#------------------------------------------------------------------------------ #$Date: 2015-04-02 14:22:18 +0300 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/56/2005689.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2005689 loop_ _publ_author_name 'Fox, S.' 'Stibrany, R. T.' 'Potenza, J. A.' 'Schugar, H. J.' _publ_section_title ; A Mixed-Metal Pentanuclear Complex Containing Linked Ni^II^N~2~S~2~ and Cu^I^I Units ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 2731 _journal_page_last 2734 _journal_paper_doi 10.1107/S0108270196001308 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac '[Cu3 Ni2 I3 (C14 H28 N2 S2)2] , 2C H3 C N' _chemical_formula_moiety 'C28 H56 Cu3 I3 N4 Ni2 S4,C4 H6 N2' _chemical_formula_structural '[(NiN2S2C14H28)2(CuI)3].2(CH3CN)' _chemical_formula_sum 'C32 H62 Cu3 I3 N6 Ni2 S4' _chemical_formula_weight 1343.87 _chemical_name_systematic ; Bis[S,S'(-)-trans-3,3'-(1,2-cyclohexandiyldinitrilo)-bis(2-methylpropane-2- thialato)nickel(II)] [(\m-iodocopper(I)-\k^2^S^1^,S^2'^)(\m-iodocopper(I)-\k^2^S^2^,S^1'^)(\m- iodocopper(I)-\k^2^S^2^,S^2'^)].diacetonitrile ; _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _atom_type_symbol IntTabIV _cell_angle_alpha 96.49(2) _cell_angle_beta 106.84(3) _cell_angle_gamma 107.77(3) _cell_formula_units_Z 2 _cell_length_a 12.837(3) _cell_length_b 18.081(4) _cell_length_c 11.747(4) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298 _cell_measurement_theta_max 16.82 _cell_measurement_theta_min 11.93 _cell_volume 2423.7(14) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'MULTAN11/82 (Main et al., 1982)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_structure_refinement MULTAN11/82 _computing_structure_solution MULTAN11/82 _diffrn_ambient_temperature 298 _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'xray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 5933 _diffrn_reflns_theta_max 22.0 _diffrn_standards_decay_% 4.1 _diffrn_standards_interval_count 300 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 4.16 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_type '\y scan (SDP; Enraf-Nonius, 1985)' _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.843 _exptl_crystal_density_meas 1.84(1) _exptl_crystal_density_method ; flotation in a mixture of carbon tetrachloride and 1,2-dibromoethane ; _exptl_crystal_description prism _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.603 _refine_diff_density_min -0.151 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.60 _refine_ls_hydrogen_treatment ; H atoms found in difference Fourier syntheses or placed at calculated positions and not refined ; _refine_ls_matrix_type full _refine_ls_number_parameters 451 _refine_ls_number_reflns 4724 _refine_ls_R_factor_all 5.25 _refine_ls_R_factor_obs 0.0388 _refine_ls_shift/esd_max 0 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 4F^2^/[\s^2^(F^2^)+0.0016F^4^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.047 _reflns_number_observed 4724 _reflns_number_total 5933 _reflns_observed_criterion I>3\s(I) _[local]_cod_data_source_file ta1057.cif _[local]_cod_data_source_block A _[local]_cod_cif_authors_sg_H-M P-1 _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value '4F^2^/[\s^2^(F^2^)+0.0016F^4^]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 4F^2^/[\s^2^(F^2^)+0.0016F^4^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 2422.0 _cod_database_code 2005689 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol I1 0.0473(2) 0.0650(3) 0.0455(3) 0.0200(2) 0.0122(2) -0.0008(2) I I2 0.0889(3) 0.0436(2) 0.0540(3) 0.0300(2) 0.0327(2) 0.0327(2) I I3 0.0800(3) 0.0650(3) 0.0389(2) 0.0409(2) 0.0250(2) 0.0209(2) I Cu 10.0501(4) 0.0489(4) 0.0337(4) 0.0210(3) 0.0177(3) 0.0113(4) Cu Cu2 0.0654(5) 0.0472(5) 0.0561(5) 0.0240(4) 0.0134(4) 0.0143(4) Cu Cu3 0.0777(5) 0.0627(5) 0.0431(5) 0.0422(4) 0.0253(4) 0.0167(4) Cu Ni1 0.0390(4) 0.0359(4) 0.0338(4) 0.0148(3) 0.0149(3) 0.0115(3) Ni Ni2 0.0511(4) 0.0439(4) 0.0300(4) 0.0222(3) 0.0206(3) 0.0175(3) Ni S1 0.0423(8) 0.0369(8) 0.0350(8) 0.0142(7) 0.0128(7) 0.0130(7) S S2 0.0500(9) 0.0375(9) 0.0520(10) 0.0138(7) 0.0175(8) 0.0150(8) S S3 0.0582(9) 0.0450(9) 0.0294(8) 0.0226(7) 0.0203(7) 0.0161(7) S S4 0.0676(9) 0.0501(9) 0.0289(8) 0.0315(7) 0.0244(7) 0.0177(7) S N1 0.038(2) 0.046(3) 0.033(3) 0.020(2) 0.017(2) 0.014(2) N N2 0.042(3) 0.046(3) 0.047(3) 0.013(2) 0.016(2) 0.008(3) N N3 0.060(3) 0.050(3) 0.038(3) 0.024(2) 0.021(2) 0.021(2) N N4 0.055(3) 0.053(3) 0.040(3) 0.030(2) 0.021(2) 0.019(2) N C1 0.044(3) 0.050(4) 0.031(3) 0.024(3) 0.010(3) 0.009(3) C C2 0.061(4) 0.058(4) 0.048(4) 0.035(3) 0.016(3) 0.020(3) C C3 0.065(4) 0.083(5) 0.054(4) 0.045(3) 0.017(3) 0.025(4) C C4 0.069(4) 0.098(5) 0.063(5) 0.050(4) 0.002(4) 0.020(4) C C5 0.056(4) 0.064(5) 0.064(5) 0.028(3) 0.010(4) 0.011(4) C C6 0.050(3) 0.044(3) 0.046(4) 0.026(3) 0.015(3) 0.009(3) C C7 0.046(3) 0.039(3) 0.038(3) 0.019(3) 0.023(3) 0.017(3) C C8 0.041(3) 0.042(3) 0.041(3) 0.018(3) 0.021(3) 0.016(3) C C9 0.055(4) 0.054(4) 0.064(5) 0.018(3) 0.019(3) 0.013(4) C C10 0.050(4) 0.043(4) 0.062(4) 0.010(3) 0.026(3) 0.016(3) C C11 0.050(4) 0.046(4) 0.053(4) 0.021(3) 0.015(3) 0.010(3) C C12 0.050(4) 0.057(4) 0.058(4) 0.012(3) 0.025(3) 0.023(3) C C13 0.067(5) 0.046(4) 0.065(5) 0.018(3) 0.012(4) 0.003(4) C C14 0.064(5) 0.059(5) 0.123(7) 0.008(4) 0.036(5) 0.030(5) C C15 0.050(4) 0.049(4) 0.052(4) 0.025(3) 0.016(3) 0.020(3) C C16 0.051(3) 0.055(4) 0.040(4) 0.028(3) 0.016(3) 0.017(3) C C17 0.055(4) 0.061(4) 0.058(4) 0.026(3) 0.022(3) 0.019(4) C C18 0.066(4) 0.070(5) 0.074(5) 0.034(3) 0.019(4) 0.017(4) C C19 0.079(4) 0.071(4) 0.098(6) 0.049(3) 0.035(4) 0.042(4) C C20 0.077(4) 0.064(4) 0.070(4) 0.041(3) 0.030(4) 0.045(3) C C21 0.060(4) 0.057(4) 0.032(3) 0.026(3) 0.023(3) 0.025(3) C C22 0.072(4) 0.064(4) 0.049(4) 0.036(3) 0.035(3) 0.036(3) C C23 0.070(4) 0.054(4) 0.033(3) 0.036(3) 0.030(3) 0.015(3) C C24 0.069(4) 0.062(4) 0.037(3) 0.032(3) 0.030(3) 0.017(3) C C25 0.075(5) 0.091(5) 0.043(4) 0.029(4) 0.017(4) 0.030(4) C C26 0.092(5) 0.088(5) 0.061(4) 0.043(4) 0.053(3) 0.046(4) C N5 0.121(7) 0.180(10) 0.200(10) 0.012(8) 0.088(6) 0.013(9) N N6 0.117(6) 0.186(9) 0.290(10) 0.005(6) 0.096(6) -0.1 N C27 0.072(4) 0.063(4) 0.031(4) 0.029(3) 0.016(3) 0.010(3) C C28 0.090(4) 0.084(5) 0.052(4) 0.045(4) 0.045(3) 0.034(4) C C29 0.121(8) 0.089(8) 0.131(9) 0.010(7) 0.047(7) -0.005(7) C C30 0.079(7) 0.140(10) 0.140(10) 0.018(7) 0.028(6) -0.016(8) C C31 0.088(6) 0.123(9) 0.145(9) 0.008(6) 0.049(6) -0.045(7) C C32 0.123(6) 0.093(7) 0.217(9) 0.016(5) 0.116(5) -0.034(7) C loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_B_iso_or_equiv _atom_site_thermal_displace_type _atom_site_type_symbol I1 -0.28551(4) 0.01678(3) -0.12310(5) 4.31(1) Uij I I2 0.14239(5) 0.48794(3) 0.28152(5) 4.58(1) Uij I I3 0.10746(4) 0.21067(3) 0.60060(4) 4.40(1) Uij I Cu1 -0.12773(7) 0.12876(5) 0.03861(7) 3.35(2) Uij Cu Cu2 0.08364(8) 0.33859(5) 0.21794(9) 4.48(3) Uij Cu Cu3 0.00611(8) 0.20467(5) 0.37623(8) 4.38(2) Uij Cu Ni1 0.17693(7) 0.16473(5) 0.31387(7) 2.76(2) Uij Ni Ni2 -0.15492(7) 0.32202(5) 0.17826(7) 3.00(2) Uij Ni S1 -0.0075(1) 0.1140(1) 0.2106(2) 2.98(4) Uij S S2 0.2109(2) 0.2765(1) 0.2570(2) 3.66(5) Uij S S3 -0.0867(2) 0.2611(1) 0.0647(2) 3.26(4) Uij S S4 -0.1342(2) 0.2550(1) 0.3183(2) 3.45(4) Uij S N1 0.1685(4) 0.0629(3) 0.3537(5) 2.8(1) Uij N N2 0.3267(5) 0.2082(3) 0.4380(5) 3.6(2) Uij N N3 -0.2060(5) 0.3741(3) 0.0500(5) 3.6(1) Uij N N4 -0.1879(5) 0.3954(3) 0.2811(5) 3.5(1) Uij N C1 0.2634(6) 0.0756(4) 0.4700(6) 3.2(2) Uij C C2 0.2953(6) 0.0026(4) 0.4929(7) 4.1(2) Uij C C3 0.3955(6) 0.0238(5) 0.6124(7) 4.9(2) Uij C C4 0.5013(7) 0.0914(5) 0.6126(8) 6.0(3) Uij C C5 0.4709(7) 0.1647(5) 0.5870(8) 4.9(2) Uij C C6 0.3698(6) 0.1431(4) 0.4690(6) 3.5(2) Uij C C7 0.0519(5) 0.0157(4) 0.3535(6) 3.0(2) Uij C C8 -0.0418(5) 0.0107(4) 0.2364(6) 3.0(2) Uij C C9 0.4092(6) 0.2768(5) 0.4153(7) 4.6(2) Uij C C10 0.3521(6) 0.3367(4) 0.3790(7) 4.1(2) Uij C C11 -0.0414(6) -0.0440(4) 0.1288(7) 3.9(2) Uij C C12 -0.1596(6) -0.0147(5) 0.2529(7) 4.2(2) Uij C C13 0.3366(7) 0.3806(5) 0.4866(8) 5.0(2) Uij C C14 0.4256(8) 0.3958(5) 0.323(1) 6.6(3) Uij C C15 -0.2176(6) 0.4484(4) 0.1028(7) 3.8(2) Uij C C16 -0.2644(6) 0.4306(4) 0.2038(6) 3.6(2) Uij C C17 -0.2770(6) 0.5043(5) 0.2703(7) 4.4(2) Uij C C18 -0.3533(7) 0.5353(5) 0.1791(8) 5.4(2) Uij C C19 -0.3062(7) 0.5539(5) 0.0772(8) 5.8(2) Uij C C20 -0.2912(7) 0.4831(4) 0.0112(7) 5.0(2) Uij C C21 -0.1216(6) 0.3045(4) -0.0718(6) 3.6(2) Uij C C22 -0.1332(6) 0.3827(4) -0.0287(6) 4.2(2) Uij C C23 -0.1425(6) 0.3239(4) 0.4428(6) 3.6(2) Uij C C24 -0.2226(6) 0.3646(4) 0.3815(6) 4.0(2) Uij C C25 -0.2350(7) 0.2479(5) -0.1667(7) 5.5(2) Uij C C26 -0.0219(7) 0.3191(5) -0.1205(7) 5.5(2) Uij C C27 -0.0238(7) 0.3814(5) 0.5198(6) 4.3(2) Uij C C28 -0.1993(7) 0.2735(5) 0.5204(7) 5.2(2) Uij C N5 0.4870(9) 0.7234(8) 0.071(1) 13.7(5) Uij N C29 0.574(1) 0.7429(7) 0.055(1) 9.7(4) Uij C C30 0.686(1) 0.7697(8) 0.035(1) 10.3(4) Uij C N6 0.4735(9) 0.7944(7) 0.781(1) 17.3(4) Uij N C31 0.4472(9) 0.8347(8) 0.834(1) 10.3(4) Uij C C32 0.4127(9) 0.8893(7) 0.903(1) 11.3(4) Uij C HC111 -0.1033 -0.0494 0.0558 5.07 Uiso H HC112 0.0391 -0.0258 0.1249 5.07 Uiso H HC113 -0.0532 -0.0915 0.1511 5.07 Uiso H HC121 -0.2161 -0.0239 0.1947 5.13 Uiso H HC122 -0.1772 -0.0673 0.2755 5.13 Uiso H HC123 -0.1447 0.0291 0.3196 5.13 Uiso H HC131 0.3015 0.4216 0.4602 6.16 Uiso H HC132 0.2729 0.3363 0.5136 6.16 Uiso H HC133 0.4223 0.4294 0.5552 6.16 Uiso H HC141 0.3886 0.4310 0.3068 7.83 Uiso H HC142 0.5079 0.4294 0.3913 7.83 Uiso H HC143 0.4308 0.3694 0.2763 7.83 Uiso H HC15 -0.1459 0.4859 0.1393 5.02 Uiso H HC16 -0.3526 0.3896 0.1643 4.92 Uiso H HC171 -0.1816 0.5465 0.3201 5.77 Uiso H HC172 -0.2989 0.4832 0.3326 5.77 Uiso H HC181 -0.3646 0.5822 0.2245 6.83 Uiso H HC182 -0.4398 0.4963 0.1399 6.83 Uiso H HC191 -0.2350 0.5963 0.1245 7.25 Uiso H HC192 -0.3551 0.5748 0.0204 7.25 Uiso H HC201 -0.3575 0.4470 -0.0141 6.16 Uiso H HC202 -0.2591 0.4959 -0.0510 6.16 Uiso H HC221 -0.0698 0.4190 0.0126 5.19 Uiso H HC222 -0.1769 0.4036 -0.1103 5.19 Uiso H HC241 -0.2820 0.3278 0.3457 5.19 Uiso H HC242 -0.2207 0.4138 0.4446 5.19 Uiso H HC251 -0.2184 0.2085 -0.1939 6.98 Uiso H HC252 -0.2973 0.2352 -0.1377 6.98 Uiso H HC253 -0.2549 0.2682 -0.2392 6.98 Uiso H HC261 -0.0126 0.2709 -0.1472 6.65 Uiso H HC262 -0.0330 0.3459 -0.1864 6.65 Uiso H HC263 0.0391 0.3574 -0.0680 6.65 Uiso H HC271 0.0120 0.3601 0.5699 5.44 Uiso H HC272 0.0131 0.4117 0.4712 5.44 Uiso H HC273 -0.0205 0.4228 0.5988 5.44 Uiso H HC281 -0.1544 0.2443 0.5543 6.17 Uiso H HC282 -0.2154 0.3163 0.5843 6.17 Uiso H HC283 -0.2645 0.2470 0.4841 6.17 Uiso H HC301 0.7370 0.7407 0.0615 12.72 Uiso H HC302 0.6733 0.7658 -0.0529 12.72 Uiso H HC303 0.7301 0.8253 0.0727 12.72 Uiso H HC321 0.3650 0.9125 0.8474 12.60 Uiso H HC322 0.3699 0.8654 0.9502 12.60 Uiso H HC323 0.4803 0.9340 0.9556 12.60 Uiso H HN1 0.1798 0.0330 0.2952 3.6545 Uiso H HN2 0.3179 0.2300 0.5047 4.9421 Uiso H HN3 -0.2767 0.3425 -0.0024 4.6250 Uiso H HN4 -0.1209 0.4353 0.3243 4.4470 Uiso H HC1 0.2591 0.1121 0.5556 4.2734 Uiso H HC21 0.3043 -0.0288 0.4196 5.1696 Uiso H HC22 0.2350 -0.0298 0.4853 5.1696 Uiso H HC31 0.4149 -0.0220 0.6304 6.3851 Uiso H HC32 0.3722 0.0421 0.6804 6.3851 Uiso H HC41 0.5258 0.0705 0.5492 7.8077 Uiso H HC42 0.5632 0.1025 0.6886 7.8077 Uiso H HC51 0.5210 0.2074 0.5821 6.2458 Uiso H HC52 0.4445 0.1858 0.6510 6.2458 Uiso H HC6 0.4025 0.1269 0.4085 4.5993 Uiso H HC71 0.0496 0.0493 0.4186 3.7088 Uiso H HC72 0.0466 -0.0415 0.3598 3.7088 Uiso H HC91 0.4179 0.2527 0.3474 5.7715 Uiso H HC92 0.4783 0.3025 0.4758 5.7715 Uiso H loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -8 2 5 7 -6 -7 2 -8 8 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag I1 Cu1 S1 124.64(6) yes I1 Cu1 S3 130.41(6) yes S1 Cu1 S3 104.44(6) yes I2 Cu2 S2 122.77(5) yes I2 Cu2 S3 122.54(7) yes S2 Cu2 S3 111.74(8) yes I3 Cu3 S1 126.12(7) yes I3 Cu3 S4 121.51(7) yes S1 Cu3 S4 108.90(7) yes S1 Ni1 S2 97.26(8) yes Cu1 S1 Ni1 136.18(9) ? Cu1 S1 Cu3 109.09(9) ? Cu3 S1 C8 112.2(2) ? Cu3 S1 Ni1 136.18(9) ? Cu2 S2 Ni1 123.60(10) ? Cu1 S3 Cu2 115.60(9) ? Cu1 S3 C21 119.1(2) ? Ni2 S3 C21 99.6(3) ? Cu2 S3 C21 114.3(2) ? Cu3 S4 C23 114.6(2) ? C1 N1 C7 113.6(5) ? Ni1 N1 C7 112.9(4) ? Ni1 N2 C9 114.4(5) ? Ni2 N3 C22 111.4(5) ? C15 N3 C22 115.8(6) ? Ni2 N4 C24 114.5(5) ? N1 C1 C2 115.3(5) ? C2 C1 C6 110.0(6) ? C2 C3 C4 111.2(7) ? C4 C5 C6 110.4(6) ? C1 C6 C5 111.6(6) ? S1 C8 C7 105.8(4) ? C7 C8 C11 111.8(6) ? S1 C8 C11 109.3(5) ? C11 C8 C12 111.7(5) ? S2 C10 C13 112.5(6) ? C9 C10 C13 111.4(7) ? N3 C15 C16 106.3(6) ? C16 C15 C20 112.2(7) ? N4 C16 C17 115.6(5) ? C16 C17 C18 109.5(6) ? C18 C19 C20 112.9(7) ? S3 C21 C22 106.5(5) ? S3 C21 C26 108.6(5) ? C22 C21 C26 110.0(6) ? N3 C22 C21 111.5(6) ? S4 C23 C27 111.0(6) ? C24 C23 C27 112.8(6) ? C27 C23 C28 110.4(6) ? N5 C29 C30 179.0(10) ? S1 Ni1 N1 88.70(10) yes S1 Ni1 N2 166.1(2) yes S2 Ni1 N1 169.5(2) yes S2 Ni1 N2 88.9(2) yes N1 Ni1 N2 87.2(2) yes S3 Ni2 S4 96.21(9) yes S3 Ni2 N3 89.9(2) yes S3 Ni2 N4 167.8(2) yes S4 Ni2 N4 89.6(2) yes N3 Ni2 N4 86.3(3) yes S4 Ni2 N3 168.4(2) yes Cu1 S1 C8 115.7(2) ? Ni1 S1 C8 100.6(2) ? Cu2 S2 C10 114.0(3) ? Ni1 S2 C10 100.0(3) ? Cu1 S3 Ni2 121.16(9) ? Cu2 S3 Ni2 80.19(6) ? Cu3 S4 Ni2 125.60(10) ? Ni2 S4 C23 99.1(2) ? Ni1 N1 C1 108.9(4) ? Ni1 N2 C6 109.7(3) ? Ni2 N3 C15 109.5(4) ? C6 N2 C9 115.9(6) ? Ni2 N4 C16 109.0(4) ? C16 N4 C24 116.8(6) ? N1 C1 C6 106.7(6) ? C1 C2 C3 110.2(6) ? C3 C4 C5 111.2(8) ? N2 C6 C1 105.1(6) ? N2 C6 C5 115.7(6) ? N1 C7 C8 110.9(6) ? N2 C9 C10 110.3(7) ? C7 C8 C12 109.9(6) ? S1 C8 C12 107.9(5) ? C13 C10 C14 110.5(6) ? S2 C10 C9 104.6(4) ? S2 C10 C14 108.0(5) ? C9 C10 C14 110.5(6) ? N3 C15 C20 115.3(6) ? N4 C16 C15 105.9(6) ? C15 C16 C17 112.0(6) ? C17 C18 C19 111.5(8) ? C15 C20 C19 110.3(6) ? S3 C21 C25 109.4(5) ? C22 C21 C25 110.7(7) ? C25 C21 C26 111.4(6) ? S4 C23 C24 106.1(4) ? S4 C23 C28 108.0(5) ? C24 C23 C28 108.3(7) ? N4 C24 C23 109.9(7) ? N6 C31 C32 178(2) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag I1 Cu1 2.4925(8) yes I2 Cu2 2.5280(10) yes I3 Cu3 2.5520(10) yes Cu1 S1 2.259(2) yes Cu1 S3 2.250(2) yes Cu2 S2 2.223(2) yes Cu2 S3 2.295(2) yes Cu3 S1 2.327(2) yes Cu3 S4 2.228(2) yes S1 C8 1.865(7) ? S3 C21 1.862(7) ? N2 C6 1.480(10) ? N1 C7 1.478(8) ? N4 C24 1.480(10) ? N3 C22 1.480(10) ? C1 C2 1.520(10) ? C3 C4 1.520(10) ? C5 C6 1.512(9) ? C9 C10 1.520(10) ? C8 C12 1.520(10) ? C10 C14 1.540(10) ? C15 C20 1.540(10) ? C17 C18 1.510(10) ? C19 C20 1.510(10) ? C21 C25 1.518(9) ? C23 C24 1.510(10) ? C23 C28 1.530(10) ? N6 C31 1.10(2) ? C31 C32 1.45(2) ? Ni1 S1 2.163(2) yes Ni1 S2 2.156(2) yes Ni1 N1 1.928(6) yes Ni1 N2 1.907(5) yes Ni2 S3 2.166(2) yes Ni2 S4 2.152(2) yes Ni2 N3 1.926(6) yes Ni2 N4 1.917(7) yes S2 C10 1.861(6) ? S4 C23 1.860(8) ? N2 C9 1.470(10) ? N1 C1 1.483(8) ? N4 C16 1.480(10) ? N3 C15 1.480(10) ? C2 C3 1.518(9) ? C1 C6 1.533(9) ? C4 C5 1.530(10) ? C7 C8 1.514(9) ? C8 C11 1.520(10) ? C10 C13 1.510(10) ? C15 C16 1.500(10) ? C16 C17 1.540(10) ? C18 C19 1.510(10) ? C21 C22 1.510(10) ? C21 C26 1.510(10) ? C23 C27 1.497(8) ? N5 C29 1.13(2) ? C29 C30 1.47(2) ?