#------------------------------------------------------------------------------ #$Date: 2018-01-16 04:34:49 +0200 (Tue, 16 Jan 2018) $ #$Revision: 205237 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/99/7229987.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_7229987 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 'C28 H34 Cu2 N4 O12 S, C H4 O, H2O' _chemical_formula_sum 'C29 H40 Cu2 N4 O14 S' _chemical_formula_weight 827.81 _chemical_name_common '[CuL30c]2SO4' _chemical_name_systematic ; ? ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -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 93.458(9) _cell_angle_beta 96.606(8) _cell_angle_gamma 97.754(8) _cell_formula_units_Z 2 _cell_length_a 6.7842(6) _cell_length_b 15.8946(15) _cell_length_c 15.9754(18) _cell_measurement_reflns_used 11131 _cell_measurement_temperature 133(2) _cell_measurement_theta_max 28.26 _cell_measurement_theta_min 1.76 _cell_volume 1690.5(3) _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 0.980 _diffrn_measured_fraction_theta_max 0.925 _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 0.2163 _diffrn_reflns_av_unetI/netI 0.1729 _diffrn_reflns_Laue_measured_fraction_full 0.980 _diffrn_reflns_Laue_measured_fraction_max 0.925 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 19376 _diffrn_reflns_point_group_measured_fraction_full 0.980 _diffrn_reflns_point_group_measured_fraction_max 0.925 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.528 _diffrn_reflns_theta_min 1.755 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 1.394 _exptl_absorpt_correction_type none _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 852 _exptl_crystal_size_max 0.157 _exptl_crystal_size_mid 0.095 _exptl_crystal_size_min 0.086 _refine_diff_density_max 1.773 _refine_diff_density_min -3.484 _refine_diff_density_rms 0.261 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 451 _refine_ls_number_reflns 7952 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.137 _refine_ls_R_factor_all 0.1789 _refine_ls_R_factor_gt 0.1353 _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 0.3285 _refine_ls_wR_factor_ref 0.3733 _reflns_number_gt 4466 _reflns_number_total 7952 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ce02007d2.cif _cod_data_source_block cl126 _cod_database_code 7229987 _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 -1 CELL 0.71073 6.7842 15.8946 15.9754 93.458 96.606 97.754 ZERR 2.00 0.0006 0.0015 0.0018 0.009 0.008 0.008 LATT 1 SFAC C H N O CU S UNIT 58 76 8 28 4 2 MERG 2 FMAP 2 PLAN 10 ACTA BOND $H CONF LIST 4 L.S. 20 TEMP -140.00 WGHT 0.200000 FVAR 0.27584 C1 1 0.317951 0.060800 -0.076501 11.00000 0.03214 0.03198 = 0.05826 0.00458 0.01000 0.00208 AFIX 43 H1 2 0.348512 0.121127 -0.070182 11.00000 -1.20000 AFIX 0 C2 1 0.328808 0.018346 -0.153123 11.00000 0.04249 0.04427 = 0.04284 0.00820 0.00806 0.00155 AFIX 43 H2 2 0.369346 0.048877 -0.199038 11.00000 -1.20000 AFIX 0 C3 1 0.280384 -0.068574 -0.162373 11.00000 0.04238 0.04497 = 0.05062 0.00219 0.00877 0.00046 AFIX 43 H3 2 0.286244 -0.098262 -0.215249 11.00000 -1.20000 AFIX 0 C4 1 0.223940 -0.112830 -0.096529 11.00000 0.03833 0.03356 = 0.06154 -0.00758 0.01300 0.00248 AFIX 43 H4 2 0.189473 -0.173009 -0.103066 11.00000 -1.20000 AFIX 0 C5 1 0.217796 -0.067636 -0.018852 11.00000 0.03542 0.03104 = 0.05624 0.00014 0.00917 0.00208 C6 1 0.161729 -0.110012 0.058187 11.00000 0.03750 0.03073 = 0.05405 0.00007 0.00953 0.00278 AFIX 23 H6A 2 0.023743 -0.141162 0.046371 11.00000 -1.20000 H6B 2 0.253900 -0.151618 0.072900 11.00000 -1.20000 AFIX 0 C7 1 0.150325 -0.074801 0.203092 11.00000 0.02972 0.02449 = 0.06172 0.00107 0.01604 0.00236 AFIX 43 H7 2 0.122588 -0.134840 0.204738 11.00000 -1.20000 AFIX 0 C8 1 0.162678 -0.025036 0.281635 11.00000 0.03293 0.03188 = 0.05721 0.00101 0.01149 0.00357 C9 1 0.206840 0.066051 0.282977 11.00000 0.03251 0.03498 = 0.05345 0.00515 0.00776 0.00295 C10 1 0.250561 0.202128 0.359227 11.00000 0.06443 0.02928 = 0.05590 -0.00283 0.01369 0.01012 AFIX 23 H10A 2 0.194291 0.228002 0.407448 11.00000 -1.20000 H10B 2 0.188302 0.222737 0.306650 11.00000 -1.20000 AFIX 0 C11 1 0.471447 0.228634 0.368676 11.00000 0.05802 0.04038 = 0.06510 -0.00303 0.01363 -0.00160 AFIX 133 H11A 2 0.526971 0.226845 0.427845 11.00000 -1.50000 H11B 2 0.500369 0.286735 0.351524 11.00000 -1.50000 H11C 2 0.532421 0.189775 0.332880 11.00000 -1.50000 AFIX 0 C12 1 0.125943 -0.075658 0.353692 11.00000 0.03339 0.03635 = 0.05942 -0.00078 0.00848 0.00399 C13 1 0.158789 -0.084527 0.501505 11.00000 0.03694 0.05039 = 0.05977 0.00510 0.01423 0.00021 AFIX 23 H13A 2 0.204849 -0.140662 0.493692 11.00000 -1.20000 H13B 2 0.013845 -0.093882 0.507204 11.00000 -1.20000 AFIX 0 C14 1 0.275118 -0.034312 0.579497 11.00000 0.05398 0.05867 = 0.05801 0.00102 0.01746 0.00768 AFIX 133 H14A 2 0.418762 -0.027731 0.574185 11.00000 -1.50000 H14B 2 0.249605 -0.064724 0.629605 11.00000 -1.50000 H14C 2 0.232224 0.021996 0.585142 11.00000 -1.50000 AFIX 0 C21 1 0.134514 0.339348 -0.141780 11.00000 0.03446 0.03202 = 0.05755 0.00382 0.01071 -0.00063 AFIX 43 H21 2 0.154276 0.290318 -0.112459 11.00000 -1.20000 AFIX 0 C22 1 0.065901 0.330735 -0.226527 11.00000 0.03888 0.03506 = 0.06471 -0.00522 0.01188 -0.00438 AFIX 43 H22 2 0.039202 0.275940 -0.256088 11.00000 -1.20000 AFIX 0 C23 1 0.035478 0.403362 -0.269180 11.00000 0.04876 0.04496 = 0.04408 0.00171 0.00905 -0.00107 AFIX 43 H23 2 -0.012872 0.398330 -0.327741 11.00000 -1.20000 AFIX 0 C24 1 0.077415 0.483458 -0.224188 11.00000 0.03730 0.03829 = 0.05681 0.00606 0.01221 0.00066 AFIX 43 H24 2 0.058718 0.533622 -0.251749 11.00000 -1.20000 AFIX 0 C25 1 0.145961 0.488100 -0.139616 11.00000 0.02927 0.03103 = 0.05291 0.00293 0.00984 -0.00055 C26 1 0.200665 0.571412 -0.087598 11.00000 0.03728 0.03399 = 0.06152 -0.00245 0.00862 -0.00289 AFIX 23 H26A 2 0.310214 0.606879 -0.110610 11.00000 -1.20000 H26B 2 0.083385 0.602499 -0.089909 11.00000 -1.20000 AFIX 0 C27 1 0.316398 0.622327 0.055864 11.00000 0.03349 0.03328 = 0.05829 0.00247 0.01563 -0.00235 AFIX 43 H27 2 0.311509 0.676517 0.034302 11.00000 -1.20000 AFIX 0 C28 1 0.375589 0.621899 0.141432 11.00000 0.03656 0.03609 = 0.05302 -0.00248 0.00631 0.00539 C29 1 0.385570 0.541684 0.179633 11.00000 0.03503 0.02834 = 0.05617 0.00872 0.01581 0.00620 C30 1 0.435038 0.462640 0.300080 11.00000 0.05169 0.04148 = 0.05792 0.00554 0.00894 0.00446 AFIX 23 H30A 2 0.542483 0.433185 0.280092 11.00000 -1.20000 H30B 2 0.305001 0.425419 0.284787 11.00000 -1.20000 AFIX 0 C31 1 0.475327 0.484430 0.395262 11.00000 0.07858 0.05022 = 0.06169 -0.00313 -0.00208 0.01759 AFIX 133 H31A 2 0.598979 0.524937 0.408660 11.00000 -1.50000 H31B 2 0.489886 0.432419 0.423941 11.00000 -1.50000 H31C 2 0.363026 0.509946 0.414398 11.00000 -1.50000 AFIX 0 C32 1 0.432469 0.706362 0.188013 11.00000 0.03428 0.03980 = 0.06504 -0.00465 0.01033 0.00964 C33 1 0.535363 0.787490 0.316814 11.00000 0.05581 0.02915 = 0.05466 -0.00596 0.01558 0.00371 AFIX 23 H33A 2 0.432315 0.825623 0.307334 11.00000 -1.20000 H33B 2 0.660431 0.814374 0.297208 11.00000 -1.20000 AFIX 0 C34 1 0.571286 0.773217 0.406859 11.00000 0.10816 0.04491 = 0.05742 0.00083 0.02023 -0.01435 AFIX 133 H34A 2 0.452430 0.739422 0.423606 11.00000 -1.50000 H34B 2 0.598659 0.828163 0.440344 11.00000 -1.50000 H34C 2 0.686756 0.742534 0.416755 11.00000 -1.50000 AFIX 0 C61 1 0.041576 0.623862 0.525869 11.00000 0.08432 0.06636 = 0.07423 -0.00396 0.01553 0.01934 AFIX 133 H61A 2 -0.085827 0.645284 0.511189 11.00000 -1.50000 H61B 2 0.052587 0.576468 0.485305 11.00000 -1.50000 H61C 2 0.152962 0.669644 0.524093 11.00000 -1.50000 AFIX 0 N1 3 0.264301 0.017912 -0.009793 11.00000 0.03388 0.03030 = 0.05669 0.00113 0.00499 0.00321 N2 3 0.173306 -0.046163 0.129067 11.00000 0.03178 0.03628 = 0.06163 -0.00706 0.01145 0.00526 N21 3 0.174264 0.417838 -0.099691 11.00000 0.03816 0.02494 = 0.05451 0.00267 0.01480 0.00163 N22 3 0.266191 0.555772 0.001193 11.00000 0.03855 0.02617 = 0.05628 0.00498 0.01182 0.00048 O1 4 0.241230 0.107126 0.220934 11.00000 0.04566 0.03440 = 0.05412 -0.00447 0.00653 0.00167 O2 4 0.203433 0.108856 0.356180 11.00000 0.05276 0.03390 = 0.05259 -0.00348 0.01583 0.00235 O3 4 0.045516 -0.148985 0.345989 11.00000 0.05960 0.03792 = 0.05170 0.00171 0.01504 -0.00630 O4 4 0.194670 -0.035130 0.430137 11.00000 0.04427 0.03711 = 0.05133 0.00621 0.00927 0.00069 O21 4 0.356192 0.470180 0.138527 11.00000 0.04334 0.02818 = 0.05708 -0.00496 0.01573 0.00128 O22 4 0.431173 0.544415 0.263088 11.00000 0.04877 0.03097 = 0.05080 0.00560 0.01054 0.00266 O23 4 0.445826 0.773435 0.151401 11.00000 0.05608 0.03377 = 0.06030 0.00600 0.01050 0.00301 O24 4 0.467485 0.705551 0.271111 11.00000 0.04852 0.02923 = 0.05367 -0.00246 0.01026 -0.00196 O52 4 0.273076 0.179573 0.064505 11.00000 0.05650 0.02817 = 0.05746 0.00208 0.00945 -0.00034 O53 4 0.471555 0.284234 0.166119 11.00000 0.04128 0.04703 = 0.06262 0.00987 0.00072 0.00144 O54 4 0.117567 0.282767 0.141728 11.00000 0.04022 0.04213 = 0.07527 0.00884 0.02674 0.00863 O55 4 0.318459 0.323576 0.031813 11.00000 0.05734 0.02563 = 0.05581 0.00706 0.01879 0.00698 O62 4 0.048572 0.596173 0.605563 11.00000 0.11764 0.07572 = 0.06985 0.00863 0.01192 -0.00507 AFIX 143 H62 2 0.083283 0.637990 0.641386 11.00000 -1.50000 AFIX 0 O71 4 0.847792 0.285709 0.258174 11.00000 0.04950 0.08446 = 0.06159 0.00296 0.01047 0.01432 CU1 5 0.240972 0.068910 0.105070 11.00000 0.03717 0.02683 = 0.05416 0.00260 0.01091 0.00135 CU2 5 0.280151 0.439604 0.021436 11.00000 0.03638 0.02662 = 0.05406 0.00192 0.01229 0.00130 S51 6 0.295688 0.268893 0.105670 11.00000 0.03571 0.02464 = 0.05467 0.00143 0.01296 0.00076 HKLF 4 REM SIR97 run in space group P -1 REM R1 = 0.1353 for 4466 Fo > 4sig(Fo) and 0.1789 for all 7952 data REM 451 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.773, deepest hole -3.484, 1-sigma level 0.261 Q1 1 0.2615 0.4625 -0.0497 11.00000 0.05 1.77 Q2 1 0.2360 0.0960 0.0362 11.00000 0.05 1.63 Q3 1 0.1925 0.3791 0.0191 11.00000 0.05 1.61 Q4 1 0.3654 0.5030 0.0281 11.00000 0.05 1.59 Q5 1 0.3052 0.4146 0.0981 11.00000 0.05 1.53 Q6 1 0.3223 0.1239 0.1019 11.00000 0.05 1.48 Q7 1 0.2392 0.0369 0.1700 11.00000 0.05 1.41 Q8 1 0.3192 0.1386 0.1165 11.00000 0.05 1.39 Q9 1 0.2285 0.1417 0.1471 11.00000 0.05 1.25 Q10 1 0.1628 0.0158 0.1173 11.00000 0.05 1.23 ; _shelx_res_checksum 2241 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 C1 C 0.3180(11) 0.0608(5) -0.0765(6) 0.0406(18) Uani 1 1 d . . H1 H 0.3485 0.1211 -0.0702 0.049 Uiso 1 1 calc R U C2 C 0.3288(12) 0.0183(6) -0.1531(6) 0.0432(18) Uani 1 1 d . . H2 H 0.3693 0.0489 -0.1990 0.052 Uiso 1 1 calc R U C3 C 0.2804(13) -0.0686(6) -0.1624(6) 0.046(2) Uani 1 1 d . . H3 H 0.2862 -0.0983 -0.2152 0.056 Uiso 1 1 calc R U C4 C 0.2239(12) -0.1128(5) -0.0965(6) 0.045(2) Uani 1 1 d . . H4 H 0.1895 -0.1730 -0.1031 0.054 Uiso 1 1 calc R U C5 C 0.2178(12) -0.0676(5) -0.0189(6) 0.0410(18) Uani 1 1 d . . C6 C 0.1617(12) -0.1100(5) 0.0582(6) 0.0408(18) Uani 1 1 d . . H6A H 0.0237 -0.1412 0.0464 0.049 Uiso 1 1 calc R U H6B H 0.2539 -0.1516 0.0729 0.049 Uiso 1 1 calc R U C7 C 0.1503(11) -0.0748(5) 0.2031(6) 0.0381(18) Uani 1 1 d . . H7 H 0.1226 -0.1348 0.2047 0.046 Uiso 1 1 calc R U C8 C 0.1627(11) -0.0250(5) 0.2816(6) 0.0404(18) Uani 1 1 d . . C9 C 0.2068(11) 0.0661(5) 0.2830(6) 0.0402(18) Uani 1 1 d . . C10 C 0.2506(15) 0.2021(5) 0.3592(7) 0.049(2) Uani 1 1 d . . H10A H 0.1943 0.2280 0.4074 0.059 Uiso 1 1 calc R U H10B H 0.1883 0.2227 0.3066 0.059 Uiso 1 1 calc R U C11 C 0.4714(15) 0.2286(6) 0.3687(7) 0.055(2) Uani 1 1 d . . H11A H 0.5270 0.2268 0.4278 0.083 Uiso 1 1 calc R U H11B H 0.5004 0.2867 0.3515 0.083 Uiso 1 1 calc R U H11C H 0.5324 0.1898 0.3329 0.083 Uiso 1 1 calc R U C12 C 0.1259(12) -0.0757(5) 0.3537(6) 0.0431(19) Uani 1 1 d . . C13 C 0.1588(13) -0.0845(6) 0.5015(6) 0.049(2) Uani 1 1 d . . H13A H 0.2048 -0.1407 0.4937 0.059 Uiso 1 1 calc R U H13B H 0.0138 -0.0939 0.5072 0.059 Uiso 1 1 calc R U C14 C 0.2751(15) -0.0343(7) 0.5795(7) 0.056(2) Uani 1 1 d . . H14A H 0.4188 -0.0277 0.5742 0.084 Uiso 1 1 calc R U H14B H 0.2496 -0.0647 0.6296 0.084 Uiso 1 1 calc R U H14C H 0.2322 0.0220 0.5851 0.084 Uiso 1 1 calc R U C21 C 0.1345(11) 0.3393(5) -0.1418(6) 0.0414(18) Uani 1 1 d . . H21 H 0.1543 0.2903 -0.1125 0.050 Uiso 1 1 calc R U C22 C 0.0659(12) 0.3307(6) -0.2265(7) 0.047(2) Uani 1 1 d . . H22 H 0.0392 0.2759 -0.2561 0.056 Uiso 1 1 calc R U C23 C 0.0355(13) 0.4034(6) -0.2692(6) 0.0465(19) Uani 1 1 d . . H23 H -0.0129 0.3983 -0.3277 0.056 Uiso 1 1 calc R U C24 C 0.0774(12) 0.4835(5) -0.2242(6) 0.0440(19) Uani 1 1 d . . H24 H 0.0587 0.5336 -0.2517 0.053 Uiso 1 1 calc R U C25 C 0.1460(11) 0.4881(5) -0.1396(6) 0.0378(17) Uani 1 1 d . . C26 C 0.2007(13) 0.5714(5) -0.0876(6) 0.045(2) Uani 1 1 d . . H26A H 0.3102 0.6069 -0.1106 0.054 Uiso 1 1 calc R U H26B H 0.0834 0.6025 -0.0899 0.054 Uiso 1 1 calc R U C27 C 0.3164(12) 0.6223(5) 0.0559(6) 0.0416(19) Uani 1 1 d . . H27 H 0.3115 0.6765 0.0343 0.050 Uiso 1 1 calc R U C28 C 0.3756(12) 0.6219(5) 0.1414(6) 0.0421(18) Uani 1 1 d . . C29 C 0.3856(11) 0.5417(5) 0.1796(6) 0.0387(18) Uani 1 1 d . . C30 C 0.4350(14) 0.4626(6) 0.3001(7) 0.050(2) Uani 1 1 d . . H30A H 0.5425 0.4332 0.2801 0.060 Uiso 1 1 calc R U H30B H 0.3050 0.4254 0.2848 0.060 Uiso 1 1 calc R U C31 C 0.4753(18) 0.4844(7) 0.3953(7) 0.064(3) Uani 1 1 d . . H31A H 0.5990 0.5249 0.4087 0.096 Uiso 1 1 calc R U H31B H 0.4899 0.4324 0.4239 0.096 Uiso 1 1 calc R U H31C H 0.3630 0.5099 0.4144 0.096 Uiso 1 1 calc R U C32 C 0.4325(12) 0.7064(6) 0.1880(7) 0.046(2) Uani 1 1 d . . C33 C 0.5354(14) 0.7875(5) 0.3168(6) 0.046(2) Uani 1 1 d . . H33A H 0.4323 0.8256 0.3073 0.056 Uiso 1 1 calc R U H33B H 0.6604 0.8144 0.2972 0.056 Uiso 1 1 calc R U C34 C 0.571(2) 0.7732(7) 0.4069(8) 0.072(3) Uani 1 1 d . . H34A H 0.4524 0.7394 0.4236 0.108 Uiso 1 1 calc R U H34B H 0.5987 0.8282 0.4403 0.108 Uiso 1 1 calc R U H34C H 0.6868 0.7425 0.4168 0.108 Uiso 1 1 calc R U C61 C 0.042(2) 0.6239(8) 0.5259(9) 0.074(3) Uani 1 1 d . . H61A H -0.0858 0.6453 0.5112 0.111 Uiso 1 1 calc R U H61B H 0.0526 0.5765 0.4853 0.111 Uiso 1 1 calc R U H61C H 0.1530 0.6696 0.5241 0.111 Uiso 1 1 calc R U N1 N 0.2643(10) 0.0179(4) -0.0098(5) 0.0406(15) Uani 1 1 d . . N2 N 0.1733(10) -0.0462(4) 0.1291(5) 0.0432(17) Uani 1 1 d . . N21 N 0.1743(10) 0.4178(4) -0.0997(5) 0.0388(15) Uani 1 1 d . . N22 N 0.2662(10) 0.5558(4) 0.0012(5) 0.0402(15) Uani 1 1 d . . O1 O 0.2412(9) 0.1071(4) 0.2209(4) 0.0454(14) Uani 1 1 d . . O2 O 0.2034(9) 0.1089(4) 0.3562(4) 0.0463(14) Uani 1 1 d . . O3 O 0.0455(10) -0.1490(4) 0.3460(4) 0.0504(15) Uani 1 1 d . . O4 O 0.1947(9) -0.0351(4) 0.4301(4) 0.0443(13) Uani 1 1 d . . O21 O 0.3562(8) 0.4702(3) 0.1385(4) 0.0428(13) Uani 1 1 d . . O22 O 0.4312(9) 0.5444(4) 0.2631(4) 0.0434(13) Uani 1 1 d . . O23 O 0.4458(10) 0.7734(4) 0.1514(4) 0.0500(15) Uani 1 1 d . . O24 O 0.4675(9) 0.7056(4) 0.2711(4) 0.0444(14) Uani 1 1 d . . O52 O 0.2731(10) 0.1796(4) 0.0645(4) 0.0478(15) Uani 1 1 d . . O53 O 0.4716(9) 0.2842(4) 0.1661(5) 0.0510(15) Uani 1 1 d . . O54 O 0.1176(9) 0.2828(4) 0.1417(5) 0.0506(16) Uani 1 1 d . . O55 O 0.3185(9) 0.3236(3) 0.0318(4) 0.0451(14) Uani 1 1 d . . O62 O 0.0486(16) 0.5962(6) 0.6056(6) 0.089(3) Uani 1 1 d . . H62 H 0.0833 0.6380 0.6414 0.134 Uiso 1 1 calc R U O71 O 0.8478(10) 0.2857(5) 0.2582(5) 0.065(2) Uani 1 1 d . . Cu1 Cu 0.24097(14) 0.06891(6) 0.10507(7) 0.0393(3) Uani 1 1 d . . Cu2 Cu 0.28015(14) 0.43960(6) 0.02144(7) 0.0388(3) Uani 1 1 d . . S51 S 0.2957(3) 0.26889(11) 0.10567(14) 0.0382(5) 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 C1 0.032(4) 0.032(4) 0.058(5) 0.005(3) 0.010(3) 0.002(3) C2 0.042(4) 0.044(4) 0.043(5) 0.008(4) 0.008(3) 0.002(3) C3 0.042(4) 0.045(5) 0.051(5) 0.002(4) 0.009(4) 0.000(4) C4 0.038(4) 0.034(4) 0.062(6) -0.008(4) 0.013(4) 0.002(3) C5 0.035(4) 0.031(4) 0.056(5) 0.000(3) 0.009(3) 0.002(3) C6 0.038(4) 0.031(4) 0.054(5) 0.000(3) 0.010(3) 0.003(3) C7 0.030(3) 0.024(3) 0.062(6) 0.001(3) 0.016(3) 0.002(3) C8 0.033(4) 0.032(4) 0.057(5) 0.001(3) 0.011(3) 0.004(3) C9 0.033(4) 0.035(4) 0.053(5) 0.005(3) 0.008(3) 0.003(3) C10 0.064(6) 0.029(4) 0.056(6) -0.003(4) 0.014(4) 0.010(4) C11 0.058(5) 0.040(5) 0.065(7) -0.003(4) 0.014(5) -0.002(4) C12 0.033(4) 0.036(4) 0.059(6) -0.001(4) 0.008(4) 0.004(3) C13 0.037(4) 0.050(5) 0.060(6) 0.005(4) 0.014(4) 0.000(4) C14 0.054(5) 0.059(6) 0.058(6) 0.001(5) 0.017(4) 0.008(4) C21 0.034(4) 0.032(4) 0.058(6) 0.004(4) 0.011(3) -0.001(3) C22 0.039(4) 0.035(4) 0.065(6) -0.005(4) 0.012(4) -0.004(3) C23 0.049(5) 0.045(5) 0.044(5) 0.002(4) 0.009(4) -0.001(4) C24 0.037(4) 0.038(4) 0.057(6) 0.006(4) 0.012(4) 0.001(3) C25 0.029(3) 0.031(4) 0.053(5) 0.003(3) 0.010(3) -0.001(3) C26 0.037(4) 0.034(4) 0.062(6) -0.002(4) 0.009(4) -0.003(3) C27 0.033(4) 0.033(4) 0.058(6) 0.002(4) 0.016(3) -0.002(3) C28 0.037(4) 0.036(4) 0.053(5) -0.002(4) 0.006(3) 0.005(3) C29 0.035(4) 0.028(4) 0.056(5) 0.009(3) 0.016(3) 0.006(3) C30 0.052(5) 0.041(5) 0.058(6) 0.006(4) 0.009(4) 0.004(4) C31 0.079(7) 0.050(5) 0.062(7) -0.003(5) -0.002(5) 0.018(5) C32 0.034(4) 0.040(4) 0.065(6) -0.005(4) 0.010(4) 0.010(3) C33 0.056(5) 0.029(4) 0.055(6) -0.006(3) 0.016(4) 0.004(3) C34 0.108(9) 0.045(5) 0.057(7) 0.001(5) 0.020(6) -0.014(6) C61 0.084(8) 0.066(7) 0.074(9) -0.004(6) 0.016(6) 0.019(6) N1 0.034(3) 0.030(3) 0.057(5) 0.001(3) 0.005(3) 0.003(3) N2 0.032(3) 0.036(3) 0.062(5) -0.007(3) 0.011(3) 0.005(3) N21 0.038(3) 0.025(3) 0.055(4) 0.003(3) 0.015(3) 0.002(2) N22 0.039(3) 0.026(3) 0.056(5) 0.005(3) 0.012(3) 0.000(3) O1 0.046(3) 0.034(3) 0.054(4) -0.004(3) 0.007(3) 0.002(2) O2 0.053(3) 0.034(3) 0.053(4) -0.003(3) 0.016(3) 0.002(2) O3 0.060(4) 0.038(3) 0.052(4) 0.002(3) 0.015(3) -0.006(3) O4 0.044(3) 0.037(3) 0.051(4) 0.006(3) 0.009(3) 0.001(2) O21 0.043(3) 0.028(3) 0.057(4) -0.005(2) 0.016(3) 0.001(2) O22 0.049(3) 0.031(3) 0.051(4) 0.006(2) 0.011(3) 0.003(2) O23 0.056(4) 0.034(3) 0.060(4) 0.006(3) 0.010(3) 0.003(3) O24 0.049(3) 0.029(3) 0.054(4) -0.002(2) 0.010(3) -0.002(2) O52 0.057(4) 0.028(3) 0.057(4) 0.002(3) 0.009(3) 0.000(2) O53 0.041(3) 0.047(3) 0.063(4) 0.010(3) 0.001(3) 0.001(3) O54 0.040(3) 0.042(3) 0.075(5) 0.009(3) 0.027(3) 0.009(2) O55 0.057(4) 0.026(3) 0.056(4) 0.007(2) 0.019(3) 0.007(2) O62 0.118(7) 0.076(6) 0.070(6) 0.009(5) 0.012(5) -0.005(5) O71 0.050(4) 0.084(5) 0.062(5) 0.003(4) 0.010(3) 0.014(4) Cu1 0.0372(5) 0.0268(5) 0.0542(7) 0.0026(4) 0.0109(4) 0.0014(4) Cu2 0.0364(5) 0.0266(5) 0.0541(7) 0.0019(4) 0.0123(4) 0.0013(4) S51 0.0357(9) 0.0246(9) 0.0547(13) 0.0014(8) 0.0130(8) 0.0008(7) 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' Cu Cu 0.3201 1.2651 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N1 C1 C2 121.1(7) N1 C1 H1 119.4 C2 C1 H1 119.4 C3 C2 C1 119.2(8) C3 C2 H2 120.4 C1 C2 H2 120.4 C4 C3 C2 120.7(9) C4 C3 H3 119.6 C2 C3 H3 119.6 C3 C4 C5 118.6(8) C3 C4 H4 120.7 C5 C4 H4 120.7 N1 C5 C4 120.7(8) N1 C5 C6 116.2(8) C4 C5 C6 123.1(7) N2 C6 C5 109.9(7) N2 C6 H6A 109.7 C5 C6 H6A 109.7 N2 C6 H6B 109.7 C5 C6 H6B 109.7 H6A C6 H6B 108.2 N2 C7 C8 126.8(7) N2 C7 H7 116.6 C8 C7 H7 116.6 C7 C8 C9 119.0(8) C7 C8 C12 114.0(7) C9 C8 C12 127.1(8) O1 C9 O2 118.2(7) O1 C9 C8 125.6(8) O2 C9 C8 116.2(8) O2 C10 C11 110.4(7) O2 C10 H10A 109.6 C11 C10 H10A 109.6 O2 C10 H10B 109.6 C11 C10 H10B 109.6 H10A C10 H10B 108.1 C10 C11 H11A 109.5 C10 C11 H11B 109.5 H11A C11 H11B 109.5 C10 C11 H11C 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 O3 C12 O4 121.8(9) O3 C12 C8 123.3(9) O4 C12 C8 114.8(7) O4 C13 C14 107.2(8) O4 C13 H13A 110.3 C14 C13 H13A 110.3 O4 C13 H13B 110.3 C14 C13 H13B 110.3 H13A C13 H13B 108.5 C13 C14 H14A 109.5 C13 C14 H14B 109.5 H14A C14 H14B 109.5 C13 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 N21 C21 C22 120.2(8) N21 C21 H21 119.9 C22 C21 H21 119.9 C21 C22 C23 119.6(8) C21 C22 H22 120.2 C23 C22 H22 120.2 C24 C23 C22 119.0(9) C24 C23 H23 120.5 C22 C23 H23 120.5 C25 C24 C23 118.8(8) C25 C24 H24 120.6 C23 C24 H24 120.6 N21 C25 C24 121.4(8) N21 C25 C26 116.4(8) C24 C25 C26 122.1(8) N22 C26 C25 109.6(7) N22 C26 H26A 109.8 C25 C26 H26A 109.8 N22 C26 H26B 109.8 C25 C26 H26B 109.8 H26A C26 H26B 108.2 N22 C27 C28 126.8(8) N22 C27 H27 116.6 C28 C27 H27 116.6 C27 C28 C29 120.1(8) C27 C28 C32 115.8(8) C29 C28 C32 124.1(9) O21 C29 O22 118.2(7) O21 C29 C28 124.0(8) O22 C29 C28 117.8(7) O22 C30 C31 105.2(8) O22 C30 H30A 110.7 C31 C30 H30A 110.7 O22 C30 H30B 110.7 C31 C30 H30B 110.7 H30A C30 H30B 108.8 C30 C31 H31A 109.5 C30 C31 H31B 109.5 H31A C31 H31B 109.5 C30 C31 H31C 109.5 H31A C31 H31C 109.5 H31B C31 H31C 109.5 O23 C32 O24 122.6(8) O23 C32 C28 122.1(9) O24 C32 C28 115.3(8) O24 C33 C34 107.5(8) O24 C33 H33A 110.2 C34 C33 H33A 110.2 O24 C33 H33B 110.2 C34 C33 H33B 110.2 H33A C33 H33B 108.5 C33 C34 H34A 109.5 C33 C34 H34B 109.5 H34A C34 H34B 109.5 C33 C34 H34C 109.5 H34A C34 H34C 109.5 H34B C34 H34C 109.5 O62 C61 H61A 109.5 O62 C61 H61B 109.5 H61A C61 H61B 109.5 O62 C61 H61C 109.5 H61A C61 H61C 109.5 H61B C61 H61C 109.5 C5 N1 C1 119.6(8) C5 N1 Cu1 113.9(6) C1 N1 Cu1 126.4(6) C7 N2 C6 116.6(7) C7 N2 Cu1 127.1(6) C6 N2 Cu1 116.0(6) C25 N21 C21 121.0(8) C25 N21 Cu2 114.6(6) C21 N21 Cu2 124.4(6) C27 N22 C26 117.5(7) C27 N22 Cu2 127.2(7) C26 N22 Cu2 115.2(5) C9 O1 Cu1 130.3(6) C9 O2 C10 117.1(7) C12 O4 C13 115.2(7) C29 O21 Cu2 130.9(6) C29 O22 C30 116.6(7) C32 O24 C33 115.6(7) S51 O52 Cu1 134.3(5) S51 O55 Cu2 129.9(4) C61 O62 H62 109.5 N2 Cu1 O52 169.9(3) N2 Cu1 O1 91.2(3) O52 Cu1 O1 95.8(3) N2 Cu1 N1 83.8(3) O52 Cu1 N1 89.9(3) O1 Cu1 N1 172.3(3) O21 Cu2 N22 90.6(3) O21 Cu2 O55 93.2(3) N22 Cu2 O55 172.8(3) O21 Cu2 N21 172.5(2) N22 Cu2 N21 84.1(3) O55 Cu2 N21 92.7(3) O53 S51 O54 112.8(4) O53 S51 O52 109.8(4) O54 S51 O52 110.5(4) O53 S51 O55 111.0(4) O54 S51 O55 109.5(4) O52 S51 O55 102.9(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N1 1.357(11) C1 C2 1.376(13) C1 H1 0.9500 C2 C3 1.371(12) C2 H2 0.9500 C3 C4 1.363(13) C3 H3 0.9500 C4 C5 1.404(13) C4 H4 0.9500 C5 N1 1.349(10) C5 C6 1.501(12) C6 N2 1.462(11) C6 H6A 0.9900 C6 H6B 0.9900 C7 N2 1.311(12) C7 C8 1.430(12) C7 H7 0.9500 C8 C9 1.437(11) C8 C12 1.469(13) C9 O1 1.246(11) C9 O2 1.321(11) C10 O2 1.470(10) C10 C11 1.489(13) C10 H10A 0.9900 C10 H10B 0.9900 C11 H11A 0.9800 C11 H11B 0.9800 C11 H11C 0.9800 C12 O3 1.211(10) C12 O4 1.348(11) C13 O4 1.448(11) C13 C14 1.515(14) C13 H13A 0.9900 C13 H13B 0.9900 C14 H14A 0.9800 C14 H14B 0.9800 C14 H14C 0.9800 C21 N21 1.359(10) C21 C22 1.373(14) C21 H21 0.9500 C22 C23 1.402(13) C22 H22 0.9500 C23 C24 1.401(13) C23 H23 0.9500 C24 C25 1.372(13) C24 H24 0.9500 C25 N21 1.344(10) C25 C26 1.499(12) C26 N22 1.483(12) C26 H26A 0.9900 C26 H26B 0.9900 C27 N22 1.312(11) C27 C28 1.380(13) C27 H27 0.9500 C28 C29 1.453(11) C28 C32 1.476(12) C29 O21 1.258(10) C29 O22 1.330(11) C30 O22 1.462(10) C30 C31 1.524(15) C30 H30A 0.9900 C30 H30B 0.9900 C31 H31A 0.9800 C31 H31B 0.9800 C31 H31C 0.9800 C32 O23 1.244(11) C32 O24 1.323(12) C33 O24 1.445(10) C33 C34 1.468(15) C33 H33A 0.9900 C33 H33B 0.9900 C34 H34A 0.9800 C34 H34B 0.9800 C34 H34C 0.9800 C61 O62 1.370(16) C61 H61A 0.9800 C61 H61B 0.9800 C61 H61C 0.9800 N1 Cu1 1.993(8) N2 Cu1 1.898(7) N21 Cu2 1.978(8) N22 Cu2 1.907(6) O1 Cu1 1.913(7) O21 Cu2 1.898(7) O52 S51 1.509(6) O52 Cu1 1.905(6) O53 S51 1.430(7) O54 S51 1.434(6) O55 S51 1.517(6) O55 Cu2 1.911(5) O62 H62 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 N1 C1 C2 C3 1.4(12) C1 C2 C3 C4 -0.6(12) C2 C3 C4 C5 -0.5(12) C3 C4 C5 N1 0.8(12) C3 C4 C5 C6 -178.8(7) N1 C5 C6 N2 -0.8(9) C4 C5 C6 N2 178.9(7) N2 C7 C8 C9 -0.8(12) N2 C7 C8 C12 178.9(7) C7 C8 C9 O1 -1.9(12) C12 C8 C9 O1 178.5(7) C7 C8 C9 O2 175.8(7) C12 C8 C9 O2 -3.9(11) C7 C8 C12 O3 -17.2(11) C9 C8 C12 O3 162.4(8) C7 C8 C12 O4 160.7(6) C9 C8 C12 O4 -19.6(11) N21 C21 C22 C23 -0.5(12) C21 C22 C23 C24 0.5(13) C22 C23 C24 C25 -0.3(12) C23 C24 C25 N21 0.3(12) C23 C24 C25 C26 178.0(8) N21 C25 C26 N22 -3.2(10) C24 C25 C26 N22 179.1(7) N22 C27 C28 C29 -0.5(13) N22 C27 C28 C32 177.4(8) C27 C28 C29 O21 5.1(12) C32 C28 C29 O21 -172.7(7) C27 C28 C29 O22 -175.8(7) C32 C28 C29 O22 6.4(12) C27 C28 C32 O23 -7.0(12) C29 C28 C32 O23 170.8(8) C27 C28 C32 O24 172.8(7) C29 C28 C32 O24 -9.3(12) C4 C5 N1 C1 -0.1(11) C6 C5 N1 C1 179.5(7) C4 C5 N1 Cu1 179.0(6) C6 C5 N1 Cu1 -1.4(8) C2 C1 N1 C5 -1.0(11) C2 C1 N1 Cu1 -180.0(6) C8 C7 N2 C6 177.6(7) C8 C7 N2 Cu1 3.0(11) C5 C6 N2 C7 -172.5(6) C5 C6 N2 Cu1 2.7(8) C24 C25 N21 C21 -0.4(11) C26 C25 N21 C21 -178.2(7) C24 C25 N21 Cu2 178.6(6) C26 C25 N21 Cu2 0.8(9) C22 C21 N21 C25 0.5(12) C22 C21 N21 Cu2 -178.4(6) C28 C27 N22 C26 178.0(7) C28 C27 N22 Cu2 -5.4(12) C25 C26 N22 C27 -178.8(7) C25 C26 N22 Cu2 4.2(8) O2 C9 O1 Cu1 -175.4(5) C8 C9 O1 Cu1 2.2(12) O1 C9 O2 C10 -2.9(11) C8 C9 O2 C10 179.3(7) C11 C10 O2 C9 -81.0(10) O3 C12 O4 C13 -2.1(11) C8 C12 O4 C13 179.9(6) C14 C13 O4 C12 170.9(7) O22 C29 O21 Cu2 177.5(5) C28 C29 O21 Cu2 -3.4(12) O21 C29 O22 C30 -2.4(10) C28 C29 O22 C30 178.5(7) C31 C30 O22 C29 -176.0(7) O23 C32 O24 C33 -3.9(11) C28 C32 O24 C33 176.3(7) C34 C33 O24 C32 -178.4(8) C7 N2 Cu1 O52 -136.2(15) C6 N2 Cu1 O52 49.1(18) C7 N2 Cu1 O1 -2.2(7) C6 N2 Cu1 O1 -176.9(5) C7 N2 Cu1 N1 171.9(7) C6 N2 Cu1 N1 -2.8(5) C29 O21 Cu2 N22 -1.2(7) C29 O21 Cu2 O55 172.6(7) Cu1 O52 S51 O53 60.6(6) Cu1 O52 S51 O54 -64.4(6) Cu1 O52 S51 O55 178.8(5) Cu2 O55 S51 O53 -82.2(6) Cu2 O55 S51 O54 42.9(6) Cu2 O55 S51 O52 160.4(5)