#------------------------------------------------------------------------------ #$Date: 2017-04-21 05:23:09 +0300 (Fri, 21 Apr 2017) $ #$Revision: 195645 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/27/7042738.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_7042738 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 Co Cu3 O24' _chemical_formula_weight 1290.84 _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 12.756(2) _cell_length_b 12.756(2) _cell_length_c 52.895(9) _cell_measurement_reflns_used 3759 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.418 _cell_measurement_theta_min 1.883 _cell_volume 7454(2) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'CCD area detector' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_unetI/netI 0.0577 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.989 _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 46 _diffrn_reflns_limit_l_min -67 _diffrn_reflns_number 16829 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.418 _diffrn_reflns_theta_min 1.883 _exptl_absorpt_coefficient_mu 1.738 _exptl_absorpt_correction_T_max 0.786 _exptl_absorpt_correction_T_min 0.634 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.725 _exptl_crystal_description bulk _exptl_crystal_F_000 3936 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.14 _refine_diff_density_max 0.907 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.100 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 234 _refine_ls_number_reflns 3759 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0450 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+16.4570P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1108 _refine_ls_wR_factor_ref 0.1239 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2836 _reflns_number_total 3759 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt00753a2.cif _cod_data_source_block 2 _cod_original_cell_volume 7454(3) _cod_database_code 7042738 _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 0.623 _shelx_estimated_absorpt_t_max 0.757 _shelx_res_file ; TITL mo_20150606Y1_0m_a.res in R-3 2.res created by SHELXL-2016/6 at 19:08:05 on 06-Apr-2017 CELL 0.71073 12.7565 12.7565 52.8954 90 90 120 ZERR 6 0.0022 0.0022 0.0091 0 0 0 LATT 3 SYMM -Y,+X-Y,+Z SYMM +Y-X,-X,+Z SFAC C H Cl Co Cu O UNIT 288 270 6 6 18 144 EQIV $1 0.667-Y+X,0.333+X,1.333-Z EQIV $2 -0.333+Y,0.333-X+Y,1.333-Z L.S. 20 PLAN -1 TEMP 20 HTAB O1 O8 HTAB C3 O10 HTAB C8 O5_$1 HTAB C9 O4_$2 BOND $H HTAB SIZE 0.2*0.18*0.17 fmap 2 acta OMIT -6 9 3 OMIT 1 5 5 OMIT 0 3 15 OMIT -2 2 8 OMIT 0 2 1 OMIT 1 1 3 OMIT -2 2 11 OMIT -2 2 2 OMIT -1 2 6 OMIT -2 3 1 OMIT 0 3 3 OMIT -3 3 12 REM REM REM WGHT 0.058900 16.456999 FVAR 0.13466 CU1 5 0.889556 0.837521 0.595180 11.00000 0.02959 0.02658 = 0.02403 -0.00425 0.00493 0.01191 CO1 4 1.000000 1.000000 0.647949 10.33333 0.02723 0.02723 = 0.02163 0.00000 0.00000 0.01362 O1 6 1.000000 1.000000 0.582124 10.33333 0.02885 0.02885 = 0.02297 0.00000 0.00000 0.01442 AFIX 13 H1 2 0.999996 0.999995 0.563597 10.33333 -1.20000 AFIX 0 O2 6 0.700140 0.805050 0.587584 11.00000 0.03117 0.04925 = 0.03031 -0.01730 -0.00555 0.01645 O3 6 0.852720 0.914142 0.624174 11.00000 0.02415 0.03375 = 0.02894 -0.01078 0.00039 0.01330 O4 6 0.893743 1.038960 0.671051 11.00000 0.03679 0.04446 = 0.03053 -0.01238 -0.00369 0.02283 O5 6 0.826312 0.688331 0.614391 11.00000 0.04288 0.03014 = 0.02803 -0.00133 0.01058 0.01132 O6 6 0.917443 0.771497 0.565964 11.00000 0.05447 0.03205 = 0.02769 -0.00266 0.01208 0.02189 O7 6 0.982239 0.728363 0.522922 11.00000 0.06100 0.05644 = 0.03029 -0.01048 0.01217 0.02432 O8 6 1.000000 1.000000 0.531070 10.33333 0.15633 0.15633 = 0.05329 0.00000 0.00000 0.07817 AFIX 3 H8A 2 0.976030 1.037850 0.521640 10.33333 -1.50000 H8B 2 1.073280 1.022200 0.517620 10.33333 -1.50000 AFIX 0 C1 1 0.626499 0.758563 0.565491 11.00000 0.04826 0.07170 = 0.03179 -0.01751 -0.01058 0.02526 AFIX 137 H1A 2 0.674237 0.754957 0.551851 11.00000 -1.50000 H1B 2 0.595482 0.810704 0.560881 11.00000 -1.50000 H1C 2 0.560313 0.678803 0.568904 11.00000 -1.50000 AFIX 0 C2 1 0.655789 0.837340 0.607687 11.00000 0.02908 0.02731 = 0.02726 -0.00098 0.00125 0.01190 C3 1 0.539715 0.818332 0.609456 11.00000 0.02880 0.03570 = 0.04171 -0.00661 -0.00518 0.01319 AFIX 43 H3 2 0.484750 0.780039 0.596397 11.00000 -1.20000 AFIX 0 C4 1 0.505270 0.856915 0.630961 11.00000 0.02903 0.04681 = 0.05516 -0.00533 0.00165 0.02052 AFIX 43 H4 2 0.426497 0.842514 0.632425 11.00000 -1.20000 AFIX 0 C5 1 0.586703 0.915698 0.649855 11.00000 0.03617 0.04139 = 0.04238 -0.00478 0.00666 0.02360 AFIX 43 H5 2 0.562922 0.941958 0.663990 11.00000 -1.20000 AFIX 0 C6 1 0.705566 0.937221 0.648343 11.00000 0.03131 0.02710 = 0.03125 -0.00241 0.00352 0.01618 C7 1 0.741820 0.896443 0.627180 11.00000 0.02351 0.02365 = 0.02718 -0.00060 0.00134 0.01047 C8 1 0.785571 1.005514 0.668663 11.00000 0.04744 0.03517 = 0.03032 -0.00686 0.00400 0.02538 AFIX 43 H8 2 0.751123 1.027197 0.681675 11.00000 -1.20000 AFIX 0 C9 1 0.829662 0.597578 0.606693 11.00000 0.03296 0.02966 = 0.03448 0.00158 0.00272 0.00796 AFIX 43 H9 2 0.804373 0.534290 0.618185 11.00000 -1.20000 AFIX 0 C10 1 0.866588 0.578431 0.582965 11.00000 0.03276 0.02839 = 0.03984 -0.00656 0.00159 0.01202 C11 1 0.855879 0.463783 0.578121 11.00000 0.06413 0.03721 = 0.07203 0.00064 0.01850 0.02686 AFIX 43 H11 2 0.830426 0.405945 0.590869 11.00000 -1.20000 AFIX 0 C12 1 0.882743 0.439102 0.554978 11.00000 0.10930 0.04222 = 0.09848 -0.00633 0.03733 0.04537 AFIX 43 H12 2 0.871908 0.362693 0.551679 11.00000 -1.20000 AFIX 0 C13 1 0.926019 0.525519 0.536151 11.00000 0.08286 0.05056 = 0.05821 -0.01426 0.02730 0.02970 AFIX 43 H13 2 0.946135 0.506914 0.520541 11.00000 -1.20000 AFIX 0 C14 1 0.939959 0.637293 0.539883 11.00000 0.04205 0.04540 = 0.03783 -0.01197 0.00637 0.02064 C15 1 0.907395 0.667100 0.563818 11.00000 0.02633 0.03244 = 0.03069 -0.00829 0.00076 0.01091 C16 1 1.022327 0.707284 0.499202 11.00000 0.07694 0.07881 = 0.03675 -0.01939 0.01618 0.02654 AFIX 137 H16A 2 1.050294 0.777618 0.488686 11.00000 -1.50000 H16B 2 0.956369 0.639037 0.491000 11.00000 -1.50000 H16C 2 1.087224 0.691049 0.501999 11.00000 -1.50000 AFIX 0 CL1 3 0.333333 0.666667 0.532309 10.33333 0.04554 0.04554 = 0.04397 0.00000 0.00000 0.02277 O9 6 0.422610 0.643951 0.523406 11.00000 0.13729 0.23244 = 0.07318 -0.04903 -0.01918 0.14711 O10 6 0.333333 0.666667 0.559806 10.33333 0.05408 0.05408 = 0.04175 0.00000 0.00000 0.02704 HKLF 4 REM mo_20150606Y1_0m_a.res in R-3 REM R1 = 0.0450 for 2836 Fo > 4sig(Fo) and 0.0664 for all 3759 data REM 234 parameters refined using 0 restraints END WGHT 0.0589 16.4438 REM Instructions for potential hydrogen bonds HTAB O1 O8 HTAB C3 O10 HTAB C8 O5_$1 HTAB C9 O4_$2 REM Highest difference peak 0.907, deepest hole -0.398, 1-sigma level 0.100 Q1 1 1.0000 1.0000 0.6657 10.33333 0.05 0.91 ; _shelx_res_checksum 12640 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 Cu1 Cu 0.88956(3) 0.83752(3) 0.59518(2) 0.02768(14) Uani 1 1 d . . . Co1 Co 1.000000 1.000000 0.64795(2) 0.02537(19) Uani 1 3 d S T P O1 O 1.000000 1.000000 0.58212(7) 0.0269(8) Uani 1 3 d S T P H1 H 0.999996 0.999995 0.563597 0.032 Uiso 1 3 calc R U P O2 O 0.7001(2) 0.8051(2) 0.58758(4) 0.0385(6) Uani 1 1 d . . . O3 O 0.85272(19) 0.9141(2) 0.62417(4) 0.0295(5) Uani 1 1 d . . . O4 O 0.8937(2) 1.0390(2) 0.67105(5) 0.0361(6) Uani 1 1 d . . . O5 O 0.8263(2) 0.6883(2) 0.61439(4) 0.0368(6) Uani 1 1 d . . . O6 O 0.9174(2) 0.7715(2) 0.56596(4) 0.0379(6) Uani 1 1 d . . . O7 O 0.9822(3) 0.7284(3) 0.52292(5) 0.0515(7) Uani 1 1 d . . . O8 O 1.000000 1.000000 0.53107(14) 0.122(3) Uani 1 3 d S T P H8A H 0.976030 1.037850 0.521640 0.183 Uiso 0.3333 1 d R U P H8B H 1.073280 1.022200 0.517620 0.183 Uiso 0.3333 1 d R U P C1 C 0.6265(4) 0.7586(4) 0.56549(7) 0.0527(11) Uani 1 1 d . . . H1A H 0.674237 0.754957 0.551851 0.079 Uiso 1 1 calc R U . H1B H 0.595482 0.810704 0.560881 0.079 Uiso 1 1 calc R U . H1C H 0.560313 0.678803 0.568904 0.079 Uiso 1 1 calc R U . C2 C 0.6558(3) 0.8373(3) 0.60769(6) 0.0289(7) Uani 1 1 d . . . C3 C 0.5397(3) 0.8183(3) 0.60946(7) 0.0367(8) Uani 1 1 d . . . H3 H 0.484750 0.780039 0.596397 0.044 Uiso 1 1 calc R U . C4 C 0.5053(3) 0.8569(3) 0.63096(8) 0.0430(9) Uani 1 1 d . . . H4 H 0.426497 0.842514 0.632425 0.052 Uiso 1 1 calc R U . C5 C 0.5867(3) 0.9157(3) 0.64985(7) 0.0381(8) Uani 1 1 d . . . H5 H 0.562922 0.941958 0.663990 0.046 Uiso 1 1 calc R U . C6 C 0.7056(3) 0.9372(3) 0.64834(6) 0.0292(7) Uani 1 1 d . . . C7 C 0.7418(3) 0.8964(3) 0.62718(6) 0.0254(6) Uani 1 1 d . . . C8 C 0.7856(3) 1.0055(3) 0.66866(7) 0.0355(8) Uani 1 1 d . . . H8 H 0.751123 1.027197 0.681675 0.043 Uiso 1 1 calc R U . C9 C 0.8297(3) 0.5976(3) 0.60669(7) 0.0358(8) Uani 1 1 d . . . H9 H 0.804373 0.534290 0.618185 0.043 Uiso 1 1 calc R U . C10 C 0.8666(3) 0.5784(3) 0.58297(7) 0.0351(8) Uani 1 1 d . . . C11 C 0.8559(4) 0.4638(4) 0.57812(10) 0.0571(12) Uani 1 1 d . . . H11 H 0.830426 0.405945 0.590869 0.069 Uiso 1 1 calc R U . C12 C 0.8827(6) 0.4391(4) 0.55498(12) 0.0800(18) Uani 1 1 d . . . H12 H 0.871908 0.362693 0.551679 0.096 Uiso 1 1 calc R U . C13 C 0.9260(5) 0.5255(4) 0.53615(9) 0.0655(14) Uani 1 1 d . . . H13 H 0.946135 0.506914 0.520541 0.079 Uiso 1 1 calc R U . C14 C 0.9400(3) 0.6373(4) 0.53988(7) 0.0423(9) Uani 1 1 d . . . C15 C 0.9074(3) 0.6671(3) 0.56382(6) 0.0315(7) Uani 1 1 d . . . C16 C 1.0223(5) 0.7073(5) 0.49920(8) 0.0697(15) Uani 1 1 d . . . H16A H 1.050294 0.777618 0.488686 0.105 Uiso 1 1 calc R U . H16B H 0.956369 0.639037 0.491000 0.105 Uiso 1 1 calc R U . H16C H 1.087224 0.691049 0.501999 0.105 Uiso 1 1 calc R U . Cl1 Cl 0.333333 0.666667 0.53231(3) 0.0450(4) Uani 1 3 d S T P O9 O 0.4226(5) 0.6440(6) 0.52341(9) 0.1233(19) Uani 1 1 d . . . O10 O 0.333333 0.666667 0.55981(9) 0.0500(12) Uani 1 3 d S T P 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 Cu1 0.0296(2) 0.0266(2) 0.0240(2) -0.00425(15) 0.00493(15) 0.01191(17) Co1 0.0272(3) 0.0272(3) 0.0216(4) 0.000 0.000 0.01362(13) O1 0.0288(12) 0.0288(12) 0.0230(18) 0.000 0.000 0.0144(6) O2 0.0312(12) 0.0493(15) 0.0303(13) -0.0173(11) -0.0056(10) 0.0164(11) O3 0.0241(11) 0.0338(12) 0.0289(12) -0.0108(9) 0.0004(9) 0.0133(10) O4 0.0368(14) 0.0445(14) 0.0305(13) -0.0124(11) -0.0037(10) 0.0228(12) O5 0.0429(14) 0.0301(12) 0.0280(12) -0.0013(10) 0.0106(10) 0.0113(11) O6 0.0545(16) 0.0320(13) 0.0277(12) -0.0027(10) 0.0121(11) 0.0219(12) O7 0.0610(18) 0.0564(17) 0.0303(14) -0.0105(13) 0.0122(13) 0.0243(15) O8 0.156(5) 0.156(5) 0.053(4) 0.000 0.000 0.078(2) C1 0.048(2) 0.072(3) 0.032(2) -0.018(2) -0.0106(18) 0.025(2) C2 0.0291(16) 0.0273(16) 0.0273(16) -0.0010(13) 0.0012(13) 0.0119(14) C3 0.0288(17) 0.0357(19) 0.042(2) -0.0066(15) -0.0052(15) 0.0132(15) C4 0.0290(18) 0.047(2) 0.055(2) -0.0053(18) 0.0016(17) 0.0205(17) C5 0.0362(19) 0.041(2) 0.042(2) -0.0048(16) 0.0067(16) 0.0236(17) C6 0.0313(17) 0.0271(16) 0.0313(17) -0.0024(13) 0.0035(13) 0.0162(14) C7 0.0235(15) 0.0237(15) 0.0272(16) -0.0006(12) 0.0013(12) 0.0105(13) C8 0.047(2) 0.0352(18) 0.0303(18) -0.0069(14) 0.0040(15) 0.0254(17) C9 0.0330(18) 0.0297(18) 0.0345(18) 0.0016(14) 0.0027(15) 0.0080(15) C10 0.0328(18) 0.0284(17) 0.0398(19) -0.0066(14) 0.0016(15) 0.0120(15) C11 0.064(3) 0.037(2) 0.072(3) 0.001(2) 0.018(2) 0.027(2) C12 0.109(4) 0.042(3) 0.098(4) -0.006(3) 0.037(4) 0.045(3) C13 0.083(3) 0.051(3) 0.058(3) -0.014(2) 0.027(3) 0.030(3) C14 0.042(2) 0.045(2) 0.038(2) -0.0120(17) 0.0064(16) 0.0206(18) C15 0.0263(16) 0.0324(18) 0.0307(17) -0.0083(14) 0.0008(13) 0.0109(14) C16 0.077(3) 0.079(3) 0.037(2) -0.019(2) 0.016(2) 0.027(3) Cl1 0.0455(6) 0.0455(6) 0.0440(9) 0.000 0.000 0.0228(3) O9 0.137(4) 0.232(6) 0.073(3) -0.049(3) -0.019(3) 0.147(4) O10 0.0541(18) 0.0541(18) 0.042(3) 0.000 0.000 0.0270(9) 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' Co Co 0.3494 0.9721 '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' 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 O6 Cu1 O5 94.02(10) . . O6 Cu1 O1 89.26(12) . . O5 Cu1 O1 161.46(10) . . O6 Cu1 O3 174.66(11) . . O5 Cu1 O3 89.64(9) . . O1 Cu1 O3 88.49(11) . . O6 Cu1 O2 101.26(10) . . O5 Cu1 O2 91.78(10) . . O1 Cu1 O2 105.49(8) . . O3 Cu1 O2 74.70(9) . . O4 Co1 O4 88.46(10) . 2_765 O4 Co1 O4 88.46(10) . 3_675 O4 Co1 O4 88.46(10) 2_765 3_675 O4 Co1 O3 87.44(9) . . O4 Co1 O3 97.93(10) 2_765 . O4 Co1 O3 172.31(9) 3_675 . O4 Co1 O3 172.31(10) . 2_765 O4 Co1 O3 87.44(9) 2_765 2_765 O4 Co1 O3 97.93(10) 3_675 2_765 O3 Co1 O3 86.68(9) . 2_765 O4 Co1 O3 97.93(10) . 3_675 O4 Co1 O3 172.31(9) 2_765 3_675 O4 Co1 O3 87.44(9) 3_675 3_675 O3 Co1 O3 86.68(9) . 3_675 O3 Co1 O3 86.68(9) 2_765 3_675 Cu1 O1 Cu1 108.28(11) 2_765 3_675 Cu1 O1 Cu1 108.28(11) 2_765 . Cu1 O1 Cu1 108.28(11) 3_675 . Cu1 O1 H1 110.6 2_765 . Cu1 O1 H1 110.6 3_675 . Cu1 O1 H1 110.6 . . C2 O2 C1 118.5(3) . . C2 O2 Cu1 111.80(19) . . C1 O2 Cu1 129.7(2) . . C7 O3 Cu1 120.06(19) . . C7 O3 Co1 128.93(19) . . Cu1 O3 Co1 110.70(10) . . C8 O4 Co1 127.9(2) . . C9 O5 Cu1 123.3(2) . . C15 O6 Cu1 126.7(2) . . C14 O7 C16 116.6(3) . . H8A O8 H8B 88.6 . . H8A O8 H8A 89.1 . 2_765 H8B O8 H8A 82.8 . 2_765 H8A O8 H8A 89.1 . 3_675 H8B O8 H8A 6.3 . 3_675 H8A O8 H8A 89.1 2_765 3_675 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 . . O2 C2 C3 124.9(3) . . O2 C2 C7 113.6(3) . . C3 C2 C7 121.5(3) . . C2 C3 C4 119.6(3) . . C2 C3 H3 120.2 . . C4 C3 H3 120.2 . . C5 C4 C3 120.2(3) . . C5 C4 H4 119.9 . . C3 C4 H4 119.9 . . C4 C5 C6 121.2(3) . . C4 C5 H5 119.4 . . C6 C5 H5 119.4 . . C5 C6 C7 119.8(3) . . C5 C6 C8 116.5(3) . . C7 C6 C8 123.6(3) . . O3 C7 C6 123.5(3) . . O3 C7 C2 118.7(3) . . C6 C7 C2 117.7(3) . . O4 C8 C6 128.3(3) . . O4 C8 H8 115.8 . . C6 C8 H8 115.8 . . O5 C9 C10 128.5(3) . . O5 C9 H9 115.7 . . C10 C9 H9 115.7 . . C9 C10 C15 121.6(3) . . C9 C10 C11 118.1(4) . . C15 C10 C11 120.2(3) . . C12 C11 C10 119.9(4) . . C12 C11 H11 120.1 . . C10 C11 H11 120.1 . . C11 C12 C13 121.0(4) . . C11 C12 H12 119.5 . . C13 C12 H12 119.5 . . C14 C13 C12 121.6(4) . . C14 C13 H13 119.2 . . C12 C13 H13 119.2 . . O7 C14 C13 126.4(4) . . O7 C14 C15 113.6(3) . . C13 C14 C15 120.0(4) . . O6 C15 C10 125.2(3) . . O6 C15 C14 117.5(3) . . C10 C15 C14 117.3(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 . . O9 Cl1 O9 109.1(2) 2_665 3_565 O9 Cl1 O9 109.1(2) 2_665 . O9 Cl1 O9 109.1(2) 3_565 . O9 Cl1 O10 109.8(2) 2_665 . O9 Cl1 O10 109.8(2) 3_565 . O9 Cl1 O10 109.8(2) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cu1 O6 1.877(2) . Cu1 O5 1.942(2) . Cu1 O1 1.9590(14) . Cu1 O3 1.997(2) . Cu1 O2 2.274(2) . Co1 O4 2.062(2) . Co1 O4 2.062(2) 2_765 Co1 O4 2.062(2) 3_675 Co1 O3 2.062(2) . Co1 O3 2.062(2) 2_765 Co1 O3 2.062(2) 3_675 O1 H1 0.9800 . O2 C2 1.361(4) . O2 C1 1.429(4) . O3 C7 1.326(4) . O4 C8 1.230(4) . O5 C9 1.248(4) . O6 C15 1.278(4) . O7 C14 1.349(5) . O7 C16 1.430(5) . O8 H8A 0.8503 . O8 H8B 1.0934 . O8 H8A 0.8504 2_765 O8 H8A 0.8504 3_675 C1 H1A 0.9600 . C1 H1B 0.9600 . C1 H1C 0.9600 . C2 C3 1.379(5) . C2 C7 1.417(4) . C3 C4 1.395(5) . C3 H3 0.9300 . C4 C5 1.364(6) . C4 H4 0.9300 . C5 C6 1.402(5) . C5 H5 0.9300 . C6 C7 1.407(4) . C6 C8 1.438(5) . C8 H8 0.9300 . C9 C10 1.404(5) . C9 H9 0.9300 . C10 C15 1.410(5) . C10 C11 1.422(5) . C11 C12 1.350(7) . C11 H11 0.9300 . C12 C13 1.380(7) . C12 H12 0.9300 . C13 C14 1.360(6) . C13 H13 0.9300 . C14 C15 1.442(5) . C16 H16A 0.9600 . C16 H16B 0.9600 . C16 H16C 0.9600 . Cl1 O9 1.390(4) 2_665 Cl1 O9 1.390(4) 3_565 Cl1 O9 1.390(4) . Cl1 O10 1.454(5) . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O8 0.98 1.72 2.701(8) 180.0 . C3 H3 O10 0.93 2.60 3.532(5) 177.8 . C8 H8 O5 0.93 2.46 3.243(4) 141.9 15_556 C9 H9 O4 0.93 2.58 3.325(4) 137.8 14_456