Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;New Bimetallic Compounds Based on the Bis(thiosemicarbazonato) Motif ; _publ_contact_author_name 'Prof. Jonathan Dilworth' _publ_contact_author_email JON.DILWORTH@CHEM.OX.AC.UK loop_ _publ_author_name J.R.Dilworth M.Christlieb A.R.Cowley P.Donnelly ; H.S.R.Struthers ; J.M.White # Attachment 'arc1219.cif' data_arc1219 _database_code_depnum_ccdc_archive 'CCDC 603106' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _exptl_crystal_thermal_history ; The material was crystallised at ambient temperature. A suitable crystal was cooled rapidly to 150K for single-crystal X-ray diffraction analysis. ; _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_special_details ; Geometric restraints were applied to the disordered solvent molecules. O-S bond lengths were restrained to 1.50(2) \%A, S-C bond lengths to 1.80(2) \%A, O-C-S angles to 106(2) \% and C-S-C angles to 98(2) \%. Similarity restraints were applied to the displacement parameters of directly-bonded pairs of atoms. The NH hydrogen atoms were located in a difference Fourier map and their coordinates and isotropic displacement parameters subsequently refined. Other hydrogen atoms were positioned geometrically, the preferred orientations of the methyl groups H61-H63 anf H71-H73 having been identified previously in the Fourier map. ; #============================================================= _cell_length_a 9.7705(2) _cell_angle_alpha 110.9320(8) _cell_length_b 13.5108(2) _cell_angle_beta 108.8954(8) _cell_length_c 13.5770(2) _cell_angle_gamma 101.1813(9) _cell_volume 1483.38(5) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B 'Zn ' 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 1 _chemical_formula_sum ' C32 H72 N14 O8 S12 Zn2 ' _chemical_formula_moiety ' C20 H36 N14 O2 S6 Zn2, 6(C2 H6 O S) ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 1296.57 _cell_measurement_reflns_used 27705 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' block ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.18 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_max 0.26 _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 678 _exptl_absorpt_coefficient_mu 1.284 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.79 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 27705 _reflns_number_total 6718 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_theta_min 5.175 _diffrn_reflns_theta_max 27.439 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.439 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -12 _reflns_limit_h_max 11 _reflns_limit_k_min -17 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _refine_diff_density_min -0.41 _refine_diff_density_max 0.38 _refine_ls_number_reflns 4449 _refine_ls_number_restraints 108 _refine_ls_number_parameters 389 #_refine_ls_R_factor_ref 0.0332 _refine_ls_wR_factor_ref 0.0383 _refine_ls_goodness_of_fit_ref 1.1058 #_reflns_number_all 6718 _refine_ls_R_factor_all 0.0608 _refine_ls_wR_factor_all 0.0619 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 4449 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_gt 0.0383 _refine_ls_shift/su_max 0.002109 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.450 0.194 0.227 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_disorder_assembly _atom_site_refinement_disorder_group Zn1 Zn 0.32989(3) 0.55486(3) 0.24941(3) 0.0244 1.0000 Uani . . . . . S1 S 0.51239(8) 0.74167(6) 0.37553(6) 0.0313 1.0000 Uani . . . . . C1 C 0.5813(3) 0.7453(2) 0.2730(2) 0.0270 1.0000 Uani . . . . . N1 N 0.5143(3) 0.68021(19) 0.15896(19) 0.0279 1.0000 Uani . . . . . N2 N 0.3798(2) 0.59626(18) 0.12497(19) 0.0259 1.0000 Uani . . . . . C2 C 0.2947(3) 0.5284(2) 0.0158(2) 0.0250 1.0000 Uani . . . . . C3 C 0.1537(3) 0.4413(2) -0.0080(2) 0.0249 1.0000 Uani . . . . . N3 N 0.1451(3) 0.43897(19) 0.0844(2) 0.0283 1.0000 Uani . . . . . N4 N 0.0180(3) 0.3616(2) 0.0719(2) 0.0296 1.0000 Uani . . . . . C4 C 0.0178(3) 0.3770(2) 0.1733(3) 0.0302 1.0000 Uani . . . . . S2 S 0.15127(8) 0.48401(6) 0.31311(6) 0.0323 1.0000 Uani . . . . . N5 N 0.7202(3) 0.8233(2) 0.3083(2) 0.0329 1.0000 Uani . . . . . N6 N 0.8136(3) 0.89818(19) 0.4226(2) 0.0302 1.0000 Uani . . . . . C5 C 0.9478(3) 0.9594(2) 0.4415(2) 0.0306 1.0000 Uani . . . . . C6 C 0.3296(3) 0.5328(2) -0.0822(2) 0.0321 1.0000 Uani . . . . . C7 C 0.0334(3) 0.3638(2) -0.1301(2) 0.0325 1.0000 Uani . . . . . N7 N -0.1020(3) 0.3039(2) 0.1693(2) 0.0352 1.0000 Uani . . . . . C8 C -0.2208(4) 0.2122(3) 0.0594(3) 0.0419 1.0000 Uani . . . . . O1 O 0.4867(3) 0.4757(2) 0.2869(3) 0.0312 0.808(3) Uani D U P 1 1 S3 S 0.43325(9) 0.35284(7) 0.26543(7) 0.0270 0.808(3) Uani D U P 1 1 C9 C 0.4853(5) 0.3572(5) 0.4064(5) 0.0379 0.808(3) Uani D U P 1 1 C10 C 0.5791(5) 0.3044(3) 0.2367(4) 0.0395 0.808(3) Uani D U P 1 1 O11 O 0.4496(17) 0.4434(12) 0.2447(10) 0.0307 0.192(3) Uani D U P 1 2 S13 S 0.5579(4) 0.4521(3) 0.3597(3) 0.0318 0.192(3) Uani D U P 1 2 C19 C 0.444(2) 0.353(2) 0.389(2) 0.0340 0.192(3) Uani D U P 1 2 C20 C 0.6739(18) 0.3734(14) 0.3176(14) 0.0404 0.192(3) Uani D U P 1 2 O2 O 0.8572(5) 0.8604(3) 0.1687(3) 0.0389 0.781(3) Uani D U P 2 1 S4 S 0.75473(11) 0.83787(8) 0.04769(8) 0.0353 0.781(3) Uani D U P 2 1 C11 C 0.6615(6) 0.9415(5) 0.0695(5) 0.0548 0.781(3) Uani D U P 2 1 C12 C 0.8814(5) 0.8960(4) -0.0014(4) 0.0473 0.781(3) Uani D U P 2 1 O12 O 0.880(2) 0.8987(12) 0.1792(13) 0.0415 0.219(3) Uani D U P 2 2 S14 S 0.8285(4) 0.9286(3) 0.0800(3) 0.0375 0.219(3) Uani D U P 2 2 C21 C 0.6279(18) 0.9082(17) 0.0401(18) 0.0449 0.219(3) Uani D U P 2 2 C22 C 0.809(2) 0.8143(14) -0.0463(12) 0.0547 0.219(3) Uani D U P 2 2 O3 O -0.1475(3) 0.2324(3) 0.3360(3) 0.0603 1.0000 Uani . . . . . S5 S -0.02092(10) 0.22120(9) 0.42539(9) 0.0544 1.0000 Uani . . . . . C13 C 0.1036(5) 0.3621(4) 0.5332(4) 0.0681 1.0000 Uani . . . . . C14 C 0.1066(4) 0.1864(4) 0.3622(3) 0.0540 1.0000 Uani . . . . . O4 O 0.3562(3) 0.0730(2) 0.2164(2) 0.0630 1.0000 Uani . . . . . S6 S 0.40182(11) -0.01517(7) 0.24758(7) 0.0466 1.0000 Uani . . . . . C15 C 0.2764(4) -0.0585(4) 0.3069(4) 0.0602 1.0000 Uani . . . . . C16 C 0.5726(4) 0.0577(3) 0.3795(3) 0.0461 1.0000 Uani . . . . . H1 H 0.754(4) 0.820(3) 0.260(3) 0.042(10) 1.0000 Uiso . . . . . H2 H -0.101(4) 0.307(3) 0.230(3) 0.043(10) 1.0000 Uiso . . . . . H51 H 0.9775 0.9500 0.3757 0.0355 1.0000 Uiso . . . . . H61 H 0.4285 0.5965 -0.0499 0.0387 1.0000 Uiso . . . . . H62 H 0.2438 0.5452 -0.1354 0.0387 1.0000 Uiso . . . . . H63 H 0.3397 0.4598 -0.1268 0.0387 1.0000 Uiso . . . . . H71 H -0.0522 0.3115 -0.1281 0.0341 1.0000 Uiso . . . . . H72 H -0.0087 0.4096 -0.1677 0.0341 1.0000 Uiso . . . . . H73 H 0.0807 0.3187 -0.1761 0.0341 1.0000 Uiso . . . . . H81 H -0.2990 0.1677 0.0746 0.0454 1.0000 Uiso . . . . . H82 H -0.2725 0.2442 0.0080 0.0454 1.0000 Uiso . . . . . H83 H -0.1727 0.1617 0.0200 0.0454 1.0000 Uiso . . . . . H91 H 0.4527 0.2784 0.3973 0.0442 0.8082 Uiso . . . 1 1 H92 H 0.5997 0.3943 0.4531 0.0442 0.8082 Uiso . . . 1 1 H93 H 0.4325 0.4013 0.4475 0.0442 0.8082 Uiso . . . 1 1 H101 H 0.5544 0.2234 0.2212 0.0515 0.8082 Uiso . . . 1 1 H102 H 0.6811 0.3512 0.3058 0.0515 0.8082 Uiso . . . 1 1 H103 H 0.5838 0.3112 0.1668 0.0515 0.8082 Uiso . . . 1 1 H191 H 0.5095 0.3546 0.4638 0.0391 0.1918 Uiso . . . 1 2 H192 H 0.3539 0.3742 0.3950 0.0391 0.1918 Uiso . . . 1 2 H193 H 0.4067 0.2749 0.3237 0.0391 0.1918 Uiso . . . 1 2 H201 H 0.7502 0.3739 0.3879 0.0459 0.1918 Uiso . . . 1 2 H202 H 0.7302 0.4086 0.2819 0.0459 0.1918 Uiso . . . 1 2 H203 H 0.6062 0.2936 0.2594 0.0459 0.1918 Uiso . . . 1 2 H111 H 0.5905 0.9319 -0.0080 0.0551 0.7811 Uiso . . . 2 1 H112 H 0.7415 1.0192 0.1144 0.0551 0.7811 Uiso . . . 2 1 H113 H 0.6009 0.9309 0.1141 0.0551 0.7811 Uiso . . . 2 1 H121 H 0.8210 0.8842 -0.0823 0.0543 0.7811 Uiso . . . 2 1 H122 H 0.9353 0.9789 0.0519 0.0543 0.7811 Uiso . . . 2 1 H123 H 0.9594 0.8579 -0.0014 0.0543 0.7811 Uiso . . . 2 1 H211 H 0.5869 0.9269 -0.0260 0.0495 0.2189 Uiso . . . 2 2 H212 H 0.6152 0.9587 0.1086 0.0495 0.2189 Uiso . . . 2 2 H213 H 0.5697 0.8275 0.0156 0.0495 0.2189 Uiso . . . 2 2 H221 H 0.7746 0.8314 -0.1144 0.0594 0.2189 Uiso . . . 2 2 H222 H 0.9101 0.8032 -0.0330 0.0594 0.2189 Uiso . . . 2 2 H223 H 0.7298 0.7438 -0.0629 0.0594 0.2189 Uiso . . . 2 2 H131 H 0.1902 0.3591 0.5950 0.0865 1.0000 Uiso . . . . . H132 H 0.0435 0.4025 0.5692 0.0865 1.0000 Uiso . . . . . H133 H 0.1465 0.4034 0.4956 0.0865 1.0000 Uiso . . . . . H141 H 0.1938 0.1778 0.4182 0.0668 1.0000 Uiso . . . . . H142 H 0.1484 0.2481 0.3441 0.0668 1.0000 Uiso . . . . . H143 H 0.0495 0.1137 0.2885 0.0668 1.0000 Uiso . . . . . H151 H 0.3021 -0.1178 0.3294 0.0713 1.0000 Uiso . . . . . H152 H 0.2902 0.0082 0.3775 0.0713 1.0000 Uiso . . . . . H153 H 0.1668 -0.0901 0.2471 0.0713 1.0000 Uiso . . . . . H161 H 0.6076 0.0019 0.4040 0.0526 1.0000 Uiso . . . . . H162 H 0.6551 0.1019 0.3676 0.0526 1.0000 Uiso . . . . . H163 H 0.5517 0.1104 0.4417 0.0526 1.0000 Uiso . . . . . 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 Zn1 0.02281(15) 0.02511(16) 0.02385(15) 0.01309(12) 0.00704(12) 0.00657(11) S1 0.0319(4) 0.0288(3) 0.0254(3) 0.0103(3) 0.0100(3) 0.0028(3) C1 0.0251(13) 0.0241(13) 0.0308(13) 0.0145(11) 0.0096(11) 0.0069(10) N1 0.0250(11) 0.0268(11) 0.0269(11) 0.0127(9) 0.0083(9) 0.0028(9) N2 0.0249(11) 0.0250(11) 0.0257(11) 0.0132(9) 0.0076(9) 0.0067(9) C2 0.0272(13) 0.0259(13) 0.0260(12) 0.0146(11) 0.0103(10) 0.0141(11) C3 0.0267(13) 0.0240(13) 0.0244(12) 0.0117(11) 0.0088(10) 0.0118(10) N3 0.0249(11) 0.0281(12) 0.0291(11) 0.0126(10) 0.0096(9) 0.0075(9) N4 0.0253(11) 0.0292(12) 0.0293(12) 0.0134(10) 0.0092(9) 0.0040(9) C4 0.0252(13) 0.0318(15) 0.0365(15) 0.0200(12) 0.0116(11) 0.0101(11) S2 0.0266(3) 0.0405(4) 0.0267(3) 0.0167(3) 0.0096(3) 0.0056(3) N5 0.0311(12) 0.0324(13) 0.0285(12) 0.0139(11) 0.0101(10) 0.0024(10) N6 0.0276(12) 0.0283(12) 0.0296(12) 0.0147(10) 0.0070(10) 0.0058(9) C5 0.0313(14) 0.0257(13) 0.0317(14) 0.0150(12) 0.0096(12) 0.0070(11) C6 0.0357(15) 0.0342(15) 0.0269(13) 0.0145(12) 0.0138(12) 0.0112(12) C7 0.0325(14) 0.0296(14) 0.0231(13) 0.0082(11) 0.0043(11) 0.0064(11) N7 0.0273(12) 0.0400(14) 0.0366(14) 0.0202(12) 0.0120(11) 0.0057(10) C8 0.0285(15) 0.0366(17) 0.0484(18) 0.0146(15) 0.0128(14) 0.0025(13) O1 0.0265(15) 0.0272(13) 0.0406(16) 0.0203(13) 0.0102(12) 0.0087(11) S3 0.0264(4) 0.0253(4) 0.0283(4) 0.0142(3) 0.0092(3) 0.0079(3) C9 0.043(3) 0.039(2) 0.0288(19) 0.0181(18) 0.0111(19) 0.010(2) C10 0.0407(18) 0.0381(18) 0.050(2) 0.0240(16) 0.0228(16) 0.0203(15) O11 0.036(4) 0.035(4) 0.021(3) 0.013(3) 0.010(3) 0.013(4) S13 0.0341(19) 0.035(2) 0.0268(18) 0.0158(15) 0.0090(15) 0.0163(15) C19 0.033(5) 0.036(5) 0.029(5) 0.018(4) 0.004(4) 0.013(4) C20 0.039(4) 0.038(4) 0.038(4) 0.013(4) 0.009(4) 0.021(3) O2 0.0405(19) 0.046(2) 0.0318(13) 0.0203(16) 0.0148(12) 0.0128(17) S4 0.0345(5) 0.0368(6) 0.0315(5) 0.0151(4) 0.0115(4) 0.0114(4) C11 0.040(2) 0.046(3) 0.051(3) 0.006(2) 0.006(2) 0.0176(19) C12 0.043(2) 0.057(2) 0.0353(19) 0.0229(18) 0.0138(16) 0.0068(18) O12 0.042(4) 0.041(5) 0.038(4) 0.022(3) 0.011(3) 0.007(4) S14 0.0391(19) 0.040(2) 0.0376(18) 0.0226(16) 0.0174(15) 0.0117(16) C21 0.038(3) 0.041(5) 0.045(5) 0.017(4) 0.007(4) 0.014(4) C22 0.058(5) 0.049(5) 0.042(4) 0.013(3) 0.012(4) 0.018(4) O3 0.0347(12) 0.094(2) 0.0789(19) 0.0672(18) 0.0230(12) 0.0251(13) S5 0.0408(4) 0.0812(7) 0.0684(6) 0.0594(6) 0.0245(4) 0.0248(4) C13 0.070(3) 0.086(3) 0.060(2) 0.039(2) 0.028(2) 0.039(2) C14 0.047(2) 0.066(2) 0.054(2) 0.035(2) 0.0166(17) 0.0234(18) O4 0.0666(17) 0.0564(16) 0.0593(16) 0.0402(14) 0.0075(13) 0.0144(13) S6 0.0564(5) 0.0386(4) 0.0333(4) 0.0137(3) 0.0105(4) 0.0140(4) C15 0.0410(19) 0.058(2) 0.080(3) 0.045(2) 0.0115(19) 0.0103(17) C16 0.0364(17) 0.051(2) 0.0441(18) 0.0190(16) 0.0123(14) 0.0151(15) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . O1 . 2.066(3) yes Zn1 . S2 . 2.3729(7) yes Zn1 . N3 . 2.123(2) yes Zn1 . N2 . 2.123(2) yes Zn1 . S1 . 2.3814(7) yes Zn1 . O11 . 2.075(15) yes Zn1 . S2 . 2.3729(7) yes Zn1 . N3 . 2.123(2) yes Zn1 . N2 . 2.123(2) yes Zn1 . S1 . 2.3814(7) yes S1 . C1 . 1.742(3) yes C1 . N5 . 1.359(4) yes C1 . N1 . 1.322(3) yes N1 . N2 . 1.372(3) yes N2 . C2 . 1.290(3) yes C2 . C6 . 1.493(4) yes C2 . C3 . 1.482(4) yes C3 . C7 . 1.499(4) yes C3 . N3 . 1.295(3) yes N3 . N4 . 1.377(3) yes N4 . C4 . 1.317(4) yes C4 . N7 . 1.349(4) yes C4 . S2 . 1.760(3) yes N5 . H1 . 0.82(4) no N5 . N6 . 1.366(3) yes N6 . C5 . 1.296(4) yes C5 . H51 . 1.000 no C5 . C5 2_776 1.428(5) yes C6 . H63 . 1.000 no C6 . H62 . 1.000 no C6 . H61 . 1.000 no C7 . H73 . 1.000 no C7 . H72 . 1.000 no C7 . H71 . 1.000 no N7 . H2 . 0.81(4) no N7 . C8 . 1.451(4) yes C8 . H83 . 1.000 no C8 . H82 . 1.000 no C8 . H81 . 1.000 no O1 . S3 . 1.527(3) yes S3 . C10 . 1.775(4) yes S3 . C9 . 1.790(5) yes C9 . H93 . 1.000 no C9 . H92 . 1.000 no C9 . H91 . 1.000 no C10 . H103 . 1.000 no C10 . H102 . 1.000 no C10 . H101 . 1.000 no O11 . S13 . 1.524(11) yes S13 . C20 . 1.788(13) yes S13 . C19 . 1.809(17) yes C19 . H193 . 1.000 no C19 . H192 . 1.000 no C19 . H191 . 1.000 no C20 . H203 . 1.000 no C20 . H202 . 1.000 no C20 . H201 . 1.000 no O2 . S4 . 1.501(4) yes S4 . C12 . 1.767(4) yes S4 . C11 . 1.803(6) yes C11 . H113 . 1.000 no C11 . H112 . 1.000 no C11 . H111 . 1.000 no C12 . H123 . 1.000 no C12 . H122 . 1.000 no C12 . H121 . 1.000 no O12 . S14 . 1.503(13) yes S14 . C22 . 1.772(13) yes S14 . C21 . 1.791(15) yes C21 . H213 . 1.000 no C21 . H212 . 1.000 no C21 . H211 . 1.000 no C22 . H223 . 1.000 no C22 . H222 . 1.000 no C22 . H221 . 1.000 no O3 . S5 . 1.503(2) yes S5 . C14 . 1.772(4) yes S5 . C13 . 1.790(5) yes C13 . H133 . 1.000 no C13 . H132 . 1.000 no C13 . H131 . 1.000 no C14 . H143 . 1.000 no C14 . H142 . 1.000 no C14 . H141 . 1.000 no O4 . S6 . 1.497(3) yes S6 . C16 . 1.769(3) yes S6 . C15 . 1.786(4) yes C15 . H153 . 1.000 no C15 . H152 . 1.000 no C15 . H151 . 1.000 no C16 . H163 . 1.000 no C16 . H162 . 1.000 no C16 . H161 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Zn1 . S2 . 100.85(9) yes O1 . Zn1 . N3 . 107.28(10) yes S2 . Zn1 . N3 . 80.82(6) yes O1 . Zn1 . N2 . 100.07(11) yes S2 . Zn1 . N2 . 151.07(6) yes N3 . Zn1 . N2 . 74.01(8) yes O1 . Zn1 . S1 . 94.95(8) yes S2 . Zn1 . S1 . 117.26(3) yes N3 . Zn1 . S1 . 148.46(6) yes N2 . Zn1 . S1 . 80.40(6) yes O11 . Zn1 . S2 . 100.1(4) yes O11 . Zn1 . N3 . 92.8(3) yes S2 . Zn1 . N3 . 80.82(6) yes O11 . Zn1 . N2 . 95.2(4) yes S2 . Zn1 . N2 . 151.07(6) yes N3 . Zn1 . N2 . 74.01(8) yes O11 . Zn1 . S1 . 107.8(4) yes S2 . Zn1 . S1 . 117.26(3) yes N3 . Zn1 . S1 . 148.46(6) yes N2 . Zn1 . S1 . 80.40(6) yes C1 . S1 . Zn1 . 93.44(9) yes N5 . C1 . N1 . 112.1(2) yes N5 . C1 . S1 . 119.6(2) yes N1 . C1 . S1 . 128.3(2) yes N2 . N1 . C1 . 111.8(2) yes C2 . N2 . N1 . 120.3(2) yes C2 . N2 . Zn1 . 117.99(18) yes N1 . N2 . Zn1 . 120.64(16) yes C6 . C2 . C3 . 120.6(2) yes C6 . C2 . N2 . 125.0(2) yes C3 . C2 . N2 . 114.4(2) yes C7 . C3 . N3 . 124.1(2) yes C7 . C3 . C2 . 121.4(2) yes N3 . C3 . C2 . 114.5(2) yes N4 . N3 . C3 . 119.1(2) yes N4 . N3 . Zn1 . 122.79(17) yes C3 . N3 . Zn1 . 118.14(18) yes C4 . N4 . N3 . 112.1(2) yes N7 . C4 . S2 . 116.0(2) yes N7 . C4 . N4 . 116.1(3) yes S2 . C4 . N4 . 127.9(2) yes Zn1 . S2 . C4 . 95.19(9) yes H1 . N5 . N6 . 118(3) no H1 . N5 . C1 . 118(3) no N6 . N5 . C1 . 123.1(2) yes C5 . N6 . N5 . 114.8(2) yes H51 . C5 . N6 . 120.751 no H51 . C5 . C5 2_776 120.751 no N6 . C5 . C5 2_776 118.5(3) yes H63 . C6 . H62 . 109.476 no H63 . C6 . H61 . 109.476 no H62 . C6 . H61 . 109.476 no H63 . C6 . C2 . 109.467 no H62 . C6 . C2 . 109.467 no H61 . C6 . C2 . 109.467 no H73 . C7 . H72 . 109.476 no H73 . C7 . H71 . 109.476 no H72 . C7 . H71 . 109.476 no H73 . C7 . C3 . 109.467 no H72 . C7 . C3 . 109.467 no H71 . C7 . C3 . 109.467 no H2 . N7 . C8 . 120(3) no H2 . N7 . C4 . 118(3) no C8 . N7 . C4 . 121.5(3) yes H83 . C8 . H82 . 109.476 no H83 . C8 . H81 . 109.476 no H82 . C8 . H81 . 109.476 no H83 . C8 . N7 . 109.467 no H82 . C8 . N7 . 109.467 no H81 . C8 . N7 . 109.467 no S3 . O1 . Zn1 . 121.18(17) yes C10 . S3 . C9 . 96.8(2) yes C10 . S3 . O1 . 103.19(19) yes C9 . S3 . O1 . 106.2(2) yes H93 . C9 . H92 . 109.476 no H93 . C9 . H91 . 109.476 no H92 . C9 . H91 . 109.476 no H93 . C9 . S3 . 109.467 no H92 . C9 . S3 . 109.467 no H91 . C9 . S3 . 109.467 no H103 . C10 . H102 . 109.476 no H103 . C10 . H101 . 109.476 no H102 . C10 . H101 . 109.476 no H103 . C10 . S3 . 109.467 no H102 . C10 . S3 . 109.467 no H101 . C10 . S3 . 109.467 no S13 . O11 . Zn1 . 118.7(8) yes C20 . S13 . C19 . 98.3(11) yes C20 . S13 . O11 . 103.0(8) yes C19 . S13 . O11 . 105.6(8) yes H193 . C19 . H192 . 109.476 no H193 . C19 . H191 . 109.475 no H192 . C19 . H191 . 109.476 no H193 . C19 . S13 . 109.466 no H192 . C19 . S13 . 109.467 no H191 . C19 . S13 . 109.467 no H203 . C20 . H202 . 109.476 no H203 . C20 . H201 . 109.476 no H202 . C20 . H201 . 109.476 no H203 . C20 . S13 . 109.467 no H202 . C20 . S13 . 109.467 no H201 . C20 . S13 . 109.467 no C12 . S4 . C11 . 98.8(3) yes C12 . S4 . O2 . 104.7(2) yes C11 . S4 . O2 . 104.6(3) yes H113 . C11 . H112 . 109.476 no H113 . C11 . H111 . 109.476 no H112 . C11 . H111 . 109.475 no H113 . C11 . S4 . 109.467 no H112 . C11 . S4 . 109.466 no H111 . C11 . S4 . 109.467 no H123 . C12 . H122 . 109.476 no H123 . C12 . H121 . 109.476 no H122 . C12 . H121 . 109.476 no H123 . C12 . S4 . 109.467 no H122 . C12 . S4 . 109.467 no H121 . C12 . S4 . 109.467 no C22 . S14 . C21 . 98.2(8) yes C22 . S14 . O12 . 107.3(9) yes C21 . S14 . O12 . 105.6(10) yes H213 . C21 . H212 . 109.475 no H213 . C21 . H211 . 109.476 no H212 . C21 . H211 . 109.476 no H213 . C21 . S14 . 109.466 no H212 . C21 . S14 . 109.467 no H211 . C21 . S14 . 109.467 no H223 . C22 . H222 . 109.477 no H223 . C22 . H221 . 109.478 no H222 . C22 . H221 . 109.473 no H223 . C22 . S14 . 109.468 no H222 . C22 . S14 . 109.465 no H221 . C22 . S14 . 109.466 no C14 . S5 . C13 . 97.4(2) yes C14 . S5 . O3 . 105.92(17) yes C13 . S5 . O3 . 106.42(19) yes H133 . C13 . H132 . 109.476 no H133 . C13 . H131 . 109.476 no H132 . C13 . H131 . 109.476 no H133 . C13 . S5 . 109.467 no H132 . C13 . S5 . 109.467 no H131 . C13 . S5 . 109.467 no H143 . C14 . H142 . 109.476 no H143 . C14 . H141 . 109.476 no H142 . C14 . H141 . 109.476 no H143 . C14 . S5 . 109.467 no H142 . C14 . S5 . 109.467 no H141 . C14 . S5 . 109.467 no C16 . S6 . C15 . 97.03(18) yes C16 . S6 . O4 . 106.60(16) yes C15 . S6 . O4 . 106.16(18) yes H153 . C15 . H152 . 109.476 no H153 . C15 . H151 . 109.476 no H152 . C15 . H151 . 109.476 no H153 . C15 . S6 . 109.467 no H152 . C15 . S6 . 109.467 no H151 . C15 . S6 . 109.467 no H163 . C16 . H162 . 109.476 no H163 . C16 . H161 . 109.476 no H162 . C16 . H161 . 109.476 no H163 . C16 . S6 . 109.467 no H162 . C16 . S6 . 109.467 no H161 . C16 . S6 . 109.467 no 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_publ_flag N5 H1 O2 0.82(4) 1.98(4) 2.775(5) 163(4) yes N5 H1 O12 0.82(4) 2.25(4) 2.994(18) 153(3) yes N7 H2 O3 0.81(4) 2.13(4) 2.880(4) 153(4) yes _chemical_name_common ; bis((diacetyl-2-(4-N-methyl-3-thiosemicarbazonato)-3-(4'-N- methinimino-3'-thiosemicarbazonato) zinc (ii))) ; # Attachment 'jmwpd4.cif' data_jmwpd4 _database_code_depnum_ccdc_archive 'CCDC 620020' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H82 Cu4 N26 O6 S6' _chemical_formula_weight 1517.88 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.2293(10) _cell_length_b 16.2421(12) _cell_length_c 14.9540(11) _cell_angle_alpha 90.00 _cell_angle_beta 110.6700(10) _cell_angle_gamma 90.00 _cell_volume 3233.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 4734 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 26.61 _exptl_crystal_description slab _exptl_crystal_colour black _exptl_crystal_size_min 0.07 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 1.557 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16715 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5692 _reflns_number_gt 4415 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5692 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0713 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.928 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1496(2) 0.92054(16) 0.0380(2) 0.0280(8) Uani 1 1 d . . . H1A H 0.1456 0.9564 -0.0143 0.042 Uiso 1 1 calc R . . H1B H 0.2122 0.9293 0.0894 0.042 Uiso 1 1 calc R . . H1C H 0.0949 0.9320 0.0596 0.042 Uiso 1 1 calc R . . C3 C 0.1401(2) 0.77337(16) 0.0638(2) 0.0186(7) Uani 1 1 d . . . C6 C 0.1461(2) 0.72804(16) 0.29010(19) 0.0182(7) Uani 1 1 d . . . C7 C 0.1357(2) 0.64929(17) 0.33274(19) 0.0178(7) Uani 1 1 d . . . C10 C 0.0917(2) 0.45190(17) 0.24064(19) 0.0193(7) Uani 1 1 d . . . C13 C 0.0954(2) 0.24036(17) 0.22607(19) 0.0183(7) Uani 1 1 d . . . C14 C 0.0987(2) 0.18458(16) 0.15072(19) 0.0165(7) Uani 1 1 d . . . C17 C 0.0927(2) 0.22716(16) -0.0774(2) 0.0176(7) Uani 1 1 d . . . C19 C 0.0791(2) 0.10415(17) -0.1752(2) 0.0302(8) Uani 1 1 d . . . H19A H 0.0734 0.0921 -0.2398 0.045 Uiso 1 1 calc R . . H19B H 0.0198 0.0856 -0.1647 0.045 Uiso 1 1 calc R . . H19C H 0.1368 0.0764 -0.1318 0.045 Uiso 1 1 calc R . . C20 C 0.1585(2) 0.80732(16) 0.3440(2) 0.0236(7) Uani 1 1 d . . . H20A H 0.1722 0.8509 0.3070 0.035 Uiso 1 1 calc R . . H20B H 0.2133 0.8024 0.4038 0.035 Uiso 1 1 calc R . . H20C H 0.0979 0.8195 0.3558 0.035 Uiso 1 1 calc R . . C21 C 0.1521(2) 0.63925(17) 0.43611(19) 0.0246(7) Uani 1 1 d . . . H21A H 0.1692 0.5830 0.4545 0.037 Uiso 1 1 calc R . . H21B H 0.0918 0.6537 0.4474 0.037 Uiso 1 1 calc R . . H21C H 0.2059 0.6746 0.4731 0.037 Uiso 1 1 calc R . . C22 C 0.1059(2) 0.21075(17) 0.32316(19) 0.0230(7) Uani 1 1 d . . . H22A H 0.0766 0.1570 0.3186 0.034 Uiso 1 1 calc R . . H22B H 0.0720 0.2481 0.3514 0.034 Uiso 1 1 calc R . . H22C H 0.1758 0.2081 0.3622 0.034 Uiso 1 1 calc R . . C23 C 0.1082(2) 0.09327(16) 0.1641(2) 0.0252(8) Uani 1 1 d . . . H23A H 0.1062 0.0678 0.1056 0.038 Uiso 1 1 calc R . . H23B H 0.0537 0.0730 0.1816 0.038 Uiso 1 1 calc R . . H23C H 0.1708 0.0805 0.2138 0.038 Uiso 1 1 calc R . . C24 C 0.3873(3) 0.5978(2) 0.9472(3) 0.0622(12) Uani 1 1 d . . . H24A H 0.4090 0.5740 0.8991 0.093 Uiso 1 1 calc R . . H24B H 0.4445 0.6077 1.0040 0.093 Uiso 1 1 calc R . . H24C H 0.3535 0.6489 0.9243 0.093 Uiso 1 1 calc R . . C25 C 0.2211(3) 0.5284(2) 0.8968(2) 0.0496(11) Uani 1 1 d . . . H25A H 0.2283 0.5012 0.8427 0.074 Uiso 1 1 calc R . . H25B H 0.1882 0.5804 0.8772 0.074 Uiso 1 1 calc R . . H25C H 0.1816 0.4947 0.9229 0.074 Uiso 1 1 calc R . . C26 C 0.3470(3) 0.50454(19) 1.0531(3) 0.0387(9) Uani 1 1 d . . . H26 H 0.2997 0.4711 1.0651 0.046 Uiso 1 1 calc R . . C27 C 0.8374(3) 0.2681(2) 0.2580(3) 0.0536(11) Uani 1 1 d . . . H27A H 0.8318 0.2614 0.1925 0.080 Uiso 1 1 calc R . . H27B H 0.8931 0.3036 0.2900 0.080 Uiso 1 1 calc R . . H27C H 0.7767 0.2920 0.2605 0.080 Uiso 1 1 calc R . . C28 C 0.8585(3) 0.1845(2) 0.4026(2) 0.0494(10) Uani 1 1 d . . . H28A H 0.8705 0.1287 0.4250 0.074 Uiso 1 1 calc R . . H28B H 0.7961 0.2033 0.4065 0.074 Uiso 1 1 calc R . . H28C H 0.9122 0.2190 0.4415 0.074 Uiso 1 1 calc R . . C29 C 0.8678(2) 0.1218(2) 0.2594(2) 0.0320(8) Uani 1 1 d . . . H29 H 0.8800 0.0725 0.2933 0.038 Uiso 1 1 calc R . . C30 C 0.6237(3) 0.0093(2) 0.1213(2) 0.0466(10) Uani 1 1 d . . . H30A H 0.5794 -0.0183 0.0656 0.070 Uiso 1 1 calc R . . H30B H 0.6085 -0.0074 0.1762 0.070 Uiso 1 1 calc R . . H30C H 0.6920 -0.0049 0.1304 0.070 Uiso 1 1 calc R . . C31 C 0.6185(3) 0.1343(2) 0.0231(2) 0.0452(10) Uani 1 1 d . . . H31A H 0.5856 0.0995 -0.0308 0.068 Uiso 1 1 calc R . . H31B H 0.6881 0.1400 0.0307 0.068 Uiso 1 1 calc R . . H31C H 0.5872 0.1875 0.0127 0.068 Uiso 1 1 calc R . . C32 C 0.5976(2) 0.1448(2) 0.1758(2) 0.0286(8) Uani 1 1 d . . . H24 H 0.5951 0.1185 0.2301 0.034 Uiso 1 1 calc R . . N2 N 0.14363(19) 0.83521(15) 0.00627(18) 0.0215(6) Uani 1 1 d . . . N4 N 0.14724(18) 0.79169(13) 0.15156(16) 0.0188(6) Uani 1 1 d . . . N5 N 0.14137(17) 0.72277(13) 0.20218(16) 0.0179(6) Uani 1 1 d . . . N8 N 0.11300(17) 0.58689(13) 0.27317(15) 0.0178(6) Uani 1 1 d . . . N9 N 0.10098(18) 0.51080(13) 0.30551(15) 0.0194(6) Uani 1 1 d . . . N11 N 0.08559(18) 0.37522(13) 0.26916(16) 0.0201(6) Uani 1 1 d . . . N12 N 0.08560(17) 0.31853(13) 0.20268(15) 0.0180(6) Uani 1 1 d . . . N15 N 0.09404(17) 0.22166(13) 0.07179(16) 0.0175(6) Uani 1 1 d . . . N16 N 0.09447(18) 0.17789(13) -0.00651(16) 0.0195(6) Uani 1 1 d . . . N18 N 0.09039(19) 0.19284(15) -0.15905(18) 0.0222(6) Uani 1 1 d . . . N19 N 0.3193(2) 0.54180(15) 0.96880(19) 0.0309(7) Uani 1 1 d . . . N20 N 0.85357(19) 0.18828(16) 0.30482(19) 0.0313(7) Uani 1 1 d . . . N21 N 0.61051(19) 0.09793(16) 0.10852(17) 0.0292(7) Uani 1 1 d . . . O1 O 0.4295(2) 0.51035(14) 1.11644(18) 0.0552(8) Uani 1 1 d . . . O2 O 0.86641(18) 0.11933(14) 0.17751(15) 0.0417(6) Uani 1 1 d . . . O3 O 0.58881(16) 0.22035(13) 0.17250(15) 0.0337(6) Uani 1 1 d . . . S1 S 0.09045(6) 0.47525(4) 0.12144(5) 0.02086(19) Uani 1 1 d . . . S2 S 0.09770(6) 0.33646(4) -0.07221(5) 0.01888(18) Uani 1 1 d . . . S3 S 0.12707(6) 0.67247(4) 0.01399(5) 0.01822(17) Uani 1 1 d . . . Cu1 Cu 0.10490(3) 0.61420(2) 0.14371(2) 0.01808(10) Uani 1 1 d . . . Cu2 Cu 0.07433(3) 0.34116(2) 0.07124(2) 0.01816(10) Uani 1 1 d . . . H2 H 0.137(2) 0.8265(17) -0.050(2) 0.022(9) Uiso 1 1 d . . . H18 H 0.086(2) 0.2237(16) -0.2048(19) 0.020(9) Uiso 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 0.040(2) 0.0147(16) 0.0298(18) 0.0004(14) 0.0125(17) -0.0034(15) C3 0.0157(18) 0.0165(15) 0.0220(16) -0.0019(13) 0.0047(14) -0.0008(13) C6 0.0163(18) 0.0186(16) 0.0166(15) -0.0037(12) 0.0021(13) 0.0006(13) C7 0.0152(17) 0.0188(16) 0.0180(15) -0.0034(13) 0.0043(13) 0.0001(13) C10 0.0171(18) 0.0226(17) 0.0163(15) 0.0011(13) 0.0035(14) 0.0026(13) C13 0.0161(18) 0.0197(16) 0.0170(15) 0.0026(13) 0.0031(13) -0.0014(13) C14 0.0138(17) 0.0148(15) 0.0180(15) 0.0010(12) 0.0018(13) -0.0013(12) C17 0.0147(17) 0.0157(15) 0.0212(16) -0.0009(13) 0.0050(14) -0.0001(12) C19 0.046(2) 0.0192(17) 0.0271(17) -0.0038(14) 0.0143(17) 0.0031(15) C20 0.030(2) 0.0178(16) 0.0210(16) -0.0056(13) 0.0064(15) -0.0023(14) C21 0.029(2) 0.0233(17) 0.0209(16) -0.0044(13) 0.0082(15) -0.0031(14) C22 0.0254(19) 0.0210(16) 0.0210(16) 0.0013(13) 0.0064(15) -0.0022(14) C23 0.034(2) 0.0183(16) 0.0242(17) 0.0020(13) 0.0114(16) 0.0006(14) C24 0.067(3) 0.065(3) 0.064(3) 0.015(2) 0.034(3) -0.009(2) C25 0.062(3) 0.031(2) 0.048(2) -0.0077(18) 0.011(2) 0.0026(19) C26 0.057(3) 0.0230(19) 0.042(2) -0.0014(17) 0.024(2) 0.0055(18) C27 0.045(3) 0.035(2) 0.075(3) 0.004(2) 0.015(2) 0.0058(19) C28 0.051(3) 0.061(3) 0.045(2) -0.020(2) 0.029(2) -0.013(2) C29 0.026(2) 0.035(2) 0.035(2) 0.0038(17) 0.0098(17) -0.0013(16) C30 0.051(3) 0.038(2) 0.044(2) -0.0131(18) 0.007(2) 0.0135(19) C31 0.043(3) 0.066(3) 0.032(2) -0.0072(18) 0.0203(19) -0.003(2) C32 0.020(2) 0.043(2) 0.0232(17) -0.0027(16) 0.0073(15) 0.0000(16) N2 0.0289(17) 0.0183(14) 0.0181(14) -0.0009(12) 0.0093(13) -0.0036(11) N4 0.0223(15) 0.0151(13) 0.0195(13) -0.0013(11) 0.0080(12) -0.0016(11) N5 0.0183(15) 0.0145(13) 0.0201(13) -0.0006(11) 0.0057(12) -0.0009(11) N8 0.0196(15) 0.0174(13) 0.0160(12) 0.0006(10) 0.0056(11) 0.0024(11) N9 0.0263(16) 0.0138(13) 0.0166(12) -0.0002(10) 0.0057(12) -0.0014(11) N11 0.0276(16) 0.0154(13) 0.0169(13) -0.0018(11) 0.0073(12) -0.0003(11) N12 0.0212(15) 0.0155(13) 0.0157(12) -0.0014(10) 0.0045(11) -0.0015(11) N15 0.0169(15) 0.0140(12) 0.0199(13) -0.0010(10) 0.0046(11) 0.0007(10) N16 0.0224(15) 0.0169(13) 0.0199(13) -0.0030(11) 0.0084(12) 0.0021(11) N18 0.0311(18) 0.0171(14) 0.0199(14) 0.0023(12) 0.0108(13) 0.0028(12) N19 0.0411(19) 0.0214(15) 0.0318(16) 0.0010(12) 0.0149(15) -0.0009(13) N20 0.0280(17) 0.0298(16) 0.0382(17) -0.0045(13) 0.0144(14) -0.0032(13) N21 0.0277(17) 0.0355(16) 0.0247(14) -0.0065(12) 0.0096(13) 0.0030(13) O1 0.066(2) 0.0387(16) 0.0481(16) -0.0040(13) 0.0041(16) 0.0111(14) O2 0.0493(17) 0.0539(16) 0.0234(13) -0.0008(11) 0.0149(12) -0.0039(13) O3 0.0402(16) 0.0304(14) 0.0333(13) -0.0042(10) 0.0165(11) -0.0011(11) S1 0.0325(5) 0.0131(4) 0.0164(4) -0.0011(3) 0.0080(4) -0.0006(3) S2 0.0224(5) 0.0150(4) 0.0190(4) 0.0000(3) 0.0071(3) -0.0008(3) S3 0.0215(4) 0.0152(4) 0.0179(4) -0.0024(3) 0.0069(3) -0.0002(3) Cu1 0.0234(2) 0.01370(19) 0.01583(19) -0.00232(15) 0.00533(16) -0.00138(16) Cu2 0.0241(2) 0.01292(18) 0.01665(19) 0.00002(15) 0.00622(17) 0.00069(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.457(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C3 N4 1.314(3) . ? C3 N2 1.335(3) . ? C3 S3 1.782(3) . ? C6 N5 1.295(3) . ? C6 C7 1.460(4) . ? C6 C20 1.496(4) . ? C7 N8 1.312(3) . ? C7 C21 1.489(4) . ? C10 N11 1.329(3) . ? C10 N9 1.335(3) . ? C10 S1 1.816(3) . ? C13 N12 1.311(3) . ? C13 C14 1.459(4) . ? C13 C22 1.486(4) . ? C14 N15 1.306(3) . ? C14 C23 1.496(4) . ? C17 N16 1.321(3) . ? C17 N18 1.332(4) . ? C17 S2 1.777(3) . ? C19 N18 1.460(3) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N19 1.445(4) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N19 1.448(4) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O1 1.224(4) . ? C26 N19 1.327(4) . ? C26 H26 0.9300 . ? C27 N20 1.453(4) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 N20 1.440(4) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 O2 1.218(4) . ? C29 N20 1.329(4) . ? C29 H29 0.9300 . ? C30 N21 1.456(4) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 N21 1.448(4) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 O3 1.233(3) . ? C32 N21 1.325(4) . ? C32 H24 0.9300 . ? N2 H2 0.83(3) . ? N4 N5 1.370(3) . ? N5 Cu1 1.955(2) . ? N8 N9 1.360(3) . ? N8 Cu1 1.949(2) . ? N11 N12 1.355(3) . ? N12 Cu2 1.950(2) . ? N15 N16 1.372(3) . ? N15 Cu2 1.961(2) . ? N18 H18 0.83(3) . ? S1 Cu1 2.2800(8) . ? S1 Cu2 2.2886(8) . ? S2 Cu2 2.2851(8) . ? S3 Cu1 2.2782(8) . ? S3 Cu2 2.7033(9) 3_565 ? Cu2 S3 2.7033(9) 3_565 ? 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 _geom_angle_publ_flag N2 C1 H1A 109.5 . . ? N2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N4 C3 N2 117.8(2) . . ? N4 C3 S3 125.8(2) . . ? N2 C3 S3 116.4(2) . . ? N5 C6 C7 114.1(2) . . ? N5 C6 C20 123.9(3) . . ? C7 C6 C20 122.0(2) . . ? N8 C7 C6 114.8(2) . . ? N8 C7 C21 122.1(2) . . ? C6 C7 C21 123.1(2) . . ? N11 C10 N9 116.0(2) . . ? N11 C10 S1 122.1(2) . . ? N9 C10 S1 121.8(2) . . ? N12 C13 C14 115.1(2) . . ? N12 C13 C22 122.6(3) . . ? C14 C13 C22 122.3(2) . . ? N15 C14 C13 114.0(2) . . ? N15 C14 C23 123.5(3) . . ? C13 C14 C23 122.5(2) . . ? N16 C17 N18 118.0(2) . . ? N16 C17 S2 125.5(2) . . ? N18 C17 S2 116.5(2) . . ? N18 C19 H19A 109.5 . . ? N18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C6 C20 H20A 109.5 . . ? C6 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C6 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C7 C21 H21A 109.5 . . ? C7 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C7 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C13 C22 H22A 109.5 . . ? C13 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C13 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C14 C23 H23A 109.5 . . ? C14 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C14 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N19 C24 H24A 109.5 . . ? N19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N19 C25 H25A 109.5 . . ? N19 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N19 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O1 C26 N19 125.6(4) . . ? O1 C26 H26 117.2 . . ? N19 C26 H26 117.2 . . ? N20 C27 H27A 109.5 . . ? N20 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N20 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N20 C28 H28A 109.5 . . ? N20 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N20 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O2 C29 N20 126.1(3) . . ? O2 C29 H29 117.0 . . ? N20 C29 H29 117.0 . . ? N21 C30 H30A 109.5 . . ? N21 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N21 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N21 C31 H31A 109.5 . . ? N21 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N21 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O3 C32 N21 125.5(3) . . ? O3 C32 H24 117.3 . . ? N21 C32 H24 117.3 . . ? C3 N2 C1 121.1(3) . . ? C3 N2 H2 121(2) . . ? C1 N2 H2 117.8(19) . . ? C3 N4 N5 111.6(2) . . ? C6 N5 N4 121.0(2) . . ? C6 N5 Cu1 115.08(18) . . ? N4 N5 Cu1 123.24(17) . . ? C7 N8 N9 119.5(2) . . ? C7 N8 Cu1 114.37(19) . . ? N9 N8 Cu1 126.11(17) . . ? C10 N9 N8 112.7(2) . . ? C10 N11 N12 112.6(2) . . ? C13 N12 N11 119.3(2) . . ? C13 N12 Cu2 114.48(18) . . ? N11 N12 Cu2 126.17(18) . . ? C14 N15 N16 121.2(2) . . ? C14 N15 Cu2 114.95(19) . . ? N16 N15 Cu2 123.59(17) . . ? C17 N16 N15 111.5(2) . . ? C17 N18 C19 122.0(3) . . ? C17 N18 H18 118.2(19) . . ? C19 N18 H18 119.0(19) . . ? C26 N19 C24 120.1(3) . . ? C26 N19 C25 121.5(3) . . ? C24 N19 C25 118.4(3) . . ? C29 N20 C28 121.5(3) . . ? C29 N20 C27 120.4(3) . . ? C28 N20 C27 118.1(3) . . ? C32 N21 C31 120.7(3) . . ? C32 N21 C30 121.0(3) . . ? C31 N21 C30 118.2(3) . . ? C10 S1 Cu1 95.40(9) . . ? C10 S1 Cu2 95.07(9) . . ? Cu1 S1 Cu2 169.52(4) . . ? C17 S2 Cu2 93.29(10) . . ? C3 S3 Cu1 92.95(10) . . ? C3 S3 Cu2 102.06(10) . 3_565 ? Cu1 S3 Cu2 85.70(3) . 3_565 ? N8 Cu1 N5 81.25(9) . . ? N8 Cu1 S3 164.30(7) . . ? N5 Cu1 S3 84.92(7) . . ? N8 Cu1 S1 83.71(7) . . ? N5 Cu1 S1 162.57(7) . . ? S3 Cu1 S1 108.62(3) . . ? N12 Cu2 N15 81.29(9) . . ? N12 Cu2 S2 162.29(7) . . ? N15 Cu2 S2 84.43(7) . . ? N12 Cu2 S1 83.44(7) . . ? N15 Cu2 S1 160.57(7) . . ? S2 Cu2 S1 107.98(3) . . ? N12 Cu2 S3 98.98(7) . 3_565 ? N15 Cu2 S3 92.70(7) . 3_565 ? S2 Cu2 S3 92.06(3) . 3_565 ? S1 Cu2 S3 101.50(3) . 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 C6 C7 N8 -6.6(4) . . . . ? C20 C6 C7 N8 171.9(3) . . . . ? N5 C6 C7 C21 171.7(3) . . . . ? C20 C6 C7 C21 -9.7(4) . . . . ? N12 C13 C14 N15 1.8(4) . . . . ? C22 C13 C14 N15 -176.3(3) . . . . ? N12 C13 C14 C23 -179.1(3) . . . . ? C22 C13 C14 C23 2.8(4) . . . . ? N4 C3 N2 C1 -3.3(4) . . . . ? S3 C3 N2 C1 177.2(2) . . . . ? N2 C3 N4 N5 179.3(2) . . . . ? S3 C3 N4 N5 -1.3(4) . . . . ? C7 C6 N5 N4 178.3(2) . . . . ? C20 C6 N5 N4 -0.3(4) . . . . ? C7 C6 N5 Cu1 7.3(3) . . . . ? C20 C6 N5 Cu1 -171.2(2) . . . . ? C3 N4 N5 C6 -179.5(3) . . . . ? C3 N4 N5 Cu1 -9.3(3) . . . . ? C6 C7 N8 N9 -179.6(2) . . . . ? C21 C7 N8 N9 2.0(4) . . . . ? C6 C7 N8 Cu1 2.6(3) . . . . ? C21 C7 N8 Cu1 -175.7(2) . . . . ? N11 C10 N9 N8 176.2(2) . . . . ? S1 C10 N9 N8 -2.4(3) . . . . ? C7 N8 N9 C10 -171.5(3) . . . . ? Cu1 N8 N9 C10 6.0(3) . . . . ? N9 C10 N11 N12 -174.3(2) . . . . ? S1 C10 N11 N12 4.3(3) . . . . ? C14 C13 N12 N11 -177.6(2) . . . . ? C22 C13 N12 N11 0.5(4) . . . . ? C14 C13 N12 Cu2 1.4(3) . . . . ? C22 C13 N12 Cu2 179.5(2) . . . . ? C10 N11 N12 C13 169.6(3) . . . . ? C10 N11 N12 Cu2 -9.3(3) . . . . ? C13 C14 N15 N16 -178.8(2) . . . . ? C23 C14 N15 N16 2.1(4) . . . . ? C13 C14 N15 Cu2 -4.1(3) . . . . ? C23 C14 N15 Cu2 176.8(2) . . . . ? N18 C17 N16 N15 -178.4(2) . . . . ? S2 C17 N16 N15 4.0(4) . . . . ? C14 N15 N16 C17 -177.8(3) . . . . ? Cu2 N15 N16 C17 7.9(3) . . . . ? N16 C17 N18 C19 6.5(4) . . . . ? S2 C17 N18 C19 -175.6(2) . . . . ? O1 C26 N19 C24 -3.1(5) . . . . ? O1 C26 N19 C25 177.4(3) . . . . ? O2 C29 N20 C28 -178.9(3) . . . . ? O2 C29 N20 C27 -2.0(5) . . . . ? O3 C32 N21 C31 1.9(5) . . . . ? O3 C32 N21 C30 177.8(3) . . . . ? N11 C10 S1 Cu1 -179.5(2) . . . . ? N9 C10 S1 Cu1 -1.0(2) . . . . ? N11 C10 S1 Cu2 0.9(2) . . . . ? N9 C10 S1 Cu2 179.4(2) . . . . ? N16 C17 S2 Cu2 -10.7(3) . . . . ? N18 C17 S2 Cu2 171.6(2) . . . . ? N4 C3 S3 Cu1 8.3(3) . . . . ? N2 C3 S3 Cu1 -172.3(2) . . . . ? N4 C3 S3 Cu2 94.5(3) . . . 3_565 ? N2 C3 S3 Cu2 -86.0(2) . . . 3_565 ? C7 N8 Cu1 N5 0.9(2) . . . . ? N9 N8 Cu1 N5 -176.7(2) . . . . ? C7 N8 Cu1 S3 29.4(4) . . . . ? N9 N8 Cu1 S3 -148.2(2) . . . . ? C7 N8 Cu1 S1 172.1(2) . . . . ? N9 N8 Cu1 S1 -5.5(2) . . . . ? C6 N5 Cu1 N8 -4.8(2) . . . . ? N4 N5 Cu1 N8 -175.5(2) . . . . ? C6 N5 Cu1 S3 -177.3(2) . . . . ? N4 N5 Cu1 S3 12.0(2) . . . . ? C6 N5 Cu1 S1 -35.4(4) . . . . ? N4 N5 Cu1 S1 153.88(18) . . . . ? C3 S3 Cu1 N8 -36.9(3) . . . . ? Cu2 S3 Cu1 N8 -138.8(3) 3_565 . . . ? C3 S3 Cu1 N5 -8.62(12) . . . . ? Cu2 S3 Cu1 N5 -110.50(7) 3_565 . . . ? C3 S3 Cu1 S1 -177.37(10) . . . . ? Cu2 S3 Cu1 S1 80.75(3) 3_565 . . . ? C10 S1 Cu1 N8 2.76(12) . . . . ? Cu2 S1 Cu1 N8 -179.7(2) . . . . ? C10 S1 Cu1 N5 33.2(3) . . . . ? Cu2 S1 Cu1 N5 -149.2(3) . . . . ? C10 S1 Cu1 S3 172.78(9) . . . . ? Cu2 S1 Cu1 S3 -9.6(2) . . . . ? C13 N12 Cu2 N15 -2.8(2) . . . . ? N11 N12 Cu2 N15 176.1(2) . . . . ? C13 N12 Cu2 S2 -39.4(4) . . . . ? N11 N12 Cu2 S2 139.6(2) . . . . ? C13 N12 Cu2 S1 -170.8(2) . . . . ? N11 N12 Cu2 S1 8.2(2) . . . . ? C13 N12 Cu2 S3 88.6(2) . . . 3_565 ? N11 N12 Cu2 S3 -92.5(2) . . . 3_565 ? C14 N15 Cu2 N12 3.9(2) . . . . ? N16 N15 Cu2 N12 178.5(2) . . . . ? C14 N15 Cu2 S2 173.4(2) . . . . ? N16 N15 Cu2 S2 -12.0(2) . . . . ? C14 N15 Cu2 S1 42.4(4) . . . . ? N16 N15 Cu2 S1 -143.00(18) . . . . ? C14 N15 Cu2 S3 -94.8(2) . . . 3_565 ? N16 N15 Cu2 S3 79.8(2) . . . 3_565 ? C17 S2 Cu2 N12 45.9(2) . . . . ? C17 S2 Cu2 N15 9.64(11) . . . . ? C17 S2 Cu2 S1 174.33(9) . . . . ? C17 S2 Cu2 S3 -82.88(9) . . . 3_565 ? C10 S1 Cu2 N12 -3.80(12) . . . . ? Cu1 S1 Cu2 N12 178.6(2) . . . . ? C10 S1 Cu2 N15 -42.1(2) . . . . ? Cu1 S1 Cu2 N15 140.3(3) . . . . ? C10 S1 Cu2 S2 -169.92(10) . . . . ? Cu1 S1 Cu2 S2 12.5(2) . . . . ? C10 S1 Cu2 S3 94.08(10) . . . 3_565 ? Cu1 S1 Cu2 S3 -83.5(2) . . . 3_565 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.467 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.070