Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_section_title ;3D-, 2D- and 1D-supramolecular structures of {Zn[S2CN(CH2CH2OH)R]2}2 and their {Zn[S2CN(CH2CH2OH)R]2}2(4,4'-bipyridine) adducts for R = CH2CH2OH, Me or Et: polymorphism and pseudo-polymorphism ; _publ_contact_author_name 'Prof. Edward Tiekink' _publ_contact_author_email EDWARD.TIEKINK@UTSA.EDU loop_ _publ_author_name E.R.T.Tiekink R.E.Benson C.A.Ellis C.E.Lewis # Attachment '1.CIF' data_(1) _database_code_depnum_ccdc_archive 'CCDC 645544' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H40 N4 O8 S8 Zn2' _chemical_formula_sum 'C20 H40 N4 O8 S8 Zn2' _chemical_formula_weight 851.90 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 orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 29.620(15) _cell_length_b 8.458(4) _cell_length_c 13.838(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3467(3) _cell_formula_units_Z 4 _cell_measurement_temperature 218(2) _cell_measurement_reflns_used 8323 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 33.4 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 1.912 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.370 _exptl_absorpt_correction_T_max 0.757 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 218(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku SCXmini diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean '4900 0 for SAT' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 1' _diffrn_reflns_number 27068 _diffrn_reflns_av_R_equivalents 0.068 _diffrn_reflns_av_sigmaI/netI 0.037 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.4 _diffrn_reflns_theta_max 27.4 _reflns_number_total 3933 _reflns_number_gt 3541 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; Rigaku (1998). Process-Auto: Automatic Data Acquisition and Processing Package for Imaging Plate and CCD Diffractometers. Rigaku Corporation, 3--9--12 Matsubara-cho, Akishima, Tokyo 196--866, JAPAN ; _computing_cell_refinement ; Rigaku (2006). SCXmini Benchtop Crystallography System software, Version 1.0. Rigaku Americas Corp., 9009 New Trails Drive, The Woodlands, TX 77381--5209, USA ; _computing_data_reduction ; Rigaku (2005). CrystalStructure: Structure Solution and Refinement program, Version 3.7. Rigaku Americas Corp., 9009 New Trails Drive, The Woodlands, TX 77381--5209, USA ; _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material SHELXL97 _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^)+(0.032P)^2^+1.590P] 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 SHELXL _refine_ls_extinction_coef 0.00062(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3933 _refine_ls_number_parameters 203 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.041 _refine_ls_R_factor_gt 0.036 _refine_ls_wR_factor_ref 0.089 _refine_ls_wR_factor_gt 0.086 _refine_ls_goodness_of_fit_ref 1.17 _refine_ls_restrained_S_all 1.17 _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 0.035477(9) 0.09809(3) 0.07902(2) 0.03140(10) Uani 1 1 d . . . S1 S 0.108017(19) 0.06718(7) 0.01257(4) 0.03119(14) Uani 1 1 d . . . S2 S 0.087580(19) 0.17404(7) 0.21158(4) 0.03002(14) Uani 1 1 d . . . S3 S 0.000475(19) -0.14989(7) 0.10995(4) 0.02983(14) Uani 1 1 d . . . S4 S 0.02120(2) -0.29104(8) -0.08262(4) 0.03325(15) Uani 1 1 d . . . O1 O 0.21065(7) -0.0886(2) 0.28481(15) 0.0416(4) Uani 1 1 d D . . H1O H 0.1928 -0.1601 0.2676 0.062 Uiso 1 1 d D . . O2 O 0.25434(6) 0.1845(3) -0.05399(14) 0.0443(5) Uani 1 1 d D . . H2O H 0.2452 0.1602 -0.1096 0.066 Uiso 1 1 d D . . O3 O 0.14923(7) -0.3062(3) 0.21530(16) 0.0527(5) Uani 1 1 d D . . H3O H 0.1551 -0.3224 0.1569 0.079 Uiso 1 1 d D . . O4 O 0.16405(7) -0.3804(3) 0.02836(16) 0.0550(6) Uani 1 1 d D . . H4O H 0.1898 -0.36034 0.0061 0.082 Uiso 1 1 d D . . N1 N 0.17130(6) 0.1308(2) 0.14446(14) 0.0281(4) Uani 1 1 d . . . N2 N 0.06380(6) -0.3725(2) 0.07923(15) 0.0285(4) Uani 1 1 d . . . C1 C 0.12713(7) 0.1246(3) 0.12527(16) 0.0256(4) Uani 1 1 d . . . C2 C 0.18836(8) 0.1805(3) 0.23966(18) 0.0357(5) Uani 1 1 d . . . H2A H 0.1708 0.2713 0.2623 0.043 Uiso 1 1 calc R . . H2B H 0.2198 0.2145 0.2331 0.043 Uiso 1 1 calc R . . C3 C 0.18565(9) 0.0492(3) 0.31430(19) 0.0396(6) Uani 1 1 d . . . H3A H 0.1976 0.0877 0.3760 0.048 Uiso 1 1 calc R . . H3B H 0.1540 0.0201 0.3243 0.048 Uiso 1 1 calc R . . C4 C 0.20548(8) 0.0860(3) 0.07251(18) 0.0304(5) Uani 1 1 d . . . H4A H 0.1935 0.0017 0.0312 0.036 Uiso 1 1 calc R . . H4B H 0.2323 0.0450 0.1056 0.036 Uiso 1 1 calc R . . C5 C 0.21869(9) 0.2263(3) 0.0104(2) 0.0392(6) Uani 1 1 d . . . H5A H 0.1925 0.2620 -0.0268 0.047 Uiso 1 1 calc R . . H5B H 0.2285 0.3137 0.0520 0.047 Uiso 1 1 calc R . . C6 C 0.03275(7) -0.2794(3) 0.03910(17) 0.0269(4) Uani 1 1 d . . . C7 C 0.06972(8) -0.3817(3) 0.18579(19) 0.0338(5) Uani 1 1 d . . . H7A H 0.0403 -0.3648 0.2164 0.041 Uiso 1 1 calc R . . H7B H 0.0797 -0.4888 0.2024 0.041 Uiso 1 1 calc R . . C8 C 0.10301(9) -0.2649(3) 0.2281(2) 0.0402(6) Uani 1 1 d . . . H8A H 0.0978 -0.1613 0.1985 0.048 Uiso 1 1 calc R . . H8B H 0.0970 -0.2545 0.2975 0.048 Uiso 1 1 calc R . . C9 C 0.08925(8) -0.4865(3) 0.0187(2) 0.0338(5) Uani 1 1 d . . . H9A H 0.0683 -0.5357 -0.0272 0.041 Uiso 1 1 calc R . . H9B H 0.1012 -0.5703 0.0604 0.041 Uiso 1 1 calc R . . C10 C 0.12811(9) -0.4137(3) -0.0373(2) 0.0391(6) Uani 1 1 d . . . H10A H 0.1385 -0.4872 -0.0873 0.047 Uiso 1 1 calc R . . H10B H 0.1182 -0.3160 -0.0688 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 0.02328(15) 0.03054(17) 0.04039(18) -0.00046(11) 0.00038(11) 0.00108(10) S1 0.0258(3) 0.0427(3) 0.0251(3) -0.0041(2) -0.0003(2) -0.0006(2) S2 0.0285(3) 0.0334(3) 0.0281(3) -0.0036(2) 0.0033(2) 0.0021(2) S3 0.0259(3) 0.0315(3) 0.0321(3) 0.0025(2) 0.0055(2) 0.0010(2) S4 0.0313(3) 0.0378(3) 0.0306(3) -0.0019(2) -0.0004(2) 0.0070(2) O1 0.0372(10) 0.0504(12) 0.0371(11) -0.0008(9) -0.0099(8) 0.0005(8) O2 0.0231(8) 0.0781(14) 0.0318(10) -0.0008(10) 0.0016(7) -0.0084(9) O3 0.0367(11) 0.0757(15) 0.0457(12) -0.0169(11) -0.0053(9) -0.0020(10) O4 0.0285(10) 0.0945(18) 0.0420(12) -0.0093(11) 0.0024(8) -0.0037(10) N1 0.0239(9) 0.0360(10) 0.0243(9) -0.0026(8) 0.0010(7) -0.0012(8) N2 0.0249(9) 0.0265(9) 0.0340(11) 0.0026(8) 0.0017(7) -0.0011(7) C1 0.0266(11) 0.0224(10) 0.0277(12) 0.0028(8) 0.0001(8) -0.0004(8) C2 0.0318(12) 0.0463(14) 0.0289(13) -0.0062(11) -0.0024(9) -0.0040(10) C3 0.0389(14) 0.0547(16) 0.0252(12) -0.0031(11) -0.0042(10) -0.0004(12) C4 0.0236(11) 0.0389(13) 0.0286(12) -0.0012(10) 0.0003(8) 0.0031(9) C5 0.0336(13) 0.0438(15) 0.0401(14) 0.0002(12) 0.0068(10) -0.0070(11) C6 0.0210(10) 0.0261(11) 0.0334(12) 0.0033(9) 0.0025(8) -0.0042(8) C7 0.0338(12) 0.0330(12) 0.0347(13) 0.0094(10) -0.0003(10) 0.0026(9) C8 0.0414(14) 0.0411(14) 0.0381(14) -0.0027(11) -0.0046(11) 0.0031(11) C9 0.0306(12) 0.0278(12) 0.0431(14) 0.0009(10) 0.0014(10) 0.0053(9) C10 0.0291(12) 0.0510(16) 0.0372(14) -0.0026(12) 0.0024(10) 0.0045(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn S4 2.3419(11) 5 ? Zn S1 2.3517(12) . ? Zn S3 2.3786(12) . ? Zn S2 2.4818(11) . ? Zn S3 2.8573(14) 5 ? S1 C1 1.729(2) . ? S2 C1 1.724(2) . ? S3 C6 1.754(2) . ? S3 Zn 2.8573(14) 5 ? S4 C6 1.722(3) . ? S4 Zn 2.3419(11) 5 ? O1 C3 1.439(3) . ? O1 H1O 0.839 . ? O2 C5 1.426(3) . ? O2 H2O 0.841 . ? O3 C8 1.424(3) . ? O3 H3O 0.838 . ? O4 C10 1.427(3) . ? O4 H4O 0.838 . ? N1 C1 1.336(3) . ? N1 C2 1.472(3) . ? N1 C4 1.470(3) . ? N2 C6 1.332(3) . ? N2 C9 1.483(3) . ? N2 C7 1.487(3) . ? C2 C3 1.519(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.517(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C7 C8 1.514(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.518(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? 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 S4 Zn S1 137.80(3) 5 . ? S4 Zn S3 107.35(4) 5 . ? S1 Zn S3 111.75(3) . . ? S4 Zn S2 104.46(3) 5 . ? S1 Zn S2 75.50(4) . . ? S3 Zn S2 111.49(3) . . ? S4 Zn S3 69.23(2) 5 5 ? S1 Zn S3 89.98(4) . 5 ? S3 Zn S3 97.90(2) . 5 ? S2 Zn S3 150.29(3) . 5 ? C1 S1 Zn 85.13(8) . . ? C1 S2 Zn 81.24(9) . . ? C6 S3 Zn 102.28(8) . . ? C6 S3 Zn 77.72(9) . 5 ? Zn S3 Zn 82.10(2) . 5 ? C6 S4 Zn 94.69(8) . 5 ? C3 O1 H1O 110 . . ? C5 O2 H2O 113 . . ? C8 O3 H3O 111 . . ? C10 O4 H4O 119 . . ? C1 N1 C2 121.68(19) . . ? C1 N1 C4 122.0(2) . . ? C2 N1 C4 116.32(19) . . ? C6 N2 C9 120.0(2) . . ? C6 N2 C7 121.7(2) . . ? C9 N2 C7 117.78(19) . . ? N1 C1 S1 120.72(17) . . ? N1 C1 S2 121.20(18) . . ? S1 C1 S2 118.07(13) . . ? N1 C2 C3 112.4(2) . . ? N1 C2 H2A 109.1 . . ? C3 C2 H2A 109.1 . . ? N1 C2 H2B 109.1 . . ? C3 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? O1 C3 C2 111.8(2) . . ? O1 C3 H3A 109.2 . . ? C2 C3 H3A 109.2 . . ? O1 C3 H3B 109.2 . . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N1 C4 C5 111.0(2) . . ? N1 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? N1 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? O2 C5 C4 110.5(2) . . ? O2 C5 H5A 109.5 . . ? C4 C5 H5A 109.5 . . ? O2 C5 H5B 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? N2 C6 S4 120.75(18) . . ? N2 C6 S3 120.84(19) . . ? S4 C6 S3 118.31(13) . . ? C8 C7 N2 115.2(2) . . ? C8 C7 H7A 108.5 . . ? N2 C7 H7A 108.5 . . ? C8 C7 H7B 108.5 . . ? N2 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? O3 C8 C7 114.7(2) . . ? O3 C8 H8A 108.6 . . ? C7 C8 H8A 108.6 . . ? O3 C8 H8B 108.6 . . ? C7 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? N2 C9 C10 114.2(2) . . ? N2 C9 H9A 108.7 . . ? C10 C9 H9A 108.7 . . ? N2 C9 H9B 108.7 . . ? C10 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? O4 C10 C9 108.7(2) . . ? O4 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? O4 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.4 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.37 _refine_diff_density_min -0.34 _refine_diff_density_rms 0.071 # Attachment '2.CIF' data_(2) _database_code_depnum_ccdc_archive 'CCDC 645545' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H40 N4 O4 S8 Zn2' _chemical_formula_sum 'C20 H40 N4 O4 S8 Zn2' _chemical_formula_weight 787.80 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 P21/n _symmetry_space_group_name_Hall '-P 2yn ' 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 8.3821(15) _cell_length_b 11.6432(18) _cell_length_c 16.978(4) _cell_angle_alpha 90 _cell_angle_beta 102.926(5) _cell_angle_gamma 90 _cell_volume 1615.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4308 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 30.4 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 2.036 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.767 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type AFC12\K/SATURN724 _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 1' _diffrn_reflns_number 13420 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_av_sigmaI/netI 0.019 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.0 _diffrn_reflns_theta_max 27.5 _reflns_number_total 3664 _reflns_number_gt 3546 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear (Rigaku, 2005)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976) & DIAMOND (Crystal Impact, 2006)' _computing_publication_material SHELXL97 _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. In the refinement, the CH2CH2OH and ethyl groups were fractionally interchanged with the major component having a site occupancy factor = 0.57(1); the atoms of the minor component was refined isotropically and the O-H atom was not included. This accounts for the discrepancy between the refined and real molecular formulae, and the non-sensible intra- and inter-molecular separations. ; _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^)+(0.056P)^2^+3.865P] 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 3664 _refine_ls_number_parameters 203 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.049 _refine_ls_R_factor_gt 0.048 _refine_ls_wR_factor_ref 0.123 _refine_ls_wR_factor_gt 0.123 _refine_ls_goodness_of_fit_ref 1.08 _refine_ls_restrained_S_all 1.08 _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 0.02482(5) 0.38648(3) 0.07967(2) 0.03104(14) Uani 1 1 d . . . S1 S -0.21695(11) 0.35513(7) 0.12452(6) 0.0360(2) Uani 1 1 d . . . S2 S 0.04837(11) 0.18704(8) 0.13074(6) 0.0379(2) Uani 1 1 d . . . S3 S -0.00366(9) 0.37262(7) -0.06278(5) 0.02890(19) Uani 1 1 d . . . S4 S -0.27856(10) 0.52961(7) -0.13217(6) 0.0348(2) Uani 1 1 d . . . O1 O -0.3689(8) -0.0669(5) 0.0392(4) 0.120(2) Uani 1 1 d D . . H1O H -0.3863 -0.1362 0.0262 0.181 Uiso 1 1 d D . . N1 N -0.2487(4) 0.1302(3) 0.1501(2) 0.0401(7) Uani 1 1 d . . . C1 C -0.1491(4) 0.2138(3) 0.1376(2) 0.0324(7) Uani 1 1 d . . . C2 C -0.1935(6) 0.0103(3) 0.1613(3) 0.0462(9) Uani 1 1 d . . . H2A H -0.2588 -0.0303 0.1946 0.055 Uiso 1 1 calc R . . H2B H -0.0774 0.0087 0.1909 0.055 Uiso 1 1 calc R . . C3 C -0.2102(7) -0.0518(4) 0.0820(3) 0.0575(12) Uani 1 1 d . . . H3A H -0.1496 -0.0083 0.0479 0.069 Uiso 1 1 calc R . . H3B H -0.1578 -0.1281 0.0926 0.069 Uiso 1 1 calc R . . C4 C -0.4256(5) 0.1505(4) 0.1495(3) 0.0480(10) Uani 1 1 d . . . H4A H -0.4913 0.0844 0.1238 0.058 Uiso 1 1 calc R . . H4B H -0.4641 0.2199 0.1171 0.058 Uiso 1 1 calc R . . C5 C -0.4506(6) 0.1662(5) 0.2336(3) 0.0642(13) Uani 1 1 d . . . H5A H -0.5672 0.1781 0.2315 0.096 Uiso 1 1 calc R . . H5B H -0.3883 0.2332 0.2585 0.096 Uiso 1 1 calc R . . H5C H -0.4125 0.0976 0.2657 0.096 Uiso 1 1 calc R . . C6 C -0.2132(4) 0.3932(3) -0.10032(19) 0.0266(6) Uani 1 1 d . . . N2 N -0.324(2) 0.3049(16) -0.1096(12) 0.022(3) Uani 0.569(10) 1 d P A 1 C7 C -0.500(3) 0.325(2) -0.1400(16) 0.030(5) Uani 0.569(10) 1 d P A 1 H7A H -0.5156 0.3747 -0.1881 0.036 Uiso 0.569(10) 1 calc PR A 1 H7B H -0.5529 0.2499 -0.1578 0.036 Uiso 0.569(10) 1 calc PR A 1 C8 C -0.5849(11) 0.3753(9) -0.0841(7) 0.035(2) Uani 0.569(10) 1 d P A 1 H8A H -0.5335 0.4497 -0.0649 0.042 Uiso 0.569(10) 1 calc PR A 1 H8B H -0.7004 0.3899 -0.1114 0.042 Uiso 0.569(10) 1 calc PR A 1 O2 O -0.5789(2) 0.3018(5) -0.0183(3) 0.0504(17) Uani 0.569(10) 1 d PD A 1 H2O H -0.6784 0.2972 -0.0171 0.076 Uiso 0.57 1 d PD A 1 C9 C -0.2790(13) 0.1897(10) -0.0883(7) 0.036(3) Uani 0.569(10) 1 d P A 1 H9A H -0.3627 0.1552 -0.0627 0.043 Uiso 0.569(10) 1 calc PR A 1 H9B H -0.1737 0.1895 -0.0479 0.043 Uiso 0.569(10) 1 calc PR A 1 C10 C -0.2623(13) 0.1178(8) -0.1576(7) 0.044(3) Uani 0.569(10) 1 d P A 1 H10A H -0.2315 0.0396 -0.1389 0.067 Uiso 0.569(10) 1 calc PR A 1 H10B H -0.1775 0.1502 -0.1825 0.067 Uiso 0.569(10) 1 calc PR A 1 H10C H -0.3668 0.1159 -0.1975 0.067 Uiso 0.569(10) 1 calc PR A 1 N2A N -0.310(3) 0.312(2) -0.1018(17) 0.028(6) Uiso 0.431(10) 1 d P A 2 C7A C -0.485(4) 0.326(3) -0.141(2) 0.037(8) Uiso 0.431(10) 1 d P A 2 H7C H -0.5293 0.2545 -0.1687 0.044 Uiso 0.431(10) 1 calc PR A 2 H7D H -0.5003 0.3895 -0.1807 0.044 Uiso 0.431(10) 1 calc PR A 2 C8A C -0.575(2) 0.3559(14) -0.0665(9) 0.037(4) Uiso 0.431(10) 1 d P A 2 H8C H -0.6926 0.3664 -0.0882 0.055 Uiso 0.431(10) 1 calc PR A 2 H8D H -0.5284 0.4265 -0.0394 0.055 Uiso 0.431(10) 1 calc PR A 2 H8E H -0.5577 0.2924 -0.0276 0.055 Uiso 0.431(10) 1 calc PR A 2 C9A C -0.2554(16) 0.1892(13) -0.0736(8) 0.019(3) Uiso 0.431(10) 1 d P A 2 H9C H -0.1552 0.1931 -0.0298 0.022 Uiso 0.431(10) 1 calc PR A 2 H9D H -0.3423 0.1521 -0.0515 0.022 Uiso 0.431(10) 1 calc PR A 2 C10A C -0.2213(19) 0.1166(16) -0.1430(10) 0.043(4) Uiso 0.431(10) 1 d P A 2 H10D H -0.1491 0.1595 -0.1715 0.052 Uiso 0.431(10) 1 calc PR A 2 H10E H -0.1648 0.0448 -0.1214 0.052 Uiso 0.431(10) 1 calc PR A 2 O3A O -0.3754(12) 0.0893(8) -0.1992(6) 0.070(3) Uiso 0.431(10) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0298(2) 0.0302(2) 0.0344(2) 0.00251(15) 0.00987(16) -0.00556(14) S1 0.0395(5) 0.0273(4) 0.0466(5) 0.0032(4) 0.0213(4) 0.0007(3) S2 0.0363(5) 0.0274(4) 0.0512(5) 0.0085(4) 0.0124(4) 0.0015(3) S3 0.0235(4) 0.0320(4) 0.0330(4) 0.0007(3) 0.0102(3) -0.0006(3) S4 0.0293(4) 0.0281(4) 0.0436(5) 0.0072(3) 0.0011(3) -0.0027(3) O1 0.118(4) 0.093(4) 0.130(5) -0.025(4) -0.014(4) -0.002(4) N1 0.0432(18) 0.0329(16) 0.0460(18) 0.0078(13) 0.0138(14) -0.0054(13) C1 0.0380(18) 0.0296(16) 0.0302(16) 0.0038(13) 0.0090(13) -0.0055(13) C2 0.055(2) 0.0301(18) 0.053(2) 0.0120(16) 0.0098(19) -0.0070(16) C3 0.074(3) 0.035(2) 0.056(3) -0.0011(19) -0.003(2) -0.014(2) C4 0.044(2) 0.055(2) 0.043(2) 0.0054(19) 0.0043(17) -0.0171(19) C5 0.056(3) 0.085(4) 0.054(3) -0.004(3) 0.018(2) -0.009(3) C6 0.0279(15) 0.0269(15) 0.0260(15) 0.0000(11) 0.0079(12) -0.0018(12) N2 0.020(5) 0.021(4) 0.023(5) -0.005(3) 0.000(3) -0.007(3) C7 0.014(5) 0.035(7) 0.039(7) 0.001(2) 0.001(4) -0.010(4) C8 0.022(4) 0.040(5) 0.041(5) 0.009(4) 0.005(3) 0.006(3) O2 0.055(3) 0.050(3) 0.047(3) -0.001(2) 0.014(2) -0.005(2) C9 0.023(4) 0.030(4) 0.044(6) 0.006(4) -0.015(3) -0.005(3) C10 0.031(5) 0.026(4) 0.071(7) -0.017(4) -0.002(5) 0.002(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 Zn S4 2.3290(10) 3_565 ? Zn S1 2.3475(10) . ? Zn S3 2.3821(10) . ? Zn S2 2.4711(10) . ? Zn S3 2.8210(10) 3_565 ? S1 C1 1.740(4) . ? S2 C1 1.714(4) . ? S3 C6 1.746(3) . ? S3 Zn 2.8210(10) 3_565 ? S4 C6 1.727(3) . ? S4 Zn 2.3290(10) 3_565 ? O1 C3 1.377(8) . ? O1 H1O 0.8401 . ? N1 C1 1.329(4) . ? N1 C2 1.470(5) . ? N1 C4 1.499(5) . ? C2 C3 1.507(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.500(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N2A 1.24(3) . ? C6 N2 1.370(17) . ? N2 C9 1.42(2) . ? N2 C7 1.47(3) . ? C7 C8 1.43(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O2 1.399(12) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? O2 H2O 0.8401 . ? C9 C10 1.476(17) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N2A C7A 1.48(4) . ? N2A C9A 1.55(3) . ? C7A C8A 1.65(4) . ? C7A H7C 0.9900 . ? C7A H7D 0.9900 . ? C8A H2O 1.4982 . ? C8A H8C 0.9800 . ? C8A H8D 0.9800 . ? C8A H8E 0.9800 . ? C9A C10A 1.53(2) . ? C9A H9C 0.9900 . ? C9A H9D 0.9900 . ? C10A O3A 1.459(16) . ? C10A H10D 0.9900 . ? C10A H10E 0.9900 . ? 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 S4 Zn S1 136.20(4) 3_565 . ? S4 Zn S3 107.01(3) 3_565 . ? S1 Zn S3 114.91(4) . . ? S4 Zn S2 105.39(3) 3_565 . ? S1 Zn S2 75.35(3) . . ? S3 Zn S2 105.94(3) . . ? S4 Zn S3 69.70(3) 3_565 3_565 ? S1 Zn S3 98.53(3) . 3_565 ? S3 Zn S3 88.53(3) . 3_565 ? S2 Zn S3 165.52(3) . 3_565 ? C1 S1 Zn 84.68(12) . . ? C1 S2 Zn 81.42(12) . . ? C6 S3 Zn 103.04(11) . . ? C6 S3 Zn 77.93(11) . 3_565 ? Zn S3 Zn 91.47(3) . 3_565 ? C6 S4 Zn 93.85(11) . 3_565 ? C3 O1 H1O 111 . . ? C1 N1 C2 121.7(3) . . ? C1 N1 C4 122.6(3) . . ? C2 N1 C4 115.7(3) . . ? N1 C1 S2 121.9(3) . . ? N1 C1 S1 120.9(3) . . ? S2 C1 S1 117.14(19) . . ? N1 C2 C3 112.1(4) . . ? N1 C2 H2A 109.2 . . ? C3 C2 H2A 109.2 . . ? N1 C2 H2B 109.2 . . ? C3 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? O1 C3 C2 114.7(5) . . ? O1 C3 H3A 108.6 . . ? C2 C3 H3A 108.6 . . ? O1 C3 H3B 108.6 . . ? C2 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? N1 C4 C5 111.2(4) . . ? N1 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? N1 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2A C6 N2 5(2) . . ? N2A C6 S4 122.2(14) . . ? N2 C6 S4 119.7(8) . . ? N2A C6 S3 120.1(14) . . ? N2 C6 S3 122.5(8) . . ? S4 C6 S3 117.63(18) . . ? C6 N2 C9 123.2(14) . . ? C6 N2 C7 121.6(16) . . ? C9 N2 C7 115.1(16) . . ? C8 C7 N2 116.1(19) . . ? C8 C7 H7A 108.3 . . ? N2 C7 H7A 108.3 . . ? C8 C7 H7B 108.3 . . ? N2 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? O2 C8 C7 110.0(13) . . ? O2 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? O2 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C8 O2 H2O 101.5 . . ? N2 C9 C10 113.6(12) . . ? N2 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? N2 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 N2A C7A 120(3) . . ? C6 N2A C9A 124(2) . . ? C7A N2A C9A 116(2) . . ? N2A C7A C8A 105(3) . . ? N2A C7A H7C 110.7 . . ? C8A C7A H7C 110.7 . . ? N2A C7A H7D 110.7 . . ? C8A C7A H7D 110.7 . . ? H7C C7A H7D 108.8 . . ? C7A C8A H2O 139.0 . . ? C7A C8A H8C 109.5 . . ? H2O C8A H8C 67.0 . . ? C7A C8A H8D 109.5 . . ? H2O C8A H8D 109.8 . . ? H8C C8A H8D 109.5 . . ? C7A C8A H8E 109.5 . . ? H2O C8A H8E 45.3 . . ? H8C C8A H8E 109.5 . . ? H8D C8A H8E 109.5 . . ? C10A C9A N2A 111.5(15) . . ? C10A C9A H9C 109.3 . . ? N2A C9A H9C 109.3 . . ? C10A C9A H9D 109.3 . . ? N2A C9A H9D 109.3 . . ? H9C C9A H9D 108.0 . . ? O3A C10A C9A 109.5(12) . . ? O3A C10A H10D 109.8 . . ? C9A C10A H10D 109.8 . . ? O3A C10A H10E 109.8 . . ? C9A C10A H10E 109.8 . . ? H10D C10A H10E 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S4 Zn S1 C1 -104.31(12) 3_565 . . . ? S3 Zn S1 C1 93.84(12) . . . . ? S2 Zn S1 C1 -7.20(12) . . . . ? S3 Zn S1 C1 -173.81(12) 3_565 . . . ? S4 Zn S2 C1 141.94(12) 3_565 . . . ? S1 Zn S2 C1 7.37(12) . . . . ? S3 Zn S2 C1 -104.84(12) . . . . ? S3 Zn S2 C1 73.83(18) 3_565 . . . ? S4 Zn S3 C6 -146.19(11) 3_565 . . . ? S1 Zn S3 C6 20.78(12) . . . . ? S2 Zn S3 C6 101.72(11) . . . . ? S3 Zn S3 C6 -77.95(11) 3_565 . . . ? S4 Zn S3 Zn -68.24(3) 3_565 . . 3_565 ? S1 Zn S3 Zn 98.73(3) . . . 3_565 ? S2 Zn S3 Zn 179.67(3) . . . 3_565 ? S3 Zn S3 Zn 0.0 3_565 . . 3_565 ? C2 N1 C1 S2 2.0(5) . . . . ? C4 N1 C1 S2 -174.8(3) . . . . ? C2 N1 C1 S1 180.0(3) . . . . ? C4 N1 C1 S1 3.2(5) . . . . ? Zn S2 C1 N1 167.3(3) . . . . ? Zn S2 C1 S1 -10.84(17) . . . . ? Zn S1 C1 N1 -166.8(3) . . . . ? Zn S1 C1 S2 11.34(18) . . . . ? C1 N1 C2 C3 -86.1(5) . . . . ? C4 N1 C2 C3 90.8(4) . . . . ? N1 C2 C3 O1 -65.9(6) . . . . ? C1 N1 C4 C5 -96.9(5) . . . . ? C2 N1 C4 C5 86.1(5) . . . . ? Zn S4 C6 N2A 168.6(16) 3_565 . . . ? Zn S4 C6 N2 174.1(10) 3_565 . . . ? Zn S4 C6 S3 -9.75(18) 3_565 . . . ? Zn S3 C6 N2A -81.5(15) . . . . ? Zn S3 C6 N2A -170.2(15) 3_565 . . . ? Zn S3 C6 N2 -87.1(10) . . . . ? Zn S3 C6 N2 -175.8(10) 3_565 . . . ? Zn S3 C6 S4 96.90(18) . . . . ? Zn S3 C6 S4 8.20(16) 3_565 . . . ? N2A C6 N2 C9 -63(24) . . . . ? S4 C6 N2 C9 177.2(12) . . . . ? S3 C6 N2 C9 1(2) . . . . ? N2A C6 N2 C7 114(25) . . . . ? S4 C6 N2 C7 -5(2) . . . . ? S3 C6 N2 C7 178.8(16) . . . . ? C6 N2 C7 C8 -75(3) . . . . ? C9 N2 C7 C8 103(2) . . . . ? N2 C7 C8 O2 -63(2) . . . . ? C6 N2 C9 C10 -98.7(16) . . . . ? C7 N2 C9 C10 84(2) . . . . ? N2 C6 N2A C7A -56(23) . . . . ? S4 C6 N2A C7A 8(3) . . . . ? S3 C6 N2A C7A -174(2) . . . . ? N2 C6 N2A C9A 117(25) . . . . ? S4 C6 N2A C9A -179.8(14) . . . . ? S3 C6 N2A C9A -1(3) . . . . ? C6 N2A C7A C8A -97(3) . . . . ? C9A N2A C7A C8A 90(3) . . . . ? C6 N2A C9A C10A -90(2) . . . . ? C7A N2A C9A C10A 83(3) . . . . ? N2A C9A C10A O3A -71.4(18) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.98 _refine_diff_density_min -0.72 _refine_diff_density_rms 0.097 # Attachment '3.CIF' data_(3) _database_code_depnum_ccdc_archive 'CCDC 645546' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H36 N4 O5 S8 Zn2' _chemical_formula_sum 'C17 H36 N4 O5 S8 Zn2' _chemical_formula_weight 763.84 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' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.470(4) _cell_length_b 12.345(6) _cell_length_c 12.615(6) _cell_angle_alpha 95.483(13) _cell_angle_beta 96.282(10) _cell_angle_gamma 100.576(11) _cell_volume 1581.9(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1913 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 30.3 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 2.078 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.858 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type AFC12\K/SATURN724 _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 1' _diffrn_reflns_number 14760 _diffrn_reflns_av_R_equivalents 0.068 _diffrn_reflns_av_sigmaI/netI 0.079 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.4 _diffrn_reflns_theta_max 26.0 _reflns_number_total 5958 _reflns_number_gt 4784 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear (Rigaku, 2005)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976) & DIAMOND (Crystal Impact, 2006)' _computing_publication_material SHELXL97 _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^)+(0.0523P)^2^+2.0169P] 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 5958 _refine_ls_number_parameters 345 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.087 _refine_ls_R_factor_gt 0.069 _refine_ls_wR_factor_ref 0.163 _refine_ls_wR_factor_gt 0.151 _refine_ls_goodness_of_fit_ref 1.14 _refine_ls_restrained_S_all 1.14 _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 0.35523(6) 0.23931(5) 0.16925(6) 0.0348(2) Uani 1 1 d . . . Zn2 Zn 0.05705(6) 0.22218(5) 0.31258(5) 0.0346(2) Uani 1 1 d . . . S1 S 0.51902(14) 0.32022(13) 0.31220(12) 0.0362(4) Uani 1 1 d . . . S2 S 0.54505(15) 0.30554(13) 0.08091(12) 0.0382(4) Uani 1 1 d . . . S3 S 0.25619(14) 0.06027(12) 0.09065(12) 0.0350(4) Uani 1 1 d . . . S4 S 0.22417(14) 0.11504(12) 0.32017(11) 0.0335(3) Uani 1 1 d . . . S5 S -0.13853(15) 0.14338(13) 0.20048(12) 0.0364(4) Uani 1 1 d . . . S6 S -0.09608(15) 0.15841(14) 0.43712(12) 0.0408(4) Uani 1 1 d . . . S7 S 0.15449(15) 0.40724(12) 0.37281(12) 0.0383(4) Uani 1 1 d . . . S8 S 0.18168(14) 0.33838(12) 0.14596(12) 0.0325(3) Uani 1 1 d . . . O1 O 0.8862(5) 0.6232(4) 0.1855(4) 0.0522(12) Uani 1 1 d D . . H1O H 0.8352 0.6541 0.2193 0.078 Uiso 1 1 d D . . O2 O 0.1265(4) -0.2889(3) 0.1500(4) 0.0441(11) Uani 1 1 d D . . H2O H 0.0531 -0.3193 0.1649 0.066 Uiso 1 1 d D . . O3 O -0.4389(4) -0.1656(4) 0.2295(4) 0.0526(12) Uani 1 1 d D . . H3O H -0.5037 -0.1643 0.2630 0.079 Uiso 1 1 d D . . O4 O 0.3275(4) 0.7700(4) 0.3068(4) 0.0463(11) Uani 1 1 d D . . H4O H 0.2641 0.7634 0.2581 0.069 Uiso 1 1 d D . . O5 O 0.7180(5) 0.7058(4) 0.2985(4) 0.0502(11) Uani 1 1 d D . . H5O H 0.6828 0.7422 0.2548 0.075 Uiso 1 1 d D . . N1 N 0.7387(4) 0.4017(4) 0.2364(4) 0.0344(11) Uani 1 1 d . . . N2 N 0.0819(4) -0.0604(4) 0.1911(4) 0.0317(11) Uani 1 1 d . . . N3 N -0.3240(5) 0.0647(4) 0.3176(4) 0.0370(11) Uani 1 1 d . . . N4 N 0.3227(4) 0.5216(4) 0.2626(4) 0.0331(11) Uani 1 1 d . . . C1 C 0.6161(5) 0.3491(4) 0.2117(5) 0.0314(12) Uani 1 1 d . . . C2 C 0.8251(6) 0.4216(5) 0.1533(5) 0.0382(14) Uani 1 1 d . . . H2A H 0.7982 0.3606 0.0937 0.046 Uiso 1 1 calc R . . H2B H 0.9159 0.4203 0.1839 0.046 Uiso 1 1 calc R . . C3 C 0.8226(7) 0.5299(5) 0.1097(5) 0.0443(16) Uani 1 1 d . . . H3A H 0.8665 0.5312 0.0441 0.053 Uiso 1 1 calc R . . H3B H 0.7305 0.5361 0.0893 0.053 Uiso 1 1 calc R . . C4 C 0.7960(6) 0.4380(5) 0.3477(5) 0.0443(15) Uani 1 1 d . . . H4A H 0.7403 0.4818 0.3832 0.066 Uiso 1 1 calc R . . H4B H 0.8835 0.4836 0.3495 0.066 Uiso 1 1 calc R . . H4C H 0.8029 0.3730 0.3853 0.066 Uiso 1 1 calc R . . C5 C 0.1764(5) 0.0281(4) 0.1986(4) 0.0273(12) Uani 1 1 d . . . C6 C 0.0362(6) -0.1327(5) 0.0891(5) 0.0359(13) Uani 1 1 d . . . H6A H 0.0364 -0.0858 0.0297 0.043 Uiso 1 1 calc R . . H6B H -0.0554 -0.1706 0.0904 0.043 Uiso 1 1 calc R . . C7 C 0.1169(6) -0.2191(5) 0.0658(5) 0.0397(14) Uani 1 1 d . . . H7A H 0.0771 -0.2658 -0.0022 0.048 Uiso 1 1 calc R . . H7B H 0.2060 -0.1816 0.0557 0.048 Uiso 1 1 calc R . . C8 C 0.0172(6) -0.0939(5) 0.2846(5) 0.0456(16) Uani 1 1 d . . . H8A H 0.0735 -0.1319 0.3290 0.068 Uiso 1 1 calc R . . H8B H -0.0669 -0.1441 0.2595 0.068 Uiso 1 1 calc R . . H8C H 0.0022 -0.0278 0.3272 0.068 Uiso 1 1 calc R . . C9 C -0.2010(5) 0.1157(4) 0.3186(5) 0.0314(12) Uani 1 1 d . . . C10 C -0.4160(6) 0.0347(5) 0.2198(5) 0.0380(14) Uani 1 1 d . . . H10A H -0.3951 0.0911 0.1703 0.046 Uiso 1 1 calc R . . H10B H -0.5054 0.0362 0.2378 0.046 Uiso 1 1 calc R . . C11 C -0.4149(7) -0.0782(5) 0.1628(6) 0.0492(17) Uani 1 1 d . . . H11A H -0.4826 -0.0939 0.0991 0.059 Uiso 1 1 calc R . . H11B H -0.3287 -0.0771 0.1371 0.059 Uiso 1 1 calc R . . C12 C -0.3784(7) 0.0418(6) 0.4180(5) 0.0508(18) Uani 1 1 d . . . H12A H -0.3080 0.0612 0.4786 0.076 Uiso 1 1 calc R . . H12B H -0.4177 -0.0372 0.4133 0.076 Uiso 1 1 calc R . . H12C H -0.4454 0.0863 0.4289 0.076 Uiso 1 1 calc R . . C13 C 0.2308(5) 0.4338(4) 0.2606(5) 0.0302(12) Uani 1 1 d . . . C14 C 0.3765(6) 0.5962(5) 0.3636(5) 0.0401(15) Uani 1 1 d . . . H14A H 0.4704 0.6263 0.3613 0.048 Uiso 1 1 calc R . . H14B H 0.3704 0.5521 0.4250 0.048 Uiso 1 1 calc R . . C15 C 0.3078(7) 0.6908(5) 0.3824(5) 0.0434(15) Uani 1 1 d . . . H15A H 0.2127 0.6611 0.3788 0.052 Uiso 1 1 calc R . . H15B H 0.3392 0.7291 0.4557 0.052 Uiso 1 1 calc R . . C16 C 0.3850(6) 0.5510(5) 0.1672(5) 0.0380(14) Uani 1 1 d . . . H16A H 0.4025 0.4840 0.1281 0.057 Uiso 1 1 calc R . . H16B H 0.4676 0.6041 0.1898 0.057 Uiso 1 1 calc R . . H16C H 0.3262 0.5846 0.1204 0.057 Uiso 1 1 calc R . . C17 C 0.7625(7) 0.7520(7) 0.4065(6) 0.061(2) Uani 1 1 d . . . H17A H 0.7889 0.8327 0.4097 0.091 Uiso 1 1 calc R . . H17B H 0.8377 0.7210 0.4337 0.091 Uiso 1 1 calc R . . H17C H 0.6917 0.7341 0.4506 0.091 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 0.0280(4) 0.0325(4) 0.0410(4) -0.0008(3) 0.0039(3) 0.0014(3) Zn2 0.0296(4) 0.0334(4) 0.0380(4) -0.0008(3) 0.0060(3) 0.0009(3) S1 0.0299(8) 0.0424(9) 0.0352(8) 0.0058(7) 0.0055(6) 0.0025(6) S2 0.0357(8) 0.0388(9) 0.0365(8) -0.0013(7) 0.0073(6) -0.0009(6) S3 0.0361(8) 0.0338(8) 0.0329(8) -0.0001(6) 0.0097(6) -0.0001(6) S4 0.0337(8) 0.0329(8) 0.0320(8) 0.0009(6) 0.0034(6) 0.0034(6) S5 0.0340(8) 0.0382(8) 0.0335(8) 0.0050(6) 0.0021(6) -0.0007(6) S6 0.0364(8) 0.0471(9) 0.0355(8) 0.0010(7) 0.0072(7) 0.0001(7) S7 0.0415(9) 0.0323(8) 0.0391(8) 0.0001(7) 0.0110(7) 0.0008(6) S8 0.0307(8) 0.0304(8) 0.0331(8) 0.0018(6) -0.0001(6) 0.0009(6) O1 0.048(3) 0.037(3) 0.068(3) -0.001(2) 0.022(2) -0.004(2) O2 0.035(2) 0.034(2) 0.066(3) 0.014(2) 0.009(2) 0.0082(19) O3 0.044(3) 0.040(3) 0.076(4) 0.016(2) 0.011(2) 0.007(2) O4 0.042(3) 0.036(2) 0.058(3) 0.004(2) 0.004(2) 0.000(2) O5 0.050(3) 0.051(3) 0.048(3) -0.001(2) -0.003(2) 0.015(2) N1 0.030(3) 0.033(3) 0.039(3) 0.003(2) 0.006(2) 0.003(2) N2 0.028(3) 0.031(3) 0.036(3) 0.002(2) 0.009(2) 0.004(2) N3 0.030(3) 0.035(3) 0.044(3) 0.004(2) 0.006(2) 0.000(2) N4 0.028(3) 0.029(3) 0.040(3) 0.001(2) 0.009(2) -0.0010(19) C1 0.032(3) 0.024(3) 0.040(3) 0.006(2) 0.008(2) 0.009(2) C2 0.031(3) 0.039(3) 0.044(4) 0.006(3) 0.010(3) 0.004(3) C3 0.053(4) 0.042(4) 0.034(3) 0.005(3) 0.011(3) -0.004(3) C4 0.037(4) 0.047(4) 0.045(4) 0.008(3) 0.000(3) 0.000(3) C5 0.023(3) 0.028(3) 0.030(3) 0.001(2) 0.003(2) 0.007(2) C6 0.035(3) 0.033(3) 0.035(3) 0.001(3) 0.002(3) 0.001(2) C7 0.038(3) 0.033(3) 0.042(3) -0.005(3) 0.000(3) 0.001(3) C8 0.044(4) 0.040(4) 0.052(4) 0.002(3) 0.020(3) 0.000(3) C9 0.031(3) 0.024(3) 0.040(3) 0.001(2) 0.007(2) 0.004(2) C10 0.028(3) 0.031(3) 0.053(4) 0.006(3) 0.002(3) 0.002(2) C11 0.043(4) 0.043(4) 0.057(4) 0.001(3) 0.009(3) -0.003(3) C12 0.044(4) 0.054(4) 0.051(4) -0.002(3) 0.020(3) -0.002(3) C13 0.022(3) 0.029(3) 0.038(3) 0.002(2) 0.000(2) 0.005(2) C14 0.038(3) 0.034(3) 0.041(4) -0.006(3) -0.002(3) -0.004(3) C15 0.049(4) 0.031(3) 0.048(4) 0.002(3) 0.006(3) 0.002(3) C16 0.043(4) 0.029(3) 0.038(3) -0.001(3) 0.014(3) -0.005(3) C17 0.059(5) 0.077(5) 0.041(4) 0.013(4) -0.002(3) 0.004(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 S3 2.3364(18) . ? Zn1 S1 2.3538(18) . ? Zn1 S8 2.3772(18) . ? Zn1 S2 2.4336(17) . ? Zn1 S4 2.8668(18) . ? Zn2 S7 2.3411(19) . ? Zn2 S5 2.3476(18) . ? Zn2 S4 2.3784(18) . ? Zn2 S6 2.4460(17) . ? Zn2 S8 2.9441(18) . ? S1 C1 1.733(6) . ? S2 C1 1.727(6) . ? S3 C5 1.715(5) . ? S4 C5 1.753(5) . ? S5 C9 1.731(6) . ? S6 C9 1.731(6) . ? S7 C13 1.729(6) . ? S8 C13 1.742(6) . ? O1 C3 1.432(8) . ? O1 H1O 0.8400 . ? O2 C7 1.436(8) . ? O2 H2O 0.8400 . ? O3 C11 1.434(8) . ? O3 H3O 0.8400 . ? O4 C15 1.434(8) . ? O4 H4O 0.8400 . ? O5 C17 1.418(8) . ? O5 H5O 0.8400 . ? N1 C1 1.317(7) . ? N1 C2 1.467(7) . ? N1 C4 1.459(8) . ? N2 C5 1.322(7) . ? N2 C6 1.473(7) . ? N2 C8 1.477(7) . ? N3 C9 1.324(7) . ? N3 C10 1.452(8) . ? N3 C12 1.475(7) . ? N4 C13 1.308(7) . ? N4 C14 1.489(7) . ? N4 C16 1.473(7) . ? C2 C3 1.497(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C6 C7 1.504(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 C11 1.508(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C14 C15 1.493(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? 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 S3 Zn1 S1 137.00(7) . . ? S3 Zn1 S8 102.57(6) . . ? S1 Zn1 S8 113.65(6) . . ? S3 Zn1 S2 109.20(6) . . ? S1 Zn1 S2 76.10(6) . . ? S8 Zn1 S2 115.18(6) . . ? S3 Zn1 S4 68.99(5) . . ? S1 Zn1 S4 87.63(6) . . ? S8 Zn1 S4 90.65(6) . . ? S2 Zn1 S4 153.27(6) . . ? S7 Zn2 S5 131.44(7) . . ? S7 Zn2 S4 108.11(7) . . ? S5 Zn2 S4 116.53(6) . . ? S7 Zn2 S6 107.78(6) . . ? S5 Zn2 S6 76.00(6) . . ? S4 Zn2 S6 108.32(6) . . ? S7 Zn2 S8 67.15(5) . . ? S5 Zn2 S8 94.93(6) . . ? S4 Zn2 S8 88.77(5) . . ? S6 Zn2 S8 162.81(6) . . ? C1 S1 Zn1 84.5(2) . . ? C1 S2 Zn1 82.24(19) . . ? C5 S3 Zn1 94.18(19) . . ? C5 S4 Zn2 100.16(18) . . ? C5 S4 Zn1 76.74(18) . . ? Zn2 S4 Zn1 91.05(6) . . ? C9 S5 Zn2 85.0(2) . . ? C9 S6 Zn2 81.95(19) . . ? C13 S7 Zn2 96.65(19) . . ? C13 S8 Zn1 97.32(19) . . ? C13 S8 Zn2 77.08(19) . . ? Zn1 S8 Zn2 89.21(5) . . ? C3 O1 H1O 115 . . ? C7 O2 H2O 113 . . ? C11 O3 H3O 114 . . ? C15 O4 H4O 114 . . ? C17 O5 H5O 121 . . ? C1 N1 C2 121.2(5) . . ? C1 N1 C4 121.5(5) . . ? C2 N1 C4 117.2(5) . . ? C5 N2 C6 121.8(5) . . ? C5 N2 C8 122.1(5) . . ? C6 N2 C8 116.0(4) . . ? C9 N3 C10 122.8(5) . . ? C9 N3 C12 121.3(5) . . ? C10 N3 C12 115.7(5) . . ? C13 N4 C14 121.8(5) . . ? C13 N4 C16 122.9(5) . . ? C14 N4 C16 115.2(4) . . ? N1 C1 S2 122.7(4) . . ? N1 C1 S1 120.2(5) . . ? S2 C1 S1 117.1(3) . . ? N1 C2 C3 113.0(5) . . ? N1 C2 H2A 109.0 . . ? C3 C2 H2A 109.0 . . ? N1 C2 H2B 109.0 . . ? C3 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? O1 C3 C2 112.5(5) . . ? O1 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? O1 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 S3 121.1(4) . . ? N2 C5 S4 120.5(4) . . ? S3 C5 S4 118.4(3) . . ? N2 C6 C7 114.5(5) . . ? N2 C6 H6A 108.6 . . ? C7 C6 H6A 108.6 . . ? N2 C6 H6B 108.6 . . ? C7 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? O2 C7 C6 112.7(5) . . ? O2 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? O2 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 S5 121.0(5) . . ? N3 C9 S6 121.9(4) . . ? S5 C9 S6 117.1(3) . . ? N3 C10 C11 113.7(5) . . ? N3 C10 H10A 108.8 . . ? C11 C10 H10A 108.8 . . ? N3 C10 H10B 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? O3 C11 C10 113.2(5) . . ? O3 C11 H11A 108.9 . . ? C10 C11 H11A 108.9 . . ? O3 C11 H11B 108.9 . . ? C10 C11 H11B 108.9 . . ? H11A C11 H11B 107.8 . . ? N3 C12 H12A 109.5 . . ? N3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 S8 121.5(4) . . ? N4 C13 S7 121.0(4) . . ? S8 C13 S7 117.4(3) . . ? N4 C14 C15 113.8(5) . . ? N4 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? N4 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? O4 C15 C14 113.5(5) . . ? O4 C15 H15A 108.9 . . ? C14 C15 H15A 108.9 . . ? O4 C15 H15B 108.9 . . ? C14 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? N4 C16 H16A 109.5 . . ? N4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O5 C17 H17A 109.5 . . ? O5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 26.0 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.59 _refine_diff_density_min -0.74 _refine_diff_density_rms 0.113 # Attachment '4.CIF' data_(4) _database_code_depnum_ccdc_archive 'CCDC 645547' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H48 N6 O8 S8 Zn2' _chemical_formula_sum 'C30 H48 N6 O8 S8 Zn2' _chemical_formula_weight 1007.96 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.249(4) _cell_length_b 13.214(5) _cell_length_c 15.581(6) _cell_angle_alpha 105.335(3) _cell_angle_beta 105.092(4) _cell_angle_gamma 93.881(5) _cell_volume 2133.2(14) _cell_formula_units_Z 2 _cell_measurement_temperature 218(2) _cell_measurement_reflns_used 5817 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 33.2 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.77 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 1.568 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.875 _exptl_absorpt_correction_T_min 0.549 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 218(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku SCXmini diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 4900 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_reflns_number 22125 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_av_sigmaI/netI 0.065 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.4 _diffrn_reflns_theta_max 27.5 _reflns_number_total 9714 _reflns_number_gt 7416 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; Rigaku (1998). Process-Auto: Automatic Data Acquisition and Processing Package for Imaging Plate and CCD Diffractometers. Rigaku Corporation, 3--9--12 Matsubara-cho, Akishima, Tokyo 196--866, JAPAN ; _computing_cell_refinement ; Rigaku (2006). SCXmini Benchtop Crystallography System software, Version 1.0. Rigaku Americas Corp., 9009 New Trails Drive, The Woodlands, TX 77381--5209, USA ; _computing_data_reduction ; Rigaku (2005). CrystalStructure: Structure Solution and Refinement program, Version 3.7. Rigaku Americas Corp., 9009 New Trails Drive, The Woodlands, TX 77381--5209, USA ; _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material SHELXL97 _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. In the refinement, the -CH2OH group with the O4 atom was disordered over two positions with the major component having a site occupancy factor of 0.64(1); the atoms of the minor component was refined isotropically and the O-H atom was not included. This accounts for the discrepancy in the refined and actual molecular formulae. The CH2CH2 atoms of the CH2CH2OH group with the O7 atom were also disordered over two positions. The major component has a site occupancy factor of 0.79(1) and the atoms of the minor component were refined isotropically. ; _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^)+(0.041P)^2^+1.287P] 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 9714 _refine_ls_number_parameters 526 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.070 _refine_ls_R_factor_gt 0.050 _refine_ls_wR_factor_ref 0.118 _refine_ls_wR_factor_gt 0.106 _refine_ls_goodness_of_fit_ref 1.06 _refine_ls_restrained_S_all 1.06 _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 0.39561(4) 0.22351(3) 0.05622(3) 0.03272(11) Uani 1 1 d . . . Zn2 Zn 0.62672(3) -0.25557(3) -0.57902(3) 0.03034(11) Uani 1 1 d . . . S1 S 0.47576(8) 0.40575(7) 0.10215(6) 0.03287(19) Uani 1 1 d . . . S2 S 0.61538(8) 0.24470(7) 0.16626(6) 0.0351(2) Uani 1 1 d . . . S3 S 0.27501(8) 0.12172(7) 0.11690(6) 0.0372(2) Uani 1 1 d . . . S4 S 0.16237(8) 0.23559(7) -0.01657(6) 0.0342(2) Uani 1 1 d . . . S5 S 0.75054(8) -0.15056(7) -0.63718(6) 0.0369(2) Uani 1 1 d . . . S6 S 0.85464(8) -0.25056(8) -0.49156(6) 0.0370(2) Uani 1 1 d . . . S7 S 0.53631(8) -0.43540(7) -0.60508(6) 0.03342(19) Uani 1 1 d . B . S8 S 0.42695(9) -0.28824(7) -0.70610(7) 0.0439(2) Uani 1 1 d . B . O1 O 0.8379(3) 0.5416(2) 0.1075(2) 0.0488(7) Uani 1 1 d D . . H1O H 0.8305 0.4768 0.0795 0.073 Uiso 1 1 d D . . O2 O 0.9218(3) 0.3868(3) 0.4137(2) 0.0631(9) Uani 1 1 d D . . H2O H 0.9883 0.4148 0.4090 0.095 Uiso 1 1 d D . . O3 O -0.1795(3) 0.3295(3) 0.0042(2) 0.0597(8) Uani 1 1 d D A . H3O H -0.1384 0.3376 -0.0320 0.089 Uiso 1 1 d D . . O5 O 1.0940(3) -0.3501(2) -0.5769(2) 0.0548(8) Uani 1 1 d D . . H5O H 1.0910 -0.3608 -0.5266 0.082 Uiso 1 1 d D . . O6 O 1.1096(4) -0.1609(3) -0.7417(2) 0.0764(10) Uani 1 1 d D . . H6O H 1.1017 -0.2134 -0.7881 0.115 Uiso 1 1 d D . . O8 O 0.1332(3) -0.5574(2) -0.6468(2) 0.0552(7) Uani 1 1 d D . . H8O H 0.1370 -0.4911 -0.6299 0.083 Uiso 1 1 d D . . N1 N 0.7091(2) 0.4509(2) 0.21525(17) 0.0283(6) Uani 1 1 d . . . N2 N 0.0313(3) 0.1369(2) 0.0666(2) 0.0364(7) Uani 1 1 d . . . N3 N 0.9949(3) -0.1412(2) -0.5632(2) 0.0343(6) Uani 1 1 d . . . N5 N 0.4329(3) 0.1403(2) -0.06513(19) 0.0323(6) Uani 1 1 d . . . N6 N 0.5798(2) -0.1633(2) -0.46472(19) 0.0315(6) Uani 1 1 d . . . C1 C 0.6113(3) 0.3755(2) 0.1673(2) 0.0259(6) Uani 1 1 d . . . C2 C 0.7082(3) 0.5628(3) 0.2134(2) 0.0343(8) Uani 1 1 d . . . H2A H 0.7744 0.6085 0.2667 0.041 Uiso 1 1 calc R . . H2B H 0.6286 0.5844 0.2198 0.041 Uiso 1 1 calc R . . C3 C 0.7269(4) 0.5790(3) 0.1246(3) 0.0415(9) Uani 1 1 d . . . H3A H 0.6549 0.5411 0.0720 0.050 Uiso 1 1 calc R . . H3B H 0.7320 0.6546 0.1291 0.050 Uiso 1 1 calc R . . C4 C 0.8240(3) 0.4262(3) 0.2714(2) 0.0332(7) Uani 1 1 d . . . H4A H 0.8950 0.4739 0.2720 0.040 Uiso 1 1 calc R . . H4B H 0.8348 0.3534 0.2422 0.040 Uiso 1 1 calc R . . C5 C 0.8241(3) 0.4372(3) 0.3710(2) 0.0389(8) Uani 1 1 d . . . H5A H 0.8364 0.5124 0.4060 0.047 Uiso 1 1 calc R . . H5B H 0.7437 0.4042 0.3717 0.047 Uiso 1 1 calc R . . C6 C 0.1436(3) 0.1619(2) 0.0564(2) 0.0292(7) Uani 1 1 d . A . C7 C -0.0795(3) 0.1718(3) 0.0152(3) 0.0443(9) Uani 1 1 d . A . H7A H -0.1539 0.1245 0.0096 0.053 Uiso 1 1 calc R . . H7B H -0.0745 0.1665 -0.0476 0.053 Uiso 1 1 calc R . . C8 C -0.0924(4) 0.2868(4) 0.0633(3) 0.0587(12) Uani 1 1 d . . . H8A H -0.1186 0.2885 0.1189 0.070 Uiso 1 1 calc R A . H8B H -0.0110 0.3311 0.0834 0.070 Uiso 1 1 calc R . . C9 C 0.0161(4) 0.0757(3) 0.1312(3) 0.0512(11) Uani 0.637(11) 1 d P A 1 H9A H 0.0674 0.0187 0.1246 0.061 Uiso 0.637(11) 1 calc PR A 1 H9B H -0.0709 0.0422 0.1115 0.061 Uiso 0.637(11) 1 calc PR A 1 C10 C 0.0495(9) 0.1373(6) 0.2339(5) 0.053(2) Uani 0.637(11) 1 d P A 1 H10A H 0.0787 0.0914 0.2727 0.063 Uiso 0.637(11) 1 calc PR A 1 H10B H 0.1150 0.1974 0.2492 0.063 Uiso 0.637(11) 1 calc PR A 1 O4 O -0.0605(6) 0.1727(6) 0.2478(2) 0.102(3) Uani 0.637(11) 1 d PD A 1 H4O H -0.0298 0.2107 0.3031 0.153 Uiso 0.64 1 d PD A 1 C39 C 0.0161(4) 0.0757(3) 0.1312(3) 0.0512(11) Uani 0.363(11) 1 d P A 2 H39A H 0.0921 0.0460 0.1522 0.061 Uiso 0.363(11) 1 calc PR A 2 H39B H -0.0533 0.0174 0.1005 0.061 Uiso 0.363(11) 1 calc PR A 2 C40 C -0.0113(18) 0.1574(15) 0.2168(14) 0.067(5) Uiso 0.363(11) 1 d P A 2 H40A H 0.0594 0.2144 0.2483 0.081 Uiso 0.363(11) 1 calc PR A 2 H40B H -0.0855 0.1891 0.1951 0.081 Uiso 0.363(11) 1 calc PR A 2 O44 O -0.0296(9) 0.1034(8) 0.2756(6) 0.064(4) Uiso 0.363(11) 1 d P A 2 C11 C 0.8804(3) -0.1771(2) -0.5635(2) 0.0296(7) Uani 1 1 d . . . C12 C 1.1082(3) -0.1599(3) -0.4996(3) 0.0445(9) Uani 1 1 d . . . H12A H 1.0863 -0.1763 -0.4474 0.053 Uiso 1 1 calc R . . H12B H 1.1680 -0.0944 -0.4744 0.053 Uiso 1 1 calc R . . C13 C 1.1707(4) -0.2496(4) -0.5449(3) 0.0546(11) Uani 1 1 d . . . H13A H 1.1921 -0.2338 -0.5976 0.065 Uiso 1 1 calc R . . H13B H 1.2483 -0.2530 -0.4998 0.065 Uiso 1 1 calc R . . C14 C 1.0109(4) -0.0797(3) -0.6276(3) 0.0438(9) Uani 1 1 d . . . H14A H 1.0939 -0.0376 -0.6027 0.053 Uiso 1 1 calc R . . H14B H 0.9499 -0.0302 -0.6292 0.053 Uiso 1 1 calc R . . C15 C 0.9959(4) -0.1469(4) -0.7269(3) 0.0586(12) Uani 1 1 d . . . H15A H 0.9477 -0.2163 -0.7384 0.070 Uiso 1 1 calc R . . H15B H 0.9498 -0.1121 -0.7706 0.070 Uiso 1 1 calc R . . C16 C 0.4147(3) -0.4110(3) -0.6877(2) 0.0291(7) Uani 1 1 d . . . O7 O 0.0712(2) -0.3748(2) -0.8762(2) 0.0561(8) Uani 0.790(10) 1 d PD B 1 H7O H -0.0045 -0.4004 -0.8937 0.084 Uiso 0.790(10) 1 d PD B 1 N4 N 0.3175(3) -0.4858(2) -0.7373(2) 0.0366(7) Uani 0.790(10) 1 d P B 1 C17 C 0.2329(4) -0.4739(3) -0.8236(3) 0.0291(12) Uani 0.790(10) 1 d P B 1 H17A H 0.2784 -0.4312 -0.8507 0.035 Uiso 0.790(10) 1 calc PR B 1 H17B H 0.2009 -0.5438 -0.8691 0.035 Uiso 0.790(10) 1 calc PR B 1 C18 C 0.1255(5) -0.4201(4) -0.8002(3) 0.0368(13) Uani 0.790(10) 1 d P B 1 H18A H 0.1554 -0.3639 -0.7408 0.044 Uiso 0.790(10) 1 calc PR B 1 H18B H 0.0628 -0.4717 -0.7951 0.044 Uiso 0.790(10) 1 calc PR B 1 O57 O 0.0712(2) -0.3748(2) -0.8762(2) 0.0561(8) Uani 0.210(10) 1 d P B 2 H17O H -0.0045 -0.4004 -0.8937 0.084 Uiso 0.210(10) 1 d P B 2 N54 N 0.3175(3) -0.4858(2) -0.7373(2) 0.0366(7) Uani 0.210(10) 1 d P B 2 C57 C 0.1808(18) -0.4437(15) -0.7727(13) 0.035(5) Uiso 0.210(10) 1 d P B 2 H57C H 0.1806 -0.3717 -0.7346 0.042 Uiso 0.210(10) 1 calc PR B 2 H57D H 0.1118 -0.4913 -0.7703 0.042 Uiso 0.210(10) 1 calc PR B 2 C58 C 0.1726(18) -0.4461(15) -0.8679(13) 0.042(6) Uiso 0.210(10) 1 d P B 2 H58C H 0.2503 -0.4149 -0.8741 0.050 Uiso 0.210(10) 1 calc PR B 2 H58D H 0.1452 -0.5176 -0.9116 0.050 Uiso 0.210(10) 1 calc PR B 2 C19 C 0.3018(3) -0.5890(3) -0.7183(2) 0.0361(8) Uani 1 1 d . . . H19A H 0.3818 -0.6160 -0.7091 0.043 Uiso 1 1 calc R B 1 H19B H 0.2424 -0.6396 -0.7730 0.043 Uiso 1 1 calc R B 1 C20 C 0.2564(3) -0.5842(3) -0.6342(3) 0.0390(8) Uani 1 1 d . B . H20A H 0.2575 -0.6532 -0.6219 0.047 Uiso 1 1 calc R . . H20B H 0.3133 -0.5312 -0.5798 0.047 Uiso 1 1 calc R . . C21 C 0.5405(3) 0.1667(3) -0.0821(2) 0.0358(8) Uani 1 1 d . . . H21 H 0.5969 0.2253 -0.0396 0.043 Uiso 1 1 calc R . . C22 C 0.5708(3) 0.1103(3) -0.1601(2) 0.0336(7) Uani 1 1 d . . . H22 H 0.6465 0.1314 -0.1698 0.040 Uiso 1 1 calc R . . C23 C 0.4900(3) 0.0228(2) -0.2239(2) 0.0278(7) Uani 1 1 d . . . C24 C 0.3777(3) -0.0032(3) -0.2070(2) 0.0322(7) Uani 1 1 d . . . H24 H 0.3192 -0.0607 -0.2490 0.039 Uiso 1 1 calc R . . C25 C 0.3531(3) 0.0566(3) -0.1274(2) 0.0361(8) Uani 1 1 d . . . H25 H 0.2774 0.0379 -0.1165 0.043 Uiso 1 1 calc R . . C26 C 0.5212(3) -0.0411(2) -0.3081(2) 0.0278(7) Uani 1 1 d . . . C27 C 0.5951(4) 0.0037(3) -0.3510(3) 0.0423(9) Uani 1 1 d . . . H27 H 0.6274 0.0763 -0.3276 0.051 Uiso 1 1 calc R . . C28 C 0.6212(3) -0.0589(3) -0.4287(3) 0.0407(9) Uani 1 1 d . . . H28 H 0.6702 -0.0268 -0.4575 0.049 Uiso 1 1 calc R . . C29 C 0.5104(3) -0.2075(3) -0.4220(2) 0.0376(8) Uani 1 1 d . . . H29 H 0.4818 -0.2808 -0.4456 0.045 Uiso 1 1 calc R . . C30 C 0.4792(3) -0.1499(3) -0.3448(2) 0.0373(8) Uani 1 1 d . . . H30 H 0.4300 -0.1839 -0.3173 0.045 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 0.0327(2) 0.0319(2) 0.0309(2) 0.00214(17) 0.01360(17) -0.00184(17) Zn2 0.0276(2) 0.0297(2) 0.0302(2) 0.00167(16) 0.01079(16) -0.00055(16) S1 0.0284(4) 0.0306(4) 0.0351(4) 0.0085(4) 0.0028(3) 0.0034(3) S2 0.0367(5) 0.0309(4) 0.0377(5) 0.0136(4) 0.0075(4) 0.0035(4) S3 0.0350(5) 0.0385(5) 0.0410(5) 0.0176(4) 0.0107(4) 0.0028(4) S4 0.0305(4) 0.0395(5) 0.0349(5) 0.0138(4) 0.0104(4) 0.0040(4) S5 0.0333(5) 0.0415(5) 0.0387(5) 0.0170(4) 0.0104(4) 0.0032(4) S6 0.0288(4) 0.0445(5) 0.0421(5) 0.0196(4) 0.0110(4) 0.0046(4) S7 0.0264(4) 0.0319(4) 0.0375(5) 0.0093(4) 0.0026(3) 0.0046(4) S8 0.0401(5) 0.0329(5) 0.0504(6) 0.0182(4) -0.0045(4) -0.0042(4) O1 0.0496(16) 0.0448(15) 0.0581(18) 0.0155(14) 0.0272(14) 0.0006(14) O2 0.0382(16) 0.108(3) 0.0607(19) 0.052(2) 0.0129(15) 0.0270(18) O3 0.0413(17) 0.0564(18) 0.081(2) 0.0082(17) 0.0281(16) 0.0135(15) O5 0.065(2) 0.0566(18) 0.0496(17) 0.0148(15) 0.0257(16) 0.0224(16) O6 0.074(2) 0.078(2) 0.071(2) -0.0076(19) 0.043(2) -0.004(2) O8 0.0359(15) 0.0534(17) 0.079(2) 0.0216(17) 0.0187(15) 0.0085(15) N1 0.0266(14) 0.0328(15) 0.0243(13) 0.0085(12) 0.0056(11) 0.0034(12) N2 0.0339(16) 0.0364(16) 0.0360(16) 0.0006(13) 0.0175(13) -0.0041(13) N3 0.0326(15) 0.0322(15) 0.0355(16) 0.0031(13) 0.0141(13) -0.0020(13) N5 0.0329(15) 0.0315(15) 0.0303(14) 0.0030(12) 0.0124(12) 0.0016(12) N6 0.0267(14) 0.0331(15) 0.0319(15) 0.0030(12) 0.0108(12) 0.0030(12) C1 0.0268(16) 0.0300(16) 0.0215(15) 0.0060(13) 0.0101(12) 0.0016(13) C2 0.0340(18) 0.0288(17) 0.0342(18) 0.0046(15) 0.0058(15) -0.0008(15) C3 0.044(2) 0.039(2) 0.045(2) 0.0205(18) 0.0108(17) 0.0017(17) C4 0.0269(17) 0.042(2) 0.0292(17) 0.0083(15) 0.0078(14) 0.0038(15) C5 0.0316(18) 0.053(2) 0.0312(18) 0.0134(17) 0.0047(15) 0.0148(17) C6 0.0308(17) 0.0238(15) 0.0295(16) 0.0005(13) 0.0114(14) -0.0002(13) C7 0.0249(18) 0.049(2) 0.054(2) 0.0029(19) 0.0158(17) 0.0010(17) C8 0.053(3) 0.058(3) 0.059(3) -0.003(2) 0.023(2) 0.019(2) C9 0.059(3) 0.046(2) 0.044(2) 0.0010(19) 0.027(2) -0.021(2) C10 0.059(5) 0.054(4) 0.035(4) -0.003(3) 0.018(3) -0.014(4) O4 0.123(6) 0.127(6) 0.067(4) 0.016(4) 0.046(4) 0.073(5) C39 0.059(3) 0.046(2) 0.044(2) 0.0010(19) 0.027(2) -0.021(2) C11 0.0293(17) 0.0263(16) 0.0300(17) 0.0004(13) 0.0125(14) -0.0004(13) C12 0.0290(19) 0.050(2) 0.043(2) -0.0016(18) 0.0107(16) -0.0071(17) C13 0.033(2) 0.073(3) 0.052(2) 0.005(2) 0.0157(19) 0.010(2) C14 0.046(2) 0.039(2) 0.044(2) 0.0033(17) 0.0224(18) -0.0113(17) C15 0.057(3) 0.068(3) 0.046(2) 0.001(2) 0.026(2) -0.006(2) C16 0.0274(16) 0.0294(17) 0.0260(16) 0.0048(13) 0.0037(13) 0.0022(14) O7 0.0333(14) 0.0584(19) 0.076(2) 0.0341(17) -0.0006(15) 0.0079(14) N4 0.0348(16) 0.0316(15) 0.0354(16) 0.0115(13) -0.0039(13) 0.0004(13) C17 0.025(2) 0.035(2) 0.023(2) 0.0049(17) 0.0023(17) 0.0058(18) C18 0.032(3) 0.045(3) 0.038(3) 0.019(2) 0.011(2) 0.013(2) O57 0.0333(14) 0.0584(19) 0.076(2) 0.0341(17) -0.0006(15) 0.0079(14) N54 0.0348(16) 0.0316(15) 0.0354(16) 0.0115(13) -0.0039(13) 0.0004(13) C19 0.0372(19) 0.0248(17) 0.0394(19) 0.0080(15) 0.0026(15) -0.0013(15) C20 0.0323(19) 0.038(2) 0.047(2) 0.0166(17) 0.0082(16) 0.0022(16) C21 0.0343(19) 0.0336(18) 0.0336(18) -0.0010(15) 0.0131(15) -0.0038(15) C22 0.0303(17) 0.0359(18) 0.0331(18) 0.0048(15) 0.0136(14) -0.0011(15) C23 0.0313(17) 0.0268(16) 0.0271(16) 0.0100(13) 0.0086(14) 0.0068(14) C24 0.0314(18) 0.0304(17) 0.0304(17) 0.0015(14) 0.0094(14) 0.0022(14) C25 0.0311(18) 0.0345(18) 0.042(2) 0.0041(16) 0.0180(15) -0.0017(15) C26 0.0248(16) 0.0270(16) 0.0280(16) 0.0035(13) 0.0062(13) 0.0039(13) C27 0.050(2) 0.0301(18) 0.046(2) -0.0002(16) 0.0266(18) -0.0037(17) C28 0.047(2) 0.0344(19) 0.044(2) 0.0039(16) 0.0277(18) -0.0027(17) C29 0.041(2) 0.0302(18) 0.0383(19) 0.0009(15) 0.0183(16) -0.0043(16) C30 0.046(2) 0.0337(19) 0.0351(19) 0.0069(16) 0.0213(17) 0.0005(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N5 2.082(3) . ? Zn1 S1 2.3628(12) . ? Zn1 S3 2.3742(11) . ? Zn1 S2 2.5641(12) . ? Zn1 S4 2.6074(13) . ? Zn2 N6 2.089(3) . ? Zn2 S5 2.3974(11) . ? Zn2 S7 2.4069(13) . ? Zn2 S8 2.5012(12) . ? Zn2 S6 2.5583(12) . ? S1 C1 1.734(3) . ? S2 C1 1.728(3) . ? S3 C6 1.733(3) . ? S4 C6 1.723(3) . ? S5 C11 1.727(3) . ? S6 C11 1.729(3) . ? S7 C16 1.730(3) . ? S8 C16 1.723(3) . ? O1 C3 1.435(5) . ? O2 C5 1.430(4) . ? O3 C8 1.417(5) . ? O5 C13 1.424(5) . ? O6 C15 1.374(5) . ? O8 C20 1.430(4) . ? N1 C1 1.338(4) . ? N1 C4 1.471(4) . ? N1 C2 1.487(4) . ? N2 C6 1.344(4) . ? N2 C7 1.470(5) . ? N2 C39 1.482(5) . ? N2 C9 1.482(5) . ? N3 C11 1.341(4) . ? N3 C12 1.477(5) . ? N3 C14 1.484(4) . ? N5 C21 1.347(4) . ? N5 C25 1.347(4) . ? N6 C29 1.344(4) . ? N6 C28 1.343(4) . ? C2 C3 1.520(5) . ? C4 C5 1.520(5) . ? C7 C8 1.541(5) . ? C9 C10 1.523(7) . ? C10 O4 1.400(12) . ? C39 C40 1.59(2) . ? C40 O44 1.35(2) . ? C12 C13 1.525(5) . ? C14 C15 1.526(5) . ? C16 N54 1.335(4) . ? C16 N4 1.335(4) . ? O7 C18 1.477(5) . ? N4 C19 1.479(4) . ? N4 C17 1.484(5) . ? C17 C18 1.518(7) . ? O57 C58 1.530(19) . ? N54 C19 1.479(4) . ? N54 C57 1.68(2) . ? C57 C58 1.45(3) . ? C19 C20 1.514(5) . ? C21 C22 1.385(4) . ? C22 C23 1.390(4) . ? C23 C24 1.396(4) . ? C23 C26 1.499(4) . ? C24 C25 1.389(4) . ? C26 C27 1.387(5) . ? C26 C30 1.396(5) . ? C27 C28 1.387(5) . ? C29 C30 1.386(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 N5 Zn1 S1 112.02(8) . . ? N5 Zn1 S3 115.27(8) . . ? S1 Zn1 S3 132.63(4) . . ? N5 Zn1 S2 97.19(8) . . ? S1 Zn1 S2 73.68(3) . . ? S3 Zn1 S2 102.54(4) . . ? N5 Zn1 S4 97.93(8) . . ? S1 Zn1 S4 98.66(3) . . ? S3 Zn1 S4 72.61(4) . . ? S2 Zn1 S4 164.75(3) . . ? N6 Zn2 S5 111.75(9) . . ? N6 Zn2 S7 106.37(8) . . ? S5 Zn2 S7 141.88(4) . . ? N6 Zn2 S8 101.97(8) . . ? S5 Zn2 S8 98.36(4) . . ? S7 Zn2 S8 73.88(3) . . ? N6 Zn2 S6 95.67(8) . . ? S5 Zn2 S6 72.86(4) . . ? S7 Zn2 S6 103.20(3) . . ? S8 Zn2 S6 162.24(4) . . ? C1 S1 Zn1 87.49(11) . . ? C1 S2 Zn1 81.38(11) . . ? C6 S3 Zn1 88.28(11) . . ? C6 S4 Zn1 81.20(11) . . ? C11 S5 Zn2 87.59(11) . . ? C11 S6 Zn2 82.52(11) . . ? C16 S7 Zn2 85.72(11) . . ? C16 S8 Zn2 82.94(11) . . ? C1 N1 C4 121.2(3) . . ? C1 N1 C2 122.1(3) . . ? C4 N1 C2 116.7(3) . . ? C6 N2 C7 120.6(3) . . ? C6 N2 C39 121.1(3) . . ? C7 N2 C39 118.3(3) . . ? C6 N2 C9 121.1(3) . . ? C7 N2 C9 118.3(3) . . ? C11 N3 C12 122.1(3) . . ? C11 N3 C14 120.1(3) . . ? C12 N3 C14 117.9(3) . . ? C21 N5 C25 117.8(3) . . ? C21 N5 Zn1 120.6(2) . . ? C25 N5 Zn1 121.5(2) . . ? C29 N6 C28 117.3(3) . . ? C29 N6 Zn2 120.9(2) . . ? C28 N6 Zn2 121.7(2) . . ? N1 C1 S2 121.8(2) . . ? N1 C1 S1 120.8(2) . . ? S2 C1 S1 117.44(18) . . ? N1 C2 C3 112.7(3) . . ? O1 C3 C2 111.9(3) . . ? N1 C4 C5 113.1(3) . . ? O2 C5 C4 109.6(3) . . ? N2 C6 S4 121.4(3) . . ? N2 C6 S3 121.0(3) . . ? S4 C6 S3 117.62(18) . . ? N2 C7 C8 112.2(3) . . ? O3 C8 C7 112.3(4) . . ? N2 C9 C10 116.8(4) . . ? O4 C10 C9 105.5(6) . . ? N2 C39 C40 106.1(7) . . ? O44 C40 C39 107.6(13) . . ? N3 C11 S5 120.4(3) . . ? N3 C11 S6 122.6(3) . . ? S5 C11 S6 116.95(18) . . ? N3 C12 C13 114.1(3) . . ? O5 C13 C12 112.8(3) . . ? N3 C14 C15 114.7(3) . . ? O6 C15 C14 111.1(4) . . ? N54 C16 S8 121.5(2) . . ? N4 C16 S8 121.5(2) . . ? N54 C16 S7 121.1(2) . . ? N4 C16 S7 121.1(2) . . ? S8 C16 S7 117.41(19) . . ? C16 N4 C19 122.0(3) . . ? C16 N4 C17 119.6(3) . . ? C19 N4 C17 117.6(3) . . ? C18 C17 N4 109.0(3) . . ? C17 C18 O7 107.1(3) . . ? C16 N54 C19 122.0(3) . . ? C16 N54 C57 116.5(7) . . ? C19 N54 C57 112.2(7) . . ? N54 C57 C58 103.1(14) . . ? O57 C58 C57 95.1(13) . . ? N54 C19 C20 114.0(3) . . ? N4 C19 C20 114.0(3) . . ? O8 C20 C19 112.2(3) . . ? N5 C21 C22 122.2(3) . . ? C21 C22 C23 120.5(3) . . ? C22 C23 C24 117.2(3) . . ? C22 C23 C26 121.7(3) . . ? C24 C23 C26 121.0(3) . . ? C25 C24 C23 119.4(3) . . ? N5 C25 C24 122.9(3) . . ? C27 C26 C30 117.2(3) . . ? C27 C26 C23 122.0(3) . . ? C30 C26 C23 120.8(3) . . ? C26 C27 C28 119.8(3) . . ? N6 C28 C27 123.1(3) . . ? N6 C29 C30 122.9(3) . . ? C29 C30 C26 119.7(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.54 _refine_diff_density_min -0.73 _refine_diff_density_rms 0.086 # Attachment '5.CIF' data_(5) _database_code_depnum_ccdc_archive 'CCDC 645548' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H48 N6 O4 S8 Zn2' _chemical_formula_sum 'C30 H48 N6 O4 S8 Zn2' _chemical_formula_weight 943.96 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.074(6) _cell_length_b 13.249(5) _cell_length_c 15.350(6) _cell_angle_alpha 104.546(7) _cell_angle_beta 107.095(15) _cell_angle_gamma 92.740(8) _cell_volume 2065.5(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1442 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 30.3 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 1.607 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.702 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type AFC12\K/SATURN724 _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 1' _diffrn_reflns_number 43962 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_av_sigmaI/netI 0.029 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.8 _diffrn_reflns_theta_max 27.5 _reflns_number_total 9411 _reflns_number_gt 8729 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear (Rigaku, 2005)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976) & DIAMOND (Crystal Impact, 2006)' _computing_publication_material SHELXL97 _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^)+(0.0882P)^2^+2.5657P] 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 9411 _refine_ls_number_parameters 451 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.064 _refine_ls_R_factor_gt 0.059 _refine_ls_wR_factor_ref 0.168 _refine_ls_wR_factor_gt 0.162 _refine_ls_goodness_of_fit_ref 1.10 _refine_ls_restrained_S_all 1.10 _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 0.40370(4) 0.72052(3) 0.55437(3) 0.03438(13) Uani 1 1 d . . . Zn2 Zn 0.63665(4) 0.24286(3) -0.07473(3) 0.03441(13) Uani 1 1 d . . . S1 S 0.48523(8) 0.89867(7) 0.59924(6) 0.0350(2) Uani 1 1 d . . . S2 S 0.63266(8) 0.73931(7) 0.66754(7) 0.0360(2) Uani 1 1 d . . . S3 S 0.28323(8) 0.61902(7) 0.61367(7) 0.0367(2) Uani 1 1 d . . . S4 S 0.16429(8) 0.73715(7) 0.47954(6) 0.0351(2) Uani 1 1 d . . . S5 S 0.54742(9) 0.06668(7) -0.09639(7) 0.0403(2) Uani 1 1 d . . . S6 S 0.43465(11) 0.20619(8) -0.20986(7) 0.0479(3) Uani 1 1 d . . . S7 S 0.75485(9) 0.35179(8) -0.13263(7) 0.0419(2) Uani 1 1 d . . . S8 S 0.87067(9) 0.24275(8) 0.00968(7) 0.0419(2) Uani 1 1 d . . . O1 O 0.8412(3) 1.04160(10) 0.6122(2) 0.0616(8) Uani 1 1 d D . . H1O H 0.8278 0.9775 0.5822 0.092 Uiso 1 1 d D . . O2 O -0.1790 0.8350 0.4998 0.0618(8) Uani 1 1 d D . . H2O H -0.1566 0.8563 0.4590 0.093 Uiso 1 1 d D . . O3 O 0.07225(15) 0.1249(3) -0.3692(3) 0.0781(12) Uani 1 1 d D . . H3O H -0.0025 0.0951 -0.3839 0.117 Uiso 1 1 d D . . O4 O 1.1122(5) 0.3372(2) -0.2324(3) 0.1176(18) Uani 1 1 d D . . H4O H 1.0899 0.2783 -0.2732 0.176 Uiso 1 1 d D . . N1 N 0.7219(3) 0.9442(2) 0.7200(2) 0.0326(6) Uani 1 1 d . . . N2 N 0.0343(3) 0.6391(2) 0.5629(2) 0.0351(6) Uani 1 1 d . . . N3 N 0.3323(3) 0.0092(3) -0.2414(2) 0.0446(8) Uani 1 1 d . . . N4 N 1.0048(3) 0.3580(3) -0.0590(2) 0.0401(7) Uani 1 1 d . . . N5 N 0.4365(3) 0.6388(2) 0.4317(2) 0.0336(6) Uani 1 1 d . . . N6 N 0.5854(3) 0.3362(2) 0.0363(2) 0.0340(6) Uani 1 1 d . . . C1 C 0.6253(3) 0.8690(3) 0.6689(2) 0.0295(6) Uani 1 1 d . . . C2 C 0.7145(4) 1.0551(3) 0.7198(3) 0.0371(7) Uani 1 1 d . . . H2A H 0.7809 1.1006 0.7766 0.045 Uiso 1 1 calc R . . H2B H 0.6305 1.0734 0.7244 0.045 Uiso 1 1 calc R . . C3 C 0.7321(4) 1.0775(3) 0.6321(3) 0.0479(9) Uani 1 1 d . . . H3A H 0.6560 1.0436 0.5770 0.058 Uiso 1 1 calc R . . H3B H 0.7378 1.1543 0.6404 0.058 Uiso 1 1 calc R . . C4 C 0.8407(3) 0.9219(3) 0.7830(3) 0.0398(8) Uani 1 1 d . . . H4A H 0.9137 0.9690 0.7841 0.048 Uiso 1 1 calc R . . H4B H 0.8541 0.8485 0.7574 0.048 Uiso 1 1 calc R . . C5 C 0.8367(5) 0.9377(4) 0.8836(3) 0.0570(11) Uani 1 1 d . . . H5A H 0.9168 0.9222 0.9230 0.085 Uiso 1 1 calc R . . H5B H 0.7654 0.8903 0.8829 0.085 Uiso 1 1 calc R . . H5C H 0.8252 1.0107 0.9097 0.085 Uiso 1 1 calc R . . C6 C 0.1482(3) 0.6627(3) 0.5530(2) 0.0301(6) Uani 1 1 d . . . C7 C -0.0801(3) 0.6776(3) 0.5107(3) 0.0414(8) Uani 1 1 d . . . H7A H -0.1569 0.6315 0.5045 0.050 Uiso 1 1 calc R . . H7B H -0.0774 0.6736 0.4461 0.050 Uiso 1 1 calc R . . C8 C -0.0902(4) 0.7897(4) 0.5598(3) 0.0514(10) Uani 1 1 d . . . H8A H -0.1159 0.7907 0.6165 0.062 Uiso 1 1 calc R . . H8B H -0.0055 0.8323 0.5814 0.062 Uiso 1 1 calc R . . C9 C 0.0191(4) 0.5771(3) 0.6269(3) 0.0418(8) Uani 1 1 d . . . H9A H 0.0933 0.5381 0.6407 0.050 Uiso 1 1 calc R . . H9B H -0.0581 0.5248 0.5941 0.050 Uiso 1 1 calc R . . C10 C 0.0079(8) 0.6424(4) 0.7193(4) 0.096(2) Uani 1 1 d . . . H10A H -0.0022 0.5963 0.7584 0.144 Uiso 1 1 calc R . . H10B H -0.0664 0.6802 0.7065 0.144 Uiso 1 1 calc R . . H10C H 0.0851 0.6931 0.7533 0.144 Uiso 1 1 calc R . . C11 C 0.4258(4) 0.0867(3) -0.1877(2) 0.0368(7) Uani 1 1 d . . . C12 C 0.2405(4) 0.0230(3) -0.3261(3) 0.0500(10) Uani 1 1 d . . . H12A H 0.2826 0.0661 -0.3557 0.060 Uiso 1 1 calc R . . H12B H 0.2044 -0.0461 -0.3727 0.060 Uiso 1 1 calc R . . C13 C 0.1395(5) 0.0757(4) -0.2980(4) 0.0607(12) Uani 1 1 d . . . H13A H 0.0791 0.0238 -0.2901 0.073 Uiso 1 1 calc R . . H13B H 0.1769 0.1297 -0.2363 0.073 Uiso 1 1 calc R . . C14 C 0.3214(4) -0.0927(3) -0.2215(3) 0.0492(10) Uani 1 1 d . . . H14A H 0.4078 -0.1108 -0.1950 0.059 Uiso 1 1 calc R . . H14B H 0.2776 -0.1476 -0.2815 0.059 Uiso 1 1 calc R . . C15 C 0.2480(5) -0.0921(4) -0.1518(4) 0.0580(11) Uani 1 1 d . . . H15A H 0.2424 -0.1617 -0.1408 0.087 Uiso 1 1 calc R . . H15B H 0.1620 -0.0752 -0.1781 0.087 Uiso 1 1 calc R . . H15C H 0.2924 -0.0392 -0.0917 0.087 Uiso 1 1 calc R . . C16 C 0.8909(3) 0.3213(3) -0.0598(2) 0.0348(7) Uani 1 1 d . . . C17 C 1.0190(4) 0.4233(3) -0.1209(3) 0.0480(9) Uani 1 1 d . . . H17A H 1.1047 0.4648 -0.0933 0.058 Uiso 1 1 calc R . . H17B H 0.9556 0.4736 -0.1215 0.058 Uiso 1 1 calc R . . C18 C 1.0025(6) 0.3630(5) -0.2208(3) 0.0670(14) Uani 1 1 d . . . H18A H 0.9420 0.2982 -0.2384 0.080 Uiso 1 1 calc R . . H18B H 0.9654 0.4060 -0.2638 0.080 Uiso 1 1 calc R . . C19 C 1.1222(4) 0.3332(4) 0.0030(3) 0.0553(11) Uani 1 1 d . . . H19A H 1.1049 0.3204 0.0594 0.066 Uiso 1 1 calc R . . H19B H 1.1887 0.3948 0.0255 0.066 Uiso 1 1 calc R . . C20 C 1.1721(6) 0.2385(6) -0.0455(4) 0.0843(18) Uani 1 1 d . . . H20A H 1.2494 0.2257 -0.0008 0.126 Uiso 1 1 calc R . . H20B H 1.1919 0.2515 -0.1002 0.126 Uiso 1 1 calc R . . H20C H 1.1073 0.1769 -0.0670 0.126 Uiso 1 1 calc R . . C21 C 0.5420(3) 0.6667(3) 0.4130(2) 0.0356(7) Uani 1 1 d . . . H21 H 0.5983 0.7270 0.4552 0.043 Uiso 1 1 calc R . . C22 C 0.5722(3) 0.6112(3) 0.3346(2) 0.0348(7) Uani 1 1 d . . . H22 H 0.6482 0.6331 0.3239 0.042 Uiso 1 1 calc R . . C23 C 0.4904(3) 0.5231(2) 0.2717(2) 0.0305(7) Uani 1 1 d . . . C24 C 0.3793(3) 0.4964(3) 0.2907(2) 0.0339(7) Uani 1 1 d . . . H24 H 0.3195 0.4381 0.2485 0.041 Uiso 1 1 calc R . . C25 C 0.3567(3) 0.5549(3) 0.3706(3) 0.0359(7) Uani 1 1 d . . . H25 H 0.2812 0.5349 0.3830 0.043 Uiso 1 1 calc R . . C26 C 0.5218(3) 0.4592(3) 0.1890(2) 0.0312(7) Uani 1 1 d . . . C27 C 0.5926(4) 0.5036(3) 0.1436(3) 0.0401(8) Uani 1 1 d . . . H27 H 0.6211 0.5770 0.1642 0.048 Uiso 1 1 calc R . . C28 C 0.6211(4) 0.4394(3) 0.0681(3) 0.0403(8) Uani 1 1 d . . . H28 H 0.6688 0.4709 0.0372 0.048 Uiso 1 1 calc R . . C29 C 0.5168(4) 0.2929(3) 0.0797(3) 0.0394(8) Uani 1 1 d . . . H29 H 0.4902 0.2192 0.0576 0.047 Uiso 1 1 calc R . . C30 C 0.4833(4) 0.3508(3) 0.1548(3) 0.0386(8) Uani 1 1 d . . . H30 H 0.4341 0.3173 0.1834 0.046 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 0.0355(2) 0.0314(2) 0.0355(2) 0.00267(16) 0.01664(17) -0.00115(16) Zn2 0.0350(2) 0.0327(2) 0.0344(2) 0.00247(16) 0.01590(17) -0.00016(16) S1 0.0315(4) 0.0305(4) 0.0397(4) 0.0081(3) 0.0082(3) 0.0026(3) S2 0.0366(4) 0.0321(4) 0.0415(5) 0.0129(3) 0.0132(4) 0.0047(3) S3 0.0320(4) 0.0371(4) 0.0426(5) 0.0166(4) 0.0100(4) 0.0027(3) S4 0.0327(4) 0.0401(5) 0.0360(4) 0.0142(4) 0.0127(3) 0.0052(3) S5 0.0387(5) 0.0342(4) 0.0463(5) 0.0102(4) 0.0118(4) 0.0043(4) S6 0.0532(6) 0.0360(5) 0.0456(5) 0.0145(4) 0.0018(4) -0.0080(4) S7 0.0384(5) 0.0497(5) 0.0416(5) 0.0182(4) 0.0143(4) 0.0034(4) S8 0.0368(5) 0.0485(5) 0.0466(5) 0.0200(4) 0.0165(4) 0.0050(4) O1 0.0591(19) 0.0565(19) 0.081(2) 0.0230(17) 0.0363(17) 0.0059(15) O2 0.0543(19) 0.063(2) 0.075(2) 0.0230(17) 0.0265(16) 0.0170(16) O3 0.0426(18) 0.099(3) 0.110(3) 0.065(3) 0.0194(19) 0.0131(18) O4 0.112(4) 0.115(4) 0.115(4) -0.010(3) 0.058(3) -0.001(3) N1 0.0311(14) 0.0321(14) 0.0327(14) 0.0068(11) 0.0093(11) 0.0019(11) N2 0.0327(14) 0.0323(15) 0.0402(15) 0.0060(12) 0.0155(12) 0.0005(11) N3 0.053(2) 0.0352(16) 0.0371(16) 0.0086(13) 0.0047(14) -0.0072(14) N4 0.0352(15) 0.0440(17) 0.0383(16) 0.0060(13) 0.0135(13) -0.0041(13) N5 0.0351(15) 0.0323(14) 0.0353(14) 0.0051(11) 0.0174(12) 0.0041(11) N6 0.0324(14) 0.0359(15) 0.0327(14) 0.0031(12) 0.0142(12) 0.0035(12) C1 0.0302(16) 0.0323(16) 0.0268(14) 0.0060(12) 0.0124(12) 0.0036(13) C2 0.0378(18) 0.0297(17) 0.0405(18) 0.0027(14) 0.0141(15) -0.0002(14) C3 0.046(2) 0.044(2) 0.061(3) 0.0210(19) 0.0223(19) 0.0007(17) C4 0.0312(17) 0.0407(19) 0.0428(19) 0.0084(16) 0.0073(15) 0.0054(14) C5 0.059(3) 0.062(3) 0.041(2) 0.0080(19) 0.0066(19) 0.019(2) C6 0.0293(15) 0.0280(15) 0.0303(15) 0.0032(12) 0.0099(12) 0.0006(12) C7 0.0291(17) 0.044(2) 0.049(2) 0.0083(17) 0.0148(15) 0.0025(15) C8 0.049(2) 0.051(2) 0.057(2) 0.013(2) 0.022(2) 0.0175(19) C9 0.046(2) 0.0371(19) 0.045(2) 0.0093(16) 0.0218(17) -0.0041(16) C10 0.196(8) 0.050(3) 0.050(3) 0.011(2) 0.057(4) 0.005(4) C11 0.0423(19) 0.0319(17) 0.0318(16) 0.0027(13) 0.0114(14) -0.0035(14) C12 0.047(2) 0.044(2) 0.049(2) 0.0080(18) 0.0068(18) 0.0004(17) C13 0.060(3) 0.064(3) 0.055(3) 0.015(2) 0.019(2) -0.005(2) C14 0.062(3) 0.0306(18) 0.047(2) 0.0070(16) 0.0102(19) -0.0088(17) C15 0.058(3) 0.059(3) 0.060(3) 0.027(2) 0.016(2) -0.005(2) C16 0.0370(18) 0.0319(17) 0.0316(16) -0.0001(13) 0.0134(14) -0.0019(14) C17 0.052(2) 0.046(2) 0.045(2) 0.0072(17) 0.0206(18) -0.0095(18) C18 0.081(4) 0.075(3) 0.050(3) 0.012(2) 0.034(2) -0.004(3) C19 0.0320(19) 0.079(3) 0.052(2) 0.016(2) 0.0121(17) -0.004(2) C20 0.067(3) 0.124(6) 0.066(3) 0.026(3) 0.024(3) 0.038(4) C21 0.0372(18) 0.0324(17) 0.0355(17) 0.0029(13) 0.0150(14) 0.0015(14) C22 0.0336(17) 0.0370(18) 0.0355(17) 0.0079(14) 0.0153(14) 0.0031(14) C23 0.0321(16) 0.0308(16) 0.0312(15) 0.0104(13) 0.0116(13) 0.0091(13) C24 0.0335(17) 0.0298(16) 0.0351(17) 0.0040(13) 0.0103(14) 0.0027(13) C25 0.0365(18) 0.0329(17) 0.0388(18) 0.0053(14) 0.0171(15) 0.0022(14) C26 0.0307(16) 0.0321(16) 0.0308(15) 0.0081(13) 0.0097(13) 0.0067(13) C27 0.044(2) 0.0348(18) 0.0429(19) 0.0054(15) 0.0201(16) 0.0026(15) C28 0.046(2) 0.0373(19) 0.0417(19) 0.0066(15) 0.0235(16) 0.0029(15) C29 0.049(2) 0.0304(17) 0.0411(19) 0.0034(14) 0.0236(16) 0.0013(15) C30 0.048(2) 0.0335(18) 0.0388(18) 0.0075(14) 0.0234(16) 0.0023(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 Zn1 N5 2.065(3) . ? Zn1 S1 2.3397(12) . ? Zn1 S3 2.3609(11) . ? Zn1 S2 2.5770(15) . ? Zn1 S4 2.6056(16) . ? Zn2 N6 2.082(3) . ? Zn2 S7 2.3945(12) . ? Zn2 S5 2.3941(13) . ? Zn2 S6 2.4908(15) . ? Zn2 S8 2.5342(16) . ? S1 C1 1.731(3) . ? S2 C1 1.720(3) . ? S3 C6 1.724(3) . ? S4 C6 1.714(3) . ? S5 C11 1.720(4) . ? S6 C11 1.705(4) . ? S7 C16 1.726(4) . ? S8 C16 1.716(4) . ? O1 C3 1.406(5) . ? O2 C8 1.407(5) . ? O3 C13 1.450(6) . ? O4 C18 1.327(7) . ? N1 C1 1.328(4) . ? N1 C2 1.476(4) . ? N1 C4 1.478(4) . ? N2 C6 1.345(4) . ? N2 C7 1.475(5) . ? N2 C9 1.469(5) . ? N3 C11 1.333(5) . ? N3 C14 1.464(5) . ? N3 C12 1.455(5) . ? N4 C16 1.325(5) . ? N4 C17 1.471(5) . ? N4 C19 1.474(5) . ? N5 C25 1.339(5) . ? N5 C21 1.338(4) . ? N6 C28 1.328(5) . ? N6 C29 1.340(5) . ? C2 C3 1.513(5) . ? C4 C5 1.520(6) . ? C7 C8 1.513(6) . ? C9 C10 1.508(6) . ? C12 C13 1.459(7) . ? C14 C15 1.521(7) . ? C17 C18 1.494(6) . ? C19 C20 1.507(8) . ? C21 C22 1.384(5) . ? C22 C23 1.391(5) . ? C23 C24 1.393(5) . ? C23 C26 1.483(5) . ? C24 C25 1.375(5) . ? C26 C30 1.397(5) . ? C26 C27 1.388(5) . ? C27 C28 1.383(5) . ? C29 C30 1.375(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 N5 Zn1 S1 111.72(9) . . ? N5 Zn1 S3 114.38(9) . . ? S1 Zn1 S3 133.77(4) . . ? N5 Zn1 S2 97.39(9) . . ? S1 Zn1 S2 73.34(3) . . ? S3 Zn1 S2 103.54(4) . . ? N5 Zn1 S4 97.83(9) . . ? S1 Zn1 S4 98.40(4) . . ? S3 Zn1 S4 72.41(4) . . ? S2 Zn1 S4 164.54(3) . . ? N6 Zn2 S7 109.42(9) . . ? N6 Zn2 S5 105.78(9) . . ? S7 Zn2 S5 144.78(4) . . ? N6 Zn2 S6 102.48(9) . . ? S7 Zn2 S6 97.17(5) . . ? S5 Zn2 S6 73.60(4) . . ? N6 Zn2 S8 99.84(9) . . ? S7 Zn2 S8 73.06(4) . . ? S5 Zn2 S8 102.47(4) . . ? S6 Zn2 S8 157.56(4) . . ? C1 S1 Zn1 88.42(12) . . ? C1 S2 Zn1 81.24(11) . . ? C6 S3 Zn1 88.58(12) . . ? C6 S4 Zn1 81.10(12) . . ? C11 S5 Zn2 85.85(12) . . ? C11 S6 Zn2 83.13(13) . . ? C16 S7 Zn2 87.02(13) . . ? C16 S8 Zn2 82.82(13) . . ? C1 N1 C2 121.8(3) . . ? C1 N1 C4 121.8(3) . . ? C2 N1 C4 116.4(3) . . ? C6 N2 C7 120.5(3) . . ? C6 N2 C9 121.9(3) . . ? C7 N2 C9 117.6(3) . . ? C11 N3 C14 122.5(3) . . ? C11 N3 C12 119.5(3) . . ? C14 N3 C12 117.9(3) . . ? C16 N4 C17 121.4(3) . . ? C16 N4 C19 121.1(3) . . ? C17 N4 C19 117.5(3) . . ? C25 N5 C21 118.0(3) . . ? C25 N5 Zn1 121.7(2) . . ? C21 N5 Zn1 120.3(2) . . ? C28 N6 C29 117.7(3) . . ? C28 N6 Zn2 121.8(2) . . ? C29 N6 Zn2 120.5(2) . . ? N1 C1 S2 122.4(3) . . ? N1 C1 S1 120.6(3) . . ? S2 C1 S1 117.00(19) . . ? N1 C2 C3 113.1(3) . . ? O1 C3 C2 113.6(4) . . ? N1 C4 C5 111.9(3) . . ? N2 C6 S4 121.2(3) . . ? N2 C6 S3 121.3(3) . . ? S4 C6 S3 117.55(19) . . ? N2 C7 C8 112.2(3) . . ? O2 C8 C7 112.0(4) . . ? N2 C9 C10 113.7(3) . . ? N3 C11 S5 120.5(3) . . ? N3 C11 S6 122.0(3) . . ? S5 C11 S6 117.4(2) . . ? C13 C12 N3 108.1(4) . . ? O3 C13 C12 110.2(4) . . ? N3 C14 C15 112.1(4) . . ? N4 C16 S8 122.7(3) . . ? N4 C16 S7 120.2(3) . . ? S8 C16 S7 117.1(2) . . ? N4 C17 C18 114.6(4) . . ? O4 C18 C17 111.9(5) . . ? N4 C19 C20 113.2(4) . . ? N5 C21 C22 122.7(3) . . ? C23 C22 C21 119.5(3) . . ? C22 C23 C24 117.3(3) . . ? C22 C23 C26 121.1(3) . . ? C24 C23 C26 121.6(3) . . ? C25 C24 C23 119.7(3) . . ? N5 C25 C24 122.8(3) . . ? C30 C26 C27 117.3(3) . . ? C30 C26 C23 120.9(3) . . ? C27 C26 C23 121.8(3) . . ? C28 C27 C26 119.1(3) . . ? N6 C28 C27 123.5(3) . . ? N6 C29 C30 122.7(3) . . ? C26 C30 C29 119.8(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.47 # in vicinity of the C20 atom _refine_diff_density_min -0.96 _refine_diff_density_rms 0.101 # Attachment '6.CIF' data_(6) _database_code_depnum_ccdc_archive 'CCDC 645549' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H56 N6 O6 S8 Zn2' _chemical_formula_sum 'C32 H56 N6 O6 S8 Zn2' _chemical_formula_weight 1008.17 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' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5416(18) _cell_length_b 11.309(2) _cell_length_c 11.418(2) _cell_angle_alpha 75.640(4) _cell_angle_beta 73.016(4) _cell_angle_gamma 85.238(4) _cell_volume 1141.4(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 459 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.77 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 526 _exptl_absorpt_coefficient_mu 1.462 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.398 _exptl_absorpt_correction_T_max 0.748 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku SCXmini diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean '4900 0 for SAT' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 1' _diffrn_reflns_number 5215 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.043 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.3 _diffrn_reflns_theta_max 27.5 _reflns_number_total 5215 _reflns_number_gt 4452 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; Rigaku (1998). Process-Auto: Automatic Data Acquisition and Processing Package for Imaging Plate and CCD Diffractometers. Rigaku Corporation, 3--9--12 Matsubara-cho, Akishima, Tokyo 196--866, JAPAN ; _computing_cell_refinement ; Rigaku (2006). SCXmini Benchtop Crystallography System software, Version 1.0. Rigaku Americas Corp., 9009 New Trails Drive, The Woodlands, TX 77381--5209, USA ; _computing_data_reduction ; Rigaku (2005). CrystalStructure: Structure Solution and Refinement program, Version 3.7. Rigaku Americas Corp., 9009 New Trails Drive, The Woodlands, TX 77381--5209, USA ; _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material SHELXL97 _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^)+(0.0481P)^2^+0.893P] 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 5215 _refine_ls_number_parameters 254 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.050 _refine_ls_R_factor_gt 0.041 _refine_ls_wR_factor_ref 0.111 _refine_ls_wR_factor_gt 0.103 _refine_ls_goodness_of_fit_ref 1.03 _refine_ls_restrained_S_all 1.03 _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 0.40281(3) 0.05456(3) 0.74326(3) 0.03441(11) Uani 1 1 d . . . S1 S 0.30210(9) -0.00568(7) 0.96229(6) 0.04086(18) Uani 1 1 d . . . S2 S 0.31087(8) -0.15930(6) 0.78623(6) 0.03804(17) Uani 1 1 d . . . S3 S 0.28706(8) 0.16305(6) 0.59238(6) 0.03465(16) Uani 1 1 d . . . S4 S 0.42754(8) 0.29059(6) 0.72387(6) 0.03389(16) Uani 1 1 d . . . O1 O -0.0941(3) -0.3604(3) 0.8976(3) 0.0679(8) Uani 1 1 d D . . H1O H -0.1822 -0.3813 0.9408 0.102 Uiso 1 1 d D . . O2 O 0.0611(2) 0.5816(2) 0.6741(2) 0.0553(6) Uani 1 1 d D . . H2O H 0.0007 0.5955 0.7418 0.083 Uiso 1 1 d D . . N1 N 0.1347(2) -0.2028(2) 1.0223(2) 0.0323(5) Uani 1 1 d . . . N2 N 0.2777(2) 0.40491(19) 0.5614(2) 0.0294(4) Uani 1 1 d . . . N3 N 0.6229(2) 0.0329(2) 0.6576(2) 0.0312(5) Uani 1 1 d . . . C1 C 0.2377(3) -0.1314(2) 0.9332(2) 0.0303(5) Uani 1 1 d . . . C2 C 0.0757(3) -0.3068(3) 0.9972(3) 0.0380(6) Uani 1 1 d . . . H2A H 0.0411 -0.3679 1.0752 0.046 Uiso 1 1 calc R . . H2B H 0.1525 -0.3436 0.9400 0.046 Uiso 1 1 calc R . . C3 C -0.0501(4) -0.2650(3) 0.9393(3) 0.0520(8) Uani 1 1 d . . . H3A H -0.1324 -0.2395 1.0013 0.062 Uiso 1 1 calc R . . H3B H -0.0195 -0.1955 0.8687 0.062 Uiso 1 1 calc R . . C4 C 0.0662(3) -0.1778(3) 1.1475(3) 0.0416(7) Uani 1 1 d . . . H4A H -0.0364 -0.1997 1.1746 0.050 Uiso 1 1 calc R . . H4B H 0.0714 -0.0911 1.1414 0.050 Uiso 1 1 calc R . . C5 C 0.1400(5) -0.2480(4) 1.2447(3) 0.0634(10) Uani 1 1 d . . . H5A H 0.0923 -0.2291 1.3245 0.095 Uiso 1 1 calc R . . H5B H 0.2412 -0.2255 1.2190 0.095 Uiso 1 1 calc R . . H5C H 0.1334 -0.3340 1.2524 0.095 Uiso 1 1 calc R . . C6 C 0.3250(3) 0.2990(2) 0.6202(2) 0.0272(5) Uani 1 1 d . . . C7 C 0.3087(3) 0.5219(2) 0.5835(3) 0.0327(5) Uani 1 1 d . . . H7A H 0.3083 0.5863 0.5094 0.039 Uiso 1 1 calc R . . H7B H 0.4061 0.5177 0.5946 0.039 Uiso 1 1 calc R . . C8 C 0.2003(3) 0.5548(3) 0.6967(3) 0.0386(6) Uani 1 1 d . . . H8A H 0.1919 0.4874 0.7699 0.046 Uiso 1 1 calc R . . H8B H 0.2348 0.6253 0.7140 0.046 Uiso 1 1 calc R . . C9 C 0.1985(3) 0.4118(3) 0.4659(3) 0.0354(6) Uani 1 1 d . . . H9A H 0.1356 0.4838 0.4629 0.042 Uiso 1 1 calc R . . H9B H 0.1369 0.3408 0.4900 0.042 Uiso 1 1 calc R . . C10 C 0.3040(4) 0.4174(3) 0.3364(3) 0.0462(7) Uani 1 1 d . . . H10A H 0.2498 0.4216 0.2767 0.069 Uiso 1 1 calc R . . H10B H 0.3655 0.3457 0.3389 0.069 Uiso 1 1 calc R . . H10C H 0.3638 0.4886 0.3117 0.069 Uiso 1 1 calc R . . C11 C 0.6881(3) 0.1075(3) 0.5475(3) 0.0413(7) Uani 1 1 d . . . H11 H 0.6319 0.1689 0.5115 0.050 Uiso 1 1 calc R . . C12 C 0.8333(3) 0.0986(3) 0.4846(3) 0.0408(7) Uani 1 1 d . . . H12 H 0.8731 0.1541 0.4088 0.049 Uiso 1 1 calc R . . C13 C 0.9213(3) 0.0071(2) 0.5332(2) 0.0286(5) Uani 1 1 d . . . C14 C 0.8527(3) -0.0721(3) 0.6463(3) 0.0524(9) Uani 1 1 d . . . H14 H 0.9059 -0.1356 0.6830 0.063 Uiso 1 1 calc R . . C15 C 0.7052(3) -0.0569(3) 0.7047(3) 0.0510(8) Uani 1 1 d . . . H15 H 0.6618 -0.1117 0.7801 0.061 Uiso 1 1 calc R . . O3 O -0.3669(3) -0.4169(2) 1.0453(2) 0.0521(6) Uani 1 1 d D . . H3O H -0.3758 -0.4008 1.1171 0.078 Uiso 1 1 d D . . C16 C -0.4772(4) -0.3439(4) 0.9995(3) 0.0575(9) Uani 1 1 d . . . H16A H -0.5721 -0.3750 1.0498 0.086 Uiso 1 1 calc R . . H16B H -0.4641 -0.3463 0.9135 0.086 Uiso 1 1 calc R . . H16C H -0.4699 -0.2611 1.0042 0.086 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 0.03510(18) 0.03410(18) 0.02918(17) -0.00421(13) -0.00426(13) -0.00080(13) S1 0.0565(4) 0.0365(4) 0.0294(3) -0.0118(3) -0.0052(3) -0.0126(3) S2 0.0512(4) 0.0343(3) 0.0269(3) -0.0109(3) -0.0027(3) -0.0097(3) S3 0.0428(4) 0.0302(3) 0.0368(4) -0.0129(3) -0.0154(3) -0.0018(3) S4 0.0430(4) 0.0315(3) 0.0327(3) -0.0110(3) -0.0159(3) -0.0013(3) O1 0.0405(13) 0.106(2) 0.0701(17) -0.0601(16) 0.0013(12) -0.0149(13) O2 0.0409(12) 0.0747(16) 0.0561(14) -0.0321(13) -0.0133(11) 0.0166(11) N1 0.0360(12) 0.0335(11) 0.0257(10) -0.0061(9) -0.0055(9) -0.0047(9) N2 0.0342(11) 0.0275(10) 0.0268(10) -0.0095(8) -0.0066(9) 0.0007(9) N3 0.0319(11) 0.0321(11) 0.0272(11) -0.0061(9) -0.0054(9) -0.0005(9) C1 0.0361(13) 0.0285(12) 0.0262(12) -0.0062(10) -0.0096(10) 0.0026(10) C2 0.0422(15) 0.0329(14) 0.0370(14) -0.0074(12) -0.0067(12) -0.0084(12) C3 0.0454(17) 0.058(2) 0.060(2) -0.0250(17) -0.0164(16) -0.0042(15) C4 0.0428(16) 0.0467(17) 0.0296(14) -0.0107(12) 0.0010(12) -0.0034(13) C5 0.079(3) 0.076(3) 0.0348(17) -0.0135(17) -0.0131(17) -0.003(2) C6 0.0291(12) 0.0283(12) 0.0238(11) -0.0107(10) -0.0029(9) -0.0012(10) C7 0.0336(13) 0.0273(12) 0.0349(14) -0.0089(11) -0.0046(11) -0.0013(10) C8 0.0420(15) 0.0371(14) 0.0427(15) -0.0212(12) -0.0125(13) 0.0045(12) C9 0.0332(13) 0.0391(14) 0.0354(14) -0.0078(12) -0.0141(11) 0.0035(11) C10 0.0510(18) 0.0584(19) 0.0325(15) -0.0114(14) -0.0168(13) 0.0017(15) C11 0.0374(15) 0.0382(15) 0.0367(15) 0.0008(12) -0.0033(12) 0.0080(12) C12 0.0429(15) 0.0354(14) 0.0312(14) 0.0054(11) -0.0025(12) 0.0027(12) C13 0.0328(13) 0.0296(12) 0.0253(12) -0.0074(10) -0.0098(10) -0.0017(10) C14 0.0392(16) 0.064(2) 0.0374(16) 0.0124(15) -0.0079(13) 0.0089(14) C15 0.0414(16) 0.059(2) 0.0371(16) 0.0108(14) -0.0064(13) 0.0027(14) O3 0.0477(13) 0.0661(15) 0.0467(13) -0.0250(12) -0.0103(11) 0.0016(11) C16 0.059(2) 0.066(2) 0.052(2) -0.0178(17) -0.0227(17) 0.0075(17) _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 N3 2.064(2) . ? Zn S1 2.3455(9) . ? Zn S3 2.3518(8) . ? Zn S2 2.5243(8) . ? Zn S4 2.6477(9) . ? S1 C1 1.733(3) . ? S2 C1 1.716(3) . ? S3 C6 1.731(2) . ? S4 C6 1.724(3) . ? O1 C3 1.419(4) . ? O1 H1O 0.860 . ? O2 C8 1.421(4) . ? O2 H2O 0.860 . ? N1 C1 1.340(3) . ? N1 C2 1.468(3) . ? N1 C4 1.474(3) . ? N2 C6 1.333(3) . ? N2 C7 1.475(3) . ? N2 C9 1.483(3) . ? N3 C15 1.335(4) . ? N3 C11 1.335(3) . ? C2 C3 1.521(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.512(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C7 C8 1.507(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.516(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.370(4) . ? C11 H11 0.9300 . ? C12 C13 1.388(4) . ? C12 H12 0.9300 . ? C13 C14 1.388(4) . ? C13 C13 1.488(5) 2_756 ? C14 C15 1.386(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? O3 C16 1.423(4) . ? O3 H3O 0.862 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? 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 N3 Zn S1 122.13(6) . . ? N3 Zn S3 109.65(6) . . ? S1 Zn S3 127.91(3) . . ? N3 Zn S2 101.35(6) . . ? S1 Zn S2 74.33(2) . . ? S3 Zn S2 102.11(3) . . ? N3 Zn S4 93.34(6) . . ? S1 Zn S4 98.31(3) . . ? S3 Zn S4 72.04(2) . . ? S2 Zn S4 165.31(3) . . ? C1 S1 Zn 85.71(9) . . ? C1 S2 Zn 80.57(9) . . ? C6 S3 Zn 89.85(9) . . ? C6 S4 Zn 80.70(8) . . ? C3 O1 H1O 110 . . ? C8 O2 H2O 108 . . ? C1 N1 C2 121.3(2) . . ? C1 N1 C4 122.8(2) . . ? C2 N1 C4 115.8(2) . . ? C6 N2 C7 121.5(2) . . ? C6 N2 C9 121.9(2) . . ? C7 N2 C9 116.6(2) . . ? C15 N3 C11 116.8(2) . . ? C15 N3 Zn 122.94(19) . . ? C11 N3 Zn 120.24(18) . . ? N1 C1 S2 121.8(2) . . ? N1 C1 S1 120.92(19) . . ? S2 C1 S1 117.25(15) . . ? N1 C2 C3 110.3(2) . . ? N1 C2 H2A 109.6 . . ? C3 C2 H2A 109.6 . . ? N1 C2 H2B 109.6 . . ? C3 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? O1 C3 C2 110.9(3) . . ? O1 C3 H3A 109.5 . . ? C2 C3 H3A 109.5 . . ? O1 C3 H3B 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? N1 C4 C5 112.2(3) . . ? N1 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? N1 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 S4 122.32(19) . . ? N2 C6 S3 120.42(19) . . ? S4 C6 S3 117.24(15) . . ? N2 C7 C8 113.6(2) . . ? N2 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? N2 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? O2 C8 C7 110.0(2) . . ? O2 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? O2 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? N2 C9 C10 111.3(2) . . ? N2 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? N2 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C12 123.7(3) . . ? N3 C11 H11 118.2 . . ? C12 C11 H11 118.2 . . ? C11 C12 C13 120.4(3) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C14 116.0(2) . . ? C12 C13 C13 122.1(3) . 2_756 ? C14 C13 C13 122.0(3) . 2_756 ? C15 C14 C13 120.4(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? N3 C15 C14 122.8(3) . . ? N3 C15 H15 118.6 . . ? C14 C15 H15 118.6 . . ? C16 O3 H3O 104 . . ? O3 C16 H16A 109.5 . . ? O3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.43 _refine_diff_density_min -0.56 _refine_diff_density_rms 0.074 # Attachment '7.CIF' data_(7) _database_code_depnum_ccdc_archive 'CCDC 645550' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H40 N6 O4 S8 Zn2' _chemical_formula_sum 'C26 H40 N6 O4 S8 Zn2' _chemical_formula_weight 887.98 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc ' 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 8.6591(7) _cell_length_b 14.0066(11) _cell_length_c 15.5984(13) _cell_angle_alpha 90 _cell_angle_beta 97.409(2) _cell_angle_gamma 90 _cell_volume 1876.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 319 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 28.8 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 1.764 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.518 _exptl_absorpt_correction_T_max 0.730 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku SCXmini diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean '4900 0 for SAT' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 1' _diffrn_reflns_number 19113 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_av_sigmaI/netI 0.022 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.0 _diffrn_reflns_theta_max 27.5 _reflns_number_total 4305 _reflns_number_gt 3683 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; Rigaku (1998). Process-Auto: Automatic Data Acquisition and Processing Package for Imaging Plate and CCD Diffractometers. Rigaku Corporation, 3--9--12 Matsubara-cho, Akishima, Tokyo 196--866, JAPAN ; _computing_cell_refinement ; Rigaku (2006). SCXmini Benchtop Crystallography System software, Version 1.0. Rigaku Americas Corp., 9009 New Trails Drive, The Woodlands, TX 77381--5209, USA ; _computing_data_reduction ; Rigaku (2005). CrystalStructure: Structure Solution and Refinement program, Version 3.7. Rigaku Americas Corp., 9009 New Trails Drive, The Woodlands, TX 77381--5209, USA ; _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material SHELXL97 _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. In the structure of {Zn[S2CN(CH2CH2OH)Me]2}2(4,4-bipyridine), the CH2CH2 atoms of the CH2CH2OH group with the O1 atom were disordered over two positions with the major component having a site occupancy factor of 0.668(8). ; _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^)+(0.026P)^2^+1.462P] 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 SHELXL _refine_ls_extinction_coef 0.0007(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4305 _refine_ls_number_parameters 227 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.040 _refine_ls_R_factor_gt 0.032 _refine_ls_wR_factor_ref 0.071 _refine_ls_wR_factor_gt 0.068 _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_restrained_S_all 1.05 _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 0.12867(3) 0.269230(19) 0.753814(16) 0.03367(9) Uani 1 1 d . . . S1 S -0.09730(7) 0.30769(5) 0.66447(4) 0.04247(15) Uani 1 1 d . A . S2 S 0.08800(7) 0.14084(4) 0.62213(4) 0.03630(14) Uani 1 1 d . A . S3 S 0.38702(7) 0.29831(4) 0.73411(4) 0.04324(16) Uani 1 1 d . . . S4 S 0.20876(7) 0.41791(4) 0.84139(4) 0.03810(14) Uani 1 1 d . . . O2 O 0.4941(2) 0.50231(15) 0.62238(12) 0.0543(5) Uani 1 1 d D . . H2O H 0.4837 0.5441 0.5818 0.081 Uiso 1 1 d D . . N2 N 0.4914(2) 0.46385(13) 0.80484(12) 0.0343(4) Uani 1 1 d . . . N3 N 0.0728(2) 0.17662(12) 0.84739(11) 0.0291(4) Uani 1 1 d . . . C1 C -0.0683(3) 0.21234(16) 0.59704(14) 0.0359(5) Uani 1 1 d . . . C4 C -0.1543(4) 0.1178(3) 0.4685(2) 0.0721(10) Uani 0.668(8) 1 d P A 1 H4A H -0.1579 0.0597 0.5008 0.108 Uiso 0.668(8) 1 calc PR A 1 H4B H -0.0575 0.1212 0.4448 0.108 Uiso 0.668(8) 1 calc PR A 1 H4C H -0.2392 0.1188 0.4224 0.108 Uiso 0.668(8) 1 calc PR A 1 N1 N -0.1670(3) 0.1997(2) 0.52559(17) 0.0706(8) Uani 0.668(8) 1 d P A 1 O1 O -0.5063(3) 0.35840(15) 0.50096(14) 0.0642(6) Uani 0.668(8) 1 d PD A 1 H1O H -0.5044 0.3951 0.5452 0.096 Uiso 0.668(8) 1 d PD A 1 C2 C -0.2721(5) 0.2823(3) 0.4892(2) 0.0403(11) Uani 0.668(8) 1 d P A 1 H2A H -0.2261 0.3430 0.5085 0.048 Uiso 0.668(8) 1 calc PR A 1 H2B H -0.2851 0.2811 0.4265 0.048 Uiso 0.668(8) 1 calc PR A 1 C3 C -0.4287(4) 0.2696(3) 0.5221(2) 0.0395(11) Uani 0.668(8) 1 d P A 1 H3A H -0.4862 0.2167 0.4933 0.047 Uiso 0.668(8) 1 calc PR A 1 H3B H -0.4156 0.2585 0.5840 0.047 Uiso 0.668(8) 1 calc PR A 1 C41 C -0.1543(4) 0.1178(3) 0.4685(2) 0.0721(10) Uani 0.332(8) 1 d P A 2 H4D H -0.0675 0.0788 0.4915 0.108 Uiso 0.332(8) 1 calc PR A 2 H4E H -0.1387 0.1401 0.4120 0.108 Uiso 0.332(8) 1 calc PR A 2 H4F H -0.2482 0.0808 0.4644 0.108 Uiso 0.332(8) 1 calc PR A 2 N11 N -0.1670(3) 0.1997(2) 0.52559(17) 0.0706(8) Uani 0.332(8) 1 d P A 2 O11 O -0.5063(3) 0.35840(15) 0.50096(14) 0.0642(6) Uani 0.332(8) 1 d PD A 2 H11O H -0.5044 0.3951 0.5452 0.096 Uiso 0.332(8) 1 d PD A 2 C21 C -0.3421(10) 0.2257(6) 0.5310(5) 0.042(2) Uiso 0.332(8) 1 d P A 2 H21A H -0.4136 0.1782 0.5035 0.051 Uiso 0.332(8) 1 calc PR A 2 H21B H -0.3625 0.2366 0.5899 0.051 Uiso 0.332(8) 1 calc PR A 2 C31 C -0.3441(12) 0.3152(7) 0.4803(6) 0.050(2) Uiso 0.332(8) 1 d P A 2 H31A H -0.3446 0.3029 0.4191 0.060 Uiso 0.332(8) 1 calc PR A 2 H31B H -0.2571 0.3564 0.5008 0.060 Uiso 0.332(8) 1 calc PR A 2 C5 C 0.3756(2) 0.40057(15) 0.79508(13) 0.0300(4) Uani 1 1 d . . . C6 C 0.6298(3) 0.45473(17) 0.76017(15) 0.0370(5) Uani 1 1 d . . . H6A H 0.6374 0.3894 0.7405 0.044 Uiso 1 1 calc R . . H6B H 0.7218 0.4681 0.8008 0.044 Uiso 1 1 calc R . . C7 C 0.6269(3) 0.52085(18) 0.68401(16) 0.0434(6) Uani 1 1 d . . . H7A H 0.6241 0.5865 0.7035 0.052 Uiso 1 1 calc R . . H7B H 0.7209 0.5122 0.6571 0.052 Uiso 1 1 calc R . . C8 C 0.4798(3) 0.55199(18) 0.85398(18) 0.0509(7) Uani 1 1 d . . . H8A H 0.4150 0.5969 0.8195 0.076 Uiso 1 1 calc R . . H8B H 0.5818 0.5788 0.8689 0.076 Uiso 1 1 calc R . . H8C H 0.4350 0.5382 0.9058 0.076 Uiso 1 1 calc R . . C9 C 0.1450(3) 0.17879(15) 0.92844(13) 0.0325(5) Uani 1 1 d . . . H9 H 0.2153 0.2278 0.9443 0.039 Uiso 1 1 calc R . . C10 C 0.1197(3) 0.11134(15) 0.98959(13) 0.0326(5) Uani 1 1 d . . . H10 H 0.1730 0.1153 1.0452 0.039 Uiso 1 1 calc R . . C11 C 0.0144(2) 0.03735(13) 0.96824(12) 0.0252(4) Uani 1 1 d . . . C12 C -0.0627(2) 0.03685(15) 0.88403(13) 0.0298(4) Uani 1 1 d . . . H12 H -0.1359 -0.0103 0.8669 0.036 Uiso 1 1 calc R . . C13 C -0.0304(3) 0.10618(15) 0.82641(13) 0.0321(4) Uani 1 1 d . . . H13 H -0.0824 0.1042 0.7704 0.039 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 0.03250(15) 0.03464(15) 0.03376(15) 0.01060(11) 0.00387(10) -0.00615(11) S1 0.0408(3) 0.0420(3) 0.0427(3) -0.0082(3) -0.0018(3) 0.0150(3) S2 0.0359(3) 0.0352(3) 0.0371(3) -0.0035(2) 0.0023(2) 0.0080(2) S3 0.0423(3) 0.0328(3) 0.0590(4) -0.0142(3) 0.0235(3) -0.0108(2) S4 0.0394(3) 0.0345(3) 0.0434(3) -0.0050(2) 0.0166(2) -0.0041(2) O2 0.0557(11) 0.0620(12) 0.0434(10) 0.0083(9) -0.0004(9) -0.0076(10) N2 0.0364(10) 0.0301(9) 0.0372(10) -0.0046(8) 0.0075(8) -0.0072(8) N3 0.0325(9) 0.0265(8) 0.0288(9) 0.0030(7) 0.0064(7) -0.0044(7) C1 0.0331(11) 0.0395(12) 0.0347(11) -0.0034(9) 0.0024(9) 0.0055(9) C4 0.0594(19) 0.094(3) 0.0572(18) -0.0395(18) -0.0127(14) 0.0133(17) N1 0.0513(14) 0.093(2) 0.0599(15) -0.0365(14) -0.0232(12) 0.0314(14) O1 0.0664(13) 0.0546(12) 0.0629(13) -0.0015(10) -0.0246(11) 0.0209(10) C2 0.035(2) 0.049(2) 0.0366(19) 0.0126(16) 0.0022(15) -0.0006(17) C3 0.033(2) 0.039(2) 0.046(2) 0.0109(16) 0.0004(15) -0.0039(16) C41 0.0594(19) 0.094(3) 0.0572(18) -0.0395(18) -0.0127(14) 0.0133(17) N11 0.0513(14) 0.093(2) 0.0599(15) -0.0365(14) -0.0232(12) 0.0314(14) O11 0.0664(13) 0.0546(12) 0.0629(13) -0.0015(10) -0.0246(11) 0.0209(10) C5 0.0340(11) 0.0274(10) 0.0289(10) 0.0028(8) 0.0051(8) -0.0025(8) C6 0.0297(11) 0.0357(12) 0.0460(13) -0.0011(10) 0.0067(10) -0.0069(9) C7 0.0417(13) 0.0458(14) 0.0446(13) 0.0020(11) 0.0124(11) -0.0094(11) C8 0.0549(16) 0.0406(14) 0.0596(16) -0.0180(12) 0.0159(13) -0.0137(12) C9 0.0375(12) 0.0292(11) 0.0310(11) -0.0006(8) 0.0053(9) -0.0112(9) C10 0.0411(12) 0.0322(11) 0.0242(10) -0.0007(8) 0.0033(9) -0.0103(9) C11 0.0293(10) 0.0238(10) 0.0238(9) -0.0003(8) 0.0081(8) -0.0020(8) C12 0.0337(11) 0.0279(10) 0.0275(10) 0.0001(8) 0.0024(8) -0.0076(8) C13 0.0363(11) 0.0336(11) 0.0257(10) 0.0025(8) 0.0015(8) -0.0069(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn N3 2.0567(16) . ? Zn S1 2.3147(7) . ? Zn S3 2.3329(7) . ? Zn S4 2.5376(6) . ? Zn S2 2.7185(6) . ? S1 C1 1.738(2) . ? S2 C1 1.689(2) . ? S3 C5 1.729(2) . ? S4 C5 1.713(2) . ? O2 C7 1.424(3) . ? O2 H2O 0.859 . ? N2 C5 1.332(3) . ? N2 C8 1.463(3) . ? N2 C6 1.468(3) . ? N3 C9 1.337(3) . ? N3 C13 1.343(3) . ? C1 N11 1.326(3) . ? C1 N1 1.326(3) . ? C4 N1 1.465(4) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? N1 C2 1.535(5) . ? O1 C3 1.431(4) . ? O1 H1O 0.860 . ? O1 H11O 0.860 . ? C2 C3 1.521(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C41 N11 1.465(4) . ? C41 H4D 0.9600 . ? C41 H4E 0.9600 . ? C41 H4F 0.9600 . ? N11 C21 1.572(9) . ? O11 C31 1.600(11) . ? O11 H1O 0.860 . ? O11 H11O 0.860 . ? C21 C31 1.481(13) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C6 C7 1.504(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.380(3) . ? C9 H9 0.9300 . ? C10 C11 1.392(3) . ? C10 H10 0.9300 . ? C11 C12 1.395(3) . ? C11 C11 1.484(4) 3_557 ? C12 C13 1.376(3) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Zn S1 108.42(5) . . ? N3 Zn S3 121.40(5) . . ? S1 Zn S3 129.10(3) . . ? N3 Zn S4 102.04(5) . . ? S1 Zn S4 106.51(2) . . ? S3 Zn S4 74.19(2) . . ? N3 Zn S2 95.72(5) . . ? S1 Zn S2 71.45(2) . . ? S3 Zn S2 92.81(2) . . ? S4 Zn S2 161.69(2) . . ? C1 S1 Zn 90.50(8) . . ? C1 S2 Zn 78.74(8) . . ? C5 S3 Zn 87.03(7) . . ? C5 S4 Zn 80.99(7) . . ? C7 O2 H2O 112 . . ? C5 N2 C8 121.30(19) . . ? C5 N2 C6 122.45(18) . . ? C8 N2 C6 115.95(18) . . ? C9 N3 C13 117.56(17) . . ? C9 N3 Zn 122.19(14) . . ? C13 N3 Zn 120.03(14) . . ? N11 C1 S2 121.73(18) . . ? N1 C1 S2 121.73(18) . . ? N11 C1 S1 118.94(18) . . ? N1 C1 S1 118.94(18) . . ? S2 C1 S1 119.30(13) . . ? C1 N1 C4 121.7(2) . . ? C1 N1 C2 119.8(3) . . ? C4 N1 C2 116.9(2) . . ? C3 O1 H1O 112 . . ? C3 O1 H11O 112 . . ? C3 C2 N1 107.4(3) . . ? C3 C2 H2A 110.2 . . ? N1 C2 H2A 110.2 . . ? C3 C2 H2B 110.2 . . ? N1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? O1 C3 C2 103.5(3) . . ? O1 C3 H3A 111.1 . . ? C2 C3 H3A 111.1 . . ? O1 C3 H3B 111.1 . . ? C2 C3 H3B 111.1 . . ? H3A C3 H3B 109.0 . . ? N11 C41 H4D 109.5 . . ? N11 C41 H4E 109.5 . . ? H4D C41 H4E 109.5 . . ? N11 C41 H4F 109.5 . . ? H4D C41 H4F 109.5 . . ? H4E C41 H4F 109.5 . . ? C1 N11 C41 121.7(2) . . ? C1 N11 C21 116.4(3) . . ? C41 N11 C21 111.3(4) . . ? C31 O11 H1O 117 . . ? C31 O11 H11O 117 . . ? C31 C21 N11 96.5(6) . . ? C31 C21 H21A 112.5 . . ? N11 C21 H21A 112.5 . . ? C31 C21 H21B 112.5 . . ? N11 C21 H21B 112.5 . . ? H21A C21 H21B 110.0 . . ? C21 C31 O11 99.4(6) . . ? C21 C31 H31A 111.9 . . ? O11 C31 H31A 111.9 . . ? C21 C31 H31B 111.9 . . ? O11 C31 H31B 111.9 . . ? H31A C31 H31B 109.6 . . ? N2 C5 S4 121.37(16) . . ? N2 C5 S3 121.21(16) . . ? S4 C5 S3 117.42(12) . . ? N2 C6 C7 112.93(19) . . ? N2 C6 H6A 109.0 . . ? C7 C6 H6A 109.0 . . ? N2 C6 H6B 109.0 . . ? C7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? O2 C7 C6 110.54(19) . . ? O2 C7 H7A 109.5 . . ? C6 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C10 122.78(19) . . ? N3 C9 H9 118.6 . . ? C10 C9 H9 118.6 . . ? C9 C10 C11 120.13(19) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 116.64(17) . . ? C10 C11 C11 121.8(2) . 3_557 ? C12 C11 C11 121.6(2) . 3_557 ? C13 C12 C11 119.91(19) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? N3 C13 C12 122.96(19) . . ? N3 C13 H13 118.5 . . ? C12 C13 H13 118.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.55 _refine_diff_density_min -0.59 _refine_diff_density_rms 0.058