#------------------------------------------------------------------------------ #$Date: 2018-01-16 04:34:49 +0200 (Tue, 16 Jan 2018) $ #$Revision: 205237 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/99/7229973.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_7229973 loop_ _publ_author_name 'Dankhoff, Katja' 'Weber, Birgit' _publ_section_title ; Novel Cu(II) complexes with NNO-Schiff base-like ligands -- structures and magnetic properties ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C7CE02007D _journal_year 2018 _chemical_formula_moiety 'C25 H30 Cu2 N4 O9 S, C H4 O' _chemical_formula_sum 'C26 H34 Cu2 N4 O10 S' _chemical_formula_weight 721.71 _chemical_name_common '[CuL30b]2SO4' _chemical_name_systematic ; ? ; _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 geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2017-07-27 _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2018-01-11 deposited with the CCDC. 2018-01-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.639(11) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.7600(18) _cell_length_b 16.897(3) _cell_length_c 13.781(2) _cell_measurement_reflns_used 9449 _cell_measurement_temperature 133(2) _cell_measurement_theta_max 26.00 _cell_measurement_theta_min 1.76 _cell_volume 2899.3(8) _computing_cell_refinement X-AREA-STOE _computing_data_collection X-AREA-STOE _computing_data_reduction X-AREA-STOE _computing_molecular_graphics ORTEP-III _computing_publication_material PLATON _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_solution SIR97 _diffrn_ambient_temperature 133(2) _diffrn_detector_area_resol_mean 9 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.927 _diffrn_measurement_device_type STOE-STADIVARI _diffrn_measurement_method omega-scan _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0615 _diffrn_reflns_av_unetI/netI 0.0794 _diffrn_reflns_Laue_measured_fraction_full 0.982 _diffrn_reflns_Laue_measured_fraction_max 0.927 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 19204 _diffrn_reflns_point_group_measured_fraction_full 0.982 _diffrn_reflns_point_group_measured_fraction_max 0.927 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.561 _diffrn_reflns_theta_min 1.935 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 1.603 _exptl_absorpt_correction_type none _exptl_crystal_colour 'blue green' _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1488 _exptl_crystal_size_max 0.170 _exptl_crystal_size_mid 0.115 _exptl_crystal_size_min 0.114 _refine_diff_density_max 1.433 _refine_diff_density_min -0.839 _refine_diff_density_rms 0.110 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 390 _refine_ls_number_reflns 6861 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.909 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_gt 0.0468 _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^)+(0.0561P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1030 _refine_ls_wR_factor_ref 0.1117 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4686 _reflns_number_total 6861 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ce02007d2.cif _cod_data_source_block cl112 _cod_original_cell_volume 2899.3(7) _cod_database_code 7229973 _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 ; shelx.res created by SHELXL-2014/7 TITL SIR97 run in space group P 21/c CELL 0.71073 12.7600 16.8967 13.7814 90.000 102.639 90.000 ZERR 4.00 0.0018 0.0026 0.0020 0.000 0.011 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S CU UNIT 104 136 16 40 4 8 MERG 2 FMAP 2 PLAN 10 ACTA BOND $H CONF LIST 4 L.S. 20 TEMP -140.00 WGHT 0.056100 FVAR 0.13761 C11 1 -0.262200 0.047437 0.632414 11.00000 0.02723 0.02494 = 0.02139 -0.00213 0.00302 -0.00133 AFIX 43 H11 2 -0.253434 0.103207 0.630480 11.00000 -1.20000 AFIX 0 C12 1 -0.359715 0.016871 0.639263 11.00000 0.02921 0.03914 = 0.02801 -0.00655 0.00904 -0.00529 AFIX 43 H12 2 -0.418393 0.051117 0.640738 11.00000 -1.20000 AFIX 0 C13 1 -0.372102 -0.064358 0.644021 11.00000 0.03434 0.04795 = 0.02865 -0.01116 0.01126 -0.02090 AFIX 43 H13 2 -0.439387 -0.086219 0.648781 11.00000 -1.20000 AFIX 0 C14 1 -0.286066 -0.113409 0.641807 11.00000 0.04103 0.02446 = 0.02521 -0.00243 0.01231 -0.01823 AFIX 43 H14 2 -0.292387 -0.169203 0.646829 11.00000 -1.20000 AFIX 0 C15 1 -0.189822 -0.078907 0.632018 11.00000 0.03327 0.01884 = 0.01295 -0.00091 0.00381 -0.00794 C16 1 -0.096446 -0.127972 0.619689 11.00000 0.03503 0.01157 = 0.02858 0.00203 0.00278 -0.00628 AFIX 23 H16A 2 -0.078136 -0.166461 0.674973 11.00000 -1.20000 H16B 2 -0.115330 -0.157902 0.556511 11.00000 -1.20000 AFIX 0 C17 1 0.085138 -0.111539 0.613513 11.00000 0.03748 0.01554 = 0.01458 -0.00068 0.00133 0.00553 AFIX 43 H17 2 0.083721 -0.167688 0.609899 11.00000 -1.20000 AFIX 0 C18 1 0.184871 -0.074154 0.612300 11.00000 0.03171 0.02388 = 0.01827 -0.00130 0.00179 0.00853 C19 1 0.194828 0.008513 0.615639 11.00000 0.02373 0.03255 = 0.01310 0.00031 0.00339 0.00272 C20 1 0.297615 0.051043 0.612383 11.00000 0.02733 0.03777 = 0.02270 -0.00303 0.00613 -0.00059 AFIX 133 H20A 2 0.283185 0.107757 0.602274 11.00000 -1.50000 H20B 2 0.326891 0.030187 0.557460 11.00000 -1.50000 H20C 2 0.349711 0.042882 0.675296 11.00000 -1.50000 AFIX 0 C21 1 0.277351 -0.126516 0.608837 11.00000 0.03858 0.04051 = 0.02346 0.00053 0.00222 0.01956 C22 1 0.255740 -0.213257 0.588989 11.00000 0.04993 0.05454 = 0.07911 -0.03571 -0.03209 0.03799 AFIX 133 H22A 2 0.319370 -0.238356 0.573507 11.00000 -1.50000 H22B 2 0.194586 -0.219610 0.532514 11.00000 -1.50000 H22C 2 0.239193 -0.238277 0.648025 11.00000 -1.50000 AFIX 0 C31 1 -0.066467 0.106086 0.850244 11.00000 0.02773 0.01998 = 0.01482 0.00136 0.00433 0.00096 AFIX 43 H31 2 -0.077496 0.161013 0.837175 11.00000 -1.20000 AFIX 0 C32 1 -0.148856 0.061640 0.872415 11.00000 0.02406 0.03123 = 0.01646 -0.00045 0.00555 -0.00364 AFIX 43 H32 2 -0.215664 0.085400 0.875013 11.00000 -1.20000 AFIX 0 C33 1 -0.131770 -0.018866 0.890893 11.00000 0.03346 0.03024 = 0.01755 -0.00171 0.00439 -0.01354 AFIX 43 H33 2 -0.187433 -0.050886 0.905726 11.00000 -1.20000 AFIX 0 C34 1 -0.034556 -0.051770 0.887635 11.00000 0.04635 0.01369 = 0.01537 -0.00141 0.00471 -0.00865 AFIX 43 H34 2 -0.022115 -0.106709 0.899561 11.00000 -1.20000 AFIX 0 C35 1 0.045848 -0.003125 0.866481 11.00000 0.03069 0.01613 = 0.01064 -0.00367 0.00272 -0.00080 C36 1 0.156461 -0.034046 0.866053 11.00000 0.03534 0.01470 = 0.01895 -0.00186 0.00553 0.00408 AFIX 23 H36A 2 0.185275 -0.063062 0.928610 11.00000 -1.20000 H36B 2 0.152720 -0.071180 0.809833 11.00000 -1.20000 AFIX 0 C37 1 0.329053 0.018990 0.869265 11.00000 0.03422 0.02945 = 0.01464 -0.00113 0.00419 0.01549 AFIX 43 H37 2 0.352347 -0.033777 0.885099 11.00000 -1.20000 AFIX 0 C38 1 0.410046 0.075916 0.862037 11.00000 0.02086 0.04326 = 0.01751 -0.00751 -0.00119 0.00907 C39 1 0.384088 0.154359 0.831846 11.00000 0.02353 0.03481 = 0.02217 -0.01198 0.00590 0.00063 C40 1 0.466854 0.213582 0.816295 11.00000 0.02537 0.05078 = 0.05546 -0.01278 0.01211 -0.00961 AFIX 133 H40A 2 0.435434 0.248710 0.760981 11.00000 -1.50000 H40B 2 0.528524 0.185683 0.800817 11.00000 -1.50000 H40C 2 0.490538 0.244944 0.876953 11.00000 -1.50000 AFIX 0 C41 1 0.522481 0.047127 0.882619 11.00000 0.03097 0.06583 = 0.02149 -0.00308 0.00406 0.02245 C42 1 0.541671 -0.039970 0.870939 11.00000 0.03895 0.06296 = 0.03334 0.00050 0.00785 0.03155 AFIX 133 H42A 2 0.610456 -0.047571 0.851589 11.00000 -1.50000 H42B 2 0.483620 -0.061979 0.819455 11.00000 -1.50000 H42C 2 0.543421 -0.067026 0.934173 11.00000 -1.50000 AFIX 0 C61 1 0.273538 0.214137 1.045869 11.00000 0.04026 0.03199 = 0.03274 -0.00057 0.00024 0.00261 AFIX 133 H61A 2 0.333553 0.182475 1.033331 11.00000 -1.50000 H61B 2 0.269130 0.208359 1.115621 11.00000 -1.50000 H61C 2 0.285061 0.269928 1.031790 11.00000 -1.50000 AFIX 0 C71 1 0.362308 -0.214229 0.867892 11.00000 0.13880 0.14773 = 0.06077 -0.04320 0.02100 -0.10481 AFIX 133 H71A 2 0.320487 -0.171693 0.889578 11.00000 -1.50000 H71B 2 0.403419 -0.192851 0.821539 11.00000 -1.50000 H71C 2 0.411759 -0.236789 0.925823 11.00000 -1.50000 AFIX 0 N11 3 -0.178052 -0.000287 0.628346 11.00000 0.02554 0.01666 = 0.01693 0.00013 0.00310 -0.00529 N12 3 -0.003809 -0.076781 0.619041 11.00000 0.02805 0.01306 = 0.01710 0.00171 0.00132 0.00004 N31 3 0.029176 0.073876 0.846585 11.00000 0.02493 0.01457 = 0.01588 -0.00068 0.00161 -0.00094 N32 3 0.227793 0.032454 0.856374 11.00000 0.02593 0.01841 = 0.01522 -0.00049 0.00125 0.00688 O11 4 0.116481 0.056054 0.619847 11.00000 0.02290 0.01825 = 0.02382 -0.00100 0.00627 -0.00111 O12 4 0.368388 -0.102163 0.621662 11.00000 0.03354 0.05635 = 0.07846 0.01881 0.02160 0.01791 O31 4 0.289143 0.181747 0.811644 11.00000 0.02135 0.02361 = 0.02794 -0.00411 0.00629 -0.00072 O32 4 0.600038 0.090418 0.908079 11.00000 0.01637 0.09070 = 0.06395 -0.01887 -0.00216 0.00642 O51 4 -0.069052 0.143277 0.631968 11.00000 0.02074 0.01061 = 0.02717 -0.00167 0.00201 -0.00100 O52 4 0.077764 0.215634 0.737109 11.00000 0.02697 0.01096 = 0.02900 0.00028 -0.00751 -0.00182 O53 4 -0.090037 0.277767 0.673464 11.00000 0.02591 0.01854 = 0.05118 -0.00800 0.00137 0.00425 O54 4 0.024375 0.244279 0.562446 11.00000 0.05528 0.03705 = 0.02328 -0.00015 0.01390 -0.02023 O60 4 0.176231 0.187537 0.983344 11.00000 0.03356 0.02617 = 0.02938 -0.01011 0.01068 -0.00204 AFIX 147 H60 2 0.123845 0.205880 1.003866 11.00000 -1.20000 AFIX 0 O70 4 0.296248 -0.270274 0.822812 11.00000 0.08610 0.06084 = 0.11721 -0.01492 0.05145 -0.01138 AFIX 147 H70 2 0.234440 -0.262405 0.832740 11.00000 -1.50000 AFIX 0 S50 5 -0.013322 0.221330 0.650195 11.00000 0.01975 0.00947 = 0.01840 0.00115 0.00321 -0.00068 CU1 6 -0.029503 0.033854 0.623096 11.00000 0.02083 0.00989 = 0.01584 0.00001 0.00248 -0.00170 CU2 6 0.155937 0.131303 0.819585 11.00000 0.01650 0.01297 = 0.02226 0.00032 0.00341 0.00127 HKLF 4 REM SIR97 run in space group P 21/c REM R1 = 0.0468 for 4686 Fo > 4sig(Fo) and 0.0742 for all 6861 data REM 390 parameters refined using 0 restraints END WGHT 0.0561 0.0000 REM Highest difference peak 1.433, deepest hole -0.839, 1-sigma level 0.110 Q1 1 0.2978 -0.1831 0.8765 11.00000 0.05 1.43 Q2 1 0.3753 -0.2565 0.9018 11.00000 0.05 0.97 Q3 1 0.0383 0.0101 0.6232 11.00000 0.05 0.87 Q4 1 -0.1007 0.0132 0.6192 11.00000 0.05 0.85 Q5 1 0.2249 0.1555 0.8228 11.00000 0.05 0.77 Q6 1 0.0413 0.0598 0.6280 11.00000 0.05 0.76 Q7 1 -0.0916 0.0594 0.6162 11.00000 0.05 0.75 Q8 1 0.0924 0.1018 0.8251 11.00000 0.05 0.72 Q9 1 0.2197 0.1059 0.8199 11.00000 0.05 0.72 Q10 1 0.0923 0.1556 0.8165 11.00000 0.05 0.60 ; _shelx_res_checksum 91313 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 C11 C -0.2622(3) 0.0474(2) 0.6324(3) 0.0249(8) Uani 1 1 d . . H11 H -0.2534 0.1032 0.6305 0.030 Uiso 1 1 calc R U C12 C -0.3597(3) 0.0169(3) 0.6393(3) 0.0317(9) Uani 1 1 d . . H12 H -0.4184 0.0511 0.6407 0.038 Uiso 1 1 calc R U C13 C -0.3721(3) -0.0644(3) 0.6440(3) 0.0363(10) Uani 1 1 d . . H13 H -0.4394 -0.0862 0.6488 0.044 Uiso 1 1 calc R U C14 C -0.2861(3) -0.1134(2) 0.6418(3) 0.0295(9) Uani 1 1 d . . H14 H -0.2924 -0.1692 0.6468 0.035 Uiso 1 1 calc R U C15 C -0.1898(3) -0.0789(2) 0.6320(3) 0.0219(7) Uani 1 1 d . . C16 C -0.0964(3) -0.1280(2) 0.6197(3) 0.0257(8) Uani 1 1 d . . H16A H -0.0781 -0.1665 0.6750 0.031 Uiso 1 1 calc R U H16B H -0.1153 -0.1579 0.5565 0.031 Uiso 1 1 calc R U C17 C 0.0851(3) -0.1115(2) 0.6135(3) 0.0232(7) Uani 1 1 d . . H17 H 0.0837 -0.1677 0.6099 0.028 Uiso 1 1 calc R U C18 C 0.1849(3) -0.0742(2) 0.6123(3) 0.0252(8) Uani 1 1 d . . C19 C 0.1948(3) 0.0085(2) 0.6156(3) 0.0232(8) Uani 1 1 d . . C20 C 0.2976(3) 0.0510(3) 0.6124(3) 0.0292(9) Uani 1 1 d . . H20A H 0.2832 0.1078 0.6023 0.044 Uiso 1 1 calc R U H20B H 0.3269 0.0302 0.5575 0.044 Uiso 1 1 calc R U H20C H 0.3497 0.0429 0.6753 0.044 Uiso 1 1 calc R U C21 C 0.2774(4) -0.1265(3) 0.6088(3) 0.0349(10) Uani 1 1 d . . C22 C 0.2557(4) -0.2133(3) 0.5890(5) 0.068(2) Uani 1 1 d . . H22A H 0.3194 -0.2384 0.5735 0.102 Uiso 1 1 calc R U H22B H 0.1946 -0.2196 0.5325 0.102 Uiso 1 1 calc R U H22C H 0.2392 -0.2383 0.6480 0.102 Uiso 1 1 calc R U C31 C -0.0665(3) 0.1061(2) 0.8502(3) 0.0209(7) Uani 1 1 d . . H31 H -0.0775 0.1610 0.8372 0.025 Uiso 1 1 calc R U C32 C -0.1489(3) 0.0616(2) 0.8724(3) 0.0237(8) Uani 1 1 d . . H32 H -0.2157 0.0854 0.8750 0.028 Uiso 1 1 calc R U C33 C -0.1318(3) -0.0189(2) 0.8909(3) 0.0273(8) Uani 1 1 d . . H33 H -0.1874 -0.0509 0.9057 0.033 Uiso 1 1 calc R U C34 C -0.0346(3) -0.0518(2) 0.8876(3) 0.0254(8) Uani 1 1 d . . H34 H -0.0221 -0.1067 0.8996 0.031 Uiso 1 1 calc R U C35 C 0.0458(3) -0.0031(2) 0.8665(2) 0.0194(7) Uani 1 1 d . . C36 C 0.1565(3) -0.0340(2) 0.8661(3) 0.0231(7) Uani 1 1 d . . H36A H 0.1853 -0.0631 0.9286 0.028 Uiso 1 1 calc R U H36B H 0.1527 -0.0712 0.8098 0.028 Uiso 1 1 calc R U C37 C 0.3291(3) 0.0190(2) 0.8693(3) 0.0263(8) Uani 1 1 d . . H37 H 0.3523 -0.0338 0.8851 0.032 Uiso 1 1 calc R U C38 C 0.4100(3) 0.0759(3) 0.8620(3) 0.0280(8) Uani 1 1 d . . C39 C 0.3841(3) 0.1544(2) 0.8318(3) 0.0267(8) Uani 1 1 d . . C40 C 0.4669(3) 0.2136(3) 0.8163(4) 0.0434(11) Uani 1 1 d . . H40A H 0.4354 0.2487 0.7610 0.065 Uiso 1 1 calc R U H40B H 0.5285 0.1857 0.8008 0.065 Uiso 1 1 calc R U H40C H 0.4905 0.2449 0.8770 0.065 Uiso 1 1 calc R U C41 C 0.5225(3) 0.0471(3) 0.8826(3) 0.0397(11) Uani 1 1 d . . C42 C 0.5417(4) -0.0400(3) 0.8709(3) 0.0451(12) Uani 1 1 d . . H42A H 0.6105 -0.0476 0.8516 0.068 Uiso 1 1 calc R U H42B H 0.4836 -0.0620 0.8195 0.068 Uiso 1 1 calc R U H42C H 0.5434 -0.0670 0.9342 0.068 Uiso 1 1 calc R U C61 C 0.2735(4) 0.2141(3) 1.0459(3) 0.0362(9) Uani 1 1 d . . H61A H 0.3336 0.1825 1.0333 0.054 Uiso 1 1 calc R U H61B H 0.2691 0.2084 1.1156 0.054 Uiso 1 1 calc R U H61C H 0.2851 0.2699 1.0318 0.054 Uiso 1 1 calc R U C71 C 0.3623(8) -0.2142(6) 0.8679(6) 0.116(4) Uani 1 1 d . . H71A H 0.3205 -0.1717 0.8896 0.174 Uiso 1 1 calc R U H71B H 0.4034 -0.1929 0.8215 0.174 Uiso 1 1 calc R U H71C H 0.4118 -0.2368 0.9258 0.174 Uiso 1 1 calc R U N11 N -0.1781(2) -0.00029(18) 0.6283(2) 0.0199(6) Uani 1 1 d . . N12 N -0.0038(2) -0.07678(17) 0.6190(2) 0.0200(6) Uani 1 1 d . . N31 N 0.0292(2) 0.07388(17) 0.8466(2) 0.0189(6) Uani 1 1 d . . N32 N 0.2278(2) 0.03245(18) 0.8564(2) 0.0203(6) Uani 1 1 d . . O11 O 0.11648(19) 0.05605(15) 0.61985(18) 0.0215(5) Uani 1 1 d . . O12 O 0.3684(3) -0.1022(2) 0.6217(3) 0.0547(10) Uani 1 1 d . . O31 O 0.28914(19) 0.18175(16) 0.81164(19) 0.0242(5) Uani 1 1 d . . O32 O 0.6000(2) 0.0904(3) 0.9081(3) 0.0587(11) Uani 1 1 d . . O51 O -0.06905(19) 0.14328(14) 0.63197(19) 0.0200(5) Uani 1 1 d . . O52 O 0.0778(2) 0.21563(14) 0.7371(2) 0.0244(5) Uani 1 1 d . . O53 O -0.0900(2) 0.27777(16) 0.6735(2) 0.0330(7) Uani 1 1 d . . O54 O 0.0244(3) 0.24428(19) 0.5624(2) 0.0377(7) Uani 1 1 d . . O60 O 0.1762(2) 0.18754(17) 0.9833(2) 0.0291(6) Uani 1 1 d . . H60 H 0.1238 0.2059 1.0039 0.035 Uiso 1 1 calc R U O70 O 0.2962(4) -0.2703(3) 0.8228(4) 0.0836(15) Uani 1 1 d . . H70 H 0.2344 -0.2624 0.8327 0.125 Uiso 1 1 calc R U S50 S -0.01332(6) 0.22133(5) 0.65019(6) 0.01602(17) Uani 1 1 d . . Cu1 Cu -0.02950(3) 0.03385(2) 0.62310(3) 0.01575(10) Uani 1 1 d . . Cu2 Cu 0.15594(3) 0.13130(2) 0.81959(3) 0.01737(11) 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 C11 0.0272(18) 0.025(2) 0.0214(18) -0.0021(15) 0.0030(14) -0.0013(14) C12 0.029(2) 0.039(2) 0.028(2) -0.0066(18) 0.0090(16) -0.0053(17) C13 0.034(2) 0.048(3) 0.029(2) -0.011(2) 0.0113(17) -0.0209(19) C14 0.041(2) 0.024(2) 0.025(2) -0.0024(16) 0.0123(17) -0.0182(16) C15 0.0333(19) 0.0188(18) 0.0129(17) -0.0009(14) 0.0038(14) -0.0079(14) C16 0.035(2) 0.0116(16) 0.029(2) 0.0020(15) 0.0028(15) -0.0063(14) C17 0.037(2) 0.0155(17) 0.0146(17) -0.0007(14) 0.0013(14) 0.0055(14) C18 0.032(2) 0.0239(19) 0.0183(18) -0.0013(15) 0.0018(14) 0.0085(15) C19 0.0237(18) 0.033(2) 0.0131(17) 0.0003(15) 0.0034(13) 0.0027(14) C20 0.0273(19) 0.038(2) 0.0227(19) -0.0030(17) 0.0061(15) -0.0006(16) C21 0.039(2) 0.041(3) 0.023(2) 0.0005(19) 0.0022(16) 0.0196(19) C22 0.050(3) 0.055(3) 0.079(4) -0.036(3) -0.032(3) 0.038(3) C31 0.0277(18) 0.0200(18) 0.0148(17) 0.0014(14) 0.0043(13) 0.0010(14) C32 0.0241(18) 0.031(2) 0.0165(17) -0.0005(15) 0.0055(13) -0.0036(14) C33 0.033(2) 0.030(2) 0.0176(18) -0.0017(16) 0.0044(15) -0.0135(16) C34 0.046(2) 0.0137(18) 0.0154(17) -0.0014(14) 0.0047(15) -0.0086(15) C35 0.0307(19) 0.0161(17) 0.0106(16) -0.0037(13) 0.0027(13) -0.0008(14) C36 0.035(2) 0.0147(17) 0.0189(17) -0.0019(14) 0.0055(14) 0.0041(14) C37 0.034(2) 0.029(2) 0.0146(17) -0.0011(15) 0.0042(14) 0.0155(16) C38 0.0209(18) 0.043(2) 0.0175(18) -0.0075(17) -0.0012(13) 0.0091(16) C39 0.0235(18) 0.035(2) 0.0222(19) -0.0120(16) 0.0059(14) 0.0006(15) C40 0.025(2) 0.051(3) 0.055(3) -0.013(2) 0.0121(19) -0.0096(19) C41 0.031(2) 0.066(3) 0.021(2) -0.003(2) 0.0041(16) 0.022(2) C42 0.039(2) 0.063(3) 0.033(2) 0.001(2) 0.0079(18) 0.032(2) C61 0.040(2) 0.032(2) 0.033(2) -0.0006(19) 0.0002(18) 0.0026(18) C71 0.139(7) 0.148(9) 0.061(5) -0.043(5) 0.021(5) -0.105(7) N11 0.0255(15) 0.0167(14) 0.0169(15) 0.0001(12) 0.0031(11) -0.0053(11) N12 0.0280(16) 0.0131(14) 0.0171(15) 0.0017(11) 0.0013(11) 0.0000(11) N31 0.0249(15) 0.0146(14) 0.0159(14) -0.0007(12) 0.0016(11) -0.0009(11) N32 0.0259(15) 0.0184(15) 0.0152(14) -0.0005(12) 0.0013(11) 0.0069(12) O11 0.0229(12) 0.0182(12) 0.0238(13) -0.0010(10) 0.0063(10) -0.0011(9) O12 0.0335(18) 0.056(2) 0.078(3) 0.019(2) 0.0216(17) 0.0179(16) O31 0.0213(12) 0.0236(14) 0.0279(14) -0.0041(11) 0.0063(10) -0.0007(10) O32 0.0164(15) 0.091(3) 0.064(2) -0.019(2) -0.0022(14) 0.0064(17) O51 0.0207(12) 0.0106(12) 0.0272(13) -0.0017(10) 0.0020(10) -0.0010(9) O52 0.0270(13) 0.0110(12) 0.0290(14) 0.0003(11) -0.0075(10) -0.0018(9) O53 0.0259(14) 0.0185(14) 0.0512(19) -0.0080(13) 0.0014(12) 0.0043(10) O54 0.0553(19) 0.0371(18) 0.0233(15) -0.0002(13) 0.0139(13) -0.0202(14) O60 0.0336(15) 0.0262(15) 0.0294(15) -0.0101(12) 0.0107(12) -0.0020(11) O70 0.086(3) 0.061(3) 0.117(4) -0.015(3) 0.051(3) -0.011(2) S50 0.0197(4) 0.0095(4) 0.0184(4) 0.0012(3) 0.0032(3) -0.0007(3) Cu1 0.0208(2) 0.00989(19) 0.0158(2) 0.00001(16) 0.00248(15) -0.00170(15) Cu2 0.0165(2) 0.0130(2) 0.0223(2) 0.00032(17) 0.00341(15) 0.00127(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N11 C11 C12 121.3(4) N11 C11 H11 119.4 C12 C11 H11 119.4 C11 C12 C13 119.5(4) C11 C12 H12 120.3 C13 C12 H12 120.3 C14 C13 C12 119.6(4) C14 C13 H13 120.2 C12 C13 H13 120.2 C13 C14 C15 118.2(4) C13 C14 H14 120.9 C15 C14 H14 120.9 N11 C15 C14 121.8(4) N11 C15 C16 116.6(3) C14 C15 C16 121.5(3) N12 C16 C15 109.8(3) N12 C16 H16A 109.7 C15 C16 H16A 109.7 N12 C16 H16B 109.7 C15 C16 H16B 109.7 H16A C16 H16B 108.2 N12 C17 C18 126.6(3) N12 C17 H17 116.7 C18 C17 H17 116.7 C19 C18 C17 121.1(3) C19 C18 C21 121.9(4) C17 C18 C21 117.1(4) O11 C19 C18 123.7(3) O11 C19 C20 113.1(3) C18 C19 C20 123.2(3) C19 C20 H20A 109.5 C19 C20 H20B 109.5 H20A C20 H20B 109.5 C19 C20 H20C 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 O12 C21 C18 122.5(4) O12 C21 C22 119.4(4) C18 C21 C22 118.1(4) C21 C22 H22A 109.5 C21 C22 H22B 109.5 H22A C22 H22B 109.5 C21 C22 H22C 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 N31 C31 C32 121.9(3) N31 C31 H31 119.0 C32 C31 H31 119.0 C31 C32 C33 118.4(3) C31 C32 H32 120.8 C33 C32 H32 120.8 C34 C33 C32 119.8(3) C34 C33 H33 120.1 C32 C33 H33 120.1 C33 C34 C35 118.7(3) C33 C34 H34 120.6 C35 C34 H34 120.6 N31 C35 C34 121.7(3) N31 C35 C36 116.4(3) C34 C35 C36 122.0(3) N32 C36 C35 109.5(3) N32 C36 H36A 109.8 C35 C36 H36A 109.8 N32 C36 H36B 109.8 C35 C36 H36B 109.8 H36A C36 H36B 108.2 N32 C37 C38 126.2(4) N32 C37 H37 116.9 C38 C37 H37 116.9 C39 C38 C37 121.8(3) C39 C38 C41 121.4(4) C37 C38 C41 116.7(4) O31 C39 C38 124.0(4) O31 C39 C40 113.1(4) C38 C39 C40 122.8(4) C39 C40 H40A 109.5 C39 C40 H40B 109.5 H40A C40 H40B 109.5 C39 C40 H40C 109.5 H40A C40 H40C 109.5 H40B C40 H40C 109.5 O32 C41 C38 123.3(5) O32 C41 C42 118.4(4) C38 C41 C42 118.3(4) C41 C42 H42A 109.5 C41 C42 H42B 109.5 H42A C42 H42B 109.5 C41 C42 H42C 109.5 H42A C42 H42C 109.5 H42B C42 H42C 109.5 O60 C61 H61A 109.5 O60 C61 H61B 109.5 H61A C61 H61B 109.5 O60 C61 H61C 109.5 H61A C61 H61C 109.5 H61B C61 H61C 109.5 O70 C71 H71A 109.5 O70 C71 H71B 109.5 H71A C71 H71B 109.5 O70 C71 H71C 109.5 H71A C71 H71C 109.5 H71B C71 H71C 109.5 C15 N11 C11 119.5(3) C15 N11 Cu1 113.8(2) C11 N11 Cu1 126.7(3) C17 N12 C16 116.8(3) C17 N12 Cu1 127.4(3) C16 N12 Cu1 115.8(2) C35 N31 C31 119.4(3) C35 N31 Cu2 114.4(2) C31 N31 Cu2 126.2(2) C37 N32 C36 118.4(3) C37 N32 Cu2 126.7(3) C36 N32 Cu2 114.8(2) C19 O11 Cu1 130.3(2) C39 O31 Cu2 129.6(3) S50 O51 Cu1 137.41(15) S50 O52 Cu2 136.82(16) C61 O60 Cu2 126.4(2) C61 O60 H60 109.5 Cu2 O60 H60 122.0 C71 O70 H70 109.5 O54 S50 O53 111.82(19) O54 S50 O52 110.36(17) O53 S50 O52 108.20(16) O54 S50 O51 109.20(16) O53 S50 O51 107.34(15) O52 S50 O51 109.87(14) N12 Cu1 O11 90.98(12) N12 Cu1 O51 173.97(11) O11 Cu1 O51 94.78(10) N12 Cu1 N11 83.58(13) O11 Cu1 N11 174.49(12) O51 Cu1 N11 90.63(11) N32 Cu2 O31 91.35(12) N32 Cu2 O52 160.29(12) O31 Cu2 O52 89.36(11) N32 Cu2 N31 83.52(12) O31 Cu2 N31 171.92(12) O52 Cu2 N31 97.58(11) N32 Cu2 O60 98.54(11) O31 Cu2 O60 87.90(10) O52 Cu2 O60 101.17(10) N31 Cu2 O60 86.69(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C11 N11 1.354(5) C11 C12 1.369(5) C11 H11 0.9500 C12 C13 1.385(6) C12 H12 0.9500 C13 C14 1.381(6) C13 H13 0.9500 C14 C15 1.392(5) C14 H14 0.9500 C15 N11 1.339(5) C15 C16 1.491(5) C16 N12 1.466(4) C16 H16A 0.9900 C16 H16B 0.9900 C17 N12 1.295(4) C17 C18 1.424(5) C17 H17 0.9500 C18 C19 1.402(5) C18 C21 1.484(5) C19 O11 1.294(4) C19 C20 1.505(5) C20 H20A 0.9800 C20 H20B 0.9800 C20 H20C 0.9800 C21 O12 1.208(6) C21 C22 1.505(7) C22 H22A 0.9800 C22 H22B 0.9800 C22 H22C 0.9800 C31 N31 1.347(4) C31 C32 1.380(5) C31 H31 0.9500 C32 C33 1.392(6) C32 H32 0.9500 C33 C34 1.369(6) C33 H33 0.9500 C34 C35 1.394(5) C34 H34 0.9500 C35 N31 1.337(4) C35 C36 1.506(5) C36 N32 1.470(5) C36 H36A 0.9900 C36 H36B 0.9900 C37 N32 1.285(5) C37 C38 1.431(6) C37 H37 0.9500 C38 C39 1.407(6) C38 C41 1.482(5) C39 O31 1.270(4) C39 C40 1.504(6) C40 H40A 0.9800 C40 H40B 0.9800 C40 H40C 0.9800 C41 O32 1.219(6) C41 C42 1.506(7) C42 H42A 0.9800 C42 H42B 0.9800 C42 H42C 0.9800 C61 O60 1.421(5) C61 H61A 0.9800 C61 H61B 0.9800 C61 H61C 0.9800 C71 O70 1.328(8) C71 H71A 0.9800 C71 H71B 0.9800 C71 H71C 0.9800 N11 Cu1 1.998(3) N12 Cu1 1.901(3) N31 Cu2 1.990(3) N32 Cu2 1.919(3) O11 Cu1 1.910(2) O31 Cu2 1.926(2) O51 S50 1.493(2) O51 Cu1 1.927(2) O52 S50 1.478(3) O52 Cu2 1.955(3) O53 S50 1.452(3) O54 S50 1.449(3) O60 Cu2 2.410(3) O60 H60 0.8400 O70 H70 0.8400 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 N11 C11 C12 C13 1.2(6) C11 C12 C13 C14 0.0(6) C12 C13 C14 C15 -1.7(6) C13 C14 C15 N11 2.4(6) C13 C14 C15 C16 -174.3(4) N11 C15 C16 N12 7.5(5) C14 C15 C16 N12 -175.6(3) N12 C17 C18 C19 -1.1(6) N12 C17 C18 C21 178.1(4) C17 C18 C19 O11 -0.1(6) C21 C18 C19 O11 -179.2(3) C17 C18 C19 C20 -178.7(3) C21 C18 C19 C20 2.2(6) C19 C18 C21 O12 9.9(6) C17 C18 C21 O12 -169.3(4) C19 C18 C21 C22 -170.4(4) C17 C18 C21 C22 10.4(6) N31 C31 C32 C33 -0.3(5) C31 C32 C33 C34 0.6(5) C32 C33 C34 C35 0.5(5) C33 C34 C35 N31 -2.0(5) C33 C34 C35 C36 177.2(3) N31 C35 C36 N32 7.7(4) C34 C35 C36 N32 -171.5(3) N32 C37 C38 C39 -4.8(6) N32 C37 C38 C41 178.4(4) C37 C38 C39 O31 2.1(6) C41 C38 C39 O31 178.8(3) C37 C38 C39 C40 -175.3(4) C41 C38 C39 C40 1.3(6) C39 C38 C41 O32 25.7(6) C37 C38 C41 O32 -157.5(4) C39 C38 C41 C42 -153.9(4) C37 C38 C41 C42 22.8(5) C14 C15 N11 C11 -1.2(5) C16 C15 N11 C11 175.6(3) C14 C15 N11 Cu1 176.2(3) C16 C15 N11 Cu1 -6.9(4) C12 C11 N11 C15 -0.6(5) C12 C11 N11 Cu1 -177.7(3) C18 C17 N12 C16 -179.7(3) C18 C17 N12 Cu1 2.1(5) C15 C16 N12 C17 176.9(3) C15 C16 N12 Cu1 -4.7(4) C34 C35 N31 C31 2.3(5) C36 C35 N31 C31 -177.0(3) C34 C35 N31 Cu2 179.6(3) C36 C35 N31 Cu2 0.4(4) C32 C31 N31 C35 -1.1(5) C32 C31 N31 Cu2 -178.1(3) C38 C37 N32 C36 179.5(3) C38 C37 N32 Cu2 2.2(5) C35 C36 N32 C37 169.9(3) C35 C36 N32 Cu2 -12.5(3) C18 C19 O11 Cu1 0.1(5) C20 C19 O11 Cu1 178.8(2) C38 C39 O31 Cu2 2.7(5) C40 C39 O31 Cu2 -179.6(3) Cu2 O52 S50 O54 -108.8(3) Cu2 O52 S50 O53 128.6(2) Cu2 O52 S50 O51 11.7(3) Cu1 O51 S50 O54 73.9(3) Cu1 O51 S50 O53 -164.7(2) Cu1 O51 S50 O52 -47.3(3)