0.13566 -0.03482 0.02912 -0.01693 AFIX 23 H11R 2 0.767305 0.228486 0.242823 11.00000 -1.20000 H11S 2 0.834071 0.266284 0.186059 11.00000 -1.20000 AFIX 0 C118 1 0.719468 0.234564 0.153504 11.00000 0.05441 0.06325 = 0.15207 -0.05055 0.05351 -0.02284 AFIX 13 H118 2 0.756728 0.190490 0.152354 11.00000 -1.20000 AFIX 0 C119 1 0.609291 0.228270 0.176244 11.00000 0.05911 0.06184 = 0.15138 -0.04871 0.05414 -0.01850 AFIX 23 H11P 2 0.575246 0.214173 0.145885 11.00000 -1.20000 H11Q 2 0.609347 0.193047 0.218917 11.00000 -1.20000 AFIX 0 C120 1 0.556091 0.294739 0.179448 11.00000 0.02203 0.04214 = 0.04983 -0.01935 0.00818 -0.01114 C121 1 0.713687 0.375912 0.134611 11.00000 0.04609 0.09304 = 0.14433 -0.02906 0.02375 -0.02637 AFIX 23 H12E 2 0.683779 0.421262 0.135507 11.00000 -1.20000 H12F 2 0.781295 0.378579 0.119567 11.00000 -1.20000 AFIX 0 C122 1 0.659405 0.357722 0.089637 11.00000 0.04181 0.08953 = 0.08563 -0.01344 0.02976 -0.01237 AFIX 13 H122 2 0.656909 0.393448 0.046481 11.00000 -1.20000 AFIX 0 C123 1 0.555292 0.348782 0.114056 11.00000 0.03334 0.09201 = 0.06327 -0.01198 0.01359 -0.01292 AFIX 23 H12A 2 0.520349 0.392418 0.116480 11.00000 -1.20000 H12B 2 0.519853 0.336080 0.083324 11.00000 -1.20000 AFIX 0 C124 1 0.707932 0.290045 0.085438 11.00000 0.07788 0.12571 = 0.13533 -0.06079 0.06699 -0.03868 AFIX 23 H12C 2 0.772741 0.294619 0.065866 11.00000 -1.20000 H12D 2 0.668401 0.275934 0.057743 11.00000 -1.20000 AFIX 66 C125 1 0.895575 0.164713 0.380992 11.00000 0.08202 0.20526 = 0.14361 -0.05436 0.01801 -0.04235 AFIX 43 H12G 2 0.933972 0.168191 0.343906 11.00000 -1.20000 AFIX 65 C126 1 0.881020 0.101398 0.422347 11.00000 0.08478 0.26334 = 0.14553 -0.03371 0.00190 -0.07540 AFIX 43 H12H 2 0.909469 0.061601 0.413524 11.00000 -1.20000 AFIX 65 C127 1 0.824839 0.096310 0.476610 11.00000 0.13565 0.28775 = 0.14882 -0.04788 -0.00779 -0.09463 AFIX 43 H12I 2 0.814892 0.053037 0.504874 11.00000 -1.20000 AFIX 65 C128 1 0.783213 0.154538 0.489519 11.00000 0.15186 0.29577 = 0.14477 -0.07085 -0.04136 -0.06805 AFIX 43 H12J 2 0.744816 0.151061 0.526606 11.00000 -1.20000 AFIX 65 C129 1 0.797768 0.217854 0.448165 11.00000 0.11230 0.27233 = 0.12333 -0.09611 -0.04284 -0.05394 AFIX 43 H12K 2 0.769318 0.257650 0.456988 11.00000 -1.20000 AFIX 65 C130 1 0.853948 0.222943 0.393901 11.00000 0.10636 0.23674 = 0.13769 -0.06056 -0.04736 -0.04142 AFIX 0 C131 1 0.871808 0.288918 0.354619 11.00000 0.24363 0.24427 = 0.23827 -0.02922 -0.07188 -0.07655 AFIX 33 H13D 2 0.912283 0.285057 0.318390 11.00000 -1.50000 H13E 2 0.905533 0.308696 0.379940 11.00000 -1.50000 H13F 2 0.809817 0.318093 0.338679 11.00000 -1.50000 AFIX 6 O1 5 0.655720 0.327696 0.536452 11.00000 0.17614 0.15928 = 0.13354 -0.07321 0.04208 -0.06783 C132 1 0.674675 0.396497 0.509604 11.00000 0.19386 0.16201 = 0.12448 -0.05236 0.03763 -0.09090 AFIX 23 H13G 2 0.661715 0.414166 0.462943 11.00000 -1.20000 H13H 2 0.743311 0.398608 0.517173 11.00000 -1.20000 AFIX 5 C133 1 0.606177 0.438172 0.543295 11.00000 0.31798 0.17328 = 0.18528 -0.07654 0.06395 -0.04027 AFIX 23 H13I 2 0.542130 0.455062 0.521369 11.00000 -1.20000 H13J 2 0.634624 0.476974 0.545942 11.00000 -1.20000 AFIX 5 C134 1 0.598030 0.385274 0.609842 11.00000 0.24665 0.22094 = 0.16969 -0.09703 0.07635 -0.09152 AFIX 23 H13K 2 0.654427 0.380373 0.637491 11.00000 -1.20000 H13L 2 0.537333 0.397013 0.631324 11.00000 -1.20000 AFIX 5 C135 1 0.597194 0.320911 0.592907 11.00000 0.22279 0.20669 = 0.10169 -0.06433 0.04857 -0.10810 AFIX 23 H13M 2 0.624853 0.280202 0.628568 11.00000 -1.20000 H13N 2 0.529919 0.316667 0.584319 11.00000 -1.20000 AFIX 0 HKLF 4 REM klat946 in P-1 REM R1 = 0.0918 for 13347 Fo > 4sig(Fo) and 0.2006 for all 30190 data REM 1362 parameters refined using 315 restraints END WGHT 0.0664 0.0000 REM Highest difference peak 0.748, deepest hole -0.574, 1-sigma level 0.079 Q1 1 0.6824 0.2384 0.1066 11.00000 0.05 0.75 Q2 1 0.6608 0.4274 0.5608 11.00000 0.05 0.74 Q3 1 0.5454 0.3967 0.5714 11.00000 0.05 0.71 Q4 1 0.8582 0.1305 0.4353 11.00000 0.05 0.62 Q5 1 0.6129 0.4278 0.5162 11.00000 0.05 0.62 Q6 1 0.1605 0.2281 0.7723 11.00000 0.05 0.58 Q7 1 0.7754 0.2173 0.4606 11.00000 0.05 0.56 Q8 1 0.8194 0.2722 0.4145 11.00000 0.05 0.56 Q9 1 0.3614 0.2929 0.2324 11.00000 0.05 0.56 Q10 1 0.3318 0.2677 0.2255 11.00000 0.05 0.52 Q11 1 0.6314 0.3306 0.6087 11.00000 0.05 0.51 Q12 1 0.6584 0.3110 0.0414 11.00000 0.05 0.50 Q13 1 0.8970 0.0407 0.4388 11.00000 0.05 0.50 Q14 1 0.8579 0.0585 0.4321 11.00000 0.05 0.46 Q15 1 0.5552 0.2382 0.1334 11.00000 0.05 0.46 Q16 1 0.5450 0.3088 0.1092 11.00000 0.05 0.46 Q17 1 0.6440 0.2736 0.2186 11.00000 0.05 0.42 Q18 1 0.2411 0.1401 0.7954 11.00000 0.05 0.40 Q19 1 0.5767 0.3522 0.5295 11.00000 0.05 0.39 Q20 1 0.5298 0.4038 0.5257 11.00000 0.05 0.39 ; _shelx_res_checksum 39160 _shelx_hkl_file ; 1 0 0 0.12 1.64 -1 0 0 0.66 1.52 -2 0 0 322.54 19.06 2 0 0 353.96 20.21 -2 0 0 364.88 20.77 3 0 0 5.74 9.07 -3 0 0 2.66 8.09 -3 0 0 -1.94 7.98 4 0 0 639.42 37.97 -4 0 0 665.84 38.31 -4 0 0 690.47 38.54 -5 0 0 -0.77 7.07 -5 0 0 1.51 7.63 5 0 0 -2.65 7.99 6 0 0 -7.97 7.85 -6 0 0 1.40 8.77 -6 0 0 13.69 10.45 7 0 0 18.29 15.07 -7 0 0 40.25 16.30 -7 0 0 19.04 12.92 8 0 0 181.10 32.33 -8 0 0 168.22 30.24 -8 0 0 146.59 29.15 -9 0 0 530.61 49.51 9 0 0 436.19 48.93 -9 0 0 426.13 44.39 10 0 0 -14.52 7.94 -10 0 0 -6.71 8.53 -10 0 0 -4.00 7.81 11 0 0 46.42 22.59 -11 0 0 56.20 23.32 -11 0 0 39.86 16.86 -12 0 0 99.80 30.84 12 0 0 98.71 31.37 -12 0 0 86.64 27.53 13 0 0 -4.65 9.53 -13 0 0 -14.13 8.00 -13 0 0 3.18 13.98 14 0 0 -3.49 10.96 -14 0 0 0.07 11.40 -14 0 0 -10.17 8.94 -15 0 0 31.14 18.56 -15 0 0 25.97 12.18 15 0 0 45.68 20.37 -16 0 0 4.25 14.67 -16 0 0 32.61 12.67 16 0 0 35.38 14.73 17 0 0 39.20 18.87 -17 0 0 16.30 15.02 17 0 0 51.32 17.39 18 0 0 -0.89 13.15 18 0 0 3.31 14.40 -18 0 0 12.47 15.31 -18 1 0 37.45 25.22 18 -1 0 49.64 15.46 18 -1 0 24.33 16.63 -17 1 0 8.79 13.70 -17 1 0 3.95 11.85 17 -1 0 20.41 12.12 -16 1 0 74.98 27.96 16 -1 0 36.29 17.04 -16 1 0 79.76 25.55 15 -1 0 46.12 19.36 -15 1 0 25.87 22.21 -15 1 0 63.90 23.48 14 -1 0 -8.64 9.41 -14 1 0 1.96 12.83 -14 1 0 -11.85 8.59 13 -1 0 77.58 29.15 -13 1 0 40.83 22.63 -13 1 0 65.07 23.70 -12 1 0 -2.19 9.73 12 -1 0 9.06 13.35 -12 1 0 -6.25 6.95 -11 1 0 9.56 11.89 11 -1 0 0.70 10.56 -11 1 0 0.91 10.45 -10 1 0 46.98 18.96 10 -1 0 58.44 22.02 -10 1 0 44.35 20.44 9 -1 0 51.49 21.53 -9 1 0 42.00 18.92 -9 1 0 68.63 24.05 -8 1 0 186.21 32.99 -8 1 0 145.91 28.77 8 -1 0 175.87 32.29 7 -1 0 54.19 19.03 -7 1 0 65.44 19.88 -7 1 0 84.68 21.88 -6 1 0 1.90 9.05 -6 1 0 3.75 8.12 6 -1 0 3.30 9.78 5 -1 0 55.09 16.03 -5 1 0 42.46 15.39 -5 1 0 57.02 15.72 -4 1 0 216.22 24.16 -4 1 0 137.46 18.90 4 -1 0 193.14 22.30 -3 1 0 836.65 41.02 3 -1 0 899.59 40.75 -3 1 0 892.93 38.85 -2 1 0 217.59 16.09 -2 1 0 200.68 17.24 2 -1 0 230.28 10.02 2 -1 0 219.93 17.39 2 -1 0 232.53 9.76 1 -1 0 3136.33 68.10 1 -1 0 2810.31 65.36 1 -1 0 2864.50 66.20 -1 1 0 3102.97 65.72 -1 1 0 3403.82 69.89 0 -1 0 -8.76 0.60 0 1 0 -9.21 0.61 0 -1 0 -5.31 1.73 0 -1 0 -7.62 1.14 0 1 0 -9.55 0.43 0 1 0 -8.92 0.39 1 1 0 8739.85 183.52 1 1 0 9998.09 190.77 2 1 0 185.41 10.08 -2 -1 0 166.50 9.12 -2 -1 0 161.88 12.72 2 1 0 173.60 14.77 -3 -1 0 211.81 19.56 3 1 0 212.22 21.66 -3 -1 0 204.54 12.00 -4 -1 0 -4.50 7.45 -4 -1 0 -0.36 3.36 4 1 0 -5.82 7.35 -5 -1 0 239.87 24.94 5 1 0 178.05 24.52 -5 -1 0 194.66 25.57 -6 -1 0 166.08 26.49 6 1 0 154.71 26.41 -6 -1 0 192.65 26.79 -7 -1 0 55.91 18.80 -7 -1 0 56.33 18.94 7 1 0 72.85 23.10 -8 -1 0 397.48 40.35 -8 -1 0 383.81 38.59 8 1 0 440.38 44.68 -9 -1 0 29.80 16.66 -9 -1 0 21.01 13.72 9 1 0 55.21 21.94 -10 -1 0 2.71 9.31 -10 -1 0 10.19 12.63 10 1 0 4.31 12.56 -11 -1 0 12.05 11.77 11 1 0 33.83 17.66 -11 -1 0 3.61 9.69 -12 -1 0 -11.79 10.60 12 1 0 -12.68 7.76 -12 -1 0 -1.57 7.99 13 1 0 -4.50 12.88 -13 -1 0 23.85 12.12 -13 -1 0 1.28 13.01 14 1 0 22.38 13.91 -14 -1 0 27.54 23.42 -14 -1 0 37.58 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1.44 8.50 -2 11 -3 2.73 9.20 2 -11 3 1.15 11.11 3 -11 3 50.82 20.28 -3 11 -3 34.18 17.89 -3 11 -3 64.12 22.10 -4 11 -3 73.33 22.87 4 -11 3 68.20 21.42 -4 11 -3 94.54 29.06 -5 11 -3 6.76 11.30 -5 11 -3 8.57 11.59 5 -11 3 1.93 8.91 6 -11 3 1.66 9.73 -6 11 -3 14.97 15.53 6 -11 3 0.53 10.82 7 -11 3 -4.39 7.87 -7 11 -3 15.68 16.28 7 -11 3 8.01 13.28 -8 11 -3 93.48 31.35 8 -11 3 68.93 27.45 8 -11 3 28.49 12.67 9 -11 3 209.44 47.36 -9 11 -3 220.96 50.01 -10 11 -3 52.99 24.65 10 -11 3 62.68 23.84 11 -11 3 5.21 13.15 -11 11 -3 15.64 21.70 -12 11 -3 14.64 16.24 12 -11 3 21.72 12.33 13 -11 3 69.86 24.14 -13 11 -3 24.51 17.03 -14 11 -3 -11.31 14.03 14 -11 3 -3.27 12.61 -15 11 -3 -2.83 15.27 15 -11 3 30.18 14.08 17 10 -3 -5.48 13.99 -17 -10 3 -6.76 13.49 16 10 -3 91.37 29.08 -16 -10 3 50.82 19.48 -15 -10 3 39.46 12.65 15 10 -3 34.57 12.51 -14 -10 3 45.97 14.90 14 10 -3 63.69 20.95 -13 -10 3 -0.47 9.66 13 10 -3 31.73 15.19 -12 -10 3 18.91 12.64 12 10 -3 8.97 11.96 -11 -10 3 100.97 30.28 11 10 -3 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21.20 -5 10 -3 20.24 7.05 -5 10 -3 21.72 15.34 -5 10 -3 26.80 16.66 5 -10 3 28.00 15.07 -6 10 -3 207.60 24.20 6 -10 3 159.69 35.38 -6 10 -3 153.77 37.08 6 -10 3 191.53 31.45 7 -10 3 13.23 10.34 -7 10 -3 10.13 15.77 7 -10 3 14.22 12.51 8 -10 3 -8.72 6.56 8 -10 3 -7.24 8.37 -8 10 -3 -17.21 10.04 -9 10 -3 28.98 21.68 9 -10 3 8.97 11.85 -10 10 -3 42.32 26.07 10 -10 3 21.81 15.44 -11 10 -3 13.49 15.34 11 -10 3 3.27 11.14 -12 10 -3 17.16 19.03 12 -10 3 6.94 13.78 -13 10 -3 3.31 20.67 13 -10 3 5.82 10.39 14 -10 3 -11.02 12.06 -14 10 -3 -6.86 12.39 -15 10 -3 29.91 14.28 15 -10 3 11.20 14.55 -17 -9 3 -28.90 12.85 17 9 -3 -8.85 13.05 -16 -9 3 -2.09 14.58 16 9 -3 24.56 12.38 -15 -9 3 50.84 19.34 15 9 -3 0.38 11.09 14 9 -3 1.17 10.08 -14 -9 3 30.86 14.67 13 9 -3 -14.26 8.86 -13 -9 3 -0.62 9.69 12 9 -3 17.24 9.80 -12 -9 3 20.15 15.10 12 9 -3 -11.85 8.45 11 9 -3 -3.06 8.09 11 9 -3 10.27 13.63 -11 -9 3 -4.92 9.49 -10 -9 3 168.17 28.69 10 9 -3 175.12 29.81 -10 -9 3 109.84 31.46 10 9 -3 165.71 38.51 9 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46.48 15.39 -15 -11 4 -3.09 11.53 -14 -11 4 -13.95 10.15 14 11 -4 8.60 9.93 13 11 -4 42.21 18.40 -13 -11 4 32.39 15.96 -12 -11 4 31.02 18.23 12 11 -4 67.87 23.47 -11 -11 4 -0.34 8.48 11 11 -4 -3.28 10.10 -11 -11 4 21.07 14.46 -10 -11 4 13.45 10.66 -10 -11 4 25.60 15.73 10 11 -4 17.27 12.63 -9 -11 4 6.26 12.84 9 11 -4 39.21 14.55 9 11 -4 17.53 14.27 -9 -11 4 37.70 18.62 -8 -11 4 186.46 34.81 -8 -11 4 184.94 36.02 8 11 -4 185.07 27.11 8 11 -4 147.05 34.08 7 11 -4 141.59 33.75 7 11 -4 106.00 20.38 -7 -11 4 136.33 30.92 6 11 -4 94.48 19.33 6 11 -4 105.55 29.01 -6 -11 4 91.02 26.05 -5 -11 4 275.67 41.68 5 11 -4 220.11 27.03 5 11 -4 217.58 38.89 -4 -11 4 62.57 22.14 4 11 -4 42.79 12.95 4 11 -4 78.09 25.26 -3 -11 4 22.51 13.91 3 11 -4 18.83 9.52 3 11 -4 14.85 12.98 2 11 -4 -1.56 8.00 2 11 -4 5.86 7.75 -2 -11 4 8.99 11.63 -1 -11 4 610.83 54.34 1 11 -4 588.55 52.68 1 11 -4 560.65 42.55 0 -11 4 39.95 20.00 0 11 -4 43.55 19.40 0 11 -4 54.20 18.07 1 -11 4 27.69 16.22 -1 11 -4 24.34 16.43 -1 11 -4 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9.13 1 13 -5 5.17 8.75 -1 -13 5 8.89 11.41 0 -13 5 5.80 11.95 0 13 -5 11.57 10.69 0 13 -5 0.35 10.29 -1 13 -5 176.15 32.94 -1 13 -5 205.74 39.82 1 -13 5 257.52 45.06 2 -13 5 -14.49 7.45 -2 13 -5 1.19 11.88 -2 13 -5 -2.20 9.30 -3 13 -5 -1.91 10.49 -3 13 -5 -0.03 6.90 3 -13 5 6.51 10.03 -4 13 -5 12.09 14.59 -4 13 -5 14.53 12.10 4 -13 5 -6.12 8.08 -5 13 -5 4.86 14.60 -5 13 -5 6.97 12.96 5 -13 5 21.05 10.88 6 -13 5 132.98 30.72 6 -13 5 161.83 42.62 -6 13 -5 78.81 30.53 -7 13 -5 153.87 41.01 7 -13 5 148.56 42.38 7 -13 5 94.06 24.84 -8 13 -5 -5.02 9.83 8 -13 5 16.79 10.38 8 -13 5 3.35 8.17 -9 13 -5 -12.86 13.33 9 -13 5 20.02 12.63 10 -13 5 -2.95 10.66 -10 13 -5 10.86 14.89 11 -13 5 26.48 12.85 -11 13 -5 32.97 18.38 12 -13 5 -14.61 12.71 -12 13 -5 8.24 14.30 13 -13 5 54.83 16.43 -13 13 -5 33.95 20.59 -16 -12 5 17.80 13.38 16 12 -5 54.27 13.80 15 12 -5 -4.96 11.58 -15 -12 5 14.02 12.84 -14 -12 5 26.66 12.07 14 12 -5 -1.29 10.20 -13 -12 5 37.26 14.09 13 12 -5 8.19 11.84 12 12 -5 16.96 12.29 -12 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-28 -19.95 13.95 -5 7 28 -10.39 15.00 5 -7 -28 43.34 14.04 -5 7 28 13.89 13.91 -4 7 28 68.11 19.67 4 -7 -28 40.20 18.43 3 -7 -28 52.15 18.07 -3 7 28 25.26 22.22 -2 7 28 -11.83 12.65 2 -7 -28 6.71 17.05 -1 7 28 -3.53 13.72 1 -7 -28 34.16 13.80 0 7 28 37.08 16.53 0 -7 -28 -3.43 12.19 1 7 28 39.00 15.40 -1 -7 -28 -13.05 14.47 -2 -7 -28 35.56 16.01 2 7 28 22.93 12.97 3 7 28 26.64 13.06 -3 -7 -28 24.13 12.83 -4 -7 -28 6.16 12.64 4 7 28 6.96 13.24 5 7 28 -20.40 13.67 -5 -7 -28 -4.28 13.19 -6 -7 -28 46.69 14.21 -5 8 28 4.40 13.88 -5 8 28 5.10 14.99 5 -8 -28 7.85 13.60 -4 8 28 -14.59 13.98 4 -8 -28 -8.67 13.52 3 -8 -28 2.10 13.23 -3 8 28 13.73 13.97 2 -8 -28 -2.71 12.36 -2 8 28 -15.89 13.07 -1 8 28 1.10 12.96 1 -8 -28 12.31 12.78 0 8 28 12.67 14.80 0 -8 -28 6.39 13.53 1 8 28 64.49 19.76 -1 -8 -28 56.64 17.19 2 8 28 -12.29 12.71 -2 -8 -28 -14.35 12.94 3 8 28 35.13 13.57 -3 -8 -28 35.19 13.92 4 8 28 118.29 38.78 -4 -8 -28 0.08 13.06 -5 -8 -28 0.44 13.16 5 8 28 -25.17 13.33 -6 -8 -28 34.71 13.87 6 8 28 -7.88 14.25 -5 9 28 20.05 15.03 -5 9 28 6.50 14.22 5 -9 -28 -17.63 13.77 4 -9 -28 49.72 14.58 -4 9 28 23.12 15.00 3 -9 -28 -4.72 13.14 -3 9 28 12.85 13.74 2 -9 -28 18.04 13.21 -2 9 28 -0.12 13.17 1 -9 -28 -8.89 12.43 -1 9 28 -1.75 13.14 0 -9 -28 23.32 13.66 0 9 28 47.52 18.20 1 9 28 11.53 12.94 -1 -9 -28 -11.09 12.36 2 9 28 47.89 18.41 -2 -9 -28 83.72 18.00 3 9 28 14.45 13.08 -3 -9 -28 24.93 13.23 -4 -9 -28 6.84 13.13 4 9 28 22.03 15.02 -5 -9 -28 13.53 13.52 5 9 28 20.63 13.56 6 9 28 -2.03 14.31 -6 -9 -28 -7.81 13.93 5 -10 -28 -0.96 13.69 -4 10 28 20.88 14.29 4 -10 -28 -7.68 13.24 -3 10 28 14.26 14.19 3 -10 -28 -4.17 13.31 2 -10 -28 25.57 12.75 -2 10 28 32.12 16.01 1 -10 -28 -8.00 12.47 -1 10 28 -7.02 12.73 0 10 28 3.03 13.63 0 -10 -28 -5.45 12.45 1 10 28 22.94 14.01 -1 -10 -28 29.22 14.07 2 10 28 -7.74 13.12 -2 -10 -28 25.14 12.95 3 10 28 -10.92 13.15 -3 -10 -28 -9.05 12.74 -4 -10 -28 10.57 13.01 4 10 28 11.18 13.74 -5 -10 -28 50.59 15.06 5 10 28 7.53 14.17 6 10 28 28.38 14.45 4 -11 -28 -16.55 13.35 -4 11 28 42.90 25.58 -3 11 28 38.01 13.86 3 -11 -28 -14.21 12.82 -2 11 28 -5.85 13.55 2 -11 -28 23.04 14.23 1 -11 -28 2.85 12.42 -1 11 28 8.57 13.76 0 -11 -28 21.51 13.99 0 11 28 37.30 17.48 -1 -11 -28 -15.49 12.74 1 11 28 -0.34 15.16 -2 -11 -28 2.04 12.30 2 11 28 -11.18 14.83 -3 -11 -28 -1.65 12.97 3 11 28 9.90 13.42 4 11 28 18.19 16.12 -4 -11 -28 20.29 13.44 5 11 28 9.96 14.37 6 11 28 31.65 14.75 -4 12 28 24.02 14.28 4 -12 -28 8.78 13.65 -3 12 28 -11.15 14.22 3 -12 -28 -3.75 12.74 2 -12 -28 69.93 22.84 -2 12 28 -0.56 15.77 1 -12 -28 -19.40 12.62 -1 12 28 -8.59 13.62 0 12 28 -7.74 13.61 0 -12 -28 -1.97 12.50 -1 -12 -28 23.80 12.77 1 12 28 3.79 15.53 2 12 28 -2.69 13.80 -2 -12 -28 41.52 13.19 -3 -12 -28 -15.32 13.12 3 12 28 -1.34 13.98 4 12 28 50.13 15.67 5 12 28 29.28 15.67 6 12 28 6.16 14.71 4 -13 -28 -11.42 14.02 3 -13 -28 40.24 13.67 -3 13 28 27.51 15.10 -2 13 28 4.84 14.26 2 -13 -28 -5.52 13.31 -1 13 28 -21.50 13.87 1 -13 -28 28.50 13.66 0 13 28 21.73 13.87 0 -13 -28 1.47 12.47 1 13 28 -0.07 13.93 -1 -13 -28 -20.74 12.64 -2 -13 -28 26.45 13.15 2 13 28 30.15 15.79 3 13 28 7.47 13.97 4 13 28 -1.70 14.72 5 13 28 1.57 15.23 6 13 28 4.46 15.40 3 -14 -28 9.84 13.37 -3 14 28 7.43 14.42 -2 14 28 7.69 14.78 2 -14 -28 25.87 13.61 1 -14 -28 -9.13 13.34 -1 14 28 12.09 14.35 0 -14 -28 20.99 12.90 0 14 28 -13.32 17.23 1 14 28 23.98 15.00 2 14 28 19.88 15.03 3 14 28 -17.52 14.87 4 14 28 -21.16 14.52 5 14 28 4.89 14.94 6 14 28 11.31 15.48 -2 15 28 7.52 15.23 2 -15 -28 -3.73 13.46 1 -15 -28 7.54 13.61 -1 15 28 -13.79 14.80 0 15 28 -17.51 15.05 1 15 28 27.08 16.60 2 15 28 15.58 15.15 3 15 28 20.75 15.66 4 15 28 15.45 15.45 5 15 28 -14.09 15.73 -1 16 28 -13.01 15.93 0 16 28 -24.57 15.81 1 16 28 11.24 15.92 2 16 28 80.87 18.29 3 16 28 19.15 15.98 4 16 28 3.95 16.50 0 17 28 17.58 16.06 1 17 28 67.43 24.58 2 17 28 0.13 16.12 3 17 28 44.34 16.47 0 -4 -29 -17.57 14.34 -1 5 29 4.78 14.33 1 -5 -29 20.66 14.03 0 5 29 -9.42 13.94 0 -5 -29 15.31 13.97 1 5 29 22.77 15.12 -1 -5 -29 18.70 14.48 -2 -5 -29 -2.65 13.93 2 5 29 -15.68 14.26 -2 6 29 15.57 14.31 2 -6 -29 -26.47 14.04 1 -6 -29 39.02 13.99 -1 6 29 -3.28 14.69 0 6 29 -6.76 13.87 0 -6 -29 12.70 13.75 1 6 29 -25.80 13.94 -1 -6 -29 15.48 13.99 -2 -6 -29 2.84 14.16 2 6 29 7.09 14.17 3 6 29 53.32 14.74 -3 -6 -29 -4.25 14.05 2 -7 -29 -3.84 14.39 -2 7 29 18.05 15.66 1 -7 -29 4.16 13.60 -1 7 29 12.65 14.66 0 -7 -29 10.60 13.35 0 7 29 14.59 13.81 1 7 29 2.95 13.52 -1 -7 -29 29.15 13.55 -2 -7 -29 34.64 13.84 2 7 29 9.04 14.13 -3 -7 -29 -6.89 13.88 3 7 29 5.53 13.95 2 -8 -29 9.58 13.46 -2 8 29 0.97 13.87 1 -8 -29 79.00 30.02 -1 8 29 43.55 13.70 0 -8 -29 5.37 14.05 0 8 29 23.60 13.58 1 8 29 19.59 13.75 -1 -8 -29 25.74 13.30 -2 -8 -29 9.66 13.79 2 8 29 -15.13 13.51 -3 -8 -29 24.29 13.48 3 8 29 15.92 13.98 -4 -8 -29 2.19 14.00 4 8 29 -7.95 14.26 -2 9 29 63.03 14.43 2 -9 -29 22.28 13.42 1 -9 -29 -19.46 13.52 -1 9 29 23.40 16.33 0 -9 -29 16.51 13.11 0 9 29 21.40 13.57 1 9 29 69.18 15.77 -1 -9 -29 7.49 13.34 -2 -9 -29 18.01 13.66 2 9 29 0.56 13.64 3 9 29 -14.64 13.74 -3 -9 -29 30.56 14.71 -4 -9 -29 2.96 13.76 4 9 29 27.85 14.23 2 -10 -29 24.35 13.61 -2 10 29 27.57 14.16 -1 10 29 -5.48 14.26 1 -10 -29 25.71 13.64 0 10 29 33.33 16.57 0 -10 -29 16.66 13.92 -1 -10 -29 12.36 14.44 1 10 29 8.99 14.40 2 10 29 -23.88 14.33 -2 -10 -29 18.51 14.66 -3 -10 -29 68.82 14.12 3 10 29 26.91 14.13 -4 -10 -29 55.00 16.39 -2 11 29 -18.75 14.87 2 -11 -29 40.04 17.26 1 -11 -29 -1.74 13.38 -1 11 29 1.85 15.01 0 -11 -29 -13.77 13.78 0 11 29 8.02 14.72 -1 -11 -29 25.19 14.43 1 11 29 -19.88 14.47 -2 -11 -29 42.41 13.56 2 11 29 42.38 15.59 -3 -11 -29 11.24 14.00 3 11 29 8.39 14.79 -4 -11 -29 37.43 14.27 4 11 29 26.56 15.21 2 -12 -29 -2.27 14.07 -1 12 29 17.91 14.74 1 -12 -29 6.73 13.47 0 12 29 -25.24 14.42 0 -12 -29 4.79 13.44 -1 -12 -29 6.46 13.91 1 12 29 34.96 16.59 2 12 29 -3.40 14.52 -2 -12 -29 -10.69 13.32 3 12 29 74.58 17.49 -3 -12 -29 37.58 14.02 4 12 29 -2.03 15.29 -1 13 29 4.55 15.15 1 -13 -29 22.03 14.04 0 -13 -29 8.69 13.65 0 13 29 5.71 15.07 1 13 29 9.52 14.82 -1 -13 -29 -5.20 13.60 2 13 29 10.59 15.08 3 13 29 4.91 15.05 0 -14 -29 -9.32 13.82 0 14 29 25.18 16.82 1 14 29 -4.48 15.47 2 14 29 17.93 17.13 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 22398 _database_code_depnum_ccdc_archive 'CCDC 971181' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_klat854s-sr # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.166 0.771 0.500 8 1 ' ' 2 0.233 0.215 0.639 11 1 ' ' 3 0.500 1.000 0.000 352 119 2(diethylether) 4 0.767 0.785 0.361 11 1 ' ' 5 0.833 0.229 0.500 8 1 ' ' _platon_squeeze_details ; Void space analysis consistent with initial solutions showing one severely disordered diethylether solvent molecule in the asymmetric unit (i.e. two in the unit cell) near an inversion center. PLATON Reference : Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13. Spek, A.L. (2009). Acta Cryst. D65, 148-155. ; # start Validation Reply Form _vrf_CHEMW03_klat854s-sr ; PROBLEM: WARNING: The ratio of given/expected molecular weight as RESPONSE: see _platon_squeeze_details ; _vrf_PLAT026_klat854s-sr ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 29 % RESPONSE: This compound consistently yielded weakly diffracting crystals. The data herewith represents the best of several trials. ; # end Validation Reply Form _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H102 Cr2 N4 O3' _chemical_formula_weight 1295.67 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -z' _cell_length_a 12.257(4) _cell_length_b 13.447(4) _cell_length_c 22.146(7) _cell_angle_alpha 90.757(6) _cell_angle_beta 100.752(5) _cell_angle_gamma 97.594(6) _cell_volume 3551.9(18) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 628 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 14.17 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_F_000 1388 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.293 _exptl_crystal_size_mid 0.231 _exptl_crystal_size_min 0.117 _exptl_absorpt_coefficient_mu 0.357 _shelx_estimated_absorpt_T_min 0.903 _shelx_estimated_absorpt_T_max 0.959 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.671 _exptl_absorpt_correction_T_max 0.959 _exptl_absorpt_process_details 'APEX2 (Bruker, 2007)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 48405 _diffrn_reflns_av_unetI/netI 0.3188 _diffrn_reflns_av_R_equivalents 0.1652 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.762 _diffrn_reflns_theta_max 28.368 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 17665 _reflns_number_gt 5165 _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 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ? ; _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^)+(0.0029P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 17665 _refine_ls_number_parameters 791 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2342 _refine_ls_R_factor_gt 0.0831 _refine_ls_wR_factor_ref 0.1248 _refine_ls_wR_factor_gt 0.1067 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _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 Cr1 Cr -0.00102(7) 0.30856(6) 0.22758(4) 0.0346(2) Uani 1 1 d . . . . . Cr2 Cr 0.24489(7) 0.37086(6) 0.30354(4) 0.0334(2) Uani 1 1 d . . . . . N1 N -0.0942(3) 0.1920(3) 0.17601(18) 0.0370(11) Uani 1 1 d . . . . . N2 N -0.1433(3) 0.3702(3) 0.19844(18) 0.0317(11) Uani 1 1 d . . . . . N3 N 0.3760(3) 0.4768(3) 0.30487(18) 0.0329(11) Uani 1 1 d . . . . . N4 N 0.3542(3) 0.3221(3) 0.37293(19) 0.0396(12) Uani 1 1 d . . . . . O1 O 0.1318(3) 0.2495(2) 0.27569(15) 0.0375(9) Uani 1 1 d . . . . . O2 O 0.1141(2) 0.4292(2) 0.25540(15) 0.0357(9) Uani 1 1 d . . . . . C1 C -0.1911(4) 0.2177(4) 0.1459(2) 0.0413(15) Uani 1 1 d . . . . . H1 H -0.2397 0.1727 0.1162 0.050 Uiso 1 1 calc R U . . . C2 C -0.2184(4) 0.3092(4) 0.1585(2) 0.0393(15) Uani 1 1 d . . . . . H2 H -0.2880 0.3290 0.1397 0.047 Uiso 1 1 calc R U . . . C3 C -0.1303(4) 0.0080(4) 0.1797(3) 0.0433(15) Uani 1 1 d . . . . . C4 C -0.1124(5) -0.0849(4) 0.1594(3) 0.0591(18) Uani 1 1 d . . . . . H4 H -0.1522 -0.1437 0.1725 0.071 Uiso 1 1 calc R U . . . C5 C -0.0389(5) -0.0943(4) 0.1210(3) 0.066(2) Uani 1 1 d . . . . . H5 H -0.0270 -0.1590 0.1082 0.079 Uiso 1 1 calc R U . . . C6 C 0.0185(5) -0.0094(4) 0.1006(3) 0.0539(17) Uani 1 1 d . . . . . H6 H 0.0690 -0.0166 0.0736 0.065 Uiso 1 1 calc R U . . . C7 C 0.0033(4) 0.0860(4) 0.1190(2) 0.0387(14) Uani 1 1 d . . . . . C8 C -0.0716(4) 0.0933(4) 0.1594(2) 0.0359(14) Uani 1 1 d . . . . . C9 C -0.2153(5) 0.0145(4) 0.2219(3) 0.0572(18) Uani 1 1 d . . . . . H9 H -0.2035 0.0846 0.2400 0.069 Uiso 1 1 calc R U . . . C10 C -0.3370(4) -0.0070(5) 0.1847(3) 0.087(2) Uani 1 1 d . . . . . H10A H -0.3451 0.0362 0.1493 0.131 Uiso 1 1 calc R U . . . H10B H -0.3896 0.0069 0.2111 0.131 Uiso 1 1 calc R U . . . H10C H -0.3531 -0.0775 0.1703 0.131 Uiso 1 1 calc R U . . . C11 C -0.2017(5) -0.0566(4) 0.2743(3) 0.0645(19) Uani 1 1 d . . . . . H11A H -0.2223 -0.1260 0.2579 0.097 Uiso 1 1 calc R U . . . H11B H -0.2506 -0.0430 0.3028 0.097 Uiso 1 1 calc R U . . . H11C H -0.1235 -0.0470 0.2960 0.097 Uiso 1 1 calc R U . . . C12 C 0.0640(4) 0.1784(4) 0.0957(3) 0.0505(16) Uani 1 1 d . . . . . H12 H 0.0871 0.2289 0.1308 0.061 Uiso 1 1 calc R U . . . C13 C -0.0120(5) 0.2248(4) 0.0451(3) 0.072(2) Uani 1 1 d . . . . . H13A H -0.0406 0.1753 0.0111 0.109 Uiso 1 1 calc R U . . . H13B H 0.0304 0.2833 0.0303 0.109 Uiso 1 1 calc R U . . . H13C H -0.0750 0.2457 0.0613 0.109 Uiso 1 1 calc R U . . . C14 C 0.1690(4) 0.1627(4) 0.0715(3) 0.073(2) Uani 1 1 d . . . . . H14A H 0.2195 0.1313 0.1029 0.110 Uiso 1 1 calc R U . . . H14B H 0.2070 0.2276 0.0618 0.110 Uiso 1 1 calc R U . . . H14C H 0.1483 0.1189 0.0343 0.110 Uiso 1 1 calc R U . . . C15 C -0.2152(4) 0.5319(4) 0.1762(3) 0.0346(14) Uani 1 1 d . . . . . C16 C -0.2611(4) 0.6122(4) 0.1973(3) 0.0445(15) Uani 1 1 d . . . . . H16 H -0.2844 0.6620 0.1696 0.053 Uiso 1 1 calc R U . . . C17 C -0.2735(4) 0.6206(4) 0.2582(3) 0.0475(16) Uani 1 1 d . . . . . H17 H -0.3036 0.6766 0.2716 0.057 Uiso 1 1 calc R U . . . C18 C -0.2430(4) 0.5495(4) 0.2988(2) 0.0415(15) Uani 1 1 d . . . . . H18 H -0.2520 0.5566 0.3403 0.050 Uiso 1 1 calc R U . . . C19 C -0.1990(4) 0.4670(4) 0.2803(2) 0.0339(13) Uani 1 1 d . . . . . C20 C -0.1842(4) 0.4585(4) 0.2184(2) 0.0318(13) Uani 1 1 d . . . . . C21 C -0.2045(4) 0.5283(4) 0.1098(2) 0.0394(14) Uani 1 1 d . . . . . H21 H -0.1589 0.4737 0.1041 0.047 Uiso 1 1 calc R U . . . C22 C -0.3194(4) 0.5024(4) 0.0670(2) 0.0582(18) Uani 1 1 d . . . . . H22A H -0.3551 0.4365 0.0767 0.087 Uiso 1 1 calc R U . . . H22B H -0.3093 0.5008 0.0241 0.087 Uiso 1 1 calc R U . . . H22C H -0.3671 0.5534 0.0728 0.087 Uiso 1 1 calc R U . . . C23 C -0.1444(4) 0.6261(4) 0.0904(2) 0.0533(17) Uani 1 1 d . . . . . H23A H -0.1868 0.6813 0.0962 0.080 Uiso 1 1 calc R U . . . H23B H -0.1391 0.6196 0.0469 0.080 Uiso 1 1 calc R U . . . H23C H -0.0690 0.6401 0.1155 0.080 Uiso 1 1 calc R U . . . C24 C -0.1753(4) 0.3832(4) 0.3234(2) 0.0411(15) Uani 1 1 d . . . . . H24 H -0.1017 0.3633 0.3182 0.049 Uiso 1 1 calc R U . . . C25 C -0.2648(4) 0.2890(4) 0.3064(2) 0.0508(16) Uani 1 1 d . . . . . H25A H -0.3390 0.3066 0.3087 0.076 Uiso 1 1 calc R U . . . H25B H -0.2471 0.2361 0.3352 0.076 Uiso 1 1 calc R U . . . H25C H -0.2647 0.2647 0.2645 0.076 Uiso 1 1 calc R U . . . C26 C -0.1656(4) 0.4107(4) 0.3913(2) 0.0591(18) Uani 1 1 d . . . . . H26A H -0.1097 0.4702 0.4027 0.089 Uiso 1 1 calc R U . . . H26B H -0.1426 0.3545 0.4160 0.089 Uiso 1 1 calc R U . . . H26C H -0.2384 0.4250 0.3988 0.089 Uiso 1 1 calc R U . . . C27 C 0.4658(4) 0.4596(4) 0.3456(2) 0.0399(15) Uani 1 1 d . . . . . H27 H 0.5356 0.5015 0.3490 0.048 Uiso 1 1 calc R U . . . C28 C 0.4537(4) 0.3796(4) 0.3821(2) 0.0431(15) Uani 1 1 d . . . . . H28 H 0.5139 0.3653 0.4131 0.052 Uiso 1 1 calc R U . . . C29 C 0.4091(4) 0.5400(4) 0.2057(3) 0.0397(15) Uani 1 1 d . . . . . C30 C 0.4362(4) 0.6212(4) 0.1699(3) 0.0479(16) Uani 1 1 d . . . . . H30 H 0.4438 0.6094 0.1286 0.057 Uiso 1 1 calc R U . . . C31 C 0.4519(4) 0.7185(4) 0.1941(3) 0.0559(18) Uani 1 1 d . . . . . H31 H 0.4722 0.7729 0.1696 0.067 Uiso 1 1 calc R U . . . C32 C 0.4382(4) 0.7371(4) 0.2540(3) 0.0537(17) Uani 1 1 d . . . . . H32 H 0.4479 0.8044 0.2697 0.064 Uiso 1 1 calc R U . . . C33 C 0.4107(4) 0.6589(4) 0.2911(3) 0.0399(15) Uani 1 1 d . . . . . C34 C 0.3980(4) 0.5603(4) 0.2664(2) 0.0338(14) Uani 1 1 d . . . . . C35 C 0.3967(4) 0.4348(4) 0.1794(2) 0.0421(15) Uani 1 1 d . . . . . H35 H 0.3316 0.3960 0.1937 0.051 Uiso 1 1 calc R U . . . C36 C 0.3722(4) 0.4266(4) 0.1102(2) 0.0622(18) Uani 1 1 d . . . . . H36A H 0.3121 0.4662 0.0944 0.093 Uiso 1 1 calc R U . . . H36B H 0.3485 0.3561 0.0967 0.093 Uiso 1 1 calc R U . . . H36C H 0.4398 0.4521 0.0946 0.093 Uiso 1 1 calc R U . . . C37 C 0.5001(4) 0.3843(4) 0.2046(2) 0.0536(17) Uani 1 1 d . . . . . H37A H 0.5674 0.4253 0.1962 0.080 Uiso 1 1 calc R U . . . H37B H 0.4924 0.3176 0.1847 0.080 Uiso 1 1 calc R U . . . H37C H 0.5065 0.3778 0.2491 0.080 Uiso 1 1 calc R U . . . C38 C 0.4001(4) 0.6835(4) 0.3558(3) 0.0490(16) Uani 1 1 d . . . . . H38 H 0.3642 0.6214 0.3726 0.059 Uiso 1 1 calc R U . . . C39 C 0.3267(5) 0.7670(4) 0.3606(3) 0.0656(19) Uani 1 1 d . . . . . H39A H 0.3584 0.8281 0.3430 0.098 Uiso 1 1 calc R U . . . H39B H 0.3247 0.7808 0.4039 0.098 Uiso 1 1 calc R U . . . H39C H 0.2504 0.7451 0.3380 0.098 Uiso 1 1 calc R U . . . C40 C 0.5142(5) 0.7148(5) 0.3970(3) 0.094(2) Uani 1 1 d . . . . . H40A H 0.5612 0.6615 0.3958 0.141 Uiso 1 1 calc R U . . . H40B H 0.5044 0.7264 0.4393 0.141 Uiso 1 1 calc R U . . . H40C H 0.5505 0.7767 0.3822 0.141 Uiso 1 1 calc R U . . . C41 C 0.2594(4) 0.2606(4) 0.4564(2) 0.0395(14) Uani 1 1 d . . . . . C42 C 0.2393(4) 0.1880(4) 0.4989(2) 0.0501(17) Uani 1 1 d . . . . . H42 H 0.1868 0.1956 0.5246 0.060 Uiso 1 1 calc R U . . . C43 C 0.2957(5) 0.1053(4) 0.5036(3) 0.0562(18) Uani 1 1 d . . . . . H43 H 0.2798 0.0551 0.5317 0.067 Uiso 1 1 calc R U . . . C44 C 0.3734(5) 0.0950(4) 0.4685(3) 0.0527(17) Uani 1 1 d . . . . . H44 H 0.4128 0.0386 0.4739 0.063 Uiso 1 1 calc R U . . . C45 C 0.3979(4) 0.1646(4) 0.4244(2) 0.0366(14) Uani 1 1 d . . . . . C46 C 0.3359(4) 0.2471(4) 0.4179(2) 0.0367(14) Uani 1 1 d . . . . . C47 C 0.2047(4) 0.3557(4) 0.4537(3) 0.0490(16) Uani 1 1 d . . . . . H47 H 0.1795 0.3688 0.4093 0.059 Uiso 1 1 calc R U . . . C48 C 0.1037(4) 0.3514(4) 0.4836(3) 0.068(2) Uani 1 1 d . . . . . H48A H 0.0539 0.2885 0.4707 0.102 Uiso 1 1 calc R U . . . H48B H 0.0637 0.4084 0.4710 0.102 Uiso 1 1 calc R U . . . H48C H 0.1278 0.3544 0.5284 0.102 Uiso 1 1 calc R U . . . C49 C 0.2891(4) 0.4465(4) 0.4821(3) 0.0613(18) Uani 1 1 d . . . . . H49A H 0.3142 0.4370 0.5260 0.092 Uiso 1 1 calc R U . . . H49B H 0.2533 0.5076 0.4767 0.092 Uiso 1 1 calc R U . . . H49C H 0.3538 0.4529 0.4615 0.092 Uiso 1 1 calc R U . . . C50 C 0.4892(4) 0.1487(4) 0.3898(3) 0.0478(16) Uani 1 1 d . . . . . H50 H 0.4870 0.1975 0.3560 0.057 Uiso 1 1 calc R U . . . C51 C 0.4778(5) 0.0444(4) 0.3612(3) 0.071(2) Uani 1 1 d . . . . . H51A H 0.4934 -0.0035 0.3936 0.106 Uiso 1 1 calc R U . . . H51B H 0.5312 0.0431 0.3334 0.106 Uiso 1 1 calc R U . . . H51C H 0.4013 0.0258 0.3379 0.106 Uiso 1 1 calc R U . . . C52 C 0.6047(4) 0.1711(4) 0.4326(3) 0.0603(18) Uani 1 1 d . . . . . H52A H 0.6200 0.2427 0.4446 0.090 Uiso 1 1 calc R U . . . H52B H 0.6627 0.1533 0.4111 0.090 Uiso 1 1 calc R U . . . H52C H 0.6048 0.1315 0.4695 0.090 Uiso 1 1 calc R U . . . C53 C 0.1405(4) 0.1524(4) 0.2885(2) 0.0375(14) Uani 1 1 d . . . . . C54 C -0.0055(4) 0.1529(4) 0.3521(3) 0.0451(16) Uani 1 1 d . . . . . H54 H -0.0251 0.2131 0.3336 0.054 Uiso 1 1 calc R U . . . C55 C -0.0631(5) 0.1128(4) 0.3956(3) 0.0576(18) Uani 1 1 d . . . . . H55 H -0.1228 0.1444 0.4055 0.069 Uiso 1 1 calc R U . . . C56 C -0.0358(5) 0.0280(4) 0.4250(3) 0.0572(17) Uani 1 1 d . . . . . H56 H -0.0763 -0.0003 0.4547 0.069 Uiso 1 1 calc R U . . . C57 C 0.0523(5) -0.0151(4) 0.4101(3) 0.0589(18) Uani 1 1 d . . . . . H57 H 0.0739 -0.0727 0.4310 0.071 Uiso 1 1 calc R U . . . C58 C 0.1098(4) 0.0233(4) 0.3658(3) 0.0453(16) Uani 1 1 d . . . . . H58 H 0.1698 -0.0087 0.3568 0.054 Uiso 1 1 calc R U . . . C59 C 0.0818(4) 0.1082(4) 0.3337(3) 0.0406(15) Uani 1 1 d . . . . . C60 C 0.1897(4) -0.0028(4) 0.2446(3) 0.0499(17) Uani 1 1 d . . . . . H60 H 0.1269 -0.0408 0.2567 0.060 Uiso 1 1 calc R U . . . C61 C 0.2588(5) -0.0512(4) 0.2146(3) 0.0576(18) Uani 1 1 d . . . . . H61 H 0.2422 -0.1216 0.2060 0.069 Uiso 1 1 calc R U . . . C62 C 0.3502(5) 0.0012(5) 0.1974(3) 0.0570(18) Uani 1 1 d . . . . . H62 H 0.3984 -0.0327 0.1779 0.068 Uiso 1 1 calc R U . . . C63 C 0.3723(5) 0.1037(4) 0.2083(3) 0.0572(18) Uani 1 1 d . . . . . H63 H 0.4353 0.1407 0.1958 0.069 Uiso 1 1 calc R U . . . C64 C 0.3032(4) 0.1525(4) 0.2371(2) 0.0443(15) Uani 1 1 d . . . . . H64 H 0.3190 0.2234 0.2436 0.053 Uiso 1 1 calc R U . . . C65 C 0.2106(4) 0.1012(4) 0.2573(2) 0.0399(15) Uani 1 1 d . . . . . C66 C 0.1041(4) 0.5257(4) 0.2407(2) 0.0322(13) Uani 1 1 d . . . . . C67 C 0.0933(4) 0.4869(4) 0.1298(3) 0.0451(15) Uani 1 1 d . . . . . H67 H 0.0678 0.4186 0.1360 0.054 Uiso 1 1 calc R U . . . C68 C 0.1053(4) 0.5157(5) 0.0715(3) 0.0547(17) Uani 1 1 d . . . . . H68 H 0.0858 0.4675 0.0382 0.066 Uiso 1 1 calc R U . . . C69 C 0.1453(5) 0.6135(5) 0.0609(3) 0.0585(18) Uani 1 1 d . . . . . H69 H 0.1544 0.6331 0.0209 0.070 Uiso 1 1 calc R U . . . C70 C 0.1718(4) 0.6819(5) 0.1103(3) 0.0553(18) Uani 1 1 d . . . . . H70 H 0.2000 0.7493 0.1037 0.066 Uiso 1 1 calc R U . . . C71 C 0.1590(4) 0.6558(4) 0.1687(3) 0.0474(16) Uani 1 1 d . . . . . H71 H 0.1780 0.7053 0.2013 0.057 Uiso 1 1 calc R U . . . C72 C 0.1181(4) 0.5568(4) 0.1807(3) 0.0371(14) Uani 1 1 d . . . . . C73 C 0.0954(4) 0.5642(4) 0.3489(3) 0.0501(16) Uani 1 1 d . . . . . H73 H 0.1240 0.5032 0.3597 0.060 Uiso 1 1 calc R U . . . C74 C 0.0706(5) 0.6247(4) 0.3951(3) 0.0585(18) Uani 1 1 d . . . . . H74 H 0.0836 0.6055 0.4367 0.070 Uiso 1 1 calc R U . . . C75 C 0.0272(5) 0.7126(4) 0.3796(3) 0.065(2) Uani 1 1 d . . . . . H75 H 0.0116 0.7548 0.4107 0.078 Uiso 1 1 calc R U . . . C76 C 0.0065(5) 0.7391(4) 0.3196(3) 0.0577(18) Uani 1 1 d . . . . . H76 H -0.0255 0.7987 0.3094 0.069 Uiso 1 1 calc R U . . . C77 C 0.0314(4) 0.6805(4) 0.2735(3) 0.0498(17) Uani 1 1 d . . . . . H77 H 0.0164 0.7003 0.2320 0.060 Uiso 1 1 calc R U . . . C78 C 0.0793(4) 0.5908(4) 0.2876(3) 0.0376(14) 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 Cr1 0.0315(5) 0.0286(6) 0.0433(6) 0.0020(4) 0.0047(5) 0.0060(4) Cr2 0.0310(5) 0.0285(6) 0.0397(6) 0.0031(4) 0.0038(5) 0.0042(4) N1 0.031(3) 0.033(3) 0.043(3) 0.002(2) -0.003(2) 0.005(2) N2 0.028(2) 0.025(3) 0.042(3) -0.003(2) 0.006(2) 0.006(2) N3 0.024(2) 0.036(3) 0.036(3) 0.010(2) 0.002(2) 0.001(2) N4 0.032(3) 0.035(3) 0.049(3) 0.006(2) 0.000(2) 0.003(2) O1 0.036(2) 0.019(2) 0.052(3) 0.0093(18) -0.0076(18) 0.0058(18) O2 0.029(2) 0.027(2) 0.048(2) 0.0042(18) -0.0018(18) 0.0048(17) C1 0.039(4) 0.033(4) 0.046(4) -0.008(3) -0.008(3) 0.007(3) C2 0.031(3) 0.038(4) 0.045(4) -0.006(3) -0.005(3) 0.006(3) C3 0.039(4) 0.026(4) 0.063(4) -0.006(3) 0.007(3) 0.005(3) C4 0.055(4) 0.040(4) 0.087(5) 0.002(4) 0.028(4) 0.004(3) C5 0.070(5) 0.030(4) 0.098(6) -0.012(4) 0.019(4) 0.008(4) C6 0.057(4) 0.046(4) 0.061(5) -0.012(3) 0.016(3) 0.009(4) C7 0.040(4) 0.033(4) 0.040(4) -0.008(3) 0.000(3) 0.005(3) C8 0.032(3) 0.026(3) 0.047(4) -0.006(3) 0.000(3) 0.008(3) C9 0.051(4) 0.038(4) 0.081(5) 0.007(4) 0.013(4) 0.001(3) C10 0.043(4) 0.103(6) 0.109(6) 0.015(5) 0.011(4) -0.008(4) C11 0.065(5) 0.047(4) 0.081(5) 0.015(4) 0.011(4) 0.008(4) C12 0.049(4) 0.039(4) 0.062(5) -0.003(3) 0.012(4) 0.002(3) C13 0.086(5) 0.081(5) 0.058(5) 0.020(4) 0.027(4) 0.019(4) C14 0.047(4) 0.079(5) 0.094(6) -0.001(4) 0.018(4) 0.006(4) C15 0.024(3) 0.028(3) 0.053(4) 0.003(3) 0.010(3) 0.003(3) C16 0.042(4) 0.050(4) 0.043(4) 0.005(3) 0.009(3) 0.008(3) C17 0.045(4) 0.031(4) 0.069(5) 0.001(3) 0.011(4) 0.015(3) C18 0.039(4) 0.049(4) 0.040(4) -0.006(3) 0.016(3) 0.007(3) C19 0.029(3) 0.031(3) 0.043(4) 0.000(3) 0.009(3) 0.003(3) C20 0.024(3) 0.030(3) 0.041(4) -0.005(3) 0.003(3) 0.007(3) C21 0.041(4) 0.043(4) 0.035(4) 0.002(3) 0.004(3) 0.010(3) C22 0.045(4) 0.067(5) 0.056(4) 0.008(3) -0.004(3) 0.002(3) C23 0.046(4) 0.053(4) 0.066(5) 0.027(3) 0.018(3) 0.012(3) C24 0.043(4) 0.046(4) 0.038(4) 0.008(3) 0.012(3) 0.014(3) C25 0.044(4) 0.047(4) 0.061(4) 0.008(3) 0.013(3) -0.001(3) C26 0.066(4) 0.065(5) 0.049(4) 0.008(3) 0.012(4) 0.018(4) C27 0.032(3) 0.039(4) 0.043(4) 0.009(3) -0.002(3) -0.005(3) C28 0.029(3) 0.049(4) 0.046(4) 0.014(3) -0.004(3) 0.004(3) C29 0.029(3) 0.044(4) 0.048(4) 0.017(3) 0.002(3) 0.014(3) C30 0.039(4) 0.053(4) 0.052(4) 0.013(4) 0.004(3) 0.013(3) C31 0.044(4) 0.047(5) 0.078(5) 0.038(4) 0.014(4) 0.006(3) C32 0.042(4) 0.042(4) 0.071(5) 0.018(4) -0.006(4) 0.003(3) C33 0.035(3) 0.036(4) 0.046(4) 0.009(3) 0.001(3) 0.005(3) C34 0.028(3) 0.028(3) 0.040(4) 0.003(3) -0.005(3) 0.001(3) C35 0.036(3) 0.045(4) 0.047(4) 0.005(3) 0.012(3) 0.007(3) C36 0.044(4) 0.092(5) 0.051(5) -0.002(4) 0.006(3) 0.013(4) C37 0.049(4) 0.045(4) 0.068(5) 0.006(3) 0.010(3) 0.014(3) C38 0.049(4) 0.040(4) 0.050(4) 0.005(3) -0.006(3) -0.003(3) C39 0.073(5) 0.044(4) 0.079(5) -0.008(4) 0.012(4) 0.009(4) C40 0.097(6) 0.095(6) 0.079(6) -0.014(4) -0.017(5) 0.023(5) C41 0.034(3) 0.037(4) 0.045(4) 0.001(3) -0.001(3) 0.007(3) C42 0.041(4) 0.066(5) 0.046(4) 0.021(3) 0.014(3) 0.008(3) C43 0.053(4) 0.061(5) 0.056(5) 0.038(4) 0.017(4) 0.002(4) C44 0.050(4) 0.048(4) 0.064(5) 0.019(3) 0.015(4) 0.013(3) C45 0.031(3) 0.035(4) 0.037(4) 0.010(3) -0.006(3) -0.001(3) C46 0.031(3) 0.038(4) 0.040(4) 0.009(3) -0.001(3) 0.011(3) C47 0.054(4) 0.050(4) 0.047(4) 0.004(3) 0.014(3) 0.016(3) C48 0.049(4) 0.090(5) 0.072(5) -0.004(4) 0.025(4) 0.015(4) C49 0.061(4) 0.047(4) 0.074(5) -0.011(3) 0.003(4) 0.015(4) C50 0.037(4) 0.048(4) 0.064(5) 0.015(3) 0.014(3) 0.018(3) C51 0.093(5) 0.051(5) 0.076(5) 0.000(4) 0.019(4) 0.034(4) C52 0.034(4) 0.061(4) 0.087(5) 0.025(4) 0.010(4) 0.009(3) C53 0.030(3) 0.043(4) 0.039(4) 0.004(3) 0.006(3) 0.002(3) C54 0.038(4) 0.032(4) 0.068(5) 0.013(3) 0.012(3) 0.008(3) C55 0.045(4) 0.057(5) 0.073(5) 0.016(4) 0.013(4) 0.013(4) C56 0.053(4) 0.052(5) 0.066(5) 0.014(4) 0.014(4) -0.002(4) C57 0.053(4) 0.055(5) 0.067(5) 0.011(4) 0.004(4) 0.010(4) C58 0.045(4) 0.036(4) 0.055(4) 0.015(3) 0.014(3) -0.001(3) C59 0.034(3) 0.037(4) 0.049(4) 0.000(3) 0.005(3) 0.001(3) C60 0.049(4) 0.041(4) 0.067(5) 0.007(3) 0.021(3) 0.014(3) C61 0.060(4) 0.027(4) 0.086(5) -0.009(3) 0.015(4) 0.005(3) C62 0.058(4) 0.057(5) 0.061(5) -0.004(4) 0.016(4) 0.019(4) C63 0.061(4) 0.035(4) 0.085(5) -0.002(3) 0.036(4) 0.008(3) C64 0.043(4) 0.039(4) 0.055(4) 0.001(3) 0.017(3) 0.008(3) C65 0.041(4) 0.028(4) 0.048(4) 0.000(3) 0.002(3) 0.006(3) C66 0.027(3) 0.033(4) 0.035(4) 0.003(3) -0.001(3) 0.009(3) C67 0.046(4) 0.040(4) 0.049(4) 0.005(3) 0.006(3) 0.011(3) C68 0.054(4) 0.068(5) 0.045(4) 0.010(4) 0.008(3) 0.024(4) C69 0.056(4) 0.071(5) 0.055(5) 0.020(4) 0.016(4) 0.022(4) C70 0.044(4) 0.046(4) 0.077(5) 0.032(4) 0.010(4) 0.012(3) C71 0.042(4) 0.041(4) 0.061(5) 0.017(3) 0.011(3) 0.006(3) C72 0.028(3) 0.039(4) 0.044(4) 0.002(3) 0.002(3) 0.009(3) C73 0.054(4) 0.042(4) 0.060(5) 0.011(3) 0.021(4) 0.013(3) C74 0.086(5) 0.047(4) 0.048(4) -0.006(3) 0.032(4) 0.002(4) C75 0.077(5) 0.038(4) 0.096(6) -0.001(4) 0.051(5) 0.018(4) C76 0.059(4) 0.043(4) 0.077(5) 0.006(4) 0.019(4) 0.017(3) C77 0.047(4) 0.032(4) 0.068(5) -0.005(3) 0.003(3) 0.010(3) C78 0.037(3) 0.029(4) 0.045(4) -0.002(3) 0.004(3) 0.004(3) _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 Cr1 O2 2.011(3) . ? Cr1 N1 2.014(4) . ? Cr1 N2 2.030(4) . ? Cr1 O1 2.033(3) . ? Cr2 N3 1.997(4) . ? Cr2 O1 2.006(3) . ? Cr2 O2 2.010(3) . ? Cr2 N4 2.019(4) . ? N1 C1 1.339(5) . ? N1 C8 1.448(6) . ? N2 C2 1.335(5) . ? N2 C20 1.443(5) . ? N3 C27 1.335(5) . ? N3 C34 1.447(6) . ? N4 C28 1.335(6) . ? N4 C46 1.453(6) . ? O1 C53 1.353(5) . ? O2 C66 1.357(5) . ? C1 C2 1.355(6) . ? C3 C4 1.380(7) . ? C3 C8 1.397(7) . ? C3 C9 1.534(7) . ? C4 C5 1.366(7) . ? C5 C6 1.386(7) . ? C6 C7 1.386(6) . ? C7 C8 1.408(7) . ? C7 C12 1.510(7) . ? C9 C11 1.512(7) . ? C9 C10 1.552(7) . ? C12 C13 1.514(6) . ? C12 C14 1.521(6) . ? C15 C16 1.395(6) . ? C15 C20 1.409(6) . ? C15 C21 1.500(6) . ? C16 C17 1.389(7) . ? C17 C18 1.361(6) . ? C18 C19 1.386(6) . ? C19 C20 1.420(6) . ? C19 C24 1.509(6) . ? C21 C23 1.528(6) . ? C21 C22 1.539(6) . ? C24 C26 1.523(6) . ? C24 C25 1.554(6) . ? C27 C28 1.364(6) . ? C29 C30 1.399(7) . ? C29 C34 1.403(7) . ? C29 C35 1.500(7) . ? C30 C31 1.382(7) . ? C31 C32 1.391(7) . ? C32 C33 1.390(7) . ? C33 C34 1.405(6) . ? C33 C38 1.500(7) . ? C35 C36 1.504(6) . ? C35 C37 1.534(6) . ? C38 C40 1.524(7) . ? C38 C39 1.543(6) . ? C41 C42 1.395(7) . ? C41 C46 1.406(6) . ? C41 C47 1.517(6) . ? C42 C43 1.380(7) . ? C43 C44 1.356(7) . ? C44 C45 1.407(7) . ? C45 C46 1.419(6) . ? C45 C50 1.505(7) . ? C47 C48 1.503(6) . ? C47 C49 1.537(6) . ? C50 C51 1.511(6) . ? C50 C52 1.540(6) . ? C53 C59 1.431(7) . ? C53 C65 1.433(7) . ? C54 C55 1.373(7) . ? C54 C59 1.413(6) . ? C55 C56 1.370(7) . ? C56 C57 1.379(7) . ? C57 C58 1.380(7) . ? C58 C59 1.400(6) . ? C60 C61 1.389(7) . ? C60 C65 1.402(6) . ? C61 C62 1.362(7) . ? C62 C63 1.378(7) . ? C63 C64 1.377(6) . ? C64 C65 1.399(6) . ? C66 C72 1.433(7) . ? C66 C78 1.449(6) . ? C67 C68 1.381(7) . ? C67 C72 1.418(7) . ? C68 C69 1.380(7) . ? C69 C70 1.381(7) . ? C70 C71 1.375(7) . ? C71 C72 1.406(6) . ? C73 C78 1.395(7) . ? C73 C74 1.399(7) . ? C74 C75 1.381(7) . ? C75 C76 1.366(7) . ? C76 C77 1.384(7) . ? C77 C78 1.423(6) . ? 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 Cr1 N1 161.88(15) . . ? O2 Cr1 N2 102.97(15) . . ? N1 Cr1 N2 80.38(16) . . ? O2 Cr1 O1 76.14(12) . . ? N1 Cr1 O1 104.56(15) . . ? N2 Cr1 O1 167.06(15) . . ? N3 Cr2 O1 159.78(15) . . ? N3 Cr2 O2 104.53(15) . . ? O1 Cr2 O2 76.79(13) . . ? N3 Cr2 N4 80.67(17) . . ? O1 Cr2 N4 104.09(15) . . ? O2 Cr2 N4 162.85(16) . . ? C1 N1 C8 115.0(4) . . ? C1 N1 Cr1 111.3(3) . . ? C8 N1 Cr1 133.2(3) . . ? C2 N2 C20 114.6(4) . . ? C2 N2 Cr1 111.9(3) . . ? C20 N2 Cr1 132.8(3) . . ? C27 N3 C34 113.6(4) . . ? C27 N3 Cr2 112.4(3) . . ? C34 N3 Cr2 133.5(3) . . ? C28 N4 C46 117.3(4) . . ? C28 N4 Cr2 111.7(3) . . ? C46 N4 Cr2 130.3(3) . . ? C53 O1 Cr2 128.0(3) . . ? C53 O1 Cr1 128.7(3) . . ? Cr2 O1 Cr1 103.22(14) . . ? C66 O2 Cr2 129.9(3) . . ? C66 O2 Cr1 126.2(3) . . ? Cr2 O2 Cr1 103.84(15) . . ? N1 C1 C2 118.8(5) . . ? N2 C2 C1 117.1(5) . . ? C4 C3 C8 118.1(5) . . ? C4 C3 C9 119.5(5) . . ? C8 C3 C9 122.3(5) . . ? C5 C4 C3 121.5(6) . . ? C4 C5 C6 120.1(6) . . ? C7 C6 C5 121.0(6) . . ? C6 C7 C8 117.6(5) . . ? C6 C7 C12 121.0(5) . . ? C8 C7 C12 121.4(5) . . ? C3 C8 C7 121.6(5) . . ? C3 C8 N1 119.7(5) . . ? C7 C8 N1 118.5(5) . . ? C11 C9 C3 112.8(5) . . ? C11 C9 C10 109.0(5) . . ? C3 C9 C10 110.7(5) . . ? C7 C12 C13 111.5(4) . . ? C7 C12 C14 115.4(5) . . ? C13 C12 C14 107.4(5) . . ? C16 C15 C20 117.7(5) . . ? C16 C15 C21 117.9(5) . . ? C20 C15 C21 124.4(5) . . ? C17 C16 C15 121.1(5) . . ? C18 C17 C16 120.9(5) . . ? C17 C18 C19 120.6(5) . . ? C18 C19 C20 119.0(5) . . ? C18 C19 C24 120.9(5) . . ? C20 C19 C24 120.0(5) . . ? C15 C20 C19 120.6(5) . . ? C15 C20 N2 120.3(5) . . ? C19 C20 N2 118.9(5) . . ? C15 C21 C23 112.7(4) . . ? C15 C21 C22 111.7(4) . . ? C23 C21 C22 109.2(4) . . ? C19 C24 C26 115.0(4) . . ? C19 C24 C25 111.5(4) . . ? C26 C24 C25 108.5(4) . . ? N3 C27 C28 117.5(5) . . ? N4 C28 C27 117.6(5) . . ? C30 C29 C34 118.1(5) . . ? C30 C29 C35 119.8(5) . . ? C34 C29 C35 122.1(5) . . ? C31 C30 C29 120.7(6) . . ? C30 C31 C32 120.3(5) . . ? C33 C32 C31 121.1(6) . . ? C32 C33 C34 117.8(6) . . ? C32 C33 C38 118.6(5) . . ? C34 C33 C38 123.6(5) . . ? C29 C34 C33 122.1(5) . . ? C29 C34 N3 118.6(5) . . ? C33 C34 N3 119.3(5) . . ? C29 C35 C36 114.4(5) . . ? C29 C35 C37 111.0(4) . . ? C36 C35 C37 110.1(4) . . ? C33 C38 C40 111.7(5) . . ? C33 C38 C39 113.4(5) . . ? C40 C38 C39 108.2(5) . . ? C42 C41 C46 119.0(5) . . ? C42 C41 C47 120.8(5) . . ? C46 C41 C47 120.1(5) . . ? C43 C42 C41 120.1(5) . . ? C44 C43 C42 120.7(5) . . ? C43 C44 C45 122.6(5) . . ? C44 C45 C46 116.3(5) . . ? C44 C45 C50 118.5(5) . . ? C46 C45 C50 125.2(5) . . ? C41 C46 C45 121.1(5) . . ? C41 C46 N4 118.5(5) . . ? C45 C46 N4 120.3(5) . . ? C48 C47 C41 115.4(5) . . ? C48 C47 C49 108.2(5) . . ? C41 C47 C49 111.2(4) . . ? C45 C50 C51 114.1(5) . . ? C45 C50 C52 110.1(5) . . ? C51 C50 C52 108.6(4) . . ? O1 C53 C59 117.8(5) . . ? O1 C53 C65 118.1(5) . . ? C59 C53 C65 124.0(5) . . ? C55 C54 C59 122.5(5) . . ? C56 C55 C54 121.0(6) . . ? C55 C56 C57 118.0(6) . . ? C56 C57 C58 121.7(6) . . ? C57 C58 C59 121.6(5) . . ? C58 C59 C54 115.1(5) . . ? C58 C59 C53 123.8(5) . . ? C54 C59 C53 121.0(5) . . ? C61 C60 C65 121.3(5) . . ? C62 C61 C60 120.6(5) . . ? C61 C62 C63 119.6(6) . . ? C64 C63 C62 120.2(6) . . ? C63 C64 C65 122.1(5) . . ? C64 C65 C60 116.2(5) . . ? C64 C65 C53 121.7(5) . . ? C60 C65 C53 122.2(5) . . ? O2 C66 C72 118.8(5) . . ? O2 C66 C78 117.0(5) . . ? C72 C66 C78 124.2(5) . . ? C68 C67 C72 121.6(6) . . ? C69 C68 C67 121.0(6) . . ? C68 C69 C70 117.9(6) . . ? C71 C70 C69 122.4(6) . . ? C70 C71 C72 120.8(6) . . ? C71 C72 C67 116.2(5) . . ? C71 C72 C66 123.0(5) . . ? C67 C72 C66 120.8(5) . . ? C78 C73 C74 121.9(5) . . ? C75 C74 C73 119.3(6) . . ? C76 C75 C74 120.3(6) . . ? C75 C76 C77 121.1(6) . . ? C76 C77 C78 120.5(6) . . ? C73 C78 C77 116.8(5) . . ? C73 C78 C66 120.6(5) . . ? C77 C78 C66 122.5(5) . . ? _refine_diff_density_max 0.416 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.067 _shelxl_version_number 2013-2 _shelx_res_file ; TITL klat854 in P-1 CELL 0.71073 12.2571 13.4468 22.1460 90.757 100.752 97.594 ZERR 2.00 0.0036 0.0038 0.0066 0.006 0.005 0.006 LATT 1 SFAC C H N O Cr UNIT 164 204 8 6 4 L.S. 10 ACTA 50 BOND FMAP 2 PLAN 20 SIZE 0.117 0.231 0.293 OMIT 0 0 1 OMIT 1 0 0 TEMP -73 WGHT 0.002900 FVAR 4.27070 CR1 5 -0.001023 0.308561 0.227585 11.00000 0.03145 0.02865 = 0.04326 0.00196 0.00468 0.00596 CR2 5 0.244892 0.370860 0.303541 11.00000 0.03102 0.02852 = 0.03972 0.00312 0.00380 0.00419 N1 3 -0.094182 0.192027 0.176012 11.00000 0.03147 0.03269 = 0.04317 0.00219 -0.00318 0.00504 N2 3 -0.143261 0.370194 0.198436 11.00000 0.02753 0.02548 = 0.04241 -0.00312 0.00575 0.00602 N3 3 0.376000 0.476782 0.304870 11.00000 0.02409 0.03640 = 0.03605 0.01040 0.00155 0.00129 N4 3 0.354184 0.322067 0.372933 11.00000 0.03220 0.03457 = 0.04860 0.00572 -0.00008 0.00254 O1 4 0.131783 0.249485 0.275692 11.00000 0.03627 0.01904 = 0.05181 0.00926 -0.00755 0.00577 O2 4 0.114085 0.429202 0.255399 11.00000 0.02907 0.02687 = 0.04789 0.00423 -0.00178 0.00484 C1 1 -0.191055 0.217719 0.145868 11.00000 0.03894 0.03272 = 0.04635 -0.00843 -0.00780 0.00682 AFIX 43 H1 2 -0.239728 0.172670 0.116190 11.00000 -1.20000 AFIX 0 C2 1 -0.218378 0.309164 0.158478 11.00000 0.03052 0.03757 = 0.04517 -0.00568 -0.00491 0.00561 AFIX 43 H2 2 -0.287986 0.328967 0.139688 11.00000 -1.20000 AFIX 0 C3 1 -0.130275 0.008003 0.179718 11.00000 0.03893 0.02636 = 0.06324 -0.00648 0.00685 0.00489 C4 1 -0.112419 -0.084912 0.159407 11.00000 0.05547 0.04014 = 0.08655 0.00246 0.02778 0.00429 AFIX 43 H4 2 -0.152170 -0.143697 0.172454 11.00000 -1.20000 AFIX 0 C5 1 -0.038873 -0.094251 0.120967 11.00000 0.07046 0.02972 = 0.09796 -0.01210 0.01895 0.00845 AFIX 43 H5 2 -0.027026 -0.159043 0.108188 11.00000 -1.20000 AFIX 0 C6 1 0.018491 -0.009351 0.100578 11.00000 0.05678 0.04572 = 0.06131 -0.01224 0.01596 0.00921 AFIX 43 H6 2 0.068995 -0.016623 0.073590 11.00000 -1.20000 AFIX 0 C7 1 0.003315 0.085976 0.118952 11.00000 0.04000 0.03314 = 0.03979 -0.00773 0.00000 0.00461 C8 1 -0.071612 0.093279 0.159385 11.00000 0.03188 0.02617 = 0.04747 -0.00553 -0.00048 0.00764 C9 1 -0.215294 0.014546 0.221910 11.00000 0.05094 0.03814 = 0.08145 0.00652 0.01307 0.00140 AFIX 13 H9 2 -0.203523 0.084560 0.239985 11.00000 -1.20000 AFIX 0 C10 1 -0.337002 -0.006970 0.184739 11.00000 0.04332 0.10286 = 0.10950 0.01462 0.01094 -0.00813 AFIX 137 H10A 2 -0.345127 0.036165 0.149301 11.00000 -1.50000 H10B 2 -0.389593 0.006886 0.211102 11.00000 -1.50000 H10C 2 -0.353146 -0.077550 0.170339 11.00000 -1.50000 AFIX 0 C11 1 -0.201739 -0.056631 0.274258 11.00000 0.06517 0.04704 = 0.08065 0.01525 0.01062 0.00817 AFIX 137 H11A 2 -0.222312 -0.126005 0.257860 11.00000 -1.50000 H11B 2 -0.250576 -0.042968 0.302849 11.00000 -1.50000 H11C 2 -0.123545 -0.047043 0.295987 11.00000 -1.50000 AFIX 0 C12 1 0.064011 0.178384 0.095679 11.00000 0.04919 0.03938 = 0.06210 -0.00291 0.01172 0.00163 AFIX 13 H12 2 0.087097 0.228903 0.130812 11.00000 -1.20000 AFIX 0 C13 1 -0.011983 0.224759 0.045123 11.00000 0.08556 0.08110 = 0.05798 0.02031 0.02674 0.01864 AFIX 137 H13A 2 -0.040567 0.175277 0.011080 11.00000 -1.50000 H13B 2 0.030403 0.283345 0.030310 11.00000 -1.50000 H13C 2 -0.074969 0.245668 0.061258 11.00000 -1.50000 AFIX 0 C14 1 0.169034 0.162651 0.071527 11.00000 0.04679 0.07937 = 0.09398 -0.00131 0.01820 0.00593 AFIX 137 H14A 2 0.219545 0.131320 0.102927 11.00000 -1.50000 H14B 2 0.206963 0.227608 0.061805 11.00000 -1.50000 H14C 2 0.148257 0.118890 0.034290 11.00000 -1.50000 AFIX 0 C15 1 -0.215179 0.531887 0.176200 11.00000 0.02385 0.02754 = 0.05320 0.00272 0.00974 0.00276 C16 1 -0.261125 0.612166 0.197310 11.00000 0.04167 0.04990 = 0.04284 0.00497 0.00948 0.00755 AFIX 43 H16 2 -0.284352 0.661953 0.169575 11.00000 -1.20000 AFIX 0 C17 1 -0.273494 0.620555 0.258171 11.00000 0.04465 0.03146 = 0.06926 0.00115 0.01075 0.01545 AFIX 43 H17 2 -0.303638 0.676626 0.271622 11.00000 -1.20000 AFIX 0 C18 1 -0.243016 0.549536 0.298814 11.00000 0.03918 0.04853 = 0.04028 -0.00585 0.01616 0.00672 AFIX 43 H18 2 -0.251980 0.556638 0.340278 11.00000 -1.20000 AFIX 0 C19 1 -0.199046 0.466990 0.280271 11.00000 0.02902 0.03083 = 0.04257 -0.00025 0.00944 0.00317 C20 1 -0.184178 0.458456 0.218414 11.00000 0.02377 0.02978 = 0.04115 -0.00531 0.00299 0.00666 C21 1 -0.204538 0.528252 0.109840 11.00000 0.04129 0.04251 = 0.03458 0.00208 0.00441 0.01036 AFIX 13 H21 2 -0.158907 0.473690 0.104080 11.00000 -1.20000 AFIX 0 C22 1 -0.319445 0.502375 0.066976 11.00000 0.04455 0.06738 = 0.05608 0.00832 -0.00419 0.00243 AFIX 137 H22A 2 -0.355078 0.436482 0.076725 11.00000 -1.50000 H22B 2 -0.309294 0.500772 0.024132 11.00000 -1.50000 H22C 2 -0.367129 0.553393 0.072776 11.00000 -1.50000 AFIX 0 C23 1 -0.144445 0.626059 0.090364 11.00000 0.04649 0.05271 = 0.06551 0.02678 0.01766 0.01175 AFIX 137 H23A 2 -0.186768 0.681251 0.096153 11.00000 -1.50000 H23B 2 -0.139054 0.619551 0.046927 11.00000 -1.50000 H23C 2 -0.068982 0.640091 0.115522 11.00000 -1.50000 AFIX 0 C24 1 -0.175312 0.383163 0.323386 11.00000 0.04301 0.04644 = 0.03787 0.00805 0.01156 0.01432 AFIX 13 H24 2 -0.101707 0.363306 0.318194 11.00000 -1.20000 AFIX 0 C25 1 -0.264765 0.288961 0.306365 11.00000 0.04356 0.04731 = 0.06091 0.00784 0.01338 -0.00129 AFIX 137 H25A 2 -0.338959 0.306623 0.308701 11.00000 -1.50000 H25B 2 -0.247082 0.236145 0.335208 11.00000 -1.50000 H25C 2 -0.264666 0.264710 0.264453 11.00000 -1.50000 AFIX 0 C26 1 -0.165640 0.410696 0.391286 11.00000 0.06589 0.06533 = 0.04932 0.00793 0.01206 0.01817 AFIX 137 H26A 2 -0.109667 0.470230 0.402730 11.00000 -1.50000 H26B 2 -0.142606 0.354530 0.416049 11.00000 -1.50000 H26C 2 -0.238424 0.425044 0.398770 11.00000 -1.50000 AFIX 0 C27 1 0.465819 0.459577 0.345590 11.00000 0.03159 0.03910 = 0.04288 0.00944 -0.00211 -0.00493 AFIX 43 H27 2 0.535606 0.501496 0.348988 11.00000 -1.20000 AFIX 0 C28 1 0.453700 0.379569 0.382148 11.00000 0.02921 0.04934 = 0.04634 0.01387 -0.00396 0.00448 AFIX 43 H28 2 0.513921 0.365296 0.413051 11.00000 -1.20000 AFIX 0 C29 1 0.409140 0.539985 0.205681 11.00000 0.02878 0.04361 = 0.04750 0.01668 0.00167 0.01442 C30 1 0.436194 0.621221 0.169913 11.00000 0.03854 0.05286 = 0.05247 0.01335 0.00398 0.01264 AFIX 43 H30 2 0.443833 0.609424 0.128613 11.00000 -1.20000 AFIX 0 C31 1 0.451934 0.718515 0.194053 11.00000 0.04411 0.04732 = 0.07802 0.03759 0.01378 0.00639 AFIX 43 H31 2 0.472196 0.772946 0.169629 11.00000 -1.20000 AFIX 0 C32 1 0.438236 0.737089 0.253953 11.00000 0.04216 0.04158 = 0.07080 0.01783 -0.00567 0.00313 AFIX 43 H32 2 0.447894 0.804382 0.269708 11.00000 -1.20000 AFIX 0 C33 1 0.410665 0.658854 0.291126 11.00000 0.03462 0.03640 = 0.04632 0.00924 0.00111 0.00525 C34 1 0.397993 0.560348 0.266353 11.00000 0.02836 0.02829 = 0.03969 0.00328 -0.00495 0.00125 C35 1 0.396729 0.434835 0.179364 11.00000 0.03573 0.04535 = 0.04740 0.00502 0.01197 0.00741 AFIX 13 H35 2 0.331558 0.396014 0.193691 11.00000 -1.20000 AFIX 0 C36 1 0.372160 0.426568 0.110235 11.00000 0.04388 0.09168 = 0.05087 -0.00191 0.00601 0.01328 AFIX 137 H36A 2 0.312124 0.466157 0.094364 11.00000 -1.50000 H36B 2 0.348509 0.356064 0.096673 11.00000 -1.50000 H36C 2 0.439834 0.452095 0.094619 11.00000 -1.50000 AFIX 0 C37 1 0.500073 0.384331 0.204650 11.00000 0.04914 0.04515 = 0.06825 0.00568 0.01036 0.01386 AFIX 137 H37A 2 0.567441 0.425333 0.196232 11.00000 -1.50000 H37B 2 0.492352 0.317598 0.184725 11.00000 -1.50000 H37C 2 0.506463 0.377790 0.249150 11.00000 -1.50000 AFIX 0 C38 1 0.400089 0.683476 0.355846 11.00000 0.04869 0.04026 = 0.04957 0.00493 -0.00635 -0.00303 AFIX 13 H38 2 0.364212 0.621371 0.372578 11.00000 -1.20000 AFIX 0 C39 1 0.326676 0.767004 0.360617 11.00000 0.07335 0.04397 = 0.07860 -0.00776 0.01185 0.00948 AFIX 137 H39A 2 0.358352 0.828142 0.342955 11.00000 -1.50000 H39B 2 0.324666 0.780771 0.403933 11.00000 -1.50000 H39C 2 0.250392 0.745138 0.337993 11.00000 -1.50000 AFIX 0 C40 1 0.514221 0.714822 0.396976 11.00000 0.09711 0.09458 = 0.07900 -0.01437 -0.01745 0.02346 AFIX 137 H40A 2 0.561177 0.661483 0.395833 11.00000 -1.50000 H40B 2 0.504414 0.726405 0.439300 11.00000 -1.50000 H40C 2 0.550458 0.776735 0.382241 11.00000 -1.50000 AFIX 0 C41 1 0.259444 0.260647 0.456424 11.00000 0.03418 0.03681 = 0.04495 0.00091 -0.00065 0.00700 C42 1 0.239323 0.188040 0.498907 11.00000 0.04113 0.06589 = 0.04597 0.02125 0.01366 0.00766 AFIX 43 H42 2 0.186757 0.195557 0.524629 11.00000 -1.20000 AFIX 0 C43 1 0.295651 0.105340 0.503617 11.00000 0.05347 0.06105 = 0.05609 0.03833 0.01702 0.00233 AFIX 43 H43 2 0.279834 0.055120 0.531721 11.00000 -1.20000 AFIX 0 C44 1 0.373385 0.095027 0.468522 11.00000 0.04986 0.04802 = 0.06404 0.01854 0.01496 0.01265 AFIX 43 H44 2 0.412849 0.038570 0.473935 11.00000 -1.20000 AFIX 0 C45 1 0.397892 0.164606 0.424427 11.00000 0.03112 0.03501 = 0.03749 0.00992 -0.00570 -0.00125 C46 1 0.335912 0.247051 0.417948 11.00000 0.03066 0.03827 = 0.04012 0.00850 -0.00073 0.01072 C47 1 0.204663 0.355666 0.453717 11.00000 0.05366 0.05000 = 0.04741 0.00389 0.01354 0.01594 AFIX 13 H47 2 0.179543 0.368782 0.409286 11.00000 -1.20000 AFIX 0 C48 1 0.103703 0.351362 0.483571 11.00000 0.04903 0.08978 = 0.07217 -0.00379 0.02531 0.01546 AFIX 137 H48A 2 0.053864 0.288523 0.470738 11.00000 -1.50000 H48B 2 0.063656 0.408398 0.471049 11.00000 -1.50000 H48C 2 0.127764 0.354359 0.528391 11.00000 -1.50000 AFIX 0 C49 1 0.289134 0.446529 0.482055 11.00000 0.06110 0.04666 = 0.07387 -0.01129 0.00268 0.01532 AFIX 137 H49A 2 0.314176 0.437034 0.526014 11.00000 -1.50000 H49B 2 0.253270 0.507608 0.476699 11.00000 -1.50000 H49C 2 0.353824 0.452890 0.461523 11.00000 -1.50000 AFIX 0 C50 1 0.489193 0.148712 0.389799 11.00000 0.03654 0.04785 = 0.06425 0.01490 0.01352 0.01756 AFIX 13 H50 2 0.487045 0.197453 0.356021 11.00000 -1.20000 AFIX 0 C51 1 0.477780 0.044380 0.361156 11.00000 0.09343 0.05084 = 0.07568 0.00044 0.01884 0.03366 AFIX 137 H51A 2 0.493397 -0.003485 0.393592 11.00000 -1.50000 H51B 2 0.531215 0.043112 0.333387 11.00000 -1.50000 H51C 2 0.401322 0.025826 0.337904 11.00000 -1.50000 AFIX 0 C52 1 0.604652 0.171098 0.432634 11.00000 0.03402 0.06086 = 0.08683 0.02528 0.00979 0.00933 AFIX 137 H52A 2 0.619971 0.242740 0.444599 11.00000 -1.50000 H52B 2 0.662688 0.153264 0.411070 11.00000 -1.50000 H52C 2 0.604762 0.131535 0.469488 11.00000 -1.50000 AFIX 0 C53 1 0.140537 0.152413 0.288456 11.00000 0.02986 0.04304 = 0.03872 0.00440 0.00643 0.00194 C54 1 -0.005468 0.152938 0.352055 11.00000 0.03751 0.03183 = 0.06792 0.01282 0.01207 0.00782 AFIX 43 H54 2 -0.025054 0.213060 0.333550 11.00000 -1.20000 AFIX 0 C55 1 -0.063074 0.112825 0.395579 11.00000 0.04481 0.05736 = 0.07347 0.01585 0.01329 0.01295 AFIX 43 H55 2 -0.122754 0.144393 0.405461 11.00000 -1.20000 AFIX 0 C56 1 -0.035782 0.027983 0.424961 11.00000 0.05294 0.05190 = 0.06558 0.01433 0.01398 -0.00183 AFIX 43 H56 2 -0.076311 -0.000328 0.454650 11.00000 -1.20000 AFIX 0 C57 1 0.052284 -0.015080 0.410144 11.00000 0.05294 0.05477 = 0.06694 0.01053 0.00407 0.00985 AFIX 43 H57 2 0.073950 -0.072692 0.431023 11.00000 -1.20000 AFIX 0 C58 1 0.109781 0.023304 0.365787 11.00000 0.04538 0.03558 = 0.05541 0.01517 0.01449 -0.00131 AFIX 43 H58 2 0.169817 -0.008682 0.356776 11.00000 -1.20000 AFIX 0 C59 1 0.081812 0.108222 0.333738 11.00000 0.03406 0.03672 = 0.04894 0.00012 0.00534 0.00059 C60 1 0.189651 -0.002791 0.244588 11.00000 0.04899 0.04051 = 0.06665 0.00668 0.02112 0.01440 AFIX 43 H60 2 0.126919 -0.040843 0.256750 11.00000 -1.20000 AFIX 0 C61 1 0.258779 -0.051228 0.214573 11.00000 0.05952 0.02734 = 0.08585 -0.00888 0.01530 0.00505 AFIX 43 H61 2 0.242166 -0.121579 0.205974 11.00000 -1.20000 AFIX 0 C62 1 0.350157 0.001181 0.197354 11.00000 0.05773 0.05716 = 0.06095 -0.00426 0.01623 0.01911 AFIX 43 H62 2 0.398364 -0.032709 0.177938 11.00000 -1.20000 AFIX 0 C63 1 0.372285 0.103654 0.208257 11.00000 0.06101 0.03470 = 0.08470 -0.00243 0.03566 0.00758 AFIX 43 H63 2 0.435348 0.140670 0.195819 11.00000 -1.20000 AFIX 0 C64 1 0.303220 0.152522 0.237135 11.00000 0.04301 0.03857 = 0.05470 0.00115 0.01660 0.00755 AFIX 43 H64 2 0.318986 0.223363 0.243562 11.00000 -1.20000 AFIX 0 C65 1 0.210567 0.101157 0.257310 11.00000 0.04075 0.02844 = 0.04829 0.00044 0.00181 0.00597 C66 1 0.104073 0.525690 0.240708 11.00000 0.02659 0.03344 = 0.03518 0.00333 -0.00085 0.00854 C67 1 0.093318 0.486893 0.129839 11.00000 0.04618 0.04023 = 0.04931 0.00544 0.00633 0.01067 AFIX 43 H67 2 0.067839 0.418629 0.136036 11.00000 -1.20000 AFIX 0 C68 1 0.105332 0.515710 0.071547 11.00000 0.05404 0.06849 = 0.04514 0.01046 0.00764 0.02355 AFIX 43 H68 2 0.085755 0.467481 0.038237 11.00000 -1.20000 AFIX 0 C69 1 0.145336 0.613478 0.060929 11.00000 0.05631 0.07071 = 0.05466 0.02025 0.01576 0.02201 AFIX 43 H69 2 0.154359 0.633139 0.020913 11.00000 -1.20000 AFIX 0 C70 1 0.171848 0.681859 0.110302 11.00000 0.04401 0.04648 = 0.07721 0.03217 0.00997 0.01219 AFIX 43 H70 2 0.199954 0.749315 0.103704 11.00000 -1.20000 AFIX 0 C71 1 0.159012 0.655783 0.168660 11.00000 0.04175 0.04057 = 0.06076 0.01720 0.01086 0.00616 AFIX 43 H71 2 0.178022 0.705287 0.201271 11.00000 -1.20000 AFIX 0 C72 1 0.118109 0.556778 0.180673 11.00000 0.02798 0.03858 = 0.04409 0.00204 0.00201 0.00932 C73 1 0.095369 0.564227 0.348947 11.00000 0.05402 0.04188 = 0.06030 0.01147 0.02055 0.01349 AFIX 43 H73 2 0.124002 0.503249 0.359732 11.00000 -1.20000 AFIX 0 C74 1 0.070611 0.624720 0.395087 11.00000 0.08626 0.04688 = 0.04782 -0.00552 0.03241 0.00171 AFIX 43 H74 2 0.083560 0.605544 0.436675 11.00000 -1.20000 AFIX 0 C75 1 0.027153 0.712602 0.379562 11.00000 0.07658 0.03836 = 0.09636 -0.00060 0.05123 0.01773 AFIX 43 H75 2 0.011577 0.754821 0.410725 11.00000 -1.20000 AFIX 0 C76 1 0.006469 0.739081 0.319580 11.00000 0.05853 0.04259 = 0.07703 0.00630 0.01860 0.01717 AFIX 43 H76 2 -0.025542 0.798691 0.309354 11.00000 -1.20000 AFIX 0 C77 1 0.031385 0.680485 0.273460 11.00000 0.04724 0.03217 = 0.06778 -0.00532 0.00278 0.00992 AFIX 43 H77 2 0.016406 0.700305 0.232045 11.00000 -1.20000 AFIX 0 C78 1 0.079255 0.590801 0.287578 11.00000 0.03685 0.02878 = 0.04545 -0.00195 0.00386 0.00420 HKLF 4 REM klat854 in P-1 REM R1 = 0.0831 for 5165 Fo > 4sig(Fo) and 0.2342 for all 17665 data REM 791 parameters refined using 0 restraints END WGHT 0.0519 0.0000 REM Highest difference peak 0.416, deepest hole -0.507, 1-sigma level 0.067 Q1 1 -0.0027 0.2390 0.1922 11.00000 0.05 0.34 Q2 1 0.2400 0.3171 0.2566 11.00000 0.05 0.32 Q3 1 0.0865 0.2678 0.2427 11.00000 0.05 0.30 Q4 1 0.2601 0.3294 0.3481 11.00000 0.05 0.29 Q5 1 0.1553 0.3384 0.2711 11.00000 0.05 0.29 Q6 1 0.0809 0.3407 0.2672 11.00000 0.05 0.28 Q7 1 0.0202 0.4028 0.2419 11.00000 0.05 0.27 Q8 1 -0.1477 0.1180 0.2715 11.00000 0.05 0.26 Q9 1 0.0028 0.3705 0.2697 11.00000 0.05 0.26 Q10 1 -0.0338 0.2155 0.2195 11.00000 0.05 0.25 Q11 1 0.2151 0.2841 0.2891 11.00000 0.05 0.25 Q12 1 0.3967 -0.0287 0.2882 11.00000 0.05 0.25 Q13 1 -0.4817 -0.0643 0.1606 11.00000 0.05 0.25 Q14 1 0.0289 0.3593 0.2787 11.00000 0.05 0.25 Q15 1 0.3368 0.4132 0.3326 11.00000 0.05 0.24 Q16 1 0.1302 0.2244 0.5225 11.00000 0.05 0.24 Q17 1 0.3057 0.2636 0.2487 11.00000 0.05 0.24 Q18 1 0.2504 0.0658 0.1703 11.00000 0.05 0.24 Q19 1 0.0428 0.3031 0.1586 11.00000 0.05 0.23 Q20 1 0.3828 0.0702 0.2799 11.00000 0.05 0.23 ; _shelx_res_checksum 78704 _shelx_hkl_file ; 2 0 0 3785 1835 9050 7.57 -0.52 1.0000 2 0 0 1820 1479 5816 7.57 -0.52 1.0000 2 0 0 4247 1638 9758 7.57 -0.52 1.0000 2 0 0 4021 1905 9414 7.57 -0.52 1.0000 3 0 0 5024 1640 2597 4.67 1.48 1.0000 3 0 0 8717 2127 5421 4.67 1.48 1.0000 3 0 0 473 1551 -941 4.67 1.48 1.0000 3 0 0 3479 1483 1514 4.67 1.48 1.0000 4 0 0 1959 1855 1258 -1.85 -0.92 1.0000 4 0 0 1888 1389 1201 -1.85 -0.92 1.0000 -4 0 0 1516 1462 1020 -1.85 0.92 1.0000 4 0 0 84 1514 -969 -1.85 -0.92 1.0000 5 0 0 45572 5347 47223 0.86 0.03 1.0000 5 0 0 47713 5594 49402 0.86 0.03 1.0000 5 0 0 53084 4643 54864 0.86 0.03 1.0000 -5 0 0 44966 4559 46603 0.86 -0.03 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-1 -1 28 112 5973 48 -0.36 -1.57 1.0000 0 -1 28 1543 6181 1373 -1.60 2.52 1.0000 0 1 -28 1369 4822 1041 -1.60 -2.52 1.0000 -1 1 -28 262 4108 -1962 3.64 0.17 1.0000 1 -1 28 262 4046 -120 3.64 -0.17 1.0000 2 -1 28 2840 4803 4414 -2.34 -2.19 1.0000 -2 1 -28 1313 4224 2437 -2.34 2.19 1.0000 8 0 -28 172 4184 -5871 2.01 2.17 1.0000 -7 0 28 4707 7776 6557 -2.57 1.66 1.0000 7 0 -28 184 4236 -2130 -2.57 -1.66 1.0000 -7 0 28 184 3723 -3550 -2.57 1.66 1.0000 -6 0 28 78 4824 -140 1.93 -0.46 1.0000 -6 0 28 1435 3300 2172 1.93 -0.46 1.0000 6 0 -28 1003 5709 1637 1.93 0.46 1.0000 5 0 -28 13 4789 -1803 -0.67 0.45 1.0000 -5 0 28 13 4492 -2602 -0.67 -0.45 1.0000 -4 0 28 2 7349 -3230 0.17 0.30 1.0000 4 0 -28 2656 6261 2594 0.17 -0.30 1.0000 -3 0 28 32 6359 -2874 -0.07 1.27 1.0000 3 0 -28 12335 7012 12571 -0.07 -1.27 1.0000 -2 0 28 18 5179 -1745 -0.42 -0.85 1.0000 2 0 -28 18 5691 -5146 -0.42 0.85 1.0000 1 0 -28 1618 7309 1686 0.06 1.74 1.0000 -1 0 28 1188 5084 1281 0.06 -1.74 1.0000 0 0 -28 197 5539 -1589 -2.19 -2.28 1.0000 0 0 28 4185 6487 5877 -2.19 2.28 1.0000 -1 0 -28 477 4693 -757 4.92 0.18 1.0000 1 0 28 5786 6135 9582 4.92 -0.18 1.0000 -2 0 -28 258 3929 -2669 -3.21 1.67 1.0000 2 0 28 3207 5481 5286 -3.21 -1.67 1.0000 8 -1 -28 1349 4983 1887 1.34 1.60 1.0000 7 -1 -28 48 3910 -9361 -1.49 0.45 1.0000 -7 1 28 1151 5691 1657 -1.49 -0.45 1.0000 -7 1 28 154 4035 366 -1.49 -0.45 1.0000 6 -1 -28 94 5816 -3104 1.38 -1.69 1.0000 -6 1 28 4260 5549 3576 1.38 1.69 1.0000 -6 1 28 756 3639 452 1.38 1.69 1.0000 5 -1 -28 73 5100 -2884 -1.57 1.12 1.0000 -5 1 28 73 5818 -1991 -1.57 -1.12 1.0000 4 -1 -28 237 4197 -5083 2.95 1.84 1.0000 -4 1 28 1797 6934 3336 2.95 -1.84 1.0000 3 -1 -28 10159 7267 14254 -2.61 -4.03 1.0000 -3 1 28 453 5043 -2459 -2.61 4.03 1.0000 2 -1 -28 7819 6419 7277 1.37 2.45 1.0000 -2 1 28 155 4337 -13097 1.37 -2.45 1.0000 1 -1 -28 685 5293 966 -1.09 -0.32 1.0000 -1 1 28 6872 7469 7695 -1.09 0.32 1.0000 0 -1 -28 5373 6418 5326 -0.09 -0.40 1.0000 0 1 28 6221 4882 6186 -0.09 0.40 1.0000 1 1 28 4814 6089 4262 1.08 0.79 1.0000 -1 -1 -28 35 4876 -9320 1.08 -0.79 1.0000 -7 2 28 7064 4550 9497 0.44 -3.64 1.0000 7 -2 -28 1974 5796 3294 0.44 3.64 1.0000 -7 2 28 264 5146 -7975 0.44 -3.64 1.0000 -6 2 28 4738 4690 5253 -0.57 3.78 1.0000 6 -2 -28 288 4211 -622 -0.57 -3.78 1.0000 -6 2 28 3804 6510 4237 -0.57 3.78 1.0000 -5 2 28 23 4964 -2057 -0.46 -0.99 1.0000 5 -2 -28 5575 5551 5407 -0.46 0.99 1.0000 -4 2 28 241 4562 -6818 1.52 -3.15 1.0000 4 -2 -28 778 4594 1856 1.52 3.15 1.0000 3 -2 -28 256 5372 -166 -1.21 -3.40 1.0000 -3 2 28 256 5820 -2290 -1.21 3.40 1.0000 -2 2 28 2968 6741 3292 0.57 -0.94 1.0000 2 -2 -28 24 5902 -472 0.57 0.94 1.0000 -1 2 28 5954 5317 6599 0.89 0.49 1.0000 1 -2 -28 13836 8410 14772 0.89 -0.49 1.0000 0 2 28 35 4729 -5238 -0.71 -1.12 1.0000 0 -2 -28 35 5016 -3297 -0.71 1.12 1.0000 -1 -2 -28 1592 6311 2142 -0.61 -1.90 1.0000 1 2 28 78 4901 -830 -0.61 1.90 1.0000 -7 3 28 1877 5920 3505 1.05 -3.55 1.0000 7 -3 -28 270 4067 -3788 1.05 3.55 1.0000 7 -3 -28 4490 6266 6874 1.05 3.55 1.0000 6 -3 -28 2234 4782 3585 -0.86 -2.92 1.0000 6 -3 -28 3883 6182 5620 -0.86 -2.92 1.0000 -6 3 28 182 4983 -4984 -0.86 2.92 1.0000 -5 3 28 10 4540 -6513 0.15 0.68 1.0000 5 -3 -28 3145 6388 3113 0.15 -0.68 1.0000 -4 3 28 368 3999 -7050 -0.92 -4.23 1.0000 4 -3 -28 368 4674 -2436 -0.92 4.23 1.0000 3 -3 -28 7421 6319 8368 0.95 -2.09 1.0000 -3 3 28 2790 7223 3382 0.95 2.09 1.0000 2 -3 -28 3615 6374 4743 0.55 -2.15 1.0000 -2 3 28 97 3868 -8432 0.55 2.15 1.0000 1 -3 -28 6660 6890 7345 -0.67 2.15 1.0000 -1 3 28 12080 7715 13164 -0.67 -2.15 1.0000 0 3 28 28 4758 -4807 1.03 -0.61 1.0000 0 -3 -28 7521 6671 6749 1.03 0.61 1.0000 -6 4 28 9 5130 -424 -0.41 -0.56 1.0000 6 -4 -28 6239 4380 6523 -0.41 0.56 1.0000 6 -4 -28 12026 6150 12422 -0.41 0.56 1.0000 5 -4 -28 3357 4432 4858 -0.16 -2.95 1.0000 -5 4 28 2162 6222 3339 -0.16 2.95 1.0000 4 -4 -28 6831 6097 10249 -0.51 4.19 1.0000 -4 4 28 351 5204 -2145 -0.51 -4.19 1.0000 -3 4 28 3721 6372 3376 0.70 1.01 1.0000 3 -4 -28 7920 6246 7472 0.70 -1.01 1.0000 -2 4 28 1035 5994 1075 -0.04 2.49 1.0000 2 -4 -28 112 5560 36 -0.04 -2.49 1.0000 1 -4 -28 94 4532 -8199 -1.15 1.85 1.0000 -1 4 28 557 5457 1022 -1.15 -1.85 1.0000 0 4 28 77 4560 -1313 1.97 -0.11 1.0000 0 -4 -28 2425 4488 3362 1.97 0.11 1.0000 5 -5 -28 147 3543 -6956 -0.12 -2.73 1.0000 -5 5 28 147 3690 -9152 -0.12 2.73 1.0000 -4 5 28 111 3778 -1647 -0.12 -2.37 1.0000 4 -5 -28 1290 5870 1638 -0.12 2.37 1.0000 3 -5 -28 3073 5316 3649 1.09 0.48 1.0000 -3 5 28 2355 5466 2859 1.09 -0.48 1.0000 -2 5 28 143 4553 -1311 -2.45 1.12 1.0000 2 -5 -28 4055 5089 2923 -2.45 -1.12 1.0000 4 3 -29 2171 4177 2952 -0.76 1.73 1.0000 -4 -3 29 70 4905 -4416 -0.76 -1.73 1.0000 -3 -3 29 97 5677 -312 0.45 2.17 1.0000 3 3 -29 97 3810 -673 0.45 -2.17 1.0000 2 3 -29 2080 4215 3651 -1.03 3.18 1.0000 -2 -3 29 4509 6449 6720 -1.03 -3.18 1.0000 1 3 -29 2283 4006 2533 1.75 -2.18 1.0000 -1 -3 29 154 4493 -878 1.75 2.18 1.0000 -5 -2 29 1393 6744 1693 0.75 1.33 1.0000 5 2 -29 6278 5488 6853 0.75 -1.33 1.0000 4 2 -29 6 3825 -5577 -0.53 -0.19 1.0000 -4 -2 29 8096 6304 7695 -0.53 0.19 1.0000 3 2 -29 26 3851 -10303 -1.11 0.30 1.0000 -3 -2 29 26 5543 -3223 -1.11 -0.30 1.0000 -2 -2 29 18 4395 -5073 0.34 -0.90 1.0000 2 2 -29 6930 5448 7319 0.34 0.90 1.0000 -1 -2 29 6085 7519 6186 -0.23 1.03 1.0000 1 2 -29 22 3821 -8718 -0.23 -1.03 1.0000 5 1 -29 3176 5266 4237 1.90 -0.66 1.0000 -5 -1 29 80 4835 -4758 1.90 0.66 1.0000 4 1 -29 5339 6365 6345 -1.27 -1.53 1.0000 -4 -1 29 3236 6455 3954 -1.27 1.53 1.0000 3 1 -29 1388 4893 1626 -0.47 2.19 1.0000 -3 -1 29 6868 6059 7563 -0.47 -2.19 1.0000 -2 -1 29 3215 6932 3847 0.92 0.94 1.0000 2 1 -29 159 4283 296 0.92 -0.94 1.0000 1 1 -29 0 4392 -6051 0.05 0.10 1.0000 -1 -1 29 0 4423 -1917 0.05 -0.10 1.0000 0 -1 29 84 4066 -233 -1.63 1.27 1.0000 0 1 -29 7417 4198 8842 -1.63 -1.27 1.0000 6 0 -29 3021 4451 2271 1.64 0.21 1.0000 -6 0 29 54 5212 -7561 1.64 -0.21 1.0000 5 0 -29 5385 5416 5788 -0.60 -0.12 1.0000 -5 0 29 961 5840 1129 -0.60 0.12 1.0000 4 0 -29 4731 5445 4940 -0.34 0.01 1.0000 -4 0 29 1025 5787 1124 -0.34 -0.01 1.0000 -3 0 29 11 6052 -547 0.62 0.42 1.0000 3 0 -29 11 6048 -1055 0.62 -0.42 1.0000 2 0 -29 7815 6162 7421 0.60 0.98 1.0000 -2 0 29 938 4207 829 0.60 -0.98 1.0000 -1 0 29 5 4505 -2138 0.21 -0.46 1.0000 1 0 -29 1275 6318 1205 0.21 0.46 1.0000 0 0 29 197 4260 -5952 -2.31 2.17 1.0000 0 0 -29 31 4739 380 -2.31 -2.17 1.0000 6 -1 -29 8273 6757 9278 1.15 -0.82 1.0000 -5 1 29 91 4573 -4730 -2.13 -0.31 1.0000 5 -1 -29 91 4885 -684 -2.13 0.31 1.0000 -4 1 29 142 4751 -1390 2.13 -1.65 1.0000 4 -1 -29 3032 5174 4403 2.13 1.65 1.0000 -3 1 29 270 4677 -3196 -1.54 3.37 1.0000 3 -1 -29 270 4352 -7025 -1.54 -3.37 1.0000 -2 1 29 1868 4830 2968 1.57 -2.70 1.0000 2 -1 -29 340 5898 833 1.57 2.70 1.0000 1 -1 -29 29 4726 -2463 -1.18 0.24 1.0000 -1 1 29 29 4928 -2943 -1.18 -0.24 1.0000 5 -2 -29 1849 4875 1876 -0.28 0.76 1.0000 -5 2 29 13 4017 -4590 -0.28 -0.76 1.0000 4 -2 -29 2988 5059 4350 1.52 2.27 1.0000 -4 2 29 284 6855 807 1.52 -2.27 1.0000 3 -2 -29 1834 5134 3439 -1.47 -3.32 1.0000 -3 2 29 259 4240 -1373 -1.47 3.32 1.0000 2 -2 -29 6389 5366 6450 -0.28 1.03 1.0000 -2 2 29 22 5145 -432 -0.28 -1.03 1.0000 1 -2 -29 5514 5796 5192 0.50 0.35 1.0000 -1 2 29 7 4815 -3224 0.50 -0.35 1.0000 4 -3 -29 5294 4637 7734 -0.16 3.43 1.0000 -4 3 29 2055 4283 3662 -0.16 -3.43 1.0000 3 -3 -29 77 4841 -783 0.19 -1.96 1.0000 -3 3 29 77 3887 -3433 0.19 1.96 1.0000 0 0 0 77 0 0 0.19 1.96 1.0000 ; _shelx_hkl_checksum 97051 _database_code_depnum_ccdc_archive 'CCDC 971182' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_klat880 # start Validation Reply Form _vrf_RINTA01_klat880 ; PROBLEM: The value of Rint is greater than 0.25 RESPONSE: This compound consistently yielded weakly diffracting crystals. The data herewith represents the best of several trials. ; _vrf_PLAT020_klat880 ; PROBLEM: The value of Rint is greater than 0.12 ......... 0.324 RESPONSE: see response to RINTA01 ; _vrf_PLAT026_klat880 ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 30 % RESPONSE: see response to RINTA01 ; _vrf_PLAT220_klat880 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.1 Ratio RESPONSE: Slight but unresolvable disorder in the isopropyl groups leads to larger C Ueq range. ; # end Validation Reply Form _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H58 Cr N4' _chemical_formula_weight 791.02 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' Cr Cr 0.3209 0.6236 '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/n' _space_group_name_Hall '-P 2yn' _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+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.213(3) _cell_length_b 23.838(8) _cell_length_c 18.280(6) _cell_angle_alpha 90 _cell_angle_beta 97.142(6) _cell_angle_gamma 90 _cell_volume 4416(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 511 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 14.22 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.190 _exptl_crystal_F_000 1688 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 0.298 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.794493 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'APEX2 (Bruker, 2007)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 51266 _diffrn_reflns_av_unetI/netI 0.3237 _diffrn_reflns_av_R_equivalents 0.3239 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.045 _diffrn_reflns_theta_max 28.449 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 11097 _reflns_number_gt 3358 _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 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ? ; _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^)+(0.0027P)^2^] 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 none _refine_ls_extinction_coef . _refine_ls_number_reflns 11097 _refine_ls_number_parameters 522 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3023 _refine_ls_R_factor_gt 0.0962 _refine_ls_wR_factor_ref 0.1202 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _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 Cr1 Cr 0.24265(8) 0.11215(3) 0.21406(5) 0.0386(2) Uani 1 1 d . . . . . N1 N 0.1247(4) 0.12326(15) 0.2853(2) 0.0334(10) Uani 1 1 d . . . . . N2 N 0.1104(4) 0.13610(15) 0.1400(2) 0.0367(11) Uani 1 1 d . . . . . N3 N 0.3510(4) 0.04788(15) 0.2117(2) 0.0357(11) Uani 1 1 d . . . . . N4 N 0.4012(4) 0.15355(17) 0.2192(2) 0.0420(12) Uani 1 1 d . . . . . C1 C 0.0268(5) 0.09658(19) 0.2418(3) 0.0390(14) Uani 1 1 d . . . . . H1 H -0.0355 0.0741 0.2628 0.047 Uiso 1 1 calc R U . . . C2 C 0.0195(4) 0.10272(19) 0.1662(3) 0.0363(13) Uani 1 1 d . . . . . H2 H -0.0468 0.0842 0.1338 0.044 Uiso 1 1 calc R U . . . C3 C 0.1537(5) 0.0886(2) 0.4137(3) 0.0418(14) Uani 1 1 d . . . . . C4 C 0.1414(5) 0.0998(2) 0.4872(3) 0.0475(15) Uani 1 1 d . . . . . H4 H 0.1613 0.0711 0.5229 0.057 Uiso 1 1 calc R U . . . C5 C 0.1012(5) 0.1516(2) 0.5096(3) 0.0528(16) Uani 1 1 d . . . . . H5 H 0.0941 0.1584 0.5601 0.063 Uiso 1 1 calc R U . . . C6 C 0.0715(5) 0.1929(2) 0.4584(3) 0.0530(16) Uani 1 1 d . . . . . H6 H 0.0431 0.2284 0.4740 0.064 Uiso 1 1 calc R U . . . C7 C 0.0818(5) 0.1844(2) 0.3845(3) 0.0410(14) Uani 1 1 d . . . . . C8 C 0.1198(4) 0.1315(2) 0.3627(3) 0.0339(13) Uani 1 1 d . . . . . C9 C 0.1959(5) 0.0309(2) 0.3926(3) 0.0518(16) Uani 1 1 d . . . . . H9 H 0.2203 0.0329 0.3414 0.062 Uiso 1 1 calc R U . . . C10 C 0.3143(5) 0.0091(2) 0.4426(3) 0.0669(18) Uani 1 1 d . . . . . H10A H 0.3857 0.0368 0.4454 0.100 Uiso 1 1 calc R U . . . H10B H 0.3442 -0.0262 0.4227 0.100 Uiso 1 1 calc R U . . . H10C H 0.2897 0.0025 0.4920 0.100 Uiso 1 1 calc R U . . . C11 C 0.0830(5) -0.0111(2) 0.3926(3) 0.0733(19) Uani 1 1 d . . . . . H11A H 0.0631 -0.0167 0.4432 0.110 Uiso 1 1 calc R U . . . H11B H 0.1090 -0.0470 0.3725 0.110 Uiso 1 1 calc R U . . . H11C H 0.0045 0.0033 0.3621 0.110 Uiso 1 1 calc R U . . . C12 C 0.0474(5) 0.2315(2) 0.3309(3) 0.0481(15) Uani 1 1 d . . . . . H12 H 0.0620 0.2176 0.2810 0.058 Uiso 1 1 calc R U . . . C13 C 0.1373(6) 0.2824(2) 0.3483(3) 0.095(2) Uani 1 1 d . . . . . H13A H 0.1248 0.2973 0.3968 0.142 Uiso 1 1 calc R U . . . H13B H 0.1152 0.3113 0.3107 0.142 Uiso 1 1 calc R U . . . H13C H 0.2296 0.2710 0.3483 0.142 Uiso 1 1 calc R U . . . C14 C -0.0946(5) 0.2493(2) 0.3267(3) 0.085(2) Uani 1 1 d . . . . . H14A H -0.1516 0.2188 0.3055 0.128 Uiso 1 1 calc R U . . . H14B H -0.1091 0.2827 0.2956 0.128 Uiso 1 1 calc R U . . . H14C H -0.1157 0.2579 0.3764 0.128 Uiso 1 1 calc R U . . . C15 C 0.1634(5) 0.1478(2) 0.0129(3) 0.0435(14) Uani 1 1 d . . . . . C16 C 0.1378(5) 0.1750(2) -0.0543(3) 0.0523(16) Uani 1 1 d . . . . . H16 H 0.1905 0.1666 -0.0922 0.063 Uiso 1 1 calc R U . . . C17 C 0.0391(6) 0.2136(2) -0.0674(3) 0.0531(16) Uani 1 1 d . . . . . H17 H 0.0227 0.2314 -0.1141 0.064 Uiso 1 1 calc R U . . . C18 C -0.0359(5) 0.2262(2) -0.0128(3) 0.0509(16) Uani 1 1 d . . . . . H18 H -0.1044 0.2532 -0.0223 0.061 Uiso 1 1 calc R U . . . C19 C -0.0150(5) 0.2009(2) 0.0559(3) 0.0381(13) Uani 1 1 d . . . . . C20 C 0.0857(5) 0.1608(2) 0.0689(3) 0.0398(14) Uani 1 1 d . . . . . C21 C 0.2749(6) 0.1051(3) 0.0227(3) 0.078(2) Uani 1 1 d . . . . . H21 H 0.2734 0.0869 0.0719 0.093 Uiso 1 1 calc R U . . . C22 C 0.2594(8) 0.0600(3) -0.0343(4) 0.170(5) Uani 1 1 d . . . . . H22A H 0.1766 0.0398 -0.0314 0.255 Uiso 1 1 calc R U . . . H22B H 0.3336 0.0338 -0.0255 0.255 Uiso 1 1 calc R U . . . H22C H 0.2579 0.0767 -0.0834 0.255 Uiso 1 1 calc R U . . . C24 C -0.1001(5) 0.2185(2) 0.1141(3) 0.0519(16) Uani 1 1 d . . . . . H24 H -0.0610 0.2019 0.1621 0.062 Uiso 1 1 calc R U . . . C25 C -0.2407(5) 0.1945(2) 0.0956(3) 0.0694(19) Uani 1 1 d . . . . . H25A H -0.2792 0.2081 0.0471 0.104 Uiso 1 1 calc R U . . . H25B H -0.2955 0.2068 0.1330 0.104 Uiso 1 1 calc R U . . . H25C H -0.2367 0.1535 0.0951 0.104 Uiso 1 1 calc R U . . . C26 C -0.1039(5) 0.2824(2) 0.1238(3) 0.075(2) Uani 1 1 d . . . . . H26A H -0.0136 0.2968 0.1342 0.113 Uiso 1 1 calc R U . . . H26B H -0.1530 0.2916 0.1650 0.113 Uiso 1 1 calc R U . . . H26C H -0.1474 0.2996 0.0786 0.113 Uiso 1 1 calc R U . . . C27 C 0.4914(5) 0.0603(2) 0.2071(3) 0.0466(15) Uani 1 1 d . . . . . H27 H 0.5030 0.0627 0.1537 0.056 Uiso 1 1 calc R U . . . C28 C 0.5189(4) 0.1194(2) 0.2410(3) 0.0383(13) Uani 1 1 d . . . . . H28 H 0.5907 0.1360 0.2153 0.046 Uiso 1 1 calc R U . . . C29 C 0.5560(6) -0.0150(2) 0.2999(3) 0.0601(17) Uani 1 1 d . . . . . H29 H 0.4760 -0.0079 0.3199 0.072 Uiso 1 1 calc R U . . . C30 C 0.6401(6) -0.0561(2) 0.3313(3) 0.0683(19) Uani 1 1 d . . . . . H30 H 0.6184 -0.0773 0.3722 0.082 Uiso 1 1 calc R U . . . C31 C 0.7546(7) -0.0658(2) 0.3025(4) 0.071(2) Uani 1 1 d . . . . . H31 H 0.8147 -0.0930 0.3251 0.086 Uiso 1 1 calc R U . . . C32 C 0.7850(6) -0.0376(3) 0.2427(4) 0.069(2) Uani 1 1 d . . . . . H32 H 0.8643 -0.0459 0.2227 0.083 Uiso 1 1 calc R U . . . C33 C 0.7000(6) 0.0034(2) 0.2106(3) 0.0574(17) Uani 1 1 d . . . . . H33 H 0.7199 0.0230 0.1682 0.069 Uiso 1 1 calc R U . . . C34 C 0.5846(5) 0.0154(2) 0.2415(3) 0.0378(14) Uani 1 1 d . . . . . C35 C 0.4876(6) 0.1313(2) 0.3738(3) 0.0556(17) Uani 1 1 d . . . . . H35 H 0.3957 0.1362 0.3594 0.067 Uiso 1 1 calc R U . . . C36 C 0.5361(7) 0.1343(2) 0.4475(3) 0.0679(19) Uani 1 1 d . . . . . H36 H 0.4771 0.1412 0.4828 0.081 Uiso 1 1 calc R U . . . C37 C 0.6677(7) 0.1276(2) 0.4708(3) 0.073(2) Uani 1 1 d . . . . . H37 H 0.7004 0.1298 0.5217 0.088 Uiso 1 1 calc R U . . . C38 C 0.7526(6) 0.1173(2) 0.4186(4) 0.0690(19) Uani 1 1 d . . . . . H38 H 0.8445 0.1125 0.4331 0.083 Uiso 1 1 calc R U . . . C39 C 0.7010(6) 0.1144(2) 0.3454(3) 0.0565(16) Uani 1 1 d . . . . . H39 H 0.7591 0.1071 0.3098 0.068 Uiso 1 1 calc R U . . . C40 C 0.5674(5) 0.1216(2) 0.3214(3) 0.0406(14) Uani 1 1 d . . . . . C41 C 0.3626(5) -0.0274(2) 0.1193(3) 0.0557(17) Uani 1 1 d . . . . . H41 H 0.4470 -0.0151 0.1093 0.067 Uiso 1 1 calc R U . . . C42 C 0.3010(6) -0.0721(2) 0.0795(3) 0.0654(19) Uani 1 1 d . . . . . H42 H 0.3431 -0.0895 0.0418 0.078 Uiso 1 1 calc R U . . . C43 C 0.1795(6) -0.0911(2) 0.0943(3) 0.0661(19) Uani 1 1 d . . . . . H43 H 0.1365 -0.1209 0.0663 0.079 Uiso 1 1 calc R U . . . C44 C 0.1228(5) -0.0670(2) 0.1491(3) 0.0612(18) Uani 1 1 d . . . . . H44 H 0.0404 -0.0805 0.1607 0.073 Uiso 1 1 calc R U . . . C45 C 0.1830(5) -0.0230(2) 0.1880(3) 0.0510(16) Uani 1 1 d . . . . . H45 H 0.1408 -0.0073 0.2266 0.061 Uiso 1 1 calc R U . . . C46 C 0.3008(5) -0.0005(2) 0.1743(3) 0.0417(14) Uani 1 1 d . . . . . C47 C 0.5343(5) 0.2386(2) 0.2396(3) 0.0426(14) Uani 1 1 d . . . . . H47 H 0.6089 0.2174 0.2598 0.051 Uiso 1 1 calc R U . . . C48 C 0.5446(5) 0.2966(2) 0.2331(3) 0.0506(16) Uani 1 1 d . . . . . H48 H 0.6266 0.3143 0.2491 0.061 Uiso 1 1 calc R U . . . C49 C 0.4407(6) 0.3287(2) 0.2045(3) 0.0622(18) Uani 1 1 d . . . . . H49 H 0.4496 0.3682 0.1999 0.075 Uiso 1 1 calc R U . . . C50 C 0.3211(6) 0.3025(2) 0.1822(3) 0.076(2) Uani 1 1 d . . . . . H50 H 0.2465 0.3242 0.1634 0.091 Uiso 1 1 calc R U . . . C51 C 0.3102(5) 0.2451(2) 0.1872(3) 0.0653(19) Uani 1 1 d . . . . . H51 H 0.2282 0.2278 0.1702 0.078 Uiso 1 1 calc R U . . . C52 C 0.4156(5) 0.2115(2) 0.2166(3) 0.0425(14) Uani 1 1 d . . . . . C23 C 0.4071(6) 0.1353(4) 0.0241(4) 0.167(4) Uani 1 1 d . . . . . H23A H 0.4084 0.1564 -0.0218 0.250 Uiso 1 1 calc R U . . . H23B H 0.4787 0.1076 0.0290 0.250 Uiso 1 1 calc R U . . . H23C H 0.4190 0.1612 0.0661 0.250 Uiso 1 1 calc R U . . . 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 Cr1 0.0318(5) 0.0418(5) 0.0422(6) 0.0030(5) 0.0049(4) 0.0010(4) N1 0.029(3) 0.043(3) 0.028(3) -0.002(2) 0.001(2) -0.001(2) N2 0.035(3) 0.043(3) 0.032(3) 0.013(2) 0.006(2) 0.001(2) N3 0.028(3) 0.034(3) 0.046(3) -0.001(2) 0.006(2) -0.003(2) N4 0.030(3) 0.035(3) 0.060(3) 0.006(2) 0.002(2) -0.002(2) C1 0.029(3) 0.045(4) 0.044(4) 0.006(3) 0.011(3) 0.002(3) C2 0.029(3) 0.044(4) 0.034(3) 0.004(3) -0.002(3) 0.007(3) C3 0.040(4) 0.053(4) 0.032(4) -0.004(3) 0.003(3) -0.004(3) C4 0.043(4) 0.052(4) 0.047(4) 0.007(3) 0.003(3) -0.012(3) C5 0.061(4) 0.066(5) 0.032(4) -0.008(3) 0.006(3) -0.009(3) C6 0.050(4) 0.057(4) 0.048(4) -0.004(3) -0.008(3) 0.005(3) C7 0.031(3) 0.051(4) 0.038(4) 0.001(3) -0.005(3) 0.000(3) C8 0.025(3) 0.045(4) 0.030(3) -0.002(3) 0.001(3) -0.005(3) C9 0.058(4) 0.058(4) 0.039(4) 0.007(3) 0.005(3) -0.001(3) C10 0.063(5) 0.066(4) 0.073(5) 0.019(4) 0.014(4) 0.011(3) C11 0.089(5) 0.063(5) 0.066(5) -0.007(4) 0.004(4) -0.010(4) C12 0.051(4) 0.048(4) 0.044(4) -0.004(3) -0.001(3) 0.001(3) C13 0.136(7) 0.062(5) 0.081(6) 0.021(4) -0.007(5) -0.034(4) C14 0.071(5) 0.092(5) 0.091(6) 0.018(4) 0.002(4) 0.029(4) C15 0.038(4) 0.057(4) 0.036(4) 0.009(3) 0.006(3) 0.006(3) C16 0.046(4) 0.068(5) 0.044(4) 0.001(3) 0.013(3) -0.003(3) C17 0.074(5) 0.055(4) 0.032(4) 0.013(3) 0.013(3) -0.002(3) C18 0.064(4) 0.047(4) 0.041(4) 0.008(3) 0.004(3) 0.003(3) C19 0.046(4) 0.038(4) 0.029(3) -0.002(3) 0.003(3) -0.001(3) C20 0.037(4) 0.044(4) 0.039(4) 0.002(3) 0.006(3) 0.001(3) C21 0.066(5) 0.108(6) 0.062(5) 0.022(4) 0.021(4) 0.032(4) C22 0.288(12) 0.159(8) 0.060(6) -0.018(5) 0.008(6) 0.161(8) C24 0.053(4) 0.060(4) 0.041(4) 0.007(3) 0.000(3) 0.015(3) C25 0.066(5) 0.081(5) 0.064(5) 0.016(4) 0.023(4) 0.015(4) C26 0.096(5) 0.062(5) 0.068(5) -0.005(4) 0.012(4) 0.031(4) C27 0.046(4) 0.043(4) 0.050(4) -0.006(3) 0.002(3) -0.007(3) C28 0.024(3) 0.037(3) 0.053(4) 0.001(3) 0.002(3) 0.000(3) C29 0.055(4) 0.060(5) 0.064(5) 0.001(4) 0.001(4) 0.011(4) C30 0.063(5) 0.067(5) 0.071(5) 0.002(4) -0.006(4) 0.009(4) C31 0.067(5) 0.065(5) 0.078(6) -0.014(4) -0.009(4) 0.018(4) C32 0.046(4) 0.087(6) 0.072(5) -0.017(4) -0.002(4) 0.021(4) C33 0.051(4) 0.058(4) 0.062(4) -0.011(3) 0.001(4) 0.008(3) C34 0.029(3) 0.027(3) 0.055(4) -0.004(3) -0.002(3) 0.008(3) C35 0.061(5) 0.046(4) 0.059(5) -0.001(3) 0.005(4) 0.000(3) C36 0.093(6) 0.065(5) 0.047(5) -0.006(4) 0.013(4) 0.009(4) C37 0.098(6) 0.062(5) 0.053(5) 0.010(4) -0.018(5) -0.006(4) C38 0.062(5) 0.059(4) 0.081(6) 0.006(4) -0.009(4) 0.004(4) C39 0.051(4) 0.059(4) 0.058(5) -0.001(4) 0.000(3) -0.003(3) C40 0.035(4) 0.037(3) 0.050(4) 0.004(3) 0.005(3) 0.003(3) C41 0.044(4) 0.053(4) 0.073(5) -0.020(3) 0.014(4) -0.006(3) C42 0.063(5) 0.058(4) 0.078(5) -0.033(4) 0.020(4) -0.009(3) C43 0.048(4) 0.055(4) 0.095(6) -0.019(4) 0.009(4) -0.024(3) C44 0.048(4) 0.057(4) 0.083(5) -0.031(4) 0.028(4) -0.010(3) C45 0.044(4) 0.046(4) 0.065(4) -0.012(3) 0.018(3) -0.002(3) C46 0.035(4) 0.035(4) 0.055(4) -0.007(3) 0.006(3) 0.003(3) C47 0.046(4) 0.038(4) 0.045(4) 0.000(3) 0.007(3) 0.001(3) C48 0.049(4) 0.052(4) 0.050(4) 0.000(3) 0.004(3) -0.007(3) C49 0.069(5) 0.039(4) 0.079(5) 0.008(3) 0.012(4) -0.004(4) C50 0.069(5) 0.049(5) 0.106(6) 0.025(4) -0.009(4) 0.002(4) C51 0.042(4) 0.042(4) 0.107(6) 0.019(4) -0.008(4) 0.000(3) C52 0.032(4) 0.045(4) 0.052(4) 0.010(3) 0.010(3) 0.000(3) C23 0.056(6) 0.329(13) 0.123(8) 0.107(8) 0.040(5) 0.060(7) _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 Cr1 N2 1.878(4) . ? Cr1 N4 1.889(4) . ? Cr1 N3 1.893(4) . ? Cr1 N1 1.899(4) . ? Cr1 C2 2.348(5) . ? Cr1 C1 2.352(5) . ? N1 C1 1.356(5) . ? N1 C8 1.435(5) . ? N2 C2 1.354(5) . ? N2 C20 1.420(6) . ? N3 C46 1.405(5) . ? N3 C27 1.477(5) . ? N4 C52 1.391(5) . ? N4 C28 1.465(5) . ? C1 C2 1.383(6) . ? C3 C4 1.392(6) . ? C3 C8 1.398(6) . ? C3 C9 1.505(6) . ? C4 C5 1.377(6) . ? C5 C6 1.366(6) . ? C6 C7 1.383(6) . ? C7 C8 1.392(6) . ? C7 C12 1.504(6) . ? C9 C10 1.515(6) . ? C9 C11 1.528(6) . ? C12 C14 1.504(6) . ? C12 C13 1.529(6) . ? C15 C16 1.385(6) . ? C15 C20 1.405(6) . ? C15 C21 1.521(7) . ? C16 C17 1.363(6) . ? C17 C18 1.365(6) . ? C18 C19 1.387(6) . ? C19 C20 1.404(6) . ? C19 C24 1.514(6) . ? C21 C22 1.493(8) . ? C21 C23 1.527(8) . ? C24 C26 1.534(6) . ? C24 C25 1.543(6) . ? C27 C34 1.516(6) . ? C27 C28 1.551(6) . ? C28 C40 1.492(6) . ? C29 C34 1.352(6) . ? C29 C30 1.380(7) . ? C30 C31 1.360(7) . ? C31 C32 1.352(7) . ? C32 C33 1.388(7) . ? C33 C34 1.398(6) . ? C35 C40 1.353(6) . ? C35 C36 1.379(7) . ? C36 C37 1.368(7) . ? C37 C38 1.388(7) . ? C38 C39 1.377(7) . ? C39 C40 1.391(6) . ? C41 C42 1.394(6) . ? C41 C46 1.406(6) . ? C42 C43 1.380(6) . ? C43 C44 1.347(6) . ? C44 C45 1.369(6) . ? C45 C46 1.368(6) . ? C47 C48 1.393(6) . ? C47 C52 1.392(6) . ? C48 C49 1.359(6) . ? C49 C50 1.388(7) . ? C50 C51 1.375(6) . ? C51 C52 1.394(6) . ? 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 N2 Cr1 N4 114.34(17) . . ? N2 Cr1 N3 126.85(17) . . ? N4 Cr1 N3 85.64(17) . . ? N2 Cr1 N1 89.48(16) . . ? N4 Cr1 N1 120.41(17) . . ? N3 Cr1 N1 123.41(16) . . ? N2 Cr1 C2 35.20(14) . . ? N4 Cr1 C2 148.75(17) . . ? N3 Cr1 C2 117.20(17) . . ? N1 Cr1 C2 66.42(16) . . ? N2 Cr1 C1 66.04(16) . . ? N4 Cr1 C1 153.19(17) . . ? N3 Cr1 C1 116.31(16) . . ? N1 Cr1 C1 35.20(14) . . ? C2 Cr1 C1 34.21(14) . . ? C1 N1 C8 121.9(4) . . ? C1 N1 Cr1 90.9(3) . . ? C8 N1 Cr1 142.9(3) . . ? C2 N2 C20 121.0(4) . . ? C2 N2 Cr1 91.7(3) . . ? C20 N2 Cr1 144.6(3) . . ? C46 N3 C27 115.8(4) . . ? C46 N3 Cr1 119.7(3) . . ? C27 N3 Cr1 114.4(3) . . ? C52 N4 C28 118.3(4) . . ? C52 N4 Cr1 127.7(3) . . ? C28 N4 Cr1 113.1(3) . . ? N1 C1 C2 118.8(5) . . ? N1 C1 Cr1 53.8(2) . . ? C2 C1 Cr1 72.8(3) . . ? N2 C2 C1 117.4(5) . . ? N2 C2 Cr1 53.1(2) . . ? C1 C2 Cr1 73.0(3) . . ? C4 C3 C8 117.3(5) . . ? C4 C3 C9 119.1(5) . . ? C8 C3 C9 123.5(5) . . ? C5 C4 C3 121.6(5) . . ? C6 C5 C4 119.5(5) . . ? C5 C6 C7 121.7(5) . . ? C6 C7 C8 118.1(5) . . ? C6 C7 C12 119.1(5) . . ? C8 C7 C12 122.7(5) . . ? C3 C8 C7 121.7(5) . . ? C3 C8 N1 121.5(5) . . ? C7 C8 N1 116.8(5) . . ? C3 C9 C10 113.1(5) . . ? C3 C9 C11 111.1(5) . . ? C10 C9 C11 108.7(4) . . ? C14 C12 C7 112.9(4) . . ? C14 C12 C13 109.8(5) . . ? C7 C12 C13 111.8(4) . . ? C16 C15 C20 118.8(5) . . ? C16 C15 C21 118.3(5) . . ? C20 C15 C21 122.9(5) . . ? C17 C16 C15 121.7(5) . . ? C16 C17 C18 119.4(5) . . ? C17 C18 C19 122.0(5) . . ? C18 C19 C20 118.5(5) . . ? C18 C19 C24 118.6(5) . . ? C20 C19 C24 122.9(5) . . ? C15 C20 C19 119.7(5) . . ? C15 C20 N2 121.6(5) . . ? C19 C20 N2 118.7(5) . . ? C22 C21 C15 112.8(6) . . ? C22 C21 C23 111.6(6) . . ? C15 C21 C23 109.5(6) . . ? C19 C24 C26 112.5(4) . . ? C19 C24 C25 110.1(4) . . ? C26 C24 C25 110.9(4) . . ? N3 C27 C34 113.4(4) . . ? N3 C27 C28 106.7(4) . . ? C34 C27 C28 113.8(4) . . ? N4 C28 C40 114.2(4) . . ? N4 C28 C27 107.1(4) . . ? C40 C28 C27 116.5(4) . . ? C34 C29 C30 121.6(6) . . ? C31 C30 C29 118.7(6) . . ? C32 C31 C30 121.5(7) . . ? C31 C32 C33 119.8(6) . . ? C32 C33 C34 119.2(6) . . ? C29 C34 C33 119.0(5) . . ? C29 C34 C27 121.3(5) . . ? C33 C34 C27 119.6(5) . . ? C40 C35 C36 121.8(6) . . ? C35 C36 C37 121.2(6) . . ? C36 C37 C38 118.7(6) . . ? C39 C38 C37 118.7(6) . . ? C38 C39 C40 122.9(6) . . ? C35 C40 C39 116.8(5) . . ? C35 C40 C28 123.3(5) . . ? C39 C40 C28 120.0(5) . . ? C42 C41 C46 120.6(5) . . ? C41 C42 C43 120.4(5) . . ? C44 C43 C42 119.1(5) . . ? C43 C44 C45 120.4(5) . . ? C44 C45 C46 123.6(5) . . ? C45 C46 C41 115.7(5) . . ? C45 C46 N3 120.6(5) . . ? C41 C46 N3 123.7(5) . . ? C48 C47 C52 120.5(5) . . ? C49 C48 C47 121.8(5) . . ? C48 C49 C50 118.4(5) . . ? C51 C50 C49 120.3(6) . . ? C50 C51 C52 122.1(5) . . ? C47 C52 N4 122.9(5) . . ? C47 C52 C51 116.8(5) . . ? N4 C52 C51 120.3(5) . . ? _refine_diff_density_max 0.314 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.062 _shelxl_version_number 2013-2 _shelx_res_file ; TITL klat880 in P2(1)/n CELL 0.71073 10.2130 23.8376 18.2799 90.000 97.142 90.000 ZERR 4.00 0.0034 0.0079 0.0061 0.000 0.006 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N Cr UNIT 208 232 16 4 L.S. 20 ACTA 50 BOND FMAP 2 PLAN 20 OMIT 0 1 1 TEMP -73 OMIT 0 2 0 WGHT 0.002700 FVAR 0.35760 CR1 4 0.242646 0.112148 0.214060 11.00000 0.03184 0.04180 = 0.04216 0.00304 0.00487 0.00103 N1 3 0.124672 0.123263 0.285288 11.00000 0.02904 0.04265 = 0.02786 -0.00151 0.00063 -0.00133 N2 3 0.110414 0.136101 0.140028 11.00000 0.03527 0.04340 = 0.03184 0.01265 0.00587 0.00122 N3 3 0.350991 0.047884 0.211731 11.00000 0.02845 0.03352 = 0.04552 -0.00055 0.00648 -0.00334 N4 3 0.401229 0.153554 0.219192 11.00000 0.02988 0.03503 = 0.06038 0.00619 0.00224 -0.00193 C1 1 0.026813 0.096576 0.241778 11.00000 0.02943 0.04503 = 0.04404 0.00556 0.01102 0.00231 AFIX 43 H1 2 -0.035541 0.074079 0.262849 11.00000 -1.20000 AFIX 0 C2 1 0.019481 0.102721 0.166173 11.00000 0.02900 0.04401 = 0.03421 0.00444 -0.00230 0.00739 AFIX 43 H2 2 -0.046783 0.084242 0.133808 11.00000 -1.20000 AFIX 0 C3 1 0.153692 0.088602 0.413673 11.00000 0.04028 0.05308 = 0.03154 -0.00401 0.00287 -0.00420 C4 1 0.141440 0.099838 0.487236 11.00000 0.04278 0.05206 = 0.04702 0.00719 0.00288 -0.01201 AFIX 43 H4 2 0.161322 0.071123 0.522928 11.00000 -1.20000 AFIX 0 C5 1 0.101208 0.151551 0.509555 11.00000 0.06084 0.06593 = 0.03175 -0.00815 0.00608 -0.00905 AFIX 43 H5 2 0.094143 0.158423 0.560106 11.00000 -1.20000 AFIX 0 C6 1 0.071549 0.192875 0.458431 11.00000 0.05036 0.05728 = 0.04779 -0.00392 -0.00804 0.00538 AFIX 43 H6 2 0.043149 0.228381 0.474040 11.00000 -1.20000 AFIX 0 C7 1 0.081792 0.184367 0.384536 11.00000 0.03117 0.05108 = 0.03820 0.00094 -0.00533 0.00014 C8 1 0.119840 0.131479 0.362677 11.00000 0.02524 0.04549 = 0.03035 -0.00237 0.00147 -0.00484 C9 1 0.195853 0.030913 0.392591 11.00000 0.05786 0.05798 = 0.03925 0.00676 0.00508 -0.00051 AFIX 13 H9 2 0.220307 0.032949 0.341358 11.00000 -1.20000 AFIX 0 C10 1 0.314332 0.009065 0.442612 11.00000 0.06349 0.06559 = 0.07306 0.01886 0.01445 0.01118 AFIX 137 H10A 2 0.385719 0.036751 0.445435 11.00000 -1.50000 H10B 2 0.344234 -0.026215 0.422718 11.00000 -1.50000 H10C 2 0.289664 0.002530 0.492030 11.00000 -1.50000 AFIX 0 C11 1 0.083017 -0.011149 0.392593 11.00000 0.08872 0.06340 = 0.06631 -0.00660 0.00396 -0.01044 AFIX 137 H11A 2 0.063106 -0.016678 0.443174 11.00000 -1.50000 H11B 2 0.109005 -0.047022 0.372531 11.00000 -1.50000 H11C 2 0.004549 0.003269 0.362074 11.00000 -1.50000 AFIX 0 C12 1 0.047433 0.231530 0.330935 11.00000 0.05052 0.04830 = 0.04396 -0.00373 -0.00063 0.00068 AFIX 13 H12 2 0.061952 0.217624 0.280963 11.00000 -1.20000 AFIX 0 C13 1 0.137335 0.282356 0.348251 11.00000 0.13556 0.06193 = 0.08098 0.02109 -0.00692 -0.03438 AFIX 137 H13A 2 0.124815 0.297322 0.396829 11.00000 -1.50000 H13B 2 0.115238 0.311330 0.310710 11.00000 -1.50000 H13C 2 0.229561 0.270985 0.348312 11.00000 -1.50000 AFIX 0 C14 1 -0.094583 0.249275 0.326737 11.00000 0.07066 0.09193 = 0.09086 0.01781 0.00197 0.02857 AFIX 137 H14A 2 -0.151568 0.218807 0.305528 11.00000 -1.50000 H14B 2 -0.109065 0.282703 0.295573 11.00000 -1.50000 H14C 2 -0.115676 0.257881 0.376374 11.00000 -1.50000 AFIX 0 C15 1 0.163395 0.147837 0.012918 11.00000 0.03803 0.05650 = 0.03628 0.00945 0.00585 0.00588 C16 1 0.137848 0.175035 -0.054271 11.00000 0.04634 0.06827 = 0.04402 0.00144 0.01262 -0.00314 AFIX 43 H16 2 0.190482 0.166623 -0.092197 11.00000 -1.20000 AFIX 0 C17 1 0.039131 0.213563 -0.067388 11.00000 0.07431 0.05453 = 0.03192 0.01347 0.01268 -0.00171 AFIX 43 H17 2 0.022695 0.231443 -0.114073 11.00000 -1.20000 AFIX 0 C18 1 -0.035886 0.226220 -0.012841 11.00000 0.06413 0.04694 = 0.04104 0.00821 0.00405 0.00287 AFIX 43 H18 2 -0.104441 0.253167 -0.022267 11.00000 -1.20000 AFIX 0 C19 1 -0.015041 0.200923 0.055937 11.00000 0.04643 0.03811 = 0.02930 -0.00210 0.00279 -0.00117 C20 1 0.085736 0.160765 0.068922 11.00000 0.03667 0.04411 = 0.03882 0.00198 0.00556 0.00090 C21 1 0.274868 0.105142 0.022722 11.00000 0.06572 0.10820 = 0.06233 0.02237 0.02109 0.03210 AFIX 13 H21 2 0.273360 0.086906 0.071876 11.00000 -1.20000 AFIX 0 C22 1 0.259407 0.059991 -0.034296 11.00000 0.28837 0.15915 = 0.05993 -0.01762 0.00826 0.16072 AFIX 137 H22A 2 0.176571 0.039831 -0.031433 11.00000 -1.50000 H22B 2 0.333586 0.033760 -0.025531 11.00000 -1.50000 H22C 2 0.257913 0.076742 -0.083351 11.00000 -1.50000 AFIX 0 C24 1 -0.100131 0.218548 0.114081 11.00000 0.05336 0.05956 = 0.04134 0.00676 0.00049 0.01505 AFIX 13 H24 2 -0.060978 0.201918 0.162091 11.00000 -1.20000 AFIX 0 C25 1 -0.240692 0.194547 0.095638 11.00000 0.06634 0.08098 = 0.06443 0.01552 0.02269 0.01485 AFIX 137 H25A 2 -0.279199 0.208099 0.047071 11.00000 -1.50000 H25B 2 -0.295487 0.206824 0.133003 11.00000 -1.50000 H25C 2 -0.236651 0.153476 0.095127 11.00000 -1.50000 AFIX 0 C26 1 -0.103886 0.282401 0.123846 11.00000 0.09608 0.06204 = 0.06780 -0.00543 0.01199 0.03073 AFIX 137 H26A 2 -0.013595 0.296793 0.134174 11.00000 -1.50000 H26B 2 -0.153015 0.291568 0.165037 11.00000 -1.50000 H26C 2 -0.147447 0.299647 0.078568 11.00000 -1.50000 AFIX 0 C27 1 0.491435 0.060325 0.207084 11.00000 0.04560 0.04330 = 0.04999 -0.00567 0.00215 -0.00667 AFIX 13 H27 2 0.503008 0.062720 0.153650 11.00000 -1.20000 AFIX 0 C28 1 0.518922 0.119448 0.241007 11.00000 0.02388 0.03730 = 0.05292 0.00114 0.00204 0.00015 AFIX 13 H28 2 0.590659 0.136007 0.215253 11.00000 -1.20000 AFIX 0 C29 1 0.555969 -0.015016 0.299922 11.00000 0.05461 0.06025 = 0.06381 0.00103 0.00086 0.01054 AFIX 43 H29 2 0.476036 -0.007889 0.319882 11.00000 -1.20000 AFIX 0 C30 1 0.640109 -0.056140 0.331281 11.00000 0.06321 0.06688 = 0.07135 0.00208 -0.00555 0.00851 AFIX 43 H30 2 0.618435 -0.077290 0.372152 11.00000 -1.20000 AFIX 0 C31 1 0.754645 -0.065797 0.302543 11.00000 0.06660 0.06496 = 0.07799 -0.01353 -0.00906 0.01795 AFIX 43 H31 2 0.814731 -0.092966 0.325050 11.00000 -1.20000 AFIX 0 C32 1 0.784969 -0.037638 0.242702 11.00000 0.04562 0.08664 = 0.07196 -0.01715 -0.00237 0.02108 AFIX 43 H32 2 0.864272 -0.045887 0.222668 11.00000 -1.20000 AFIX 0 C33 1 0.699965 0.003353 0.210602 11.00000 0.05137 0.05760 = 0.06151 -0.01143 0.00065 0.00824 AFIX 43 H33 2 0.719950 0.023011 0.168162 11.00000 -1.20000 AFIX 0 C34 1 0.584555 0.015375 0.241473 11.00000 0.02934 0.02704 = 0.05506 -0.00378 -0.00243 0.00768 C35 1 0.487622 0.131317 0.373810 11.00000 0.06116 0.04578 = 0.05930 -0.00087 0.00472 0.00023 AFIX 43 H35 2 0.395703 0.136202 0.359444 11.00000 -1.20000 AFIX 0 C36 1 0.536126 0.134313 0.447542 11.00000 0.09333 0.06475 = 0.04660 -0.00589 0.01301 0.00917 AFIX 43 H36 2 0.477091 0.141184 0.482805 11.00000 -1.20000 AFIX 0 C37 1 0.667745 0.127567 0.470833 11.00000 0.09779 0.06188 = 0.05303 0.00991 -0.01819 -0.00636 AFIX 43 H37 2 0.700432 0.129836 0.521722 11.00000 -1.20000 AFIX 0 C38 1 0.752578 0.117340 0.418596 11.00000 0.06245 0.05851 = 0.08134 0.00567 -0.00923 0.00408 AFIX 43 H38 2 0.844475 0.112468 0.433051 11.00000 -1.20000 AFIX 0 C39 1 0.700965 0.114394 0.345438 11.00000 0.05128 0.05866 = 0.05794 -0.00106 -0.00011 -0.00348 AFIX 43 H39 2 0.759130 0.107114 0.309842 11.00000 -1.20000 AFIX 0 C40 1 0.567384 0.121609 0.321365 11.00000 0.03546 0.03670 = 0.04961 0.00391 0.00482 0.00313 C41 1 0.362553 -0.027440 0.119332 11.00000 0.04356 0.05255 = 0.07286 -0.01985 0.01441 -0.00567 AFIX 43 H41 2 0.446971 -0.015131 0.109287 11.00000 -1.20000 AFIX 0 C42 1 0.301046 -0.072078 0.079460 11.00000 0.06347 0.05771 = 0.07773 -0.03292 0.01991 -0.00853 AFIX 43 H42 2 0.343062 -0.089473 0.041835 11.00000 -1.20000 AFIX 0 C43 1 0.179547 -0.091144 0.094305 11.00000 0.04832 0.05538 = 0.09457 -0.01876 0.00920 -0.02388 AFIX 43 H43 2 0.136532 -0.120904 0.066294 11.00000 -1.20000 AFIX 0 C44 1 0.122774 -0.066984 0.149052 11.00000 0.04840 0.05707 = 0.08305 -0.03139 0.02765 -0.01033 AFIX 43 H44 2 0.040396 -0.080534 0.160740 11.00000 -1.20000 AFIX 0 C45 1 0.183039 -0.023014 0.187971 11.00000 0.04421 0.04620 = 0.06547 -0.01249 0.01769 -0.00208 AFIX 43 H45 2 0.140755 -0.007282 0.226633 11.00000 -1.20000 AFIX 0 C46 1 0.300773 -0.000472 0.174278 11.00000 0.03522 0.03507 = 0.05480 -0.00682 0.00586 0.00262 C47 1 0.534331 0.238631 0.239567 11.00000 0.04565 0.03789 = 0.04462 0.00040 0.00724 0.00105 AFIX 43 H47 2 0.608879 0.217417 0.259833 11.00000 -1.20000 AFIX 0 C48 1 0.544642 0.296646 0.233105 11.00000 0.04896 0.05232 = 0.04985 -0.00042 0.00401 -0.00718 AFIX 43 H48 2 0.626626 0.314278 0.249122 11.00000 -1.20000 AFIX 0 C49 1 0.440670 0.328724 0.204522 11.00000 0.06858 0.03929 = 0.07924 0.00804 0.01175 -0.00357 AFIX 43 H49 2 0.449634 0.368191 0.199917 11.00000 -1.20000 AFIX 0 C50 1 0.321120 0.302452 0.182229 11.00000 0.06869 0.04938 = 0.10554 0.02510 -0.00934 0.00188 AFIX 43 H50 2 0.246461 0.324171 0.163417 11.00000 -1.20000 AFIX 0 C51 1 0.310207 0.245109 0.187241 11.00000 0.04174 0.04235 = 0.10732 0.01873 -0.00794 -0.00046 AFIX 43 H51 2 0.228234 0.227848 0.170185 11.00000 -1.20000 AFIX 0 C52 1 0.415617 0.211500 0.216556 11.00000 0.03240 0.04454 = 0.05179 0.00979 0.01007 0.00041 C23 1 0.407069 0.135280 0.024125 11.00000 0.05566 0.32925 = 0.12253 0.10710 0.04000 0.05994 AFIX 137 H23A 2 0.408376 0.156385 -0.021786 11.00000 -1.50000 H23B 2 0.478653 0.107638 0.028982 11.00000 -1.50000 H23C 2 0.419035 0.161161 0.066079 11.00000 -1.50000 AFIX 0 HKLF 4 REM klat880 in P2(1)/n REM R1 = 0.0962 for 3358 Fo > 4sig(Fo) and 0.3023 for all 11097 data REM 522 parameters refined using 0 restraints END WGHT 0.0459 0.0000 REM Highest difference peak 0.314, deepest hole -0.401, 1-sigma level 0.062 Q1 1 0.2386 0.1152 0.1366 11.00000 0.05 0.31 Q2 1 0.4004 0.1448 0.2839 11.00000 0.05 0.31 Q3 1 0.2598 0.1648 0.2815 11.00000 0.05 0.28 Q4 1 0.2783 0.1124 0.3620 11.00000 0.05 0.28 Q5 1 0.2785 0.0720 -0.0423 11.00000 0.05 0.27 Q6 1 0.4521 0.0559 0.2806 11.00000 0.05 0.27 Q7 1 0.2046 0.0016 0.1392 11.00000 0.05 0.26 Q8 1 -0.2586 0.3460 0.1398 11.00000 0.05 0.26 Q9 1 0.3004 -0.0360 0.2635 11.00000 0.05 0.25 Q10 1 0.2193 -0.0886 0.2355 11.00000 0.05 0.25 Q11 1 0.3637 0.0871 0.1589 11.00000 0.05 0.24 Q12 1 0.2030 0.1653 -0.1414 11.00000 0.05 0.24 Q13 1 0.2168 0.0661 0.0182 11.00000 0.05 0.24 Q14 1 0.5993 0.2143 0.2386 11.00000 0.05 0.23 Q15 1 0.4202 0.2020 -0.0430 11.00000 0.05 0.23 Q16 1 0.7671 0.1351 0.5149 11.00000 0.05 0.23 Q17 1 0.2589 0.1194 0.0170 11.00000 0.05 0.23 Q18 1 0.1698 0.1516 0.2012 11.00000 0.05 0.22 Q19 1 0.5831 0.2393 0.3160 11.00000 0.05 0.22 Q20 1 0.3638 0.2498 0.1142 11.00000 0.05 0.22 ; _shelx_res_checksum 34568 _shelx_hkl_file ; 1 0 0 0.99 6.86 -1 0 0 5.67 5.28 -1 0 0 1.62 5.54 -2 0 0 95.55 15.16 2 0 0 59.43 19.28 -2 0 0 75.36 24.81 -3 0 0 -6.95 6.63 3 0 0 24.35 18.20 -3 0 0 -9.57 17.98 4 0 0 -2.89 14.14 -4 0 0 5.96 9.85 -4 0 0 10.49 20.58 5 0 0 2.88 16.12 -5 0 0 -13.85 10.07 -5 0 0 30.80 26.23 6 0 0 395.42 40.36 -6 0 0 534.04 83.67 6 0 0 371.77 56.82 -7 0 0 16.86 23.74 7 0 0 21.24 23.15 7 0 0 -24.62 10.35 -8 0 0 117.20 56.97 8 0 0 94.12 37.41 -9 0 0 49.13 44.67 -9 0 0 0.68 20.13 -10 0 0 31.90 45.27 -11 0 0 -25.93 39.34 -12 0 0 16.92 50.00 -13 0 0 -38.78 48.31 0 -1 0 -1.05 0.70 0 -1 0 -0.37 0.79 0 1 0 0.58 0.69 1 -1 0 22.59 11.92 -1 1 0 13.01 9.35 -1 -1 0 -6.68 7.89 1 -1 0 8.87 5.75 1 1 0 -0.40 6.82 -1 -1 0 -3.20 6.90 -2 -1 0 813.64 51.35 2 -1 0 781.22 46.50 2 -1 0 824.51 31.89 2 1 0 767.28 40.07 -2 -1 0 769.41 38.17 -2 1 0 831.53 51.21 3 1 0 103.65 24.14 3 -1 0 95.14 29.07 -3 -1 0 100.36 19.43 -3 -1 0 51.16 26.62 -3 1 0 42.15 24.45 3 -1 0 83.77 16.06 4 -1 0 25.00 22.05 -4 -1 0 47.31 17.19 4 1 0 40.36 21.38 4 -1 0 13.73 9.94 -4 1 0 39.87 25.30 -4 -1 0 17.23 20.97 5 -1 0 113.84 19.88 -5 -1 0 65.32 33.48 5 1 0 60.32 26.51 -5 -1 0 40.54 18.09 -5 1 0 80.80 35.40 5 -1 0 110.37 34.20 6 1 0 28.65 20.88 -6 -1 0 65.01 36.37 6 -1 0 61.85 11.25 -6 1 0 66.10 35.33 6 -1 0 20.24 22.79 -6 -1 0 44.97 18.14 7 -1 0 -8.15 16.41 7 1 0 12.65 18.78 7 -1 0 2.21 9.45 -7 -1 0 -2.49 12.00 -7 1 0 2.23 21.25 -7 -1 0 -13.38 21.40 8 -1 0 56.95 31.69 8 1 0 38.32 24.47 -8 -1 0 1.37 36.39 -8 1 0 24.15 35.77 -9 -1 0 -2.13 34.60 9 1 0 49.80 30.72 -9 1 0 1.49 17.56 -9 1 0 -38.43 32.23 -10 1 0 18.44 40.29 -10 -1 0 46.73 47.40 -11 -1 0 13.87 40.18 -11 1 0 13.33 37.81 -12 1 0 -14.89 51.10 -12 -1 0 67.20 45.98 -13 1 0 -49.81 50.45 -13 -1 0 20.59 56.69 0 2 0 -5.81 4.83 0 -2 0 5.03 5.97 0 -2 0 -1.80 4.86 1 -2 0 5383.18 100.92 -1 -2 0 5206.49 90.00 1 -2 0 5343.95 79.12 1 2 0 5242.63 79.89 -1 2 0 5162.56 83.18 -1 2 0 5128.42 98.53 -1 -2 0 5276.66 96.70 2 -2 0 5863.05 133.40 2 2 0 5925.42 103.29 -2 -2 0 5943.05 115.14 -2 2 0 6007.96 125.95 -2 -2 0 5927.39 132.07 2 -2 0 5931.36 85.87 -3 -2 0 589.53 42.07 -3 -2 0 560.78 57.17 3 -2 0 578.26 55.09 -3 2 0 573.28 55.44 3 2 0 632.33 42.73 3 -2 0 619.97 31.83 4 -2 0 104.95 34.62 -4 2 0 121.47 35.65 -4 -2 0 89.85 22.67 4 -2 0 112.93 17.83 4 2 0 91.58 25.98 -4 -2 0 134.48 38.95 -5 -2 0 41.91 26.28 5 2 0 59.67 24.86 5 -2 0 88.45 33.72 -5 2 0 53.80 29.56 5 -2 0 58.05 13.09 -5 -2 0 60.08 20.07 6 -2 0 284.90 58.36 6 -2 0 277.67 29.74 6 2 0 265.60 46.25 -6 2 0 295.97 65.66 -6 -2 0 271.58 62.61 -6 -2 0 286.67 41.15 7 2 0 892.76 74.84 -7 -2 0 816.69 63.31 -7 2 0 791.36 105.87 7 -2 0 756.15 93.99 -7 -2 0 675.73 101.19 -8 2 0 0.40 33.41 -8 -2 0 -25.21 28.69 -8 2 0 33.65 19.35 8 2 0 10.91 19.55 9 2 0 157.04 47.78 -9 2 0 175.12 47.88 -9 2 0 148.84 63.76 -9 -2 0 219.17 74.84 -10 2 0 -37.63 33.48 -10 2 0 22.56 28.62 -10 -2 0 11.33 35.54 -11 -2 0 68.09 39.41 -11 2 0 -33.25 29.94 -12 2 0 -84.68 35.78 -12 -2 0 -5.79 52.00 -13 -2 0 -2.78 50.51 -13 2 0 50.68 67.94 0 -3 0 -1.99 8.97 0 -3 0 2.04 9.33 0 3 0 0.13 8.85 1 -3 0 3254.15 87.50 -1 3 0 3217.78 63.94 -1 3 0 3308.89 89.53 -1 -3 0 3286.88 72.66 1 3 0 3215.32 68.86 -1 -3 0 3205.68 87.67 1 -3 0 3257.09 73.49 -2 -3 0 1334.27 65.57 2 -3 0 1258.13 45.04 -2 -3 0 1295.41 64.15 2 3 0 1246.53 49.00 2 -3 0 1193.79 68.03 -2 3 0 1311.83 66.96 -2 3 0 1317.33 60.43 3 -3 0 357.07 25.27 -3 3 0 407.21 49.65 -3 -3 0 304.36 45.26 -3 3 0 324.88 43.26 -3 -3 0 337.75 38.71 3 3 0 345.41 33.97 4 3 0 158.29 30.40 -4 3 0 159.75 41.76 4 -3 0 185.57 20.57 -4 -3 0 206.34 45.92 4 -3 0 222.81 49.18 -4 -3 0 202.76 34.55 5 -3 0 33.58 29.67 -5 -3 0 12.03 14.04 5 3 0 31.76 17.95 5 -3 0 21.12 10.44 -5 -3 0 30.24 28.85 -5 3 0 3.62 19.42 6 -3 0 -9.14 7.11 6 3 0 -6.30 13.64 -6 3 0 23.10 19.10 -6 -3 0 31.46 27.59 -6 3 0 19.87 26.93 -6 -3 0 39.14 14.76 -7 3 0 -21.42 12.23 -7 -3 0 20.17 12.60 -7 3 0 -10.19 20.04 -7 -3 0 -2.10 25.03 7 3 0 21.85 17.35 -8 -3 0 92.23 49.43 -8 3 0 85.93 31.56 8 3 0 61.79 21.93 -8 3 0 94.08 51.24 -8 -3 0 54.80 19.72 -9 3 0 -3.56 38.34 -9 -3 0 -30.51 37.06 9 3 0 -7.10 17.58 -9 3 0 15.59 30.87 -10 3 0 18.89 34.45 -10 3 0 7.93 44.37 -10 -3 0 84.35 63.13 -11 -3 0 35.48 43.06 -11 3 0 12.64 31.94 -12 3 0 0.05 42.61 -12 -3 0 -10.35 59.10 13 -3 0 -15.94 39.42 -13 -3 0 -41.84 39.36 -13 3 0 32.08 74.23 0 -4 0 1115.17 56.02 0 4 0 1146.99 53.10 0 -4 0 1035.06 51.85 1 4 0 547.06 34.47 -1 4 0 496.32 42.00 -1 -4 0 488.59 31.76 1 -4 0 530.58 37.83 -1 -4 0 419.91 42.37 -1 4 0 528.43 26.92 1 -4 0 484.76 43.21 2 -4 0 372.75 31.49 2 4 0 394.79 31.26 2 -4 0 397.48 47.66 -2 -4 0 378.89 40.41 -2 4 0 395.09 36.27 -2 4 0 381.68 47.34 -2 -4 0 407.40 43.92 -3 -4 0 3071.54 117.26 -3 4 0 3142.65 121.24 -3 4 0 3194.88 111.06 3 4 0 3014.50 90.13 3 -4 0 3207.29 78.42 -3 -4 0 3039.84 109.59 3 -4 0 2969.72 125.66 -4 4 0 216.03 43.88 4 4 0 241.81 34.77 -4 -4 0 189.94 37.11 -4 4 0 222.50 45.39 -4 -4 0 212.00 45.39 4 -4 0 186.75 21.62 -5 -4 0 18.63 15.17 5 4 0 14.10 13.73 -5 -4 0 36.49 26.10 -5 4 0 22.92 23.58 -5 4 0 36.20 21.07 5 -4 0 41.40 9.73 -6 4 0 259.00 54.24 -6 -4 0 173.78 53.40 6 -4 0 183.63 21.26 6 4 0 261.71 42.52 -6 4 0 202.76 53.01 -6 -4 0 240.68 41.48 -7 4 0 4.39 20.38 -7 -4 0 17.43 32.96 7 4 0 -10.16 13.69 -7 -4 0 1.82 13.53 -7 4 0 -10.16 17.55 -8 4 0 646.79 105.31 -8 -4 0 618.65 108.74 -8 -4 0 811.98 70.60 -8 4 0 748.20 99.13 8 4 0 750.47 80.53 -9 4 0 365.03 82.62 -9 4 0 284.09 82.71 -9 -4 0 253.97 83.16 -10 4 0 80.61 56.28 -10 -4 0 52.26 49.95 -10 4 0 26.62 32.46 -11 4 0 16.32 42.78 11 -4 0 -1.66 30.36 -11 -4 0 -22.99 32.50 -12 4 0 124.73 57.72 -12 -4 0 -22.84 43.19 12 -4 0 60.03 43.84 -13 -4 0 -34.37 44.47 -13 4 0 90.08 61.83 13 -4 0 -35.81 33.41 0 -5 0 4.97 16.01 0 -5 0 -16.53 13.28 0 5 0 -9.69 16.46 1 -5 0 194.21 30.60 -1 5 0 221.91 35.67 1 5 0 241.12 30.03 1 -5 0 145.15 30.67 -1 -5 0 259.62 26.15 -1 5 0 178.67 16.84 -1 -5 0 196.46 35.57 2 5 0 3055.01 84.86 -2 -5 0 3084.19 99.33 -2 -5 0 3131.78 115.98 -2 5 0 2995.37 85.80 2 -5 0 3049.67 113.66 -2 5 0 3029.41 116.02 2 -5 0 3147.87 90.69 -3 5 0 1188.57 68.54 3 5 0 1204.69 59.35 -3 5 0 1166.95 81.50 3 -5 0 1258.94 55.45 3 -5 0 1053.62 78.83 -3 -5 0 1115.91 73.56 -3 -5 0 1153.62 76.10 4 5 0 2.34 14.02 4 -5 0 5.84 20.56 -4 -5 0 0.45 18.68 -4 -5 0 -5.13 10.52 4 -5 0 20.40 7.62 -4 5 0 24.07 19.19 -4 5 0 -1.28 17.15 -5 -5 0 125.20 40.60 5 5 0 45.45 17.91 5 -5 0 36.77 30.19 -5 5 0 69.84 29.45 -5 5 0 36.31 20.17 -5 -5 0 46.87 21.30 5 -5 0 43.99 10.49 6 5 0 263.34 44.02 6 -5 0 197.28 52.99 -6 5 0 307.34 62.07 -6 5 0 265.86 60.52 -6 -5 0 324.88 49.93 6 -5 0 271.84 23.55 -6 -5 0 237.91 58.38 -7 -5 0 52.22 39.71 -7 5 0 41.21 30.17 -7 5 0 57.06 34.13 -7 -5 0 3.95 13.07 7 5 0 35.28 22.42 -8 -5 0 -24.03 15.75 -8 5 0 -2.95 20.79 -8 5 0 -33.88 23.95 8 5 0 -6.42 14.64 -8 -5 0 -4.74 32.20 -9 5 0 81.21 48.58 9 -5 0 20.09 27.87 -9 5 0 57.86 40.87 -9 -5 0 63.38 49.92 -10 5 0 -30.27 25.89 -10 -5 0 -13.05 42.55 -10 5 0 14.67 38.21 10 -5 0 37.43 37.57 -11 -5 0 91.72 54.42 11 -5 0 -20.02 36.47 -11 5 0 72.31 42.68 -12 -5 0 -48.57 38.73 -12 5 0 -42.26 39.60 12 -5 0 -6.50 33.39 13 -5 0 -26.56 33.57 -13 -5 0 -26.72 43.47 -13 5 0 1.18 47.81 0 -6 0 22.03 20.87 0 -6 0 7.25 18.96 0 6 0 63.15 25.76 -1 6 0 434.54 49.41 -1 6 0 381.53 20.54 1 -6 0 382.62 45.55 -1 -6 0 406.17 50.62 1 6 0 451.82 41.60 1 -6 0 362.58 41.36 -1 -6 0 438.46 30.55 2 6 0 249.13 32.01 -2 -6 0 278.28 36.03 2 -6 0 206.00 40.00 -2 6 0 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