#------------------------------------------------------------------------------ #$Date: 2019-11-17 04:50:51 +0200 (Sun, 17 Nov 2019) $ #$Revision: 227957 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/00/1550033.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1550033 loop_ _publ_author_name 'Zelenay, Benjamin' 'Besora, Maria' 'Monasterio, Zaira' 'Ventura-Espinosa, David' 'White, Andrew J. P.' 'Maseras, Feliu' 'D\'iez-Gonz\'alez, Silvia' _publ_section_title ; Copper-mediated reduction of azides under seemingly oxidising conditions: catalytic and computational studies ; _journal_issue 22 _journal_name_full 'Catalysis Science & Technology' _journal_page_first 5763 _journal_paper_doi 10.1039/C8CY00515J _journal_volume 8 _journal_year 2018 _chemical_formula_moiety 'C36 H44 Cu N8, B F4, C H2 Cl2' _chemical_formula_sum 'C37 H46 B Cl2 Cu F4 N8' _chemical_formula_weight 824.07 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-11-03 deposited with the CCDC. 2018-08-30 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.694(11) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 20.808(3) _cell_length_b 31.071(2) _cell_length_c 12.2164(11) _cell_measurement_reflns_used 5346 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 72.6120 _cell_measurement_theta_min 2.4970 _cell_volume 7897.6(14) _computing_cell_refinement CrysAlisPro, _computing_data_collection CrysAlisPro, _computing_data_reduction CrysAlisPro, _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'CIFTAB-2014 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 10.4115 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.913 _diffrn_measurement_device_type 'Agilent Xcalibur PX Ultra A' _diffrn_measurement_method 'omega scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0662 _diffrn_reflns_av_unetI/netI 0.0762 _diffrn_reflns_Laue_measured_fraction_full 0.988 _diffrn_reflns_Laue_measured_fraction_max 0.913 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 25996 _diffrn_reflns_point_group_measured_fraction_full 0.988 _diffrn_reflns_point_group_measured_fraction_max 0.913 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.740 _diffrn_reflns_theta_min 2.123 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.504 _exptl_absorpt_correction_T_max 0.876 _exptl_absorpt_correction_T_min 0.540 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour 'Dark red' _exptl_crystal_density_diffrn 1.386 _exptl_crystal_description needles _exptl_crystal_F_000 3424 _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.07 _refine_diff_density_max 3.368 _refine_diff_density_min -1.547 _refine_diff_density_rms 0.216 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.855 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1014 _refine_ls_number_reflns 15216 _refine_ls_number_restraints 266 _refine_ls_restrained_S_all 1.860 _refine_ls_R_factor_all 0.2276 _refine_ls_R_factor_gt 0.2039 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.4806 _refine_ls_wR_factor_ref 0.5109 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10628 _reflns_number_total 15216 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8cy00515j2.cif _cod_data_source_block 3 _cod_depositor_comments 'Adding full bibliography for 1550033--1550035.cif.' _cod_original_cell_volume 7897.6(15) _cod_database_code 1550033 _shelx_shelxl_version_number 2014/7 _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. ; _shelx_res_file ; SDG1401.res created by SHELXL-2014/7 TITL SDG1401 in P2(1)/c REM P2(1)/c (#14 in standard setting) REM TXJ-019-1 CELL 1.54184 20.808008 31.070662 12.216443 90.0000 90.6945 90.0000 ZERR 8.00 0.003054 0.002250 0.001136 0.0000 0.0107 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H B Cl Cu F N UNIT 296 368 8 16 8 32 64 TEMP -100 L.S. 30 FMAP 2 PLAN 10 ACTA REM 'C36 H44 Cu N8, B F4, C H2 Cl2' REM C37 H46 B Cl2 Cu F4 N8 SADI C6B N9B C6B N9" SADI N9B C10B N9B C11B N9" C10" N9" C11" SADI C6B C10B C6B C11B C6B C10" C6B C11" SADI C10B C11B C10" C11" FLAT C6B C10B C11B N9B FLAT C6B C10" C11" N9" DFIX 2.50 0.01 C7B C11" ! to avoid short H7BA to C11"-H H...H contacts SIMU 0.02 0.02 1 N9B > C11" SADI B20 F21 B20 F22 B20 F23 B20 F24 = B20' F21' B20' F22' B20' F23' B20' F24' SADI F21 F22 F21 F23 F21 F24 F22 F23 F22 F24 F23 F24 = F21' F22' F21' F23' F21' F24' F22' F23' F22' F24' F23' F24' SIMU 0.02 0.02 2 B20 > F24' SADI C50 CL51 C50 CL52 C50' CL53 C50' CL54 SADI CL51 CL52 CL53 CL54 SIMU 0.02 0.02 1 C50 > CL54 REM AFIX 3 used for C11B to prevent short intramolecular contact of one of REM the C11B protons with H7BA REM AFIX 33 used for C39B to prevent short intermolecular contact of one of REM the C39B protons with H36A WGHT 0.200000 FVAR 0.76068 0.54941 0.76433 0.85356 CU1A 5 0.126339 0.334625 0.584345 11.00000 0.06335 0.05020 = 0.03306 0.00367 0.00440 0.00585 N1A 7 0.096440 0.305144 0.722936 11.00000 0.04891 0.04713 = 0.03441 -0.00010 -0.00018 0.00959 C1A 1 0.127755 0.318669 0.808706 11.00000 0.07191 0.05591 = 0.02041 0.00007 0.00042 -0.00306 AFIX 43 H1AA 2 0.119651 0.307605 0.879706 11.00000 -1.20000 AFIX 0 C2A 1 0.174959 0.351017 0.790620 11.00000 0.05749 0.05645 = 0.04089 0.00133 -0.00062 0.00653 AFIX 43 H2AA 2 0.198967 0.362642 0.850287 11.00000 -1.20000 AFIX 0 N2A 7 0.184867 0.364571 0.690360 11.00000 0.05069 0.04845 = 0.05757 -0.00083 0.00251 0.00357 C3A 1 0.047240 0.273313 0.731897 11.00000 0.05066 0.04991 = 0.02998 0.00469 0.00302 0.00599 C4A 1 0.019730 0.258383 0.635989 11.00000 0.07895 0.08625 = 0.03056 0.00247 0.00176 -0.02527 AFIX 43 H4AA 2 0.035706 0.268210 0.567891 11.00000 -1.20000 AFIX 0 C5A 1 -0.029410 0.230106 0.636902 11.00000 0.08580 0.11785 = 0.03872 -0.00906 -0.00006 -0.04152 AFIX 43 H5AA 2 -0.050701 0.223417 0.569808 11.00000 -1.20000 AFIX 0 C6A 1 -0.050151 0.210316 0.732609 11.00000 0.06449 0.06655 = 0.05080 0.00056 -0.00349 -0.00227 C7A 1 -0.024054 0.225373 0.828722 11.00000 0.07483 0.11154 = 0.04352 0.02339 0.00228 -0.02804 AFIX 43 H7AA 2 -0.039104 0.214218 0.896127 11.00000 -1.20000 AFIX 0 C8A 1 0.023835 0.256521 0.830199 11.00000 0.07497 0.12368 = 0.03716 0.01849 -0.00416 -0.03579 AFIX 43 H8AA 2 0.040809 0.266493 0.898138 11.00000 -1.20000 AFIX 0 N9A 7 -0.097102 0.178530 0.731275 11.00000 0.07775 0.09658 = 0.05866 0.00688 0.00772 -0.02849 C10A 1 -0.132303 0.168656 0.639628 11.00000 0.14325 0.18769 = 0.09977 -0.06426 0.03960 -0.11379 AFIX 137 H10A 2 -0.137065 0.194405 0.593917 11.00000 -1.50000 H10B 2 -0.174856 0.158322 0.660928 11.00000 -1.50000 H10C 2 -0.110253 0.146153 0.598258 11.00000 -1.50000 AFIX 0 C11A 1 -0.122315 0.163211 0.836388 11.00000 0.11842 0.11960 = 0.06065 0.00299 0.01859 -0.04611 AFIX 137 H11A 2 -0.094558 0.140267 0.865160 11.00000 -1.50000 H11B 2 -0.165961 0.152051 0.825302 11.00000 -1.50000 H11C 2 -0.123211 0.187117 0.888678 11.00000 -1.50000 AFIX 0 C12A 1 0.228908 0.397662 0.663256 11.00000 0.06625 0.05477 = 0.05530 -0.00324 0.00482 -0.00160 C13A 1 0.243573 0.403675 0.556138 11.00000 0.07202 0.05551 = 0.06976 0.00546 0.00799 0.00186 AFIX 43 H13A 2 0.222856 0.386052 0.502857 11.00000 -1.20000 AFIX 0 C14A 1 0.287612 0.434493 0.520477 11.00000 0.09118 0.06199 = 0.05270 0.01231 0.01581 -0.00328 AFIX 43 H14A 2 0.294488 0.438814 0.444531 11.00000 -1.20000 AFIX 0 C15A 1 0.320651 0.458333 0.596745 11.00000 0.07593 0.07787 = 0.08139 0.02227 0.01283 -0.01139 C16A 1 0.302862 0.452523 0.708010 11.00000 0.10735 0.08923 = 0.07351 -0.00893 0.01669 -0.03262 AFIX 43 H16A 2 0.321460 0.471199 0.761194 11.00000 -1.20000 AFIX 0 C17A 1 0.261052 0.422039 0.743134 11.00000 0.10988 0.09023 = 0.05463 -0.00074 0.02083 -0.04156 AFIX 43 H17A 2 0.253936 0.417465 0.818915 11.00000 -1.20000 AFIX 0 N18A 7 0.364534 0.489276 0.560281 11.00000 0.11339 0.11103 = 0.10845 0.00778 0.03870 -0.05140 C19A 1 0.386735 0.489149 0.451375 11.00000 0.13733 0.11508 = 0.11050 -0.01122 0.03876 -0.06032 AFIX 137 H19A 2 0.408329 0.461778 0.436448 11.00000 -1.50000 H19B 2 0.417066 0.512916 0.441390 11.00000 -1.50000 H19C 2 0.350200 0.492665 0.400788 11.00000 -1.50000 AFIX 0 C20A 1 0.404126 0.509249 0.643763 11.00000 0.15558 0.19362 = 0.10638 0.02358 0.01281 -0.09039 AFIX 33 H20A 2 0.432891 0.530217 0.609843 11.00000 -1.50000 H20B 2 0.376667 0.523924 0.696629 11.00000 -1.50000 H20C 2 0.429699 0.487168 0.681496 11.00000 -1.50000 AFIX 0 N21A 7 0.150269 0.312582 0.434171 11.00000 0.07288 0.04836 = 0.03398 0.00291 0.00395 0.00276 C21A 1 0.120958 0.332379 0.360837 11.00000 0.09816 0.10617 = 0.02835 -0.00005 0.00317 0.04780 AFIX 43 H21A 2 0.129579 0.327346 0.285731 11.00000 -1.20000 AFIX 0 C22A 1 0.072009 0.364161 0.394806 11.00000 0.12240 0.08074 = 0.04754 0.01757 0.00054 0.05474 AFIX 43 H22A 2 0.045850 0.378183 0.341443 11.00000 -1.20000 AFIX 0 N22A 7 0.065233 0.372575 0.496387 11.00000 0.07842 0.05685 = 0.04737 0.00259 0.01588 0.01963 C23A 1 0.197013 0.281072 0.405735 11.00000 0.04606 0.05342 = 0.03811 -0.00341 0.00293 -0.00340 C24A 1 0.221096 0.256108 0.488899 11.00000 0.06044 0.06046 = 0.03279 -0.00447 0.00157 0.00441 AFIX 43 H24A 2 0.207062 0.260846 0.561621 11.00000 -1.20000 AFIX 0 C25A 1 0.265589 0.224064 0.468654 11.00000 0.05769 0.07827 = 0.04372 -0.00703 -0.00388 0.01690 AFIX 43 H25A 2 0.280515 0.206493 0.527305 11.00000 -1.20000 AFIX 0 C26A 1 0.289211 0.217049 0.361982 11.00000 0.04580 0.07052 = 0.05104 -0.02008 -0.00248 -0.00661 C27A 1 0.265763 0.243038 0.276823 11.00000 0.05657 0.06276 = 0.04691 -0.01769 0.01140 -0.00510 AFIX 43 H27A 2 0.280489 0.239175 0.204176 11.00000 -1.20000 AFIX 0 C28A 1 0.220647 0.274547 0.300216 11.00000 0.06130 0.06244 = 0.04321 0.00302 0.00342 -0.00396 AFIX 43 H28A 2 0.205225 0.292358 0.242407 11.00000 -1.20000 AFIX 0 N29A 7 0.333183 0.185232 0.339378 11.00000 0.05615 0.08807 = 0.06671 -0.01875 0.00134 0.01533 C30A 1 0.367731 0.164992 0.424705 11.00000 0.06764 0.12690 = 0.09595 -0.01425 -0.01952 0.02217 AFIX 137 H30A 2 0.400130 0.184886 0.454190 11.00000 -1.50000 H30B 2 0.389004 0.139210 0.396463 11.00000 -1.50000 H30C 2 0.338117 0.156787 0.482880 11.00000 -1.50000 AFIX 0 C31A 1 0.354899 0.178344 0.224660 11.00000 0.05961 0.10280 = 0.08095 -0.04227 0.00347 0.00794 AFIX 137 H31A 2 0.317580 0.172273 0.177447 11.00000 -1.50000 H31B 2 0.384698 0.153940 0.222638 11.00000 -1.50000 H31C 2 0.376673 0.204297 0.198600 11.00000 -1.50000 AFIX 0 C32A 1 0.025527 0.404468 0.539843 11.00000 0.08555 0.06310 = 0.05396 0.01000 0.00524 0.03630 C33A 1 0.019238 0.408973 0.648265 11.00000 0.05086 0.04887 = 0.04613 -0.00126 0.00466 0.00267 AFIX 43 H33A 2 0.043427 0.390454 0.694932 11.00000 -1.20000 AFIX 0 C34A 1 -0.021960 0.440184 0.697669 11.00000 0.05765 0.05270 = 0.05266 -0.00227 0.00724 -0.00011 AFIX 43 H34A 2 -0.022594 0.442998 0.775083 11.00000 -1.20000 AFIX 0 C35A 1 -0.060377 0.465946 0.633998 11.00000 0.07290 0.06953 = 0.06296 -0.00979 0.00464 0.02083 C36A 1 -0.054263 0.460112 0.519400 11.00000 0.14609 0.11968 = 0.06021 0.00260 -0.00249 0.08954 AFIX 43 H36A 2 -0.081163 0.476443 0.471697 11.00000 -1.20000 AFIX 0 C37A 1 -0.011370 0.432026 0.474576 11.00000 0.19931 0.16510 = 0.04091 0.01606 0.00900 0.12664 AFIX 43 H37A 2 -0.006615 0.431277 0.397356 11.00000 -1.20000 AFIX 0 N38A 7 -0.099367 0.496589 0.679625 11.00000 0.10706 0.08708 = 0.08370 0.00024 0.02724 0.03655 C39A 1 -0.110713 0.495256 0.794812 11.00000 0.12340 0.10492 = 0.10493 -0.01679 0.02426 0.03273 AFIX 137 H39A 2 -0.121451 0.465773 0.816450 11.00000 -1.50000 H39B 2 -0.146500 0.514452 0.812426 11.00000 -1.50000 H39C 2 -0.071963 0.504631 0.834486 11.00000 -1.50000 AFIX 0 C40A 1 -0.139196 0.524436 0.609292 11.00000 0.10615 0.10618 = 0.13173 -0.00526 0.00907 0.05012 AFIX 137 H40A 2 -0.122166 0.524341 0.534852 11.00000 -1.50000 H40B 2 -0.138524 0.553858 0.638191 11.00000 -1.50000 H40C 2 -0.183479 0.513691 0.607897 11.00000 -1.50000 AFIX 0 CU1B 5 0.622959 0.168424 0.579874 11.00000 0.05364 0.05764 = 0.03931 -0.00373 -0.00202 0.00023 N1B 7 0.650579 0.197947 0.718678 11.00000 0.04884 0.05630 = 0.03963 -0.00483 0.00397 0.00359 C1B 1 0.619760 0.182667 0.800800 11.00000 0.05864 0.06348 = 0.03786 -0.00885 -0.00622 0.01162 AFIX 43 H1BA 2 0.628915 0.193144 0.872362 11.00000 -1.20000 AFIX 0 C2B 1 0.571344 0.149722 0.785299 11.00000 0.05456 0.05996 = 0.05110 0.00910 0.00748 0.01064 AFIX 43 H2BA 2 0.547919 0.138018 0.844559 11.00000 -1.20000 AFIX 0 N2B 7 0.562250 0.137461 0.686672 11.00000 0.04844 0.05485 = 0.05126 0.00346 -0.00344 0.00520 C3B 1 0.699966 0.229194 0.727638 11.00000 0.05772 0.05511 = 0.04411 -0.01239 -0.00900 0.00934 C4B 1 0.718298 0.250482 0.634399 11.00000 0.08352 0.10560 = 0.03837 -0.00306 -0.00462 -0.03515 AFIX 43 H4BA 2 0.697472 0.243671 0.566968 11.00000 -1.20000 AFIX 0 C5B 1 0.765945 0.281421 0.635435 11.00000 0.09575 0.10143 = 0.05274 -0.00827 -0.00283 -0.04422 AFIX 43 H5BA 2 0.777284 0.295572 0.569495 11.00000 -1.20000 AFIX 0 C6B 1 0.796885 0.291715 0.731650 11.00000 0.05589 0.06382 = 0.06558 -0.00926 -0.00192 -0.00816 C7B 1 0.779004 0.271237 0.821460 11.00000 0.08783 0.07487 = 0.06058 -0.01561 -0.03131 -0.00103 AFIX 43 H7BA 2 0.799416 0.278795 0.888733 11.00000 -1.20000 AFIX 0 C8B 1 0.731387 0.238835 0.823064 11.00000 0.06912 0.07824 = 0.04196 0.00128 -0.00685 -0.00339 AFIX 43 H8BA 2 0.721523 0.224146 0.888961 11.00000 -1.20000 AFIX 0 PART 1 N9B 7 0.844063 0.323739 0.730672 41.00000 0.08384 0.07108 = 0.07216 -0.00805 -0.02450 -0.02151 C10B 1 0.870194 0.338876 0.636927 41.00000 0.08691 0.08788 = 0.08283 -0.00680 -0.00113 -0.02758 AFIX 33 H10D 2 0.902117 0.361061 0.654769 41.00000 -1.50000 H10E 2 0.891029 0.315197 0.597997 41.00000 -1.50000 H10F 2 0.836296 0.351294 0.590351 41.00000 -1.50000 AFIX 0 C11B 1 0.875130 0.335007 0.829000 41.00000 0.08775 0.08657 = 0.07340 -0.00411 -0.02961 -0.01926 AFIX 3 H11D 2 0.912650 0.352967 0.813510 41.00000 -1.50000 H11E 2 0.845240 0.351077 0.875000 41.00000 -1.50000 H11F 2 0.889020 0.308857 0.867400 41.00000 -1.50000 AFIX 0 PART 2 N9" 7 0.852937 0.313196 0.763224 -41.00000 0.08736 C10" 1 0.898533 0.324147 0.687227 -41.00000 0.09044 AFIX 33 H10G 2 0.884488 0.314334 0.614549 -41.00000 -1.50000 H10H 2 0.904024 0.355471 0.686413 -41.00000 -1.50000 H10I 2 0.939512 0.310425 0.706676 -41.00000 -1.50000 AFIX 0 C11" 1 0.864580 0.324493 0.870647 -41.00000 0.08208 AFIX 3 H11G 2 0.880920 0.298143 0.905177 -41.00000 -1.50000 H11H 2 0.825980 0.334133 0.908717 -41.00000 -1.50000 H11I 2 0.897550 0.346983 0.874997 -41.00000 -1.50000 AFIX 0 PART 0 C12B 1 0.519414 0.105044 0.659476 11.00000 0.05743 0.05059 = 0.07728 0.01321 -0.00992 -0.00242 C13B 1 0.508997 0.097728 0.548340 11.00000 0.07601 0.07693 = 0.08681 0.00090 -0.01108 -0.01906 AFIX 43 H13B 2 0.530404 0.114884 0.495735 11.00000 -1.20000 AFIX 0 C14B 1 0.468427 0.066219 0.515158 11.00000 0.08162 0.09142 = 0.08788 -0.00272 -0.02281 -0.01827 AFIX 43 H14B 2 0.461021 0.062698 0.438795 11.00000 -1.20000 AFIX 0 C15B 1 0.435692 0.037598 0.589095 11.00000 0.11068 0.06970 = 0.09101 0.02310 -0.03043 -0.02613 C16B 1 0.451955 0.043903 0.698136 11.00000 0.10092 0.08694 = 0.06934 0.00814 -0.00685 -0.01912 AFIX 43 H16B 2 0.436613 0.023891 0.750486 11.00000 -1.20000 AFIX 0 C17B 1 0.489366 0.077827 0.734630 11.00000 0.10787 0.08216 = 0.06974 0.01584 -0.00374 -0.03410 AFIX 43 H17B 2 0.494743 0.082724 0.810953 11.00000 -1.20000 AFIX 0 N18B 7 0.399311 0.004998 0.553215 11.00000 0.16855 0.11222 = 0.10060 0.02528 -0.06114 -0.04683 C19B 1 0.387321 -0.002160 0.438623 11.00000 0.14528 0.12188 = 0.12069 0.01582 -0.05696 -0.04118 AFIX 137 H19D 2 0.348779 0.013730 0.415622 11.00000 -1.50000 H19E 2 0.380768 -0.032971 0.425462 11.00000 -1.50000 H19F 2 0.424235 0.007879 0.396598 11.00000 -1.50000 AFIX 0 C20B 1 0.377251 -0.025454 0.630571 11.00000 0.16079 0.11295 = 0.10459 0.03116 -0.03464 -0.07855 AFIX 137 H20D 2 0.410911 -0.046889 0.644561 11.00000 -1.50000 H20E 2 0.338719 -0.039818 0.601602 11.00000 -1.50000 H20F 2 0.366873 -0.010707 0.699030 11.00000 -1.50000 AFIX 0 N21B 7 0.602637 0.189164 0.428994 11.00000 0.05095 0.05729 = 0.04250 0.00058 -0.00524 -0.01004 C21B 1 0.637926 0.169847 0.353386 11.00000 0.08680 0.06165 = 0.03362 -0.00528 -0.00429 -0.00271 AFIX 43 H21B 2 0.632688 0.176756 0.278052 11.00000 -1.20000 AFIX 0 C22B 1 0.683297 0.138858 0.387934 11.00000 0.06896 0.06807 = 0.06401 -0.01292 0.01077 0.00385 AFIX 43 H22B 2 0.709664 0.124153 0.337178 11.00000 -1.20000 AFIX 0 N22B 7 0.687460 0.131208 0.494167 11.00000 0.05477 0.05388 = 0.05232 -0.00756 -0.00204 -0.00313 C23B 1 0.554163 0.218883 0.401153 11.00000 0.05329 0.04865 = 0.03990 -0.00536 0.00289 -0.01026 C24B 1 0.528401 0.245109 0.483787 11.00000 0.05069 0.06377 = 0.03980 0.00126 -0.00015 0.00217 AFIX 43 H24B 2 0.543547 0.241347 0.556834 11.00000 -1.20000 AFIX 0 C25B 1 0.481261 0.276623 0.463068 11.00000 0.06359 0.06566 = 0.05199 -0.00793 0.00443 0.00723 AFIX 43 H25B 2 0.465471 0.294067 0.520671 11.00000 -1.20000 AFIX 0 C26B 1 0.458731 0.281602 0.358678 11.00000 0.04427 0.06265 = 0.05101 0.00752 0.00165 0.00269 C27B 1 0.483818 0.253975 0.273493 11.00000 0.06217 0.06106 = 0.03544 -0.00106 -0.00490 -0.00452 AFIX 43 H27B 2 0.468006 0.256958 0.200611 11.00000 -1.20000 AFIX 0 C28B 1 0.529425 0.223977 0.296032 11.00000 0.07052 0.05539 = 0.04276 -0.00415 -0.00013 -0.00471 AFIX 43 H28B 2 0.544700 0.206136 0.238801 11.00000 -1.20000 AFIX 0 N29B 7 0.415358 0.312987 0.332328 11.00000 0.06442 0.09841 = 0.05526 0.00667 -0.00305 0.02190 C30B 1 0.380454 0.335867 0.418879 11.00000 0.07646 0.12993 = 0.08366 0.01701 0.01729 0.04263 AFIX 137 H30D 2 0.362519 0.314931 0.470151 11.00000 -1.50000 H30E 2 0.345537 0.352805 0.385866 11.00000 -1.50000 H30F 2 0.410082 0.355089 0.458207 11.00000 -1.50000 AFIX 0 C31B 1 0.393707 0.320512 0.219722 11.00000 0.06903 0.09346 = 0.07664 0.02127 -0.01994 0.00522 AFIX 137 H31D 2 0.425890 0.309430 0.169040 11.00000 -1.50000 H31E 2 0.387973 0.351469 0.207735 11.00000 -1.50000 H31F 2 0.352737 0.305685 0.206866 11.00000 -1.50000 AFIX 0 C32B 1 0.729494 0.100768 0.538570 11.00000 0.04991 0.05448 = 0.05889 -0.00665 -0.00055 0.01107 C33B 1 0.726187 0.093353 0.650771 11.00000 0.06312 0.04906 = 0.05596 -0.00052 -0.01286 0.00126 AFIX 43 H33B 2 0.696794 0.109393 0.693487 11.00000 -1.20000 AFIX 0 C34B 1 0.765730 0.062485 0.701531 11.00000 0.06030 0.06492 = 0.06008 -0.00050 -0.00733 0.00555 AFIX 43 H34B 2 0.765475 0.060053 0.779042 11.00000 -1.20000 AFIX 0 C35B 1 0.805137 0.035440 0.642098 11.00000 0.05989 0.07710 = 0.08048 -0.00592 -0.00716 0.01211 C36B 1 0.808303 0.043551 0.530113 11.00000 0.09598 0.12097 = 0.06816 0.00488 0.01142 0.06090 AFIX 43 H36B 2 0.837423 0.027243 0.487503 11.00000 -1.20000 AFIX 0 C37B 1 0.771604 0.073701 0.479587 11.00000 0.07755 0.11407 = 0.06256 -0.01003 0.00451 0.03903 AFIX 43 H37B 2 0.774124 0.076821 0.402400 11.00000 -1.20000 AFIX 0 N38B 7 0.843467 0.004393 0.690453 11.00000 0.08847 0.10301 = 0.07026 -0.00629 -0.00363 0.01669 C39B 1 0.846376 0.002418 0.805406 11.00000 0.11454 0.11114 = 0.09738 -0.01113 -0.03154 0.03119 AFIX 33 H39D 2 0.875195 -0.020971 0.828074 11.00000 -1.50000 H39E 2 0.862682 0.029783 0.834378 11.00000 -1.50000 H39F 2 0.803278 -0.002933 0.833876 11.00000 -1.50000 AFIX 0 C40B 1 0.877950 -0.026427 0.622490 11.00000 0.14232 0.12068 = 0.10457 -0.04482 -0.03485 0.06117 AFIX 137 H40D 2 0.916847 -0.012869 0.594011 11.00000 -1.50000 H40E 2 0.850241 -0.035485 0.561277 11.00000 -1.50000 H40F 2 0.889886 -0.051595 0.666607 11.00000 -1.50000 AFIX 0 B10 3 0.532865 0.389780 0.615410 11.00000 0.08132 0.09023 = 0.11077 0.00706 -0.02268 -0.02166 F11 6 0.565325 0.413632 0.686467 11.00000 0.22017 0.22099 = 0.14155 -0.06104 0.03210 -0.06406 F12 6 0.483230 0.368502 0.657506 11.00000 0.15913 0.14421 = 0.29378 0.03465 0.07558 -0.04192 F13 6 0.575097 0.351513 0.592797 11.00000 0.13313 0.12941 = 0.20477 0.02873 -0.02790 -0.00833 F14 6 0.524818 0.406541 0.515475 11.00000 0.17837 0.13233 = 0.10612 0.02330 -0.00034 0.00066 PART 1 B20 3 0.228043 0.400306 0.125757 21.00000 0.11532 0.11963 = 0.12109 0.00522 -0.00115 0.01308 F21 6 0.168407 0.420968 0.120491 21.00000 0.13503 0.13694 = 0.14518 -0.00012 -0.00474 0.00907 F22 6 0.241495 0.389283 0.234884 21.00000 0.08429 0.09021 = 0.09321 0.00110 -0.01833 0.01900 F23 6 0.274586 0.428507 0.082165 21.00000 0.14095 0.15785 = 0.17380 -0.00558 0.00283 -0.01803 F24 6 0.228039 0.362658 0.063306 21.00000 0.14844 0.14066 = 0.13166 -0.00175 -0.00283 0.00867 PART 2 B20' 3 0.203029 0.382998 0.117065 -21.00000 0.09508 F21' 6 0.167053 0.408000 0.188837 -21.00000 0.09768 F22' 6 0.257926 0.368357 0.172313 -21.00000 0.11264 F23' 6 0.221587 0.405900 0.025256 -21.00000 0.13501 F24' 6 0.164865 0.347319 0.085821 -21.00000 0.08705 PART 1 C50 1 0.696346 0.410869 0.560949 31.00000 0.08076 0.33984 = 0.30217 -0.23496 0.03896 -0.04533 AFIX 23 H50A 2 0.669199 0.434883 0.533944 31.00000 -1.20000 H50B 2 0.668863 0.391391 0.604224 31.00000 -1.20000 AFIX 0 CL51 4 0.727303 0.382455 0.448285 31.00000 0.12378 0.12221 = 0.07517 -0.00319 -0.00536 0.00093 CL52 4 0.757376 0.431366 0.645099 31.00000 0.13325 0.12510 = 0.10540 -0.01683 0.00064 -0.02257 PART 2 C50' 1 0.716083 0.386215 0.607675 -31.00000 0.12272 AFIX 23 H50C 2 0.677717 0.404797 0.598903 -31.00000 -1.20000 H50D 2 0.704219 0.361431 0.654179 -31.00000 -1.20000 AFIX 0 CL53 4 0.740072 0.367417 0.478119 -31.00000 0.13412 CL54 4 0.778065 0.415548 0.672242 -31.00000 0.13894 PART 0 C60 1 0.034271 0.389469 0.101413 11.00000 0.13043 0.09564 = 0.10170 0.00093 0.00681 0.01906 AFIX 23 H60A 2 0.034848 0.362345 0.143935 11.00000 -1.20000 H60B 2 0.077125 0.403165 0.107463 11.00000 -1.20000 AFIX 0 CL61 4 0.013031 0.378875 -0.043678 11.00000 0.10859 0.19125 = 0.06613 -0.00989 -0.00374 -0.01372 CL62 4 -0.027909 0.425605 0.151443 11.00000 0.13045 0.16588 = 0.12931 -0.01772 0.01850 0.02324 HKLF 4 REM SDG1401 in P2(1)/c REM R1 = 0.2039 for 10628 Fo > 4sig(Fo) and 0.2276 for all 15216 data REM 1014 parameters refined using 266 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 3.368, deepest hole -1.547, 1-sigma level 0.216 Q1 1 0.1264 0.3307 0.5437 11.00000 0.05 3.37 Q2 1 0.6214 0.1709 0.6194 11.00000 0.05 3.22 Q3 1 0.1073 0.3414 0.0621 11.00000 0.05 1.65 Q4 1 0.1296 0.3333 0.6967 11.00000 0.05 1.56 Q5 1 0.2542 0.4476 0.0383 11.00000 0.05 1.29 Q6 1 0.4823 0.4037 0.5788 11.00000 0.05 1.18 Q7 1 0.0950 0.4069 -0.0232 11.00000 0.05 1.16 Q8 1 0.7462 0.3860 0.4919 11.00000 0.05 1.10 Q9 1 0.1948 0.3644 0.6300 11.00000 0.05 1.07 Q10 1 0.6763 0.1383 0.5178 11.00000 0.05 1.03 ; _shelx_res_checksum 46578 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 Cu1A Cu 0.12634(6) 0.33462(4) 0.58435(9) 0.0488(4) Uani 1 1 d . . . . . N1A N 0.0964(3) 0.3051(2) 0.7229(5) 0.0435(12) Uani 1 1 d . . . . . C1A C 0.1278(4) 0.3187(3) 0.8087(5) 0.0494(16) Uani 1 1 d . . . . . H1AA H 0.1197 0.3076 0.8797 0.059 Uiso 1 1 calc R U . . . C2A C 0.1750(4) 0.3510(3) 0.7906(7) 0.0516(17) Uani 1 1 d . . . . . H2AA H 0.1990 0.3626 0.8503 0.062 Uiso 1 1 calc R U . . . N2A N 0.1849(3) 0.3646(2) 0.6904(6) 0.0522(15) Uani 1 1 d . . . . . C3A C 0.0472(4) 0.2733(2) 0.7319(6) 0.0435(14) Uani 1 1 d . . . . . C4A C 0.0197(5) 0.2584(4) 0.6360(7) 0.065(2) Uani 1 1 d . . . . . H4AA H 0.0357 0.2682 0.5679 0.078 Uiso 1 1 calc R U . . . C5A C -0.0294(6) 0.2301(5) 0.6369(8) 0.081(3) Uani 1 1 d . . . . . H5AA H -0.0507 0.2234 0.5698 0.097 Uiso 1 1 calc R U . . . C6A C -0.0502(5) 0.2103(3) 0.7326(8) 0.061(2) Uani 1 1 d . . . . . C7A C -0.0241(6) 0.2254(4) 0.8287(8) 0.077(3) Uani 1 1 d . . . . . H7AA H -0.0391 0.2142 0.8961 0.092 Uiso 1 1 calc R U . . . C8A C 0.0238(5) 0.2565(5) 0.8302(8) 0.079(3) Uani 1 1 d . . . . . H8AA H 0.0408 0.2665 0.8981 0.094 Uiso 1 1 calc R U . . . N9A N -0.0971(5) 0.1785(4) 0.7313(8) 0.078(2) Uani 1 1 d . . . . . C10A C -0.1323(10) 0.1687(7) 0.6396(15) 0.143(10) Uani 1 1 d . . . . . H10A H -0.1371 0.1944 0.5939 0.215 Uiso 1 1 calc R U . . . H10B H -0.1749 0.1583 0.6609 0.215 Uiso 1 1 calc R U . . . H10C H -0.1103 0.1462 0.5983 0.215 Uiso 1 1 calc R U . . . C11A C -0.1223(8) 0.1632(5) 0.8364(11) 0.099(5) Uani 1 1 d . . . . . H11A H -0.0946 0.1403 0.8652 0.149 Uiso 1 1 calc R U . . . H11B H -0.1660 0.1521 0.8253 0.149 Uiso 1 1 calc R U . . . H11C H -0.1232 0.1871 0.8887 0.149 Uiso 1 1 calc R U . . . C12A C 0.2289(5) 0.3977(3) 0.6633(8) 0.0587(19) Uani 1 1 d . . . . . C13A C 0.2436(5) 0.4037(3) 0.5561(9) 0.066(2) Uani 1 1 d . . . . . H13A H 0.2229 0.3861 0.5029 0.079 Uiso 1 1 calc R U . . . C14A C 0.2876(6) 0.4345(3) 0.5205(9) 0.069(2) Uani 1 1 d . . . . . H14A H 0.2945 0.4388 0.4445 0.082 Uiso 1 1 calc R U . . . C15A C 0.3207(6) 0.4583(4) 0.5967(11) 0.078(3) Uani 1 1 d . . . . . C16A C 0.3029(8) 0.4525(5) 0.7080(12) 0.090(4) Uani 1 1 d . . . . . H16A H 0.3215 0.4712 0.7612 0.108 Uiso 1 1 calc R U . . . C17A C 0.2611(7) 0.4220(4) 0.7431(10) 0.085(4) Uani 1 1 d . . . . . H17A H 0.2539 0.4175 0.8189 0.102 Uiso 1 1 calc R U . . . N18A N 0.3645(7) 0.4893(5) 0.5603(13) 0.111(5) Uani 1 1 d . . . . . C19A C 0.3867(10) 0.4891(6) 0.4514(16) 0.121(6) Uani 1 1 d . . . . . H19A H 0.4083 0.4618 0.4364 0.181 Uiso 1 1 calc R U . . . H19B H 0.4171 0.5129 0.4414 0.181 Uiso 1 1 calc R U . . . H19C H 0.3502 0.4927 0.4008 0.181 Uiso 1 1 calc R U . . . C20A C 0.4041(12) 0.5092(9) 0.6438(18) 0.152(10) Uani 1 1 d . . . . . H20A H 0.4329 0.5302 0.6098 0.228 Uiso 1 1 calc R U . . . H20B H 0.3767 0.5239 0.6966 0.228 Uiso 1 1 calc R U . . . H20C H 0.4297 0.4872 0.6815 0.228 Uiso 1 1 calc R U . . . N21A N 0.1503(4) 0.3126(2) 0.4342(5) 0.0517(15) Uani 1 1 d . . . . . C21A C 0.1210(6) 0.3324(4) 0.3608(7) 0.078(3) Uani 1 1 d . . . . . H21A H 0.1296 0.3273 0.2857 0.093 Uiso 1 1 calc R U . . . C22A C 0.0720(7) 0.3642(4) 0.3948(8) 0.084(4) Uani 1 1 d . . . . . H22A H 0.0458 0.3782 0.3414 0.100 Uiso 1 1 calc R U . . . N22A N 0.0652(4) 0.3726(2) 0.4964(6) 0.0608(18) Uani 1 1 d . . . . . C23A C 0.1970(4) 0.2811(2) 0.4057(6) 0.0458(15) Uani 1 1 d . . . . . C24A C 0.2211(4) 0.2561(3) 0.4889(6) 0.0512(16) Uani 1 1 d . . . . . H24A H 0.2071 0.2608 0.5616 0.061 Uiso 1 1 calc R U . . . C25A C 0.2656(4) 0.2241(3) 0.4687(7) 0.060(2) Uani 1 1 d . . . . . H25A H 0.2805 0.2065 0.5273 0.072 Uiso 1 1 calc R U . . . C26A C 0.2892(4) 0.2170(3) 0.3620(7) 0.0558(19) Uani 1 1 d . . . . . C27A C 0.2658(4) 0.2430(3) 0.2768(7) 0.0553(18) Uani 1 1 d . . . . . H27A H 0.2805 0.2392 0.2042 0.066 Uiso 1 1 calc R U . . . C28A C 0.2206(4) 0.2745(3) 0.3002(7) 0.0556(18) Uani 1 1 d . . . . . H28A H 0.2052 0.2924 0.2424 0.067 Uiso 1 1 calc R U . . . N29A N 0.3332(4) 0.1852(3) 0.3394(8) 0.070(2) Uani 1 1 d . . . . . C30A C 0.3677(6) 0.1650(6) 0.4247(14) 0.097(4) Uani 1 1 d . . . . . H30A H 0.4001 0.1849 0.4542 0.145 Uiso 1 1 calc R U . . . H30B H 0.3890 0.1392 0.3965 0.145 Uiso 1 1 calc R U . . . H30C H 0.3381 0.1568 0.4829 0.145 Uiso 1 1 calc R U . . . C31A C 0.3549(5) 0.1783(5) 0.2247(11) 0.081(3) Uani 1 1 d . . . . . H31A H 0.3176 0.1723 0.1774 0.122 Uiso 1 1 calc R U . . . H31B H 0.3847 0.1539 0.2226 0.122 Uiso 1 1 calc R U . . . H31C H 0.3767 0.2043 0.1986 0.122 Uiso 1 1 calc R U . . . C32A C 0.0255(6) 0.4045(3) 0.5398(8) 0.067(3) Uani 1 1 d . . . . . C33A C 0.0192(4) 0.4090(3) 0.6483(7) 0.0486(16) Uani 1 1 d . . . . . H33A H 0.0434 0.3905 0.6949 0.058 Uiso 1 1 calc R U . . . C34A C -0.0220(4) 0.4402(3) 0.6977(8) 0.0543(18) Uani 1 1 d . . . . . H34A H -0.0226 0.4430 0.7751 0.065 Uiso 1 1 calc R U . . . C35A C -0.0604(5) 0.4659(4) 0.6340(9) 0.068(2) Uani 1 1 d . . . . . C36A C -0.0543(9) 0.4601(5) 0.5194(11) 0.109(6) Uani 1 1 d . . . . . H36A H -0.0812 0.4764 0.4717 0.130 Uiso 1 1 calc R U . . . C37A C -0.0114(11) 0.4320(6) 0.4746(10) 0.135(9) Uani 1 1 d . . . . . H37A H -0.0066 0.4313 0.3974 0.162 Uiso 1 1 calc R U . . . N38A N -0.0994(6) 0.4966(4) 0.6796(10) 0.092(3) Uani 1 1 d . . . . . C39A C -0.1107(10) 0.4953(6) 0.7948(15) 0.111(5) Uani 1 1 d . . . . . H39A H -0.1215 0.4658 0.8165 0.166 Uiso 1 1 calc R U . . . H39B H -0.1465 0.5145 0.8124 0.166 Uiso 1 1 calc R U . . . H39C H -0.0720 0.5046 0.8345 0.166 Uiso 1 1 calc R U . . . C40A C -0.1392(9) 0.5244(6) 0.6093(18) 0.115(6) Uani 1 1 d . . . . . H40A H -0.1222 0.5243 0.5349 0.172 Uiso 1 1 calc R U . . . H40B H -0.1385 0.5539 0.6382 0.172 Uiso 1 1 calc R U . . . H40C H -0.1835 0.5137 0.6079 0.172 Uiso 1 1 calc R U . . . Cu1B Cu 0.62296(6) 0.16842(4) 0.57987(10) 0.0502(4) Uani 1 1 d . . . . . N1B N 0.6506(3) 0.1979(2) 0.7187(5) 0.0482(13) Uani 1 1 d . . . . . C1B C 0.6198(4) 0.1827(3) 0.8008(7) 0.0534(18) Uani 1 1 d . . . . . H1BA H 0.6289 0.1931 0.8724 0.064 Uiso 1 1 calc R U . . . C2B C 0.5713(4) 0.1497(3) 0.7853(7) 0.0552(18) Uani 1 1 d . . . . . H2BA H 0.5479 0.1380 0.8446 0.066 Uiso 1 1 calc R U . . . N2B N 0.5623(3) 0.1375(2) 0.6867(6) 0.0515(14) Uani 1 1 d . . . . . C3B C 0.7000(4) 0.2292(3) 0.7276(7) 0.0524(17) Uani 1 1 d . . . . . C4B C 0.7183(6) 0.2505(4) 0.6344(8) 0.076(3) Uani 1 1 d . . . . . H4BA H 0.6975 0.2437 0.5670 0.091 Uiso 1 1 calc R U . . . C5B C 0.7659(7) 0.2814(4) 0.6354(9) 0.083(3) Uani 1 1 d . . . . . H5BA H 0.7773 0.2956 0.5695 0.100 Uiso 1 1 calc R U . . . C6B C 0.7969(5) 0.2917(3) 0.7317(8) 0.062(2) Uani 1 1 d D . . . . C7B C 0.7790(6) 0.2712(4) 0.8215(9) 0.075(3) Uani 1 1 d D . . . . H7BA H 0.7994 0.2788 0.8887 0.090 Uiso 1 1 calc R U . . . C8B C 0.7314(5) 0.2388(4) 0.8231(8) 0.063(2) Uani 1 1 d . . . . . H8BA H 0.7215 0.2241 0.8890 0.076 Uiso 1 1 calc R U . . . N9B N 0.8441(5) 0.3237(4) 0.7307(9) 0.076(3) Uani 0.85(2) 1 d D U P A 1 C10B C 0.8702(8) 0.3389(5) 0.6369(13) 0.086(4) Uani 0.85(2) 1 d D U P A 1 H10D H 0.9021 0.3611 0.6548 0.129 Uiso 0.85(2) 1 calc R U P A 1 H10E H 0.8910 0.3152 0.5980 0.129 Uiso 0.85(2) 1 calc R U P A 1 H10F H 0.8363 0.3513 0.5904 0.129 Uiso 0.85(2) 1 calc R U P A 1 C11B C 0.8751(7) 0.3350(5) 0.8290(13) 0.083(4) Uani 0.85(2) 1 d D U P A 1 H11D H 0.9126 0.3530 0.8135 0.124 Uiso 0.85(2) 1 d R U P A 1 H11E H 0.8452 0.3511 0.8750 0.124 Uiso 0.85(2) 1 d R U P A 1 H11F H 0.8890 0.3089 0.8674 0.124 Uiso 0.85(2) 1 d R U P A 1 N9" N 0.8529(15) 0.3132(14) 0.763(3) 0.087(11) Uiso 0.15(2) 1 d D U P A 2 C10" C 0.899(3) 0.324(3) 0.687(5) 0.090(11) Uiso 0.15(2) 1 d D U P A 2 H10G H 0.8845 0.3143 0.6145 0.136 Uiso 0.15(2) 1 calc R U P A 2 H10H H 0.9040 0.3555 0.6864 0.136 Uiso 0.15(2) 1 calc R U P A 2 H10I H 0.9395 0.3104 0.7067 0.136 Uiso 0.15(2) 1 calc R U P A 2 C11" C 0.865(3) 0.324(2) 0.871(3) 0.082(12) Uiso 0.15(2) 1 d D U P A 2 H11G H 0.8809 0.2981 0.9052 0.123 Uiso 0.15(2) 1 d R U P A 2 H11H H 0.8260 0.3341 0.9087 0.123 Uiso 0.15(2) 1 d R U P A 2 H11I H 0.8975 0.3470 0.8750 0.123 Uiso 0.15(2) 1 d R U P A 2 C12B C 0.5194(5) 0.1050(3) 0.6595(9) 0.062(2) Uani 1 1 d . . . . . C13B C 0.5090(6) 0.0977(4) 0.5483(12) 0.080(3) Uani 1 1 d . . . . . H13B H 0.5304 0.1149 0.4957 0.096 Uiso 1 1 calc R U . . . C14B C 0.4684(7) 0.0662(5) 0.5152(12) 0.087(3) Uani 1 1 d . . . . . H14B H 0.4610 0.0627 0.4388 0.105 Uiso 1 1 calc R U . . . C15B C 0.4357(8) 0.0376(4) 0.5891(12) 0.091(4) Uani 1 1 d . . . . . C16B C 0.4520(7) 0.0439(4) 0.6981(11) 0.086(3) Uani 1 1 d . . . . . H16B H 0.4366 0.0239 0.7505 0.103 Uiso 1 1 calc R U . . . C17B C 0.4894(7) 0.0778(4) 0.7346(11) 0.087(4) Uani 1 1 d . . . . . H17B H 0.4947 0.0827 0.8110 0.104 Uiso 1 1 calc R U . . . N18B N 0.3993(10) 0.0050(5) 0.5532(13) 0.128(6) Uani 1 1 d . . . . . C19B C 0.3873(11) -0.0022(7) 0.4386(17) 0.130(8) Uani 1 1 d . . . . . H19D H 0.3488 0.0137 0.4156 0.195 Uiso 1 1 calc R U . . . H19E H 0.3808 -0.0330 0.4255 0.195 Uiso 1 1 calc R U . . . H19F H 0.4242 0.0079 0.3966 0.195 Uiso 1 1 calc R U . . . C20B C 0.3773(11) -0.0255(6) 0.6306(16) 0.126(8) Uani 1 1 d . . . . . H20D H 0.4109 -0.0469 0.6446 0.190 Uiso 1 1 calc R U . . . H20E H 0.3387 -0.0398 0.6016 0.190 Uiso 1 1 calc R U . . . H20F H 0.3669 -0.0107 0.6990 0.190 Uiso 1 1 calc R U . . . N21B N 0.6026(3) 0.1892(2) 0.4290(6) 0.0503(14) Uani 1 1 d . . . . . C21B C 0.6379(5) 0.1698(3) 0.3534(7) 0.061(2) Uani 1 1 d . . . . . H21B H 0.6327 0.1768 0.2781 0.073 Uiso 1 1 calc R U . . . C22B C 0.6833(5) 0.1389(3) 0.3879(9) 0.067(2) Uani 1 1 d . . . . . H22B H 0.7097 0.1242 0.3372 0.080 Uiso 1 1 calc R U . . . N22B N 0.6875(3) 0.1312(2) 0.4942(6) 0.0537(15) Uani 1 1 d . . . . . C23B C 0.5542(4) 0.2189(2) 0.4012(6) 0.0473(15) Uani 1 1 d . . . . . C24B C 0.5284(4) 0.2451(3) 0.4838(7) 0.0514(17) Uani 1 1 d . . . . . H24B H 0.5435 0.2413 0.5568 0.062 Uiso 1 1 calc R U . . . C25B C 0.4813(5) 0.2766(3) 0.4631(8) 0.060(2) Uani 1 1 d . . . . . H25B H 0.4655 0.2941 0.5207 0.072 Uiso 1 1 calc R U . . . C26B C 0.4587(4) 0.2816(3) 0.3587(7) 0.0526(17) Uani 1 1 d . . . . . C27B C 0.4838(4) 0.2540(3) 0.2735(6) 0.0529(17) Uani 1 1 d . . . . . H27B H 0.4680 0.2570 0.2006 0.064 Uiso 1 1 calc R U . . . C28B C 0.5294(5) 0.2240(3) 0.2960(7) 0.0562(18) Uani 1 1 d . . . . . H28B H 0.5447 0.2061 0.2388 0.067 Uiso 1 1 calc R U . . . N29B N 0.4154(4) 0.3130(4) 0.3323(7) 0.073(2) Uani 1 1 d . . . . . C30B C 0.3805(7) 0.3359(6) 0.4189(13) 0.097(5) Uani 1 1 d . . . . . H30D H 0.3625 0.3149 0.4702 0.145 Uiso 1 1 calc R U . . . H30E H 0.3455 0.3528 0.3859 0.145 Uiso 1 1 calc R U . . . H30F H 0.4101 0.3551 0.4582 0.145 Uiso 1 1 calc R U . . . C31B C 0.3937(6) 0.3205(4) 0.2197(11) 0.080(3) Uani 1 1 d . . . . . H31D H 0.4259 0.3094 0.1690 0.120 Uiso 1 1 calc R U . . . H31E H 0.3880 0.3515 0.2077 0.120 Uiso 1 1 calc R U . . . H31F H 0.3527 0.3057 0.2069 0.120 Uiso 1 1 calc R U . . . C32B C 0.7295(4) 0.1008(3) 0.5386(8) 0.0544(18) Uani 1 1 d . . . . . C33B C 0.7262(4) 0.0934(3) 0.6508(8) 0.0562(19) Uani 1 1 d . . . . . H33B H 0.6968 0.1094 0.6935 0.067 Uiso 1 1 calc R U . . . C34B C 0.7657(5) 0.0625(3) 0.7015(9) 0.062(2) Uani 1 1 d . . . . . H34B H 0.7655 0.0601 0.7790 0.074 Uiso 1 1 calc R U . . . C35B C 0.8051(5) 0.0354(4) 0.6421(11) 0.073(3) Uani 1 1 d . . . . . C36B C 0.8083(7) 0.0436(5) 0.5301(11) 0.095(4) Uani 1 1 d . . . . . H36B H 0.8374 0.0272 0.4875 0.114 Uiso 1 1 calc R U . . . C37B C 0.7716(6) 0.0737(5) 0.4796(10) 0.085(3) Uani 1 1 d . . . . . H37B H 0.7741 0.0768 0.4024 0.102 Uiso 1 1 calc R U . . . N38B N 0.8435(6) 0.0044(4) 0.6905(9) 0.087(3) Uani 1 1 d . . . . . C39B C 0.8464(9) 0.0024(6) 0.8054(14) 0.108(5) Uani 1 1 d . . . . . H39D H 0.8752 -0.0210 0.8281 0.162 Uiso 1 1 calc R U . . . H39E H 0.8627 0.0298 0.8344 0.162 Uiso 1 1 calc R U . . . H39F H 0.8033 -0.0029 0.8339 0.162 Uiso 1 1 calc R U . . . C40B C 0.8779(10) -0.0264(6) 0.6225(16) 0.123(7) Uani 1 1 d . . . . . H40D H 0.9168 -0.0129 0.5940 0.184 Uiso 1 1 calc R U . . . H40E H 0.8502 -0.0355 0.5613 0.184 Uiso 1 1 calc R U . . . H40F H 0.8899 -0.0516 0.6666 0.184 Uiso 1 1 calc R U . . . B10 B 0.5329(8) 0.3898(6) 0.6154(17) 0.094(5) Uani 1 1 d . . . . . F11 F 0.5653(10) 0.4136(6) 0.6865(14) 0.194(8) Uani 1 1 d . . . . . F12 F 0.4832(8) 0.3685(5) 0.6575(19) 0.198(9) Uani 1 1 d . . . . . F13 F 0.5751(7) 0.3515(4) 0.5928(15) 0.156(5) Uani 1 1 d . . . . . F14 F 0.5248(8) 0.4065(4) 0.5155(11) 0.139(4) Uani 1 1 d . . . . . B20 B 0.2280(8) 0.4003(6) 0.1258(14) 0.119(4) Uani 0.549(11) 1 d D U P B 1 F21 F 0.1684(9) 0.4210(6) 0.1205(17) 0.139(5) Uani 0.549(11) 1 d D U P B 1 F22 F 0.2415(6) 0.3893(4) 0.2349(11) 0.089(3) Uani 0.549(11) 1 d D U P B 1 F23 F 0.2746(10) 0.4285(7) 0.0822(18) 0.158(6) Uani 0.549(11) 1 d D U P B 1 F24 F 0.2280(11) 0.3627(6) 0.0633(15) 0.140(5) Uani 0.549(11) 1 d D U P B 1 B20' B 0.2030(8) 0.3830(5) 0.1171(14) 0.095(5) Uiso 0.451(11) 1 d D U P B 2 F21' F 0.1671(8) 0.4080(5) 0.1888(15) 0.098(4) Uiso 0.451(11) 1 d D U P B 2 F22' F 0.2579(8) 0.3684(6) 0.1723(17) 0.113(5) Uiso 0.451(11) 1 d D U P B 2 F23' F 0.2216(11) 0.4059(7) 0.0253(16) 0.135(5) Uiso 0.451(11) 1 d D U P B 2 F24' F 0.1649(7) 0.3473(5) 0.0858(14) 0.087(4) Uiso 0.451(11) 1 d D U P B 2 C50 C 0.6963(12) 0.4109(18) 0.561(3) 0.24(3) Uani 0.76(3) 1 d D . P C 1 H50A H 0.6692 0.4349 0.5339 0.289 Uiso 0.76(3) 1 calc R U P C 1 H50B H 0.6689 0.3914 0.6042 0.289 Uiso 0.76(3) 1 calc R U P C 1 Cl51 Cl 0.7273(4) 0.3825(3) 0.4483(5) 0.107(2) Uani 0.76(3) 1 d D U P C 1 Cl52 Cl 0.7574(5) 0.4314(4) 0.6451(7) 0.121(3) Uani 0.76(3) 1 d D U P C 1 C50' C 0.716(3) 0.386(3) 0.608(5) 0.12(3) Uiso 0.24(3) 1 d D . P C 2 H50C H 0.6777 0.4048 0.5989 0.147 Uiso 0.24(3) 1 calc R U P C 2 H50D H 0.7042 0.3614 0.6542 0.147 Uiso 0.24(3) 1 calc R U P C 2 Cl53 Cl 0.7401(17) 0.3674(12) 0.478(3) 0.134(8) Uiso 0.24(3) 1 d D U P C 2 Cl54 Cl 0.7781(19) 0.4155(12) 0.672(3) 0.139(8) Uiso 0.24(3) 1 d D U P C 2 C60 C 0.0343(10) 0.3895(6) 0.1014(15) 0.109(5) Uani 1 1 d . . . . . H60A H 0.0348 0.3623 0.1439 0.131 Uiso 1 1 calc R U . . . H60B H 0.0771 0.4032 0.1075 0.131 Uiso 1 1 calc R U . . . Cl61 Cl 0.0130(2) 0.3789(2) -0.0437(3) 0.1220(16) Uani 1 1 d . . . . . Cl62 Cl -0.0279(3) 0.4256(2) 0.1514(5) 0.1417(19) 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 Cu1A 0.0633(7) 0.0502(6) 0.0331(6) 0.0037(4) 0.0044(5) 0.0058(5) N1A 0.049(3) 0.047(3) 0.034(3) 0.000(2) 0.000(2) 0.010(2) C1A 0.072(5) 0.056(4) 0.020(3) 0.000(3) 0.000(3) -0.003(4) C2A 0.057(4) 0.056(4) 0.041(4) 0.001(3) -0.001(3) 0.007(3) N2A 0.051(3) 0.048(3) 0.058(4) -0.001(3) 0.003(3) 0.004(3) C3A 0.051(3) 0.050(3) 0.030(3) 0.005(3) 0.003(3) 0.006(3) C4A 0.079(6) 0.086(6) 0.031(4) 0.002(4) 0.002(3) -0.025(5) C5A 0.086(7) 0.118(9) 0.039(4) -0.009(5) 0.000(4) -0.042(7) C6A 0.064(5) 0.067(5) 0.051(5) 0.001(4) -0.003(4) -0.002(4) C7A 0.075(6) 0.112(8) 0.044(5) 0.023(5) 0.002(4) -0.028(6) C8A 0.075(6) 0.124(9) 0.037(4) 0.018(5) -0.004(4) -0.036(6) N9A 0.078(5) 0.097(6) 0.059(5) 0.007(4) 0.008(4) -0.028(5) C10A 0.143(15) 0.188(19) 0.100(12) -0.064(12) 0.040(11) -0.114(15) C11A 0.118(11) 0.120(11) 0.061(7) 0.003(6) 0.019(7) -0.046(9) C12A 0.066(5) 0.055(4) 0.055(5) -0.003(4) 0.005(4) -0.002(4) C13A 0.072(5) 0.056(4) 0.070(6) 0.005(4) 0.008(4) 0.002(4) C14A 0.091(7) 0.062(5) 0.053(5) 0.012(4) 0.016(5) -0.003(5) C15A 0.076(6) 0.078(6) 0.081(7) 0.022(6) 0.013(5) -0.011(5) C16A 0.107(9) 0.089(7) 0.074(7) -0.009(6) 0.017(7) -0.033(7) C17A 0.110(9) 0.090(7) 0.055(5) -0.001(5) 0.021(6) -0.042(7) N18A 0.113(9) 0.111(8) 0.108(10) 0.008(7) 0.039(8) -0.051(8) C19A 0.137(14) 0.115(12) 0.110(12) -0.011(10) 0.039(11) -0.060(11) C20A 0.156(18) 0.19(2) 0.106(14) 0.024(14) 0.013(13) -0.090(18) N21A 0.073(4) 0.048(3) 0.034(3) 0.003(2) 0.004(3) 0.003(3) C21A 0.098(7) 0.106(8) 0.028(4) 0.000(4) 0.003(4) 0.048(7) C22A 0.122(9) 0.081(6) 0.048(5) 0.018(4) 0.001(5) 0.055(7) N22A 0.078(5) 0.057(4) 0.047(4) 0.003(3) 0.016(3) 0.020(4) C23A 0.046(3) 0.053(4) 0.038(3) -0.003(3) 0.003(3) -0.003(3) C24A 0.060(4) 0.060(4) 0.033(3) -0.004(3) 0.002(3) 0.004(4) C25A 0.058(4) 0.078(5) 0.044(4) -0.007(4) -0.004(3) 0.017(4) C26A 0.046(4) 0.071(5) 0.051(4) -0.020(4) -0.002(3) -0.007(4) C27A 0.057(4) 0.063(4) 0.047(4) -0.018(3) 0.011(3) -0.005(4) C28A 0.061(4) 0.062(5) 0.043(4) 0.003(3) 0.003(3) -0.004(4) N29A 0.056(4) 0.088(6) 0.067(5) -0.019(4) 0.001(4) 0.015(4) C30A 0.068(7) 0.127(12) 0.096(10) -0.014(8) -0.020(6) 0.022(7) C31A 0.060(5) 0.103(8) 0.081(7) -0.042(6) 0.003(5) 0.008(5) C32A 0.086(6) 0.063(5) 0.054(5) 0.010(4) 0.005(4) 0.036(5) C33A 0.051(4) 0.049(4) 0.046(4) -0.001(3) 0.005(3) 0.003(3) C34A 0.058(4) 0.053(4) 0.053(4) -0.002(3) 0.007(3) 0.000(3) C35A 0.073(6) 0.070(5) 0.063(6) -0.010(4) 0.005(4) 0.021(5) C36A 0.146(13) 0.120(10) 0.060(6) 0.003(6) -0.002(7) 0.090(11) C37A 0.199(18) 0.165(15) 0.041(5) 0.016(7) 0.009(8) 0.127(15) N38A 0.107(8) 0.087(6) 0.084(7) 0.000(5) 0.027(6) 0.037(6) C39A 0.123(12) 0.105(10) 0.105(11) -0.017(9) 0.024(10) 0.033(10) C40A 0.106(11) 0.106(10) 0.132(14) -0.005(10) 0.009(10) 0.050(9) Cu1B 0.0536(7) 0.0576(7) 0.0393(6) -0.0037(4) -0.0020(5) 0.0002(5) N1B 0.049(3) 0.056(3) 0.040(3) -0.005(3) 0.004(2) 0.004(3) C1B 0.059(4) 0.063(4) 0.038(4) -0.009(3) -0.006(3) 0.012(4) C2B 0.055(4) 0.060(4) 0.051(4) 0.009(3) 0.007(3) 0.011(3) N2B 0.048(3) 0.055(3) 0.051(4) 0.003(3) -0.003(3) 0.005(3) C3B 0.058(4) 0.055(4) 0.044(4) -0.012(3) -0.009(3) 0.009(3) C4B 0.084(6) 0.106(8) 0.038(4) -0.003(5) -0.005(4) -0.035(6) C5B 0.096(8) 0.101(8) 0.053(5) -0.008(5) -0.003(5) -0.044(7) C6B 0.056(4) 0.064(5) 0.066(6) -0.009(4) -0.002(4) -0.008(4) C7B 0.088(7) 0.075(6) 0.061(6) -0.016(5) -0.031(5) -0.001(5) C8B 0.069(5) 0.078(6) 0.042(4) 0.001(4) -0.007(4) -0.003(4) N9B 0.084(6) 0.071(6) 0.072(7) -0.008(5) -0.025(5) -0.022(5) C10B 0.087(8) 0.088(8) 0.083(9) -0.007(7) -0.001(7) -0.028(7) C11B 0.088(8) 0.087(8) 0.073(9) -0.004(6) -0.030(7) -0.019(7) C12B 0.057(4) 0.051(4) 0.077(6) 0.013(4) -0.010(4) -0.002(4) C13B 0.076(6) 0.077(6) 0.087(8) 0.001(6) -0.011(6) -0.019(5) C14B 0.082(7) 0.091(8) 0.088(8) -0.003(6) -0.023(6) -0.018(6) C15B 0.111(9) 0.070(6) 0.091(9) 0.023(6) -0.030(7) -0.026(6) C16B 0.101(8) 0.087(7) 0.069(7) 0.008(6) -0.007(6) -0.019(7) C17B 0.108(9) 0.082(7) 0.070(7) 0.016(5) -0.004(6) -0.034(7) N18B 0.169(14) 0.112(9) 0.101(10) 0.025(8) -0.061(10) -0.047(10) C19B 0.145(16) 0.122(13) 0.121(14) 0.016(11) -0.057(13) -0.041(12) C20B 0.161(16) 0.113(11) 0.105(12) 0.031(9) -0.035(11) -0.079(12) N21B 0.051(3) 0.057(3) 0.042(3) 0.001(3) -0.005(3) -0.010(3) C21B 0.087(6) 0.062(5) 0.034(4) -0.005(3) -0.004(4) -0.003(4) C22B 0.069(5) 0.068(5) 0.064(6) -0.013(4) 0.011(4) 0.004(4) N22B 0.055(4) 0.054(3) 0.052(4) -0.008(3) -0.002(3) -0.003(3) C23B 0.053(4) 0.049(4) 0.040(4) -0.005(3) 0.003(3) -0.010(3) C24B 0.051(4) 0.064(4) 0.040(4) 0.001(3) 0.000(3) 0.002(3) C25B 0.064(5) 0.066(5) 0.052(5) -0.008(4) 0.004(4) 0.007(4) C26B 0.044(3) 0.063(4) 0.051(4) 0.008(3) 0.002(3) 0.003(3) C27B 0.062(4) 0.061(4) 0.035(3) -0.001(3) -0.005(3) -0.005(4) C28B 0.071(5) 0.055(4) 0.043(4) -0.004(3) 0.000(3) -0.005(4) N29B 0.064(4) 0.098(6) 0.055(4) 0.007(4) -0.003(4) 0.022(4) C30B 0.076(7) 0.130(12) 0.084(9) 0.017(7) 0.017(6) 0.043(8) C31B 0.069(6) 0.093(7) 0.077(7) 0.021(6) -0.020(5) 0.005(6) C32B 0.050(4) 0.054(4) 0.059(5) -0.007(3) -0.001(3) 0.011(3) C33B 0.063(5) 0.049(4) 0.056(5) -0.001(3) -0.013(4) 0.001(3) C34B 0.060(5) 0.065(5) 0.060(5) -0.001(4) -0.007(4) 0.006(4) C35B 0.060(5) 0.077(6) 0.080(7) -0.006(5) -0.007(5) 0.012(5) C36B 0.096(8) 0.121(10) 0.068(7) 0.005(7) 0.011(6) 0.061(8) C37B 0.078(6) 0.114(9) 0.063(6) -0.010(6) 0.005(5) 0.039(7) N38B 0.088(6) 0.103(7) 0.070(6) -0.006(5) -0.004(5) 0.017(6) C39B 0.115(11) 0.111(11) 0.097(10) -0.011(8) -0.032(9) 0.031(9) C40B 0.142(14) 0.121(12) 0.105(12) -0.045(10) -0.035(11) 0.061(12) B10 0.081(8) 0.090(9) 0.111(13) 0.007(9) -0.023(8) -0.022(8) F11 0.220(17) 0.221(17) 0.142(13) -0.061(12) 0.032(12) -0.064(15) F12 0.159(12) 0.144(10) 0.29(2) 0.035(13) 0.076(14) -0.042(10) F13 0.133(9) 0.129(8) 0.205(16) 0.029(10) -0.028(10) -0.008(8) F14 0.178(11) 0.132(8) 0.106(8) 0.023(6) 0.000(8) 0.001(8) B20 0.115(7) 0.120(8) 0.121(8) 0.005(7) -0.001(7) 0.013(7) F21 0.135(9) 0.137(9) 0.145(9) 0.000(9) -0.005(8) 0.009(8) F22 0.084(6) 0.090(6) 0.093(7) 0.001(6) -0.018(5) 0.019(6) F23 0.141(11) 0.158(12) 0.174(13) -0.006(12) 0.003(11) -0.018(11) F24 0.148(8) 0.141(8) 0.132(8) -0.002(8) -0.003(8) 0.009(8) C50 0.081(14) 0.34(7) 0.30(6) -0.23(6) 0.04(2) -0.05(3) Cl51 0.124(4) 0.122(5) 0.075(3) -0.003(3) -0.005(3) 0.001(4) Cl52 0.133(5) 0.125(6) 0.105(4) -0.017(4) 0.001(4) -0.023(5) C60 0.130(13) 0.096(9) 0.102(11) 0.001(8) 0.007(10) 0.019(9) Cl61 0.109(3) 0.191(5) 0.0661(18) -0.010(2) -0.0037(17) -0.014(3) Cl62 0.130(4) 0.166(5) 0.129(4) -0.018(4) 0.018(3) 0.023(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N2A Cu1A N21A 126.2(3) N2A Cu1A N1A 81.9(3) N21A Cu1A N1A 133.2(3) N2A Cu1A N22A 116.4(3) N21A Cu1A N22A 82.9(3) N1A Cu1A N22A 120.5(3) C1A N1A C3A 121.1(6) C1A N1A Cu1A 111.8(5) C3A N1A Cu1A 127.1(5) N1A C1A C2A 116.4(7) N2A C2A C1A 119.1(7) C2A N2A C12A 124.0(8) C2A N2A Cu1A 110.7(6) C12A N2A Cu1A 125.2(6) C4A C3A C8A 117.3(8) C4A C3A N1A 117.3(7) C8A C3A N1A 125.4(7) C5A C4A C3A 121.3(8) C4A C5A C6A 122.5(9) C7A C6A N9A 121.6(9) C7A C6A C5A 116.4(9) N9A C6A C5A 121.9(9) C6A C7A C8A 121.7(9) C7A C8A C3A 120.3(9) C10A N9A C6A 122.7(11) C10A N9A C11A 116.7(11) C6A N9A C11A 118.5(10) C13A C12A C17A 119.1(9) C13A C12A N2A 118.5(9) C17A C12A N2A 122.3(9) C12A C13A C14A 123.3(11) C15A C14A C13A 118.9(10) C14A C15A N18A 118.6(12) C14A C15A C16A 116.5(10) N18A C15A C16A 124.6(14) C17A C16A C15A 124.4(13) C16A C17A C12A 117.4(11) C15A N18A C19A 121.2(14) C15A N18A C20A 116.0(14) C19A N18A C20A 118.4(13) C21A N21A C23A 119.7(7) C21A N21A Cu1A 111.2(6) C23A N21A Cu1A 128.9(5) N21A C21A C22A 117.5(8) N22A C22A C21A 119.5(9) C22A N22A C32A 125.9(9) C22A N22A Cu1A 108.6(6) C32A N22A Cu1A 125.4(7) C24A C23A C28A 118.2(8) C24A C23A N21A 116.9(7) C28A C23A N21A 124.9(7) C23A C24A C25A 121.0(7) C24A C25A C26A 121.1(8) N29A C26A C27A 119.4(8) N29A C26A C25A 122.3(9) C27A C26A C25A 118.3(8) C28A C27A C26A 119.0(8) C27A C28A C23A 122.5(8) C26A N29A C30A 120.5(10) C26A N29A C31A 120.0(10) C30A N29A C31A 118.3(10) C33A C32A C37A 116.2(9) C33A C32A N22A 121.0(8) C37A C32A N22A 122.8(10) C32A C33A C34A 123.6(8) C35A C34A C33A 120.4(9) C34A C35A N38A 121.3(11) C34A C35A C36A 115.3(9) N38A C35A C36A 123.3(11) C37A C36A C35A 122.9(11) C36A C37A C32A 121.4(11) C35A N38A C39A 119.0(12) C35A N38A C40A 120.2(12) C39A N38A C40A 119.6(12) N21B Cu1B N1B 133.6(3) N21B Cu1B N2B 127.6(3) N1B Cu1B N2B 81.4(3) N21B Cu1B N22B 81.0(3) N1B Cu1B N22B 120.2(3) N2B Cu1B N22B 117.7(3) C1B N1B C3B 124.0(7) C1B N1B Cu1B 110.5(6) C3B N1B Cu1B 125.4(5) N1B C1B C2B 120.7(7) N2B C2B C1B 115.5(8) C2B N2B C12B 122.2(8) C2B N2B Cu1B 111.9(6) C12B N2B Cu1B 125.8(7) C8B C3B C4B 117.9(9) C8B C3B N1B 123.8(9) C4B C3B N1B 118.3(7) C3B C4B C5B 122.2(9) C6B C5B C4B 120.0(10) C7B C6B C5B 117.6(9) C7B C6B N9" 104.1(15) C5B C6B N9" 137.0(16) C7B C6B N9B 123.6(9) C5B C6B N9B 118.8(9) C6B C7B C8B 123.9(8) C3B C8B C7B 118.3(9) C10B N9B C6B 122.8(9) C10B N9B C11B 116.8(12) C6B N9B C11B 119.1(10) C11" N9" C10" 118(2) C11" N9" C6B 121.5(15) C10" N9" C6B 120.8(15) N2B C12B C13B 116.5(9) N2B C12B C17B 125.0(11) C13B C12B C17B 118.4(10) C14B C13B C12B 120.0(13) C13B C14B C15B 123.8(14) N18B C15B C16B 123.7(13) N18B C15B C14B 122.1(15) C16B C15B C14B 113.8(11) C17B C16B C15B 123.3(12) C16B C17B C12B 120.2(12) C15B N18B C20B 118.3(14) C15B N18B C19B 121.9(16) C20B N18B C19B 119.5(15) C21B N21B C23B 121.9(7) C21B N21B Cu1B 112.6(6) C23B N21B Cu1B 125.4(6) N21B C21B C22B 118.3(8) N22B C22B C21B 116.9(8) C22B N22B C32B 122.5(8) C22B N22B Cu1B 111.2(6) C32B N22B Cu1B 126.2(6) C28B C23B N21B 123.8(7) C28B C23B C24B 117.2(8) N21B C23B C24B 119.0(7) C25B C24B C23B 123.0(8) C26B C25B C24B 118.6(8) C25B C26B N29B 121.4(9) C25B C26B C27B 118.8(8) N29B C26B C27B 119.8(8) C28B C27B C26B 121.2(7) C27B C28B C23B 121.2(8) C26B N29B C31B 122.1(10) C26B N29B C30B 120.4(9) C31B N29B C30B 116.7(10) C33B C32B N22B 117.2(8) C33B C32B C37B 116.1(9) N22B C32B C37B 126.4(10) C32B C33B C34B 120.8(9) C35B C34B C33B 122.0(10) N38B C35B C34B 122.8(12) N38B C35B C36B 120.8(11) C34B C35B C36B 116.1(10) C37B C36B C35B 122.7(11) C36B C37B C32B 121.9(12) C35B N38B C39B 118.4(12) C35B N38B C40B 120.0(12) C39B N38B C40B 121.6(13) F11 B10 F12 115(2) F11 B10 F14 116.1(16) F12 B10 F14 117.1(17) F11 B10 F13 105.6(15) F12 B10 F13 97.8(14) F14 B10 F13 102.0(17) F24 B20 F21 111.4(12) F24 B20 F22 108.3(11) F21 B20 F22 108.8(11) F24 B20 F23 108.0(12) F21 B20 F23 108.0(11) F22 B20 F23 112.3(12) F23' B20' F21' 112.3(12) F23' B20' F22' 108.9(12) F21' B20' F22' 108.6(12) F23' B20' F24' 110.2(12) F21' B20' F24' 107.6(11) F22' B20' F24' 109.2(11) Cl52 C50 Cl51 111.9(14) Cl54 C50' Cl53 111(2) Cl62 C60 Cl61 105.6(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Cu1A N2A 1.997(8) Cu1A N21A 2.026(7) Cu1A N1A 2.029(6) Cu1A N22A 2.032(8) N1A C1A 1.297(10) N1A C3A 1.429(10) C1A C2A 1.424(13) C2A N2A 1.314(11) N2A C12A 1.419(12) C3A C4A 1.378(11) C3A C8A 1.402(12) C4A C5A 1.348(15) C5A C6A 1.394(15) C6A C7A 1.370(15) C6A N9A 1.389(14) C7A C8A 1.389(16) N9A C10A 1.37(2) N9A C11A 1.472(15) C12A C13A 1.360(15) C12A C17A 1.399(16) C13A C14A 1.399(15) C14A C15A 1.369(19) C15A N18A 1.402(15) C15A C16A 1.425(19) C16A C17A 1.359(17) N18A C19A 1.41(2) N18A C20A 1.44(3) N21A C21A 1.241(12) N21A C23A 1.426(11) C21A C22A 1.482(14) C22A N22A 1.278(14) N22A C32A 1.399(12) C23A C24A 1.368(11) C23A C28A 1.400(12) C24A C25A 1.384(12) C25A C26A 1.415(13) C26A N29A 1.377(13) C26A C27A 1.400(14) C27A C28A 1.389(13) N29A C30A 1.407(18) N29A C31A 1.493(15) C32A C33A 1.340(13) C32A C37A 1.394(15) C33A C34A 1.432(12) C34A C35A 1.367(14) C35A N38A 1.373(14) C35A C36A 1.419(17) C36A C37A 1.367(18) N38A C39A 1.43(2) N38A C40A 1.47(2) Cu1B N21B 1.993(7) Cu1B N1B 2.006(7) Cu1B N2B 2.065(7) Cu1B N22B 2.066(7) N1B C1B 1.288(12) N1B C3B 1.417(12) C1B C2B 1.447(14) C2B N2B 1.276(12) N2B C12B 1.383(12) C3B C8B 1.363(12) C3B C4B 1.375(14) C4B C5B 1.381(15) C5B C6B 1.371(14) C6B C7B 1.325(17) C6B N9" 1.39(2) C6B N9B 1.398(14) C7B C8B 1.413(16) N9B C10B 1.358(15) N9B C11B 1.402(13) N9" C11" 1.377(18) N9" C10" 1.378(18) C12B C13B 1.391(18) C12B C17B 1.401(16) C13B C14B 1.352(17) C14B C15B 1.44(2) C15B N18B 1.335(19) C15B C16B 1.38(2) C16B C17B 1.381(18) N18B C20B 1.42(2) N18B C19B 1.44(2) N21B C21B 1.330(13) N21B C23B 1.406(11) C21B C22B 1.410(15) C22B N22B 1.321(14) N22B C32B 1.394(11) C23B C28B 1.387(12) C23B C24B 1.408(12) C24B C25B 1.407(13) C25B C26B 1.362(13) C26B N29B 1.365(12) C26B C27B 1.451(13) C27B C28B 1.356(13) N29B C31B 1.461(14) N29B C30B 1.473(17) C32B C33B 1.392(14) C32B C37B 1.418(14) C33B C34B 1.403(13) C34B C35B 1.386(16) C35B N38B 1.380(16) C35B C36B 1.393(18) C36B C37B 1.353(17) N38B C39B 1.41(2) N38B C40B 1.461(19) B10 F11 1.32(2) B10 F12 1.33(2) B10 F14 1.34(2) B10 F13 1.51(3) B20 F24 1.397(14) B20 F21 1.398(14) B20 F22 1.401(14) B20 F23 1.415(14) B20' F23' 1.387(14) B20' F21' 1.396(14) B20' F22' 1.396(14) B20' F24' 1.413(14) C50 Cl52 1.745(18) C50 Cl51 1.764(17) C50' Cl54 1.76(2) C50' Cl53 1.76(2) C60 Cl62 1.824(18) C60 Cl61 1.85(2)