#------------------------------------------------------------------------------ #$Date: 2017-04-21 05:23:09 +0300 (Fri, 21 Apr 2017) $ #$Revision: 195645 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/27/7042739.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_7042739 loop_ _publ_author_name 'Song, You' 'Yang, Li' 'Li, Jing' 'Pu, Tian-Cheng' 'Kong, Ming' _publ_section_title ; Metal-ion induced ferromagnetic polarization in mixed-spin system ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT00753A _journal_year 2017 _chemical_formula_sum 'C48 H45 Cl Cu3 Ni O24' _chemical_formula_weight 1290.62 _space_group_crystal_system trigonal _space_group_IT_number 148 _space_group_name_Hall '-R 3' _space_group_name_H-M_alt 'R -3 :H' _symmetry_space_group_name_Hall '-R 3' _symmetry_space_group_name_H-M 'R -3 :H' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2017-04-06 deposited with the CCDC. 2017-04-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 6 _cell_length_a 12.8633(8) _cell_length_b 12.8633(8) _cell_length_c 53.095(7) _cell_measurement_reflns_used 3897 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.499 _cell_measurement_theta_min 1.868 _cell_volume 7608.3(12) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_unetI/netI 0.0363 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_limit_l_min -68 _diffrn_reflns_number 23217 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.499 _diffrn_reflns_theta_min 1.868 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 1.747 _exptl_absorpt_correction_T_max 0.739 _exptl_absorpt_correction_T_min 0.647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.690 _exptl_crystal_description bulk _exptl_crystal_F_000 3942 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _refine_diff_density_max 0.517 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.070 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 234 _refine_ls_number_reflns 3897 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.032 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0391 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+11.0805P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1029 _refine_ls_wR_factor_ref 0.1167 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2849 _reflns_number_total 3897 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt00753a2.cif _cod_data_source_block 2 _cod_original_cell_volume 7608.3(14) _cod_database_code 7042739 _shelx_shelxl_version_number 2016/6 _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_estimated_absorpt_t_min 0.653 _shelx_estimated_absorpt_t_max 0.746 _shelx_res_file ; TITL 2 in R-3 2.res created by SHELXL-2016/6 at 19:08:18 on 06-Apr-2017 CELL 0.71073 12.8633 12.8633 53.095 90 90 120 ZERR 6 0.0008 0.0008 0.007 0 0 0 LATT 3 SYMM -Y,+X-Y,+Z SYMM +Y-X,-X,+Z SFAC C H Cl Cu Ni O UNIT 288 270 6 18 6 144 L.S. 5 PLAN 5 BOND $H HTAB CONF fmap 2 acta REM REM REM WGHT 0.057400 11.080500 FVAR 0.04813 C9 1 0.568469 1.067957 0.059905 11.00000 0.07239 0.04207 = 0.05432 0.00429 0.00132 0.02895 AFIX 43 H9 2 0.606805 1.130849 0.048508 11.00000 -1.20000 AFIX 0 C10 1 0.621214 1.086896 0.083596 11.00000 0.05595 0.04693 = 0.06390 -0.00510 -0.00926 0.02479 C11 1 0.723615 1.201541 0.088596 11.00000 0.08208 0.05476 = 0.10021 0.00591 -0.01556 0.01277 AFIX 43 H11 2 0.756807 1.258551 0.075851 11.00000 -1.20000 AFIX 0 C12 1 0.772246 1.226967 0.111976 11.00000 0.09858 0.06158 = 0.13496 -0.00420 -0.05815 0.00037 AFIX 43 H12 2 0.836483 1.303038 0.115406 11.00000 -1.20000 AFIX 0 C13 1 0.728476 1.142943 0.130438 11.00000 0.10567 0.06990 = 0.09404 -0.01808 -0.05782 0.01955 AFIX 43 H13 2 0.764688 1.162387 0.146217 11.00000 -1.20000 AFIX 0 C14 1 0.632737 1.030489 0.126581 11.00000 0.07507 0.06669 = 0.06060 -0.01670 -0.02867 0.03599 C15 1 0.573973 0.999742 0.102572 11.00000 0.05321 0.04522 = 0.05133 -0.01273 -0.01356 0.02726 C16 1 0.638169 0.963176 0.168119 11.00000 0.16481 0.11185 = 0.06167 -0.01919 -0.05680 0.06376 AFIX 137 H16A 2 0.718581 0.977331 0.166558 11.00000 -1.50000 H16B 2 0.592412 0.894777 0.178756 11.00000 -1.50000 H16C 2 0.640097 1.032439 0.175396 11.00000 -1.50000 AFIX 0 C8 1 0.118429 0.658966 -0.001653 11.00000 0.05021 0.06312 = 0.04567 -0.00903 -0.01508 0.02196 AFIX 43 H8 2 0.062213 0.636241 -0.014536 11.00000 -1.20000 AFIX 0 C6 1 0.109195 0.730789 0.017656 11.00000 0.04371 0.04541 = 0.04613 -0.00139 -0.00923 0.01968 C5 1 0.012450 0.753262 0.015980 11.00000 0.05048 0.06952 = 0.06638 -0.00428 -0.01759 0.02951 AFIX 43 H5 2 -0.037657 0.726180 0.001978 11.00000 -1.20000 AFIX 0 C4 1 -0.008629 0.813065 0.034238 11.00000 0.05903 0.08516 = 0.08820 -0.01032 -0.01407 0.04857 AFIX 43 H4 2 -0.071737 0.828350 0.032593 11.00000 -1.20000 AFIX 0 C3 1 0.064317 0.852227 0.055682 11.00000 0.06352 0.06777 = 0.06814 -0.01072 -0.00412 0.04280 AFIX 43 H3 2 0.048352 0.891593 0.068488 11.00000 -1.20000 AFIX 0 C2 1 0.158654 0.832701 0.057798 11.00000 0.05096 0.04505 = 0.04714 -0.00549 -0.00597 0.02660 C7 1 0.185108 0.772592 0.038697 11.00000 0.04368 0.03825 = 0.03984 0.00001 -0.00344 0.02019 C1 1 0.206936 0.910034 0.100020 11.00000 0.11218 0.13114 = 0.05972 -0.04215 -0.01852 0.08247 AFIX 137 H1A 2 0.218210 0.988442 0.096781 11.00000 -1.50000 H1B 2 0.259064 0.914717 0.113454 11.00000 -1.50000 H1C 2 0.124998 0.856658 0.104746 11.00000 -1.50000 AFIX 0 CL1 3 1.000000 1.000000 0.132830 10.33330 0.07978 0.07978 = 0.08198 0.00000 0.00000 0.03989 CU1 4 0.389036 0.829352 0.071038 11.00000 0.04977 0.04189 = 0.03608 -0.00506 -0.01079 0.02291 NI1 5 0.333333 0.666667 0.018853 10.33330 0.04522 0.04522 = 0.03203 0.00000 0.00000 0.02261 O1 6 0.333333 0.666667 0.084079 10.33330 0.04638 0.04638 = 0.03188 0.00000 0.00000 0.02319 AFIX 3 H1 2 0.333333 0.666667 0.100099 10.33333 -1.50000 AFIX 0 O5 6 0.476221 0.977305 0.051981 11.00000 0.07586 0.04698 = 0.04475 0.00035 -0.01216 0.02935 O6 6 0.481797 0.894868 0.100160 11.00000 0.06562 0.04909 = 0.04346 -0.00464 -0.01872 0.01769 O7 6 0.583665 0.940799 0.143758 11.00000 0.10578 0.08208 = 0.04942 -0.01093 -0.03120 0.03772 O4 6 0.190029 0.622868 -0.003688 11.00000 0.06025 0.06914 = 0.04459 -0.01653 -0.01278 0.03292 O3 6 0.276937 0.753780 0.041986 11.00000 0.05246 0.05113 = 0.03972 -0.01230 -0.01321 0.03261 O2 6 0.234413 0.865984 0.077903 11.00000 0.07563 0.07830 = 0.04560 -0.02011 -0.01286 0.05309 O8 6 0.333333 0.666667 0.135144 10.33330 0.22236 0.22236 = 0.08203 0.00000 0.00000 0.11118 AFIX 3 H8A 2 0.315550 0.639350 0.150054 10.33330 -1.20000 H8B 2 0.382250 0.741840 0.145194 10.33330 -1.20000 AFIX 0 O10 6 1.000000 1.000000 0.105518 10.33330 0.11810 0.11810 = 0.07363 0.00000 0.00000 0.05905 O9 6 0.937311 0.888678 0.141616 11.00000 0.34558 0.11886 = 0.15704 0.07040 -0.00448 0.02720 HKLF 4 1 0 1 0 -1 -1 0 0 0 1 REM 2 in R-3 REM R1 = 0.0391 for 2849 Fo > 4sig(Fo) and 0.0619 for all 3897 data REM 234 parameters refined using 0 restraints END WGHT 0.0572 10.7686 REM Instructions for potential hydrogen bonds EQIV $5 x-y+1, x+1, -z HTAB C9 O4_$5 EQIV $6 y-1, -x+y, -z HTAB C8 O5_$6 EQIV $7 x-1, y, z HTAB C3 O10_$7 HTAB O1 O8 EQIV $8 -x+2/3, -y+4/3, -z+1/3 HTAB O8 O8_$8 HTAB O8 O7 REM Highest difference peak 0.517, deepest hole -0.473, 1-sigma level 0.070 Q1 1 0.8869 0.9496 0.1409 11.00000 0.05 0.52 Q2 1 1.0000 1.0000 0.1668 10.33333 0.05 0.40 Q3 1 0.3333 0.6667 0.1133 10.33333 0.05 0.36 Q4 1 0.3333 0.6667 -0.0039 10.33333 0.05 0.35 Q5 1 0.4256 0.9159 0.0953 11.00000 0.05 0.31 ; _shelx_res_checksum 39019 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' 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 C9 C 0.5685(3) 1.0680(3) 0.05991(7) 0.0561(9) Uani 1 1 d . . . H9 H 0.606805 1.130849 0.048508 0.067 Uiso 1 1 calc R U . C10 C 0.6212(3) 1.0869(3) 0.08360(7) 0.0560(9) Uani 1 1 d . . . C11 C 0.7236(4) 1.2015(4) 0.08860(10) 0.0885(14) Uani 1 1 d . . . H11 H 0.756807 1.258551 0.075851 0.106 Uiso 1 1 calc R U . C12 C 0.7722(5) 1.2270(4) 0.11198(12) 0.116(2) Uani 1 1 d . . . H12 H 0.836483 1.303038 0.115406 0.139 Uiso 1 1 calc R U . C13 C 0.7285(5) 1.1429(4) 0.13044(10) 0.1007(18) Uani 1 1 d . . . H13 H 0.764688 1.162387 0.146217 0.121 Uiso 1 1 calc R U . C14 C 0.6327(4) 1.0305(4) 0.12658(8) 0.0672(10) Uani 1 1 d . . . C15 C 0.5740(3) 0.9997(3) 0.10257(6) 0.0487(8) Uani 1 1 d . . . C16 C 0.6382(6) 0.9632(5) 0.16812(9) 0.115(2) Uani 1 1 d . . . H16A H 0.718581 0.977331 0.166558 0.173 Uiso 1 1 calc R U . H16B H 0.592412 0.894777 0.178756 0.173 Uiso 1 1 calc R U . H16C H 0.640097 1.032439 0.175396 0.173 Uiso 1 1 calc R U . C8 C 0.1184(3) 0.6590(3) -0.00165(7) 0.0558(9) Uani 1 1 d . . . H8 H 0.062213 0.636241 -0.014536 0.067 Uiso 1 1 calc R U . C6 C 0.1092(3) 0.7308(3) 0.01766(6) 0.0462(7) Uani 1 1 d . . . C5 C 0.0124(3) 0.7533(3) 0.01598(8) 0.0623(10) Uani 1 1 d . . . H5 H -0.037657 0.726180 0.001978 0.075 Uiso 1 1 calc R U . C4 C -0.0086(4) 0.8131(4) 0.03424(9) 0.0719(11) Uani 1 1 d . . . H4 H -0.071737 0.828350 0.032593 0.086 Uiso 1 1 calc R U . C3 C 0.0643(3) 0.8522(3) 0.05568(8) 0.0620(9) Uani 1 1 d . . . H3 H 0.048352 0.891593 0.068488 0.074 Uiso 1 1 calc R U . C2 C 0.1587(3) 0.8327(3) 0.05780(6) 0.0466(7) Uani 1 1 d . . . C7 C 0.1851(3) 0.7726(3) 0.03870(5) 0.0407(6) Uani 1 1 d . . . C1 C 0.2069(5) 0.9100(5) 0.10002(8) 0.0914(15) Uani 1 1 d . . . H1A H 0.218210 0.988442 0.096781 0.137 Uiso 1 1 calc R U . H1B H 0.259064 0.914717 0.113454 0.137 Uiso 1 1 calc R U . H1C H 0.124998 0.856658 0.104746 0.137 Uiso 1 1 calc R U . Cl1 Cl 1.000000 1.000000 0.13283(4) 0.0805(5) Uani 1 3 d S T P Cu1 Cu 0.38904(3) 0.82935(3) 0.07104(2) 0.04258(14) Uani 1 1 d . . . Ni1 Ni 0.333333 0.666667 0.01885(2) 0.04082(18) Uani 1 3 d S T P O1 O 0.333333 0.666667 0.08408(6) 0.0415(8) Uani 1 3 d S T P H1 H 0.333333 0.666667 0.100099 0.062 Uiso 1 3 d R U P O5 O 0.4762(2) 0.9773(2) 0.05198(4) 0.0565(6) Uani 1 1 d . . . O6 O 0.4818(2) 0.8949(2) 0.10016(4) 0.0576(6) Uani 1 1 d . . . O7 O 0.5837(3) 0.9408(3) 0.14376(5) 0.0832(9) Uani 1 1 d . . . O4 O 0.1900(2) 0.6229(2) -0.00369(4) 0.0577(6) Uani 1 1 d . . . O3 O 0.2769(2) 0.75378(19) 0.04199(4) 0.0448(5) Uani 1 1 d . . . O2 O 0.2344(2) 0.8660(2) 0.07790(4) 0.0600(6) Uani 1 1 d . . . O8 O 0.333333 0.666667 0.13514(15) 0.176(4) Uani 1 3 d S T P H8A H 0.315550 0.639350 0.150054 0.211 Uiso 0.3333 1 d R U P H8B H 0.382250 0.741840 0.145194 0.211 Uiso 0.3333 1 d R U P O10 O 1.000000 1.000000 0.10552(11) 0.1033(19) Uani 1 3 d S T P O9 O 0.9373(8) 0.8887(5) 0.14162(12) 0.247(4) 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 C9 0.072(2) 0.0421(18) 0.054(2) 0.0043(15) 0.0013(18) 0.0289(18) C10 0.056(2) 0.0469(18) 0.064(2) -0.0051(16) -0.0093(17) 0.0248(16) C11 0.082(3) 0.055(2) 0.100(4) 0.006(2) -0.016(3) 0.013(2) C12 0.099(4) 0.062(3) 0.135(5) -0.004(3) -0.058(4) 0.000(3) C13 0.106(4) 0.070(3) 0.094(4) -0.018(3) -0.058(3) 0.020(3) C14 0.075(3) 0.067(2) 0.061(2) -0.017(2) -0.029(2) 0.036(2) C15 0.0532(18) 0.0452(17) 0.0513(19) -0.0127(14) -0.0136(15) 0.0273(15) C16 0.165(6) 0.112(4) 0.062(3) -0.019(3) -0.057(3) 0.064(4) C8 0.0502(19) 0.063(2) 0.0457(19) -0.0090(16) -0.0151(15) 0.0220(17) C6 0.0437(17) 0.0454(17) 0.0461(18) -0.0014(14) -0.0092(14) 0.0197(14) C5 0.050(2) 0.070(2) 0.066(2) -0.0043(19) -0.0176(17) 0.0295(18) C4 0.059(2) 0.085(3) 0.088(3) -0.010(2) -0.014(2) 0.049(2) C3 0.064(2) 0.068(2) 0.068(2) -0.0107(19) -0.0041(19) 0.043(2) C2 0.0510(18) 0.0451(17) 0.0471(18) -0.0055(14) -0.0060(14) 0.0266(15) C7 0.0437(16) 0.0382(15) 0.0398(16) 0.0000(12) -0.0034(13) 0.0202(13) C1 0.112(4) 0.131(4) 0.060(3) -0.042(3) -0.019(2) 0.082(3) Cl1 0.0798(8) 0.0798(8) 0.0820(13) 0.000 0.000 0.0399(4) Cu1 0.0498(2) 0.0419(2) 0.0361(2) -0.00506(15) -0.01079(16) 0.02291(17) Ni1 0.0452(2) 0.0452(2) 0.0320(3) 0.000 0.000 0.02261(12) O1 0.0464(12) 0.0464(12) 0.0319(18) 0.000 0.000 0.0232(6) O5 0.0759(16) 0.0470(13) 0.0447(13) 0.0003(10) -0.0122(12) 0.0294(12) O6 0.0656(15) 0.0491(13) 0.0435(13) -0.0046(10) -0.0187(11) 0.0177(12) O7 0.106(2) 0.082(2) 0.0494(15) -0.0109(14) -0.0312(15) 0.0377(18) O4 0.0603(15) 0.0691(16) 0.0446(13) -0.0165(11) -0.0128(11) 0.0329(13) O3 0.0525(12) 0.0511(12) 0.0397(11) -0.0123(9) -0.0132(9) 0.0326(10) O2 0.0756(16) 0.0783(17) 0.0456(13) -0.0201(12) -0.0129(12) 0.0531(14) O8 0.222(6) 0.222(6) 0.082(5) 0.000 0.000 0.111(3) O10 0.118(3) 0.118(3) 0.074(4) 0.000 0.000 0.0591(15) O9 0.346(9) 0.119(4) 0.157(5) 0.070(4) -0.004(6) 0.027(5) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' 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 O5 C9 C10 128.3(3) . . O5 C9 H9 115.8 . . C10 C9 H9 115.8 . . C9 C10 C15 122.1(3) . . C9 C10 C11 117.8(4) . . C15 C10 C11 120.0(4) . . C12 C11 C10 119.7(4) . . C12 C11 H11 120.1 . . C10 C11 H11 120.1 . . C11 C12 C13 120.8(4) . . C11 C12 H12 119.6 . . C13 C12 H12 119.6 . . C12 C13 C14 122.0(4) . . C12 C13 H13 119.0 . . C14 C13 H13 119.0 . . O7 C14 C13 126.2(4) . . O7 C14 C15 114.0(3) . . C13 C14 C15 119.8(4) . . O6 C15 C10 125.0(3) . . O6 C15 C14 117.5(3) . . C10 C15 C14 117.5(3) . . O7 C16 H16A 109.5 . . O7 C16 H16B 109.5 . . H16A C16 H16B 109.5 . . O7 C16 H16C 109.5 . . H16A C16 H16C 109.5 . . H16B C16 H16C 109.5 . . O4 C8 C6 129.1(3) . . O4 C8 H8 115.4 . . C6 C8 H8 115.4 . . C7 C6 C5 119.1(3) . . C7 C6 C8 123.7(3) . . C5 C6 C8 117.0(3) . . C4 C5 C6 121.4(3) . . C4 C5 H5 119.3 . . C6 C5 H5 119.3 . . C5 C4 C3 120.1(3) . . C5 C4 H4 120.0 . . C3 C4 H4 120.0 . . C2 C3 C4 120.0(3) . . C2 C3 H3 120.0 . . C4 C3 H3 120.0 . . C3 C2 O2 124.8(3) . . C3 C2 C7 121.4(3) . . O2 C2 C7 113.8(3) . . O3 C7 C6 123.1(3) . . O3 C7 C2 118.9(3) . . C6 C7 C2 117.9(3) . . O2 C1 H1A 109.5 . . O2 C1 H1B 109.5 . . H1A C1 H1B 109.5 . . O2 C1 H1C 109.5 . . H1A C1 H1C 109.5 . . H1B C1 H1C 109.5 . . O9 Cl1 O9 108.4(3) 2_765 3_675 O9 Cl1 O9 108.4(3) 2_765 . O9 Cl1 O9 108.4(3) 3_675 . O9 Cl1 O10 110.6(3) 2_765 . O9 Cl1 O10 110.6(3) 3_675 . O9 Cl1 O10 110.6(3) . . O6 Cu1 O5 93.63(10) . . O6 Cu1 O1 89.96(11) . . O5 Cu1 O1 161.90(10) . . O6 Cu1 O3 174.80(10) . . O5 Cu1 O3 89.84(9) . . O1 Cu1 O3 87.93(10) . . O6 Cu1 O2 101.48(10) . . O5 Cu1 O2 90.96(10) . . O1 Cu1 O2 105.71(8) . . O3 Cu1 O2 74.55(8) . . O3 Ni1 O3 87.05(9) . 2_665 O3 Ni1 O3 87.05(9) . 3_565 O3 Ni1 O3 87.05(9) 2_665 3_565 O3 Ni1 O4 89.10(9) . . O3 Ni1 O4 95.33(10) 2_665 . O3 Ni1 O4 175.37(9) 3_565 . O3 Ni1 O4 95.33(10) . 3_565 O3 Ni1 O4 175.37(9) 2_665 3_565 O3 Ni1 O4 89.11(9) 3_565 3_565 O4 Ni1 O4 88.69(10) . 3_565 O3 Ni1 O4 175.37(9) . 2_665 O3 Ni1 O4 89.11(9) 2_665 2_665 O3 Ni1 O4 95.34(10) 3_565 2_665 O4 Ni1 O4 88.69(10) . 2_665 O4 Ni1 O4 88.68(10) 3_565 2_665 Cu1 O1 Cu1 108.32(10) . 2_665 Cu1 O1 Cu1 108.32(10) . 3_565 Cu1 O1 Cu1 108.31(10) 2_665 3_565 Cu1 O1 H1 110.6 . . Cu1 O1 H1 110.6 2_665 . Cu1 O1 H1 110.6 3_565 . C9 O5 Cu1 123.6(2) . . C15 O6 Cu1 127.0(2) . . C14 O7 C16 117.7(4) . . C8 O4 Ni1 126.4(2) . . C7 O3 Cu1 120.17(17) . . C7 O3 Ni1 128.10(18) . . Cu1 O3 Ni1 111.46(10) . . C2 O2 C1 119.4(3) . . C2 O2 Cu1 111.65(18) . . C1 O2 Cu1 128.8(2) . . H8A O8 H8B 79.2 . . H8A O8 H8A 36.7 . 2_665 H8B O8 H8A 49.5 . 2_665 H8A O8 H8A 36.7 . 3_565 H8B O8 H8A 49.5 . 3_565 H8A O8 H8A 36.7 2_665 3_565 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C9 O5 1.249(4) . C9 C10 1.392(5) . C9 H9 0.9300 . C10 C15 1.400(5) . C10 C11 1.428(5) . C11 C12 1.354(7) . C11 H11 0.9300 . C12 C13 1.356(7) . C12 H12 0.9300 . C13 C14 1.367(6) . C13 H13 0.9300 . C14 O7 1.354(5) . C14 C15 1.433(5) . C15 O6 1.282(4) . C16 O7 1.430(5) . C16 H16A 0.9600 . C16 H16B 0.9600 . C16 H16C 0.9600 . C8 O4 1.226(4) . C8 C6 1.424(5) . C8 H8 0.9300 . C6 C7 1.402(4) . C6 C5 1.414(5) . C5 C4 1.347(6) . C5 H5 0.9300 . C4 C3 1.399(5) . C4 H4 0.9300 . C3 C2 1.361(5) . C3 H3 0.9300 . C2 O2 1.362(4) . C2 C7 1.416(4) . C7 O3 1.330(4) . C1 O2 1.423(4) . C1 H1A 0.9600 . C1 H1B 0.9600 . C1 H1C 0.9600 . Cl1 O9 1.328(5) 2_765 Cl1 O9 1.328(5) 3_675 Cl1 O9 1.328(5) . Cl1 O10 1.450(6) . Cu1 O6 1.876(2) . Cu1 O5 1.941(2) . Cu1 O1 1.9679(13) . Cu1 O3 2.000(2) . Cu1 O2 2.291(2) . Ni1 O3 2.026(2) . Ni1 O3 2.026(2) 2_665 Ni1 O3 2.026(2) 3_565 Ni1 O4 2.027(2) . Ni1 O4 2.027(2) 3_565 Ni1 O4 2.027(2) 2_665 O1 H1 0.8506 . O8 H8A 0.8498 . O8 H8B 1.0036 . O8 H8A 0.8496 2_665 O8 H8A 0.8496 3_565 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 O5 C9 C10 C15 0.6(6) O5 C9 C10 C11 -176.6(4) C9 C10 C11 C12 175.0(5) C15 C10 C11 C12 -2.2(7) C10 C11 C12 C13 3.1(9) C11 C12 C13 C14 -1.3(10) C12 C13 C14 O7 179.4(5) C12 C13 C14 C15 -1.5(8) C9 C10 C15 O6 2.0(6) C11 C10 C15 O6 179.1(4) C9 C10 C15 C14 -177.6(3) C11 C10 C15 C14 -0.4(5) O7 C14 C15 O6 1.9(5) C13 C14 C15 O6 -177.3(4) O7 C14 C15 C10 -178.5(3) C13 C14 C15 C10 2.3(6) O4 C8 C6 C7 -0.7(6) O4 C8 C6 C5 -176.3(4) C7 C6 C5 C4 -0.5(6) C8 C6 C5 C4 175.3(4) C6 C5 C4 C3 -1.4(6) C5 C4 C3 C2 1.7(6) C4 C3 C2 O2 -179.4(4) C4 C3 C2 C7 -0.3(6) C5 C6 C7 O3 178.9(3) C8 C6 C7 O3 3.4(5) C5 C6 C7 C2 1.9(5) C8 C6 C7 C2 -173.6(3) C3 C2 C7 O3 -178.6(3) O2 C2 C7 O3 0.5(4) C3 C2 C7 C6 -1.5(5) O2 C2 C7 C6 177.6(3) C10 C9 O5 Cu1 -5.8(5) C10 C15 O6 Cu1 1.5(5) C14 C15 O6 Cu1 -178.9(3) O5 Cu1 O6 C15 -4.8(3) O1 Cu1 O6 C15 157.4(3) O2 Cu1 O6 C15 -96.6(3) C13 C14 O7 C16 -1.9(7) C15 C14 O7 C16 178.9(4) C6 C8 O4 Ni1 -6.0(6) C6 C7 O3 Cu1 174.5(2) C2 C7 O3 Cu1 -8.5(4) C6 C7 O3 Ni1 0.9(4) C2 C7 O3 Ni1 177.9(2) C3 C2 O2 C1 8.9(6) C7 C2 O2 C1 -170.2(4) C3 C2 O2 Cu1 -174.7(3) C7 C2 O2 Cu1 6.2(3)