# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email PARKIN@COLUMBIA.EDU _publ_contact_author_name 'Gerard Parkin' _publ_author_name 'Gerard Parkin' data_finalp _database_code_depnum_ccdc_archive 'CCDC 867641' #TrackingRef '- finalp(ZnOH).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H38 N6 O2 S6 Zn2' _chemical_formula_weight 1005.90 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.575(2) _cell_length_b 13.205(3) _cell_length_c 14.031(3) _cell_angle_alpha 112.044(3) _cell_angle_beta 95.622(3) _cell_angle_gamma 104.585(3) _cell_volume 2041.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5555 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.12 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 1.531 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.7102 _exptl_absorpt_correction_T_max 0.9700 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12639 _diffrn_reflns_av_R_equivalents 0.1028 _diffrn_reflns_av_sigmaI/netI 0.1355 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 30.74 _reflns_number_total 12639 _reflns_number_gt 6248 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0132P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12639 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1127 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.0957 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.505 0.500 435 157 ' ' _platon_squeeze_details ; The unit cell contains 4 benzene molecules which have been treated as a diffuse cotribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; 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 0.04674(4) 0.59673(4) 0.11403(3) 0.02862(12) Uani 1 1 d . . . Zn2 Zn 0.12586(3) 0.03977(3) 0.05023(3) 0.02296(11) Uani 1 1 d . . . S1 S 0.12378(8) 0.86453(8) 0.28452(7) 0.0307(2) Uani 1 1 d . . . S2 S -0.01808(8) 0.69456(8) 0.34369(7) 0.0304(2) Uani 1 1 d . . . S3 S -0.11314(8) 0.74657(8) 0.17235(7) 0.0288(2) Uani 1 1 d . . . S4 S 0.36218(7) 0.20356(8) 0.22006(7) 0.0268(2) Uani 1 1 d . . . S5 S 0.38101(7) 0.08621(8) 0.00324(7) 0.0275(2) Uani 1 1 d . . . S6 S 0.27451(7) 0.27130(8) 0.05823(7) 0.0253(2) Uani 1 1 d . . . N1 N 0.1902(2) 0.7242(3) 0.1240(2) 0.0283(7) Uani 1 1 d . . . N2 N 0.0749(3) 0.5379(2) 0.2325(2) 0.0300(7) Uani 1 1 d . . . N3 N -0.1043(2) 0.8914(2) 0.3679(2) 0.0275(7) Uani 1 1 d . . . N4 N 0.1445(2) 0.1202(2) 0.2174(2) 0.0264(7) Uani 1 1 d . . . N5 N 0.1885(2) -0.0881(2) -0.0522(2) 0.0257(7) Uani 1 1 d . . . N6 N 0.5002(2) 0.3574(2) 0.1205(2) 0.0308(8) Uani 1 1 d . . . O1 O 0.0859(2) 0.4685(2) 0.0007(2) 0.0397(8) Uani 1 1 d . . . H1 H 0.133(3) 0.440(3) -0.005(3) 0.048 Uiso 1 1 d . . . O2 O -0.0216(2) -0.0811(2) 0.0298(2) 0.0281(6) Uani 1 1 d . . . H2 H -0.034(3) -0.111(3) 0.064(3) 0.034 Uiso 1 1 d . . . C1 C 0.0075(3) 0.7355(3) 0.2377(3) 0.0241(8) Uani 1 1 d . . . C2 C 0.2980(3) 0.1564(3) 0.0849(2) 0.0217(8) Uani 1 1 d . . . C11 C 0.2146(3) 0.8307(3) 0.1997(3) 0.0257(8) Uani 1 1 d . . . C12 C 0.3110(3) 0.9165(3) 0.2140(3) 0.0382(10) Uani 1 1 d . . . H12A H 0.3263 0.9914 0.2681 0.046 Uiso 1 1 calc R . . C13 C 0.3845(3) 0.8933(4) 0.1498(4) 0.0468(12) Uani 1 1 d . . . H13A H 0.4516 0.9521 0.1593 0.056 Uiso 1 1 calc R . . C14 C 0.3614(3) 0.7841(4) 0.0707(3) 0.0396(11) Uani 1 1 d . . . H14A H 0.4119 0.7662 0.0255 0.048 Uiso 1 1 calc R . . C15 C 0.2633(3) 0.7029(3) 0.0601(3) 0.0342(10) Uani 1 1 d . . . H15A H 0.2457 0.6281 0.0053 0.041 Uiso 1 1 calc R . . C21 C 0.0458(3) 0.5865(3) 0.3238(3) 0.0279(9) Uani 1 1 d . . . C22 C 0.0653(3) 0.5550(3) 0.4070(3) 0.0364(10) Uani 1 1 d . . . H22A H 0.0433 0.5901 0.4712 0.044 Uiso 1 1 calc R . . C23 C 0.1171(3) 0.4719(4) 0.3938(4) 0.0472(12) Uani 1 1 d . . . H23A H 0.1312 0.4493 0.4493 0.057 Uiso 1 1 calc R . . C24 C 0.1486(4) 0.4215(3) 0.3006(4) 0.0438(11) Uani 1 1 d . . . H24A H 0.1849 0.3645 0.2907 0.053 Uiso 1 1 calc R . . C25 C 0.1256(3) 0.4566(3) 0.2222(3) 0.0391(11) Uani 1 1 d . . . H25A H 0.1465 0.4217 0.1574 0.047 Uiso 1 1 calc R . . C31 C -0.1547(3) 0.8520(3) 0.2687(3) 0.0266(8) Uani 1 1 d . . . C32 C -0.2412(4) 0.8865(4) 0.2353(3) 0.0624(15) Uani 1 1 d . . . H32A H -0.2758 0.8561 0.1629 0.075 Uiso 1 1 calc R . . C33 C -0.2755(4) 0.9671(5) 0.3115(4) 0.088(2) Uani 1 1 d . . . H33A H -0.3348 0.9927 0.2919 0.106 Uiso 1 1 calc R . . C34 C -0.2230(4) 1.0093(4) 0.4148(3) 0.0551(14) Uani 1 1 d . . . H34A H -0.2440 1.0655 0.4682 0.066 Uiso 1 1 calc R . . C35 C -0.1396(3) 0.9682(3) 0.4390(3) 0.0331(9) Uani 1 1 d . . . H35A H -0.1045 0.9962 0.5110 0.040 Uiso 1 1 calc R . . C41 C 0.2464(3) 0.1801(3) 0.2778(3) 0.0251(8) Uani 1 1 d . . . C42 C 0.2648(3) 0.2293(3) 0.3869(3) 0.0356(10) Uani 1 1 d . . . H42A H 0.3390 0.2702 0.4282 0.043 Uiso 1 1 calc R . . C43 C 0.1748(4) 0.2181(3) 0.4344(3) 0.0380(10) Uani 1 1 d . . . H43A H 0.1855 0.2505 0.5089 0.046 Uiso 1 1 calc R . . C44 C 0.0674(4) 0.1583(3) 0.3710(3) 0.0380(10) Uani 1 1 d . . . H44A H 0.0033 0.1512 0.4015 0.046 Uiso 1 1 calc R . . C45 C 0.0559(3) 0.1103(3) 0.2648(3) 0.0308(9) Uani 1 1 d . . . H45A H -0.0173 0.0680 0.2220 0.037 Uiso 1 1 calc R . . C51 C 0.2915(3) -0.0553(3) -0.0682(3) 0.0256(8) Uani 1 1 d . . . C52 C 0.3335(3) -0.1315(3) -0.1416(3) 0.0308(9) Uani 1 1 d . . . H52A H 0.4081 -0.1074 -0.1510 0.037 Uiso 1 1 calc R . . C53 C 0.2643(3) -0.2423(3) -0.2000(3) 0.0368(10) Uani 1 1 d . . . H53A H 0.2904 -0.2952 -0.2517 0.044 Uiso 1 1 calc R . . C54 C 0.1576(3) -0.2769(3) -0.1841(3) 0.0429(11) Uani 1 1 d . . . H54A H 0.1091 -0.3533 -0.2241 0.051 Uiso 1 1 calc R . . C55 C 0.1229(3) -0.1974(3) -0.1083(3) 0.0383(10) Uani 1 1 d . . . H55A H 0.0500 -0.2209 -0.0954 0.046 Uiso 1 1 calc R . . C61 C 0.4054(3) 0.3802(3) 0.0986(3) 0.0279(9) Uani 1 1 d . . . C62 C 0.4052(4) 0.4874(3) 0.1062(3) 0.0424(11) Uani 1 1 d . . . H62A H 0.3363 0.5012 0.0908 0.051 Uiso 1 1 calc R . . C63 C 0.5045(4) 0.5733(4) 0.1360(4) 0.0575(14) Uani 1 1 d . . . H63A H 0.5054 0.6469 0.1399 0.069 Uiso 1 1 calc R . . C64 C 0.6039(4) 0.5534(4) 0.1605(3) 0.0495(12) Uani 1 1 d . . . H64A H 0.6742 0.6124 0.1831 0.059 Uiso 1 1 calc R . . C65 C 0.5967(3) 0.4440(3) 0.1508(3) 0.0408(11) Uani 1 1 d . . . H65A H 0.6648 0.4290 0.1667 0.049 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 0.0264(2) 0.0289(3) 0.0201(2) 0.0025(2) 0.00790(19) 0.0022(2) Zn2 0.0166(2) 0.0236(2) 0.0261(2) 0.0089(2) 0.00498(18) 0.00417(18) S1 0.0273(5) 0.0268(5) 0.0297(5) 0.0064(4) 0.0067(4) 0.0030(4) S2 0.0442(6) 0.0305(5) 0.0241(5) 0.0134(5) 0.0175(5) 0.0175(5) S3 0.0263(5) 0.0351(6) 0.0216(5) 0.0094(4) 0.0050(4) 0.0076(4) S4 0.0230(5) 0.0301(5) 0.0231(5) 0.0100(4) 0.0019(4) 0.0041(4) S5 0.0187(5) 0.0278(5) 0.0290(5) 0.0054(4) 0.0066(4) 0.0052(4) S6 0.0224(5) 0.0267(5) 0.0254(5) 0.0106(4) 0.0041(4) 0.0061(4) N1 0.0234(17) 0.037(2) 0.0261(18) 0.0136(16) 0.0096(14) 0.0095(15) N2 0.0359(19) 0.0175(16) 0.0325(19) 0.0069(15) 0.0125(15) 0.0049(15) N3 0.0272(18) 0.0296(18) 0.0218(17) 0.0076(15) 0.0031(14) 0.0081(15) N4 0.0278(18) 0.0247(17) 0.0293(18) 0.0130(15) 0.0104(15) 0.0083(15) N5 0.0194(16) 0.0192(16) 0.0329(18) 0.0073(14) 0.0018(14) 0.0041(13) N6 0.0226(17) 0.0292(18) 0.0331(19) 0.0095(15) 0.0065(15) 0.0008(15) O1 0.0290(17) 0.0441(18) 0.0274(15) -0.0029(14) 0.0039(13) 0.0095(13) O2 0.0223(14) 0.0276(15) 0.0359(17) 0.0184(12) 0.0062(12) 0.0024(12) C1 0.0234(19) 0.028(2) 0.0224(19) 0.0132(17) 0.0075(16) 0.0048(16) C2 0.0230(19) 0.0222(19) 0.0153(18) 0.0038(15) 0.0066(15) 0.0047(16) C11 0.024(2) 0.029(2) 0.026(2) 0.0147(18) 0.0035(17) 0.0068(17) C12 0.033(2) 0.024(2) 0.061(3) 0.020(2) 0.016(2) 0.0088(19) C13 0.028(2) 0.036(3) 0.082(4) 0.035(3) 0.016(2) 0.003(2) C14 0.026(2) 0.052(3) 0.058(3) 0.037(3) 0.024(2) 0.012(2) C15 0.036(2) 0.040(2) 0.034(2) 0.019(2) 0.013(2) 0.017(2) C21 0.031(2) 0.021(2) 0.031(2) 0.0095(17) 0.0143(18) 0.0051(17) C22 0.048(3) 0.037(2) 0.040(3) 0.024(2) 0.025(2) 0.020(2) C23 0.048(3) 0.046(3) 0.061(3) 0.036(3) 0.015(2) 0.017(2) C24 0.048(3) 0.034(3) 0.059(3) 0.022(2) 0.024(2) 0.021(2) C25 0.046(3) 0.021(2) 0.052(3) 0.011(2) 0.026(2) 0.013(2) C31 0.023(2) 0.035(2) 0.026(2) 0.0149(18) 0.0102(17) 0.0090(18) C32 0.058(3) 0.116(4) 0.025(2) 0.021(3) 0.012(2) 0.058(3) C33 0.090(4) 0.169(6) 0.033(3) 0.029(3) 0.017(3) 0.106(4) C34 0.054(3) 0.094(4) 0.029(3) 0.018(3) 0.019(2) 0.050(3) C35 0.034(2) 0.043(2) 0.021(2) 0.0123(19) 0.0065(18) 0.011(2) C41 0.027(2) 0.022(2) 0.031(2) 0.0147(17) 0.0067(17) 0.0081(17) C42 0.035(2) 0.033(2) 0.030(2) 0.0077(19) 0.0094(19) 0.0051(19) C43 0.058(3) 0.033(2) 0.028(2) 0.014(2) 0.016(2) 0.017(2) C44 0.048(3) 0.034(2) 0.041(3) 0.017(2) 0.027(2) 0.020(2) C45 0.024(2) 0.032(2) 0.034(2) 0.0140(19) 0.0078(18) 0.0043(18) C51 0.021(2) 0.030(2) 0.024(2) 0.0114(17) 0.0031(16) 0.0065(17) C52 0.030(2) 0.032(2) 0.030(2) 0.0090(19) 0.0098(18) 0.0141(19) C53 0.042(3) 0.029(2) 0.033(2) 0.0029(19) 0.012(2) 0.015(2) C54 0.038(3) 0.028(2) 0.048(3) 0.003(2) 0.008(2) 0.007(2) C55 0.024(2) 0.028(2) 0.053(3) 0.010(2) 0.005(2) 0.0031(18) C61 0.030(2) 0.028(2) 0.025(2) 0.0108(17) 0.0102(17) 0.0064(18) C62 0.039(3) 0.038(3) 0.061(3) 0.029(2) 0.017(2) 0.014(2) C63 0.049(3) 0.039(3) 0.095(4) 0.039(3) 0.021(3) 0.011(3) C64 0.039(3) 0.037(3) 0.064(3) 0.020(2) 0.013(2) -0.001(2) C65 0.027(2) 0.045(3) 0.050(3) 0.020(2) 0.013(2) 0.010(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 Zn1 O1 1.956(3) 2_565 ? Zn1 O1 2.047(3) . ? Zn1 N1 2.086(3) . ? Zn1 N2 2.117(3) . ? Zn1 C1 2.202(3) . ? Zn1 Zn1 3.1244(9) 2_565 ? Zn2 O2 1.952(3) 2 ? Zn2 O2 2.033(2) . ? Zn2 N4 2.140(3) . ? Zn2 N5 2.146(3) . ? Zn2 C2 2.202(3) . ? Zn2 Zn2 3.0743(10) 2 ? S1 C11 1.745(4) . ? S1 C1 1.786(3) . ? S2 C21 1.755(4) . ? S2 C1 1.793(3) . ? S3 C1 1.761(4) . ? S3 C31 1.769(4) . ? S4 C41 1.751(4) . ? S4 C2 1.788(3) . ? S5 C51 1.754(4) . ? S5 C2 1.785(3) . ? S6 C2 1.777(3) . ? S6 C61 1.764(4) . ? N1 C11 1.341(4) . ? N1 C15 1.353(4) . ? N2 C21 1.334(4) . ? N2 C25 1.353(4) . ? N3 C31 1.314(4) . ? N3 C35 1.332(4) . ? N4 C41 1.327(4) . ? N4 C45 1.355(4) . ? N5 C51 1.328(4) . ? N5 C55 1.343(4) . ? N6 C61 1.337(4) . ? N6 C65 1.341(4) . ? O1 Zn1 1.956(3) 2_565 ? O2 Zn2 1.952(3) 2 ? C11 C12 1.372(5) . ? C12 C13 1.364(5) . ? C13 C14 1.386(5) . ? C14 C15 1.368(5) . ? C21 C22 1.399(5) . ? C22 C23 1.376(5) . ? C23 C24 1.374(5) . ? C24 C25 1.377(5) . ? C31 C32 1.387(5) . ? C32 C33 1.388(6) . ? C33 C34 1.368(6) . ? C34 C35 1.365(5) . ? C41 C42 1.387(5) . ? C42 C43 1.374(5) . ? C43 C44 1.392(5) . ? C44 C45 1.359(5) . ? C51 C52 1.397(4) . ? C52 C53 1.374(5) . ? C53 C54 1.373(5) . ? C54 C55 1.381(5) . ? C61 C62 1.379(5) . ? C62 C63 1.360(5) . ? C63 C64 1.377(6) . ? C64 C65 1.377(5) . ? 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 O1 Zn1 O1 77.41(12) 2_565 . ? O1 Zn1 N1 122.91(12) 2_565 . ? O1 Zn1 N1 93.43(11) . . ? O1 Zn1 N2 126.30(12) 2_565 . ? O1 Zn1 N2 94.48(12) . . ? N1 Zn1 N2 110.40(11) . . ? O1 Zn1 C1 103.59(12) 2_565 . ? O1 Zn1 C1 179.00(12) . . ? N1 Zn1 C1 86.01(12) . . ? N2 Zn1 C1 84.95(12) . . ? O1 Zn1 Zn1 39.75(7) 2_565 2_565 ? O1 Zn1 Zn1 37.67(8) . 2_565 ? N1 Zn1 Zn1 112.30(8) . 2_565 ? N2 Zn1 Zn1 114.95(8) . 2_565 ? C1 Zn1 Zn1 143.34(9) . 2_565 ? O2 Zn2 O2 79.07(10) 2 . ? O2 Zn2 N4 114.75(11) 2 . ? O2 Zn2 N4 93.41(11) . . ? O2 Zn2 N5 111.29(11) 2 . ? O2 Zn2 N5 91.41(11) . . ? N4 Zn2 N5 133.80(11) . . ? O2 Zn2 C2 110.14(11) 2 . ? O2 Zn2 C2 170.78(12) . . ? N4 Zn2 C2 83.24(11) . . ? N5 Zn2 C2 84.82(11) . . ? O2 Zn2 Zn2 40.49(7) 2 2 ? O2 Zn2 Zn2 38.58(7) . 2 ? N4 Zn2 Zn2 107.77(8) . 2 ? N5 Zn2 Zn2 104.29(8) . 2 ? C2 Zn2 Zn2 150.62(9) . 2 ? C11 S1 C1 104.32(17) . . ? C21 S2 C1 102.95(16) . . ? C1 S3 C31 106.12(17) . . ? C41 S4 C2 102.90(16) . . ? C51 S5 C2 104.01(16) . . ? C2 S6 C61 107.04(17) . . ? C11 N1 C15 118.0(3) . . ? C11 N1 Zn1 119.2(2) . . ? C15 N1 Zn1 122.7(3) . . ? C21 N2 C25 117.8(3) . . ? C21 N2 Zn1 118.8(2) . . ? C25 N2 Zn1 123.2(3) . . ? C31 N3 C35 117.4(3) . . ? C41 N4 C45 118.2(3) . . ? C41 N4 Zn2 119.3(2) . . ? C45 N4 Zn2 122.5(2) . . ? C51 N5 C55 119.1(3) . . ? C51 N5 Zn2 118.6(2) . . ? C55 N5 Zn2 121.9(2) . . ? C61 N6 C65 116.9(3) . . ? Zn1 O1 Zn1 102.59(12) 2_565 . ? Zn2 O2 Zn2 100.93(10) 2 . ? S3 C1 S1 112.33(19) . . ? S3 C1 S2 112.83(18) . . ? S1 C1 S2 109.85(18) . . ? S3 C1 Zn1 103.30(16) . . ? S1 C1 Zn1 109.27(16) . . ? S2 C1 Zn1 108.99(16) . . ? S6 C2 S5 112.78(18) . . ? S6 C2 S4 111.68(17) . . ? S5 C2 S4 109.36(18) . . ? S6 C2 Zn2 102.34(16) . . ? S5 C2 Zn2 110.86(16) . . ? S4 C2 Zn2 109.64(16) . . ? N1 C11 C12 121.9(3) . . ? N1 C11 S1 120.5(3) . . ? C12 C11 S1 117.6(3) . . ? C11 C12 C13 119.3(4) . . ? C12 C13 C14 120.0(4) . . ? C15 C14 C13 117.6(4) . . ? N1 C15 C14 123.0(4) . . ? N2 C21 C22 122.1(3) . . ? N2 C21 S2 120.4(3) . . ? C22 C21 S2 117.5(3) . . ? C23 C22 C21 118.4(4) . . ? C24 C23 C22 120.4(4) . . ? C25 C24 C23 117.7(4) . . ? N2 C25 C24 123.6(4) . . ? N3 C31 C32 123.4(3) . . ? N3 C31 S3 118.8(3) . . ? C32 C31 S3 117.8(3) . . ? C31 C32 C33 117.6(4) . . ? C34 C33 C32 119.4(4) . . ? C33 C34 C35 118.1(4) . . ? N3 C35 C34 124.1(4) . . ? N4 C41 C42 122.2(3) . . ? N4 C41 S4 119.8(3) . . ? C42 C41 S4 117.9(3) . . ? C43 C42 C41 119.3(4) . . ? C42 C43 C44 118.6(4) . . ? C45 C44 C43 118.9(4) . . ? N4 C45 C44 122.8(4) . . ? N5 C51 C52 121.7(3) . . ? N5 C51 S5 121.1(3) . . ? C52 C51 S5 117.2(3) . . ? C53 C52 C51 118.3(3) . . ? C54 C53 C52 120.3(4) . . ? C53 C54 C55 118.0(4) . . ? N5 C55 C54 122.5(4) . . ? N6 C61 C62 122.3(4) . . ? N6 C61 S6 120.0(3) . . ? C62 C61 S6 117.7(3) . . ? C63 C62 C61 119.4(4) . . ? C62 C63 C64 119.9(4) . . ? C63 C64 C65 117.0(4) . . ? N6 C65 C64 124.4(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.74 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.517 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.116 # Attachment '- tpbis10(bicarb).cif' data_tpbis10 _database_code_depnum_ccdc_archive 'CCDC 867642' #TrackingRef '- tpbis10(bicarb).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H47 B N6 O3 Zn' _chemical_formula_weight 627.93 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' B B 0.0013 0.0007 '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' 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(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.750(4) _cell_length_b 19.725(7) _cell_length_c 15.634(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.283(6) _cell_angle_gamma 90.00 _cell_volume 3314(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1637 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 17.60 _exptl_crystal_description PLATE _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.258 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.781 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.9122 _exptl_absorpt_correction_T_max 0.9846 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33541 _diffrn_reflns_av_R_equivalents 0.1485 _diffrn_reflns_av_sigmaI/netI 0.0965 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 24.41 _reflns_number_total 5450 _reflns_number_gt 3335 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+1.2710P] 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 5450 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1079 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.0867 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 Zn Zn 1.16128(4) 0.70444(2) 0.36706(3) 0.02597(15) Uani 1 1 d . . . O1 O 1.0904(3) 0.61781(14) 0.37042(17) 0.0373(8) Uani 1 1 d . . . O2 O 1.0607(3) 0.57824(15) 0.5019(2) 0.0531(10) Uani 1 1 d . . . O3 O 1.0197(3) 0.51537(16) 0.3883(2) 0.0510(10) Uani 1 1 d . . . H2 H 1.003(4) 0.483(2) 0.431(3) 0.061 Uiso 1 1 d . . . N11 N 1.1984(3) 0.84379(16) 0.4010(2) 0.0255(8) Uani 1 1 d . . . N12 N 1.1323(3) 0.79073(17) 0.43462(19) 0.0245(8) Uani 1 1 d . . . N21 N 1.2023(3) 0.80836(16) 0.2465(2) 0.0243(8) Uani 1 1 d . . . N22 N 1.1280(3) 0.75162(17) 0.2530(2) 0.0265(8) Uani 1 1 d . . . N31 N 1.3819(3) 0.77977(15) 0.3463(2) 0.0232(8) Uani 1 1 d . . . N32 N 1.3491(3) 0.71318(16) 0.36052(19) 0.0249(8) Uani 1 1 d . . . B B 1.2820(4) 0.8329(2) 0.3240(3) 0.0251(12) Uani 1 1 d . . . H1 H 1.327(3) 0.8824(19) 0.309(2) 0.030 Uiso 1 1 d . . . C C 1.0573(4) 0.5730(2) 0.4242(3) 0.0321(11) Uani 1 1 d . . . C11 C 1.2295(4) 0.9682(2) 0.4233(3) 0.0437(13) Uani 1 1 d . . . H11A H 1.3205 0.9650 0.4264 0.066 Uiso 1 1 calc R . . H11B H 1.2013 1.0022 0.4642 0.066 Uiso 1 1 calc R . . H11C H 1.2029 0.9814 0.3653 0.066 Uiso 1 1 calc R . . C12 C 1.1746(4) 0.9013(2) 0.4444(3) 0.0283(10) Uani 1 1 d . . . C13 C 1.0910(4) 0.8848(2) 0.5067(3) 0.0302(10) Uani 1 1 d . . . H13A H 1.0568 0.9149 0.5474 0.036 Uiso 1 1 calc R . . C14 C 1.0663(4) 0.8166(2) 0.4988(2) 0.0275(10) Uani 1 1 d . . . C15 C 0.9802(4) 0.7724(2) 0.5505(3) 0.0363(12) Uani 1 1 d . . . C16 C 0.8910(4) 0.7347(2) 0.4891(3) 0.0427(12) Uani 1 1 d . . . H16A H 0.9378 0.7015 0.4561 0.064 Uiso 1 1 calc R . . H16B H 0.8508 0.7672 0.4500 0.064 Uiso 1 1 calc R . . H16C H 0.8276 0.7112 0.5221 0.064 Uiso 1 1 calc R . . C17 C 0.9050(5) 0.8182(3) 0.6085(3) 0.0728(19) Uani 1 1 d . . . H17A H 0.9619 0.8448 0.6451 0.109 Uiso 1 1 calc R . . H17B H 0.8515 0.7904 0.6443 0.109 Uiso 1 1 calc R . . H17C H 0.8535 0.8489 0.5734 0.109 Uiso 1 1 calc R . . C18 C 1.0559(5) 0.7227(2) 0.6049(3) 0.0530(15) Uani 1 1 d . . . H18A H 1.1119 0.7478 0.6437 0.079 Uiso 1 1 calc R . . H18B H 1.1050 0.6936 0.5676 0.079 Uiso 1 1 calc R . . H18C H 0.9997 0.6946 0.6383 0.079 Uiso 1 1 calc R . . C21 C 1.2559(4) 0.8980(2) 0.1411(3) 0.0361(11) Uani 1 1 d . . . H21A H 1.2458 0.9335 0.1842 0.054 Uiso 1 1 calc R . . H21B H 1.2220 0.9137 0.0859 0.054 Uiso 1 1 calc R . . H21C H 1.3445 0.8875 0.1356 0.054 Uiso 1 1 calc R . . C22 C 1.1882(4) 0.8359(2) 0.1678(3) 0.0247(10) Uani 1 1 d . . . C23 C 1.1044(3) 0.7966(2) 0.1234(2) 0.0293(10) Uani 1 1 d . . . H23A H 1.0761 0.8034 0.0661 0.035 Uiso 1 1 calc R . . C24 C 1.0683(4) 0.7449(2) 0.1774(3) 0.0260(10) Uani 1 1 d . . . C25 C 0.9755(4) 0.6884(2) 0.1593(2) 0.0293(11) Uani 1 1 d . . . C26 C 1.0442(4) 0.6206(2) 0.1547(3) 0.0425(12) Uani 1 1 d . . . H26A H 1.0802 0.6095 0.2112 0.064 Uiso 1 1 calc R . . H26B H 1.1107 0.6238 0.1131 0.064 Uiso 1 1 calc R . . H26C H 0.9856 0.5849 0.1371 0.064 Uiso 1 1 calc R . . C27 C 0.9083(4) 0.7019(3) 0.0740(3) 0.0475(13) Uani 1 1 d . . . H27A H 0.8637 0.7451 0.0769 0.071 Uiso 1 1 calc R . . H27B H 0.8489 0.6653 0.0619 0.071 Uiso 1 1 calc R . . H27C H 0.9691 0.7040 0.0283 0.071 Uiso 1 1 calc R . . C28 C 0.8787(4) 0.6859(2) 0.2287(3) 0.0365(12) Uani 1 1 d . . . H28A H 0.8400 0.7306 0.2344 0.055 Uiso 1 1 calc R . . H28B H 0.9190 0.6731 0.2832 0.055 Uiso 1 1 calc R . . H28C H 0.8148 0.6524 0.2133 0.055 Uiso 1 1 calc R . . C31 C 1.5709(4) 0.8518(2) 0.3395(3) 0.0422(12) Uani 1 1 d . . . H31A H 1.5462 0.8724 0.2847 0.063 Uiso 1 1 calc R . . H31B H 1.6611 0.8446 0.3413 0.063 Uiso 1 1 calc R . . H31C H 1.5479 0.8820 0.3863 0.063 Uiso 1 1 calc R . . C32 C 1.5067(4) 0.7858(2) 0.3490(2) 0.0273(10) Uani 1 1 d . . . C33 C 1.5547(4) 0.7225(2) 0.3642(3) 0.0320(11) Uani 1 1 d . . . H33A H 1.6404 0.7110 0.3693 0.038 Uiso 1 1 calc R . . C34 C 1.4550(4) 0.6784(2) 0.3709(2) 0.0278(10) Uani 1 1 d . . . C35 C 1.4576(4) 0.6028(2) 0.3844(3) 0.0364(11) Uani 1 1 d . . . C36 C 1.5924(4) 0.5791(2) 0.3929(3) 0.0536(14) Uani 1 1 d . . . H36A H 1.6309 0.5988 0.4446 0.080 Uiso 1 1 calc R . . H36B H 1.6383 0.5938 0.3426 0.080 Uiso 1 1 calc R . . H36C H 1.5947 0.5295 0.3968 0.080 Uiso 1 1 calc R . . C37 C 1.3903(4) 0.5840(2) 0.4656(3) 0.0391(12) Uani 1 1 d . . . H37A H 1.4347 0.6035 0.5152 0.059 Uiso 1 1 calc R . . H37B H 1.3877 0.5346 0.4714 0.059 Uiso 1 1 calc R . . H37C H 1.3053 0.6019 0.4627 0.059 Uiso 1 1 calc R . . C38 C 1.3956(5) 0.5674(2) 0.3070(3) 0.0560(15) Uani 1 1 d . . . H38A H 1.4368 0.5814 0.2547 0.084 Uiso 1 1 calc R . . H38B H 1.3075 0.5800 0.3033 0.084 Uiso 1 1 calc R . . H38C H 1.4029 0.5182 0.3138 0.084 Uiso 1 1 calc R . . C41 C 1.6273(4) 0.4513(2) 0.1546(3) 0.0445(13) Uani 1 1 d . . . H41A H 1.5851 0.4563 0.1009 0.053 Uiso 1 1 calc R . . C42 C 1.5918(4) 0.4015(2) 0.2102(3) 0.0448(13) Uani 1 1 d . . . H42A H 1.5250 0.3718 0.1955 0.054 Uiso 1 1 calc R . . C43 C 1.6546(4) 0.3950(2) 0.2876(3) 0.0422(12) Uani 1 1 d . . . H43A H 1.6307 0.3606 0.3265 0.051 Uiso 1 1 calc R . . C44 C 1.7515(4) 0.4378(2) 0.3093(3) 0.0377(12) Uani 1 1 d . . . H44A H 1.7937 0.4330 0.3629 0.045 Uiso 1 1 calc R . . C45 C 1.7873(4) 0.4876(2) 0.2532(3) 0.0349(11) Uani 1 1 d . . . H45A H 1.8548 0.5168 0.2675 0.042 Uiso 1 1 calc R . . C46 C 1.7244(4) 0.4945(2) 0.1767(3) 0.0395(12) Uani 1 1 d . . . H46A H 1.7477 0.5293 0.1382 0.047 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 Zn 0.0272(3) 0.0259(3) 0.0248(3) 0.0010(3) 0.00193(19) -0.0057(3) O1 0.0466(19) 0.0354(18) 0.0299(17) 0.0096(15) -0.0022(15) -0.0150(15) O2 0.086(3) 0.040(2) 0.034(2) 0.0023(17) -0.0007(19) -0.0242(18) O3 0.085(3) 0.032(2) 0.037(2) 0.0029(16) 0.0022(19) -0.0187(19) N11 0.026(2) 0.024(2) 0.027(2) 0.0016(16) 0.0012(16) 0.0003(16) N12 0.0234(18) 0.029(2) 0.0210(18) 0.0019(17) 0.0011(15) -0.0039(17) N21 0.0201(18) 0.027(2) 0.0257(19) 0.0016(16) 0.0006(15) -0.0042(16) N22 0.0218(19) 0.031(2) 0.027(2) -0.0005(17) 0.0030(16) -0.0030(17) N31 0.023(2) 0.0190(19) 0.0278(19) 0.0034(15) 0.0004(15) -0.0005(15) N32 0.0277(19) 0.023(2) 0.0241(18) 0.0014(16) 0.0014(15) -0.0003(17) B 0.023(3) 0.021(3) 0.031(3) -0.001(2) 0.001(2) -0.006(2) C 0.038(3) 0.028(3) 0.030(3) -0.002(2) -0.002(2) -0.006(2) C11 0.057(3) 0.032(3) 0.042(3) 0.001(2) 0.010(3) -0.001(2) C12 0.027(2) 0.030(3) 0.027(2) -0.001(2) -0.001(2) 0.002(2) C13 0.028(3) 0.030(3) 0.032(3) -0.005(2) 0.000(2) 0.004(2) C14 0.025(2) 0.034(3) 0.023(2) -0.005(2) 0.001(2) -0.001(2) C15 0.036(3) 0.045(3) 0.028(3) -0.008(2) 0.011(2) -0.011(2) C16 0.033(3) 0.057(3) 0.038(3) -0.001(2) 0.007(2) -0.011(2) C17 0.074(4) 0.073(4) 0.073(4) -0.030(3) 0.051(3) -0.029(3) C18 0.059(3) 0.062(4) 0.037(3) 0.015(3) -0.004(3) -0.027(3) C21 0.040(3) 0.031(3) 0.038(3) 0.007(2) 0.006(2) 0.003(2) C22 0.024(2) 0.026(2) 0.025(2) 0.004(2) 0.009(2) 0.0083(19) C23 0.027(2) 0.039(3) 0.022(2) -0.001(2) -0.0006(19) 0.008(2) C24 0.019(2) 0.038(3) 0.021(2) -0.001(2) 0.0040(19) 0.003(2) C25 0.026(2) 0.038(3) 0.024(2) -0.001(2) 0.0001(19) -0.004(2) C26 0.043(3) 0.046(3) 0.039(3) -0.012(2) 0.004(2) -0.008(2) C27 0.051(3) 0.062(3) 0.029(3) 0.002(3) -0.009(2) -0.013(3) C28 0.027(2) 0.044(3) 0.038(3) 0.001(2) -0.002(2) -0.007(2) C31 0.028(3) 0.043(3) 0.056(3) 0.004(3) 0.005(2) -0.007(2) C32 0.024(2) 0.035(3) 0.023(2) 0.001(2) 0.0030(18) -0.003(2) C33 0.022(2) 0.041(3) 0.033(3) -0.001(2) 0.002(2) 0.005(2) C34 0.031(3) 0.032(3) 0.021(2) -0.0038(19) 0.0002(19) 0.007(2) C35 0.051(3) 0.030(3) 0.028(3) 0.005(2) 0.001(2) 0.009(2) C36 0.059(4) 0.048(3) 0.054(3) 0.012(3) 0.020(3) 0.027(3) C37 0.054(3) 0.033(3) 0.031(3) 0.008(2) 0.005(2) 0.003(2) C38 0.106(5) 0.024(3) 0.038(3) -0.003(2) -0.003(3) -0.006(3) C41 0.034(3) 0.050(3) 0.049(3) 0.003(3) -0.002(2) 0.000(3) C42 0.029(3) 0.047(3) 0.059(4) -0.001(3) 0.004(3) -0.004(2) C43 0.040(3) 0.041(3) 0.047(3) -0.001(3) 0.020(3) -0.002(3) C44 0.042(3) 0.039(3) 0.033(3) -0.005(2) 0.002(2) 0.006(2) C45 0.035(3) 0.035(3) 0.034(3) -0.006(2) 0.001(2) 0.002(2) C46 0.039(3) 0.033(3) 0.047(3) 0.007(2) 0.000(2) -0.004(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 Zn O1 1.872(3) . ? Zn N12 2.031(3) . ? Zn N32 2.032(3) . ? Zn N22 2.036(3) . ? Zn O2 3.451(3) . ? O1 C 1.277(5) . ? O2 C 1.218(5) . ? O3 H2 0.94(5) . ? O3 C 1.326(5) . ? N11 C12 1.349(5) . ? N11 N12 1.376(4) . ? N11 B 1.533(6) . ? N12 C14 1.343(5) . ? N21 C22 1.350(5) . ? N21 N22 1.380(4) . ? N21 B 1.547(6) . ? N22 C24 1.339(5) . ? N31 C32 1.346(5) . ? N31 N32 1.379(4) . ? N31 B 1.535(6) . ? N32 C34 1.336(5) . ? B H1 1.12(4) . ? C11 C12 1.485(6) . ? C12 C13 1.380(5) . ? C13 C14 1.377(5) . ? C14 C15 1.517(6) . ? C15 C18 1.522(6) . ? C15 C17 1.525(6) . ? C15 C16 1.534(6) . ? C21 C22 1.489(5) . ? C22 C23 1.366(5) . ? C23 C24 1.383(5) . ? C24 C25 1.518(5) . ? C25 C28 1.521(5) . ? C25 C27 1.526(5) . ? C25 C26 1.532(6) . ? C31 C32 1.482(5) . ? C32 C33 1.370(5) . ? C33 C34 1.387(6) . ? C34 C35 1.507(6) . ? C35 C37 1.522(6) . ? C35 C36 1.525(6) . ? C35 C38 1.535(6) . ? C41 C42 1.372(6) . ? C41 C46 1.384(6) . ? C42 C43 1.379(6) . ? C43 C44 1.378(6) . ? C44 C45 1.377(6) . ? C45 C46 1.367(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 O1 Zn N12 133.10(13) . . ? O1 Zn N32 118.97(13) . . ? N12 Zn N32 96.84(12) . . ? O1 Zn N22 112.22(13) . . ? N12 Zn N22 92.65(13) . . ? N32 Zn N22 94.17(13) . . ? O1 Zn O2 36.04(10) . . ? N12 Zn O2 103.48(11) . . ? N32 Zn O2 114.66(11) . . ? N22 Zn O2 144.42(11) . . ? C O1 Zn 140.4(3) . . ? C O2 Zn 57.0(2) . . ? H2 O3 C 110(3) . . ? C12 N11 N12 110.0(3) . . ? C12 N11 B 129.3(3) . . ? N12 N11 B 120.7(3) . . ? C14 N12 N11 106.4(3) . . ? C14 N12 Zn 142.8(3) . . ? N11 N12 Zn 110.6(2) . . ? C22 N21 N22 109.9(3) . . ? C22 N21 B 129.6(3) . . ? N22 N21 B 120.5(3) . . ? C24 N22 N21 106.3(3) . . ? C24 N22 Zn 143.1(3) . . ? N21 N22 Zn 110.2(2) . . ? C32 N31 N32 109.7(3) . . ? C32 N31 B 129.7(3) . . ? N32 N31 B 120.5(3) . . ? C34 N32 N31 106.8(3) . . ? C34 N32 Zn 142.7(3) . . ? N31 N32 Zn 110.3(2) . . ? H1 B N11 107.9(18) . . ? H1 B N31 109.9(18) . . ? N11 B N31 109.7(3) . . ? H1 B N21 110.1(18) . . ? N11 B N21 109.6(3) . . ? N31 B N21 109.6(3) . . ? O2 C O1 126.5(4) . . ? O2 C O3 119.8(4) . . ? O1 C O3 113.6(4) . . ? N11 C12 C13 106.9(4) . . ? N11 C12 C11 123.7(4) . . ? C13 C12 C11 129.4(4) . . ? C14 C13 C12 107.1(4) . . ? N12 C14 C13 109.5(4) . . ? N12 C14 C15 121.3(4) . . ? C13 C14 C15 129.2(4) . . ? C14 C15 C18 110.0(4) . . ? C14 C15 C17 108.3(4) . . ? C18 C15 C17 109.5(4) . . ? C14 C15 C16 109.0(3) . . ? C18 C15 C16 110.8(4) . . ? C17 C15 C16 109.2(4) . . ? N21 C22 C23 107.1(3) . . ? N21 C22 C21 122.7(4) . . ? C23 C22 C21 130.2(4) . . ? C22 C23 C24 107.4(4) . . ? N22 C24 C23 109.3(4) . . ? N22 C24 C25 122.5(4) . . ? C23 C24 C25 128.2(4) . . ? C24 C25 C28 110.3(3) . . ? C24 C25 C27 109.4(3) . . ? C28 C25 C27 108.2(3) . . ? C24 C25 C26 109.6(3) . . ? C28 C25 C26 110.0(3) . . ? C27 C25 C26 109.3(4) . . ? N31 C32 C33 107.2(4) . . ? N31 C32 C31 122.7(4) . . ? C33 C32 C31 130.0(4) . . ? C32 C33 C34 107.2(4) . . ? N32 C34 C33 109.1(4) . . ? N32 C34 C35 122.6(4) . . ? C33 C34 C35 128.3(4) . . ? C34 C35 C37 110.5(3) . . ? C34 C35 C36 109.3(4) . . ? C37 C35 C36 108.8(4) . . ? C34 C35 C38 109.5(3) . . ? C37 C35 C38 109.9(4) . . ? C36 C35 C38 108.9(4) . . ? C42 C41 C46 120.1(5) . . ? C41 C42 C43 119.0(5) . . ? C44 C43 C42 120.8(5) . . ? C45 C44 C43 120.1(4) . . ? C46 C45 C44 119.2(4) . . ? C45 C46 C41 120.9(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H2 O2 0.94(5) 1.76(5) 2.678(4) 167(4) 3_766 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.41 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.308 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.071 # Attachment '- zn2co3s10(carb).cif' data_zn2co3s10 _database_code_depnum_ccdc_archive 'CCDC 867643' #TrackingRef '- zn2co3s10(carb).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H30 N6 O3 S6 Zn2' _chemical_formula_weight 953.79 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.3176(17) _cell_length_b 10.4067(8) _cell_length_c 17.2733(14) _cell_angle_alpha 90.00 _cell_angle_beta 99.2290(10) _cell_angle_gamma 90.00 _cell_volume 3959.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9941 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 30.43 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 1.575 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.6668 _exptl_absorpt_correction_T_max 0.9397 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 60665 _diffrn_reflns_av_R_equivalents 0.1008 _diffrn_reflns_av_sigmaI/netI 0.0832 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 30.58 _reflns_number_total 12104 _reflns_number_gt 7567 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+12.6781P] 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 12104 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1231 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1801 _refine_ls_wR_factor_gt 0.1536 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _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 Zn1 Zn 0.39181(2) 0.27508(5) 0.11478(3) 0.01733(12) Uani 1 1 d . . . Zn2 Zn 0.20857(3) 0.52552(5) 0.08393(3) 0.01987(13) Uani 1 1 d . . . S1 S 0.36452(6) -0.00318(12) 0.02887(7) 0.0242(3) Uani 1 1 d . . . S2 S 0.49251(6) 0.07453(12) 0.07720(7) 0.0217(2) Uani 1 1 d . . . S3 S 0.41543(7) 0.19317(12) -0.05959(6) 0.0265(3) Uani 1 1 d . . . S4 S 0.06458(6) 0.54142(12) 0.06745(8) 0.0258(3) Uani 1 1 d . . . S5 S 0.12894(6) 0.77465(12) 0.03017(7) 0.0247(3) Uani 1 1 d . . . S6 S 0.14191(6) 0.68492(13) 0.19566(7) 0.0260(3) Uani 1 1 d . . . O1 O 0.36240(15) 0.4153(3) 0.18127(18) 0.0208(7) Uani 1 1 d . . . O2 O 0.28871(16) 0.4011(3) 0.07789(18) 0.0231(7) Uani 1 1 d . . . O3 O 0.27956(15) 0.5405(3) 0.17258(19) 0.0216(7) Uani 1 1 d . . . N1 N 0.33603(18) 0.1283(4) 0.1520(2) 0.0220(8) Uani 1 1 d . . . N2 N 0.47448(18) 0.2458(4) 0.1887(2) 0.0175(8) Uani 1 1 d . . . N3 N 0.41464(18) 0.4061(4) 0.0281(2) 0.0206(8) Uani 1 1 d . . . N4 N 0.15333(19) 0.3638(4) 0.0753(2) 0.0228(8) Uani 1 1 d . . . N5 N 0.22246(19) 0.6385(4) -0.0112(2) 0.0224(8) Uani 1 1 d . . . N6 N 0.0389(2) 0.8113(5) 0.1422(3) 0.0305(10) Uani 1 1 d . . . C1 C 0.4172(2) 0.1273(4) 0.0364(3) 0.0195(9) Uani 1 1 d . . . C2 C 0.1314(2) 0.6396(5) 0.0949(3) 0.0218(9) Uani 1 1 d . . . C3 C 0.3111(2) 0.4526(4) 0.1447(3) 0.0197(9) Uani 1 1 d . . . C11 C 0.3269(2) 0.0205(5) 0.1105(3) 0.0219(9) Uani 1 1 d . . . C12 C 0.2888(3) -0.0766(5) 0.1295(3) 0.0308(12) Uani 1 1 d . . . H12A H 0.2828 -0.1527 0.0989 0.037 Uiso 1 1 calc R . . C13 C 0.2600(3) -0.0600(6) 0.1938(3) 0.0376(13) Uani 1 1 d . . . H13A H 0.2337 -0.1247 0.2079 0.045 Uiso 1 1 calc R . . C14 C 0.2696(3) 0.0513(6) 0.2375(3) 0.0339(12) Uani 1 1 d . . . H14A H 0.2505 0.0640 0.2823 0.041 Uiso 1 1 calc R . . C15 C 0.3074(2) 0.1433(5) 0.2149(3) 0.0272(11) Uani 1 1 d . . . H15A H 0.3137 0.2205 0.2444 0.033 Uiso 1 1 calc R . . C21 C 0.5128(2) 0.1614(4) 0.1652(2) 0.0190(9) Uani 1 1 d . . . C22 C 0.5709(2) 0.1387(5) 0.2074(3) 0.0222(9) Uani 1 1 d . . . H22A H 0.5970 0.0771 0.1898 0.027 Uiso 1 1 calc R . . C23 C 0.5892(2) 0.2079(5) 0.2753(3) 0.0240(10) Uani 1 1 d . . . H23A H 0.6284 0.1947 0.3049 0.029 Uiso 1 1 calc R . . C24 C 0.5498(2) 0.2970(5) 0.2997(3) 0.0270(11) Uani 1 1 d . . . H24A H 0.5617 0.3463 0.3459 0.032 Uiso 1 1 calc R . . C25 C 0.4931(2) 0.3125(5) 0.2558(3) 0.0225(10) Uani 1 1 d . . . H25A H 0.4659 0.3723 0.2731 0.027 Uiso 1 1 calc R . . C31 C 0.4164(2) 0.3603(5) -0.0428(3) 0.0214(9) Uani 1 1 d . . . C32 C 0.4211(2) 0.4402(5) -0.1070(3) 0.0272(11) Uani 1 1 d . . . H32A H 0.4210 0.4050 -0.1578 0.033 Uiso 1 1 calc R . . C33 C 0.4259(2) 0.5691(5) -0.0948(3) 0.0323(12) Uani 1 1 d . . . H33A H 0.4292 0.6252 -0.1373 0.039 Uiso 1 1 calc R . . C34 C 0.4261(3) 0.6193(5) -0.0192(4) 0.0334(12) Uani 1 1 d . . . H34A H 0.4303 0.7089 -0.0093 0.040 Uiso 1 1 calc R . . C35 C 0.4199(2) 0.5338(5) 0.0401(3) 0.0279(11) Uani 1 1 d . . . H35A H 0.4194 0.5663 0.0913 0.033 Uiso 1 1 calc R . . C41 C 0.0935(2) 0.3839(5) 0.0673(3) 0.0230(10) Uani 1 1 d . . . C42 C 0.0520(3) 0.2830(5) 0.0608(3) 0.0305(11) Uani 1 1 d . . . H42A H 0.0096 0.2993 0.0548 0.037 Uiso 1 1 calc R . . C43 C 0.0742(3) 0.1570(5) 0.0635(3) 0.0347(13) Uani 1 1 d . . . H43A H 0.0470 0.0862 0.0590 0.042 Uiso 1 1 calc R . . C44 C 0.1362(3) 0.1368(5) 0.0728(3) 0.0326(12) Uani 1 1 d . . . H44A H 0.1522 0.0520 0.0754 0.039 Uiso 1 1 calc R . . C45 C 0.1743(3) 0.2409(5) 0.0782(3) 0.0268(11) Uani 1 1 d . . . H45A H 0.2169 0.2268 0.0842 0.032 Uiso 1 1 calc R . . C51 C 0.1887(2) 0.7445(5) -0.0234(3) 0.0233(10) Uani 1 1 d . . . C52 C 0.1990(3) 0.8375(5) -0.0795(3) 0.0296(11) Uani 1 1 d . . . H52A H 0.1748 0.9129 -0.0872 0.036 Uiso 1 1 calc R . . C53 C 0.2446(3) 0.8165(5) -0.1225(3) 0.0306(12) Uani 1 1 d . . . H53A H 0.2525 0.8778 -0.1603 0.037 Uiso 1 1 calc R . . C54 C 0.2791(3) 0.7050(5) -0.1105(3) 0.0291(11) Uani 1 1 d . . . H54A H 0.3103 0.6883 -0.1407 0.035 Uiso 1 1 calc R . . C55 C 0.2674(2) 0.6191(5) -0.0541(3) 0.0261(10) Uani 1 1 d . . . H55A H 0.2916 0.5439 -0.0450 0.031 Uiso 1 1 calc R . . C61 C 0.0801(2) 0.7882(5) 0.2047(3) 0.0281(11) Uani 1 1 d . . . C62 C 0.0785(3) 0.8413(6) 0.2796(4) 0.0399(14) Uani 1 1 d . . . H62A H 0.1085 0.8206 0.3233 0.048 Uiso 1 1 calc R . . C63 C 0.0317(3) 0.9243(7) 0.2867(4) 0.0486(17) Uani 1 1 d . . . H63A H 0.0293 0.9631 0.3359 0.058 Uiso 1 1 calc R . . C64 C -0.0117(3) 0.9511(6) 0.2226(4) 0.0455(16) Uani 1 1 d . . . H64A H -0.0442 1.0084 0.2266 0.055 Uiso 1 1 calc R . . C65 C -0.0064(3) 0.8917(6) 0.1519(4) 0.0412(14) Uani 1 1 d . . . H65A H -0.0367 0.9090 0.1079 0.049 Uiso 1 1 calc R . . C94 C 0.1307(3) 0.2026(7) 0.3159(4) 0.0446(15) Uani 1 1 d . . . H94A H 0.0925 0.1625 0.3002 0.054 Uiso 1 1 calc R . . C95 C 0.1493(3) 0.3022(6) 0.2723(3) 0.0351(13) Uani 1 1 d . . . H95A H 0.1234 0.3304 0.2264 0.042 Uiso 1 1 calc R . . C96 C 0.2040(3) 0.3607(6) 0.2938(3) 0.0332(12) Uani 1 1 d . . . H96A H 0.2164 0.4277 0.2625 0.040 Uiso 1 1 calc R . . C97 C 0.2417(3) 0.3219(7) 0.3619(3) 0.0421(15) Uani 1 1 d . . . H97A H 0.2795 0.3636 0.3784 0.051 Uiso 1 1 calc R . . C98 C 0.2230(4) 0.2205(7) 0.4056(3) 0.0492(18) Uani 1 1 d . . . H98A H 0.2485 0.1920 0.4517 0.059 Uiso 1 1 calc R . . C99 C 0.1684(4) 0.1626(7) 0.3824(4) 0.0505(18) Uani 1 1 d . . . H99A H 0.1563 0.0936 0.4124 0.061 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 0.0250(3) 0.0165(3) 0.0105(2) -0.00049(19) 0.00301(19) 0.0011(2) Zn2 0.0250(3) 0.0190(3) 0.0151(2) 0.0009(2) 0.0017(2) -0.0003(2) S1 0.0367(7) 0.0184(6) 0.0164(5) -0.0040(4) 0.0008(5) -0.0031(5) S2 0.0297(6) 0.0209(6) 0.0145(5) -0.0040(4) 0.0032(4) 0.0040(5) S3 0.0468(8) 0.0229(6) 0.0098(5) 0.0007(4) 0.0049(5) 0.0035(5) S4 0.0234(6) 0.0247(6) 0.0280(6) 0.0006(5) 0.0006(5) -0.0014(5) S5 0.0289(6) 0.0227(6) 0.0229(6) 0.0038(5) 0.0052(5) 0.0025(5) S6 0.0327(7) 0.0279(6) 0.0171(5) -0.0015(5) 0.0031(5) -0.0003(5) O1 0.0246(17) 0.0210(17) 0.0166(15) -0.0030(12) 0.0022(13) 0.0046(13) O2 0.0330(19) 0.0225(17) 0.0134(14) -0.0042(13) 0.0026(13) -0.0020(14) O3 0.0238(17) 0.0204(17) 0.0201(16) -0.0058(13) 0.0021(13) 0.0027(13) N1 0.025(2) 0.023(2) 0.0180(18) 0.0034(15) 0.0034(15) 0.0012(16) N2 0.025(2) 0.0153(18) 0.0122(16) -0.0006(13) 0.0036(14) 0.0003(14) N3 0.028(2) 0.0177(19) 0.0174(18) 0.0037(15) 0.0060(15) -0.0001(16) N4 0.028(2) 0.024(2) 0.0155(18) -0.0014(15) 0.0012(16) -0.0024(17) N5 0.027(2) 0.023(2) 0.0163(18) 0.0003(15) 0.0010(15) -0.0005(16) N6 0.033(2) 0.032(2) 0.028(2) 0.0032(19) 0.0095(19) 0.0026(19) C1 0.030(2) 0.017(2) 0.0121(18) 0.0016(16) 0.0035(17) 0.0006(18) C2 0.025(2) 0.022(2) 0.018(2) 0.0010(17) 0.0030(18) -0.0027(18) C3 0.028(2) 0.015(2) 0.017(2) -0.0016(16) 0.0042(18) -0.0036(18) C11 0.029(2) 0.018(2) 0.017(2) 0.0031(17) -0.0011(18) 0.0006(19) C12 0.038(3) 0.024(3) 0.028(3) 0.002(2) 0.000(2) -0.008(2) C13 0.039(3) 0.040(3) 0.034(3) 0.014(3) 0.007(2) -0.009(3) C14 0.037(3) 0.040(3) 0.026(3) 0.005(2) 0.011(2) -0.002(2) C15 0.033(3) 0.029(3) 0.021(2) 0.004(2) 0.008(2) 0.000(2) C21 0.030(3) 0.014(2) 0.0123(19) 0.0018(16) 0.0032(17) 0.0015(17) C22 0.028(3) 0.017(2) 0.021(2) 0.0022(17) 0.0033(19) 0.0009(18) C23 0.027(3) 0.025(2) 0.019(2) 0.0047(18) -0.0025(18) -0.0019(19) C24 0.034(3) 0.029(3) 0.016(2) -0.0034(19) -0.0008(19) 0.000(2) C25 0.032(3) 0.022(2) 0.014(2) -0.0034(17) 0.0048(18) 0.0005(19) C31 0.026(2) 0.019(2) 0.019(2) 0.0060(17) 0.0023(18) 0.0030(18) C32 0.033(3) 0.030(3) 0.020(2) 0.009(2) 0.007(2) 0.003(2) C33 0.034(3) 0.030(3) 0.034(3) 0.016(2) 0.010(2) 0.001(2) C34 0.035(3) 0.020(3) 0.047(3) 0.004(2) 0.010(2) -0.002(2) C35 0.036(3) 0.022(2) 0.027(2) -0.001(2) 0.009(2) 0.001(2) C41 0.029(3) 0.028(3) 0.0104(19) 0.0022(17) -0.0001(17) -0.003(2) C42 0.030(3) 0.033(3) 0.026(2) 0.004(2) -0.002(2) -0.005(2) C43 0.046(3) 0.023(3) 0.033(3) 0.002(2) -0.002(2) -0.013(2) C44 0.050(3) 0.016(2) 0.032(3) -0.002(2) 0.003(2) -0.001(2) C45 0.034(3) 0.024(3) 0.022(2) -0.0001(19) 0.002(2) 0.003(2) C51 0.026(2) 0.026(2) 0.017(2) 0.0024(18) -0.0003(18) -0.0065(19) C52 0.036(3) 0.027(3) 0.024(2) 0.009(2) 0.002(2) 0.001(2) C53 0.036(3) 0.034(3) 0.022(2) 0.009(2) 0.003(2) -0.004(2) C54 0.036(3) 0.036(3) 0.017(2) 0.001(2) 0.008(2) -0.002(2) C55 0.032(3) 0.026(3) 0.020(2) -0.0026(19) 0.005(2) 0.001(2) C61 0.034(3) 0.024(3) 0.029(3) -0.003(2) 0.012(2) -0.003(2) C62 0.054(4) 0.035(3) 0.033(3) -0.012(3) 0.015(3) -0.002(3) C63 0.061(4) 0.045(4) 0.047(4) -0.014(3) 0.029(3) 0.000(3) C64 0.049(4) 0.030(3) 0.064(4) -0.001(3) 0.031(3) 0.003(3) C65 0.035(3) 0.038(3) 0.052(4) 0.006(3) 0.014(3) 0.005(3) C94 0.049(4) 0.053(4) 0.035(3) -0.002(3) 0.017(3) -0.002(3) C95 0.040(3) 0.046(3) 0.019(2) 0.004(2) 0.002(2) 0.008(3) C96 0.045(3) 0.030(3) 0.025(3) 0.001(2) 0.010(2) 0.003(2) C97 0.044(4) 0.049(4) 0.031(3) -0.013(3) -0.004(3) 0.010(3) C98 0.075(5) 0.055(4) 0.016(2) 0.001(3) 0.001(3) 0.026(4) C99 0.085(6) 0.037(4) 0.035(3) 0.010(3) 0.029(4) 0.007(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 Zn1 O1 2.030(3) . ? Zn1 N2 2.091(4) . ? Zn1 N1 2.134(4) . ? Zn1 N3 2.146(4) . ? Zn1 C1 2.182(5) . ? Zn1 O2 2.636(4) . ? Zn1 O3 3.963(3) . ? Zn2 O3 2.025(3) . ? Zn2 N4 2.078(4) . ? Zn2 N5 2.083(4) . ? Zn2 C2 2.125(5) . ? Zn2 O2 2.224(4) . ? Zn2 C3 2.478(5) . ? Zn2 O1 3.752(3) . ? S1 C11 1.769(5) . ? S1 C1 1.787(5) . ? S2 C21 1.763(4) . ? S2 C1 1.801(5) . ? S3 C31 1.763(5) . ? S3 C1 1.789(4) . ? S4 C41 1.762(5) . ? S4 C2 1.807(5) . ? S5 C51 1.768(5) . ? S5 C2 1.792(5) . ? S6 C61 1.775(6) . ? S6 C2 1.781(5) . ? O1 C3 1.276(6) . ? O2 C3 1.298(5) . ? O3 C3 1.294(6) . ? N1 C11 1.329(6) . ? N1 C15 1.355(6) . ? N2 C21 1.335(6) . ? N2 C25 1.357(6) . ? N3 C31 1.320(6) . ? N3 C35 1.348(6) . ? N4 C41 1.336(6) . ? N4 C45 1.360(6) . ? N5 C51 1.334(6) . ? N5 C55 1.353(6) . ? N6 C61 1.324(7) . ? N6 C65 1.344(7) . ? C11 C12 1.393(7) . ? C12 C13 1.382(8) . ? C13 C14 1.380(9) . ? C14 C15 1.375(7) . ? C21 C22 1.401(7) . ? C22 C23 1.380(7) . ? C23 C24 1.391(7) . ? C24 C25 1.376(7) . ? C31 C32 1.404(6) . ? C32 C33 1.360(8) . ? C33 C34 1.405(8) . ? C34 C35 1.380(7) . ? C41 C42 1.393(7) . ? C42 C43 1.400(8) . ? C43 C44 1.384(8) . ? C44 C45 1.371(7) . ? C51 C52 1.414(7) . ? C52 C53 1.371(8) . ? C53 C54 1.390(8) . ? C54 C55 1.379(7) . ? C61 C62 1.412(7) . ? C62 C63 1.375(9) . ? C63 C64 1.378(10) . ? C64 C65 1.390(9) . ? C94 C99 1.374(10) . ? C94 C95 1.384(9) . ? C95 C96 1.361(8) . ? C96 C97 1.390(8) . ? C97 C98 1.400(10) . ? C98 C99 1.360(10) . ? 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 O1 Zn1 N2 95.32(14) . . ? O1 Zn1 N1 94.99(15) . . ? N2 Zn1 N1 102.24(15) . . ? O1 Zn1 N3 94.16(14) . . ? N2 Zn1 N3 103.52(15) . . ? N1 Zn1 N3 151.68(15) . . ? O1 Zn1 C1 175.52(15) . . ? N2 Zn1 C1 89.13(16) . . ? N1 Zn1 C1 84.50(16) . . ? N3 Zn1 C1 84.30(16) . . ? O1 Zn1 O2 55.27(11) . . ? N2 Zn1 O2 150.52(12) . . ? N1 Zn1 O2 84.27(13) . . ? N3 Zn1 O2 79.11(13) . . ? C1 Zn1 O2 120.26(14) . . ? O1 Zn1 O3 23.31(10) . . ? N2 Zn1 O3 118.62(11) . . ? N1 Zn1 O3 90.02(12) . . ? N3 Zn1 O3 87.90(12) . . ? C1 Zn1 O3 152.23(13) . . ? O2 Zn1 O3 31.97(8) . . ? O3 Zn2 N4 120.00(15) . . ? O3 Zn2 N5 110.82(15) . . ? N4 Zn2 N5 124.21(15) . . ? O3 Zn2 C2 115.86(16) . . ? N4 Zn2 C2 88.79(18) . . ? N5 Zn2 C2 88.89(17) . . ? O3 Zn2 O2 62.80(12) . . ? N4 Zn2 O2 89.84(15) . . ? N5 Zn2 O2 93.96(14) . . ? C2 Zn2 O2 177.13(15) . . ? O3 Zn2 C3 31.38(13) . . ? N4 Zn2 C3 106.20(16) . . ? N5 Zn2 C3 105.24(16) . . ? C2 Zn2 C3 147.09(16) . . ? O2 Zn2 C3 31.45(13) . . ? O3 Zn2 O1 30.24(10) . . ? N4 Zn2 O1 105.91(13) . . ? N5 Zn2 O1 106.54(13) . . ? C2 Zn2 O1 145.80(14) . . ? O2 Zn2 O1 32.66(9) . . ? C3 Zn2 O1 1.55(11) . . ? C11 S1 C1 103.1(2) . . ? C21 S2 C1 106.0(2) . . ? C31 S3 C1 103.1(2) . . ? C41 S4 C2 103.8(2) . . ? C51 S5 C2 103.7(2) . . ? C61 S6 C2 105.3(2) . . ? C3 O1 Zn1 106.5(3) . . ? C3 O1 Zn2 3.0(2) . . ? Zn1 O1 Zn2 108.77(12) . . ? C3 O2 Zn2 85.2(3) . . ? C3 O2 Zn1 78.1(3) . . ? Zn2 O2 Zn1 162.86(15) . . ? C3 O3 Zn2 94.0(3) . . ? C3 O3 Zn1 7.9(2) . . ? Zn2 O3 Zn1 101.84(11) . . ? C11 N1 C15 118.7(4) . . ? C11 N1 Zn1 119.2(3) . . ? C15 N1 Zn1 122.1(3) . . ? C21 N2 C25 118.3(4) . . ? C21 N2 Zn1 117.1(3) . . ? C25 N2 Zn1 124.5(3) . . ? C31 N3 C35 118.9(4) . . ? C31 N3 Zn1 117.6(3) . . ? C35 N3 Zn1 123.0(3) . . ? C41 N4 C45 119.0(4) . . ? C41 N4 Zn2 116.8(3) . . ? C45 N4 Zn2 124.2(3) . . ? C51 N5 C55 119.1(4) . . ? C51 N5 Zn2 116.1(3) . . ? C55 N5 Zn2 124.4(3) . . ? C61 N6 C65 116.6(5) . . ? S1 C1 S3 107.9(2) . . ? S1 C1 S2 111.0(2) . . ? S3 C1 S2 111.1(3) . . ? S1 C1 Zn1 110.3(2) . . ? S3 C1 Zn1 109.6(2) . . ? S2 C1 Zn1 106.9(2) . . ? S6 C2 S5 112.8(3) . . ? S6 C2 S4 112.3(3) . . ? S5 C2 S4 109.8(3) . . ? S6 C2 Zn2 104.7(2) . . ? S5 C2 Zn2 109.0(2) . . ? S4 C2 Zn2 107.9(2) . . ? O1 C3 O3 122.0(4) . . ? O1 C3 O2 120.1(4) . . ? O3 C3 O2 117.9(4) . . ? O1 C3 Zn2 175.4(3) . . ? O3 C3 Zn2 54.6(2) . . ? O2 C3 Zn2 63.4(2) . . ? N1 C11 C12 122.0(5) . . ? N1 C11 S1 119.8(4) . . ? C12 C11 S1 118.2(4) . . ? C13 C12 C11 118.7(5) . . ? C14 C13 C12 119.6(5) . . ? C15 C14 C13 118.5(5) . . ? N1 C15 C14 122.5(5) . . ? N2 C21 C22 122.4(4) . . ? N2 C21 S2 120.8(3) . . ? C22 C21 S2 116.8(4) . . ? C23 C22 C21 118.5(5) . . ? C22 C23 C24 119.4(5) . . ? C25 C24 C23 118.7(4) . . ? N2 C25 C24 122.6(5) . . ? N3 C31 C32 122.4(5) . . ? N3 C31 S3 120.5(3) . . ? C32 C31 S3 117.0(4) . . ? C33 C32 C31 118.4(5) . . ? C32 C33 C34 119.9(5) . . ? C35 C34 C33 117.7(5) . . ? N3 C35 C34 122.6(5) . . ? N4 C41 C42 122.1(5) . . ? N4 C41 S4 120.4(4) . . ? C42 C41 S4 117.5(4) . . ? C41 C42 C43 118.4(5) . . ? C44 C43 C42 119.2(5) . . ? C45 C44 C43 119.1(5) . . ? N4 C45 C44 122.3(5) . . ? N5 C51 C52 121.6(5) . . ? N5 C51 S5 121.2(4) . . ? C52 C51 S5 117.1(4) . . ? C53 C52 C51 118.6(5) . . ? C52 C53 C54 119.6(5) . . ? C55 C54 C53 118.9(5) . . ? N5 C55 C54 122.1(5) . . ? N6 C61 C62 124.0(5) . . ? N6 C61 S6 119.0(4) . . ? C62 C61 S6 116.9(5) . . ? C63 C62 C61 117.3(6) . . ? C62 C63 C64 120.1(6) . . ? C63 C64 C65 117.9(6) . . ? N6 C65 C64 124.0(6) . . ? C99 C94 C95 119.0(7) . . ? C96 C95 C94 121.3(6) . . ? C95 C96 C97 119.7(6) . . ? C96 C97 C98 118.8(6) . . ? C99 C98 C97 120.3(6) . . ? C98 C99 C94 120.8(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.58 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.895 _refine_diff_density_min -1.144 _refine_diff_density_rms 0.159 # Attachment '- znco3s10(bicarb).cif' data_znco3s10 _database_code_depnum_ccdc_archive 'CCDC 867644' #TrackingRef '- znco3s10(bicarb).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H19 N3 O3 S3 Zn' _chemical_formula_weight 546.96 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.9280(7) _cell_length_b 14.6268(12) _cell_length_c 18.4948(15) _cell_angle_alpha 90.00 _cell_angle_beta 103.8610(10) _cell_angle_gamma 90.00 _cell_volume 2344.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9941 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 29.88 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 1.346 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.7211 _exptl_absorpt_correction_T_max 0.9481 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 37376 _diffrn_reflns_av_R_equivalents 0.0733 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 30.51 _reflns_number_total 7148 _reflns_number_gt 4814 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.7384P] 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 7148 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 Zn Zn 0.75028(3) 0.465433(18) 0.239009(14) 0.01961(7) Uani 1 1 d . . . S1 S 0.83245(7) 0.51141(5) 0.08043(3) 0.02992(15) Uani 1 1 d . . . S2 S 0.53569(8) 0.42485(5) 0.07324(3) 0.03223(16) Uani 1 1 d . . . S3 S 0.58551(9) 0.61761(5) 0.11824(4) 0.03745(18) Uani 1 1 d . . . O3 O 0.8732(2) 0.40544(13) 0.46631(10) 0.0321(4) Uani 1 1 d . . . H1 H 0.925(3) 0.4334(19) 0.5023(16) 0.030(8) Uiso 1 1 d . . . O2 O 0.9664(2) 0.52129(12) 0.41129(9) 0.0312(4) Uani 1 1 d . . . O1 O 0.81079(19) 0.41691(12) 0.34538(9) 0.0278(4) Uani 1 1 d . . . N1 N 0.9749(2) 0.46846(13) 0.22207(10) 0.0208(4) Uani 1 1 d . . . N2 N 0.6136(2) 0.34773(14) 0.20958(10) 0.0234(4) Uani 1 1 d . . . N3 N 0.6273(2) 0.57865(14) 0.26415(10) 0.0233(4) Uani 1 1 d . . . C C 0.6714(3) 0.50706(16) 0.12179(12) 0.0224(5) Uani 1 1 d . . . C1 C 0.8847(3) 0.45057(16) 0.40452(13) 0.0221(5) Uani 1 1 d . . . C11 C 0.9924(3) 0.48647(15) 0.15345(13) 0.0220(5) Uani 1 1 d . . . C12 C 1.1376(3) 0.48852(17) 0.13735(15) 0.0285(5) Uani 1 1 d . . . H12A H 1.1471 0.5007 0.0882 0.034 Uiso 1 1 calc R . . C13 C 1.2657(3) 0.47273(18) 0.19354(15) 0.0311(6) Uani 1 1 d . . . H13A H 1.3655 0.4749 0.1840 0.037 Uiso 1 1 calc R . . C14 C 1.2485(3) 0.45358(19) 0.26438(15) 0.0329(6) Uani 1 1 d . . . H14A H 1.3360 0.4417 0.3039 0.039 Uiso 1 1 calc R . . C15 C 1.1027(3) 0.45210(17) 0.27645(13) 0.0270(5) Uani 1 1 d . . . H15A H 1.0913 0.4390 0.3252 0.032 Uiso 1 1 calc R . . C21 C 0.5334(3) 0.33837(17) 0.13890(13) 0.0251(5) Uani 1 1 d . . . C22 C 0.4409(3) 0.26225(19) 0.11467(16) 0.0371(6) Uani 1 1 d . . . H22A H 0.3876 0.2562 0.0639 0.045 Uiso 1 1 calc R . . C23 C 0.4282(4) 0.19618(19) 0.16571(18) 0.0432(7) Uani 1 1 d . . . H23A H 0.3652 0.1440 0.1507 0.052 Uiso 1 1 calc R . . C24 C 0.5082(4) 0.20650(19) 0.23911(18) 0.0426(7) Uani 1 1 d . . . H24A H 0.4991 0.1623 0.2754 0.051 Uiso 1 1 calc R . . C25 C 0.6008(3) 0.28138(18) 0.25865(15) 0.0331(6) Uani 1 1 d . . . H25A H 0.6584 0.2870 0.3088 0.040 Uiso 1 1 calc R . . C31 C 0.5655(3) 0.63640(17) 0.20922(13) 0.0251(5) Uani 1 1 d . . . C32 C 0.4796(3) 0.71234(19) 0.22051(15) 0.0379(7) Uani 1 1 d . . . H32A H 0.4382 0.7529 0.1806 0.045 Uiso 1 1 calc R . . C33 C 0.4558(3) 0.72775(19) 0.28995(15) 0.0377(7) Uani 1 1 d . . . H33A H 0.3964 0.7787 0.2986 0.045 Uiso 1 1 calc R . . C34 C 0.5192(3) 0.6684(2) 0.34727(14) 0.0382(7) Uani 1 1 d . . . H34A H 0.5049 0.6779 0.3960 0.046 Uiso 1 1 calc R . . C35 C 0.6032(3) 0.59572(19) 0.33211(14) 0.0336(6) Uani 1 1 d . . . H35A H 0.6469 0.5551 0.3716 0.040 Uiso 1 1 calc R . . C41 C 0.0478(4) 0.7187(2) 0.0336(2) 0.0568(9) Uani 1 1 d . . . H41A H 0.0038 0.6594 0.0319 0.068 Uiso 1 1 calc R . . C42 C -0.0370(4) 0.7932(3) 0.04393(16) 0.0509(9) Uani 1 1 d . . . H42A H -0.1394 0.7860 0.0494 0.061 Uiso 1 1 calc R . . C43 C 0.0266(4) 0.8777(3) 0.04625(17) 0.0555(10) Uani 1 1 d . . . H43A H -0.0320 0.9299 0.0531 0.067 Uiso 1 1 calc R . . C44 C 0.1753(4) 0.8886(2) 0.03876(16) 0.0520(9) Uani 1 1 d . . . H44A H 0.2194 0.9479 0.0408 0.062 Uiso 1 1 calc R . . C45 C 0.2592(3) 0.8136(3) 0.02836(16) 0.0478(8) Uani 1 1 d . . . H45A H 0.3618 0.8206 0.0231 0.057 Uiso 1 1 calc R . . C46 C 0.1950(4) 0.7286(2) 0.0256(2) 0.0545(9) Uani 1 1 d . . . H46A H 0.2528 0.6764 0.0182 0.065 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 Zn 0.01972(13) 0.02373(14) 0.01483(12) 0.00050(11) 0.00305(9) -0.00087(11) S1 0.0255(3) 0.0463(4) 0.0189(3) 0.0067(3) 0.0071(2) -0.0015(3) S2 0.0308(3) 0.0484(4) 0.0152(3) -0.0010(3) 0.0010(2) -0.0117(3) S3 0.0586(5) 0.0361(4) 0.0190(3) 0.0073(3) 0.0119(3) 0.0192(3) O3 0.0360(10) 0.0412(11) 0.0168(9) 0.0022(8) 0.0020(8) -0.0111(9) O2 0.0415(11) 0.0317(10) 0.0199(8) 0.0023(7) 0.0060(8) -0.0089(8) O1 0.0308(9) 0.0308(10) 0.0205(8) 0.0035(7) 0.0033(7) -0.0030(8) N1 0.0210(9) 0.0213(10) 0.0206(9) -0.0009(8) 0.0057(7) 0.0010(8) N2 0.0237(10) 0.0241(11) 0.0218(10) -0.0016(8) 0.0044(8) -0.0015(8) N3 0.0234(10) 0.0273(11) 0.0182(9) -0.0024(8) 0.0030(8) 0.0012(8) C 0.0225(12) 0.0271(12) 0.0182(11) 0.0006(9) 0.0058(9) -0.0019(9) C1 0.0203(11) 0.0258(13) 0.0214(11) 0.0078(9) 0.0070(9) 0.0069(9) C11 0.0231(12) 0.0207(12) 0.0228(11) -0.0023(9) 0.0065(9) -0.0016(9) C12 0.0286(13) 0.0302(14) 0.0300(13) -0.0008(11) 0.0138(11) -0.0015(10) C13 0.0234(12) 0.0361(15) 0.0355(14) -0.0048(12) 0.0107(11) -0.0022(11) C14 0.0244(12) 0.0441(16) 0.0279(13) -0.0056(12) 0.0019(10) 0.0018(12) C15 0.0276(13) 0.0315(14) 0.0211(11) -0.0032(10) 0.0043(10) 0.0025(10) C21 0.0239(12) 0.0289(13) 0.0228(12) -0.0062(10) 0.0064(10) -0.0004(10) C22 0.0360(15) 0.0389(16) 0.0350(15) -0.0128(12) 0.0056(12) -0.0097(12) C23 0.0451(18) 0.0283(15) 0.056(2) -0.0125(14) 0.0118(15) -0.0125(13) C24 0.0513(18) 0.0252(15) 0.0492(19) 0.0071(13) 0.0082(15) -0.0076(13) C25 0.0359(15) 0.0279(14) 0.0323(14) 0.0042(11) 0.0017(12) 0.0002(11) C31 0.0322(13) 0.0254(13) 0.0173(11) -0.0009(9) 0.0053(10) 0.0004(10) C32 0.0526(18) 0.0341(15) 0.0271(14) 0.0072(11) 0.0100(13) 0.0140(13) C33 0.0467(17) 0.0369(16) 0.0316(15) -0.0023(12) 0.0132(13) 0.0158(13) C34 0.0456(17) 0.0483(18) 0.0216(13) -0.0028(12) 0.0098(12) 0.0146(14) C35 0.0372(15) 0.0418(16) 0.0218(12) 0.0015(11) 0.0068(11) 0.0118(12) C41 0.050(2) 0.045(2) 0.069(2) 0.0248(17) 0.0028(18) -0.0095(16) C42 0.0302(16) 0.093(3) 0.0315(16) 0.0102(17) 0.0124(13) 0.0033(17) C43 0.064(2) 0.062(2) 0.0326(16) -0.0167(15) -0.0025(16) 0.0256(19) C44 0.078(3) 0.0384(18) 0.0292(15) -0.0014(13) -0.0085(16) -0.0196(17) C45 0.0293(15) 0.081(3) 0.0331(16) -0.0002(16) 0.0071(12) -0.0128(16) C46 0.0410(18) 0.045(2) 0.072(2) -0.0036(17) 0.0023(17) 0.0168(15) _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 Zn O1 2.0388(16) . ? Zn N3 2.100(2) . ? Zn N1 2.1033(19) . ? Zn N2 2.105(2) . ? Zn C 2.199(2) . ? S1 C11 1.753(2) . ? S1 C 1.784(2) . ? S2 C21 1.757(3) . ? S2 C 1.788(2) . ? S3 C31 1.756(2) . ? S3 C 1.784(2) . ? O3 C1 1.345(3) . ? O2 C1 1.255(3) . ? O1 C1 1.236(3) . ? N1 C11 1.341(3) . ? N1 C15 1.349(3) . ? N2 C21 1.339(3) . ? N2 C25 1.352(3) . ? N3 C31 1.335(3) . ? N3 C35 1.348(3) . ? C11 C12 1.398(3) . ? C12 C13 1.368(4) . ? C13 C14 1.384(4) . ? C14 C15 1.373(3) . ? C21 C22 1.395(3) . ? C22 C23 1.374(4) . ? C23 C24 1.382(4) . ? C24 C25 1.367(4) . ? C31 C32 1.394(4) . ? C32 C33 1.370(4) . ? C33 C34 1.382(4) . ? C34 C35 1.368(4) . ? C41 C46 1.365(5) . ? C41 C42 1.367(5) . ? C42 C43 1.356(5) . ? C43 C44 1.377(5) . ? C44 C45 1.368(5) . ? C45 C46 1.365(5) . ? 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 O1 Zn N3 95.31(7) . . ? O1 Zn N1 96.28(7) . . ? N3 Zn N1 125.76(8) . . ? O1 Zn N2 88.16(7) . . ? N3 Zn N2 113.62(8) . . ? N1 Zn N2 119.54(8) . . ? O1 Zn C 174.87(8) . . ? N3 Zn C 86.50(8) . . ? N1 Zn C 86.50(8) . . ? N2 Zn C 86.71(8) . . ? C11 S1 C 104.69(11) . . ? C21 S2 C 104.82(11) . . ? C31 S3 C 104.37(11) . . ? C1 O1 Zn 132.60(16) . . ? C11 N1 C15 118.1(2) . . ? C11 N1 Zn 118.43(15) . . ? C15 N1 Zn 123.46(16) . . ? C21 N2 C25 118.1(2) . . ? C21 N2 Zn 118.52(16) . . ? C25 N2 Zn 123.41(17) . . ? C31 N3 C35 117.6(2) . . ? C31 N3 Zn 118.24(15) . . ? C35 N3 Zn 124.14(17) . . ? S3 C S1 109.59(13) . . ? S3 C S2 110.95(13) . . ? S1 C S2 109.11(12) . . ? S3 C Zn 108.70(11) . . ? S1 C Zn 109.38(11) . . ? S2 C Zn 109.10(11) . . ? O1 C1 O2 126.2(2) . . ? O1 C1 O3 115.0(2) . . ? O2 C1 O3 118.7(2) . . ? N1 C11 C12 122.0(2) . . ? N1 C11 S1 120.81(17) . . ? C12 C11 S1 117.20(18) . . ? C13 C12 C11 118.9(2) . . ? C12 C13 C14 119.4(2) . . ? C15 C14 C13 118.8(2) . . ? N1 C15 C14 122.8(2) . . ? N2 C21 C22 122.2(2) . . ? N2 C21 S2 120.61(18) . . ? C22 C21 S2 117.18(19) . . ? C23 C22 C21 118.7(3) . . ? C22 C23 C24 119.3(3) . . ? C25 C24 C23 119.0(3) . . ? N2 C25 C24 122.7(3) . . ? N3 C31 C32 122.2(2) . . ? N3 C31 S3 120.80(18) . . ? C32 C31 S3 117.02(19) . . ? C33 C32 C31 119.1(2) . . ? C32 C33 C34 119.3(2) . . ? C35 C34 C33 118.3(2) . . ? N3 C35 C34 123.5(2) . . ? C46 C41 C42 120.7(3) . . ? C43 C42 C41 119.3(3) . . ? C42 C43 C44 120.6(3) . . ? C45 C44 C43 119.7(3) . . ? C46 C45 C44 119.8(3) . . ? C45 C46 C41 120.0(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H1 O2 0.82(3) 1.78(3) 2.602(2) 171(3) 3_766 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.488 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.084 # Attachment '- zncs10(carb).cif' data_zncs10 _database_code_depnum_ccdc_archive 'CCDC 867645' #TrackingRef '- zncs10(carb).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H28 N6 O3.50 S6 Zn2' _chemical_formula_weight 911.73 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.669(6) _cell_length_b 8.7545(18) _cell_length_c 28.505(6) _cell_angle_alpha 90.00 _cell_angle_beta 108.802(3) _cell_angle_gamma 90.00 _cell_volume 7481(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9910 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 31.36 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3712 _exptl_absorpt_coefficient_mu 1.664 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.7651 _exptl_absorpt_correction_T_max 0.9364 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 61941 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 31.36 _reflns_number_total 12294 _reflns_number_gt 8024 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+5.6820P] 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 12294 _refine_ls_number_parameters 472 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.039 _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 Zn1 Zn 0.135253(11) 0.21415(4) 0.048179(12) 0.02041(8) Uani 1 1 d . . . Zn2 Zn 0.292074(10) 0.23129(4) 0.143220(12) 0.01837(8) Uani 1 1 d . . . S1 S 0.09171(3) 0.53886(10) 0.06038(4) 0.0375(2) Uani 1 1 d . . . S2 S 0.02994(3) 0.28335(11) 0.01623(3) 0.0344(2) Uani 1 1 d . . . S3 S 0.07894(3) 0.29084(10) 0.12263(3) 0.02870(17) Uani 1 1 d . . . S4 S 0.38523(2) 0.40421(9) 0.18146(3) 0.02529(16) Uani 1 1 d . . . S5 S 0.38023(2) 0.09707(9) 0.22176(3) 0.02555(16) Uani 1 1 d . . . S6 S 0.37447(2) 0.13054(9) 0.11640(3) 0.02442(16) Uani 1 1 d . . . O1 O 0.18898(6) 0.1000(2) 0.04318(7) 0.0232(4) Uani 1 1 d . . . O2 O 0.21740(6) 0.2422(2) 0.11164(8) 0.0224(4) Uani 1 1 d . . . O3 O 0.26261(6) 0.1058(2) 0.08313(7) 0.0240(4) Uani 1 1 d . . . N1 N 0.15444(8) 0.4252(3) 0.02455(8) 0.0213(5) Uani 1 1 d . . . N2 N 0.08873(8) 0.1227(3) -0.01494(9) 0.0241(5) Uani 1 1 d . . . N3 N 0.13225(8) 0.0699(3) 0.10853(9) 0.0252(5) Uani 1 1 d . . . N4 N 0.29720(8) 0.4660(3) 0.14058(9) 0.0209(5) Uani 1 1 d . . . N5 N 0.29159(8) 0.1197(3) 0.20730(9) 0.0225(5) Uani 1 1 d . . . N6 N 0.45794(8) 0.1796(3) 0.17733(9) 0.0263(5) Uani 1 1 d . . . C1 C 0.08151(10) 0.3385(4) 0.06253(11) 0.0247(6) Uani 1 1 d . . . C2 C 0.36263(9) 0.2147(3) 0.16748(10) 0.0205(5) Uani 1 1 d . . . C3 C 0.22270(9) 0.1482(3) 0.07901(10) 0.0199(5) Uani 1 1 d . . . C11 C 0.13384(10) 0.5513(3) 0.03221(11) 0.0239(6) Uani 1 1 d . . . C12 C 0.14467(11) 0.6959(4) 0.01923(13) 0.0327(7) Uani 1 1 d . . . H12A H 0.1289 0.7834 0.0242 0.039 Uiso 1 1 calc R . . C13 C 0.17881(12) 0.7106(4) -0.00099(13) 0.0355(8) Uani 1 1 d . . . H13A H 0.1876 0.8084 -0.0090 0.043 Uiso 1 1 calc R . . C14 C 0.20001(11) 0.5790(4) -0.00934(12) 0.0297(7) Uani 1 1 d . . . H14A H 0.2232 0.5853 -0.0236 0.036 Uiso 1 1 calc R . . C15 C 0.18680(10) 0.4398(4) 0.00338(10) 0.0247(6) Uani 1 1 d . . . H15A H 0.2010 0.3502 -0.0030 0.030 Uiso 1 1 calc R . . C21 C 0.04572(10) 0.1509(4) -0.02126(11) 0.0293(7) Uani 1 1 d . . . C22 C 0.01167(12) 0.0789(5) -0.05897(13) 0.0415(9) Uani 1 1 d . . . H22A H -0.0188 0.0983 -0.0627 0.050 Uiso 1 1 calc R . . C23 C 0.02283(13) -0.0195(5) -0.09023(14) 0.0474(10) Uani 1 1 d . . . H23A H 0.0002 -0.0703 -0.1157 0.057 Uiso 1 1 calc R . . C24 C 0.06773(13) -0.0448(4) -0.08458(13) 0.0399(9) Uani 1 1 d . . . H24A H 0.0762 -0.1112 -0.1064 0.048 Uiso 1 1 calc R . . C25 C 0.09937(11) 0.0286(4) -0.04677(12) 0.0303(7) Uani 1 1 d . . . H25A H 0.1300 0.0123 -0.0429 0.036 Uiso 1 1 calc R . . C31 C 0.11038(10) 0.1223(4) 0.13816(11) 0.0261(6) Uani 1 1 d . . . C32 C 0.11123(13) 0.0460(5) 0.18144(14) 0.0419(9) Uani 1 1 d . . . H32A H 0.0956 0.0860 0.2021 0.050 Uiso 1 1 calc R . . C33 C 0.13483(15) -0.0866(5) 0.19376(16) 0.0518(11) Uani 1 1 d . . . H33A H 0.1355 -0.1405 0.2229 0.062 Uiso 1 1 calc R . . C34 C 0.15783(14) -0.1421(4) 0.16332(16) 0.0468(10) Uani 1 1 d . . . H34A H 0.1744 -0.2344 0.1711 0.056 Uiso 1 1 calc R . . C35 C 0.15593(11) -0.0596(4) 0.12155(13) 0.0331(7) Uani 1 1 d . . . H35A H 0.1721 -0.0960 0.1010 0.040 Uiso 1 1 calc R . . C41 C 0.33836(9) 0.5245(3) 0.15831(10) 0.0216(6) Uani 1 1 d . . . C42 C 0.34624(11) 0.6820(4) 0.15831(13) 0.0312(7) Uani 1 1 d . . . H42A H 0.3756 0.7215 0.1724 0.037 Uiso 1 1 calc R . . C43 C 0.31091(12) 0.7786(4) 0.13758(13) 0.0325(7) Uani 1 1 d . . . H43A H 0.3156 0.8854 0.1361 0.039 Uiso 1 1 calc R . . C44 C 0.26821(12) 0.7179(4) 0.11879(13) 0.0317(7) Uani 1 1 d . . . H44A H 0.2433 0.7828 0.1046 0.038 Uiso 1 1 calc R . . C45 C 0.26243(10) 0.5632(3) 0.12097(11) 0.0262(6) Uani 1 1 d . . . H45A H 0.2331 0.5224 0.1083 0.031 Uiso 1 1 calc R . . C51 C 0.33082(10) 0.0647(3) 0.23621(10) 0.0233(6) Uani 1 1 d . . . C52 C 0.33448(12) -0.0188(4) 0.27925(12) 0.0323(7) Uani 1 1 d . . . H52A H 0.3626 -0.0573 0.2992 0.039 Uiso 1 1 calc R . . C53 C 0.29694(13) -0.0441(4) 0.29217(13) 0.0390(8) Uani 1 1 d . . . H53A H 0.2990 -0.0977 0.3218 0.047 Uiso 1 1 calc R . . C54 C 0.25603(12) 0.0090(4) 0.26177(13) 0.0360(8) Uani 1 1 d . . . H54A H 0.2296 -0.0106 0.2696 0.043 Uiso 1 1 calc R . . C55 C 0.25453(11) 0.0907(4) 0.21988(12) 0.0291(7) Uani 1 1 d . . . H55A H 0.2266 0.1279 0.1991 0.035 Uiso 1 1 calc R . . C61 C 0.43353(10) 0.1259(3) 0.13352(11) 0.0232(6) Uani 1 1 d . . . C62 C 0.45150(11) 0.0655(4) 0.09878(12) 0.0317(7) Uani 1 1 d . . . H62A H 0.4328 0.0243 0.0684 0.038 Uiso 1 1 calc R . . C63 C 0.49734(12) 0.0672(5) 0.10983(13) 0.0399(9) Uani 1 1 d . . . H63A H 0.5107 0.0291 0.0867 0.048 Uiso 1 1 calc R . . C64 C 0.52366(11) 0.1254(5) 0.15517(13) 0.0383(8) Uani 1 1 d . . . H64A H 0.5552 0.1289 0.1636 0.046 Uiso 1 1 calc R . . C65 C 0.50276(10) 0.1780(4) 0.18763(12) 0.0305(7) Uani 1 1 d . . . H65A H 0.5208 0.2152 0.2190 0.037 Uiso 1 1 calc R . . O101 O 0.5036(4) 0.5695(9) 0.2303(4) 0.115(2) Uani 0.50 1 d PD A -1 C101 C 0.4716(4) 0.6710(13) 0.1994(5) 0.115(2) Uani 0.50 1 d PD A -1 H10A H 0.4747 0.6769 0.1660 0.138 Uiso 0.50 1 calc PR A -1 H10B H 0.4409 0.6372 0.1961 0.138 Uiso 0.50 1 calc PR A -1 C102 C 0.4808(4) 0.8113(11) 0.2234(6) 0.115(2) Uani 0.50 1 d PD A -1 H10C H 0.4670 0.8969 0.2010 0.138 Uiso 0.50 1 calc PR A -1 H10D H 0.4712 0.8146 0.2531 0.138 Uiso 0.50 1 calc PR A -1 C103 C 0.5257(4) 0.8117(11) 0.2353(6) 0.115(2) Uani 0.50 1 d PD A -1 H10E H 0.5348 0.8612 0.2089 0.138 Uiso 0.50 1 calc PR A -1 H10F H 0.5394 0.8683 0.2667 0.138 Uiso 0.50 1 calc PR A -1 C104 C 0.5385(4) 0.6686(13) 0.2405(6) 0.115(2) Uani 0.50 1 d PD A -1 H10G H 0.5582 0.6517 0.2749 0.138 Uiso 0.50 1 calc PR A -1 H10H H 0.5560 0.6472 0.2180 0.138 Uiso 0.50 1 calc PR A -1 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 0.01667(16) 0.02079(17) 0.02221(17) -0.00143(13) 0.00411(13) 0.00133(13) Zn2 0.01634(15) 0.01894(16) 0.01919(16) 0.00151(12) 0.00485(12) -0.00004(12) S1 0.0353(5) 0.0247(4) 0.0625(6) 0.0025(4) 0.0297(4) 0.0080(3) S2 0.0167(3) 0.0555(6) 0.0287(4) 0.0004(4) 0.0040(3) 0.0032(4) S3 0.0269(4) 0.0345(4) 0.0252(4) -0.0020(3) 0.0090(3) 0.0048(3) S4 0.0182(3) 0.0244(4) 0.0309(4) -0.0028(3) 0.0046(3) -0.0028(3) S5 0.0222(4) 0.0292(4) 0.0221(3) 0.0038(3) 0.0027(3) 0.0051(3) S6 0.0192(3) 0.0321(4) 0.0207(3) -0.0049(3) 0.0046(3) -0.0004(3) O1 0.0192(10) 0.0232(10) 0.0247(10) -0.0031(8) 0.0038(8) 0.0019(8) O2 0.0191(10) 0.0239(11) 0.0240(10) -0.0036(8) 0.0066(8) 0.0013(8) O3 0.0164(10) 0.0290(11) 0.0262(10) -0.0046(9) 0.0063(8) 0.0025(8) N1 0.0204(12) 0.0234(12) 0.0183(11) -0.0006(9) 0.0038(9) 0.0009(9) N2 0.0237(13) 0.0254(13) 0.0208(12) 0.0023(10) 0.0037(10) -0.0031(10) N3 0.0228(13) 0.0236(13) 0.0281(13) 0.0008(10) 0.0069(11) -0.0013(10) N4 0.0229(12) 0.0194(12) 0.0196(11) 0.0004(9) 0.0059(10) 0.0012(9) N5 0.0245(12) 0.0227(12) 0.0210(12) 0.0010(10) 0.0083(10) -0.0016(10) N6 0.0194(12) 0.0330(14) 0.0247(13) -0.0025(11) 0.0046(10) 0.0030(10) C1 0.0184(14) 0.0284(16) 0.0275(15) 0.0010(12) 0.0076(12) 0.0029(12) C2 0.0193(13) 0.0220(14) 0.0190(13) -0.0004(11) 0.0045(10) 0.0018(11) C3 0.0214(13) 0.0172(13) 0.0220(13) 0.0018(11) 0.0081(11) 0.0001(11) C11 0.0216(14) 0.0232(15) 0.0257(15) -0.0003(12) 0.0061(12) 0.0014(11) C12 0.0357(18) 0.0247(16) 0.0401(19) 0.0013(14) 0.0156(15) 0.0043(13) C13 0.043(2) 0.0267(17) 0.0369(19) 0.0024(14) 0.0138(16) -0.0027(15) C14 0.0303(17) 0.0335(18) 0.0275(16) 0.0003(13) 0.0125(13) 0.0009(13) C15 0.0251(15) 0.0273(15) 0.0220(14) -0.0034(12) 0.0078(12) 0.0001(12) C21 0.0230(15) 0.0383(18) 0.0238(15) 0.0059(13) 0.0035(12) -0.0059(13) C22 0.0267(17) 0.058(2) 0.0350(19) -0.0011(18) 0.0033(15) -0.0164(17) C23 0.043(2) 0.058(3) 0.0338(19) -0.0087(18) 0.0023(17) -0.0265(19) C24 0.049(2) 0.038(2) 0.0303(18) -0.0100(15) 0.0090(16) -0.0140(17) C25 0.0338(17) 0.0273(16) 0.0278(16) -0.0020(13) 0.0072(14) -0.0067(13) C31 0.0222(15) 0.0291(16) 0.0261(15) -0.0004(12) 0.0065(12) -0.0037(12) C32 0.043(2) 0.051(2) 0.038(2) 0.0128(17) 0.0218(17) 0.0029(17) C33 0.062(3) 0.049(2) 0.052(2) 0.024(2) 0.030(2) 0.007(2) C34 0.050(2) 0.035(2) 0.059(3) 0.0184(18) 0.024(2) 0.0081(18) C35 0.0366(18) 0.0254(16) 0.0404(19) 0.0040(14) 0.0165(15) 0.0041(14) C41 0.0215(14) 0.0227(14) 0.0210(14) -0.0008(11) 0.0072(11) 0.0000(11) C42 0.0278(16) 0.0235(16) 0.0415(19) -0.0059(13) 0.0102(14) -0.0053(12) C43 0.0369(18) 0.0193(15) 0.0402(19) -0.0019(13) 0.0112(15) -0.0012(13) C44 0.0343(17) 0.0204(15) 0.0376(18) 0.0016(13) 0.0075(14) 0.0051(13) C45 0.0266(15) 0.0238(15) 0.0275(15) 0.0016(12) 0.0078(12) 0.0017(12) C51 0.0292(15) 0.0200(14) 0.0189(13) 0.0006(11) 0.0054(12) -0.0010(12) C52 0.0398(19) 0.0285(17) 0.0247(16) 0.0042(13) 0.0050(14) -0.0008(14) C53 0.060(2) 0.0319(18) 0.0271(17) 0.0037(14) 0.0174(17) -0.0108(17) C54 0.041(2) 0.0383(19) 0.0347(18) 0.0018(15) 0.0211(16) -0.0078(16) C55 0.0290(16) 0.0310(17) 0.0296(16) 0.0031(13) 0.0126(13) -0.0026(13) C61 0.0198(14) 0.0266(15) 0.0238(14) 0.0033(12) 0.0078(11) 0.0048(11) C62 0.0306(17) 0.0421(19) 0.0224(15) -0.0020(14) 0.0085(13) 0.0098(14) C63 0.0315(18) 0.059(2) 0.0337(18) 0.0017(17) 0.0170(15) 0.0173(17) C64 0.0211(16) 0.056(2) 0.0376(19) 0.0061(17) 0.0093(14) 0.0122(15) C65 0.0215(15) 0.0412(19) 0.0265(16) -0.0003(14) 0.0047(12) 0.0051(13) O101 0.132(5) 0.089(4) 0.142(6) 0.021(4) 0.068(5) 0.032(4) C101 0.132(5) 0.089(4) 0.142(6) 0.021(4) 0.068(5) 0.032(4) C102 0.132(5) 0.089(4) 0.142(6) 0.021(4) 0.068(5) 0.032(4) C103 0.132(5) 0.089(4) 0.142(6) 0.021(4) 0.068(5) 0.032(4) C104 0.132(5) 0.089(4) 0.142(6) 0.021(4) 0.068(5) 0.032(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 Zn1 O1 2.017(2) . ? Zn1 N2 2.083(2) . ? Zn1 N1 2.121(2) . ? Zn1 N3 2.161(3) . ? Zn1 C1 2.167(3) . ? Zn1 O2 2.658(2) . ? Zn1 O3 3.946(2) . ? Zn2 O3 1.995(2) . ? Zn2 N4 2.064(2) . ? Zn2 N5 2.076(2) . ? Zn2 C2 2.120(3) . ? Zn2 O2 2.245(2) . ? Zn2 C3 2.473(3) . ? Zn2 O1 3.756(2) . ? S1 C11 1.768(3) . ? S1 C1 1.788(3) . ? S2 C21 1.755(4) . ? S2 C1 1.804(3) . ? S3 C31 1.755(3) . ? S3 C1 1.790(3) . ? S4 C41 1.765(3) . ? S4 C2 1.800(3) . ? S5 C51 1.765(3) . ? S5 C2 1.792(3) . ? S6 C61 1.775(3) . ? S6 C2 1.777(3) . ? O1 C3 1.288(3) . ? O2 C3 1.293(3) . ? O3 C3 1.286(3) . ? N1 C11 1.336(4) . ? N1 C15 1.353(4) . ? N2 C21 1.338(4) . ? N2 C25 1.346(4) . ? N3 C31 1.334(4) . ? N3 C35 1.344(4) . ? N4 C41 1.339(4) . ? N4 C45 1.361(4) . ? N5 C51 1.339(4) . ? N5 C55 1.357(4) . ? N6 C61 1.325(4) . ? N6 C65 1.354(4) . ? C11 C12 1.392(4) . ? C12 C13 1.385(5) . ? C13 C14 1.392(5) . ? C14 C15 1.375(4) . ? C21 C22 1.403(4) . ? C22 C23 1.365(5) . ? C23 C24 1.396(5) . ? C24 C25 1.372(4) . ? C31 C32 1.395(4) . ? C32 C33 1.364(5) . ? C33 C34 1.389(5) . ? C34 C35 1.377(5) . ? C41 C42 1.401(4) . ? C42 C43 1.374(5) . ? C43 C44 1.390(5) . ? C44 C45 1.371(4) . ? C51 C52 1.400(4) . ? C52 C53 1.371(5) . ? C53 C54 1.386(5) . ? C54 C55 1.380(4) . ? C61 C62 1.395(4) . ? C62 C63 1.383(5) . ? C63 C64 1.389(5) . ? C64 C65 1.378(4) . ? O101 C104 1.360(10) . ? O101 C101 1.421(10) . ? C101 C102 1.390(11) . ? C102 C103 1.350(12) . ? C103 C104 1.311(10) . ? 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 O1 Zn1 N2 97.27(9) . . ? O1 Zn1 N1 94.27(9) . . ? N2 Zn1 N1 104.81(9) . . ? O1 Zn1 N3 91.22(9) . . ? N2 Zn1 N3 105.23(10) . . ? N1 Zn1 N3 148.48(9) . . ? O1 Zn1 C1 173.47(10) . . ? N2 Zn1 C1 88.64(11) . . ? N1 Zn1 C1 86.87(10) . . ? N3 Zn1 C1 84.52(11) . . ? O1 Zn1 O2 55.33(7) . . ? N2 Zn1 O2 152.59(8) . . ? N1 Zn1 O2 79.51(8) . . ? N3 Zn1 O2 78.27(8) . . ? C1 Zn1 O2 118.75(9) . . ? O1 Zn1 O3 23.37(6) . . ? N2 Zn1 O3 120.43(8) . . ? N1 Zn1 O3 85.15(7) . . ? N3 Zn1 O3 87.83(7) . . ? C1 Zn1 O3 150.93(9) . . ? O2 Zn1 O3 32.21(5) . . ? O3 Zn2 N4 122.50(9) . . ? O3 Zn2 N5 111.24(9) . . ? N4 Zn2 N5 121.56(9) . . ? O3 Zn2 C2 113.23(9) . . ? N4 Zn2 C2 89.60(10) . . ? N5 Zn2 C2 89.24(10) . . ? O3 Zn2 O2 62.52(7) . . ? N4 Zn2 O2 91.60(8) . . ? N5 Zn2 O2 93.86(9) . . ? C2 Zn2 O2 175.45(9) . . ? O3 Zn2 C3 31.19(8) . . ? N4 Zn2 C3 109.10(9) . . ? N5 Zn2 C3 104.85(9) . . ? C2 Zn2 C3 144.38(10) . . ? O2 Zn2 C3 31.33(8) . . ? O3 Zn2 O1 29.35(6) . . ? N4 Zn2 O1 109.64(7) . . ? N5 Zn2 O1 105.84(8) . . ? C2 Zn2 O1 142.51(8) . . ? O2 Zn2 O1 33.18(6) . . ? C3 Zn2 O1 1.91(7) . . ? C11 S1 C1 104.31(14) . . ? C21 S2 C1 104.71(14) . . ? C31 S3 C1 103.90(14) . . ? C41 S4 C2 103.92(14) . . ? C51 S5 C2 103.97(13) . . ? C61 S6 C2 105.44(14) . . ? C3 O1 Zn1 106.53(17) . . ? C3 O1 Zn2 3.67(14) . . ? Zn1 O1 Zn2 109.96(7) . . ? C3 O2 Zn2 84.11(16) . . ? C3 O2 Zn1 77.11(16) . . ? Zn2 O2 Zn1 160.45(9) . . ? C3 O3 Zn2 95.35(17) . . ? C3 O3 Zn1 9.21(14) . . ? Zn2 O3 Zn1 103.97(7) . . ? C11 N1 C15 118.3(3) . . ? C11 N1 Zn1 117.6(2) . . ? C15 N1 Zn1 124.0(2) . . ? C21 N2 C25 119.2(3) . . ? C21 N2 Zn1 116.8(2) . . ? C25 N2 Zn1 123.8(2) . . ? C31 N3 C35 118.2(3) . . ? C31 N3 Zn1 117.9(2) . . ? C35 N3 Zn1 123.3(2) . . ? C41 N4 C45 118.5(3) . . ? C41 N4 Zn2 116.45(19) . . ? C45 N4 Zn2 125.1(2) . . ? C51 N5 C55 118.6(3) . . ? C51 N5 Zn2 116.24(19) . . ? C55 N5 Zn2 125.0(2) . . ? C61 N6 C65 116.9(3) . . ? S1 C1 S3 109.01(17) . . ? S1 C1 S2 111.62(17) . . ? S3 C1 S2 109.16(16) . . ? S1 C1 Zn1 108.94(14) . . ? S3 C1 Zn1 110.13(15) . . ? S2 C1 Zn1 107.97(15) . . ? S6 C2 S5 112.35(15) . . ? S6 C2 S4 112.95(15) . . ? S5 C2 S4 110.35(15) . . ? S6 C2 Zn2 103.87(13) . . ? S5 C2 Zn2 108.83(14) . . ? S4 C2 Zn2 108.14(14) . . ? O3 C3 O1 121.1(3) . . ? O3 C3 O2 118.0(3) . . ? O1 C3 O2 120.8(3) . . ? O3 C3 Zn2 53.46(14) . . ? O1 C3 Zn2 174.4(2) . . ? O2 C3 Zn2 64.56(15) . . ? N1 C11 C12 122.2(3) . . ? N1 C11 S1 120.2(2) . . ? C12 C11 S1 117.6(2) . . ? C13 C12 C11 119.1(3) . . ? C12 C13 C14 118.6(3) . . ? C15 C14 C13 118.9(3) . . ? N1 C15 C14 122.7(3) . . ? N2 C21 C22 121.2(3) . . ? N2 C21 S2 121.2(2) . . ? C22 C21 S2 117.6(3) . . ? C23 C22 C21 119.1(3) . . ? C22 C23 C24 119.6(3) . . ? C25 C24 C23 118.4(3) . . ? N2 C25 C24 122.6(3) . . ? N3 C31 C32 122.0(3) . . ? N3 C31 S3 119.8(2) . . ? C32 C31 S3 118.2(3) . . ? C33 C32 C31 119.2(3) . . ? C32 C33 C34 119.4(3) . . ? C35 C34 C33 118.1(4) . . ? N3 C35 C34 123.1(3) . . ? N4 C41 C42 121.9(3) . . ? N4 C41 S4 120.8(2) . . ? C42 C41 S4 117.3(2) . . ? C43 C42 C41 119.0(3) . . ? C42 C43 C44 119.1(3) . . ? C45 C44 C43 119.2(3) . . ? N4 C45 C44 122.3(3) . . ? N5 C51 C52 121.7(3) . . ? N5 C51 S5 121.0(2) . . ? C52 C51 S5 117.3(2) . . ? C53 C52 C51 119.0(3) . . ? C52 C53 C54 119.6(3) . . ? C55 C54 C53 118.6(3) . . ? N5 C55 C54 122.3(3) . . ? N6 C61 C62 123.8(3) . . ? N6 C61 S6 119.6(2) . . ? C62 C61 S6 116.6(2) . . ? C63 C62 C61 118.2(3) . . ? C62 C63 C64 119.1(3) . . ? C65 C64 C63 118.2(3) . . ? N6 C65 C64 123.7(3) . . ? C104 O101 C101 95.9(8) . . ? C102 C101 O101 104.6(8) . . ? C103 C102 C101 99.5(8) . . ? C104 C103 C102 106.8(7) . . ? C103 C104 O101 112.7(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 31.36 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.266 _refine_diff_density_min -1.136 _refine_diff_density_rms 0.108 # Attachment '- znns10(ZnOH).cif' data_znns10 _database_code_depnum_ccdc_archive 'CCDC 867646' #TrackingRef '- znns10(ZnOH).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40.75 H36 N6 O2 S6 Zn2' _chemical_formula_weight 964.86 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.632(3) _cell_length_b 15.474(3) _cell_length_c 22.903(5) _cell_angle_alpha 93.590(3) _cell_angle_beta 96.263(3) _cell_angle_gamma 107.390(3) _cell_volume 4225.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9870 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 30.39 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1978 _exptl_absorpt_coefficient_mu 1.475 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.7771 _exptl_absorpt_correction_T_max 0.8911 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 67413 _diffrn_reflns_av_R_equivalents 0.0910 _diffrn_reflns_av_sigmaI/netI 0.1479 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 30.62 _reflns_number_total 25729 _reflns_number_gt 11732 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+2.0071P] 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 25729 _refine_ls_number_parameters 1066 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1762 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1867 _refine_ls_wR_factor_gt 0.1477 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Zn1 Zn 0.94024(5) 1.14168(4) 0.26212(3) 0.02181(14) Uani 1 1 d . . . O1 O 0.8979(3) 1.2621(2) 0.26805(17) 0.0293(9) Uani 1 1 d D . . H11 H 0.847(3) 1.272(4) 0.283(2) 0.035 Uiso 1 1 d D . . N1 N 0.9213(4) 1.1153(3) 0.34993(18) 0.0297(11) Uani 1 1 d . . . C1 C 0.9828(4) 1.0117(3) 0.2527(2) 0.0246(12) Uani 1 1 d . . . S1 S 1.00383(16) 0.97639(12) 0.32546(6) 0.0433(4) Uani 1 1 d . . . Zn2 Zn 1.03259(5) 1.35097(4) 0.24598(3) 0.02033(14) Uani 1 1 d . . . O2 O 1.0738(3) 1.2322(2) 0.24111(18) 0.0309(9) Uani 1 1 d D . . H21 H 1.138(2) 1.230(4) 0.243(3) 0.037 Uiso 1 1 d D . . N2 N 0.7910(4) 1.0694(3) 0.20735(18) 0.0249(10) Uani 1 1 d . . . C2 C 0.9894(4) 1.4793(3) 0.2481(2) 0.0203(11) Uani 1 1 d . . . N3 N 1.0972(4) 0.8725(3) 0.24023(18) 0.0243(10) Uani 1 1 d . . . S2 S 0.87109(12) 0.92602(9) 0.20844(7) 0.0322(3) Uani 1 1 d . . . Zn3 Zn 0.87522(5) 0.45589(4) 0.50621(2) 0.02030(14) Uani 1 1 d . . . S3 S 1.10562(11) 1.04222(9) 0.21806(6) 0.0234(3) Uani 1 1 d . . . O3 O 0.9749(3) 0.4731(3) 0.44497(15) 0.0264(9) Uani 1 1 d D . . H31 H 0.955(4) 0.475(4) 0.4106(11) 0.032 Uiso 1 1 d D . . C3 C 0.7029(4) 0.3807(3) 0.4667(2) 0.0224(11) Uani 1 1 d . . . Zn4 Zn 0.87524(5) 0.95174(4) 0.00471(3) 0.02332(15) Uani 1 1 d . . . O4 O 1.0236(3) 1.0214(3) 0.05535(15) 0.0328(10) Uani 1 1 d D . . H41 H 1.042(5) 1.027(4) 0.0899(10) 0.039 Uiso 1 1 d D . . S4 S 0.94611(12) 1.49795(9) 0.17381(6) 0.0251(3) Uani 1 1 d . . . C4 C 0.7073(4) 0.8756(3) -0.0413(2) 0.0217(11) Uani 1 1 d . . . N4 N 1.0500(3) 1.3714(3) 0.15581(18) 0.0219(9) Uani 1 1 d . . . N5 N 1.1776(3) 1.4248(3) 0.30206(18) 0.0230(9) Uani 1 1 d . . . S5 S 1.10963(11) 1.57107(8) 0.28094(6) 0.0236(3) Uani 1 1 d . . . S6 S 0.87888(10) 1.45990(8) 0.29207(5) 0.0203(3) Uani 1 1 d . . . N6 N 0.8821(3) 1.6249(3) 0.26029(18) 0.0229(9) Uani 1 1 d . . . S11 S 0.64151(11) 0.29255(9) 0.51196(6) 0.0260(3) Uani 1 1 d . . . N11 N 0.8621(4) 0.3357(3) 0.55099(18) 0.0239(10) Uani 1 1 d . . . C11 C 0.9465(6) 1.0439(4) 0.3706(2) 0.0403(16) Uani 1 1 d . . . C12 C 0.9292(6) 1.0174(5) 0.4273(3) 0.0544(19) Uani 1 1 d . . . H12A H 0.9458 0.9650 0.4401 0.065 Uiso 1 1 calc R . . C13 C 0.8866(7) 1.0710(5) 0.4643(3) 0.062(2) Uani 1 1 d . . . H13A H 0.8754 1.0564 0.5033 0.075 Uiso 1 1 calc R . . C14 C 0.8612(6) 1.1451(5) 0.4433(3) 0.056(2) Uani 1 1 d . . . H14A H 0.8322 1.1822 0.4676 0.067 Uiso 1 1 calc R . . C15 C 0.8786(5) 1.1642(4) 0.3867(3) 0.0375(15) Uani 1 1 d . . . H15A H 0.8595 1.2147 0.3724 0.045 Uiso 1 1 calc R . . S21 S 0.61766(10) 0.45496(9) 0.46046(6) 0.0256(3) Uani 1 1 d . . . N21 N 0.8115(4) 0.5689(3) 0.5186(2) 0.0297(11) Uani 1 1 d . . . C21 C 0.7735(4) 0.9823(3) 0.1883(2) 0.0240(11) Uani 1 1 d . . . C22 C 0.6756(5) 0.9316(4) 0.1505(2) 0.0354(14) Uani 1 1 d . . . H22A H 0.6657 0.8705 0.1359 0.043 Uiso 1 1 calc R . . C23 C 0.5952(5) 0.9718(4) 0.1352(3) 0.0392(15) Uani 1 1 d . . . H23A H 0.5279 0.9383 0.1107 0.047 Uiso 1 1 calc R . . C24 C 0.6126(5) 1.0614(4) 0.1555(3) 0.0404(15) Uani 1 1 d . . . H24A H 0.5576 1.0905 0.1456 0.048 Uiso 1 1 calc R . . C25 C 0.7106(5) 1.1074(4) 0.1903(2) 0.0341(14) Uani 1 1 d . . . H25A H 0.7231 1.1696 0.2032 0.041 Uiso 1 1 calc R . . S31 S 0.72044(11) 0.33357(9) 0.39640(6) 0.0235(3) Uani 1 1 d . . . C31 C 1.1539(4) 0.9445(3) 0.2162(2) 0.0223(11) Uani 1 1 d . . . N31 N 0.4946(4) 0.2648(3) 0.3868(2) 0.0355(12) Uani 1 1 d . . . C32 C 1.2504(5) 0.9496(4) 0.1907(3) 0.0374(15) Uani 1 1 d . . . H32A H 1.2867 1.0018 0.1723 0.045 Uiso 1 1 calc R . . C33 C 1.2911(5) 0.8779(4) 0.1927(3) 0.0483(18) Uani 1 1 d . . . H33A H 1.3583 0.8803 0.1769 0.058 Uiso 1 1 calc R . . C34 C 1.2342(5) 0.8003(4) 0.2182(3) 0.0369(14) Uani 1 1 d . . . H34A H 1.2607 0.7491 0.2197 0.044 Uiso 1 1 calc R . . C35 C 1.1379(5) 0.8014(4) 0.2409(2) 0.0283(12) Uani 1 1 d . . . H35A H 1.0981 0.7491 0.2580 0.034 Uiso 1 1 calc R . . C41 C 1.0014(4) 1.4281(3) 0.1303(2) 0.0244(11) Uani 1 1 d . . . S42 S 0.62378(11) 0.95027(9) -0.04949(6) 0.0268(3) Uani 1 1 d . . . N42 N 0.8016(4) 1.0548(3) 0.02587(19) 0.0274(10) Uani 1 1 d . . . C42 C 0.9967(6) 1.4360(4) 0.0698(2) 0.0402(16) Uani 1 1 d . . . H42A H 0.9603 1.4754 0.0524 0.048 Uiso 1 1 calc R . . C43 C 1.0449(6) 1.3863(5) 0.0358(3) 0.0512(19) Uani 1 1 d . . . H43A H 1.0407 1.3895 -0.0057 0.061 Uiso 1 1 calc R . . C44 C 1.0993(6) 1.3319(4) 0.0627(3) 0.0451(17) Uani 1 1 d . . . H44A H 1.1367 1.2992 0.0404 0.054 Uiso 1 1 calc R . . C45 C 1.0994(5) 1.3252(4) 0.1218(2) 0.0331(13) Uani 1 1 d . . . H45A H 1.1360 1.2862 0.1398 0.040 Uiso 1 1 calc R . . C51 C 1.2027(4) 1.5148(3) 0.3104(2) 0.0232(11) Uani 1 1 d . . . S52 S 0.64150(11) 0.78495(10) 0.00134(6) 0.0268(3) Uani 1 1 d . . . N52 N 0.8595(4) 0.8312(3) 0.04759(18) 0.0270(10) Uani 1 1 d . . . C52 C 1.3038(4) 1.5703(4) 0.3437(2) 0.0280(12) Uani 1 1 d . . . H52A H 1.3189 1.6344 0.3497 0.034 Uiso 1 1 calc R . . C53 C 1.3796(5) 1.5301(4) 0.3672(2) 0.0338(14) Uani 1 1 d . . . H53A H 1.4486 1.5661 0.3891 0.041 Uiso 1 1 calc R . . C54 C 1.3542(5) 1.4353(4) 0.3585(2) 0.0357(14) Uani 1 1 d . . . H54A H 1.4053 1.4060 0.3747 0.043 Uiso 1 1 calc R . . C55 C 1.2539(5) 1.3857(4) 0.3261(2) 0.0336(14) Uani 1 1 d . . . H55A H 1.2368 1.3215 0.3201 0.040 Uiso 1 1 calc R . . C61 C 0.8370(4) 1.5604(3) 0.2943(2) 0.0206(11) Uani 1 1 d . . . S62 S 0.73529(10) 0.83364(9) -0.11028(6) 0.0228(3) Uani 1 1 d . . . N62 N 0.5096(3) 0.7637(3) -0.13125(19) 0.0273(10) Uani 1 1 d . . . C62 C 0.7595(5) 1.5683(4) 0.3323(2) 0.0306(13) Uani 1 1 d . . . H62B H 0.7301 1.5217 0.3566 0.037 Uiso 1 1 calc R . . C63 C 0.7280(5) 1.6453(4) 0.3331(3) 0.0364(14) Uani 1 1 d . . . H63A H 0.6745 1.6521 0.3577 0.044 Uiso 1 1 calc R . . C64 C 0.7737(5) 1.7143(4) 0.2982(2) 0.0317(13) Uani 1 1 d . . . H64A H 0.7532 1.7686 0.2987 0.038 Uiso 1 1 calc R . . C65 C 0.8494(4) 1.7002(4) 0.2631(2) 0.0268(12) Uani 1 1 d . . . H65A H 0.8809 1.7466 0.2392 0.032 Uiso 1 1 calc R . . C71 C 0.7010(4) 1.0492(4) -0.0026(2) 0.0256(12) Uani 1 1 d . . . C72 C 0.6531(5) 1.1193(4) 0.0046(2) 0.0324(13) Uani 1 1 d . . . H72A H 0.5822 1.1142 -0.0166 0.039 Uiso 1 1 calc R . . C73 C 0.7091(6) 1.1948(4) 0.0421(3) 0.0443(16) Uani 1 1 d . . . H73A H 0.6767 1.2422 0.0479 0.053 Uiso 1 1 calc R . . C74 C 0.8138(6) 1.2024(4) 0.0717(3) 0.0480(18) Uani 1 1 d . . . H74A H 0.8548 1.2551 0.0974 0.058 Uiso 1 1 calc R . . C75 C 0.8567(5) 1.1310(4) 0.0628(3) 0.0412(16) Uani 1 1 d . . . H75A H 0.9279 1.1354 0.0833 0.049 Uiso 1 1 calc R . . C81 C 0.7576(5) 0.7702(4) 0.0447(2) 0.0257(12) Uani 1 1 d . . . C82 C 0.7389(6) 0.6923(4) 0.0753(2) 0.0375(15) Uani 1 1 d . . . H82A H 0.6658 0.6507 0.0735 0.045 Uiso 1 1 calc R . . C83 C 0.8278(7) 0.6775(5) 0.1077(3) 0.0474(18) Uani 1 1 d . . . H83A H 0.8170 0.6258 0.1293 0.057 Uiso 1 1 calc R . . C84 C 0.9349(6) 0.7388(5) 0.1090(3) 0.0480(19) Uani 1 1 d . . . H84A H 0.9981 0.7277 0.1298 0.058 Uiso 1 1 calc R . . C85 C 0.9474(5) 0.8150(4) 0.0798(2) 0.0375(15) Uani 1 1 d . . . H85A H 1.0198 0.8580 0.0821 0.045 Uiso 1 1 calc R . . C91 C 0.6069(4) 0.7619(4) -0.1486(2) 0.0243(11) Uani 1 1 d . . . C92 C 0.6114(5) 0.7043(4) -0.1979(3) 0.0407(16) Uani 1 1 d . . . H92A H 0.6812 0.7040 -0.2095 0.049 Uiso 1 1 calc R . . C93 C 0.5117(6) 0.6484(5) -0.2289(3) 0.0517(19) Uani 1 1 d . . . H93A H 0.5123 0.6094 -0.2626 0.062 Uiso 1 1 calc R . . C94 C 0.4111(5) 0.6493(4) -0.2108(3) 0.0416(16) Uani 1 1 d . . . H94A H 0.3417 0.6110 -0.2311 0.050 Uiso 1 1 calc R . . C95 C 0.4151(5) 0.7078(4) -0.1622(3) 0.0349(14) Uani 1 1 d . . . H95A H 0.3461 0.7087 -0.1498 0.042 Uiso 1 1 calc R . . C101 C 0.2372(8) -0.3315(6) 0.0875(4) 0.084(3) Uani 1 1 d D . . H10A H 0.2717 -0.2787 0.0670 0.126 Uiso 1 1 calc R . . H10B H 0.1836 -0.3175 0.1114 0.126 Uiso 1 1 calc R . . H10C H 0.1983 -0.3838 0.0585 0.126 Uiso 1 1 calc R . . C102 C 0.3269(6) -0.3541(5) 0.1271(3) 0.0514(18) Uani 1 1 d D . . C103 C 0.3004(6) -0.4272(4) 0.1617(3) 0.0468(17) Uani 1 1 d D . . H10D H 0.2243 -0.4624 0.1605 0.056 Uiso 1 1 calc R . . C104 C 0.3809(6) -0.4493(5) 0.1971(3) 0.0494(18) Uani 1 1 d D . . H10E H 0.3601 -0.5001 0.2194 0.059 Uiso 1 1 calc R . . C105 C 0.4904(6) -0.3990(5) 0.2007(3) 0.057(2) Uani 1 1 d D . . H10F H 0.5458 -0.4147 0.2255 0.068 Uiso 1 1 calc R . . C106 C 0.5215(7) -0.3250(6) 0.1682(4) 0.072(3) Uani 1 1 d D . . H10G H 0.5979 -0.2895 0.1711 0.086 Uiso 1 1 calc R . . C107 C 0.4397(7) -0.3028(5) 0.1309(3) 0.065(2) Uani 1 1 d D . . H10H H 0.4611 -0.2526 0.1082 0.078 Uiso 1 1 calc R . . C111 C 0.3940(8) 0.0672(7) 0.5181(4) 0.105(3) Uani 1 1 d . . . H11A H 0.3765 0.0009 0.5113 0.157 Uiso 1 1 calc R . . H11B H 0.4625 0.0967 0.5014 0.157 Uiso 1 1 calc R . . H11C H 0.3319 0.0855 0.4990 0.157 Uiso 1 1 calc R . . C112 C 0.4117(7) 0.0965(7) 0.5860(5) 0.082(3) Uani 1 1 d . . . C113 C 0.4394(7) 0.1881(6) 0.6100(4) 0.072(2) Uani 1 1 d . . . H11D H 0.4417 0.2347 0.5845 0.086 Uiso 1 1 calc R . . C114 C 0.4629(8) 0.2097(7) 0.6699(5) 0.089(3) Uani 1 1 d . . . H11E H 0.4889 0.2716 0.6859 0.107 Uiso 1 1 calc R . . C115 C 0.4490(9) 0.1418(7) 0.7065(5) 0.099(3) Uani 1 1 d . . . H11F H 0.4694 0.1584 0.7478 0.119 Uiso 1 1 calc R . . C116 C 0.4091(10) 0.0552(7) 0.6878(4) 0.100(4) Uani 1 1 d . . . H11G H 0.3851 0.0106 0.7143 0.120 Uiso 1 1 calc R . . C117 C 0.4029(10) 0.0301(7) 0.6265(5) 0.114(4) Uani 1 1 d . . . H11H H 0.3929 -0.0313 0.6126 0.137 Uiso 1 1 calc R . . C121 C 0.378(3) 0.558(3) -0.0408(13) 0.16(2) Uani 0.50 1 d PD A -1 H12B H 0.3977 0.5826 -0.0779 0.237 Uiso 0.50 1 calc PR A -1 H12C H 0.3676 0.6061 -0.0140 0.237 Uiso 0.50 1 calc PR A -1 H12D H 0.3081 0.5074 -0.0487 0.237 Uiso 0.50 1 calc PR A -1 C122 C 0.4707(16) 0.5250(9) -0.0125(7) 0.075(6) Uani 0.50 1 d PD A -1 C123 C 0.454(2) 0.488(2) 0.0418(12) 0.051(8) Uani 0.50 1 d PD A -1 H12E H 0.3885 0.4856 0.0589 0.061 Uiso 0.50 1 calc PR A -1 C124 C 0.5341(13) 0.4544(9) 0.0701(6) 0.057(5) Uani 0.50 1 d PD A -1 H12F H 0.5254 0.4347 0.1082 0.068 Uiso 0.50 1 calc PR A -1 C125 C 0.6241(19) 0.4491(14) 0.0448(11) 0.077(11) Uani 0.50 1 d PD A -1 H12G H 0.6716 0.4182 0.0628 0.093 Uiso 0.50 1 calc PR A -1 C126 C 0.6482(17) 0.4881(11) -0.0071(9) 0.083(7) Uani 0.50 1 d PD A -1 H12H H 0.7159 0.4910 -0.0224 0.100 Uiso 0.50 1 calc PR A -1 C127 C 0.568(3) 0.523(3) -0.0360(14) 0.095(15) Uani 0.50 1 d PD A -1 H12I H 0.5805 0.5465 -0.0729 0.114 Uiso 0.50 1 calc PR A -1 C411 C 0.7605(4) 0.2763(4) 0.5520(2) 0.0226(11) Uani 1 1 d . . . C421 C 0.7445(5) 0.1991(4) 0.5829(2) 0.0323(13) Uani 1 1 d . . . H42B H 0.6713 0.1594 0.5842 0.039 Uiso 1 1 calc R . . C431 C 0.8359(5) 0.1817(4) 0.6110(2) 0.0368(15) Uani 1 1 d . . . H43B H 0.8270 0.1297 0.6322 0.044 Uiso 1 1 calc R . . C441 C 0.9433(5) 0.2417(4) 0.6083(2) 0.0332(14) Uani 1 1 d . . . H44B H 1.0082 0.2297 0.6263 0.040 Uiso 1 1 calc R . . C451 C 0.9525(4) 0.3187(4) 0.5789(2) 0.0289(13) Uani 1 1 d . . . H45B H 1.0246 0.3607 0.5783 0.035 Uiso 1 1 calc R . . C511 C 0.7074(4) 0.5605(4) 0.4946(2) 0.0236(11) Uani 1 1 d . . . C521 C 0.6658(5) 0.6353(4) 0.4946(2) 0.0317(13) Uani 1 1 d . . . H52B H 0.5911 0.6279 0.4777 0.038 Uiso 1 1 calc R . . C531 C 0.7340(6) 0.7184(5) 0.5191(3) 0.054(2) Uani 1 1 d . . . H53B H 0.7072 0.7695 0.5189 0.065 Uiso 1 1 calc R . . C541 C 0.8435(6) 0.7288(5) 0.5446(3) 0.058(2) Uani 1 1 d . . . H54B H 0.8925 0.7864 0.5615 0.069 Uiso 1 1 calc R . . C551 C 0.8771(5) 0.6516(4) 0.5439(3) 0.0442(17) Uani 1 1 d . . . H55B H 0.9503 0.6570 0.5622 0.053 Uiso 1 1 calc R . . C611 C 0.5876(4) 0.2583(4) 0.3650(2) 0.0277(12) Uani 1 1 d . . . C621 C 0.5836(5) 0.1959(4) 0.3177(3) 0.0440(17) Uani 1 1 d . . . H62C H 0.6502 0.1937 0.3028 0.053 Uiso 1 1 calc R . . C631 C 0.4804(6) 0.1372(5) 0.2930(3) 0.064(2) Uani 1 1 d . . . H63B H 0.4753 0.0931 0.2612 0.077 Uiso 1 1 calc R . . C641 C 0.3863(6) 0.1430(5) 0.3144(4) 0.060(2) Uani 1 1 d . . . H64B H 0.3148 0.1038 0.2974 0.072 Uiso 1 1 calc R . . C651 C 0.3966(5) 0.2075(4) 0.3617(3) 0.0498(18) Uani 1 1 d . . . H65B H 0.3306 0.2107 0.3767 0.060 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 0.0286(3) 0.0159(3) 0.0217(3) -0.0019(2) -0.0018(3) 0.0105(3) O1 0.030(2) 0.019(2) 0.041(2) 0.0001(17) 0.0027(18) 0.0122(17) N1 0.042(3) 0.033(3) 0.019(2) -0.005(2) 0.000(2) 0.023(2) C1 0.035(3) 0.023(3) 0.020(3) 0.000(2) 0.004(2) 0.016(2) S1 0.0825(13) 0.0460(10) 0.0224(7) 0.0083(7) 0.0114(8) 0.0488(10) Zn2 0.0242(3) 0.0139(3) 0.0227(3) -0.0015(2) -0.0021(2) 0.0081(2) O2 0.032(2) 0.0121(18) 0.051(3) 0.0044(17) 0.007(2) 0.0095(17) N2 0.033(3) 0.022(2) 0.022(2) -0.0001(18) -0.0018(19) 0.014(2) C2 0.024(3) 0.017(3) 0.020(2) 0.001(2) 0.002(2) 0.007(2) N3 0.035(3) 0.019(2) 0.024(2) -0.0003(18) 0.006(2) 0.015(2) S2 0.0325(8) 0.0168(7) 0.0486(9) -0.0032(6) 0.0089(7) 0.0094(6) Zn3 0.0144(3) 0.0247(3) 0.0201(3) -0.0035(2) -0.0003(2) 0.0056(2) S3 0.0261(7) 0.0170(6) 0.0286(7) 0.0012(5) 0.0027(6) 0.0094(5) O3 0.0154(18) 0.044(2) 0.0170(18) -0.0067(17) -0.0002(15) 0.0077(16) C3 0.020(3) 0.021(3) 0.028(3) 0.004(2) 0.003(2) 0.010(2) Zn4 0.0161(3) 0.0301(4) 0.0206(3) -0.0033(3) -0.0003(2) 0.0044(3) O4 0.0209(19) 0.055(3) 0.0145(18) -0.0057(19) -0.0016(16) 0.0035(18) S4 0.0374(8) 0.0261(7) 0.0186(6) 0.0025(5) 0.0015(6) 0.0207(6) C4 0.022(3) 0.022(3) 0.021(3) -0.001(2) -0.001(2) 0.009(2) N4 0.023(2) 0.017(2) 0.025(2) -0.0024(18) 0.0009(18) 0.0073(18) N5 0.023(2) 0.018(2) 0.027(2) -0.0052(18) -0.0037(18) 0.0089(18) S5 0.0221(7) 0.0139(6) 0.0339(7) -0.0013(5) 0.0017(6) 0.0055(5) S6 0.0230(6) 0.0182(6) 0.0208(6) 0.0013(5) 0.0028(5) 0.0082(5) N6 0.024(2) 0.020(2) 0.027(2) 0.0045(18) 0.0053(19) 0.0086(18) S11 0.0219(7) 0.0261(7) 0.0281(7) 0.0051(6) 0.0017(6) 0.0046(6) N11 0.026(2) 0.028(3) 0.017(2) -0.0046(18) -0.0028(18) 0.011(2) C11 0.063(4) 0.052(4) 0.021(3) 0.000(3) 0.008(3) 0.038(4) C12 0.086(6) 0.061(5) 0.029(3) 0.009(3) 0.006(4) 0.040(4) C13 0.091(6) 0.073(6) 0.031(4) 0.000(4) 0.015(4) 0.038(5) C14 0.084(6) 0.066(5) 0.027(3) -0.015(3) 0.001(3) 0.045(4) C15 0.047(4) 0.036(4) 0.035(3) -0.009(3) -0.002(3) 0.027(3) S21 0.0179(6) 0.0238(7) 0.0336(8) -0.0004(6) -0.0023(6) 0.0067(5) N21 0.021(2) 0.030(3) 0.036(3) -0.008(2) -0.003(2) 0.008(2) C21 0.034(3) 0.022(3) 0.018(3) -0.002(2) 0.009(2) 0.009(2) C22 0.038(3) 0.029(3) 0.032(3) -0.009(3) 0.007(3) 0.001(3) C23 0.032(3) 0.042(4) 0.037(3) -0.007(3) -0.007(3) 0.008(3) C24 0.037(3) 0.041(4) 0.039(4) 0.005(3) -0.015(3) 0.012(3) C25 0.043(4) 0.029(3) 0.027(3) -0.003(2) -0.009(3) 0.014(3) S31 0.0239(7) 0.0242(7) 0.0208(6) -0.0014(5) 0.0002(5) 0.0066(5) C31 0.024(3) 0.019(3) 0.025(3) 0.002(2) 0.001(2) 0.009(2) N31 0.025(3) 0.026(3) 0.048(3) -0.007(2) -0.010(2) 0.004(2) C32 0.036(3) 0.027(3) 0.054(4) 0.013(3) 0.022(3) 0.011(3) C33 0.042(4) 0.043(4) 0.072(5) 0.008(4) 0.025(4) 0.026(3) C34 0.046(4) 0.029(3) 0.046(4) 0.006(3) 0.012(3) 0.025(3) C35 0.038(3) 0.025(3) 0.029(3) 0.005(2) 0.008(3) 0.018(3) C41 0.032(3) 0.021(3) 0.020(3) -0.001(2) 0.003(2) 0.008(2) S42 0.0244(7) 0.0279(8) 0.0274(7) -0.0058(6) -0.0061(6) 0.0122(6) N42 0.024(2) 0.025(3) 0.029(2) -0.002(2) 0.004(2) 0.0013(19) C42 0.070(5) 0.039(4) 0.023(3) 0.006(3) 0.007(3) 0.033(3) C43 0.096(6) 0.050(4) 0.022(3) 0.006(3) 0.019(4) 0.041(4) C44 0.068(5) 0.043(4) 0.036(4) -0.004(3) 0.019(3) 0.032(4) C45 0.043(4) 0.031(3) 0.031(3) 0.001(3) 0.009(3) 0.020(3) C51 0.024(3) 0.022(3) 0.025(3) -0.001(2) 0.006(2) 0.008(2) S52 0.0244(7) 0.0301(8) 0.0235(7) 0.0041(6) 0.0018(6) 0.0048(6) N52 0.031(3) 0.031(3) 0.022(2) -0.0031(19) -0.002(2) 0.016(2) C52 0.029(3) 0.026(3) 0.026(3) -0.011(2) 0.000(2) 0.008(2) C53 0.023(3) 0.045(4) 0.030(3) -0.013(3) -0.007(2) 0.012(3) C54 0.032(3) 0.047(4) 0.032(3) -0.002(3) -0.007(3) 0.024(3) C55 0.035(3) 0.031(3) 0.034(3) -0.005(3) -0.010(3) 0.016(3) C61 0.018(2) 0.023(3) 0.021(3) 0.002(2) 0.000(2) 0.007(2) S62 0.0201(6) 0.0270(7) 0.0209(6) -0.0018(5) 0.0009(5) 0.0082(5) N62 0.021(2) 0.033(3) 0.028(2) -0.001(2) -0.0028(19) 0.012(2) C62 0.034(3) 0.032(3) 0.031(3) 0.009(2) 0.010(3) 0.014(3) C63 0.033(3) 0.034(3) 0.049(4) 0.006(3) 0.016(3) 0.017(3) C64 0.037(3) 0.026(3) 0.039(3) 0.002(3) 0.011(3) 0.019(3) C65 0.035(3) 0.021(3) 0.027(3) 0.004(2) 0.006(2) 0.011(2) C71 0.031(3) 0.023(3) 0.021(3) 0.001(2) 0.006(2) 0.005(2) C72 0.040(3) 0.035(3) 0.027(3) -0.003(2) 0.005(3) 0.019(3) C73 0.056(4) 0.034(4) 0.046(4) -0.008(3) 0.013(3) 0.018(3) C74 0.048(4) 0.038(4) 0.049(4) -0.021(3) -0.001(3) 0.008(3) C75 0.038(4) 0.034(4) 0.042(4) -0.017(3) 0.004(3) 0.002(3) C81 0.040(3) 0.030(3) 0.013(2) -0.005(2) 0.000(2) 0.022(3) C82 0.057(4) 0.032(3) 0.028(3) -0.001(3) 0.005(3) 0.022(3) C83 0.088(6) 0.046(4) 0.021(3) 0.004(3) 0.003(3) 0.041(4) C84 0.067(5) 0.069(5) 0.024(3) -0.002(3) -0.007(3) 0.050(4) C85 0.037(3) 0.049(4) 0.031(3) -0.011(3) -0.008(3) 0.026(3) C91 0.025(3) 0.026(3) 0.022(3) -0.004(2) -0.007(2) 0.012(2) C92 0.037(3) 0.050(4) 0.036(3) -0.017(3) -0.003(3) 0.022(3) C93 0.059(5) 0.055(4) 0.034(4) -0.031(3) -0.019(3) 0.023(4) C94 0.033(3) 0.040(4) 0.044(4) -0.016(3) -0.017(3) 0.012(3) C95 0.024(3) 0.040(4) 0.039(3) 0.000(3) -0.003(3) 0.010(3) C101 0.113(8) 0.076(7) 0.065(6) 0.005(5) -0.004(5) 0.040(6) C102 0.071(5) 0.035(4) 0.049(4) -0.007(3) 0.021(4) 0.015(4) C103 0.055(4) 0.035(4) 0.041(4) -0.004(3) 0.015(3) -0.001(3) C104 0.060(5) 0.052(5) 0.039(4) 0.002(3) 0.016(4) 0.019(4) C105 0.048(5) 0.057(5) 0.062(5) -0.014(4) 0.004(4) 0.016(4) C106 0.053(5) 0.056(6) 0.100(7) -0.016(5) 0.027(5) 0.006(4) C107 0.085(6) 0.043(5) 0.058(5) -0.007(4) 0.044(5) -0.001(4) C111 0.098(8) 0.110(9) 0.096(8) 0.012(7) 0.012(7) 0.017(7) C112 0.062(6) 0.080(7) 0.096(8) 0.021(6) 0.003(5) 0.010(5) C113 0.075(6) 0.050(5) 0.098(7) 0.015(5) 0.034(5) 0.023(4) C114 0.079(7) 0.075(7) 0.104(8) 0.010(6) 0.036(6) 0.000(5) C115 0.116(9) 0.077(8) 0.092(8) 0.036(6) -0.001(7) 0.011(6) C116 0.174(11) 0.053(6) 0.070(7) 0.017(5) 0.017(7) 0.028(7) C117 0.160(11) 0.055(6) 0.115(10) 0.032(6) 0.001(8) 0.014(7) C121 0.16(4) 0.17(4) 0.12(3) 0.02(3) -0.10(3) 0.04(3) C122 0.126(17) 0.023(8) 0.043(9) -0.002(7) -0.018(10) -0.018(10) C123 0.072(14) 0.027(10) 0.058(18) 0.002(11) 0.025(12) 0.017(12) C124 0.110(15) 0.016(6) 0.044(9) 0.004(6) 0.011(9) 0.018(8) C125 0.11(2) 0.020(9) 0.12(3) 0.012(11) 0.043(18) 0.025(12) C126 0.098(16) 0.036(10) 0.104(17) -0.029(11) 0.049(14) 0.000(10) C127 0.14(3) 0.07(2) 0.036(15) -0.013(13) 0.031(17) -0.029(18) C411 0.027(3) 0.025(3) 0.016(2) -0.006(2) 0.003(2) 0.010(2) C421 0.040(3) 0.029(3) 0.028(3) 0.003(2) 0.002(3) 0.011(3) C431 0.060(4) 0.031(3) 0.022(3) 0.002(2) -0.002(3) 0.021(3) C441 0.040(3) 0.040(4) 0.023(3) -0.002(3) -0.009(3) 0.023(3) C451 0.024(3) 0.037(3) 0.024(3) -0.012(2) -0.009(2) 0.013(2) C511 0.020(3) 0.030(3) 0.020(3) -0.004(2) 0.003(2) 0.008(2) C521 0.027(3) 0.036(3) 0.033(3) -0.009(3) 0.001(2) 0.014(3) C531 0.052(4) 0.048(4) 0.063(5) -0.026(4) -0.007(4) 0.031(4) C541 0.047(4) 0.038(4) 0.079(5) -0.030(4) -0.021(4) 0.017(3) C551 0.032(3) 0.037(4) 0.057(4) -0.025(3) -0.016(3) 0.014(3) C611 0.028(3) 0.023(3) 0.028(3) -0.004(2) -0.009(2) 0.006(2) C621 0.040(4) 0.048(4) 0.042(4) -0.019(3) -0.008(3) 0.020(3) C631 0.062(5) 0.052(5) 0.068(5) -0.040(4) -0.021(4) 0.020(4) C641 0.037(4) 0.047(4) 0.085(6) -0.024(4) -0.031(4) 0.014(3) C651 0.025(3) 0.037(4) 0.082(5) -0.009(4) -0.002(3) 0.007(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 Zn1 O2 1.972(4) . ? Zn1 O1 2.088(4) . ? Zn1 N1 2.102(4) . ? Zn1 N2 2.104(4) . ? Zn1 C1 2.235(5) . ? Zn1 Zn2 3.1578(10) . ? O1 Zn2 1.979(4) . ? N1 C11 1.337(7) . ? N1 C15 1.354(6) . ? C1 S3 1.772(5) . ? C1 S2 1.783(5) . ? C1 S1 1.803(5) . ? S1 C11 1.779(6) . ? Zn2 O2 2.054(4) . ? Zn2 N5 2.088(4) . ? Zn2 N4 2.134(4) . ? Zn2 C2 2.210(5) . ? N2 C21 1.336(6) . ? N2 C25 1.351(7) . ? C2 S6 1.773(5) . ? C2 S5 1.794(5) . ? C2 S4 1.798(5) . ? N3 C31 1.321(6) . ? N3 C35 1.347(6) . ? S2 C21 1.749(5) . ? Zn3 O3 1.963(3) . ? Zn3 O3 2.045(3) 2_766 ? Zn3 N21 2.149(4) . ? Zn3 N11 2.152(4) . ? Zn3 C3 2.199(5) . ? Zn3 Zn3 3.0911(13) 2_766 ? S3 C31 1.791(5) . ? O3 Zn3 2.045(3) 2_766 ? C3 S31 1.789(5) . ? C3 S21 1.797(5) . ? C3 S11 1.804(5) . ? Zn4 O4 1.958(4) 2_775 ? Zn4 O4 2.045(4) . ? Zn4 N42 2.129(4) . ? Zn4 N52 2.129(5) . ? Zn4 C4 2.204(5) . ? Zn4 Zn4 3.0964(13) 2_775 ? O4 Zn4 1.959(4) 2_775 ? S4 C41 1.765(5) . ? C4 S62 1.782(5) . ? C4 S42 1.788(5) . ? C4 S52 1.807(5) . ? N4 C41 1.341(6) . ? N4 C45 1.345(6) . ? N5 C51 1.328(6) . ? N5 C55 1.368(6) . ? S5 C51 1.764(5) . ? S6 C61 1.786(5) . ? N6 C61 1.334(6) . ? N6 C65 1.349(6) . ? S11 C411 1.765(5) . ? N11 C411 1.340(6) . ? N11 C451 1.350(6) . ? C11 C12 1.407(8) . ? C12 C13 1.405(9) . ? C13 C14 1.380(10) . ? C14 C15 1.375(9) . ? S21 C511 1.762(5) . ? N21 C511 1.333(6) . ? N21 C551 1.353(7) . ? C21 C22 1.413(7) . ? C22 C23 1.366(8) . ? C23 C24 1.379(8) . ? C24 C25 1.364(8) . ? S31 C611 1.775(5) . ? C31 C32 1.392(7) . ? N31 C651 1.332(7) . ? N31 C611 1.355(7) . ? C32 C33 1.356(8) . ? C33 C34 1.401(9) . ? C34 C35 1.378(7) . ? C41 C42 1.394(7) . ? S42 C71 1.766(5) . ? N42 C71 1.340(7) . ? N42 C75 1.358(7) . ? C42 C43 1.371(8) . ? C43 C44 1.371(9) . ? C44 C45 1.365(8) . ? C51 C52 1.414(7) . ? S52 C81 1.761(5) . ? N52 C81 1.342(7) . ? N52 C85 1.360(7) . ? C52 C53 1.371(7) . ? C53 C54 1.400(8) . ? C54 C55 1.375(7) . ? C61 C62 1.405(7) . ? S62 C91 1.767(5) . ? N62 C91 1.339(6) . ? N62 C95 1.341(7) . ? C62 C63 1.364(7) . ? C63 C64 1.398(8) . ? C64 C65 1.369(7) . ? C71 C72 1.401(7) . ? C72 C73 1.360(8) . ? C73 C74 1.387(9) . ? C74 C75 1.382(8) . ? C81 C82 1.405(8) . ? C82 C83 1.362(8) . ? C83 C84 1.397(10) . ? C84 C85 1.369(9) . ? C91 C92 1.412(7) . ? C92 C93 1.385(8) . ? C93 C94 1.383(9) . ? C94 C95 1.376(8) . ? C101 C102 1.509(10) . ? C102 C107 1.399(10) . ? C102 C103 1.400(9) . ? C103 C104 1.368(9) . ? C104 C105 1.361(9) . ? C105 C106 1.386(11) . ? C106 C107 1.404(11) . ? C111 C112 1.565(13) . ? C112 C113 1.413(12) . ? C112 C117 1.415(12) . ? C113 C114 1.370(12) . ? C114 C115 1.369(12) . ? C115 C116 1.307(12) . ? C116 C117 1.422(13) . ? C121 C122 1.515(18) . ? C122 C127 1.403(18) . ? C122 C123 1.414(17) . ? C123 C124 1.382(17) . ? C124 C125 1.352(17) . ? C125 C126 1.387(19) . ? C126 C127 1.409(18) . ? C411 C421 1.400(7) . ? C421 C431 1.366(8) . ? C431 C441 1.407(8) . ? C441 C451 1.386(8) . ? C511 C521 1.407(7) . ? C521 C531 1.361(8) . ? C531 C541 1.399(9) . ? C541 C551 1.382(8) . ? C611 C621 1.392(7) . ? C621 C631 1.383(9) . ? C631 C641 1.359(10) . ? C641 C651 1.394(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 Zn1 O1 77.10(15) . . ? O2 Zn1 N1 122.20(18) . . ? O1 Zn1 N1 95.25(16) . . ? O2 Zn1 N2 128.49(17) . . ? O1 Zn1 N2 93.44(16) . . ? N1 Zn1 N2 108.94(18) . . ? O2 Zn1 C1 103.01(17) . . ? O1 Zn1 C1 178.11(17) . . ? N1 Zn1 C1 86.30(18) . . ? N2 Zn1 C1 85.02(18) . . ? O2 Zn1 Zn2 39.27(10) . . ? O1 Zn1 Zn2 37.83(11) . . ? N1 Zn1 Zn2 113.56(13) . . ? N2 Zn1 Zn2 115.20(12) . . ? C1 Zn1 Zn2 142.22(14) . . ? Zn2 O1 Zn1 101.85(16) . . ? C11 N1 C15 117.1(5) . . ? C11 N1 Zn1 119.4(3) . . ? C15 N1 Zn1 123.4(4) . . ? S3 C1 S2 112.0(3) . . ? S3 C1 S1 113.7(3) . . ? S2 C1 S1 109.5(3) . . ? S3 C1 Zn1 103.2(2) . . ? S2 C1 Zn1 110.2(2) . . ? S1 C1 Zn1 107.9(2) . . ? C11 S1 C1 104.1(3) . . ? O1 Zn2 O2 77.75(15) . . ? O1 Zn2 N5 127.08(17) . . ? O2 Zn2 N5 94.76(16) . . ? O1 Zn2 N4 121.16(16) . . ? O2 Zn2 N4 93.66(16) . . ? N5 Zn2 N4 111.50(17) . . ? O1 Zn2 C2 103.35(17) . . ? O2 Zn2 C2 178.09(17) . . ? N5 Zn2 C2 85.83(17) . . ? N4 Zn2 C2 84.43(16) . . ? O1 Zn2 Zn1 40.32(10) . . ? O2 Zn2 Zn1 37.44(11) . . ? N5 Zn2 Zn1 115.77(12) . . ? N4 Zn2 Zn1 111.03(11) . . ? C2 Zn2 Zn1 143.62(13) . . ? Zn1 O2 Zn2 103.29(16) . . ? C21 N2 C25 117.8(5) . . ? C21 N2 Zn1 119.4(3) . . ? C25 N2 Zn1 122.8(4) . . ? S6 C2 S5 112.0(3) . . ? S6 C2 S4 112.4(3) . . ? S5 C2 S4 110.6(3) . . ? S6 C2 Zn2 103.9(2) . . ? S5 C2 Zn2 109.1(2) . . ? S4 C2 Zn2 108.7(2) . . ? C31 N3 C35 117.1(5) . . ? C21 S2 C1 103.7(2) . . ? O3 Zn3 O3 79.12(15) . 2_766 ? O3 Zn3 N21 111.60(18) . . ? O3 Zn3 N21 91.48(16) 2_766 . ? O3 Zn3 N11 114.84(16) . . ? O3 Zn3 N11 93.09(16) 2_766 . ? N21 Zn3 N11 133.36(17) . . ? O3 Zn3 C3 109.86(17) . . ? O3 Zn3 C3 171.01(16) 2_766 . ? N21 Zn3 C3 84.82(17) . . ? N11 Zn3 C3 83.60(17) . . ? O3 Zn3 Zn3 40.53(10) . 2_766 ? O3 Zn3 Zn3 38.59(10) 2_766 2_766 ? N21 Zn3 Zn3 104.53(12) . 2_766 ? N11 Zn3 Zn3 107.61(12) . 2_766 ? C3 Zn3 Zn3 150.38(13) . 2_766 ? C1 S3 C31 105.9(2) . . ? Zn3 O3 Zn3 100.88(15) . 2_766 ? S31 C3 S21 112.5(3) . . ? S31 C3 S11 111.4(3) . . ? S21 C3 S11 108.5(3) . . ? S31 C3 Zn3 103.3(2) . . ? S21 C3 Zn3 111.1(2) . . ? S11 C3 Zn3 109.9(2) . . ? O4 Zn4 O4 78.69(15) 2_775 . ? O4 Zn4 N42 115.13(18) 2_775 . ? O4 Zn4 N42 92.43(17) . . ? O4 Zn4 N52 118.57(17) 2_775 . ? O4 Zn4 N52 93.19(17) . . ? N42 Zn4 N52 126.07(17) . . ? O4 Zn4 C4 107.29(17) 2_775 . ? O4 Zn4 C4 174.02(17) . . ? N42 Zn4 C4 84.94(17) . . ? N52 Zn4 C4 84.07(18) . . ? O4 Zn4 Zn4 40.35(10) 2_775 2_775 ? O4 Zn4 Zn4 38.33(10) . 2_775 ? N42 Zn4 Zn4 107.25(12) . 2_775 ? N52 Zn4 Zn4 109.83(12) . 2_775 ? C4 Zn4 Zn4 147.65(13) . 2_775 ? Zn4 O4 Zn4 101.31(15) 2_775 . ? C41 S4 C2 103.5(2) . . ? S62 C4 S42 112.5(3) . . ? S62 C4 S52 112.3(3) . . ? S42 C4 S52 109.4(3) . . ? S62 C4 Zn4 103.4(2) . . ? S42 C4 Zn4 109.8(2) . . ? S52 C4 Zn4 109.3(2) . . ? C41 N4 C45 118.0(5) . . ? C41 N4 Zn2 118.2(3) . . ? C45 N4 Zn2 123.6(4) . . ? C51 N5 C55 118.0(5) . . ? C51 N5 Zn2 118.9(3) . . ? C55 N5 Zn2 122.8(4) . . ? C51 S5 C2 103.2(2) . . ? C2 S6 C61 106.4(2) . . ? C61 N6 C65 117.0(4) . . ? C411 S11 C3 102.4(2) . . ? C411 N11 C451 118.9(5) . . ? C411 N11 Zn3 118.9(3) . . ? C451 N11 Zn3 122.3(4) . . ? N1 C11 C12 123.4(5) . . ? N1 C11 S1 120.1(4) . . ? C12 C11 S1 116.5(5) . . ? C13 C12 C11 117.6(6) . . ? C14 C13 C12 119.2(6) . . ? C15 C14 C13 118.7(6) . . ? N1 C15 C14 123.9(6) . . ? C511 S21 C3 103.7(2) . . ? C511 N21 C551 118.4(5) . . ? C511 N21 Zn3 119.0(3) . . ? C551 N21 Zn3 122.2(4) . . ? N2 C21 C22 121.4(5) . . ? N2 C21 S2 121.6(4) . . ? C22 C21 S2 117.0(4) . . ? C23 C22 C21 119.1(5) . . ? C22 C23 C24 119.5(6) . . ? C25 C24 C23 118.5(6) . . ? N2 C25 C24 123.7(5) . . ? C611 S31 C3 106.8(2) . . ? N3 C31 C32 123.8(5) . . ? N3 C31 S3 118.0(4) . . ? C32 C31 S3 118.2(4) . . ? C651 N31 C611 117.3(5) . . ? C33 C32 C31 118.2(6) . . ? C32 C33 C34 120.0(6) . . ? C35 C34 C33 117.2(5) . . ? N3 C35 C34 123.7(5) . . ? N4 C41 C42 121.4(5) . . ? N4 C41 S4 120.0(4) . . ? C42 C41 S4 118.5(4) . . ? C71 S42 C4 104.1(2) . . ? C71 N42 C75 117.9(5) . . ? C71 N42 Zn4 118.9(3) . . ? C75 N42 Zn4 122.8(4) . . ? C43 C42 C41 119.5(6) . . ? C42 C43 C44 118.7(6) . . ? C45 C44 C43 119.4(5) . . ? N4 C45 C44 122.9(5) . . ? N5 C51 C52 122.4(5) . . ? N5 C51 S5 121.2(4) . . ? C52 C51 S5 116.5(4) . . ? C81 S52 C4 102.0(3) . . ? C81 N52 C85 118.5(5) . . ? C81 N52 Zn4 118.5(3) . . ? C85 N52 Zn4 122.9(4) . . ? C53 C52 C51 118.8(5) . . ? C52 C53 C54 119.4(5) . . ? C55 C54 C53 118.5(5) . . ? N5 C55 C54 122.9(5) . . ? N6 C61 C62 123.2(5) . . ? N6 C61 S6 118.3(4) . . ? C62 C61 S6 118.5(4) . . ? C91 S62 C4 107.5(2) . . ? C91 N62 C95 117.7(5) . . ? C63 C62 C61 117.7(5) . . ? C62 C63 C64 120.6(5) . . ? C65 C64 C63 117.0(5) . . ? N6 C65 C64 124.5(5) . . ? N42 C71 C72 121.8(5) . . ? N42 C71 S42 119.9(4) . . ? C72 C71 S42 118.3(4) . . ? C73 C72 C71 119.4(6) . . ? C72 C73 C74 119.8(6) . . ? C75 C74 C73 118.1(6) . . ? N42 C75 C74 122.9(6) . . ? N52 C81 C82 122.0(5) . . ? N52 C81 S52 120.7(4) . . ? C82 C81 S52 117.3(5) . . ? C83 C82 C81 118.7(6) . . ? C82 C83 C84 119.7(6) . . ? C85 C84 C83 119.0(6) . . ? N52 C85 C84 122.1(6) . . ? N62 C91 C92 122.0(5) . . ? N62 C91 S62 120.5(4) . . ? C92 C91 S62 117.5(4) . . ? C93 C92 C91 118.4(5) . . ? C94 C93 C92 119.8(5) . . ? C95 C94 C93 117.6(5) . . ? N62 C95 C94 124.5(5) . . ? C107 C102 C103 117.2(7) . . ? C107 C102 C101 121.4(7) . . ? C103 C102 C101 121.3(7) . . ? C104 C103 C102 122.0(7) . . ? C105 C104 C103 120.4(7) . . ? C104 C105 C106 120.2(8) . . ? C105 C106 C107 119.8(7) . . ? C102 C107 C106 120.4(7) . . ? C113 C112 C117 117.0(10) . . ? C113 C112 C111 123.1(9) . . ? C117 C112 C111 119.9(10) . . ? C114 C113 C112 120.0(9) . . ? C115 C114 C113 119.8(10) . . ? C116 C115 C114 123.6(11) . . ? C115 C116 C117 117.6(10) . . ? C112 C117 C116 120.1(10) . . ? C127 C122 C123 116.8(14) . . ? C127 C122 C121 126.9(17) . . ? C123 C122 C121 116.3(17) . . ? C124 C123 C122 120.0(16) . . ? C125 C124 C123 121.6(16) . . ? C124 C125 C126 121.2(16) . . ? C125 C126 C127 117.3(17) . . ? C122 C127 C126 122.6(18) . . ? N11 C411 C421 122.2(5) . . ? N11 C411 S11 120.0(4) . . ? C421 C411 S11 117.8(4) . . ? C431 C421 C411 119.0(6) . . ? C421 C431 C441 119.2(6) . . ? C451 C441 C431 118.6(5) . . ? N11 C451 C441 122.0(5) . . ? N21 C511 C521 121.6(5) . . ? N21 C511 S21 120.8(4) . . ? C521 C511 S21 117.5(4) . . ? C531 C521 C511 119.0(5) . . ? C521 C531 C541 120.4(6) . . ? C551 C541 C531 117.0(6) . . ? N21 C551 C541 123.5(6) . . ? N31 C611 C621 122.7(5) . . ? N31 C611 S31 119.3(4) . . ? C621 C611 S31 118.0(5) . . ? C631 C621 C611 118.3(6) . . ? C641 C631 C621 119.7(6) . . ? C631 C641 C651 118.9(6) . . ? N31 C651 C641 123.2(6) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 30.62 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.930 _refine_diff_density_min -1.280 _refine_diff_density_rms 0.129 # Attachment '- znos10(carb).cif' data_znos10 _database_code_depnum_ccdc_archive 'CCDC 867647' #TrackingRef '- znos10(carb).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H24 N6 O3 S6 Zn2' _chemical_formula_weight 875.68 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.8656(9) _cell_length_b 28.048(3) _cell_length_c 14.4431(15) _cell_angle_alpha 90.00 _cell_angle_beta 102.816(2) _cell_angle_gamma 90.00 _cell_volume 3501.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5690 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 23.36 _exptl_crystal_description ROD _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 1.773 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.6274 _exptl_absorpt_correction_T_max 0.9487 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48636 _diffrn_reflns_av_R_equivalents 0.1551 _diffrn_reflns_av_sigmaI/netI 0.1215 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8686 _reflns_number_gt 4447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+2.5476P] 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 8686 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1413 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 Zn2 Zn -0.94426(6) -0.203101(19) -0.93885(4) 0.02730(14) Uani 1 1 d . . . Zn1 Zn -0.87081(6) -0.07128(2) -0.74915(4) 0.02990(15) Uani 1 1 d . . . S1 S -0.72737(19) 0.03482(6) -0.71728(12) 0.0609(5) Uani 1 1 d . . . S2 S -0.68415(18) -0.02624(7) -0.55407(11) 0.0665(5) Uani 1 1 d . . . S3 S -1.00026(16) 0.01137(5) -0.63880(10) 0.0411(3) Uani 1 1 d . . . S4 S -1.14130(14) -0.26484(5) -1.10846(9) 0.0423(4) Uani 1 1 d . . . S5 S -1.31395(14) -0.20157(5) -1.00106(9) 0.0403(3) Uani 1 1 d . . . S6 S -1.15239(16) -0.16118(6) -1.13472(10) 0.0568(4) Uani 1 1 d . . . O1 O -0.9275(3) -0.13468(11) -0.8524(2) 0.0326(8) Uani 1 1 d . . . O2 O -0.7044(4) -0.12185(11) -0.7523(2) 0.0329(8) Uani 1 1 d . . . O3 O -0.7431(3) -0.18895(11) -0.8399(2) 0.0284(7) Uani 1 1 d . . . N1 N -0.8196(5) -0.02699(15) -0.8613(3) 0.0369(10) Uani 1 1 d . . . N2 N -0.8657(6) -0.10192(18) -0.5943(3) 0.0504(13) Uani 1 1 d . . . N3 N -1.1047(4) -0.06317(14) -0.7543(3) 0.0307(9) Uani 1 1 d . . . N4 N -0.8878(4) -0.27375(14) -0.9648(3) 0.0308(9) Uani 1 1 d . . . N5 N -1.0972(4) -0.22617(13) -0.8482(3) 0.0305(9) Uani 1 1 d . . . N6 N -0.8527(4) -0.16489(14) -1.0482(3) 0.0325(10) Uani 1 1 d . . . C2 C -1.1460(5) -0.20812(18) -1.0499(3) 0.0333(12) Uani 1 1 d . . . C1 C -0.8196(6) -0.01002(18) -0.6626(4) 0.0403(13) Uani 1 1 d . . . C3 C -0.7887(5) -0.14893(17) -0.8143(3) 0.0255(10) Uani 1 1 d . . . C11 C -0.7512(7) 0.0145(2) -0.8355(4) 0.0503(15) Uani 1 1 d . . . C12 C -0.6961(9) 0.0430(2) -0.8980(5) 0.087(3) Uani 1 1 d . . . H12A H -0.6464 0.0723 -0.8774 0.105 Uiso 1 1 calc R . . C13 C -0.7137(10) 0.0285(3) -0.9909(6) 0.094(3) Uani 1 1 d . . . H13A H -0.6756 0.0476 -1.0350 0.113 Uiso 1 1 calc R . . C14 C -0.7869(9) -0.0139(2) -1.0188(5) 0.075(2) Uani 1 1 d . . . H14A H -0.8015 -0.0245 -1.0826 0.090 Uiso 1 1 calc R . . C15 C -0.8386(7) -0.0407(2) -0.9524(4) 0.0509(15) Uani 1 1 d . . . H15A H -0.8899 -0.0700 -0.9716 0.061 Uiso 1 1 calc R . . C21 C -0.7558(7) -0.0820(2) -0.5284(4) 0.0530(16) Uani 1 1 d . . . C22 C -0.6972(10) -0.1032(3) -0.4401(4) 0.091(3) Uani 1 1 d . . . H22A H -0.6170 -0.0883 -0.3948 0.109 Uiso 1 1 calc R . . C23 C -0.7574(15) -0.1456(4) -0.4204(6) 0.131(5) Uani 1 1 d . . . H23A H -0.7184 -0.1613 -0.3617 0.157 Uiso 1 1 calc R . . C24 C -0.8747(12) -0.1651(3) -0.4866(6) 0.106(4) Uani 1 1 d . . . H24A H -0.9220 -0.1938 -0.4729 0.128 Uiso 1 1 calc R . . C25 C -0.9249(9) -0.1431(2) -0.5730(5) 0.078(2) Uani 1 1 d . . . H25A H -1.0045 -0.1578 -0.6191 0.094 Uiso 1 1 calc R . . C31 C -1.1413(5) -0.02880(16) -0.6996(3) 0.0277(11) Uani 1 1 d . . . C32 C -1.2919(6) -0.02405(18) -0.6865(3) 0.0370(13) Uani 1 1 d . . . H32A H -1.3172 0.0012 -0.6487 0.044 Uiso 1 1 calc R . . C33 C -1.4025(6) -0.0559(2) -0.7284(4) 0.0448(14) Uani 1 1 d . . . H33A H -1.5051 -0.0533 -0.7193 0.054 Uiso 1 1 calc R . . C34 C -1.3642(6) -0.09186(19) -0.7840(4) 0.0441(14) Uani 1 1 d . . . H34A H -1.4394 -0.1144 -0.8139 0.053 Uiso 1 1 calc R . . C35 C -1.2158(6) -0.09428(19) -0.7951(4) 0.0450(14) Uani 1 1 d . . . H35A H -1.1892 -0.1191 -0.8334 0.054 Uiso 1 1 calc R . . C41 C -0.9798(5) -0.29554(18) -1.0396(3) 0.0335(12) Uani 1 1 d . . . C42 C -0.9532(6) -0.34205(19) -1.0661(4) 0.0427(14) Uani 1 1 d . . . H42A H -1.0168 -0.3562 -1.1208 0.051 Uiso 1 1 calc R . . C43 C -0.8337(7) -0.3667(2) -1.0114(4) 0.0537(16) Uani 1 1 d . . . H43A H -0.8142 -0.3987 -1.0269 0.064 Uiso 1 1 calc R . . C44 C -0.7404(7) -0.3449(2) -0.9331(4) 0.0518(15) Uani 1 1 d . . . H44A H -0.6568 -0.3617 -0.8943 0.062 Uiso 1 1 calc R . . C45 C -0.7707(6) -0.29899(18) -0.9127(4) 0.0387(12) Uani 1 1 d . . . H45A H -0.7060 -0.2842 -0.8591 0.046 Uiso 1 1 calc R . . C51 C -1.2474(5) -0.21967(16) -0.8815(3) 0.0322(12) Uani 1 1 d . . . C52 C -1.3573(6) -0.22673(18) -0.8264(4) 0.0386(13) Uani 1 1 d . . . H52A H -1.4643 -0.2214 -0.8518 0.046 Uiso 1 1 calc R . . C53 C -1.3047(7) -0.2416(2) -0.7347(4) 0.0479(15) Uani 1 1 d . . . H53A H -1.3756 -0.2466 -0.6950 0.058 Uiso 1 1 calc R . . C54 C -1.1490(7) -0.2492(2) -0.6998(4) 0.0487(15) Uani 1 1 d . . . H54A H -1.1117 -0.2603 -0.6366 0.058 Uiso 1 1 calc R . . C55 C -1.0497(6) -0.24076(19) -0.7573(3) 0.0402(13) Uani 1 1 d . . . H55A H -0.9421 -0.2453 -0.7324 0.048 Uiso 1 1 calc R . . C61 C -0.9552(6) -0.14700(19) -1.1219(3) 0.0395(13) Uani 1 1 d . . . C62 C -0.9093(7) -0.1167(2) -1.1883(4) 0.0575(17) Uani 1 1 d . . . H62A H -0.9838 -0.1035 -1.2394 0.069 Uiso 1 1 calc R . . C63 C -0.7561(7) -0.1068(2) -1.1781(4) 0.0573(17) Uani 1 1 d . . . H63A H -0.7230 -0.0862 -1.2219 0.069 Uiso 1 1 calc R . . C64 C -0.6497(7) -0.1266(2) -1.1046(4) 0.0518(15) Uani 1 1 d . . . H64A H -0.5422 -0.1210 -1.0981 0.062 Uiso 1 1 calc R . . C65 C -0.7025(6) -0.15478(18) -1.0402(4) 0.0397(13) Uani 1 1 d . . . H65B H -0.6293 -0.1676 -0.9880 0.048 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 Zn2 0.0209(3) 0.0351(3) 0.0247(3) -0.0011(3) 0.0026(2) -0.0016(3) Zn1 0.0290(3) 0.0316(3) 0.0303(3) -0.0053(3) 0.0093(2) -0.0012(3) S1 0.0671(11) 0.0489(10) 0.0779(12) -0.0264(8) 0.0403(10) -0.0299(8) S2 0.0484(9) 0.1063(15) 0.0405(9) -0.0308(9) 0.0002(8) -0.0045(9) S3 0.0483(8) 0.0358(8) 0.0440(8) -0.0140(6) 0.0203(7) -0.0031(6) S4 0.0249(7) 0.0654(10) 0.0340(8) -0.0160(7) 0.0009(6) -0.0023(7) S5 0.0226(6) 0.0559(9) 0.0403(8) -0.0030(7) 0.0022(6) 0.0067(6) S6 0.0397(8) 0.0746(11) 0.0461(9) 0.0258(8) -0.0121(7) -0.0072(8) O1 0.0189(17) 0.0338(19) 0.044(2) -0.0002(16) 0.0056(15) 0.0014(15) O2 0.0360(19) 0.0333(19) 0.0265(18) -0.0044(15) 0.0008(15) -0.0061(16) O3 0.0305(18) 0.0308(19) 0.0229(17) -0.0046(14) 0.0036(14) 0.0006(15) N1 0.043(3) 0.034(3) 0.037(3) 0.001(2) 0.017(2) 0.004(2) N2 0.055(3) 0.054(3) 0.047(3) 0.016(3) 0.022(3) 0.019(3) N3 0.032(2) 0.034(2) 0.027(2) -0.0030(19) 0.0086(18) -0.0004(19) N4 0.022(2) 0.040(3) 0.029(2) -0.0063(19) 0.0034(18) -0.0067(19) N5 0.026(2) 0.035(2) 0.030(2) -0.0042(19) 0.0059(18) -0.0084(18) N6 0.026(2) 0.036(2) 0.036(2) 0.000(2) 0.0092(19) 0.0000(19) C2 0.024(2) 0.048(3) 0.026(3) 0.009(2) 0.002(2) -0.003(2) C1 0.040(3) 0.045(3) 0.037(3) -0.010(3) 0.011(3) -0.008(3) C3 0.028(3) 0.031(3) 0.020(2) 0.000(2) 0.009(2) -0.004(2) C11 0.060(4) 0.040(4) 0.061(4) -0.003(3) 0.036(3) -0.002(3) C12 0.140(7) 0.047(4) 0.103(6) -0.014(4) 0.087(6) -0.027(4) C13 0.149(8) 0.055(5) 0.110(7) 0.025(5) 0.099(6) 0.013(5) C14 0.124(6) 0.064(5) 0.048(4) 0.019(4) 0.043(4) 0.018(5) C15 0.071(4) 0.050(4) 0.037(3) 0.009(3) 0.023(3) 0.015(3) C21 0.053(4) 0.077(5) 0.033(3) 0.002(3) 0.017(3) 0.032(3) C22 0.123(7) 0.114(7) 0.030(4) -0.003(4) 0.005(4) 0.084(6) C23 0.235(13) 0.119(9) 0.051(5) 0.030(6) 0.059(7) 0.135(9) C24 0.192(11) 0.063(6) 0.089(7) 0.041(5) 0.085(7) 0.061(6) C25 0.117(6) 0.054(5) 0.080(5) 0.023(4) 0.057(5) 0.032(4) C31 0.034(3) 0.027(3) 0.025(3) 0.006(2) 0.012(2) 0.001(2) C32 0.047(3) 0.032(3) 0.039(3) 0.005(2) 0.024(3) 0.008(3) C33 0.031(3) 0.053(4) 0.055(4) 0.012(3) 0.019(3) 0.003(3) C34 0.032(3) 0.048(4) 0.054(4) -0.013(3) 0.014(3) -0.009(3) C35 0.044(3) 0.045(3) 0.050(4) -0.012(3) 0.019(3) -0.009(3) C41 0.025(3) 0.046(3) 0.034(3) -0.002(3) 0.015(2) -0.004(2) C42 0.042(3) 0.042(3) 0.048(3) -0.019(3) 0.017(3) -0.011(3) C43 0.062(4) 0.035(3) 0.066(4) -0.010(3) 0.017(4) 0.002(3) C44 0.049(4) 0.044(4) 0.058(4) -0.003(3) 0.003(3) 0.013(3) C45 0.034(3) 0.039(3) 0.040(3) -0.001(3) 0.001(2) 0.002(3) C51 0.026(3) 0.029(3) 0.044(3) -0.009(2) 0.012(2) -0.005(2) C52 0.026(3) 0.044(3) 0.048(3) -0.020(3) 0.013(3) -0.009(2) C53 0.052(4) 0.059(4) 0.042(4) -0.015(3) 0.029(3) -0.014(3) C54 0.054(4) 0.062(4) 0.030(3) 0.006(3) 0.009(3) -0.017(3) C55 0.036(3) 0.052(4) 0.031(3) 0.003(3) 0.004(2) -0.010(3) C61 0.044(3) 0.047(3) 0.026(3) 0.004(2) 0.005(2) 0.000(3) C62 0.069(4) 0.071(4) 0.028(3) 0.015(3) 0.001(3) -0.011(4) C63 0.068(4) 0.067(4) 0.044(4) 0.009(3) 0.029(3) -0.011(4) C64 0.042(3) 0.060(4) 0.058(4) 0.005(3) 0.022(3) -0.003(3) C65 0.031(3) 0.050(3) 0.041(3) -0.002(3) 0.014(2) 0.003(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 Zn2 O3 2.062(3) . ? Zn2 N4 2.098(4) . ? Zn2 C2 2.126(4) . ? Zn2 N5 2.181(4) . ? Zn2 N6 2.207(4) . ? Zn2 O1 2.277(3) . ? Zn2 C3 2.519(5) . ? Zn1 O2 2.054(3) . ? Zn1 N3 2.071(4) . ? Zn1 C1 2.114(5) . ? Zn1 N1 2.167(4) . ? Zn1 O1 2.303(3) . ? Zn1 N2 2.387(4) . ? Zn1 C3 2.542(5) . ? S1 C11 1.767(6) . ? S1 C1 1.778(5) . ? S2 C21 1.759(7) . ? S2 C1 1.808(5) . ? S3 C31 1.766(5) . ? S3 C1 1.813(5) . ? S4 C41 1.774(5) . ? S4 C2 1.806(5) . ? S5 C51 1.771(5) . ? S5 C2 1.793(5) . ? S6 C61 1.762(5) . ? S6 C2 1.790(5) . ? O1 C3 1.295(5) . ? O2 C3 1.281(5) . ? O3 C3 1.275(5) . ? N1 C11 1.327(6) . ? N1 C15 1.345(6) . ? N2 C21 1.325(7) . ? N2 C25 1.334(7) . ? N3 C31 1.331(5) . ? N3 C35 1.350(6) . ? N4 C45 1.341(6) . ? N4 C41 1.347(6) . ? N5 C51 1.324(6) . ? N5 C55 1.351(6) . ? N6 C61 1.334(6) . ? N6 C65 1.342(6) . ? C11 C12 1.373(8) . ? C12 C13 1.378(9) . ? C13 C14 1.371(9) . ? C14 C15 1.374(8) . ? C21 C22 1.398(8) . ? C22 C23 1.358(13) . ? C23 C24 1.361(13) . ? C24 C25 1.374(9) . ? C31 C32 1.396(6) . ? C32 C33 1.365(7) . ? C33 C34 1.378(7) . ? C34 C35 1.362(7) . ? C41 C42 1.394(7) . ? C42 C43 1.361(7) . ? C43 C44 1.387(7) . ? C44 C45 1.361(7) . ? C51 C52 1.403(6) . ? C52 C53 1.368(7) . ? C53 C54 1.377(7) . ? C54 C55 1.359(7) . ? C61 C62 1.408(7) . ? C62 C63 1.362(8) . ? C63 C64 1.372(8) . ? C64 C65 1.379(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 O3 Zn2 N4 95.82(13) . . ? O3 Zn2 C2 171.70(16) . . ? N4 Zn2 C2 89.82(17) . . ? O3 Zn2 N5 101.46(13) . . ? N4 Zn2 N5 91.83(14) . . ? C2 Zn2 N5 84.39(16) . . ? O3 Zn2 N6 90.21(13) . . ? N4 Zn2 N6 100.99(14) . . ? C2 Zn2 N6 82.73(16) . . ? N5 Zn2 N6 161.75(15) . . ? O3 Zn2 O1 61.08(11) . . ? N4 Zn2 O1 154.84(13) . . ? C2 Zn2 O1 114.30(16) . . ? N5 Zn2 O1 83.95(12) . . ? N6 Zn2 O1 89.63(13) . . ? O3 Zn2 C3 30.28(12) . . ? N4 Zn2 C3 125.64(15) . . ? C2 Zn2 C3 144.54(18) . . ? N5 Zn2 C3 93.75(14) . . ? N6 Zn2 C3 89.31(14) . . ? O1 Zn2 C3 30.80(12) . . ? O2 Zn1 N3 142.50(14) . . ? O2 Zn1 C1 120.87(17) . . ? N3 Zn1 C1 90.80(17) . . ? O2 Zn1 N1 96.24(13) . . ? N3 Zn1 N1 106.51(15) . . ? C1 Zn1 N1 85.59(18) . . ? O2 Zn1 O1 60.48(11) . . ? N3 Zn1 O1 89.35(13) . . ? C1 Zn1 O1 176.08(16) . . ? N1 Zn1 O1 90.61(14) . . ? O2 Zn1 N2 84.70(13) . . ? N3 Zn1 N2 83.35(15) . . ? C1 Zn1 N2 77.37(19) . . ? N1 Zn1 N2 160.53(18) . . ? O1 Zn1 N2 106.53(15) . . ? O2 Zn1 C3 30.03(12) . . ? N3 Zn1 C3 116.59(15) . . ? C1 Zn1 C3 150.87(18) . . ? N1 Zn1 C3 95.15(14) . . ? O1 Zn1 C3 30.49(12) . . ? N2 Zn1 C3 95.21(15) . . ? C11 S1 C1 103.5(3) . . ? C21 S2 C1 101.8(3) . . ? C31 S3 C1 104.6(2) . . ? C41 S4 C2 105.3(2) . . ? C51 S5 C2 103.2(2) . . ? C61 S6 C2 102.4(2) . . ? C3 O1 Zn2 85.0(3) . . ? C3 O1 Zn1 85.0(3) . . ? Zn2 O1 Zn1 169.83(15) . . ? C3 O2 Zn1 96.6(3) . . ? C3 O3 Zn2 95.1(3) . . ? C11 N1 C15 118.4(5) . . ? C11 N1 Zn1 116.8(4) . . ? C15 N1 Zn1 124.5(4) . . ? C21 N2 C25 117.6(6) . . ? C21 N2 Zn1 112.3(4) . . ? C25 N2 Zn1 127.0(5) . . ? C31 N3 C35 118.4(4) . . ? C31 N3 Zn1 115.6(3) . . ? C35 N3 Zn1 125.0(3) . . ? C45 N4 C41 117.8(4) . . ? C45 N4 Zn2 125.7(3) . . ? C41 N4 Zn2 116.5(3) . . ? C51 N5 C55 117.8(4) . . ? C51 N5 Zn2 116.8(3) . . ? C55 N5 Zn2 124.9(3) . . ? C61 N6 C65 118.5(4) . . ? C61 N6 Zn2 117.4(3) . . ? C65 N6 Zn2 123.8(3) . . ? S6 C2 S5 106.9(3) . . ? S6 C2 S4 109.1(2) . . ? S5 C2 S4 112.5(3) . . ? S6 C2 Zn2 111.2(2) . . ? S5 C2 Zn2 109.2(2) . . ? S4 C2 Zn2 108.0(2) . . ? S1 C1 S2 106.3(3) . . ? S1 C1 S3 111.3(3) . . ? S2 C1 S3 111.3(3) . . ? S1 C1 Zn1 111.8(2) . . ? S2 C1 Zn1 108.8(3) . . ? S3 C1 Zn1 107.3(2) . . ? O3 C3 O2 123.5(4) . . ? O3 C3 O1 118.8(4) . . ? O2 C3 O1 117.8(4) . . ? O3 C3 Zn2 54.6(2) . . ? O2 C3 Zn2 177.6(3) . . ? O1 C3 Zn2 64.2(2) . . ? O3 C3 Zn1 175.3(3) . . ? O2 C3 Zn1 53.4(2) . . ? O1 C3 Zn1 64.5(2) . . ? Zn2 C3 Zn1 128.64(19) . . ? N1 C11 C12 122.1(6) . . ? N1 C11 S1 120.2(4) . . ? C12 C11 S1 117.6(5) . . ? C11 C12 C13 119.3(6) . . ? C14 C13 C12 119.1(6) . . ? C13 C14 C15 118.5(6) . . ? N1 C15 C14 122.6(6) . . ? N2 C21 C22 122.8(7) . . ? N2 C21 S2 117.8(4) . . ? C22 C21 S2 119.4(6) . . ? C23 C22 C21 118.6(9) . . ? C22 C23 C24 118.6(8) . . ? C23 C24 C25 120.1(9) . . ? N2 C25 C24 122.2(8) . . ? N3 C31 C32 121.1(4) . . ? N3 C31 S3 121.2(3) . . ? C32 C31 S3 117.7(4) . . ? C33 C32 C31 119.5(5) . . ? C32 C33 C34 119.4(5) . . ? C35 C34 C33 118.3(5) . . ? N3 C35 C34 123.2(5) . . ? N4 C41 C42 122.3(5) . . ? N4 C41 S4 120.0(4) . . ? C42 C41 S4 117.7(4) . . ? C43 C42 C41 118.3(5) . . ? C42 C43 C44 119.7(5) . . ? C45 C44 C43 118.9(5) . . ? N4 C45 C44 122.9(5) . . ? N5 C51 C52 123.0(5) . . ? N5 C51 S5 118.9(4) . . ? C52 C51 S5 118.1(4) . . ? C53 C52 C51 117.5(5) . . ? C52 C53 C54 120.0(5) . . ? C55 C54 C53 118.8(5) . . ? N5 C55 C54 122.9(5) . . ? N6 C61 C62 121.5(5) . . ? N6 C61 S6 118.9(4) . . ? C62 C61 S6 119.6(4) . . ? C63 C62 C61 118.8(5) . . ? C62 C63 C64 119.9(5) . . ? C63 C64 C65 118.5(5) . . ? N6 C65 C64 122.8(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.543 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.113