# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Felix Zamora' _publ_contact_author_email FELIX.ZAMORA@UAM.ES _publ_section_title ; Dynamic Combinatorial Chemistry in a Solvothermal Process of Cu(I,II) and Organosulfur Ligands ; loop_ _publ_author_name 'Felix Zamora' 'Oscar Castillo' 'Salome Delgado' 'Adriano Santana' # Attachment 'CIFs_2.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 741279' _chemical_name_systematic ; bis(mu-Pyridine-2(1H)-thione-k2S:S)-tetrakis(pyridine-2(1H)-thione-S) dicopper(i) sulphate - ethanol (1/5) ; _chemical_melting_point ? _chemical_formula_moiety '2(C30 H30 Cu2 N6 S6), 1(O4 S), 5(C2 H6 O)' _chemical_formula_sum 'C40 H60 Cu2 N6 O9 S7' _chemical_formula_iupac '[Cu2(mu-C5H5NS)2(C5H5NS)4](SO4).5CH3CH2OH' _chemical_formula_weight 1120.44 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5968(7) _cell_length_b 16.9983(17) _cell_length_c 18.4105(18) _cell_angle_alpha 113.803(6) _cell_angle_beta 92.864(6) _cell_angle_gamma 90.628(6) _cell_volume 2171.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 53579 _cell_measurement_theta_min 1.21 _cell_measurement_theta_max 26.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 1.381 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'CrysAlis RED (Oxford Diffraction, 2003)' _exptl_absorpt_correction_T_min 0.6436 _exptl_absorpt_correction_T_max 0.8196 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _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_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 53579 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 26.48 _reflns_number_total 8703 _reflns_number_gt 6398 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Sir92 (Altamore et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.1342P)^2^+0.1835P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8703 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.2024 _refine_ls_wR_factor_gt 0.1922 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.000 _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 Cu1 Cu 0.53173(6) 0.42722(3) 0.43253(3) 0.02737(18) Uani 1 1 d . . . Cu2 Cu 0.96751(7) 0.06580(3) 0.07233(3) 0.03021(18) Uani 1 1 d . . . C1 C 0.5853(5) 0.2225(3) 0.3906(3) 0.0260(9) Uani 1 1 d . . . C2 C 0.5160(5) 0.2028(3) 0.3128(3) 0.0273(9) Uani 1 1 d . . . H2 H 0.5149 0.2458 0.2922 0.033 Uiso 1 1 calc R . . C3 C 0.4503(6) 0.1219(3) 0.2670(3) 0.0340(11) Uani 1 1 d . . . H3 H 0.4048 0.1083 0.2141 0.041 Uiso 1 1 calc R . . C4 C 0.4500(7) 0.0588(3) 0.2977(3) 0.0403(12) Uani 1 1 d . . . H4 H 0.4038 0.0025 0.2660 0.048 Uiso 1 1 calc R . . C5 C 0.5149(7) 0.0784(3) 0.3717(3) 0.0410(12) Uani 1 1 d . . . H5 H 0.5150 0.0360 0.3931 0.049 Uiso 1 1 calc R . . C6 C 0.7032(6) 0.4346(3) 0.2799(2) 0.0284(10) Uani 1 1 d . . . C7 C 0.8491(6) 0.3958(3) 0.2996(3) 0.0294(10) Uani 1 1 d . . . H7 H 0.8351 0.3658 0.3329 0.035 Uiso 1 1 calc R . . C8 C 1.0101(6) 0.4001(3) 0.2722(3) 0.0379(12) Uani 1 1 d . . . H8 H 1.1071 0.3735 0.2867 0.046 Uiso 1 1 calc R . . C9 C 1.0338(7) 0.4434(3) 0.2230(3) 0.0442(13) Uani 1 1 d . . . H9 H 1.1463 0.4474 0.2041 0.053 Uiso 1 1 calc R . . C10 C 0.8945(8) 0.4788(4) 0.2032(3) 0.0482(13) Uani 1 1 d . . . H10 H 0.9071 0.5075 0.1688 0.058 Uiso 1 1 calc R . . C11 C 0.2152(6) 0.4026(2) 0.5432(3) 0.0260(9) Uani 1 1 d . . . C12 C 0.0510(6) 0.4009(3) 0.5730(3) 0.0318(10) Uani 1 1 d . . . H12 H -0.0437 0.4303 0.5607 0.038 Uiso 1 1 calc R . . C13 C 0.0250(8) 0.3565(3) 0.6205(3) 0.0439(13) Uani 1 1 d . . . H13 H -0.0874 0.3551 0.6405 0.053 Uiso 1 1 calc R . . C14 C 0.1670(9) 0.3132(4) 0.6392(3) 0.0510(14) Uani 1 1 d . . . H14 H 0.1508 0.2828 0.6719 0.061 Uiso 1 1 calc R . . C15 C 0.3242(8) 0.3158(3) 0.6103(3) 0.0475(14) Uani 1 1 d . . . H15 H 0.4202 0.2869 0.6224 0.057 Uiso 1 1 calc R . . C16 C 0.9275(5) 0.0877(3) 0.2556(3) 0.0289(10) Uani 1 1 d . . . C17 C 0.9926(5) 0.1729(3) 0.2817(3) 0.0289(10) Uani 1 1 d . . . H17 H 0.9900 0.2010 0.2464 0.035 Uiso 1 1 calc R . . C18 C 1.0602(6) 0.2153(3) 0.3588(3) 0.0351(11) Uani 1 1 d . . . H18 H 1.1029 0.2732 0.3766 0.042 Uiso 1 1 calc R . . C19 C 1.0672(7) 0.1747(3) 0.4117(3) 0.0387(12) Uani 1 1 d . . . H19 H 1.1133 0.2043 0.4650 0.046 Uiso 1 1 calc R . . C20 C 1.0061(8) 0.0916(4) 0.3845(3) 0.0463(13) Uani 1 1 d . . . H20 H 1.0102 0.0624 0.4190 0.056 Uiso 1 1 calc R . . C21 C 0.7841(6) 0.2403(3) 0.0865(3) 0.0330(11) Uani 1 1 d . . . C22 C 0.6442(6) 0.2126(3) 0.1177(3) 0.0328(10) Uani 1 1 d . . . H22 H 0.6630 0.1703 0.1384 0.039 Uiso 1 1 calc R . . C23 C 0.4806(6) 0.2456(4) 0.1188(3) 0.0420(12) Uani 1 1 d . . . H23 H 0.3873 0.2270 0.1413 0.050 Uiso 1 1 calc R . . C24 C 0.4505(8) 0.3063(4) 0.0871(4) 0.0544(16) Uani 1 1 d . . . H24 H 0.3368 0.3288 0.0867 0.065 Uiso 1 1 calc R . . C25 C 0.5833(8) 0.3318(3) 0.0577(4) 0.0495(14) Uani 1 1 d . . . H25 H 0.5652 0.3735 0.0361 0.059 Uiso 1 1 calc R . . C26 C 1.2973(6) -0.0617(3) 0.0787(2) 0.0275(9) Uani 1 1 d . . . C27 C 1.4622(7) -0.0953(3) 0.0758(3) 0.0363(11) Uani 1 1 d . . . H27 H 1.5531 -0.0780 0.0512 0.044 Uiso 1 1 calc R . . C28 C 1.4961(8) -0.1546(4) 0.1090(3) 0.0499(14) Uani 1 1 d . . . H28 H 1.6102 -0.1774 0.1073 0.060 Uiso 1 1 calc R . . C29 C 1.3646(10) -0.1800(4) 0.1439(4) 0.0618(17) Uani 1 1 d . . . H29 H 1.3884 -0.2198 0.1672 0.074 Uiso 1 1 calc R . . C30 C 1.2041(10) -0.1494(4) 0.1453(4) 0.0608(18) Uani 1 1 d . . . H30 H 1.1114 -0.1686 0.1676 0.073 Uiso 1 1 calc R . . N1 N 0.5808(5) 0.1591(2) 0.4165(2) 0.0343(9) Uani 1 1 d . . . H1 H 0.6230 0.1705 0.4653 0.041 Uiso 1 1 calc R . . N2 N 0.7354(6) 0.4748(3) 0.2312(2) 0.0416(10) Uani 1 1 d . . . H2A H 0.6472 0.4998 0.2171 0.050 Uiso 1 1 calc R . . N3 N 0.3470(5) 0.3593(2) 0.5637(2) 0.0343(9) Uani 1 1 d . . . H3A H 0.4518 0.3599 0.5456 0.041 Uiso 1 1 calc R . . N4 N 0.9394(5) 0.0503(3) 0.3083(2) 0.0370(9) Uani 1 1 d . . . H4A H 0.9018 -0.0036 0.2922 0.044 Uiso 1 1 calc R . . N5 N 0.7451(6) 0.2994(3) 0.0577(3) 0.0473(11) Uani 1 1 d . . . H5A H 0.8301 0.3184 0.0376 0.057 Uiso 1 1 calc R . . N6 N 1.1749(6) -0.0905(3) 0.1144(2) 0.0409(10) Uani 1 1 d . . . H6 H 1.0691 -0.0692 0.1177 0.049 Uiso 1 1 calc R . . S1 S 0.68245(14) 0.32052(7) 0.45368(7) 0.0317(3) Uani 1 1 d . . . S2 S 0.49605(14) 0.43567(7) 0.31197(7) 0.0326(3) Uani 1 1 d . . . S3 S 0.25632(13) 0.45439(6) 0.48279(6) 0.0226(2) Uani 1 1 d . . . S4 S 0.82929(15) 0.02779(8) 0.16278(7) 0.0361(3) Uani 1 1 d . . . S5 S 0.99379(15) 0.20354(8) 0.08107(8) 0.0364(3) Uani 1 1 d . . . S6 S 1.24572(13) 0.01410(7) 0.04191(6) 0.0247(3) 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 Cu1 0.0219(3) 0.0206(3) 0.0298(3) 0.0002(2) -0.0006(2) 0.0001(2) Cu2 0.0243(3) 0.0323(3) 0.0227(3) -0.0004(2) 0.0003(2) -0.0014(2) C1 0.0147(19) 0.023(2) 0.033(2) 0.0042(19) 0.0005(17) -0.0005(16) C2 0.021(2) 0.027(2) 0.026(2) 0.0037(19) 0.0021(18) -0.0052(17) C3 0.028(2) 0.035(2) 0.025(2) -0.002(2) -0.0001(19) -0.003(2) C4 0.038(3) 0.022(2) 0.045(3) -0.003(2) 0.008(2) -0.013(2) C5 0.048(3) 0.023(2) 0.048(3) 0.009(2) 0.011(3) -0.003(2) C6 0.027(2) 0.024(2) 0.019(2) -0.0056(18) -0.0079(18) -0.0043(17) C7 0.024(2) 0.024(2) 0.035(2) 0.0064(19) -0.0066(19) -0.0062(17) C8 0.021(2) 0.036(3) 0.047(3) 0.008(2) -0.003(2) -0.0012(19) C9 0.038(3) 0.045(3) 0.041(3) 0.009(3) 0.007(2) -0.005(2) C10 0.051(3) 0.054(3) 0.039(3) 0.019(3) 0.000(3) -0.005(3) C11 0.027(2) 0.0139(18) 0.025(2) -0.0028(16) -0.0112(18) -0.0048(16) C12 0.030(2) 0.021(2) 0.033(2) 0.0001(19) -0.007(2) -0.0085(18) C13 0.051(3) 0.032(3) 0.038(3) 0.003(2) 0.004(3) -0.014(2) C14 0.077(4) 0.039(3) 0.040(3) 0.020(3) -0.002(3) -0.006(3) C15 0.066(4) 0.036(3) 0.039(3) 0.014(2) -0.010(3) 0.009(3) C16 0.0131(19) 0.034(2) 0.027(2) -0.001(2) -0.0013(17) -0.0009(17) C17 0.020(2) 0.030(2) 0.027(2) 0.0006(19) 0.0014(18) 0.0038(17) C18 0.027(2) 0.031(2) 0.033(3) -0.001(2) -0.006(2) -0.0003(19) C19 0.039(3) 0.041(3) 0.023(2) 0.000(2) -0.009(2) 0.006(2) C20 0.057(3) 0.048(3) 0.029(3) 0.012(2) -0.005(3) 0.008(3) C21 0.031(2) 0.020(2) 0.031(2) -0.0053(19) -0.008(2) -0.0080(18) C22 0.023(2) 0.036(2) 0.029(2) 0.004(2) -0.0086(19) -0.0054(19) C23 0.024(2) 0.055(3) 0.037(3) 0.008(3) -0.004(2) -0.003(2) C24 0.047(3) 0.043(3) 0.054(4) 0.000(3) -0.012(3) 0.010(3) C25 0.048(3) 0.036(3) 0.055(4) 0.011(3) -0.012(3) 0.001(2) C26 0.030(2) 0.026(2) 0.0150(19) -0.0031(17) -0.0055(18) -0.0110(18) C27 0.034(3) 0.036(3) 0.026(2) 0.001(2) -0.011(2) -0.011(2) C28 0.055(4) 0.043(3) 0.037(3) 0.003(3) -0.014(3) 0.001(3) C29 0.095(5) 0.041(3) 0.045(3) 0.014(3) 0.001(4) -0.004(3) C30 0.087(5) 0.040(3) 0.050(4) 0.012(3) 0.020(4) -0.013(3) N1 0.034(2) 0.030(2) 0.031(2) 0.0049(17) -0.0063(17) -0.0016(17) N2 0.040(2) 0.046(2) 0.033(2) 0.011(2) -0.0071(19) -0.001(2) N3 0.036(2) 0.0250(19) 0.036(2) 0.0072(17) -0.0070(18) 0.0029(16) N4 0.034(2) 0.031(2) 0.033(2) 0.0009(18) -0.0055(18) -0.0066(17) N5 0.043(3) 0.038(2) 0.051(3) 0.009(2) -0.004(2) -0.010(2) N6 0.048(3) 0.033(2) 0.035(2) 0.0067(19) 0.009(2) -0.0089(19) S1 0.0207(5) 0.0191(5) 0.0386(7) -0.0044(5) -0.0101(5) 0.0012(4) S2 0.0188(5) 0.0363(6) 0.0291(6) 0.0002(5) -0.0082(5) -0.0003(4) S3 0.0162(5) 0.0178(5) 0.0283(5) 0.0044(4) -0.0053(4) -0.0016(4) S4 0.0237(6) 0.0470(7) 0.0197(5) -0.0043(5) -0.0012(5) -0.0137(5) S5 0.0219(6) 0.0314(6) 0.0392(7) -0.0023(5) -0.0025(5) -0.0091(5) S6 0.0188(5) 0.0292(5) 0.0207(5) 0.0051(4) -0.0018(4) -0.0075(4) _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 Cu1 S2 2.2844(14) . ? Cu1 S3 2.3058(11) . ? Cu1 S1 2.3072(12) . ? Cu1 S3 2.4938(11) 2_666 ? Cu1 Cu1 2.7769(10) 2_666 ? Cu2 S5 2.2869(14) . ? Cu2 S6 2.3053(11) . ? Cu2 S4 2.3068(14) . ? Cu2 S6 2.4894(12) 2_755 ? Cu2 Cu2 2.7725(10) 2_755 ? C1 N1 1.344(6) . ? C1 C2 1.404(6) . ? C1 S1 1.731(4) . ? C2 C3 1.363(6) . ? C2 H2 0.9500 . ? C3 C4 1.399(7) . ? C3 H3 0.9500 . ? C4 C5 1.332(8) . ? C4 H4 0.9500 . ? C5 N1 1.357(6) . ? C5 H5 0.9500 . ? C6 N2 1.357(6) . ? C6 C7 1.402(6) . ? C6 S2 1.706(5) . ? C7 C8 1.359(7) . ? C7 H7 0.9500 . ? C8 C9 1.395(8) . ? C8 H8 0.9500 . ? C9 C10 1.330(8) . ? C9 H9 0.9500 . ? C10 N2 1.349(7) . ? C10 H10 0.9500 . ? C11 N3 1.375(6) . ? C11 C12 1.392(6) . ? C11 S3 1.711(5) . ? C12 C13 1.386(7) . ? C12 H12 0.9500 . ? C13 C14 1.417(8) . ? C13 H13 0.9500 . ? C14 C15 1.339(9) . ? C14 H14 0.9500 . ? C15 N3 1.356(7) . ? C15 H15 0.9500 . ? C16 N4 1.357(6) . ? C16 C17 1.404(6) . ? C16 S4 1.722(4) . ? C17 C18 1.375(6) . ? C17 H17 0.9500 . ? C18 C19 1.402(7) . ? C18 H18 0.9500 . ? C19 C20 1.361(8) . ? C19 H19 0.9500 . ? C20 N4 1.358(6) . ? C20 H20 0.9500 . ? C21 N5 1.341(7) . ? C21 C22 1.396(7) . ? C21 S5 1.710(5) . ? C22 C23 1.366(7) . ? C22 H22 0.9500 . ? C23 C24 1.392(8) . ? C23 H23 0.9500 . ? C24 C25 1.317(9) . ? C24 H24 0.9500 . ? C25 N5 1.352(7) . ? C25 H25 0.9500 . ? C26 N6 1.360(6) . ? C26 C27 1.377(7) . ? C26 S6 1.720(5) . ? C27 C28 1.393(8) . ? C27 H27 0.9500 . ? C28 C29 1.371(9) . ? C28 H28 0.9500 . ? C29 C30 1.329(10) . ? C29 H29 0.9500 . ? C30 N6 1.352(8) . ? C30 H30 0.9500 . ? N1 H1 0.8800 . ? N2 H2A 0.8800 . ? N3 H3A 0.8800 . ? N4 H4A 0.8800 . ? N5 H5A 0.8800 . ? N6 H6 0.8800 . ? S3 Cu1 2.4938(11) 2_666 ? S6 Cu2 2.4894(12) 2_755 ? 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 S2 Cu1 S3 104.01(4) . . ? S2 Cu1 S1 124.13(5) . . ? S3 Cu1 S1 115.95(5) . . ? S2 Cu1 S3 107.28(4) . 2_666 ? S3 Cu1 S3 109.42(3) . 2_666 ? S1 Cu1 S3 94.87(4) . 2_666 ? S2 Cu1 Cu1 117.89(4) . 2_666 ? S3 Cu1 Cu1 57.88(3) . 2_666 ? S1 Cu1 Cu1 116.07(4) . 2_666 ? S3 Cu1 Cu1 51.54(3) 2_666 2_666 ? S5 Cu2 S6 103.19(4) . . ? S5 Cu2 S4 124.21(5) . . ? S6 Cu2 S4 116.10(5) . . ? S5 Cu2 S6 107.24(5) . 2_755 ? S6 Cu2 S6 109.47(4) . 2_755 ? S4 Cu2 S6 95.62(4) . 2_755 ? S5 Cu2 Cu2 117.12(5) . 2_755 ? S6 Cu2 Cu2 57.84(3) . 2_755 ? S4 Cu2 Cu2 116.99(4) . 2_755 ? S6 Cu2 Cu2 51.63(3) 2_755 2_755 ? N1 C1 C2 117.1(4) . . ? N1 C1 S1 117.9(3) . . ? C2 C1 S1 125.0(3) . . ? C3 C2 C1 120.0(4) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.0(5) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 119.5(4) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 N1 119.8(5) . . ? C4 C5 H5 120.1 . . ? N1 C5 H5 120.1 . . ? N2 C6 C7 115.1(4) . . ? N2 C6 S2 119.1(4) . . ? C7 C6 S2 125.9(4) . . ? C8 C7 C6 121.4(5) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C7 C8 C9 120.4(5) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 118.1(5) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? C9 C10 N2 121.1(5) . . ? C9 C10 H10 119.4 . . ? N2 C10 H10 119.4 . . ? N3 C11 C12 117.0(4) . . ? N3 C11 S3 120.0(4) . . ? C12 C11 S3 123.1(3) . . ? C13 C12 C11 120.4(5) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 119.6(5) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C15 C14 C13 119.3(5) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C15 N3 120.3(5) . . ? C14 C15 H15 119.9 . . ? N3 C15 H15 119.9 . . ? N4 C16 C17 117.4(4) . . ? N4 C16 S4 117.5(3) . . ? C17 C16 S4 125.1(4) . . ? C18 C17 C16 119.5(5) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 121.1(5) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C20 C19 C18 118.2(5) . . ? C20 C19 H19 120.9 . . ? C18 C19 H19 120.9 . . ? N4 C20 C19 120.2(5) . . ? N4 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? N5 C21 C22 115.4(4) . . ? N5 C21 S5 119.2(4) . . ? C22 C21 S5 125.3(4) . . ? C23 C22 C21 120.9(5) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 120.1(5) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 118.5(5) . . ? C25 C24 H24 120.8 . . ? C23 C24 H24 120.8 . . ? C24 C25 N5 120.9(6) . . ? C24 C25 H25 119.5 . . ? N5 C25 H25 119.5 . . ? N6 C26 C27 116.0(4) . . ? N6 C26 S6 120.7(4) . . ? C27 C26 S6 123.2(4) . . ? C26 C27 C28 120.2(5) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 119.9(6) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C30 C29 C28 120.3(6) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 N6 118.8(6) . . ? C29 C30 H30 120.6 . . ? N6 C30 H30 120.6 . . ? C1 N1 C5 123.6(4) . . ? C1 N1 H1 118.2 . . ? C5 N1 H1 118.2 . . ? C10 N2 C6 124.0(5) . . ? C10 N2 H2A 118.0 . . ? C6 N2 H2A 118.0 . . ? C15 N3 C11 123.5(5) . . ? C15 N3 H3A 118.2 . . ? C11 N3 H3A 118.2 . . ? C16 N4 C20 123.5(4) . . ? C16 N4 H4A 118.3 . . ? C20 N4 H4A 118.3 . . ? C21 N5 C25 124.1(5) . . ? C21 N5 H5A 117.9 . . ? C25 N5 H5A 117.9 . . ? C30 N6 C26 124.7(5) . . ? C30 N6 H6 117.6 . . ? C26 N6 H6 117.6 . . ? C1 S1 Cu1 107.85(15) . . ? C6 S2 Cu1 105.84(16) . . ? C11 S3 Cu1 112.52(15) . . ? C11 S3 Cu1 102.61(14) . 2_666 ? Cu1 S3 Cu1 70.58(3) . 2_666 ? C16 S4 Cu2 107.75(16) . . ? C21 S5 Cu2 106.00(16) . . ? C26 S6 Cu2 112.27(16) . . ? C26 S6 Cu2 102.86(14) . 2_755 ? Cu2 S6 Cu2 70.53(4) . 2_755 ? 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 N1 C1 C2 C3 -0.8(6) . . . . ? S1 C1 C2 C3 176.7(3) . . . . ? C1 C2 C3 C4 0.8(7) . . . . ? C2 C3 C4 C5 -0.3(7) . . . . ? C3 C4 C5 N1 -0.1(8) . . . . ? N2 C6 C7 C8 0.9(6) . . . . ? S2 C6 C7 C8 -178.6(4) . . . . ? C6 C7 C8 C9 -0.3(7) . . . . ? C7 C8 C9 C10 -0.9(8) . . . . ? C8 C9 C10 N2 1.4(8) . . . . ? N3 C11 C12 C13 -0.4(6) . . . . ? S3 C11 C12 C13 178.8(3) . . . . ? C11 C12 C13 C14 0.4(7) . . . . ? C12 C13 C14 C15 -0.2(8) . . . . ? C13 C14 C15 N3 0.0(8) . . . . ? N4 C16 C17 C18 -1.8(6) . . . . ? S4 C16 C17 C18 176.7(3) . . . . ? C16 C17 C18 C19 0.7(7) . . . . ? C17 C18 C19 C20 0.4(7) . . . . ? C18 C19 C20 N4 -0.5(8) . . . . ? N5 C21 C22 C23 -0.8(7) . . . . ? S5 C21 C22 C23 -179.5(4) . . . . ? C21 C22 C23 C24 1.4(7) . . . . ? C22 C23 C24 C25 -1.2(8) . . . . ? C23 C24 C25 N5 0.4(9) . . . . ? N6 C26 C27 C28 -0.5(6) . . . . ? S6 C26 C27 C28 178.1(3) . . . . ? C26 C27 C28 C29 0.5(7) . . . . ? C27 C28 C29 C30 1.0(9) . . . . ? C28 C29 C30 N6 -2.5(9) . . . . ? C2 C1 N1 C5 0.4(6) . . . . ? S1 C1 N1 C5 -177.3(4) . . . . ? C4 C5 N1 C1 0.0(7) . . . . ? C9 C10 N2 C6 -0.8(8) . . . . ? C7 C6 N2 C10 -0.4(7) . . . . ? S2 C6 N2 C10 179.2(4) . . . . ? C14 C15 N3 C11 -0.1(8) . . . . ? C12 C11 N3 C15 0.3(6) . . . . ? S3 C11 N3 C15 -179.0(4) . . . . ? C17 C16 N4 C20 1.7(7) . . . . ? S4 C16 N4 C20 -176.8(4) . . . . ? C19 C20 N4 C16 -0.6(8) . . . . ? C22 C21 N5 C25 0.0(7) . . . . ? S5 C21 N5 C25 178.8(4) . . . . ? C24 C25 N5 C21 0.2(9) . . . . ? C29 C30 N6 C26 2.6(8) . . . . ? C27 C26 N6 C30 -1.1(7) . . . . ? S6 C26 N6 C30 -179.7(4) . . . . ? N1 C1 S1 Cu1 -146.0(3) . . . . ? C2 C1 S1 Cu1 36.5(4) . . . . ? S2 Cu1 S1 C1 -57.12(17) . . . . ? S3 Cu1 S1 C1 73.81(17) . . . . ? S3 Cu1 S1 C1 -171.82(16) 2_666 . . . ? Cu1 Cu1 S1 C1 138.96(16) 2_666 . . . ? N2 C6 S2 Cu1 -151.5(3) . . . . ? C7 C6 S2 Cu1 28.1(4) . . . . ? S3 Cu1 S2 C6 169.76(15) . . . . ? S1 Cu1 S2 C6 -54.69(16) . . . . ? S3 Cu1 S2 C6 53.87(16) 2_666 . . . ? Cu1 Cu1 S2 C6 108.96(15) 2_666 . . . ? N3 C11 S3 Cu1 7.0(4) . . . . ? C12 C11 S3 Cu1 -172.3(3) . . . . ? N3 C11 S3 Cu1 -67.0(3) . . . 2_666 ? C12 C11 S3 Cu1 113.8(3) . . . 2_666 ? S2 Cu1 S3 C11 149.63(15) . . . . ? S1 Cu1 S3 C11 9.76(15) . . . . ? S3 Cu1 S3 C11 -96.00(15) 2_666 . . . ? Cu1 Cu1 S3 C11 -96.00(15) 2_666 . . . ? S2 Cu1 S3 Cu1 -114.37(4) . . . 2_666 ? S1 Cu1 S3 Cu1 105.76(5) . . . 2_666 ? S3 Cu1 S3 Cu1 0.0 2_666 . . 2_666 ? N4 C16 S4 Cu2 -146.5(3) . . . . ? C17 C16 S4 Cu2 35.0(4) . . . . ? S5 Cu2 S4 C16 -55.51(17) . . . . ? S6 Cu2 S4 C16 74.31(17) . . . . ? S6 Cu2 S4 C16 -170.79(16) 2_755 . . . ? Cu2 Cu2 S4 C16 139.75(16) 2_755 . . . ? N5 C21 S5 Cu2 -150.7(3) . . . . ? C22 C21 S5 Cu2 28.0(4) . . . . ? S6 Cu2 S5 C21 169.80(18) . . . . ? S4 Cu2 S5 C21 -55.31(19) . . . . ? S6 Cu2 S5 C21 54.26(18) 2_755 . . . ? Cu2 Cu2 S5 C21 109.42(18) 2_755 . . . ? N6 C26 S6 Cu2 5.7(4) . . . . ? C27 C26 S6 Cu2 -172.8(3) . . . . ? N6 C26 S6 Cu2 -68.3(3) . . . 2_755 ? C27 C26 S6 Cu2 113.2(3) . . . 2_755 ? S5 Cu2 S6 C26 149.73(15) . . . . ? S4 Cu2 S6 C26 10.46(15) . . . . ? S6 Cu2 S6 C26 -96.33(15) 2_755 . . . ? Cu2 Cu2 S6 C26 -96.33(15) 2_755 . . . ? S5 Cu2 S6 Cu2 -113.94(5) . . . 2_755 ? S4 Cu2 S6 Cu2 106.79(5) . . . 2_755 ? S6 Cu2 S6 Cu2 0.0 2_755 . . 2_755 ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 26.48 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.853 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.157 _chemical_name_common ; bis(mu-Pyridine-2(1H)-thione-k2S:S)-tetrakis(pyridine-2(1H)- thione-S) dicopper(i) sulphate - ethanol (1/5) ; #===END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 741280' _chemical_name_systematic ; hexaaquacopper(II) catena-dodekakis(mu-Pyridine-2(1H)-thione-k2S:S)- hexacopper(i) di(sulphate) - water (1/4) ; _chemical_melting_point ? _chemical_formula_moiety '2(C30 H30 Cu3 N6 S6), Cu H12 O6, 4(O4 S), 4(H2 O)' _chemical_formula_sum 'C60 H80 Cu7 N12 O26 S16' _chemical_formula_iupac '[Cu(H2O)6][Cu6(mu-C5H5NS)12](SO4)4.4H2O' _chemical_formula_weight 2343.10 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 orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.7630(13) _cell_length_b 20.5969(17) _cell_length_c 29.110(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8851.6(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 74682 _cell_measurement_theta_min 1.40 _cell_measurement_theta_max 25.78 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4764 _exptl_absorpt_coefficient_mu 2.105 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'CrysAlis RED (Oxford Diffraction, 2003)' _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.887 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _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_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 74682 _diffrn_reflns_av_R_equivalents 0.1062 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 25.78 _reflns_number_total 8481 _reflns_number_gt 5688 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Sir92 (Altamore et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0648P)^2^+5.1619P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8481 _refine_ls_number_parameters 546 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0835 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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 Cu1 Cu 0.55406(4) 0.13670(3) 0.27402(2) 0.01387(16) Uani 1 1 d . . . Cu2 Cu 0.37934(4) 0.14167(3) 0.27309(2) 0.01354(16) Uani 1 1 d . . . Cu3 Cu 0.21472(4) 0.12436(3) 0.25440(2) 0.01349(16) Uani 1 1 d . . . S1 S 0.46863(9) 0.22242(6) 0.23779(4) 0.0140(3) Uani 1 1 d . . . S2 S 0.46374(9) 0.09591(6) 0.33289(4) 0.0155(3) Uani 1 1 d . . . S3 S 0.32962(8) 0.06671(6) 0.21752(4) 0.0143(3) Uani 1 1 d . . . S4 S 0.26032(8) 0.20805(6) 0.30459(4) 0.0126(3) Uani 1 1 d . . . S5 S 0.09485(8) 0.06348(6) 0.28361(4) 0.0130(3) Uani 1 1 d . . . S6 S 0.17296(8) 0.20357(6) 0.19652(4) 0.0134(3) Uani 1 1 d . . . C1 C 0.4727(3) 0.2166(2) 0.17926(19) 0.0164(11) Uani 1 1 d . . . C2 C 0.4853(4) 0.2714(3) 0.1507(2) 0.0301(15) Uani 1 1 d . . . H2 H 0.4897 0.3135 0.1639 0.036 Uiso 1 1 calc R . . C3 C 0.4911(5) 0.2639(3) 0.1043(2) 0.048(2) Uani 1 1 d . . . H3 H 0.4991 0.3011 0.0855 0.057 Uiso 1 1 calc R . . C4 C 0.4856(5) 0.2033(3) 0.0839(2) 0.0439(19) Uani 1 1 d . . . H4 H 0.4913 0.1985 0.0516 0.053 Uiso 1 1 calc R . . C5 C 0.4717(4) 0.1510(3) 0.1114(2) 0.0281(14) Uani 1 1 d . . . H5 H 0.4661 0.1090 0.0983 0.034 Uiso 1 1 calc R . . C6 C 0.4658(3) 0.1554(3) 0.37460(18) 0.0175(11) Uani 1 1 d . . . C7 C 0.4750(3) 0.2217(3) 0.3675(2) 0.0210(12) Uani 1 1 d . . . H7 H 0.4779 0.2383 0.3371 0.025 Uiso 1 1 calc R . . C8 C 0.4798(4) 0.2632(3) 0.4038(2) 0.0287(14) Uani 1 1 d . . . H8 H 0.4875 0.3084 0.3985 0.034 Uiso 1 1 calc R . . C9 C 0.4738(5) 0.2403(3) 0.4486(2) 0.0460(19) Uani 1 1 d . . . H9A H 0.4773 0.2693 0.4739 0.055 Uiso 1 1 calc R . . C10 C 0.4629(5) 0.1763(3) 0.4552(2) 0.0473(19) Uani 1 1 d . . . H10A H 0.4578 0.1594 0.4855 0.057 Uiso 1 1 calc R . . C11 C 0.3504(3) -0.0110(2) 0.23879(17) 0.0127(11) Uani 1 1 d . . . C12 C 0.3472(3) -0.0290(2) 0.28457(18) 0.0160(11) Uani 1 1 d . . . H12 H 0.3329 0.0024 0.3073 0.019 Uiso 1 1 calc R . . C13 C 0.3648(4) -0.0926(2) 0.2975(2) 0.0205(12) Uani 1 1 d . . . H13 H 0.3629 -0.1045 0.3290 0.025 Uiso 1 1 calc R . . C14 C 0.3852(4) -0.1389(3) 0.2641(2) 0.0243(13) Uani 1 1 d . . . H14 H 0.3974 -0.1826 0.2725 0.029 Uiso 1 1 calc R . . C15 C 0.3871(4) -0.1199(3) 0.2196(2) 0.0229(13) Uani 1 1 d . . . H15 H 0.4008 -0.1507 0.1963 0.027 Uiso 1 1 calc R . . C16 C 0.2435(3) 0.1849(2) 0.36088(17) 0.0137(11) Uani 1 1 d . . . C17 C 0.2326(4) 0.1212(2) 0.37656(18) 0.0177(12) Uani 1 1 d . . . H17 H 0.2343 0.0862 0.3553 0.021 Uiso 1 1 calc R . . C18 C 0.2193(4) 0.1086(3) 0.42228(19) 0.0275(14) Uani 1 1 d . . . H18 H 0.2120 0.0651 0.4325 0.033 Uiso 1 1 calc R . . C19 C 0.2166(4) 0.1595(3) 0.4540(2) 0.0316(15) Uani 1 1 d . . . H19 H 0.2070 0.1514 0.4857 0.038 Uiso 1 1 calc R . . C20 C 0.2281(4) 0.2207(3) 0.43807(18) 0.0266(14) Uani 1 1 d . . . H20 H 0.2271 0.2562 0.4589 0.032 Uiso 1 1 calc R . . C21 C 0.1134(3) -0.0138(2) 0.26074(17) 0.0123(11) Uani 1 1 d . . . C22 C 0.1167(3) -0.0284(3) 0.21421(19) 0.0188(12) Uani 1 1 d . . . H22 H 0.1029 0.0041 0.1921 0.023 Uiso 1 1 calc R . . C23 C 0.1398(3) -0.0897(2) 0.20019(19) 0.0198(12) Uani 1 1 d . . . H23 H 0.1433 -0.0993 0.1683 0.024 Uiso 1 1 calc R . . C24 C 0.1581(4) -0.1377(2) 0.2320(2) 0.0217(13) Uani 1 1 d . . . H24 H 0.1754 -0.1799 0.2222 0.026 Uiso 1 1 calc R . . C25 C 0.1509(4) -0.1235(2) 0.2775(2) 0.0202(12) Uani 1 1 d . . . H25 H 0.1614 -0.1563 0.2998 0.024 Uiso 1 1 calc R . . C26 C 0.1978(3) 0.1786(2) 0.14159(17) 0.0133(11) Uani 1 1 d . . . C27 C 0.1980(3) 0.1145(2) 0.12531(18) 0.0175(12) Uani 1 1 d . . . H27 H 0.1837 0.0801 0.1458 0.021 Uiso 1 1 calc R . . C28 C 0.2183(4) 0.1005(3) 0.08047(19) 0.0228(13) Uani 1 1 d . . . H28 H 0.2176 0.0568 0.0701 0.027 Uiso 1 1 calc R . . C29 C 0.2402(4) 0.1507(3) 0.0500(2) 0.0305(15) Uani 1 1 d . . . H29 H 0.2550 0.1417 0.0189 0.037 Uiso 1 1 calc R . . C30 C 0.2395(4) 0.2127(3) 0.0660(2) 0.0315(15) Uani 1 1 d . . . H30 H 0.2531 0.2477 0.0459 0.038 Uiso 1 1 calc R . . N1 N 0.4658(3) 0.1591(2) 0.15742(15) 0.0196(10) Uani 1 1 d . . . H1N H 0.4568 0.1243 0.1743 0.023 Uiso 1 1 calc R . . N2 N 0.4593(3) 0.1355(2) 0.41850(16) 0.0280(12) Uani 1 1 d . . . H2N H 0.4522 0.0938 0.4238 0.034 Uiso 1 1 calc R . . N3 N 0.3700(3) -0.05814(19) 0.20801(16) 0.0173(10) Uani 1 1 d . . . H3N H 0.3715 -0.0477 0.1787 0.021 Uiso 1 1 calc R . . N4 N 0.2408(3) 0.2315(2) 0.39309(15) 0.0180(10) Uani 1 1 d . . . H4N H 0.2479 0.2720 0.3841 0.022 Uiso 1 1 calc R . . N5 N 0.1288(3) -0.06286(19) 0.29093(15) 0.0151(9) Uani 1 1 d . . . H5N H 0.1241 -0.0547 0.3205 0.018 Uiso 1 1 calc R . . N6 N 0.2196(3) 0.2248(2) 0.11055(15) 0.0192(10) Uani 1 1 d . . . H6N H 0.2210 0.2654 0.1199 0.023 Uiso 1 1 calc R . . S8 S 0.68605(10) 0.39513(6) 0.40938(5) 0.0204(3) Uani 1 1 d . . . O5 O 0.7361(3) 0.35427(17) 0.37670(13) 0.0245(9) Uani 1 1 d . . . O6 O 0.7483(3) 0.4364(2) 0.43564(16) 0.0355(11) Uani 1 1 d . . . O7 O 0.6227(3) 0.4379(2) 0.38420(14) 0.0409(12) Uani 1 1 d . . . O8 O 0.6344(3) 0.35399(17) 0.44094(12) 0.0213(9) Uani 1 1 d . . . O1W O 0.4247(3) 1.0106(2) 0.44663(17) 0.0473(13) Uani 1 1 d . . . H1A H 0.3801 0.9857 0.4410 0.071 Uiso 1 1 d . . . H1B H 0.4696 0.9814 0.4484 0.071 Uiso 1 1 d . . . O2W O 0.9256(4) 0.4317(3) 0.4627(2) 0.0706(17) Uani 1 1 d . . . H2A H 0.9097 0.4479 0.4887 0.106 Uiso 1 1 d . . . H2B H 0.8743 0.4277 0.4484 0.106 Uiso 1 1 d . . . Cu4 Cu 0.0000 0.0000 0.5000 0.0182(2) Uani 1 2 d S . . O3W O -0.0045(3) 0.10195(17) 0.50757(12) 0.0201(8) Uani 1 1 d . . . O4W O 0.0047(3) 0.00712(17) 0.42794(13) 0.0213(8) Uani 1 1 d . . . O5W O 0.1416(2) 0.00014(17) 0.50320(13) 0.0250(9) Uani 1 1 d . . . H3A H 0.0431 0.1217 0.5263 0.037 Uiso 1 1 d . . . H3B H -0.0470 0.1156 0.5249 0.037 Uiso 1 1 d . . . H4A H 0.0565 -0.0130 0.4141 0.037 Uiso 1 1 d . . . H4B H -0.0335 -0.0176 0.4146 0.037 Uiso 1 1 d . . . H5A H 0.1671 -0.0243 0.4843 0.037 Uiso 1 1 d . . . H5B H 0.1822 0.0231 0.5226 0.037 Uiso 1 1 d . . . S7 S 0.79376(10) 0.09434(7) 0.58992(6) 0.0282(4) Uani 1 1 d . . . O1 O 0.8541(3) 0.0505(2) 0.61552(14) 0.0411(12) Uani 1 1 d . A . O2A O 0.7362(4) 0.1374(3) 0.6164(2) 0.0207(14) Uiso 0.623(4) 1 d P A 1 O3A O 0.7363(4) 0.0557(3) 0.5566(2) 0.0302(17) Uiso 0.623(4) 1 d P A 1 O4A O 0.8481(4) 0.1399(3) 0.5562(2) 0.0228(15) Uiso 0.623(4) 1 d P A 1 O2B O 0.7863(7) 0.1461(4) 0.6251(3) 0.015(2) Uiso 0.377(4) 1 d P A 2 O3B O 0.7047(8) 0.0591(6) 0.5916(4) 0.041(3) Uiso 0.377(4) 1 d P A 2 O4B O 0.8272(7) 0.1071(5) 0.5495(3) 0.019(2) Uiso 0.377(4) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0137(3) 0.0113(3) 0.0167(3) -0.0016(3) 0.0004(2) 0.0009(2) Cu2 0.0132(3) 0.0107(3) 0.0166(3) -0.0015(3) -0.0006(3) -0.0013(2) Cu3 0.0134(3) 0.0094(3) 0.0177(3) -0.0014(3) -0.0018(3) 0.0004(2) S1 0.0151(6) 0.0100(6) 0.0170(7) 0.0014(5) 0.0002(5) 0.0000(5) S2 0.0191(6) 0.0122(6) 0.0153(7) -0.0007(5) 0.0004(5) -0.0009(5) S3 0.0169(7) 0.0092(6) 0.0169(7) -0.0033(5) -0.0009(5) 0.0008(5) S4 0.0194(7) 0.0073(6) 0.0111(6) -0.0002(5) 0.0015(5) -0.0001(5) S5 0.0167(6) 0.0076(6) 0.0147(7) 0.0010(5) 0.0014(5) 0.0006(5) S6 0.0187(7) 0.0089(6) 0.0125(6) 0.0009(5) 0.0020(5) 0.0006(5) C1 0.014(3) 0.015(3) 0.021(3) -0.001(2) 0.000(2) 0.003(2) C2 0.057(4) 0.013(3) 0.021(3) 0.000(2) 0.000(3) -0.006(3) C3 0.091(6) 0.025(4) 0.027(4) 0.011(3) 0.000(4) -0.007(4) C4 0.082(6) 0.035(4) 0.015(3) 0.005(3) 0.000(3) 0.002(4) C5 0.040(4) 0.022(3) 0.022(3) -0.005(3) -0.004(3) 0.007(3) C6 0.013(3) 0.024(3) 0.016(3) -0.002(2) -0.002(2) -0.001(2) C7 0.014(3) 0.025(3) 0.024(3) -0.004(3) 0.000(2) -0.004(2) C8 0.034(4) 0.015(3) 0.037(4) -0.012(3) 0.003(3) -0.005(3) C9 0.077(6) 0.036(4) 0.025(4) -0.012(3) -0.003(3) -0.013(4) C10 0.080(6) 0.046(5) 0.016(3) -0.003(3) -0.003(3) -0.009(4) C11 0.010(2) 0.011(3) 0.018(3) -0.002(2) 0.000(2) 0.000(2) C12 0.016(3) 0.011(3) 0.021(3) -0.005(2) 0.000(2) -0.002(2) C13 0.021(3) 0.016(3) 0.025(3) 0.003(2) -0.003(2) 0.003(2) C14 0.020(3) 0.012(3) 0.041(4) 0.000(3) -0.003(3) 0.006(2) C15 0.019(3) 0.015(3) 0.034(4) -0.011(3) -0.003(2) 0.007(2) C16 0.017(3) 0.012(3) 0.013(3) -0.002(2) 0.000(2) 0.000(2) C17 0.025(3) 0.009(3) 0.019(3) -0.002(2) -0.001(2) -0.003(2) C18 0.044(4) 0.019(3) 0.019(3) 0.008(3) 0.001(3) -0.010(3) C19 0.056(4) 0.028(3) 0.012(3) -0.001(3) 0.008(3) -0.012(3) C20 0.047(4) 0.022(3) 0.011(3) -0.006(2) 0.007(3) -0.005(3) C21 0.012(3) 0.008(2) 0.017(3) 0.003(2) 0.000(2) -0.002(2) C22 0.015(3) 0.016(3) 0.026(3) 0.000(2) 0.000(2) -0.002(2) C23 0.017(3) 0.017(3) 0.026(3) -0.008(2) 0.004(2) -0.005(2) C24 0.016(3) 0.009(3) 0.040(4) -0.003(3) 0.005(2) -0.004(2) C25 0.019(3) 0.009(3) 0.033(3) 0.003(2) 0.003(2) -0.002(2) C26 0.009(2) 0.014(3) 0.017(3) -0.001(2) 0.001(2) 0.005(2) C27 0.020(3) 0.013(3) 0.020(3) 0.000(2) 0.001(2) 0.001(2) C28 0.031(3) 0.014(3) 0.024(3) -0.003(2) -0.001(3) 0.005(2) C29 0.051(4) 0.027(4) 0.013(3) 0.002(3) 0.007(3) 0.014(3) C30 0.055(4) 0.024(3) 0.016(3) 0.006(3) 0.010(3) 0.007(3) N1 0.030(3) 0.011(2) 0.018(2) 0.0067(19) -0.002(2) 0.005(2) N2 0.044(3) 0.024(3) 0.016(3) 0.002(2) -0.001(2) -0.003(2) N3 0.016(2) 0.012(2) 0.024(3) -0.0051(19) 0.0028(19) 0.0015(18) N4 0.027(3) 0.013(2) 0.014(2) -0.0022(19) 0.0043(19) -0.0048(19) N5 0.021(2) 0.007(2) 0.017(2) 0.0026(18) 0.0046(19) 0.0003(18) N6 0.033(3) 0.011(2) 0.013(2) 0.0022(19) 0.005(2) 0.005(2) S8 0.0285(8) 0.0147(7) 0.0181(7) 0.0014(6) 0.0045(6) -0.0003(6) O5 0.037(2) 0.015(2) 0.022(2) 0.0015(16) 0.0119(18) 0.0044(17) O6 0.030(2) 0.025(2) 0.052(3) -0.019(2) 0.004(2) -0.0106(19) O7 0.061(3) 0.041(3) 0.020(2) 0.012(2) 0.007(2) 0.030(2) O8 0.029(2) 0.0140(19) 0.020(2) -0.0007(16) 0.0042(17) -0.0028(16) O1W 0.044(3) 0.043(3) 0.054(3) 0.013(2) -0.007(2) -0.008(2) O2W 0.057(4) 0.090(5) 0.065(4) 0.013(3) -0.005(3) 0.002(3) Cu4 0.0294(5) 0.0119(5) 0.0133(5) -0.0017(4) 0.0030(4) -0.0038(4) O3W 0.027(2) 0.0138(19) 0.019(2) -0.0022(16) 0.0039(17) 0.0007(16) O4W 0.032(2) 0.015(2) 0.017(2) -0.0016(16) 0.0033(17) 0.0000(17) O5W 0.028(2) 0.019(2) 0.028(2) -0.0110(17) 0.0069(18) -0.0021(17) S7 0.0259(8) 0.0205(8) 0.0381(9) -0.0159(7) 0.0043(7) 0.0021(6) O1 0.054(3) 0.049(3) 0.021(2) -0.003(2) 0.003(2) 0.022(2) _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 Cu1 S2 2.3282(14) . ? Cu1 S5 2.3351(14) 6_656 ? Cu1 S6 2.3901(14) 6_656 ? Cu1 S1 2.4126(14) . ? Cu1 Cu3 2.5248(9) 6_656 ? Cu1 Cu2 2.5815(8) . ? Cu2 S2 2.3390(14) . ? Cu2 S3 2.3534(14) . ? Cu2 S1 2.3579(14) . ? Cu2 S4 2.4079(14) . ? Cu2 Cu3 2.5159(9) . ? Cu3 S5 2.3298(14) . ? Cu3 S3 2.3324(14) . ? Cu3 S4 2.3577(14) . ? Cu3 S6 2.4248(14) . ? Cu3 Cu1 2.5248(9) 6_556 ? S1 C1 1.709(6) . ? S2 C6 1.725(5) . ? S3 C11 1.743(5) . ? S4 C16 1.724(5) . ? S5 C21 1.748(5) . ? S5 Cu1 2.3351(14) 6_556 ? S6 C26 1.719(5) . ? S6 Cu1 2.3901(14) 6_556 ? C1 N1 1.348(7) . ? C1 C2 1.414(8) . ? C2 C3 1.363(9) . ? C2 H2 0.9500 . ? C3 C4 1.384(9) . ? C3 H3 0.9500 . ? C4 C5 1.357(9) . ? C4 H4 0.9500 . ? C5 N1 1.354(7) . ? C5 H5 0.9500 . ? C6 N2 1.345(7) . ? C6 C7 1.389(7) . ? C7 C8 1.361(8) . ? C7 H7 0.9500 . ? C8 C9 1.388(9) . ? C8 H8 0.9500 . ? C9 C10 1.343(9) . ? C9 H9A 0.9500 . ? C10 N2 1.360(8) . ? C10 H10A 0.9500 . ? C11 N3 1.353(6) . ? C11 C12 1.384(7) . ? C12 C13 1.387(7) . ? C12 H12 0.9500 . ? C13 C14 1.393(8) . ? C13 H13 0.9500 . ? C14 C15 1.355(8) . ? C14 H14 0.9500 . ? C15 N3 1.340(7) . ? C15 H15 0.9500 . ? C16 N4 1.343(6) . ? C16 C17 1.400(7) . ? C17 C18 1.370(7) . ? C17 H17 0.9500 . ? C18 C19 1.397(8) . ? C18 H18 0.9500 . ? C19 C20 1.355(8) . ? C19 H19 0.9500 . ? C20 N4 1.342(7) . ? C20 H20 0.9500 . ? C21 N5 1.358(6) . ? C21 C22 1.388(7) . ? C22 C23 1.372(7) . ? C22 H22 0.9500 . ? C23 C24 1.379(8) . ? C23 H23 0.9500 . ? C24 C25 1.363(8) . ? C24 H24 0.9500 . ? C25 N5 1.348(6) . ? C25 H25 0.9500 . ? C26 N6 1.351(6) . ? C26 C27 1.403(7) . ? C27 C28 1.370(7) . ? C27 H27 0.9500 . ? C28 C29 1.401(8) . ? C28 H28 0.9500 . ? C29 C30 1.360(8) . ? C29 H29 0.9500 . ? C30 N6 1.353(7) . ? C30 H30 0.9500 . ? N1 H1N 0.8800 . ? N2 H2N 0.8800 . ? N3 H3N 0.8800 . ? N4 H4N 0.8800 . ? N5 H5N 0.8800 . ? N6 H6N 0.8800 . ? S8 O8 1.464(4) . ? S8 O6 1.467(4) . ? S8 O5 1.470(4) . ? S8 O7 1.479(4) . ? O1W H1A 0.8514 . ? O1W H1B 0.8955 . ? O2W H2A 0.8594 . ? O2W H2B 0.8677 . ? Cu4 O5W 2.093(4) 5_556 ? Cu4 O5W 2.093(4) . ? Cu4 O4W 2.104(4) . ? Cu4 O4W 2.104(4) 5_556 ? Cu4 O3W 2.112(3) 5_556 ? Cu4 O3W 2.112(3) . ? O3W H3A 0.9779 . ? O3W H3B 0.8522 . ? O4W H4A 0.9583 . ? O4W H4B 0.8539 . ? O5W H5A 0.8354 . ? O5W H5B 0.9494 . ? S7 O4B 1.303(10) . ? S7 O2A 1.450(6) . ? S7 O1 1.471(5) . ? S7 O2B 1.483(9) . ? S7 O3B 1.503(12) . ? S7 O3A 1.514(7) . ? S7 O4A 1.577(7) . ? 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 S2 Cu1 S5 116.32(5) . 6_656 ? S2 Cu1 S6 111.38(5) . 6_656 ? S5 Cu1 S6 116.14(5) 6_656 6_656 ? S2 Cu1 S1 106.65(5) . . ? S5 Cu1 S1 107.06(5) 6_656 . ? S6 Cu1 S1 96.84(5) 6_656 . ? S2 Cu1 Cu3 137.98(4) . 6_656 ? S5 Cu1 Cu3 57.13(4) 6_656 6_656 ? S6 Cu1 Cu3 59.05(4) 6_656 6_656 ? S1 Cu1 Cu3 114.93(4) . 6_656 ? S2 Cu1 Cu2 56.62(4) . . ? S5 Cu1 Cu2 106.00(4) 6_656 . ? S6 Cu1 Cu2 135.62(4) 6_656 . ? S1 Cu1 Cu2 56.22(4) . . ? Cu3 Cu1 Cu2 159.91(3) 6_656 . ? S2 Cu2 S3 114.41(5) . . ? S2 Cu2 S1 108.11(5) . . ? S3 Cu2 S1 109.73(5) . . ? S2 Cu2 S4 109.52(5) . . ? S3 Cu2 S4 113.99(5) . . ? S1 Cu2 S4 99.98(5) . . ? S2 Cu2 Cu3 128.20(4) . . ? S3 Cu2 Cu3 57.12(4) . . ? S1 Cu2 Cu3 123.07(4) . . ? S4 Cu2 Cu3 57.17(4) . . ? S2 Cu2 Cu1 56.22(4) . . ? S3 Cu2 Cu1 107.03(4) . . ? S1 Cu2 Cu1 58.26(4) . . ? S4 Cu2 Cu1 138.38(4) . . ? Cu3 Cu2 Cu1 164.13(3) . . ? S5 Cu3 S3 116.51(5) . . ? S5 Cu3 S4 112.60(5) . . ? S3 Cu3 S4 116.73(5) . . ? S5 Cu3 S6 115.00(5) . . ? S3 Cu3 S6 101.98(5) . . ? S4 Cu3 S6 90.65(5) . . ? S5 Cu3 Cu2 136.98(4) . . ? S3 Cu3 Cu2 57.93(4) . . ? S4 Cu3 Cu2 59.11(4) . . ? S6 Cu3 Cu2 107.49(4) . . ? S5 Cu3 Cu1 57.33(4) . 6_556 ? S3 Cu3 Cu1 125.71(4) . 6_556 ? S4 Cu3 Cu1 113.43(4) . 6_556 ? S6 Cu3 Cu1 57.71(4) . 6_556 ? Cu2 Cu3 Cu1 164.60(3) . 6_556 ? C1 S1 Cu2 113.89(18) . . ? C1 S1 Cu1 111.47(18) . . ? Cu2 S1 Cu1 65.51(4) . . ? C6 S2 Cu1 104.56(18) . . ? C6 S2 Cu2 104.32(18) . . ? Cu1 S2 Cu2 67.16(4) . . ? C11 S3 Cu3 115.59(17) . . ? C11 S3 Cu2 107.65(17) . . ? Cu3 S3 Cu2 64.95(4) . . ? C16 S4 Cu3 110.22(18) . . ? C16 S4 Cu2 108.04(18) . . ? Cu3 S4 Cu2 63.72(4) . . ? C21 S5 Cu3 103.43(17) . . ? C21 S5 Cu1 110.80(17) . 6_556 ? Cu3 S5 Cu1 65.54(4) . 6_556 ? C26 S6 Cu1 108.53(18) . 6_556 ? C26 S6 Cu3 113.01(17) . . ? Cu1 S6 Cu3 63.25(4) 6_556 . ? N1 C1 C2 115.7(5) . . ? N1 C1 S1 121.9(4) . . ? C2 C1 S1 122.3(4) . . ? C3 C2 C1 120.0(5) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 121.6(6) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 118.2(6) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? N1 C5 C4 119.7(5) . . ? N1 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? N2 C6 C7 116.5(5) . . ? N2 C6 S2 116.9(4) . . ? C7 C6 S2 126.6(4) . . ? C8 C7 C6 120.5(6) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 120.9(6) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 118.4(6) . . ? C10 C9 H9A 120.8 . . ? C8 C9 H9A 120.8 . . ? C9 C10 N2 119.8(6) . . ? C9 C10 H10A 120.1 . . ? N2 C10 H10A 120.1 . . ? N3 C11 C12 116.9(4) . . ? N3 C11 S3 117.5(4) . . ? C12 C11 S3 125.6(4) . . ? C11 C12 C13 120.5(5) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C14 119.9(5) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 118.3(5) . . ? C15 C14 H14 120.9 . . ? C13 C14 H14 120.9 . . ? N3 C15 C14 120.7(5) . . ? N3 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? N4 C16 C17 116.1(5) . . ? N4 C16 S4 118.0(4) . . ? C17 C16 S4 125.9(4) . . ? C18 C17 C16 120.8(5) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 120.2(5) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 118.0(5) . . ? C20 C19 H19 121.0 . . ? C18 C19 H19 121.0 . . ? N4 C20 C19 120.4(5) . . ? N4 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? N5 C21 C22 117.8(4) . . ? N5 C21 S5 117.2(4) . . ? C22 C21 S5 125.0(4) . . ? C23 C22 C21 119.8(5) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.6(5) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C25 C24 C23 119.0(5) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? N5 C25 C24 119.9(5) . . ? N5 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? N6 C26 C27 115.9(5) . . ? N6 C26 S6 117.6(4) . . ? C27 C26 S6 126.6(4) . . ? C28 C27 C26 121.4(5) . . ? C28 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? C27 C28 C29 119.9(5) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 118.3(5) . . ? C30 C29 H29 120.8 . . ? C28 C29 H29 120.8 . . ? N6 C30 C29 120.2(5) . . ? N6 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C1 N1 C5 124.8(5) . . ? C1 N1 H1N 117.6 . . ? C5 N1 H1N 117.6 . . ? C6 N2 C10 123.8(5) . . ? C6 N2 H2N 118.1 . . ? C10 N2 H2N 118.1 . . ? C15 N3 C11 123.8(5) . . ? C15 N3 H3N 118.1 . . ? C11 N3 H3N 118.1 . . ? C20 N4 C16 124.5(5) . . ? C20 N4 H4N 117.7 . . ? C16 N4 H4N 117.7 . . ? C25 N5 C21 122.8(5) . . ? C25 N5 H5N 118.6 . . ? C21 N5 H5N 118.6 . . ? C26 N6 C30 124.3(5) . . ? C26 N6 H6N 117.8 . . ? C30 N6 H6N 117.8 . . ? O8 S8 O6 109.6(2) . . ? O8 S8 O5 109.7(2) . . ? O6 S8 O5 110.7(2) . . ? O8 S8 O7 109.0(2) . . ? O6 S8 O7 108.0(3) . . ? O5 S8 O7 109.8(2) . . ? H1A O1W H1B 100.4 . . ? H2A O2W H2B 102.8 . . ? O5W Cu4 O5W 180.0(2) 5_556 . ? O5W Cu4 O4W 89.36(15) 5_556 . ? O5W Cu4 O4W 90.64(15) . . ? O5W Cu4 O4W 90.64(15) 5_556 5_556 ? O5W Cu4 O4W 89.36(15) . 5_556 ? O4W Cu4 O4W 180.000(1) . 5_556 ? O5W Cu4 O3W 91.45(14) 5_556 5_556 ? O5W Cu4 O3W 88.55(14) . 5_556 ? O4W Cu4 O3W 87.95(14) . 5_556 ? O4W Cu4 O3W 92.05(14) 5_556 5_556 ? O5W Cu4 O3W 88.55(14) 5_556 . ? O5W Cu4 O3W 91.45(14) . . ? O4W Cu4 O3W 92.05(14) . . ? O4W Cu4 O3W 87.95(14) 5_556 . ? O3W Cu4 O3W 180.0(2) 5_556 . ? Cu4 O3W H3A 116.7 . . ? Cu4 O3W H3B 114.4 . . ? H3A O3W H3B 93.6 . . ? Cu4 O4W H4A 114.6 . . ? Cu4 O4W H4B 112.9 . . ? H4A O4W H4B 94.5 . . ? Cu4 O5W H5A 114.8 . . ? Cu4 O5W H5B 131.1 . . ? H5A O5W H5B 114.1 . . ? O4B S7 O1 110.6(5) . . ? O2A S7 O1 117.5(3) . . ? O4B S7 O2B 120.4(6) . . ? O1 S7 O2B 97.9(4) . . ? O4B S7 O3B 117.3(7) . . ? O1 S7 O3B 102.6(5) . . ? O2B S7 O3B 105.1(6) . . ? O2A S7 O3A 109.5(4) . . ? O1 S7 O3A 110.0(3) . . ? O2A S7 O4A 105.3(3) . . ? O1 S7 O4A 111.9(3) . . ? O3A S7 O4A 101.5(4) . . ? 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 S5 Cu1 Cu2 S2 111.32(6) 6_656 . . . ? S6 Cu1 Cu2 S2 -87.18(7) 6_656 . . . ? S1 Cu1 Cu2 S2 -148.59(6) . . . . ? Cu3 Cu1 Cu2 S2 142.05(10) 6_656 . . . ? S2 Cu1 Cu2 S3 -108.37(6) . . . . ? S5 Cu1 Cu2 S3 2.95(6) 6_656 . . . ? S6 Cu1 Cu2 S3 164.45(6) 6_656 . . . ? S1 Cu1 Cu2 S3 103.04(6) . . . . ? Cu3 Cu1 Cu2 S3 33.68(11) 6_656 . . . ? S2 Cu1 Cu2 S1 148.59(6) . . . . ? S5 Cu1 Cu2 S1 -100.10(5) 6_656 . . . ? S6 Cu1 Cu2 S1 61.41(7) 6_656 . . . ? Cu3 Cu1 Cu2 S1 -69.36(10) 6_656 . . . ? S2 Cu1 Cu2 S4 81.50(7) . . . . ? S5 Cu1 Cu2 S4 -167.18(6) 6_656 . . . ? S6 Cu1 Cu2 S4 -5.68(10) 6_656 . . . ? S1 Cu1 Cu2 S4 -67.09(7) . . . . ? Cu3 Cu1 Cu2 S4 -136.45(9) 6_656 . . . ? S2 Cu1 Cu2 Cu3 -111.57(13) . . . . ? S5 Cu1 Cu2 Cu3 -0.26(14) 6_656 . . . ? S6 Cu1 Cu2 Cu3 161.25(11) 6_656 . . . ? S1 Cu1 Cu2 Cu3 99.84(13) . . . . ? Cu3 Cu1 Cu2 Cu3 30.48(18) 6_656 . . . ? S2 Cu2 Cu3 S5 -0.97(9) . . . . ? S3 Cu2 Cu3 S5 95.78(7) . . . . ? S1 Cu2 Cu3 S5 -170.85(6) . . . . ? S4 Cu2 Cu3 S5 -90.87(7) . . . . ? Cu1 Cu2 Cu3 S5 99.43(13) . . . . ? S2 Cu2 Cu3 S3 -96.75(6) . . . . ? S1 Cu2 Cu3 S3 93.37(6) . . . . ? S4 Cu2 Cu3 S3 173.35(6) . . . . ? Cu1 Cu2 Cu3 S3 3.64(12) . . . . ? S2 Cu2 Cu3 S4 89.90(6) . . . . ? S3 Cu2 Cu3 S4 -173.35(6) . . . . ? S1 Cu2 Cu3 S4 -79.98(6) . . . . ? Cu1 Cu2 Cu3 S4 -169.70(13) . . . . ? S2 Cu2 Cu3 S6 169.84(6) . . . . ? S3 Cu2 Cu3 S6 -93.41(5) . . . . ? S1 Cu2 Cu3 S6 -0.04(6) . . . . ? S4 Cu2 Cu3 S6 79.94(5) . . . . ? Cu1 Cu2 Cu3 S6 -89.77(13) . . . . ? S2 Cu2 Cu3 Cu1 154.65(12) . . . 6_556 ? S3 Cu2 Cu3 Cu1 -108.60(13) . . . 6_556 ? S1 Cu2 Cu3 Cu1 -15.23(15) . . . 6_556 ? S4 Cu2 Cu3 Cu1 64.75(13) . . . 6_556 ? Cu1 Cu2 Cu3 Cu1 -104.95(14) . . . 6_556 ? S2 Cu2 S1 C1 130.90(19) . . . . ? S3 Cu2 S1 C1 5.5(2) . . . . ? S4 Cu2 S1 C1 -114.62(19) . . . . ? Cu3 Cu2 S1 C1 -57.5(2) . . . . ? Cu1 Cu2 S1 C1 103.78(19) . . . . ? S2 Cu2 S1 Cu1 27.11(5) . . . . ? S3 Cu2 S1 Cu1 -98.28(5) . . . . ? S4 Cu2 S1 Cu1 141.60(4) . . . . ? Cu3 Cu2 S1 Cu1 -161.24(4) . . . . ? S2 Cu1 S1 C1 -134.42(19) . . . . ? S5 Cu1 S1 C1 -9.3(2) 6_656 . . . ? S6 Cu1 S1 C1 110.81(19) 6_656 . . . ? Cu3 Cu1 S1 C1 51.8(2) 6_656 . . . ? Cu2 Cu1 S1 C1 -107.40(19) . . . . ? S2 Cu1 S1 Cu2 -27.02(5) . . . . ? S5 Cu1 S1 Cu2 98.15(5) 6_656 . . . ? S6 Cu1 S1 Cu2 -141.79(5) 6_656 . . . ? Cu3 Cu1 S1 Cu2 159.24(4) 6_656 . . . ? S5 Cu1 S2 C6 167.91(18) 6_656 . . . ? S6 Cu1 S2 C6 31.73(19) 6_656 . . . ? S1 Cu1 S2 C6 -72.79(19) . . . . ? Cu3 Cu1 S2 C6 98.73(19) 6_656 . . . ? Cu2 Cu1 S2 C6 -99.67(18) . . . . ? S5 Cu1 S2 Cu2 -92.42(5) 6_656 . . . ? S6 Cu1 S2 Cu2 131.40(5) 6_656 . . . ? S1 Cu1 S2 Cu2 26.88(5) . . . . ? Cu3 Cu1 S2 Cu2 -161.60(5) 6_656 . . . ? S3 Cu2 S2 C6 -165.19(18) . . . . ? S1 Cu2 S2 C6 72.23(19) . . . . ? S4 Cu2 S2 C6 -35.80(19) . . . . ? Cu3 Cu2 S2 C6 -98.86(19) . . . . ? Cu1 Cu2 S2 C6 100.03(19) . . . . ? S3 Cu2 S2 Cu1 94.78(5) . . . . ? S1 Cu2 S2 Cu1 -27.80(5) . . . . ? S4 Cu2 S2 Cu1 -135.82(5) . . . . ? Cu3 Cu2 S2 Cu1 161.12(4) . . . . ? S5 Cu3 S3 C11 -32.2(2) . . . . ? S4 Cu3 S3 C11 104.85(19) . . . . ? S6 Cu3 S3 C11 -158.26(19) . . . . ? Cu2 Cu3 S3 C11 98.46(19) . . . . ? Cu1 Cu3 S3 C11 -99.60(19) 6_556 . . . ? S5 Cu3 S3 Cu2 -130.66(5) . . . . ? S4 Cu3 S3 Cu2 6.39(5) . . . . ? S6 Cu3 S3 Cu2 103.27(4) . . . . ? Cu1 Cu3 S3 Cu2 161.94(4) 6_556 . . . ? S2 Cu2 S3 C11 10.43(18) . . . . ? S1 Cu2 S3 C11 132.13(18) . . . . ? S4 Cu2 S3 C11 -116.70(18) . . . . ? Cu3 Cu2 S3 C11 -110.58(18) . . . . ? Cu1 Cu2 S3 C11 70.46(18) . . . . ? S2 Cu2 S3 Cu3 121.02(5) . . . . ? S1 Cu2 S3 Cu3 -117.29(5) . . . . ? S4 Cu2 S3 Cu3 -6.12(5) . . . . ? Cu1 Cu2 S3 Cu3 -178.96(4) . . . . ? S5 Cu3 S4 C16 31.62(19) . . . . ? S3 Cu3 S4 C16 -107.04(19) . . . . ? S6 Cu3 S4 C16 149.17(19) . . . . ? Cu2 Cu3 S4 C16 -100.74(19) . . . . ? Cu1 Cu3 S4 C16 94.44(19) 6_556 . . . ? S5 Cu3 S4 Cu2 132.36(5) . . . . ? S3 Cu3 S4 Cu2 -6.31(5) . . . . ? S6 Cu3 S4 Cu2 -110.09(4) . . . . ? Cu1 Cu3 S4 Cu2 -164.82(4) 6_556 . . . ? S2 Cu2 S4 C16 -19.36(19) . . . . ? S3 Cu2 S4 C16 110.27(18) . . . . ? S1 Cu2 S4 C16 -132.76(18) . . . . ? Cu3 Cu2 S4 C16 104.15(18) . . . . ? Cu1 Cu2 S4 C16 -80.07(19) . . . . ? S2 Cu2 S4 Cu3 -123.51(5) . . . . ? S3 Cu2 S4 Cu3 6.11(5) . . . . ? S1 Cu2 S4 Cu3 123.08(5) . . . . ? Cu1 Cu2 S4 Cu3 175.78(5) . . . . ? S3 Cu3 S5 C21 -10.05(18) . . . . ? S4 Cu3 S5 C21 -148.82(17) . . . . ? S6 Cu3 S5 C21 109.20(18) . . . . ? Cu2 Cu3 S5 C21 -80.47(18) . . . . ? Cu1 Cu3 S5 C21 107.01(18) 6_556 . . . ? S3 Cu3 S5 Cu1 -117.06(5) . . . 6_556 ? S4 Cu3 S5 Cu1 104.17(5) . . . 6_556 ? S6 Cu3 S5 Cu1 2.19(5) . . . 6_556 ? Cu2 Cu3 S5 Cu1 172.52(5) . . . 6_556 ? S5 Cu3 S6 C26 -102.12(19) . . . . ? S3 Cu3 S6 C26 24.93(19) . . . . ? S4 Cu3 S6 C26 142.46(19) . . . . ? Cu2 Cu3 S6 C26 84.78(19) . . . . ? Cu1 Cu3 S6 C26 -99.94(19) 6_556 . . . ? S5 Cu3 S6 Cu1 -2.18(5) . . . 6_556 ? S3 Cu3 S6 Cu1 124.87(4) . . . 6_556 ? S4 Cu3 S6 Cu1 -117.60(4) . . . 6_556 ? Cu2 Cu3 S6 Cu1 -175.28(3) . . . 6_556 ? Cu2 S1 C1 N1 -30.2(5) . . . . ? Cu1 S1 C1 N1 41.6(5) . . . . ? Cu2 S1 C1 C2 151.0(4) . . . . ? Cu1 S1 C1 C2 -137.2(4) . . . . ? N1 C1 C2 C3 -1.0(9) . . . . ? S1 C1 C2 C3 177.8(5) . . . . ? C1 C2 C3 C4 -0.4(11) . . . . ? C2 C3 C4 C5 1.7(12) . . . . ? C3 C4 C5 N1 -1.5(10) . . . . ? Cu1 S2 C6 N2 -148.5(4) . . . . ? Cu2 S2 C6 N2 141.8(4) . . . . ? Cu1 S2 C6 C7 30.5(5) . . . . ? Cu2 S2 C6 C7 -39.2(5) . . . . ? N2 C6 C7 C8 2.1(8) . . . . ? S2 C6 C7 C8 -176.9(4) . . . . ? C6 C7 C8 C9 -1.4(9) . . . . ? C7 C8 C9 C10 -0.1(11) . . . . ? C8 C9 C10 N2 0.8(11) . . . . ? Cu3 S3 C11 N3 141.5(3) . . . . ? Cu2 S3 C11 N3 -148.4(3) . . . . ? Cu3 S3 C11 C12 -37.4(5) . . . . ? Cu2 S3 C11 C12 32.7(5) . . . . ? N3 C11 C12 C13 0.9(7) . . . . ? S3 C11 C12 C13 179.8(4) . . . . ? C11 C12 C13 C14 -0.4(8) . . . . ? C12 C13 C14 C15 -0.1(8) . . . . ? C13 C14 C15 N3 0.1(8) . . . . ? Cu3 S4 C16 N4 -161.3(3) . . . . ? Cu2 S4 C16 N4 130.8(4) . . . . ? Cu3 S4 C16 C17 18.9(5) . . . . ? Cu2 S4 C16 C17 -49.0(5) . . . . ? N4 C16 C17 C18 0.4(8) . . . . ? S4 C16 C17 C18 -179.8(4) . . . . ? C16 C17 C18 C19 0.0(9) . . . . ? C17 C18 C19 C20 -0.5(9) . . . . ? C18 C19 C20 N4 0.5(9) . . . . ? Cu3 S5 C21 N5 117.8(4) . . . . ? Cu1 S5 C21 N5 -173.6(3) 6_556 . . . ? Cu3 S5 C21 C22 -59.9(5) . . . . ? Cu1 S5 C21 C22 8.7(5) 6_556 . . . ? N5 C21 C22 C23 -3.6(7) . . . . ? S5 C21 C22 C23 174.1(4) . . . . ? C21 C22 C23 C24 1.4(8) . . . . ? C22 C23 C24 C25 1.4(8) . . . . ? C23 C24 C25 N5 -1.9(8) . . . . ? Cu1 S6 C26 N6 143.3(3) 6_556 . . . ? Cu3 S6 C26 N6 -148.6(3) . . . . ? Cu1 S6 C26 C27 -36.9(5) 6_556 . . . ? Cu3 S6 C26 C27 31.2(5) . . . . ? N6 C26 C27 C28 -0.6(7) . . . . ? S6 C26 C27 C28 179.5(4) . . . . ? C26 C27 C28 C29 0.5(8) . . . . ? C27 C28 C29 C30 -0.7(9) . . . . ? C28 C29 C30 N6 1.0(9) . . . . ? C2 C1 N1 C5 1.3(8) . . . . ? S1 C1 N1 C5 -177.6(4) . . . . ? C4 C5 N1 C1 0.0(9) . . . . ? C7 C6 N2 C10 -1.4(8) . . . . ? S2 C6 N2 C10 177.7(5) . . . . ? C9 C10 N2 C6 -0.1(11) . . . . ? C14 C15 N3 C11 0.4(8) . . . . ? C12 C11 N3 C15 -0.9(7) . . . . ? S3 C11 N3 C15 -179.9(4) . . . . ? C19 C20 N4 C16 -0.1(9) . . . . ? C17 C16 N4 C20 -0.4(8) . . . . ? S4 C16 N4 C20 179.8(4) . . . . ? C24 C25 N5 C21 -0.4(8) . . . . ? C22 C21 N5 C25 3.1(7) . . . . ? S5 C21 N5 C25 -174.7(4) . . . . ? C27 C26 N6 C30 1.1(8) . . . . ? S6 C26 N6 C30 -179.1(5) . . . . ? C29 C30 N6 C26 -1.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.78 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.492 _refine_diff_density_min -0.906 _refine_diff_density_rms 0.246 _chemical_name_common ; hexaaquacopper(ii) catena-dodekakis(mu-Pyridine-2(1H)-thione- k2S:S)-hexacopper(i) di(sulphate) - water (1/4) ; #===END data_compound3 _database_code_depnum_ccdc_archive 'CCDC 741281' _chemical_name_systematic ; di-mu-sulphato-k4O,O'-bis(2,2'-dipyridylsulphide-k2N,N')-dicopper(II) - water (1/3) ; _chemical_melting_point ? _chemical_formula_moiety 'C20 H20 Cu2 N4 O10 S4, 3(H2 O)' _chemical_formula_sum 'C20 H26 Cu2 N4 O13 S4' _chemical_formula_iupac '[Cu2(mu-SO4)2(C10H8N2S)2(H2O)2].3H2O' _chemical_formula_weight 785.77 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1397(5) _cell_length_b 9.3421(9) _cell_length_c 11.5895(11) _cell_angle_alpha 113.487(4) _cell_angle_beta 93.318(4) _cell_angle_gamma 98.026(4) _cell_volume 696.52(11) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 30792 _cell_measurement_theta_min 1.93 _cell_measurement_theta_max 28.70 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.873 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 1.900 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'CrysAlis RED (Oxford Diffraction, 2003)' _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.887 _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 30792 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 28.70 _reflns_number_total 3563 _reflns_number_gt 3413 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Sir92 (Altamore et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0267P)^2^+3.1470P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary geom _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3563 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 1.189 _refine_ls_restrained_S_all 1.189 _refine_ls_shift/su_max 0.000 _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 Cu1 Cu 0.22280(6) 0.72121(5) 0.16720(4) 0.00821(12) Uani 1 1 d . . . S1 S 0.27561(14) 1.09732(11) 0.23206(9) 0.0139(2) Uani 1 1 d . . . S2 S -0.14342(12) 0.47641(10) 0.13214(8) 0.00867(18) Uani 1 1 d . . . C1 C 0.2610(5) 1.0472(4) 0.3641(3) 0.0118(7) Uani 1 1 d . . . C2 C 0.2688(6) 1.1668(5) 0.4834(4) 0.0167(8) Uani 1 1 d . . . H2 H 0.2877 1.2749 0.4960 0.020 Uiso 1 1 calc R . . C3 C 0.2481(6) 1.1240(5) 0.5846(4) 0.0188(8) Uani 1 1 d . . . H3 H 0.2489 1.2026 0.6678 0.023 Uiso 1 1 calc R . . C4 C 0.2263(6) 0.9657(5) 0.5627(4) 0.0178(8) Uani 1 1 d . . . H4 H 0.2149 0.9345 0.6310 0.021 Uiso 1 1 calc R . . C5 C 0.2213(5) 0.8535(5) 0.4411(4) 0.0149(7) Uani 1 1 d . . . H5 H 0.2064 0.7448 0.4267 0.018 Uiso 1 1 calc R . . C6 C 0.4676(5) 1.0023(4) 0.1682(3) 0.0102(7) Uani 1 1 d . . . C7 C 0.6254(5) 1.0903(5) 0.1496(4) 0.0130(7) Uani 1 1 d . . . H7 H 0.6335 1.2010 0.1735 0.016 Uiso 1 1 calc R . . C8 C 0.7720(5) 1.0142(5) 0.0955(4) 0.0145(7) Uani 1 1 d . . . H8 H 0.8813 1.0717 0.0804 0.017 Uiso 1 1 calc R . . C9 C 0.7568(5) 0.8525(5) 0.0636(4) 0.0137(7) Uani 1 1 d . . . H9 H 0.8564 0.7982 0.0278 0.016 Uiso 1 1 calc R . . C10 C 0.5934(5) 0.7720(4) 0.0850(3) 0.0121(7) Uani 1 1 d . . . H10 H 0.5825 0.6615 0.0628 0.015 Uiso 1 1 calc R . . N1 N 0.2367(4) 0.8928(4) 0.3420(3) 0.0109(6) Uani 1 1 d . . . N2 N 0.4501(4) 0.8450(4) 0.1359(3) 0.0095(6) Uani 1 1 d . . . O1 O -0.2157(4) 0.4487(3) 0.0006(2) 0.0120(5) Uani 1 1 d . . . O2 O -0.0316(4) 0.6415(3) 0.1932(2) 0.0108(5) Uani 1 1 d . . . O3 O -0.0242(4) 0.3615(3) 0.1325(3) 0.0132(5) Uani 1 1 d . . . O4 O -0.3053(4) 0.4711(3) 0.2030(3) 0.0143(5) Uani 1 1 d . . . O1W O 0.3413(4) 0.5522(3) 0.2402(3) 0.0145(5) Uani 1 1 d . . . H1A H 0.2628 0.4672 0.2254 0.022 Uiso 1 1 d . . . H1B H 0.4531 0.5326 0.2494 0.022 Uiso 1 1 d . . . O2W O 0.0533(10) 0.6377(8) 0.6089(6) 0.0258(14) Uiso 0.50 1 d P . . O3W O 0.2675(9) 0.5683(8) 0.5540(6) 0.0241(13) Uiso 0.50 1 d P . . O4W O 0.3789(10) 0.5373(8) 0.4925(7) 0.0278(14) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0099(2) 0.0066(2) 0.0066(2) 0.00156(16) 0.00163(15) -0.00008(15) S1 0.0152(4) 0.0122(4) 0.0167(4) 0.0068(4) 0.0035(3) 0.0063(3) S2 0.0083(4) 0.0075(4) 0.0089(4) 0.0018(3) 0.0028(3) 0.0011(3) C1 0.0103(16) 0.0116(17) 0.0115(16) 0.0024(14) 0.0016(13) 0.0026(13) C2 0.0157(18) 0.0134(18) 0.0151(18) -0.0009(15) 0.0017(14) 0.0049(14) C3 0.0156(18) 0.024(2) 0.0081(16) -0.0028(15) 0.0015(14) 0.0060(16) C4 0.0142(18) 0.028(2) 0.0091(17) 0.0057(16) 0.0016(14) 0.0025(16) C5 0.0133(17) 0.0164(18) 0.0141(17) 0.0066(15) 0.0007(14) -0.0004(14) C6 0.0120(16) 0.0091(16) 0.0091(15) 0.0030(13) 0.0009(12) 0.0031(13) C7 0.0131(17) 0.0133(17) 0.0137(17) 0.0079(14) -0.0011(13) -0.0002(13) C8 0.0122(17) 0.0199(19) 0.0138(17) 0.0104(15) 0.0011(13) 0.0001(14) C9 0.0131(17) 0.0186(19) 0.0127(17) 0.0075(15) 0.0058(13) 0.0076(14) C10 0.0147(17) 0.0118(16) 0.0102(16) 0.0039(13) 0.0025(13) 0.0050(13) N1 0.0097(14) 0.0105(14) 0.0100(14) 0.0020(12) 0.0007(11) 0.0007(11) N2 0.0133(14) 0.0080(14) 0.0069(13) 0.0030(11) 0.0021(11) 0.0011(11) O1 0.0136(12) 0.0098(12) 0.0094(12) 0.0010(10) 0.0001(10) 0.0018(10) O2 0.0108(12) 0.0068(11) 0.0118(12) 0.0008(10) 0.0025(9) 0.0006(9) O3 0.0133(12) 0.0104(12) 0.0180(13) 0.0071(11) 0.0034(10) 0.0043(10) O4 0.0113(12) 0.0149(13) 0.0164(13) 0.0057(11) 0.0071(10) 0.0015(10) O1W 0.0116(12) 0.0142(13) 0.0178(13) 0.0056(11) 0.0023(10) 0.0051(10) _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 Cu1 O2 1.952(3) . ? Cu1 O1 1.952(3) 2_565 ? Cu1 N2 1.995(3) . ? Cu1 N1 2.006(3) . ? Cu1 O1W 2.298(3) . ? S1 C1 1.774(4) . ? S1 C6 1.775(4) . ? S2 O3 1.461(3) . ? S2 O4 1.463(3) . ? S2 O1 1.488(3) . ? S2 O2 1.496(3) . ? C1 N1 1.345(5) . ? C1 C2 1.380(5) . ? C2 C3 1.391(6) . ? C2 H2 0.9500 . ? C3 C4 1.381(6) . ? C3 H3 0.9500 . ? C4 C5 1.376(5) . ? C4 H4 0.9500 . ? C5 N1 1.344(5) . ? C5 H5 0.9500 . ? C6 N2 1.349(5) . ? C6 C7 1.379(5) . ? C7 C8 1.387(6) . ? C7 H7 0.9500 . ? C8 C9 1.391(6) . ? C8 H8 0.9500 . ? C9 C10 1.387(5) . ? C9 H9 0.9500 . ? C10 N2 1.344(5) . ? C10 H10 0.9500 . ? O1 Cu1 1.952(3) 2_565 ? O1W H1A 0.8539 . ? O1W H1B 0.8534 . ? O2W O3W 1.796(10) . ? O3W O4W 1.091(9) . ? 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 O2 Cu1 O1 94.67(11) . 2_565 ? O2 Cu1 N2 165.43(12) . . ? O1 Cu1 N2 89.95(12) 2_565 . ? O2 Cu1 N1 86.00(12) . . ? O1 Cu1 N1 178.07(12) 2_565 . ? N2 Cu1 N1 89.84(13) . . ? O2 Cu1 O1W 88.77(11) . . ? O1 Cu1 O1W 84.83(11) 2_565 . ? N2 Cu1 O1W 105.43(11) . . ? N1 Cu1 O1W 93.37(12) . . ? C1 S1 C6 99.25(17) . . ? O3 S2 O4 111.48(16) . . ? O3 S2 O1 111.31(16) . . ? O4 S2 O1 109.07(16) . . ? O3 S2 O2 110.69(16) . . ? O4 S2 O2 107.16(16) . . ? O1 S2 O2 106.94(15) . . ? N1 C1 C2 123.1(4) . . ? N1 C1 S1 117.9(3) . . ? C2 C1 S1 119.0(3) . . ? C1 C2 C3 117.9(4) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? C4 C3 C2 119.2(4) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C5 C4 C3 119.4(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? N1 C5 C4 122.0(4) . . ? N1 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? N2 C6 C7 122.7(3) . . ? N2 C6 S1 118.3(3) . . ? C7 C6 S1 119.0(3) . . ? C6 C7 C8 118.7(4) . . ? C6 C7 H7 120.6 . . ? C8 C7 H7 120.6 . . ? C7 C8 C9 119.1(4) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C10 C9 C8 118.7(3) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? N2 C10 C9 122.3(3) . . ? N2 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C5 N1 C1 118.3(3) . . ? C5 N1 Cu1 119.4(3) . . ? C1 N1 Cu1 122.3(3) . . ? C10 N2 C6 118.4(3) . . ? C10 N2 Cu1 119.6(3) . . ? C6 N2 Cu1 121.9(3) . . ? S2 O1 Cu1 135.12(17) . 2_565 ? S2 O2 Cu1 128.71(16) . . ? Cu1 O1W H1A 114.0 . . ? Cu1 O1W H1B 133.0 . . ? H1A O1W H1B 107.0 . . ? O4W O3W O2W 158.8(7) . . ? 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 C6 S1 C1 N1 -56.0(3) . . . . ? C6 S1 C1 C2 126.0(3) . . . . ? N1 C1 C2 C3 -0.8(6) . . . . ? S1 C1 C2 C3 177.0(3) . . . . ? C1 C2 C3 C4 1.8(6) . . . . ? C2 C3 C4 C5 -1.4(6) . . . . ? C3 C4 C5 N1 -0.1(6) . . . . ? C1 S1 C6 N2 57.5(3) . . . . ? C1 S1 C6 C7 -124.5(3) . . . . ? N2 C6 C7 C8 0.1(6) . . . . ? S1 C6 C7 C8 -177.7(3) . . . . ? C6 C7 C8 C9 -1.1(6) . . . . ? C7 C8 C9 C10 1.2(6) . . . . ? C8 C9 C10 N2 -0.3(6) . . . . ? C4 C5 N1 C1 1.2(6) . . . . ? C4 C5 N1 Cu1 -178.8(3) . . . . ? C2 C1 N1 C5 -0.7(6) . . . . ? S1 C1 N1 C5 -178.6(3) . . . . ? C2 C1 N1 Cu1 179.3(3) . . . . ? S1 C1 N1 Cu1 1.4(4) . . . . ? O2 Cu1 N1 C5 60.2(3) . . . . ? N2 Cu1 N1 C5 -133.8(3) . . . . ? O1W Cu1 N1 C5 -28.3(3) . . . . ? O2 Cu1 N1 C1 -119.8(3) . . . . ? N2 Cu1 N1 C1 46.2(3) . . . . ? O1W Cu1 N1 C1 151.7(3) . . . . ? C9 C10 N2 C6 -0.6(5) . . . . ? C9 C10 N2 Cu1 -178.6(3) . . . . ? C7 C6 N2 C10 0.7(5) . . . . ? S1 C6 N2 C10 178.6(3) . . . . ? C7 C6 N2 Cu1 178.6(3) . . . . ? S1 C6 N2 Cu1 -3.5(4) . . . . ? O2 Cu1 N2 C10 -153.7(4) . . . . ? O1 Cu1 N2 C10 -45.0(3) 2_565 . . . ? N1 Cu1 N2 C10 133.1(3) . . . . ? O1W Cu1 N2 C10 39.6(3) . . . . ? O2 Cu1 N2 C6 28.4(6) . . . . ? O1 Cu1 N2 C6 137.1(3) 2_565 . . . ? N1 Cu1 N2 C6 -44.8(3) . . . . ? O1W Cu1 N2 C6 -138.3(3) . . . . ? O3 S2 O1 Cu1 11.8(3) . . . 2_565 ? O4 S2 O1 Cu1 -111.6(2) . . . 2_565 ? O2 S2 O1 Cu1 132.8(2) . . . 2_565 ? O3 S2 O2 Cu1 46.1(3) . . . . ? O4 S2 O2 Cu1 167.9(2) . . . . ? O1 S2 O2 Cu1 -75.3(2) . . . . ? O1 Cu1 O2 S2 23.0(2) 2_565 . . . ? N2 Cu1 O2 S2 131.1(4) . . . . ? N1 Cu1 O2 S2 -155.2(2) . . . . ? O1W Cu1 O2 S2 -61.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.769 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.172 _chemical_name_common ; di-mu-sulphato-k4O,O'-bis(2,2'-dipyridylsulphide-k2N,N')- dicopper(ii) - water (1 ;