data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Cheng, Peng' _publ_contact_author_email pcheng@nankai.edu.cn _publ_section_title ; Metal-Organic Frameworks Based on Transition-Metal Carboxylate Clusters as Secondary Building Units: Synthesis, Structures and Properties ; _publ_author_name 'Peng Cheng' # Attachment '- 1.CIF' data_c090322g _database_code_depnum_ccdc_archive 'CCDC 756342' #TrackingRef '- 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H19 N6 O10 S Zn2.50' _chemical_formula_weight 734.99 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7882(13) _cell_length_b 12.3072(12) _cell_length_c 14.2893(14) _cell_angle_alpha 83.183(7) _cell_angle_beta 69.590(7) _cell_angle_gamma 65.174(8) _cell_volume 1612.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 1.972 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6938 _exptl_absorpt_correction_T_max 0.6938 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10272 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5643 _reflns_number_gt 4426 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1309P)^2^+7.9060P] 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 5643 _refine_ls_number_parameters 376 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.2274 _refine_ls_wR_factor_gt 0.2159 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.077 _refine_ls_shift/su_mean 0.001 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 Zn1 Zn 0.75157(9) 0.55432(7) 0.03820(6) 0.0254(3) Uani 1 1 d . . . Zn3 Zn 0.78919(11) -0.20392(8) -0.09321(7) 0.0379(3) Uani 1 1 d . . . Zn2 Zn 0.5000 0.5000 0.0000 0.0246(3) Uani 1 2 d S . . S1 S 1.3961(4) 0.0143(3) -0.2234(3) 0.0783(8) Uani 1 1 d U . . O4 O 1.4212(10) 0.0896(8) -0.1745(7) 0.0858(13) Uani 1 1 d U . . O6 O 1.4277(10) 0.0459(9) -0.3205(7) 0.0925(13) Uani 1 1 d U . . O5 O 1.4644(10) -0.1019(8) -0.1932(7) 0.0810(13) Uani 1 1 d U . . O8 O 0.8975(6) 0.3957(5) -0.0311(4) 0.0335(12) Uani 1 1 d . . . O7 O 0.7088(3) 0.3505(3) -0.0041(2) 0.0374(13) Uani 1 1 d . . . O9 O 0.5755(3) 0.6148(3) 0.0100(2) 0.0313(12) Uani 1 1 d R . . H9A H 0.5019 0.6814 0.0223 0.038 Uiso 1 1 d R . . O10 O 0.8445(3) 0.6627(3) -0.0099(2) 0.0370(13) Uani 1 1 d R . . H10A H 0.9260 0.6448 -0.0031 0.044 Uiso 1 1 d R . . O1 O 0.5633(3) -0.1356(3) -0.0410(2) 0.074(2) Uani 1 1 d R . . H1A H 0.5236 -0.1176 -0.0858 0.089 Uiso 1 1 d R . . H2B H 0.4975 -0.1057 0.0144 0.089 Uiso 1 1 d R . . O2 O 0.8003(8) -0.0494(6) -0.0957(6) 0.0585(18) Uani 1 1 d . . . O3 O 1.0217(9) -0.1876(6) -0.1437(8) 0.082(3) Uani 1 1 d . . . N4 N 0.5818(7) 0.5132(6) 0.8359(5) 0.0331(15) Uani 1 1 d . . . C11 C 0.8425(8) 0.3258(6) -0.0361(5) 0.0270(16) Uani 1 1 d . . . N1 N 0.7209(7) 0.5326(6) 0.1866(5) 0.0320(14) Uani 1 1 d . . . C2 C 0.5710(10) 0.6386(9) 0.6954(6) 0.046(2) Uani 1 1 d . . . H2 H 0.5460 0.7153 0.6703 0.056 Uiso 1 1 calc R . . C1 C 0.5486(9) 0.6195(7) 0.7955(6) 0.0342(18) Uani 1 1 d . . . H1 H 0.5069 0.6864 0.8380 0.041 Uiso 1 1 calc R . . C12 C 0.9522(9) 0.2036(7) -0.0855(6) 0.0308(17) Uani 1 1 d . . . C5 C 0.6451(10) 0.4175(8) 0.7742(6) 0.041(2) Uani 1 1 d . . . H5 H 0.6718 0.3414 0.8003 0.050 Uiso 1 1 calc R . . C10 C 0.6523(10) 0.6192(9) 0.3431(6) 0.048(2) Uani 1 1 d . . . H10 H 0.6191 0.6869 0.3827 0.057 Uiso 1 1 calc R . . C13 C 1.1027(9) 0.1702(7) -0.1276(7) 0.0387(19) Uani 1 1 d . . . H13 H 1.1395 0.2262 -0.1274 0.046 Uiso 1 1 calc R . . N5 N 0.8477(9) -0.2806(7) -0.2283(5) 0.0449(18) Uani 1 1 d . . . C17 C 0.8970(8) 0.1226(7) -0.0850(6) 0.0335(17) Uani 1 1 d . . . H17 H 0.7980 0.1425 -0.0582 0.040 Uiso 1 1 calc R . . C16 C 0.9951(9) 0.0071(7) -0.1266(6) 0.0360(18) Uani 1 1 d . . . C8 C 0.7457(9) 0.4265(7) 0.2285(6) 0.0389(19) Uani 1 1 d . . . H8 H 0.7758 0.3602 0.1880 0.047 Uiso 1 1 calc R . . C14 C 1.1982(9) 0.0565(7) -0.1694(7) 0.041(2) Uani 1 1 d . . . C21 C 0.9393(11) -0.3947(10) -0.4069(7) 0.055(3) Uani 1 1 d . . . C4 C 0.6713(10) 0.4286(9) 0.6739(7) 0.048(2) Uani 1 1 d . . . H4 H 0.7160 0.3608 0.6321 0.057 Uiso 1 1 calc R . . C20 C 0.8827(15) -0.2720(11) -0.3995(8) 0.073(3) Uani 1 1 d . . . H20 H 0.8745 -0.2264 -0.4555 0.087 Uiso 1 1 calc R . . N2 N 0.6675(10) 0.4816(8) 0.4884(6) 0.054(2) Uani 1 1 d . . . C18 C 0.9379(11) -0.0822(9) -0.1230(7) 0.048(2) Uani 1 1 d . . . C22 C 0.9491(11) -0.4594(9) -0.3227(7) 0.051(2) Uani 1 1 d . . . H22 H 0.9872 -0.5426 -0.3258 0.061 Uiso 1 1 calc R . . C6 C 0.6828(10) 0.5064(9) 0.3844(6) 0.045(2) Uani 1 1 d . . . N3 N 0.6480(10) 0.5643(8) 0.5307(6) 0.056(2) Uani 1 1 d . . . C15 C 1.1453(10) -0.0236(7) -0.1680(7) 0.048(2) Uani 1 1 d . . . H15 H 1.2076 -0.1005 -0.1944 0.057 Uiso 1 1 calc R . . C19 C 0.8398(14) -0.2195(11) -0.3113(8) 0.068(3) Uani 1 1 d . . . H19 H 0.8024 -0.1363 -0.3070 0.081 Uiso 1 1 calc R . . C9 C 0.6721(10) 0.6282(8) 0.2433(7) 0.043(2) Uani 1 1 d . . . H9 H 0.6508 0.7031 0.2150 0.051 Uiso 1 1 calc R . . C3 C 0.6314(9) 0.5403(8) 0.6354(6) 0.040(2) Uani 1 1 d . . . N6 N 0.9834(10) -0.4456(8) -0.5002(6) 0.060(2) Uani 1 1 d . . . C7 C 0.7297(10) 0.4092(8) 0.3264(6) 0.045(2) Uani 1 1 d . . . H7 H 0.7502 0.3332 0.3527 0.053 Uiso 1 1 calc R . . C23 C 0.9022(11) -0.3995(9) -0.2348(7) 0.047(2) Uani 1 1 d . . . H23 H 0.9083 -0.4429 -0.1775 0.056 Uiso 1 1 calc R . . 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 0.0316(5) 0.0260(5) 0.0276(5) -0.0004(3) -0.0139(4) -0.0166(4) Zn3 0.0520(6) 0.0304(5) 0.0439(6) 0.0011(4) -0.0219(5) -0.0235(5) Zn2 0.0285(6) 0.0265(6) 0.0277(6) 0.0002(5) -0.0128(5) -0.0164(5) S1 0.0750(10) 0.0774(10) 0.0824(10) 0.0036(7) -0.0238(7) -0.0330(8) O4 0.0839(15) 0.0848(15) 0.0878(15) 0.0020(9) -0.0265(9) -0.0348(9) O6 0.0897(15) 0.0920(15) 0.0913(15) 0.0046(9) -0.0280(9) -0.0348(9) O5 0.0798(15) 0.0799(15) 0.0833(15) 0.0030(9) -0.0264(9) -0.0329(9) O8 0.034(3) 0.027(3) 0.045(3) -0.008(2) -0.017(2) -0.012(2) O7 0.026(3) 0.023(3) 0.064(4) 0.001(3) -0.019(3) -0.008(2) O9 0.038(3) 0.028(3) 0.042(3) 0.006(2) -0.027(2) -0.017(2) O10 0.045(3) 0.034(3) 0.053(3) 0.010(3) -0.026(3) -0.030(3) O1 0.047(4) 0.059(5) 0.107(6) -0.006(4) -0.024(4) -0.013(4) O2 0.068(5) 0.033(3) 0.089(5) -0.002(3) -0.032(4) -0.027(3) O3 0.082(6) 0.030(4) 0.136(8) -0.024(4) -0.028(5) -0.022(4) N4 0.039(4) 0.039(4) 0.031(3) 0.000(3) -0.013(3) -0.022(3) C11 0.035(4) 0.023(4) 0.029(4) 0.001(3) -0.017(3) -0.013(3) N1 0.035(4) 0.036(4) 0.029(3) -0.002(3) -0.016(3) -0.014(3) C2 0.058(6) 0.054(6) 0.036(5) 0.011(4) -0.020(4) -0.029(5) C1 0.040(5) 0.033(4) 0.029(4) -0.001(3) -0.005(3) -0.018(4) C12 0.041(4) 0.024(4) 0.035(4) 0.003(3) -0.019(3) -0.015(3) C5 0.052(5) 0.043(5) 0.031(4) -0.002(4) -0.014(4) -0.020(4) C10 0.062(6) 0.057(6) 0.032(5) -0.014(4) -0.011(4) -0.031(5) C13 0.037(5) 0.029(4) 0.054(5) -0.003(4) -0.014(4) -0.016(4) N5 0.066(5) 0.041(4) 0.042(4) 0.003(3) -0.026(4) -0.029(4) C17 0.031(4) 0.030(4) 0.044(5) 0.001(3) -0.013(3) -0.016(3) C16 0.054(5) 0.027(4) 0.036(4) -0.001(3) -0.016(4) -0.023(4) C8 0.049(5) 0.031(4) 0.040(5) 0.004(4) -0.021(4) -0.015(4) C14 0.039(5) 0.027(4) 0.056(5) -0.003(4) -0.012(4) -0.014(4) C21 0.059(6) 0.077(7) 0.046(6) -0.002(5) -0.017(5) -0.041(6) C4 0.054(6) 0.056(6) 0.039(5) -0.012(4) -0.015(4) -0.024(5) C20 0.114(10) 0.067(8) 0.048(6) 0.011(5) -0.035(6) -0.042(7) N2 0.070(6) 0.063(6) 0.038(4) -0.005(4) -0.015(4) -0.034(5) C18 0.056(6) 0.051(6) 0.048(5) 0.010(4) -0.023(5) -0.028(5) C22 0.061(6) 0.048(6) 0.052(6) -0.007(4) -0.019(5) -0.029(5) C6 0.058(6) 0.064(6) 0.029(4) 0.014(4) -0.021(4) -0.038(5) N3 0.069(6) 0.071(6) 0.036(4) 0.000(4) -0.013(4) -0.039(5) C15 0.056(6) 0.021(4) 0.059(6) -0.008(4) -0.017(5) -0.008(4) C19 0.107(10) 0.059(7) 0.053(6) 0.002(5) -0.035(6) -0.042(7) C9 0.061(6) 0.032(5) 0.044(5) 0.004(4) -0.025(4) -0.023(4) C3 0.047(5) 0.056(6) 0.025(4) 0.007(4) -0.016(4) -0.027(4) N6 0.073(6) 0.085(6) 0.035(4) -0.008(5) -0.018(4) -0.042(6) C7 0.064(6) 0.041(5) 0.035(5) 0.008(4) -0.028(4) -0.020(4) C23 0.064(6) 0.049(6) 0.034(5) -0.002(4) -0.018(4) -0.027(5) _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 Zn1 O9 1.897(3) . ? Zn1 O10 1.919(3) . ? Zn1 O8 2.015(5) . ? Zn1 N1 2.031(6) . ? Zn3 O10 1.917(3) 1_545 ? Zn3 O2 1.951(6) . ? Zn3 N5 2.024(7) . ? Zn3 O1 2.089(3) . ? Zn3 O3 2.445(9) . ? Zn2 O9 1.944(3) 2_665 ? Zn2 O9 1.944(3) . ? Zn2 N4 2.211(6) 1_554 ? Zn2 N4 2.211(6) 2_666 ? Zn2 O7 2.217(3) . ? Zn2 O7 2.217(3) 2_665 ? Zn2 Zn1 3.2794(8) 2_665 ? S1 O6 1.359(10) . ? S1 O4 1.385(10) . ? S1 O5 1.402(9) . ? S1 C14 1.854(9) . ? O8 C11 1.252(9) . ? O7 C11 1.260(8) . ? O9 H9A 0.8500 . ? O10 Zn3 1.917(3) 1_565 ? O10 H10A 0.8500 . ? O1 H1A 0.8501 . ? O1 H2B 0.8500 . ? O2 C18 1.284(12) . ? O3 C18 1.227(12) . ? N4 C1 1.321(10) . ? N4 C5 1.335(10) . ? N4 Zn2 2.211(6) 1_556 ? C11 C12 1.528(10) . ? N1 C9 1.314(10) . ? N1 C8 1.330(10) . ? C2 C3 1.349(13) . ? C2 C1 1.374(12) . ? C2 H2 0.9300 . ? C1 H1 0.9300 . ? C12 C17 1.358(11) . ? C12 C13 1.408(11) . ? C5 C4 1.362(12) . ? C5 H5 0.9300 . ? C10 C9 1.364(12) . ? C10 C6 1.394(13) . ? C10 H10 0.9300 . ? C13 C14 1.391(11) . ? C13 H13 0.9300 . ? N5 C23 1.329(12) . ? N5 C19 1.336(13) . ? C17 C16 1.412(11) . ? C17 H17 0.9300 . ? C16 C15 1.410(13) . ? C16 C18 1.458(12) . ? C8 C7 1.351(12) . ? C8 H8 0.9300 . ? C14 C15 1.326(12) . ? C21 C22 1.372(14) . ? C21 C20 1.372(16) . ? C21 N6 1.379(12) . ? C4 C3 1.367(13) . ? C4 H4 0.9300 . ? C20 C19 1.325(15) . ? C20 H20 0.9300 . ? N2 N3 1.150(11) . ? N2 C6 1.446(11) . ? C22 C23 1.356(13) . ? C22 H22 0.9300 . ? C6 C7 1.344(13) . ? N3 C3 1.452(11) . ? C15 H15 0.9300 . ? C19 H19 0.9300 . ? C9 H9 0.9300 . ? N6 N6 1.232(18) 2_744 ? C7 H7 0.9300 . ? C23 H23 0.9300 . ? 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 O9 Zn1 O10 109.15(14) . . ? O9 Zn1 O8 114.00(17) . . ? O10 Zn1 O8 105.10(18) . . ? O9 Zn1 N1 112.5(2) . . ? O10 Zn1 N1 108.9(2) . . ? O8 Zn1 N1 106.8(2) . . ? O10 Zn3 O2 129.5(2) 1_545 . ? O10 Zn3 N5 104.0(2) 1_545 . ? O2 Zn3 N5 115.7(3) . . ? O10 Zn3 O1 103.56(14) 1_545 . ? O2 Zn3 O1 95.6(2) . . ? N5 Zn3 O1 104.5(2) . . ? O10 Zn3 O3 93.8(2) 1_545 . ? O2 Zn3 O3 58.4(3) . . ? N5 Zn3 O3 89.6(3) . . ? O1 Zn3 O3 154.00(18) . . ? O9 Zn2 O9 180.00(18) 2_665 . ? O9 Zn2 N4 92.38(18) 2_665 1_554 ? O9 Zn2 N4 87.62(18) . 1_554 ? O9 Zn2 N4 87.62(18) 2_665 2_666 ? O9 Zn2 N4 92.38(18) . 2_666 ? N4 Zn2 N4 180.000(1) 1_554 2_666 ? O9 Zn2 O7 89.84(11) 2_665 . ? O9 Zn2 O7 90.16(11) . . ? N4 Zn2 O7 90.57(19) 1_554 . ? N4 Zn2 O7 89.43(19) 2_666 . ? O9 Zn2 O7 90.16(11) 2_665 2_665 ? O9 Zn2 O7 89.84(11) . 2_665 ? N4 Zn2 O7 89.43(19) 1_554 2_665 ? N4 Zn2 O7 90.57(19) 2_666 2_665 ? O7 Zn2 O7 180.0 . 2_665 ? O9 Zn2 Zn1 30.94(8) 2_665 2_665 ? O9 Zn2 Zn1 149.06(8) . 2_665 ? N4 Zn2 Zn1 85.49(16) 1_554 2_665 ? N4 Zn2 Zn1 94.51(16) 2_666 2_665 ? O7 Zn2 Zn1 120.00(7) . 2_665 ? O7 Zn2 Zn1 60.00(7) 2_665 2_665 ? O6 S1 O4 105.7(6) . . ? O6 S1 O5 123.0(6) . . ? O4 S1 O5 106.5(6) . . ? O6 S1 C14 108.4(5) . . ? O4 S1 C14 104.7(5) . . ? O5 S1 C14 107.2(5) . . ? C11 O8 Zn1 113.8(5) . . ? C11 O7 Zn2 140.2(4) . . ? Zn1 O9 Zn2 117.26(15) . . ? Zn1 O9 H9A 133.9 . . ? Zn2 O9 H9A 103.9 . . ? Zn3 O10 Zn1 126.15(15) 1_565 . ? Zn3 O10 H10A 114.5 1_565 . ? Zn1 O10 H10A 118.4 . . ? Zn3 O1 H1A 115.5 . . ? Zn3 O1 H2B 135.1 . . ? H1A O1 H2B 107.7 . . ? C18 O2 Zn3 100.8(6) . . ? C18 O3 Zn3 79.5(6) . . ? C1 N4 C5 117.3(7) . . ? C1 N4 Zn2 119.8(5) . 1_556 ? C5 N4 Zn2 122.1(6) . 1_556 ? O8 C11 O7 124.7(6) . . ? O8 C11 C12 114.4(6) . . ? O7 C11 C12 120.9(6) . . ? C9 N1 C8 119.0(7) . . ? C9 N1 Zn1 118.2(6) . . ? C8 N1 Zn1 122.8(5) . . ? C3 C2 C1 116.4(9) . . ? C3 C2 H2 121.8 . . ? C1 C2 H2 121.8 . . ? N4 C1 C2 124.8(8) . . ? N4 C1 H1 117.6 . . ? C2 C1 H1 117.6 . . ? C17 C12 C13 119.4(7) . . ? C17 C12 C11 115.8(7) . . ? C13 C12 C11 124.8(7) . . ? N4 C5 C4 121.6(9) . . ? N4 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C9 C10 C6 118.7(8) . . ? C9 C10 H10 120.7 . . ? C6 C10 H10 120.7 . . ? C14 C13 C12 122.4(7) . . ? C14 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C23 N5 C19 118.4(8) . . ? C23 N5 Zn3 117.5(6) . . ? C19 N5 Zn3 124.1(7) . . ? C12 C17 C16 117.7(7) . . ? C12 C17 H17 121.2 . . ? C16 C17 H17 121.2 . . ? C15 C16 C17 121.6(7) . . ? C15 C16 C18 120.2(8) . . ? C17 C16 C18 118.2(8) . . ? N1 C8 C7 123.9(8) . . ? N1 C8 H8 118.0 . . ? C7 C8 H8 118.0 . . ? C15 C14 C13 118.5(8) . . ? C15 C14 S1 119.9(7) . . ? C13 C14 S1 121.6(6) . . ? C22 C21 C20 119.0(9) . . ? C22 C21 N6 123.9(10) . . ? C20 C21 N6 117.1(10) . . ? C5 C4 C3 119.4(8) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C19 C20 C21 119.0(11) . . ? C19 C20 H20 120.5 . . ? C21 C20 H20 120.5 . . ? N3 N2 C6 110.9(9) . . ? O3 C18 O2 121.2(9) . . ? O3 C18 C16 119.5(9) . . ? O2 C18 C16 119.2(9) . . ? C23 C22 C21 118.7(10) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? C7 C6 C10 120.1(8) . . ? C7 C6 N2 114.4(8) . . ? C10 C6 N2 125.5(8) . . ? N2 N3 C3 111.2(9) . . ? C14 C15 C16 120.4(8) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C20 C19 N5 122.9(11) . . ? C20 C19 H19 118.5 . . ? N5 C19 H19 118.5 . . ? N1 C9 C10 121.0(8) . . ? N1 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C2 C3 C4 120.5(8) . . ? C2 C3 N3 114.9(8) . . ? C4 C3 N3 124.7(8) . . ? N6 N6 C21 113.8(11) 2_744 . ? C6 C7 C8 117.3(8) . . ? C6 C7 H7 121.4 . . ? C8 C7 H7 121.4 . . ? N5 C23 C22 121.9(9) . . ? N5 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.001 _refine_diff_density_min -3.036 _refine_diff_density_rms 0.157 # Attachment '- 3.CIF' data_c090530q _database_code_depnum_ccdc_archive 'CCDC 756343' #TrackingRef '- 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H19 Cd11 N8 O1.50 S8.25 Zn' _chemical_formula_weight 2057.78 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' O O 0.0106 0.0060 '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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 17.4744(13) _cell_length_b 9.8931(8) _cell_length_c 25.4804(14) _cell_angle_alpha 90.00 _cell_angle_beta 131.238(3) _cell_angle_gamma 90.00 _cell_volume 3312.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.126 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3780 _exptl_absorpt_coefficient_mu 8.184 _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 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17938 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5834 _reflns_number_gt 4809 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0731P)^2^+20.8424P] 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 5834 _refine_ls_number_parameters 443 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.1193 _refine_ls_R_factor_gt 0.1023 _refine_ls_wR_factor_ref 0.2613 _refine_ls_wR_factor_gt 0.2532 _refine_ls_goodness_of_fit_ref 1.657 _refine_ls_restrained_S_all 1.677 _refine_ls_shift/su_max 0.174 _refine_ls_shift/su_mean 0.015 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 Cd1 Cd 0.45581(7) 0.19744(8) 0.32413(4) 0.0373(3) Uani 1 1 d . . . Zn2 Zn 0.0000 -0.5000 0.0000 0.0183(4) Uani 1 2 d S . . C1 C 0.4121(8) -0.0662(11) 0.2697(6) 0.035(2) Uani 1 1 d . . . C2 C 0.3747(8) -0.1871(11) 0.2241(6) 0.034(2) Uani 1 1 d . . . C3 C 0.3989(8) -0.3145(11) 0.2509(6) 0.037(3) Uani 1 1 d . . . H3 H 0.4430 -0.3262 0.2991 0.045 Uiso 1 1 calc R . . C4 C 0.3594(9) -0.4266(12) 0.2083(6) 0.040(3) Uani 1 1 d . . . C5 C 0.2938(10) -0.4093(12) 0.1362(6) 0.048(3) Uani 1 1 d . . . H5 H 0.2672 -0.4841 0.1068 0.057 Uiso 1 1 calc R . . C6 C 0.2685(10) -0.2797(12) 0.1088(6) 0.046(3) Uani 1 1 d . . . C7 C 0.3070(9) -0.1697(12) 0.1512(6) 0.042(3) Uani 1 1 d . . . H7 H 0.2888 -0.0832 0.1322 0.050 Uiso 1 1 calc R . . C8 C 0.3785(10) -0.5680(12) 0.2365(7) 0.046(3) Uani 1 1 d . . . C10 C 0.3032(12) 0.2061(16) 0.3617(8) 0.063(4) Uani 1 1 d . . . H10 H 0.3642 0.2213 0.4069 0.075 Uiso 1 1 calc R . . C11 C 0.2182(13) 0.2048(18) 0.3514(9) 0.075(5) Uani 1 1 d . . . H11 H 0.2200 0.2194 0.3883 0.090 Uiso 1 1 calc R . . C12 C 0.1282(12) 0.1816(16) 0.2857(9) 0.064(4) Uani 1 1 d . . . C13 C 0.1280(11) 0.1576(16) 0.2321(9) 0.067(4) Uani 1 1 d . . . H13 H 0.0677 0.1396 0.1871 0.081 Uiso 1 1 calc R . . C14 C 0.2193(10) 0.1609(14) 0.2475(8) 0.056(3) Uani 1 1 d . . . H14 H 0.2199 0.1444 0.2118 0.067 Uiso 1 1 calc R . . C15 C 0.5804(10) 0.1468(15) 0.4881(6) 0.056(4) Uani 1 1 d . . . H15 H 0.5706 0.0564 0.4751 0.067 Uiso 1 1 calc R . . C16 C 0.6340(11) 0.1800(16) 0.5581(7) 0.059(4) Uani 1 1 d . . . H16 H 0.6581 0.1123 0.5910 0.071 Uiso 1 1 calc R . . C17 C 0.6503(10) 0.3115(15) 0.5771(7) 0.055(4) Uani 1 1 d . . . C18 C 0.6091(11) 0.4124(16) 0.5256(7) 0.061(4) Uani 1 1 d . . . H18 H 0.6167 0.5034 0.5373 0.073 Uiso 1 1 calc R . . C19 C 0.5575(11) 0.3739(14) 0.4578(7) 0.056(3) Uani 1 1 d . . . H19 H 0.5325 0.4403 0.4241 0.067 Uiso 1 1 calc R . . C20 C 0.8163(10) 0.3262(14) 0.7593(6) 0.047(3) Uani 1 1 d . . . C21 C 0.8547(10) 0.2343(14) 0.8124(6) 0.050(3) Uani 1 1 d . . . H21 H 0.8418 0.1423 0.8031 0.060 Uiso 1 1 calc R . . C22 C 0.9121(10) 0.2823(13) 0.8792(6) 0.048(3) Uani 1 1 d . . . H22 H 0.9373 0.2210 0.9150 0.058 Uiso 1 1 calc R . . C23 C 0.8990(11) 0.5010(14) 0.8439(6) 0.054(3) Uani 1 1 d . . . H23 H 0.9150 0.5920 0.8550 0.065 Uiso 1 1 calc R . . C24 C 0.8413(11) 0.4613(14) 0.7764(7) 0.053(3) Uani 1 1 d . . . H24 H 0.8188 0.5246 0.7419 0.063 Uiso 1 1 calc R . . C25 C 0.0729(10) 0.7614(18) 0.3311(4) 0.081(5) Uani 1 1 d GD . . C26 C 0.1047(11) 0.6372(14) 0.3650(7) 0.124(3) Uani 1 1 d GU . . H26 H 0.0854 0.5578 0.3394 0.148 Uiso 1 1 calc R . . C27 C 0.1654(12) 0.6316(14) 0.4370(7) 0.124(3) Uani 1 1 d GU . . H27 H 0.1867 0.5485 0.4597 0.149 Uiso 1 1 calc R . . N7 N 0.1943(10) 0.7503(19) 0.4752(4) 0.124(3) Uani 1 1 d GU . . C29 C 0.1625(13) 0.8745(15) 0.4414(7) 0.124(3) Uani 1 1 d GU . . H29 H 0.1802 0.9568 0.4644 0.149 Uiso 1 1 calc R . . N1 N 0.3075(8) 0.1869(11) 0.3114(6) 0.050(3) Uani 1 1 d . . . N2 N 0.0368(11) 0.1812(14) 0.2802(7) 0.082(4) Uani 1 1 d . . . N3 N 0.5422(8) 0.2445(12) 0.4387(5) 0.052(3) Uani 1 1 d . . . N4 N 0.7068(9) 0.3608(13) 0.6461(6) 0.061(3) Uani 1 1 d . . . N5 N 0.7573(9) 0.2723(13) 0.6906(5) 0.055(3) Uani 1 1 d . . . N6 N 0.9333(8) 0.4122(11) 0.8950(5) 0.045(2) Uani 1 1 d . . . C30 C 0.1063(12) 0.864(2) 0.3752(9) 0.084(6) Uani 1 1 d G . . H30 H 0.0834 0.9470 0.3527 0.100 Uiso 1 1 calc R . . O1 O 0.4573(8) -0.0739(9) 0.3329(5) 0.061(3) Uani 1 1 d . . . O2 O 0.3934(7) 0.0494(8) 0.2409(4) 0.049(2) Uani 1 1 d . . . O3 O 0.4523(8) -0.5860(9) 0.3001(5) 0.066(3) Uani 1 1 d . . . O4 O 0.3202(8) -0.6608(9) 0.1974(5) 0.064(3) Uani 1 1 d . . . O5 O 0.2210(11) -0.267(2) -0.0103(6) 0.148(8) Uani 1 1 d . . . O6 O 0.1305(13) -0.1262(13) 0.0059(6) 0.149(8) Uani 1 1 d . . . O7 O 0.1014(8) -0.3633(10) -0.0081(4) 0.063(3) Uani 1 1 d . . . O8 O -0.1256(8) -0.3287(9) -0.0617(5) 0.064(3) Uani 1 1 d . . . O9 O 0.6184(7) 0.1650(11) 0.3647(5) 0.063(3) Uani 1 1 d . . . O10 O 0.4246(12) 0.7630(18) 0.0408(8) 0.122(6) Uani 1 1 d . . . O11 O 0.0751(19) 0.0700(16) 0.0730(10) 0.178(9) Uani 1 1 d . . . S1 S 0.1740(3) -0.2590(4) 0.01657(17) 0.0708(13) Uani 1 1 d . . . N8 N 0.0000 0.779(4) 0.2500 0.155(7) Uani 1 2 d SDU . . N9 N 0.0000 0.696(4) 0.2500 0.155(7) Uani 1 2 d SU . . 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 Cd1 0.0437(5) 0.0347(5) 0.0308(5) -0.0059(3) 0.0234(4) -0.0032(4) Zn2 0.0362(9) 0.0124(7) 0.0003(6) -0.0076(5) 0.0095(6) -0.0093(6) C1 0.037(6) 0.030(6) 0.037(6) -0.001(5) 0.024(5) 0.000(5) C2 0.036(6) 0.027(6) 0.042(6) -0.003(5) 0.027(5) -0.004(5) C3 0.035(6) 0.039(6) 0.032(6) 0.003(5) 0.020(5) 0.002(5) C4 0.048(7) 0.035(6) 0.041(6) -0.002(5) 0.031(6) -0.001(5) C5 0.063(8) 0.035(6) 0.038(6) -0.010(5) 0.030(6) -0.010(6) C6 0.059(8) 0.039(7) 0.037(6) -0.005(5) 0.030(6) -0.018(6) C7 0.043(7) 0.031(6) 0.041(6) 0.004(5) 0.023(6) -0.005(5) C8 0.061(8) 0.032(7) 0.053(8) 0.002(6) 0.041(7) 0.005(6) C10 0.060(9) 0.081(11) 0.060(9) -0.007(8) 0.045(8) -0.003(8) C11 0.075(11) 0.099(13) 0.077(11) -0.002(10) 0.062(10) 0.000(10) C12 0.066(10) 0.063(10) 0.093(12) 0.005(8) 0.066(10) 0.001(8) C13 0.049(8) 0.064(10) 0.074(10) 0.006(8) 0.034(8) -0.006(7) C14 0.053(8) 0.058(9) 0.061(9) -0.002(7) 0.040(8) 0.001(7) C15 0.056(8) 0.050(8) 0.039(7) -0.014(6) 0.022(6) -0.005(6) C16 0.063(9) 0.076(10) 0.035(7) -0.006(7) 0.031(7) 0.000(8) C17 0.052(8) 0.071(10) 0.037(7) -0.021(7) 0.027(7) -0.012(7) C18 0.067(9) 0.061(9) 0.044(7) -0.019(7) 0.032(7) -0.007(7) C19 0.066(9) 0.048(8) 0.045(7) -0.008(6) 0.032(7) -0.003(7) C20 0.048(7) 0.063(9) 0.033(6) -0.014(6) 0.028(6) -0.006(6) C21 0.060(8) 0.049(8) 0.042(7) -0.011(6) 0.035(7) -0.007(6) C22 0.059(8) 0.051(8) 0.036(6) -0.009(6) 0.032(6) -0.002(6) C23 0.070(9) 0.050(8) 0.035(6) -0.002(6) 0.032(7) -0.008(7) C24 0.062(9) 0.050(8) 0.039(7) -0.006(6) 0.030(7) -0.003(6) C25 0.074(11) 0.096(13) 0.096(13) -0.024(11) 0.066(11) -0.011(10) C26 0.124(4) 0.124(4) 0.124(4) -0.0001(8) 0.082(2) 0.0000(8) C27 0.124(3) 0.124(4) 0.124(3) 0.0000(7) 0.082(2) 0.0001(7) N7 0.124(3) 0.124(4) 0.124(3) -0.0001(7) 0.082(2) 0.0002(7) C29 0.124(4) 0.124(4) 0.124(4) -0.0002(8) 0.082(2) 0.0003(8) N1 0.050(6) 0.052(7) 0.052(6) -0.008(5) 0.035(6) -0.009(5) N2 0.096(12) 0.083(10) 0.064(8) -0.003(7) 0.051(8) -0.003(8) N3 0.050(6) 0.065(7) 0.036(5) -0.007(5) 0.027(5) 0.001(6) N4 0.061(7) 0.074(9) 0.039(6) -0.020(6) 0.029(6) -0.003(7) N5 0.049(6) 0.076(8) 0.032(6) -0.009(6) 0.023(5) -0.005(6) N6 0.055(6) 0.046(6) 0.031(5) -0.005(4) 0.027(5) -0.007(5) C30 0.056(10) 0.117(15) 0.071(11) 0.046(11) 0.040(9) 0.024(10) O1 0.079(7) 0.041(5) 0.046(5) -0.009(4) 0.033(5) 0.003(5) O2 0.069(6) 0.032(4) 0.048(5) -0.010(4) 0.039(5) -0.010(4) O3 0.082(7) 0.040(5) 0.051(6) 0.009(4) 0.034(6) 0.007(5) O4 0.094(8) 0.028(5) 0.071(6) -0.003(4) 0.054(6) -0.008(5) O5 0.102(10) 0.28(2) 0.050(7) -0.026(10) 0.047(7) -0.103(13) O6 0.174(15) 0.054(8) 0.056(7) 0.012(6) 0.005(9) -0.003(9) O7 0.071(6) 0.064(6) 0.039(5) -0.009(4) 0.031(5) -0.029(5) O8 0.073(7) 0.046(5) 0.061(6) 0.002(4) 0.039(5) 0.010(5) O9 0.052(6) 0.077(7) 0.056(6) -0.006(5) 0.034(5) 0.002(5) O10 0.125(12) 0.166(15) 0.106(11) -0.050(10) 0.088(11) -0.043(11) O11 0.30(3) 0.076(11) 0.159(17) -0.010(11) 0.149(19) -0.028(14) S1 0.086(3) 0.059(2) 0.0331(17) -0.0015(15) 0.0245(19) -0.034(2) N8 0.155(7) 0.155(7) 0.155(7) 0.000 0.102(5) 0.000 N9 0.155(7) 0.155(7) 0.155(7) 0.000 0.102(5) 0.000 _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 Cd1 O2 2.188(8) . ? Cd1 O3 2.218(9) 1_565 ? Cd1 N3 2.283(10) . ? Cd1 O9 2.317(9) . ? Cd1 N1 2.393(11) . ? Zn2 N6 2.272(9) 1_444 ? Zn2 N6 2.272(9) 3_656 ? Zn2 O7 2.344(9) . ? Zn2 O7 2.344(9) 3_545 ? Zn2 O8 2.369(9) . ? Zn2 O8 2.369(9) 3_545 ? C1 O1 1.243(13) . ? C1 O2 1.279(13) . ? C1 C2 1.485(15) . ? C2 C3 1.361(15) . ? C2 C7 1.408(16) . ? C3 C4 1.377(16) . ? C3 H3 0.9300 . ? C4 C5 1.393(16) . ? C4 C8 1.506(16) . ? C5 C6 1.386(17) . ? C5 H5 0.9300 . ? C6 C7 1.360(16) . ? C6 S1 1.781(12) . ? C7 H7 0.9300 . ? C8 O4 1.239(15) . ? C8 O3 1.252(15) . ? C10 N1 1.346(17) . ? C10 C11 1.33(2) . ? C10 H10 0.9300 . ? C11 C12 1.36(2) . ? C11 H11 0.9300 . ? C12 C13 1.38(2) . ? C12 N2 1.51(2) . ? C13 C14 1.37(2) . ? C13 H13 0.9300 . ? C14 N1 1.336(17) . ? C14 H14 0.9300 . ? C15 N3 1.361(17) . ? C15 C16 1.401(17) . ? C15 H15 0.9300 . ? C16 C17 1.35(2) . ? C16 H16 0.9300 . ? C17 C18 1.41(2) . ? C17 N4 1.421(15) . ? C18 C19 1.374(17) . ? C18 H18 0.9300 . ? C19 N3 1.332(17) . ? C19 H19 0.9300 . ? C20 C21 1.383(18) . ? C20 C24 1.385(18) . ? C20 N5 1.425(15) . ? C21 C22 1.370(17) . ? C21 H21 0.9300 . ? C22 N6 1.325(16) . ? C22 H22 0.9300 . ? C23 N6 1.340(16) . ? C23 C24 1.356(17) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.3900 . ? C25 C30 1.33(2) . ? C25 N8 1.566(8) . ? C25 N9 1.687(18) . ? C26 C27 1.3900 . ? C26 H26 0.9300 . ? C27 N7 1.3900 . ? C27 H27 0.9300 . ? N7 C29 1.3900 . ? C29 C30 1.279(19) . ? C29 H29 0.9300 . ? N2 N2 1.19(3) 2 ? N4 N5 1.229(16) . ? N6 Zn2 2.272(9) 1_666 ? C30 H30 0.9300 . ? O3 Cd1 2.218(9) 1_545 ? O5 S1 1.375(15) . ? O6 S1 1.451(15) . ? O7 S1 1.421(10) . ? N8 N9 0.83(5) . ? N8 C25 1.566(8) 2 ? N9 C25 1.687(18) 2 ? 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 Cd1 O3 118.3(3) . 1_565 ? O2 Cd1 N3 149.7(4) . . ? O3 Cd1 N3 91.8(4) 1_565 . ? O2 Cd1 O9 91.2(3) . . ? O3 Cd1 O9 93.4(4) 1_565 . ? N3 Cd1 O9 82.8(4) . . ? O2 Cd1 N1 92.1(4) . . ? O3 Cd1 N1 100.0(4) 1_565 . ? N3 Cd1 N1 85.8(4) . . ? O9 Cd1 N1 162.6(4) . . ? N6 Zn2 N6 180.0(3) 1_444 3_656 ? N6 Zn2 O7 87.0(3) 1_444 . ? N6 Zn2 O7 93.0(3) 3_656 . ? N6 Zn2 O7 93.0(3) 1_444 3_545 ? N6 Zn2 O7 87.0(3) 3_656 3_545 ? O7 Zn2 O7 180.0(4) . 3_545 ? N6 Zn2 O8 87.7(4) 1_444 . ? N6 Zn2 O8 92.3(4) 3_656 . ? O7 Zn2 O8 87.2(4) . . ? O7 Zn2 O8 92.8(4) 3_545 . ? N6 Zn2 O8 92.3(4) 1_444 3_545 ? N6 Zn2 O8 87.7(4) 3_656 3_545 ? O7 Zn2 O8 92.8(4) . 3_545 ? O7 Zn2 O8 87.2(4) 3_545 3_545 ? O8 Zn2 O8 179.999(1) . 3_545 ? O1 C1 O2 120.1(10) . . ? O1 C1 C2 122.6(10) . . ? O2 C1 C2 117.2(10) . . ? C3 C2 C7 119.2(10) . . ? C3 C2 C1 121.5(10) . . ? C7 C2 C1 119.1(10) . . ? C4 C3 C2 121.4(10) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 119.4(11) . . ? C3 C4 C8 122.2(10) . . ? C5 C4 C8 118.3(11) . . ? C6 C5 C4 119.4(11) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C7 C6 C5 120.9(11) . . ? C7 C6 S1 120.0(10) . . ? C5 C6 S1 118.8(9) . . ? C6 C7 C2 119.7(11) . . ? C6 C7 H7 120.1 . . ? C2 C7 H7 120.1 . . ? O4 C8 O3 122.4(12) . . ? O4 C8 C4 119.9(12) . . ? O3 C8 C4 117.7(11) . . ? N1 C10 C11 124.6(15) . . ? N1 C10 H10 117.7 . . ? C11 C10 H10 117.7 . . ? C12 C11 C10 118.6(15) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C11 C12 C13 119.5(14) . . ? C11 C12 N2 114.0(13) . . ? C13 C12 N2 126.4(15) . . ? C14 C13 C12 118.0(15) . . ? C14 C13 H13 121.0 . . ? C12 C13 H13 121.0 . . ? N1 C14 C13 122.9(14) . . ? N1 C14 H14 118.6 . . ? C13 C14 H14 118.5 . . ? N3 C15 C16 121.2(13) . . ? N3 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C17 C16 C15 119.2(14) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C18 C17 C16 119.3(12) . . ? C18 C17 N4 114.9(13) . . ? C16 C17 N4 125.8(14) . . ? C17 C18 C19 118.8(13) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? N3 C19 C18 122.2(14) . . ? N3 C19 H19 118.9 . . ? C18 C19 H19 118.9 . . ? C21 C20 C24 118.5(11) . . ? C21 C20 N5 116.6(12) . . ? C24 C20 N5 124.8(12) . . ? C20 C21 C22 118.2(12) . . ? C20 C21 H21 120.9 . . ? C22 C21 H21 120.9 . . ? N6 C22 C21 122.9(12) . . ? N6 C22 H22 118.6 . . ? C21 C22 H22 118.5 . . ? N6 C23 C24 121.6(13) . . ? N6 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C20 C24 C23 119.7(13) . . ? C20 C24 H24 120.1 . . ? C23 C24 H24 120.2 . . ? C26 C25 C30 112.1(8) . . ? C26 C25 N8 124.3(17) . . ? C30 C25 N8 123.5(18) . . ? C26 C25 N9 95.2(15) . . ? C30 C25 N9 152.4(17) . . ? N8 C25 N9 29.1(17) . . ? C27 C26 C25 120.0 . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 N7 120.0 . . ? C26 C27 H27 120.0 . . ? N7 C27 H27 120.0 . . ? C29 N7 C27 120.0 . . ? N7 C29 C30 113.0(11) . . ? N7 C29 H29 123.4 . . ? C30 C29 H29 123.6 . . ? C14 N1 C10 116.4(12) . . ? C14 N1 Cd1 116.7(9) . . ? C10 N1 Cd1 126.8(9) . . ? N2 N2 C12 107.4(18) 2 . ? C15 N3 C19 119.2(11) . . ? C15 N3 Cd1 123.0(9) . . ? C19 N3 Cd1 117.8(9) . . ? N5 N4 C17 112.8(12) . . ? N4 N5 C20 111.4(12) . . ? C22 N6 C23 119.0(11) . . ? C22 N6 Zn2 123.5(8) . 1_666 ? C23 N6 Zn2 116.5(8) . 1_666 ? C29 C30 C25 134.9(17) . . ? C29 C30 H30 112.5 . . ? C25 C30 H30 112.6 . . ? C1 O2 Cd1 105.4(7) . . ? C8 O3 Cd1 108.2(8) . 1_545 ? S1 O7 Zn2 152.5(6) . . ? O5 S1 O7 112.8(9) . . ? O5 S1 O6 112.0(12) . . ? O7 S1 O6 111.7(9) . . ? O5 S1 C6 108.1(8) . . ? O7 S1 C6 106.3(5) . . ? O6 S1 C6 105.5(7) . . ? N9 N8 C25 83.5(15) . . ? N9 N8 C25 83.5(15) . 2 ? C25 N8 C25 167(3) . 2 ? N8 N9 C25 67.3(13) . . ? N8 N9 C25 67.3(13) . 2 ? C25 N9 C25 135(3) . 2 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 5.084 _refine_diff_density_min -1.666 _refine_diff_density_rms 0.227 # Attachment '- 4.CIF' data_p090718f _database_code_depnum_ccdc_archive 'CCDC 756345' #TrackingRef '- 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H7.50 Cd2.25 O8 S0.50' _chemical_formula_weight 452.53 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 25.0558(7) _cell_length_b 6.88418(18) _cell_length_c 11.5251(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.977(3) _cell_angle_gamma 90.00 _cell_volume 1879.90(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1692 _exptl_absorpt_coefficient_mu 5.205 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.3561 _exptl_absorpt_correction_T_max 0.4225 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3520 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1807 _reflns_number_gt 1644 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0332P)^2^+1.0484P] 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 1807 _refine_ls_number_parameters 180 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0574 _refine_ls_wR_factor_gt 0.0564 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.056 _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 Cd1 Cd 0.5000 0.5000 0.0000 0.01152(16) Uani 1 4 d S . . Cd2 Cd 0.745903(17) 1.0000 0.95626(4) 0.00876(12) Uani 1 2 d S . . Cd3 Cd 0.520634(17) 1.0000 0.19478(4) 0.00950(13) Uani 1 2 d S . . Cd4 Cd 0.881469(12) 0.74215(4) 0.96501(3) 0.00877(11) Uani 1 1 d . . . C1 C 0.7808(2) 1.0000 0.6004(5) 0.0099(12) Uani 1 2 d S . . C2 C 0.7267(2) 1.0000 0.5116(5) 0.0114(13) Uani 1 2 d S . . H2 H 0.6949 1.0000 0.5362 0.014 Uiso 1 2 calc SR . . C3 C 0.7206(2) 1.0000 0.3864(5) 0.0098(12) Uani 1 2 d S . . C4 C 0.7684(2) 1.0000 0.3497(5) 0.0124(13) Uani 1 2 d S . . H4 H 0.7647 1.0000 0.2667 0.015 Uiso 1 2 calc SR . . C5 C 0.8214(2) 1.0000 0.4370(6) 0.0121(13) Uani 1 2 d S . . C6 C 0.8277(2) 1.0000 0.5613(5) 0.0120(13) Uani 1 2 d S . . H6 H 0.8637 1.0000 0.6190 0.014 Uiso 1 2 calc SR . . C7 C 0.7868(2) 1.0000 0.7336(5) 0.0100(12) Uani 1 2 d S . . C8 C 0.6623(2) 1.0000 0.2909(5) 0.0106(13) Uani 1 2 d S . . O1 O 0.83679(17) 1.0000 0.8099(4) 0.0128(9) Uani 1 2 d S . . O2 O 0.74301(17) 1.0000 0.7615(4) 0.0194(10) Uani 1 2 d S . . O3 O 0.62020(16) 1.0000 0.3258(4) 0.0145(10) Uani 1 2 d S . . O4 O 0.66221(17) 1.0000 0.1786(4) 0.0124(9) Uani 1 2 d S . . O5 O 0.91320(14) 0.8250(6) 0.4405(3) 0.0324(9) Uani 1 1 d . . . O6 O 0.86229(18) 1.0000 0.2571(4) 0.0187(10) Uani 1 2 d S . . O7 O 0.80923(12) 0.7567(4) 1.0396(3) 0.0098(7) Uani 1 1 d . . . O8 O 0.92771(16) 0.5000 1.0909(4) 0.0099(9) Uani 1 2 d S . . O9 O 0.92534(17) 1.0000 1.0700(4) 0.0091(9) Uani 1 2 d S . . O10 O 0.50728(16) 1.2293(6) 0.3368(3) 0.0342(10) Uani 1 1 d D . . O11 O 0.55177(12) 0.7362(4) 0.1257(3) 0.0110(7) Uani 1 1 d . . . O12 O 0.3842(2) 1.0000 0.2854(5) 0.0449(15) Uani 1 2 d S . . H12A H 0.3627 1.0877 0.2428 0.054 Uiso 0.50 1 d PR . . H12B H 0.3694 0.8906 0.2594 0.054 Uiso 0.50 1 d PR . . S1 S 0.88196(6) 1.0000 0.38990(14) 0.0150(3) Uani 1 2 d S . . H7 H 0.825(2) 0.795(8) 1.091(4) 0.018 Uiso 1 1 d . . . H11 H 0.565(2) 0.696(8) 0.177(5) 0.018 Uiso 1 1 d . . . H10A H 0.5346(10) 1.272(6) 0.397(3) 0.018 Uiso 1 1 d D . . H10B H 0.4758(8) 1.216(6) 0.351(3) 0.018 Uiso 1 1 d D . . H9 H 0.930(3) 1.0000 1.132(6) 0.018 Uiso 1 2 d S . . H8 H 0.911(3) 0.5000 1.143(6) 0.018 Uiso 1 2 d S . . 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 Cd1 0.0058(3) 0.0072(3) 0.0226(3) 0.000 0.0061(2) 0.000 Cd2 0.0102(2) 0.0064(2) 0.0129(2) 0.000 0.00821(17) 0.000 Cd3 0.0082(2) 0.0105(2) 0.0106(2) 0.000 0.00410(17) 0.000 Cd4 0.00657(17) 0.00720(19) 0.01391(18) -0.00058(13) 0.00523(13) -0.00066(12) C1 0.014(3) 0.006(3) 0.010(3) 0.000 0.004(2) 0.000 C2 0.007(3) 0.011(3) 0.017(3) 0.000 0.005(2) 0.000 C3 0.007(3) 0.005(3) 0.013(3) 0.000 -0.001(2) 0.000 C4 0.016(3) 0.009(3) 0.012(3) 0.000 0.004(2) 0.000 C5 0.008(3) 0.013(3) 0.018(3) 0.000 0.008(2) 0.000 C6 0.006(3) 0.011(3) 0.015(3) 0.000 -0.002(2) 0.000 C7 0.013(3) 0.004(3) 0.011(3) 0.000 0.001(2) 0.000 C8 0.016(3) 0.004(3) 0.009(3) 0.000 -0.001(2) 0.000 O1 0.014(2) 0.012(2) 0.011(2) 0.000 0.0033(17) 0.000 O2 0.015(2) 0.035(3) 0.008(2) 0.000 0.0044(17) 0.000 O3 0.006(2) 0.025(3) 0.012(2) 0.000 0.0033(16) 0.000 O4 0.013(2) 0.012(2) 0.011(2) 0.000 0.0013(17) 0.000 O5 0.0222(18) 0.046(2) 0.0314(19) 0.0149(19) 0.0127(15) 0.0182(18) O6 0.018(2) 0.029(3) 0.010(2) 0.000 0.0068(18) 0.000 O7 0.0097(15) 0.0090(17) 0.0105(15) -0.0018(13) 0.0028(12) -0.0017(12) O8 0.005(2) 0.014(2) 0.012(2) 0.000 0.0041(16) 0.000 O9 0.010(2) 0.009(2) 0.0086(19) 0.000 0.0040(17) 0.000 O10 0.029(2) 0.053(3) 0.0232(18) -0.0186(19) 0.0121(16) -0.0008(19) O11 0.0100(16) 0.0122(18) 0.0121(15) -0.0011(14) 0.0053(13) 0.0009(12) O12 0.047(4) 0.052(4) 0.048(4) 0.000 0.031(3) 0.000 S1 0.0090(7) 0.0251(9) 0.0124(7) 0.000 0.0056(6) 0.000 _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 Cd1 O9 2.265(4) 7_666 ? Cd1 O9 2.265(4) 3_444 ? Cd1 O11 2.281(3) . ? Cd1 O11 2.281(3) 5_665 ? Cd1 O11 2.281(3) 6_565 ? Cd1 O11 2.281(3) 2_655 ? Cd1 Cd4 3.3697(3) 7_666 ? Cd1 Cd4 3.3697(3) 4_646 ? Cd1 Cd4 3.3697(3) 3_444 ? Cd1 Cd4 3.3697(3) 8_464 ? Cd2 O2 2.222(4) . ? Cd2 O7 2.253(3) 7_667 ? Cd2 O7 2.253(3) 4_657 ? Cd2 O7 2.293(3) 6_575 ? Cd2 O7 2.293(3) . ? Cd3 O11 2.224(3) 6_575 ? Cd3 O11 2.224(3) . ? Cd3 O8 2.245(4) 3_454 ? Cd3 O10 2.374(3) . ? Cd3 O10 2.374(3) 6_575 ? Cd3 O3 2.460(4) . ? Cd4 O9 2.227(2) . ? Cd4 O7 2.245(3) . ? Cd4 O11 2.247(3) 7_666 ? Cd4 O8 2.266(3) . ? Cd4 O4 2.354(3) 7_666 ? Cd4 O1 2.509(3) . ? Cd4 Cd4 3.3341(6) 6_565 ? Cd4 Cd1 3.3697(3) 3_556 ? C1 C6 1.388(8) . ? C1 C2 1.409(8) . ? C1 C7 1.492(8) . ? C2 C3 1.400(8) . ? C3 C4 1.396(8) . ? C3 C8 1.517(8) . ? C4 C5 1.380(8) . ? C5 C6 1.390(8) . ? C5 S1 1.770(6) . ? C7 O2 1.241(7) . ? C7 O1 1.275(7) . ? C8 O3 1.244(7) . ? C8 O4 1.293(7) . ? O1 Cd4 2.509(3) 6_575 ? O4 Cd4 2.354(3) 7_666 ? O4 Cd4 2.354(3) 4_656 ? O5 S1 1.452(3) . ? O6 S1 1.447(4) . ? O7 Cd2 2.253(3) 7_667 ? O8 Cd3 2.245(4) 3_546 ? O8 Cd4 2.266(3) 6_565 ? O9 Cd4 2.227(2) 6_575 ? O9 Cd1 2.265(4) 3_556 ? O11 Cd4 2.247(3) 7_666 ? S1 O5 1.452(4) 6_575 ? 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 O9 Cd1 O9 180.00(16) 7_666 3_444 ? O9 Cd1 O11 82.03(10) 7_666 . ? O9 Cd1 O11 97.97(10) 3_444 . ? O9 Cd1 O11 97.97(10) 7_666 5_665 ? O9 Cd1 O11 82.03(10) 3_444 5_665 ? O11 Cd1 O11 180.00(15) . 5_665 ? O9 Cd1 O11 82.03(10) 7_666 6_565 ? O9 Cd1 O11 97.97(10) 3_444 6_565 ? O11 Cd1 O11 90.94(15) . 6_565 ? O11 Cd1 O11 89.06(15) 5_665 6_565 ? O9 Cd1 O11 97.97(10) 7_666 2_655 ? O9 Cd1 O11 82.03(10) 3_444 2_655 ? O11 Cd1 O11 89.06(15) . 2_655 ? O11 Cd1 O11 90.94(15) 5_665 2_655 ? O11 Cd1 O11 180.0(2) 6_565 2_655 ? O9 Cd1 Cd4 40.97(6) 7_666 7_666 ? O9 Cd1 Cd4 139.03(6) 3_444 7_666 ? O11 Cd1 Cd4 41.53(8) . 7_666 ? O11 Cd1 Cd4 138.47(8) 5_665 7_666 ? O11 Cd1 Cd4 90.14(7) 6_565 7_666 ? O11 Cd1 Cd4 89.86(7) 2_655 7_666 ? O9 Cd1 Cd4 40.97(6) 7_666 4_646 ? O9 Cd1 Cd4 139.03(6) 3_444 4_646 ? O11 Cd1 Cd4 90.14(7) . 4_646 ? O11 Cd1 Cd4 89.86(7) 5_665 4_646 ? O11 Cd1 Cd4 41.53(8) 6_565 4_646 ? O11 Cd1 Cd4 138.47(8) 2_655 4_646 ? Cd4 Cd1 Cd4 63.575(10) 7_666 4_646 ? O9 Cd1 Cd4 139.03(6) 7_666 3_444 ? O9 Cd1 Cd4 40.97(6) 3_444 3_444 ? O11 Cd1 Cd4 138.47(8) . 3_444 ? O11 Cd1 Cd4 41.53(8) 5_665 3_444 ? O11 Cd1 Cd4 89.86(7) 6_565 3_444 ? O11 Cd1 Cd4 90.14(7) 2_655 3_444 ? Cd4 Cd1 Cd4 180.000(10) 7_666 3_444 ? Cd4 Cd1 Cd4 116.425(10) 4_646 3_444 ? O9 Cd1 Cd4 139.03(6) 7_666 8_464 ? O9 Cd1 Cd4 40.97(6) 3_444 8_464 ? O11 Cd1 Cd4 89.86(7) . 8_464 ? O11 Cd1 Cd4 90.14(7) 5_665 8_464 ? O11 Cd1 Cd4 138.47(8) 6_565 8_464 ? O11 Cd1 Cd4 41.53(8) 2_655 8_464 ? Cd4 Cd1 Cd4 116.425(10) 7_666 8_464 ? Cd4 Cd1 Cd4 180.000(10) 4_646 8_464 ? Cd4 Cd1 Cd4 63.575(10) 3_444 8_464 ? O2 Cd2 O7 101.68(10) . 7_667 ? O2 Cd2 O7 101.68(10) . 4_657 ? O7 Cd2 O7 103.31(15) 7_667 4_657 ? O2 Cd2 O7 102.37(10) . 6_575 ? O7 Cd2 O7 155.49(3) 7_667 6_575 ? O7 Cd2 O7 76.33(12) 4_657 6_575 ? O2 Cd2 O7 102.37(10) . . ? O7 Cd2 O7 76.33(12) 7_667 . ? O7 Cd2 O7 155.49(3) 4_657 . ? O7 Cd2 O7 93.89(14) 6_575 . ? O11 Cd3 O11 109.51(16) 6_575 . ? O11 Cd3 O8 103.47(10) 6_575 3_454 ? O11 Cd3 O8 103.47(10) . 3_454 ? O11 Cd3 O10 81.28(13) 6_575 . ? O11 Cd3 O10 159.10(12) . . ? O8 Cd3 O10 90.75(12) 3_454 . ? O11 Cd3 O10 159.10(12) 6_575 6_575 ? O11 Cd3 O10 81.28(13) . 6_575 ? O8 Cd3 O10 90.75(12) 3_454 6_575 ? O10 Cd3 O10 83.3(2) . 6_575 ? O11 Cd3 O3 79.39(9) 6_575 . ? O11 Cd3 O3 79.39(9) . . ? O8 Cd3 O3 174.80(14) 3_454 . ? O10 Cd3 O3 85.36(11) . . ? O10 Cd3 O3 85.36(11) 6_575 . ? O9 Cd4 O7 94.20(13) . . ? O9 Cd4 O11 83.65(13) . 7_666 ? O7 Cd4 O11 171.98(11) . 7_666 ? O9 Cd4 O8 100.32(11) . . ? O7 Cd4 O8 95.47(13) . . ? O11 Cd4 O8 92.51(13) 7_666 . ? O9 Cd4 O4 168.92(13) . 7_666 ? O7 Cd4 O4 93.02(12) . 7_666 ? O11 Cd4 O4 88.05(12) 7_666 7_666 ? O8 Cd4 O4 87.33(10) . 7_666 ? O9 Cd4 O1 81.39(11) . . ? O7 Cd4 O1 90.74(12) . . ? O11 Cd4 O1 81.31(12) 7_666 . ? O8 Cd4 O1 173.40(14) . . ? O4 Cd4 O1 90.13(9) 7_666 . ? O9 Cd4 Cd4 142.85(8) . 6_565 ? O7 Cd4 Cd4 92.55(7) . 6_565 ? O11 Cd4 Cd4 93.81(8) 7_666 6_565 ? O8 Cd4 Cd4 42.63(7) . 6_565 ? O4 Cd4 Cd4 44.90(7) 7_666 6_565 ? O1 Cd4 Cd4 135.02(6) . 6_565 ? O9 Cd4 Cd1 41.84(11) . 3_556 ? O7 Cd4 Cd1 136.04(7) . 3_556 ? O11 Cd4 Cd1 42.29(8) 7_666 3_556 ? O8 Cd4 Cd1 93.65(9) . 3_556 ? O4 Cd4 Cd1 130.35(10) 7_666 3_556 ? O1 Cd4 Cd1 83.35(8) . 3_556 ? Cd4 Cd4 Cd1 121.788(5) 6_565 3_556 ? C6 C1 C2 118.7(5) . . ? C6 C1 C7 121.4(5) . . ? C2 C1 C7 119.9(5) . . ? C3 C2 C1 120.4(5) . . ? C4 C3 C2 119.7(5) . . ? C4 C3 C8 120.0(5) . . ? C2 C3 C8 120.3(5) . . ? C5 C4 C3 119.7(6) . . ? C4 C5 C6 120.8(6) . . ? C4 C5 S1 119.5(5) . . ? C6 C5 S1 119.7(4) . . ? C1 C6 C5 120.7(5) . . ? O2 C7 O1 125.0(6) . . ? O2 C7 C1 117.7(5) . . ? O1 C7 C1 117.3(5) . . ? O3 C8 O4 126.7(5) . . ? O3 C8 C3 118.9(5) . . ? O4 C8 C3 114.4(5) . . ? C7 O1 Cd4 127.03(19) . 6_575 ? C7 O1 Cd4 127.03(19) . . ? Cd4 O1 Cd4 90.04(13) 6_575 . ? C7 O2 Cd2 121.4(4) . . ? C8 O3 Cd3 126.7(4) . . ? C8 O4 Cd4 123.6(2) . 7_666 ? C8 O4 Cd4 123.6(2) . 4_656 ? Cd4 O4 Cd4 90.19(13) 7_666 4_656 ? Cd4 O7 Cd2 123.34(13) . 7_667 ? Cd4 O7 Cd2 113.97(12) . . ? Cd2 O7 Cd2 103.67(12) 7_667 . ? Cd3 O8 Cd4 124.54(11) 3_546 6_565 ? Cd3 O8 Cd4 124.54(11) 3_546 . ? Cd4 O8 Cd4 94.73(15) 6_565 . ? Cd4 O9 Cd4 105.71(17) . 6_575 ? Cd4 O9 Cd1 97.19(13) . 3_556 ? Cd4 O9 Cd1 97.19(13) 6_575 3_556 ? Cd3 O11 Cd4 120.88(14) . 7_666 ? Cd3 O11 Cd1 128.05(13) . . ? Cd4 O11 Cd1 96.18(11) 7_666 . ? O6 S1 O5 112.26(17) . 6_575 ? O6 S1 O5 112.26(17) . . ? O5 S1 O5 112.2(3) 6_575 . ? O6 S1 C5 107.1(3) . . ? O5 S1 C5 106.30(18) 6_575 . ? O5 S1 C5 106.30(18) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.703 _refine_diff_density_min -0.909 _refine_diff_density_rms 0.168 # Attachment '- 2.CIF' data_p090718z _database_code_depnum_ccdc_archive 'CCDC 756347' #TrackingRef '- 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H19 N8 O11 S Zn1.50' _chemical_formula_weight 773.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' Zn Zn 0.2839 1.4301 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 17.181(3) _cell_length_b 9.5978(11) _cell_length_c 24.677(3) _cell_angle_alpha 90.00 _cell_angle_beta 130.288(9) _cell_angle_gamma 90.00 _cell_volume 3104.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 25.01 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 1.311 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7353 _exptl_absorpt_correction_T_max 0.7795 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12517 _diffrn_reflns_av_R_equivalents 0.0768 _diffrn_reflns_av_sigmaI/netI 0.1218 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5383 _reflns_number_gt 3309 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1051P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5383 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1290 _refine_ls_R_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.1950 _refine_ls_wR_factor_gt 0.1777 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 O7 O 0.0956(4) 0.8555(6) -0.0058(2) 0.0244(13) Uani 1 1 d . . . Zn1 Zn 0.45750(6) 0.30619(9) 0.32971(4) 0.0166(3) Uani 1 1 d . . . Zn2 Zn 1.0000 0.0000 1.0000 0.0224(3) Uani 1 2 d S . . C1 C 0.9038(5) -0.0090(9) 0.8479(4) 0.0212(18) Uani 1 1 d . . . H1 H 0.9201 -0.1029 0.8585 0.025 Uiso 1 1 calc R . . C2 C 0.8435(6) 0.0317(8) 0.7775(4) 0.0208(18) Uani 1 1 d . . . H2 H 0.8184 -0.0326 0.7414 0.025 Uiso 1 1 calc R . . C3 C 0.8222(5) 0.1726(8) 0.7633(3) 0.0179(17) Uani 1 1 d . . . C4 C 0.8638(5) 0.2656(9) 0.8179(4) 0.0212(18) Uani 1 1 d . . . H4 H 0.8528 0.3609 0.8091 0.025 Uiso 1 1 calc R . . C5 C 0.9229(6) 0.2140(8) 0.8871(4) 0.0215(18) Uani 1 1 d . . . H5 H 0.9516 0.2762 0.9246 0.026 Uiso 1 1 calc R . . C6 C 0.6450(5) 0.1916(9) 0.5758(4) 0.0181(17) Uani 1 1 d . . . C7 C 0.6277(5) 0.3303(8) 0.5567(4) 0.0210(18) Uani 1 1 d . . . H7 H 0.6519 0.4004 0.5902 0.025 Uiso 1 1 calc R . . C8 C 0.5727(6) 0.3609(8) 0.4856(4) 0.0213(18) Uani 1 1 d . . . H8 H 0.5607 0.4540 0.4718 0.026 Uiso 1 1 calc R . . C9 C 0.5515(6) 0.1319(9) 0.4546(4) 0.0222(18) Uani 1 1 d . . . H9 H 0.5253 0.0644 0.4196 0.027 Uiso 1 1 calc R . . C10 C 0.6050(6) 0.0894(9) 0.5243(4) 0.0244(19) Uani 1 1 d . . . H10 H 0.6138 -0.0046 0.5361 0.029 Uiso 1 1 calc R . . C11 C 0.4182(5) 0.5699(8) 0.2824(4) 0.0164(17) Uani 1 1 d . . . C12 C 0.3777(5) 0.6903(8) 0.2311(4) 0.0174(16) Uani 1 1 d . . . C13 C 0.3096(5) 0.6620(8) 0.1582(4) 0.0162(17) Uani 1 1 d . . . H13 H 0.2934 0.5708 0.1416 0.019 Uiso 1 1 calc R . . C14 C 0.2668(5) 0.7729(7) 0.1114(4) 0.0149(16) Uani 1 1 d . . . C15 C 0.2899(6) 0.9082(8) 0.1350(4) 0.0183(17) Uani 1 1 d . . . H15 H 0.2619 0.9812 0.1026 0.022 Uiso 1 1 calc R . . C16 C 0.3556(5) 0.9358(8) 0.2076(4) 0.0179(17) Uani 1 1 d . . . C17 C 0.3992(5) 0.8266(8) 0.2555(4) 0.0185(17) Uani 1 1 d . . . H17 H 0.4429 0.8446 0.3041 0.022 Uiso 1 1 calc R . . C18 C 0.3691(6) 1.0848(8) 0.2301(4) 0.0186(18) Uani 1 1 d . . . C19 C 0.3077(6) 0.2906(8) 0.3658(4) 0.0266(19) Uani 1 1 d . . . H19 H 0.3677 0.2707 0.4114 0.032 Uiso 1 1 calc R . . C20 C 0.2181(7) 0.2932(10) 0.3543(5) 0.039(2) Uani 1 1 d . . . H20 H 0.2178 0.2767 0.3913 0.047 Uiso 1 1 calc R . . C21 C 0.1292(7) 0.3206(9) 0.2870(5) 0.037(2) Uani 1 1 d . . . C22 C 0.1311(6) 0.3470(8) 0.2330(4) 0.032(2) Uani 1 1 d . . . H22 H 0.0714 0.3669 0.1873 0.038 Uiso 1 1 calc R . . C23 C 0.2259(6) 0.3429(9) 0.2488(4) 0.027(2) Uani 1 1 d . . . H23 H 0.2275 0.3600 0.2125 0.032 Uiso 1 1 calc R . . C24 C 0.1822(7) 0.6419(14) 0.4542(6) 0.057(3) Uani 1 1 d . . . H24 H 0.2023 0.5582 0.4789 0.069 Uiso 1 1 calc R . . C25 C 0.1153(7) 0.6368(12) 0.3809(5) 0.043(3) Uani 1 1 d . . . H25 H 0.0914 0.5516 0.3575 0.052 Uiso 1 1 calc R . . C26 C 0.0853(7) 0.7558(13) 0.3440(5) 0.045(3) Uani 1 1 d . . . C27 C 0.1205(9) 0.8858(14) 0.3810(8) 0.066(4) Uani 1 1 d . . . H27 H 0.1007 0.9715 0.3580 0.079 Uiso 1 1 calc R . . C28 C 0.1873(10) 0.8729(16) 0.4551(8) 0.072(4) Uani 1 1 d . . . H28 H 0.2114 0.9550 0.4814 0.087 Uiso 1 1 calc R . . N1 N 0.5363(5) 0.2642(7) 0.4360(3) 0.0177(14) Uani 1 1 d . . . N2 N 0.7026(5) 0.1405(7) 0.6472(3) 0.0228(16) Uani 1 1 d . . . N3 N 0.7611(5) 0.2297(7) 0.6929(3) 0.0225(16) Uani 1 1 d . . . N4 N 0.9394(4) 0.0780(7) 0.9010(3) 0.0164(14) Uani 1 1 d . . . N5 N 0.3141(5) 0.3155(7) 0.3141(3) 0.0221(15) Uani 1 1 d . . . N6 N 0.0366(6) 0.3200(8) 0.2800(3) 0.0396(19) Uani 1 1 d . . . N7 N 0.2187(7) 0.7564(14) 0.4905(5) 0.064(3) Uani 1 1 d . . . N8 N 0.0191(10) 0.7524(17) 0.2684(5) 0.148(6) Uani 1 1 d . . . O1 O 0.4061(4) 0.4485(5) 0.2568(3) 0.0182(12) Uani 1 1 d . . . O2 O 0.4587(4) 0.5903(6) 0.3454(3) 0.0262(13) Uani 1 1 d . . . O3 O 0.4417(4) 1.1130(5) 0.2953(3) 0.0218(12) Uani 1 1 d . . . O4 O 0.3070(4) 1.1713(5) 0.1846(3) 0.0254(13) Uani 1 1 d . . . O5 O 0.1271(5) 0.6081(6) 0.0107(3) 0.0427(16) Uani 1 1 d . . . O6 O 0.2168(4) 0.7533(7) -0.0128(3) 0.0402(16) Uani 1 1 d . . . O8 O 0.6071(4) 0.3403(5) 0.3614(3) 0.0242(13) Uani 1 1 d . . . O9 O 0.8856(4) -0.1599(6) 0.9466(3) 0.0269(13) Uani 1 1 d . . . O10 O 0.5803(5) 0.7700(7) 0.4629(3) 0.0452(17) Uani 1 1 d . . . O11 O 0.9194(5) 0.5736(8) 0.9214(4) 0.063(2) Uani 1 1 d . . . S1 S 0.16933(15) 0.7449(2) 0.01807(10) 0.0227(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O7 0.023(3) 0.030(4) 0.009(3) 0.003(2) 0.006(2) 0.009(3) Zn1 0.0201(5) 0.0177(5) 0.0063(4) 0.0012(4) 0.0060(4) 0.0003(4) Zn2 0.0269(7) 0.0259(8) 0.0078(6) 0.0028(6) 0.0082(6) 0.0005(6) C1 0.026(4) 0.021(5) 0.016(4) 0.004(4) 0.014(4) 0.007(4) C2 0.025(4) 0.028(5) 0.014(4) -0.002(3) 0.015(4) -0.002(4) C3 0.016(4) 0.027(5) 0.006(3) 0.007(3) 0.005(3) 0.001(4) C4 0.022(4) 0.023(5) 0.016(4) 0.007(4) 0.011(4) 0.002(4) C5 0.028(4) 0.024(5) 0.013(4) -0.007(3) 0.014(4) 0.000(4) C6 0.018(4) 0.024(5) 0.011(4) 0.004(4) 0.008(3) 0.003(4) C7 0.023(4) 0.025(5) 0.010(4) -0.003(3) 0.008(3) -0.001(4) C8 0.027(4) 0.019(5) 0.014(4) 0.005(3) 0.011(4) 0.004(4) C9 0.027(4) 0.025(5) 0.013(4) -0.001(4) 0.012(4) -0.003(4) C10 0.026(4) 0.022(5) 0.011(4) 0.006(3) 0.006(4) 0.002(4) C11 0.010(4) 0.016(5) 0.023(4) 0.007(3) 0.011(3) 0.001(3) C12 0.016(4) 0.018(4) 0.020(4) 0.007(4) 0.012(3) -0.001(4) C13 0.021(4) 0.010(4) 0.015(4) -0.005(3) 0.010(3) -0.008(3) C14 0.018(4) 0.015(5) 0.010(4) 0.001(3) 0.009(3) 0.007(3) C15 0.033(4) 0.010(4) 0.010(4) 0.003(3) 0.013(4) -0.004(4) C16 0.014(4) 0.023(5) 0.016(4) -0.004(3) 0.009(3) -0.007(3) C17 0.019(4) 0.022(5) 0.012(4) 0.001(3) 0.008(3) 0.001(4) C18 0.022(4) 0.023(5) 0.018(4) 0.002(4) 0.016(4) -0.006(4) C19 0.038(5) 0.022(5) 0.026(4) 0.004(4) 0.023(4) 0.003(4) C20 0.035(5) 0.057(7) 0.031(5) 0.000(5) 0.024(5) 0.000(5) C21 0.042(6) 0.029(6) 0.059(6) -0.005(5) 0.041(5) -0.001(5) C22 0.021(4) 0.024(5) 0.026(5) 0.003(4) 0.005(4) 0.006(4) C23 0.023(4) 0.030(5) 0.022(4) -0.004(4) 0.012(4) -0.002(4) C24 0.033(6) 0.081(10) 0.055(7) 0.028(7) 0.027(6) 0.006(6) C25 0.027(5) 0.056(7) 0.046(6) -0.014(6) 0.023(5) -0.003(5) C26 0.019(5) 0.077(9) 0.040(6) 0.013(6) 0.019(5) 0.004(5) C27 0.053(8) 0.063(9) 0.116(11) 0.027(8) 0.070(9) 0.025(7) C28 0.077(10) 0.077(11) 0.094(11) -0.050(9) 0.069(10) -0.023(8) N1 0.023(3) 0.019(4) 0.007(3) 0.000(3) 0.008(3) 0.000(3) N2 0.027(4) 0.028(4) 0.008(3) 0.003(3) 0.009(3) 0.004(3) N3 0.020(3) 0.030(4) 0.013(3) 0.009(3) 0.008(3) 0.010(3) N4 0.019(3) 0.019(4) 0.010(3) 0.004(3) 0.009(3) -0.001(3) N5 0.021(3) 0.023(4) 0.019(3) -0.006(3) 0.011(3) -0.005(3) N6 0.053(5) 0.033(5) 0.023(4) 0.001(3) 0.020(4) -0.002(4) N7 0.059(6) 0.098(9) 0.049(6) -0.021(6) 0.042(6) -0.038(7) N8 0.027(10) 0.372(19) 0.039(10) 0.040(10) 0.018(8) 0.017(10) O1 0.023(3) 0.009(3) 0.019(3) 0.004(2) 0.012(2) 0.004(2) O2 0.030(3) 0.026(3) 0.012(3) 0.001(2) 0.009(3) -0.003(3) O3 0.025(3) 0.018(3) 0.013(3) -0.002(2) 0.008(2) -0.002(2) O4 0.032(3) 0.017(3) 0.014(3) 0.000(2) 0.009(3) -0.002(3) O5 0.047(4) 0.026(4) 0.019(3) -0.009(3) 0.005(3) -0.011(3) O6 0.030(3) 0.067(5) 0.022(3) -0.008(3) 0.016(3) 0.002(3) O8 0.028(3) 0.025(3) 0.027(3) -0.001(2) 0.021(3) 0.001(3) O9 0.026(3) 0.029(4) 0.019(3) 0.000(2) 0.012(3) -0.003(3) O10 0.043(4) 0.057(5) 0.035(4) -0.021(3) 0.025(3) -0.013(3) O11 0.068(5) 0.055(5) 0.054(5) 0.000(4) 0.034(4) -0.009(4) S1 0.0254(11) 0.0233(12) 0.0107(9) -0.0019(9) 0.0078(9) 0.0027(9) _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 O7 S1 1.453(5) . ? O7 Zn2 2.225(5) 1_464 ? Zn1 O1 1.957(5) . ? Zn1 O3 1.984(5) 1_545 ? Zn1 N1 2.070(6) . ? Zn1 O8 2.174(5) . ? Zn1 N5 2.235(6) . ? Zn2 N4 2.080(5) . ? Zn2 N4 2.080(5) 3_757 ? Zn2 O9 2.146(5) 3_757 ? Zn2 O9 2.146(5) . ? Zn2 O7 2.225(5) 3_666 ? Zn2 O7 2.225(5) 1_646 ? C1 N4 1.322(9) . ? C1 C2 1.385(10) . ? C1 H1 0.9300 . ? C2 C3 1.386(10) . ? C2 H2 0.9300 . ? C3 C4 1.371(10) . ? C3 N3 1.434(9) . ? C4 C5 1.397(10) . ? C4 H4 0.9300 . ? C5 N4 1.332(9) . ? C5 H5 0.9300 . ? C6 C7 1.379(11) . ? C6 C10 1.386(11) . ? C6 N2 1.439(9) . ? C7 C8 1.383(9) . ? C7 H7 0.9300 . ? C8 N1 1.326(9) . ? C8 H8 0.9300 . ? C9 N1 1.317(9) . ? C9 C10 1.387(10) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 O2 1.241(8) . ? C11 O1 1.277(9) . ? C11 C12 1.512(10) . ? C12 C17 1.387(10) . ? C12 C13 1.399(10) . ? C13 C14 1.382(10) . ? C13 H13 0.9300 . ? C14 C15 1.372(10) . ? C14 S1 1.787(7) . ? C15 C16 1.394(9) . ? C15 H15 0.9300 . ? C16 C17 1.382(10) . ? C16 C18 1.497(11) . ? C17 H17 0.9300 . ? C18 O4 1.242(9) . ? C18 O3 1.273(8) . ? C19 N5 1.370(9) . ? C19 C20 1.374(11) . ? C19 H19 0.9300 . ? C20 C21 1.371(12) . ? C20 H20 0.9300 . ? C21 C22 1.379(12) . ? C21 N6 1.485(11) . ? C22 C23 1.409(11) . ? C22 H22 0.9300 . ? C23 N5 1.343(9) . ? C23 H23 0.9300 . ? C24 N7 1.296(14) . ? C24 C25 1.380(13) . ? C24 H24 0.9300 . ? C25 C26 1.339(14) . ? C25 H25 0.9300 . ? C26 N8 1.423(13) . ? C26 C27 1.430(16) . ? C27 C28 1.400(16) . ? C27 H27 0.9300 . ? C28 N7 1.302(16) . ? C28 H28 0.9300 . ? N2 N3 1.245(9) . ? N6 N6 1.168(13) 2 ? N8 N8 0.698(18) 2 ? O3 Zn1 1.984(5) 1_565 ? O5 S1 1.453(6) . ? O6 S1 1.434(6) . ? 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 S1 O7 Zn2 156.2(3) . 1_464 ? O1 Zn1 O3 113.8(2) . 1_545 ? O1 Zn1 N1 146.9(2) . . ? O3 Zn1 N1 99.0(2) 1_545 . ? O1 Zn1 O8 87.21(19) . . ? O3 Zn1 O8 95.6(2) 1_545 . ? N1 Zn1 O8 85.5(2) . . ? O1 Zn1 N5 91.3(2) . . ? O3 Zn1 N5 97.7(2) 1_545 . ? N1 Zn1 N5 88.3(2) . . ? O8 Zn1 N5 166.1(2) . . ? N4 Zn2 N4 180.0(2) . 3_757 ? N4 Zn2 O9 91.6(2) . 3_757 ? N4 Zn2 O9 88.4(2) 3_757 3_757 ? N4 Zn2 O9 88.4(2) . . ? N4 Zn2 O9 91.6(2) 3_757 . ? O9 Zn2 O9 180.0(4) 3_757 . ? N4 Zn2 O7 91.3(2) . 3_666 ? N4 Zn2 O7 88.7(2) 3_757 3_666 ? O9 Zn2 O7 86.3(2) 3_757 3_666 ? O9 Zn2 O7 93.7(2) . 3_666 ? N4 Zn2 O7 88.7(2) . 1_646 ? N4 Zn2 O7 91.3(2) 3_757 1_646 ? O9 Zn2 O7 93.7(2) 3_757 1_646 ? O9 Zn2 O7 86.3(2) . 1_646 ? O7 Zn2 O7 180.0(3) 3_666 1_646 ? N4 C1 C2 123.8(8) . . ? N4 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C1 C2 C3 117.0(7) . . ? C1 C2 H2 121.5 . . ? C3 C2 H2 121.5 . . ? C4 C3 C2 120.1(7) . . ? C4 C3 N3 116.7(7) . . ? C2 C3 N3 123.1(7) . . ? C3 C4 C5 118.4(7) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N4 C5 C4 121.8(7) . . ? N4 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C7 C6 C10 120.0(7) . . ? C7 C6 N2 125.0(7) . . ? C10 C6 N2 115.0(7) . . ? C6 C7 C8 117.3(7) . . ? C6 C7 H7 121.4 . . ? C8 C7 H7 121.4 . . ? N1 C8 C7 123.3(8) . . ? N1 C8 H8 118.4 . . ? C7 C8 H8 118.4 . . ? N1 C9 C10 122.6(7) . . ? N1 C9 H9 118.7 . . ? C10 C9 H9 118.7 . . ? C6 C10 C9 117.8(8) . . ? C6 C10 H10 121.1 . . ? C9 C10 H10 121.1 . . ? O2 C11 O1 123.0(7) . . ? O2 C11 C12 120.7(7) . . ? O1 C11 C12 116.3(6) . . ? C17 C12 C13 120.5(7) . . ? C17 C12 C11 120.6(7) . . ? C13 C12 C11 118.6(7) . . ? C14 C13 C12 118.4(7) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C15 C14 C13 121.5(7) . . ? C15 C14 S1 117.5(5) . . ? C13 C14 S1 120.7(6) . . ? C14 C15 C16 119.8(7) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 119.8(7) . . ? C17 C16 C18 122.6(7) . . ? C15 C16 C18 117.5(7) . . ? C16 C17 C12 119.9(7) . . ? C16 C17 H17 120.0 . . ? C12 C17 H17 120.0 . . ? O4 C18 O3 124.6(7) . . ? O4 C18 C16 117.8(7) . . ? O3 C18 C16 117.5(7) . . ? N5 C19 C20 124.0(8) . . ? N5 C19 H19 118.0 . . ? C20 C19 H19 118.0 . . ? C21 C20 C19 118.4(8) . . ? C21 C20 H20 120.8 . . ? C19 C20 H20 120.8 . . ? C20 C21 C22 120.1(8) . . ? C20 C21 N6 114.3(7) . . ? C22 C21 N6 125.6(8) . . ? C21 C22 C23 118.3(8) . . ? C21 C22 H22 120.9 . . ? C23 C22 H22 120.9 . . ? N5 C23 C22 122.9(7) . . ? N5 C23 H23 118.5 . . ? C22 C23 H23 118.5 . . ? N7 C24 C25 123.9(11) . . ? N7 C24 H24 118.1 . . ? C25 C24 H24 118.1 . . ? C26 C25 C24 119.3(11) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 N8 120.1(12) . . ? C25 C26 C27 119.4(10) . . ? N8 C26 C27 120.5(12) . . ? C28 C27 C26 114.1(11) . . ? C28 C27 H27 122.9 . . ? C26 C27 H27 122.9 . . ? N7 C28 C27 125.9(12) . . ? N7 C28 H28 117.0 . . ? C27 C28 H28 117.0 . . ? C9 N1 C8 119.0(6) . . ? C9 N1 Zn1 116.7(5) . . ? C8 N1 Zn1 124.3(5) . . ? N3 N2 C6 112.9(6) . . ? N2 N3 C3 111.4(6) . . ? C1 N4 C5 118.6(6) . . ? C1 N4 Zn2 119.7(5) . . ? C5 N4 Zn2 121.1(5) . . ? C23 N5 C19 116.3(7) . . ? C23 N5 Zn1 118.5(5) . . ? C19 N5 Zn1 125.2(5) . . ? N6 N6 C21 109.9(9) 2 . ? C24 N7 C28 117.3(11) . . ? N8 N8 C26 172(4) 2 . ? C11 O1 Zn1 110.4(4) . . ? C18 O3 Zn1 119.4(5) . 1_565 ? O6 S1 O7 112.9(3) . . ? O6 S1 O5 113.2(4) . . ? O7 S1 O5 112.1(3) . . ? O6 S1 C14 107.2(3) . . ? O7 S1 C14 104.9(3) . . ? O5 S1 C14 105.9(3) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.571 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.152 # Attachment '- 5.CIF' data_p090726f _database_code_depnum_ccdc_archive 'CCDC 756348' #TrackingRef '- 5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H11 Cu3 O13 S' _chemical_formula_weight 561.87 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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7544(7) _cell_length_b 10.1037(7) _cell_length_c 10.4206(6) _cell_angle_alpha 72.928(5) _cell_angle_beta 79.968(5) _cell_angle_gamma 69.699(7) _cell_volume 823.68(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 26.41 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 4.035 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4320 _exptl_absorpt_correction_T_max 0.4992 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9136 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2906 _reflns_number_gt 2558 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0352P)^2^+0.2314P] 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 2906 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0632 _refine_ls_wR_factor_gt 0.0624 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.002 _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 0.78333(4) 0.21491(3) 0.11589(3) 0.01001(11) Uani 1 1 d . . . Cu2 Cu 0.09367(4) 0.95618(4) 0.12374(3) 0.00974(11) Uani 1 1 d . . . Cu3 Cu 0.87209(4) -0.02181(3) 0.41685(3) 0.00972(11) Uani 1 1 d . . . C1 C 0.4651(4) 0.3562(3) 0.4410(3) 0.0108(6) Uani 1 1 d . . . C2 C 0.4310(4) 0.3038(3) 0.5780(3) 0.0117(6) Uani 1 1 d . . . H2 H 0.4999 0.2163 0.6251 0.014 Uiso 1 1 calc R . . C3 C 0.2947(4) 0.3818(3) 0.6442(3) 0.0100(6) Uani 1 1 d . . . C4 C 0.1912(4) 0.5136(3) 0.5767(3) 0.0111(6) Uani 1 1 d . . . H4 H 0.0982 0.5645 0.6217 0.013 Uiso 1 1 calc R . . C5 C 0.2294(4) 0.5685(3) 0.4403(3) 0.0100(6) Uani 1 1 d . . . C6 C 0.3649(4) 0.4895(3) 0.3714(3) 0.0103(6) Uani 1 1 d . . . H6 H 0.3881 0.5255 0.2798 0.012 Uiso 1 1 calc R . . C7 C 0.6096(4) 0.2645(3) 0.3694(3) 0.0114(6) Uani 1 1 d . . . C8 C 0.1262(4) 0.7170(3) 0.3687(3) 0.0100(6) Uani 1 1 d . . . C9 C 0.1920(4) 1.0888(3) 0.2939(3) 0.0153(7) Uani 1 1 d . . . C10 C 0.3107(5) 1.1574(5) 0.3154(4) 0.0384(10) Uani 1 1 d . . . H10A H 0.3256 1.1321 0.4097 0.058 Uiso 1 1 calc R . . H10B H 0.2681 1.2615 0.2835 0.058 Uiso 1 1 calc R . . H10C H 0.4138 1.1223 0.2667 0.058 Uiso 1 1 calc R . . O1 O 0.6999(3) 0.1541(2) 0.4432(2) 0.0238(6) Uani 1 1 d . . . O2 O 0.6273(3) 0.3078(2) 0.2436(2) 0.0172(5) Uani 1 1 d . . . O3 O 0.1847(3) 0.7738(2) 0.2553(2) 0.0159(5) Uani 1 1 d . . . O4 O -0.0069(2) 0.7725(2) 0.4306(2) 0.0142(5) Uani 1 1 d . . . O8 O 0.1983(3) 1.0696(2) 0.1792(2) 0.0192(5) Uani 1 1 d . . . O9 O 0.0935(2) 1.0544(2) 0.39127(19) 0.0127(4) Uani 1 1 d . . . O10 O 0.8387(2) 0.01905(19) 0.23198(19) 0.0100(4) Uani 1 1 d . . . H10 H 0.7864 -0.0286 0.2155 0.012 Uiso 1 1 d R . . O11 O 0.6295(3) 0.1417(2) 0.0093(2) 0.0199(5) Uani 1 1 d . . . H11 H 0.5583 0.2132 -0.0285 0.024 Uiso 1 1 d R . . O12 O 0.9697(2) 0.13456(19) -0.00500(19) 0.0103(4) Uani 1 1 d . . . H12 H 1.0094 0.1932 -0.0648 0.012 Uiso 1 1 d R . . O13 O 0.7627(3) 0.4131(2) 0.0019(2) 0.0245(6) Uani 1 1 d . . . H13A H 0.7218 0.4896 -0.0586 0.029 Uiso 1 1 d R . . H13B H 0.8567 0.4128 0.0130 0.029 Uiso 1 1 d R . . O7A O 0.3111(3) 0.1529(2) 0.8407(2) 0.0177(5) Uani 1 1 d . . . O5C O 0.3580(3) 0.3553(2) 0.8863(2) 0.0166(5) Uani 1 1 d . . . O6C O 0.0844(3) 0.3721(2) 0.8530(2) 0.0221(5) Uani 1 1 d . . . S1 S 0.25796(9) 0.31042(7) 0.81989(7) 0.01173(17) 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 0.0123(2) 0.00693(18) 0.00727(19) -0.00209(14) 0.00188(15) 0.00029(14) Cu2 0.0120(2) 0.00865(19) 0.00633(19) -0.00162(14) -0.00176(14) -0.00022(14) Cu3 0.0102(2) 0.00896(19) 0.00665(19) -0.00232(14) -0.00123(14) 0.00168(14) C1 0.0117(16) 0.0089(14) 0.0111(15) -0.0027(12) -0.0003(12) -0.0026(12) C2 0.0111(16) 0.0079(14) 0.0132(16) -0.0014(12) -0.0029(12) 0.0006(12) C3 0.0142(16) 0.0073(14) 0.0087(15) -0.0011(11) -0.0005(12) -0.0044(12) C4 0.0077(15) 0.0129(15) 0.0125(15) -0.0044(12) 0.0003(12) -0.0023(12) C5 0.0090(15) 0.0086(14) 0.0105(15) -0.0012(12) -0.0009(12) -0.0012(11) C6 0.0109(15) 0.0111(14) 0.0082(15) -0.0025(11) -0.0010(12) -0.0026(12) C7 0.0093(15) 0.0120(15) 0.0122(16) -0.0053(12) -0.0028(12) 0.0001(12) C8 0.0116(16) 0.0083(14) 0.0087(15) -0.0018(12) -0.0029(12) -0.0010(12) C9 0.0187(17) 0.0155(16) 0.0118(16) -0.0029(12) -0.0025(14) -0.0053(13) C10 0.049(3) 0.064(3) 0.025(2) -0.0194(19) 0.0109(19) -0.045(2) O1 0.0242(13) 0.0221(12) 0.0109(11) -0.0069(9) -0.0050(10) 0.0139(10) O2 0.0213(12) 0.0110(10) 0.0108(11) -0.0027(8) 0.0048(9) 0.0022(9) O3 0.0165(12) 0.0128(11) 0.0088(11) 0.0024(9) 0.0003(9) 0.0021(9) O4 0.0152(12) 0.0082(10) 0.0125(11) -0.0025(8) 0.0018(9) 0.0031(8) O8 0.0253(13) 0.0269(12) 0.0110(11) -0.0073(9) 0.0016(10) -0.0146(10) O9 0.0130(11) 0.0161(11) 0.0085(11) -0.0033(8) 0.0000(9) -0.0042(9) O10 0.0125(11) 0.0096(10) 0.0079(10) -0.0031(8) -0.0005(8) -0.0028(8) O11 0.0191(12) 0.0193(12) 0.0182(12) 0.0020(9) -0.0100(10) -0.0039(9) O12 0.0124(11) 0.0096(10) 0.0063(10) -0.0010(8) 0.0033(8) -0.0032(8) O13 0.0320(14) 0.0109(11) 0.0199(12) 0.0021(9) 0.0026(11) -0.0010(10) O7A 0.0275(13) 0.0111(11) 0.0138(11) 0.0011(9) -0.0027(10) -0.0084(9) O5C 0.0218(13) 0.0152(11) 0.0138(11) -0.0049(9) -0.0028(9) -0.0053(9) O6C 0.0148(12) 0.0274(12) 0.0154(12) -0.0003(10) 0.0057(10) -0.0036(10) S1 0.0134(4) 0.0113(4) 0.0083(4) -0.0004(3) 0.0010(3) -0.0038(3) _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 1.931(2) . ? Cu1 O10 1.9358(18) . ? Cu1 O12 1.9682(19) . ? Cu1 O13 1.970(2) . ? Cu1 O11 2.300(2) . ? Cu1 Cu2 3.0406(6) 1_645 ? Cu2 O8 1.946(2) . ? Cu2 O3 1.9465(19) . ? Cu2 O12 1.984(2) 2_665 ? Cu2 O12 1.9890(19) 1_465 ? Cu2 O10 2.284(2) 1_465 ? Cu2 Cu1 3.0406(6) 1_465 ? Cu2 Cu2 3.0413(7) 2_575 ? Cu3 O10 1.9006(19) . ? Cu3 O1 1.947(2) . ? Cu3 O4 1.9520(19) 1_645 ? Cu3 O9 1.988(2) 2_666 ? Cu3 O9 2.270(2) 1_645 ? C1 C2 1.388(4) . ? C1 C6 1.392(4) . ? C1 C7 1.510(4) . ? C2 C3 1.378(4) . ? C2 H2 0.9300 . ? C3 C4 1.387(4) . ? C3 S1 1.776(3) . ? C4 C5 1.393(4) . ? C4 H4 0.9300 . ? C5 C6 1.393(4) . ? C5 C8 1.504(4) . ? C6 H6 0.9300 . ? C7 O1 1.248(3) . ? C7 O2 1.254(4) . ? C8 O3 1.259(3) . ? C8 O4 1.259(3) . ? C9 O8 1.255(4) . ? C9 O9 1.262(4) . ? C9 C10 1.511(5) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? O4 Cu3 1.9520(19) 1_465 ? O9 Cu3 1.988(2) 2_666 ? O9 Cu3 2.270(2) 1_465 ? O10 Cu2 2.284(2) 1_645 ? O10 H10 0.8365 . ? O11 H11 0.8200 . ? O12 Cu2 1.984(2) 2_665 ? O12 Cu2 1.9890(19) 1_645 ? O12 H12 0.8430 . ? O13 H13A 0.8500 . ? O13 H13B 0.8500 . ? O7A S1 1.454(2) . ? O5C S1 1.457(2) . ? O6C S1 1.450(2) . ? 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 O10 96.60(8) . . ? O2 Cu1 O12 169.57(9) . . ? O10 Cu1 O12 85.51(8) . . ? O2 Cu1 O13 86.49(8) . . ? O10 Cu1 O13 170.71(9) . . ? O12 Cu1 O13 89.91(8) . . ? O2 Cu1 O11 103.86(9) . . ? O10 Cu1 O11 86.49(8) . . ? O12 Cu1 O11 86.44(8) . . ? O13 Cu1 O11 101.31(9) . . ? O2 Cu1 Cu2 137.39(6) . 1_645 ? O10 Cu1 Cu2 48.66(6) . 1_645 ? O12 Cu1 Cu2 40.04(5) . 1_645 ? O13 Cu1 Cu2 124.31(7) . 1_645 ? O11 Cu1 Cu2 98.23(6) . 1_645 ? O8 Cu2 O3 96.24(9) . . ? O8 Cu2 O12 159.22(8) . 2_665 ? O3 Cu2 O12 95.22(8) . 2_665 ? O8 Cu2 O12 90.45(9) . 1_465 ? O3 Cu2 O12 171.35(9) . 1_465 ? O12 Cu2 O12 80.11(8) 2_665 1_465 ? O8 Cu2 O10 101.77(8) . 1_465 ? O3 Cu2 O10 96.88(8) . 1_465 ? O12 Cu2 O10 93.98(7) 2_665 1_465 ? O12 Cu2 O10 76.33(7) 1_465 1_465 ? O8 Cu2 Cu1 86.70(7) . 1_465 ? O3 Cu2 Cu1 135.20(6) . 1_465 ? O12 Cu2 Cu1 97.25(5) 2_665 1_465 ? O12 Cu2 Cu1 39.54(5) 1_465 1_465 ? O10 Cu2 Cu1 39.52(5) 1_465 1_465 ? O8 Cu2 Cu2 127.96(7) . 2_575 ? O3 Cu2 Cu2 134.90(7) . 2_575 ? O12 Cu2 Cu2 40.11(5) 2_665 2_575 ? O12 Cu2 Cu2 40.00(6) 1_465 2_575 ? O10 Cu2 Cu2 83.72(5) 1_465 2_575 ? Cu1 Cu2 Cu2 65.037(14) 1_465 2_575 ? O10 Cu3 O1 93.58(8) . . ? O10 Cu3 O4 93.89(8) . 1_645 ? O1 Cu3 O4 160.86(10) . 1_645 ? O10 Cu3 O9 177.17(8) . 2_666 ? O1 Cu3 O9 84.46(8) . 2_666 ? O4 Cu3 O9 88.60(8) 1_645 2_666 ? O10 Cu3 O9 98.52(8) . 1_645 ? O1 Cu3 O9 99.75(9) . 1_645 ? O4 Cu3 O9 96.54(8) 1_645 1_645 ? O9 Cu3 O9 79.84(8) 2_666 1_645 ? C2 C1 C6 120.1(3) . . ? C2 C1 C7 118.8(2) . . ? C6 C1 C7 121.1(3) . . ? C3 C2 C1 119.9(3) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 121.2(3) . . ? C2 C3 S1 117.9(2) . . ? C4 C3 S1 120.9(2) . . ? C3 C4 C5 118.7(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 120.7(3) . . ? C6 C5 C8 120.1(3) . . ? C4 C5 C8 119.2(3) . . ? C1 C6 C5 119.4(3) . . ? C1 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? O1 C7 O2 127.1(3) . . ? O1 C7 C1 115.7(3) . . ? O2 C7 C1 117.1(2) . . ? O3 C8 O4 127.2(3) . . ? O3 C8 C5 116.3(2) . . ? O4 C8 C5 116.4(2) . . ? O8 C9 O9 124.1(3) . . ? O8 C9 C10 117.4(3) . . ? O9 C9 C10 118.5(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 O1 Cu3 135.9(2) . . ? C7 O2 Cu1 129.65(19) . . ? C8 O3 Cu2 131.05(19) . . ? C8 O4 Cu3 128.82(19) . 1_465 ? C9 O8 Cu2 128.6(2) . . ? C9 O9 Cu3 123.8(2) . 2_666 ? C9 O9 Cu3 135.3(2) . 1_465 ? Cu3 O9 Cu3 100.16(8) 2_666 1_465 ? Cu3 O10 Cu1 122.51(10) . . ? Cu3 O10 Cu2 105.69(9) . 1_645 ? Cu1 O10 Cu2 91.82(8) . 1_645 ? Cu3 O10 H10 114.6 . . ? Cu1 O10 H10 110.8 . . ? Cu2 O10 H10 107.7 1_645 . ? Cu1 O11 H11 109.4 . . ? Cu1 O12 Cu2 111.62(10) . 2_665 ? Cu1 O12 Cu2 100.41(8) . 1_645 ? Cu2 O12 Cu2 99.89(8) 2_665 1_645 ? Cu1 O12 H12 118.3 . . ? Cu2 O12 H12 98.6 2_665 . ? Cu2 O12 H12 126.4 1_645 . ? Cu1 O13 H13A 155.0 . . ? Cu1 O13 H13B 96.0 . . ? H13A O13 H13B 107.7 . . ? O6C S1 O7A 113.33(14) . . ? O6C S1 O5C 112.76(13) . . ? O7A S1 O5C 111.61(13) . . ? O6C S1 C3 106.67(13) . . ? O7A S1 C3 105.51(13) . . ? O5C S1 C3 106.30(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.611 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.085