# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Peng Cheng' _publ_contact_author_email PCHENG@NANKAI.EDU.CN _publ_section_title ; 1D, 2D and 3D Luminescent Zinc(II) Coordination Polymers Assembled by Varying Flexible Sulfur-ether Ligands ; loop_ _publ_author_name 'Peng Cheng.' 'Dai-Zheng Liao.' 'Ming-Li Liu.' 'Peng Ren.' 'Wei Shi.' ; Shi-Ping Yan ; 'Jun Zhang.' # Attachment '3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 643830' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H80 N8 O17 S8 Zn4' _chemical_formula_weight 2231.72 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 P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.4090(11) _cell_length_b 10.5542(14) _cell_length_c 26.799(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2378.4(5) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 2708 _cell_measurement_theta_min 2.456 _cell_measurement_theta_max 25.145 _exptl_crystal_description block _exptl_crystal_colour cololess _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 1.247 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8067 _exptl_absorpt_correction_T_max 0.8855 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13662 _diffrn_reflns_av_R_equivalents 0.0798 _diffrn_reflns_av_sigmaI/netI 0.1050 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 26.39 _reflns_number_total 4848 _reflns_number_gt 2829 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment geom _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0016(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.020(15) _refine_ls_number_reflns 4848 _refine_ls_number_parameters 326 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1127 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.980 _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 N1 N 0.2316(5) 0.6336(4) 0.30435(12) 0.0436(11) Uani 1 1 d . . . C13 C 0.2225(6) 0.6372(5) 0.35434(15) 0.0460(14) Uani 1 1 d . . . H13 H 0.1888 0.5645 0.3708 0.055 Uiso 1 1 calc R . . C12 C 0.2800(7) 0.7374(6) 0.28119(19) 0.0701(18) Uani 1 1 d . . . H12 H 0.2867 0.7372 0.2465 0.084 Uiso 1 1 calc R . . C11 C 0.3204(11) 0.8445(6) 0.3066(2) 0.114(3) Uani 1 1 d . . . H11 H 0.3560 0.9155 0.2893 0.137 Uiso 1 1 calc R . . C10 C 0.3087(10) 0.8477(6) 0.3574(2) 0.093(2) Uani 1 1 d . . . H10 H 0.3337 0.9214 0.3748 0.112 Uiso 1 1 calc R . . C9 C 0.2597(6) 0.7415(5) 0.38271(17) 0.0500(14) Uani 1 1 d . . . C8 C 0.2541(6) 0.7327(5) 0.43886(16) 0.0530(15) Uani 1 1 d . . . H8A H 0.1540 0.6962 0.4496 0.064 Uiso 1 1 calc R . . H8B H 0.2649 0.8161 0.4537 0.064 Uiso 1 1 calc R . . O3 O 0.7408(4) 0.8588(4) 1.17463(11) 0.0600(11) Uani 1 1 d . . . C14 C 0.6399(7) 0.7741(5) 1.16840(18) 0.0515(15) Uani 1 1 d . . . Zn1 Zn 0.32597(7) 0.53729(6) 0.771309(19) 0.0460(2) Uani 1 1 d . . . S2 S 0.60164(17) 0.54845(14) 0.96135(4) 0.0539(4) Uani 1 1 d . . . S1 S 0.41598(19) 0.63366(17) 0.45695(5) 0.0661(5) Uani 1 1 d . . . C1 C 0.3675(7) 0.5200(6) 0.67701(18) 0.0607(17) Uani 1 1 d . . . C20 C 0.7157(6) 0.7753(4) 1.07815(15) 0.0384(13) Uani 1 1 d . . . H20 H 0.7844 0.8420 1.0851 0.046 Uiso 1 1 calc R . . O1 O 0.3000(6) 0.6000(4) 0.70512(12) 0.0973(17) Uani 1 1 d . . . O2 O 0.4191(6) 0.4219(4) 0.69276(12) 0.0739(13) Uani 1 1 d . . . C19 C 0.7083(6) 0.7270(4) 1.02998(16) 0.0455(14) Uani 1 1 d . . . H19 H 0.7716 0.7616 1.0050 0.055 Uiso 1 1 calc R . . C6 C 0.3047(7) 0.6832(5) 0.55258(16) 0.0498(14) Uani 1 1 d . . . H6 H 0.2517 0.7534 0.5399 0.060 Uiso 1 1 calc R . . C7 C 0.2959(7) 0.6566(5) 0.60317(16) 0.0511(15) Uani 1 1 d . . . H7 H 0.2372 0.7087 0.6242 0.061 Uiso 1 1 calc R . . C15 C 0.6222(5) 0.7256(4) 1.11609(16) 0.0364(12) Uani 1 1 d . . . N2 N 0.5584(5) 0.5358(4) 0.79872(12) 0.0419(10) Uani 1 1 d . . . C16 C 0.5168(6) 0.6321(5) 1.10393(18) 0.0507(14) Uani 1 1 d . . . H16 H 0.4483 0.6011 1.1283 0.061 Uiso 1 1 calc R . . C2 C 0.3746(6) 0.5525(5) 0.62215(15) 0.0416(13) Uani 1 1 d . . . C4 C 0.4684(6) 0.5007(4) 0.53991(17) 0.0480(15) Uani 1 1 d . . . H4 H 0.5253 0.4475 0.5188 0.058 Uiso 1 1 calc R . . C3 C 0.4593(6) 0.4757(5) 0.59064(16) 0.0521(14) Uani 1 1 d . . . H3 H 0.5117 0.4054 0.6035 0.063 Uiso 1 1 calc R . . C5 C 0.3905(6) 0.6074(5) 0.52117(15) 0.0388(12) Uani 1 1 d . . . C18 C 0.6065(6) 0.6273(5) 1.01916(17) 0.0417(12) Uani 1 1 d . . . C25 C 0.6663(7) 0.4501(5) 0.78302(16) 0.0518(13) Uani 1 1 d . . . H25 H 0.6458 0.4043 0.7541 0.062 Uiso 1 1 calc R . . C22 C 0.7225(6) 0.5743(4) 0.87031(16) 0.0434(13) Uani 1 1 d . . . C17 C 0.5097(6) 0.5831(5) 1.05669(18) 0.0503(15) Uani 1 1 d . . . H17 H 0.4379 0.5184 1.0498 0.060 Uiso 1 1 calc R . . C21 C 0.7350(6) 0.6340(5) 0.92101(16) 0.0530(15) Uani 1 1 d . . . H21A H 0.7051 0.7226 0.9195 0.064 Uiso 1 1 calc R . . H21B H 0.8432 0.6282 0.9333 0.064 Uiso 1 1 calc R . . C26 C 0.5903(6) 0.5968(5) 0.84119(16) 0.0427(13) Uani 1 1 d . . . H26 H 0.5188 0.6583 0.8518 0.051 Uiso 1 1 calc R . . C24 C 0.8042(7) 0.4283(5) 0.80818(18) 0.0600(16) Uani 1 1 d . . . H24 H 0.8786 0.3716 0.7955 0.072 Uiso 1 1 calc R . . C23 C 0.8332(7) 0.4906(5) 0.85243(19) 0.0601(16) Uani 1 1 d . . . H23 H 0.9269 0.4759 0.8700 0.072 Uiso 1 1 calc R . . O4 O 0.5642(7) 0.7244(5) 1.20192(15) 0.127(2) Uani 1 1 d . . . O5 O 0.0760(17) 0.5186(13) 0.7367(5) 0.067(4) Uani 0.25 1 d PU . . 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 N1 0.048(3) 0.060(3) 0.0225(19) 0.007(2) -0.0040(19) 0.003(2) C13 0.062(4) 0.051(3) 0.025(2) 0.004(2) 0.004(2) -0.009(3) C12 0.105(5) 0.070(4) 0.036(3) 0.016(3) -0.010(3) -0.001(4) C11 0.215(9) 0.071(5) 0.056(4) 0.028(4) -0.037(6) -0.036(6) C10 0.175(7) 0.054(4) 0.050(3) 0.011(3) -0.040(5) -0.031(5) C9 0.060(4) 0.057(4) 0.033(3) 0.002(3) -0.006(3) 0.007(3) C8 0.070(4) 0.054(3) 0.036(3) -0.007(2) -0.007(3) 0.003(3) O3 0.072(3) 0.079(3) 0.0292(18) -0.0106(19) 0.0049(18) -0.031(2) C14 0.052(4) 0.070(4) 0.033(3) -0.002(3) 0.002(3) -0.021(3) Zn1 0.0548(4) 0.0578(4) 0.0255(3) -0.0002(3) -0.0003(3) 0.0099(3) S2 0.0643(10) 0.0579(9) 0.0396(7) -0.0131(7) -0.0062(7) -0.0117(8) S1 0.0613(10) 0.1081(13) 0.0287(7) 0.0120(8) 0.0071(7) 0.0210(10) C1 0.074(5) 0.080(4) 0.028(3) 0.004(3) -0.003(3) 0.009(4) C20 0.039(3) 0.045(3) 0.031(2) -0.007(2) 0.000(2) -0.011(2) O1 0.158(5) 0.108(3) 0.0260(18) -0.006(2) -0.004(3) 0.057(4) O2 0.106(4) 0.080(3) 0.036(2) 0.017(2) -0.005(2) 0.007(3) C19 0.060(4) 0.045(3) 0.032(3) 0.002(2) -0.002(3) -0.010(3) C6 0.066(4) 0.051(3) 0.033(3) 0.001(2) -0.003(3) 0.008(3) C7 0.067(4) 0.055(4) 0.031(3) -0.012(2) -0.004(3) 0.018(3) C15 0.033(3) 0.044(3) 0.033(3) -0.006(2) -0.005(2) 0.000(2) N2 0.051(3) 0.047(2) 0.0283(19) -0.002(2) -0.0001(18) 0.005(3) C16 0.050(4) 0.062(4) 0.040(3) -0.005(3) 0.000(3) -0.021(3) C2 0.045(3) 0.054(3) 0.025(2) -0.005(2) -0.005(2) 0.004(3) C4 0.048(4) 0.061(4) 0.035(3) -0.009(2) -0.006(3) 0.014(3) C3 0.069(4) 0.053(3) 0.034(3) 0.001(3) -0.009(3) 0.012(3) C5 0.035(3) 0.055(3) 0.026(2) -0.003(2) 0.003(2) 0.003(3) C18 0.041(3) 0.045(3) 0.039(3) -0.008(2) -0.010(3) 0.001(3) C25 0.064(4) 0.058(3) 0.034(3) -0.010(2) 0.000(3) 0.014(3) C22 0.054(4) 0.047(3) 0.030(2) -0.004(2) -0.007(3) 0.000(3) C17 0.046(4) 0.060(4) 0.046(3) -0.003(3) -0.006(3) -0.017(3) C21 0.049(4) 0.069(4) 0.041(3) -0.013(3) -0.005(3) 0.000(3) C26 0.045(3) 0.053(3) 0.029(3) -0.009(2) 0.002(3) 0.003(3) C24 0.063(4) 0.065(4) 0.051(3) -0.011(3) -0.006(3) 0.024(3) C23 0.054(4) 0.070(4) 0.056(3) -0.004(3) -0.017(3) 0.015(3) O4 0.145(5) 0.190(5) 0.045(2) -0.017(3) 0.023(3) -0.102(4) O5 0.067(4) 0.068(4) 0.067(4) -0.0004(10) 0.0000(10) -0.0002(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 N1 C12 1.323(6) . ? N1 C13 1.343(5) . ? N1 Zn1 2.067(4) 2_564 ? C13 C9 1.374(6) . ? C13 H13 0.9300 . ? C12 C11 1.363(7) . ? C12 H12 0.9300 . ? C11 C10 1.366(7) . ? C11 H11 0.9300 . ? C10 C9 1.373(7) . ? C10 H10 0.9300 . ? C9 C8 1.508(6) . ? C8 S1 1.783(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? O3 C14 1.244(6) . ? O3 Zn1 1.953(3) 4_567 ? C14 O4 1.220(6) . ? C14 C15 1.500(6) . ? Zn1 O1 1.906(3) . ? Zn1 O3 1.953(3) 4_467 ? Zn1 N1 2.067(4) 2_565 ? Zn1 N2 2.088(4) . ? Zn1 O5 2.306(15) . ? Zn1 C1 2.558(5) . ? S2 C18 1.759(5) . ? S2 C21 1.800(5) . ? S1 C5 1.756(4) . ? C1 O2 1.200(6) . ? C1 O1 1.266(6) . ? C1 C2 1.511(6) . ? C20 C15 1.388(6) . ? C20 C19 1.389(6) . ? C20 H20 0.9300 . ? C19 C18 1.387(7) . ? C19 H19 0.9300 . ? C6 C5 1.367(6) . ? C6 C7 1.387(6) . ? C6 H6 0.9300 . ? C7 C2 1.380(6) . ? C7 H7 0.9300 . ? C15 C16 1.366(6) . ? N2 C26 1.334(5) . ? N2 C25 1.349(6) . ? C16 C17 1.369(6) . ? C16 H16 0.9300 . ? C2 C3 1.369(6) . ? C4 C3 1.387(6) . ? C4 C5 1.396(6) . ? C4 H4 0.9300 . ? C3 H3 0.9300 . ? C18 C17 1.376(6) . ? C25 C24 1.361(7) . ? C25 H25 0.9300 . ? C22 C23 1.370(6) . ? C22 C26 1.379(6) . ? C22 C21 1.501(6) . ? C17 H17 0.9300 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C26 H26 0.9300 . ? C24 C23 1.377(6) . ? C24 H24 0.9300 . ? C23 H23 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 N1 C13 117.5(5) . . ? C12 N1 Zn1 126.4(3) . 2_564 ? C13 N1 Zn1 116.0(3) . 2_564 ? N1 C13 C9 124.2(5) . . ? N1 C13 H13 117.9 . . ? C9 C13 H13 117.9 . . ? N1 C12 C11 121.9(5) . . ? N1 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? C12 C11 C10 120.0(6) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C10 C9 119.6(6) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C9 C13 116.7(5) . . ? C10 C9 C8 123.6(5) . . ? C13 C9 C8 119.7(5) . . ? C9 C8 S1 106.5(3) . . ? C9 C8 H8A 110.4 . . ? S1 C8 H8A 110.4 . . ? C9 C8 H8B 110.4 . . ? S1 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? C14 O3 Zn1 138.9(3) . 4_567 ? O4 C14 O3 124.5(5) . . ? O4 C14 C15 119.3(5) . . ? O3 C14 C15 116.0(5) . . ? O1 Zn1 O3 116.95(17) . 4_467 ? O1 Zn1 N1 132.45(19) . 2_565 ? O3 Zn1 N1 94.96(15) 4_467 2_565 ? O1 Zn1 N2 115.93(19) . . ? O3 Zn1 N2 94.96(15) 4_467 . ? N1 Zn1 N2 93.57(16) 2_565 . ? O1 Zn1 O5 63.3(4) . . ? O3 Zn1 O5 90.7(4) 4_467 . ? N1 Zn1 O5 83.3(4) 2_565 . ? N2 Zn1 O5 173.8(4) . . ? O1 Zn1 C1 28.45(18) . . ? O3 Zn1 C1 145.38(19) 4_467 . ? N1 Zn1 C1 113.15(19) 2_565 . ? N2 Zn1 C1 102.66(17) . . ? O5 Zn1 C1 73.8(4) . . ? C18 S2 C21 106.1(2) . . ? C5 S1 C8 105.4(2) . . ? O2 C1 O1 121.9(5) . . ? O2 C1 C2 121.6(5) . . ? O1 C1 C2 116.5(5) . . ? O2 C1 Zn1 76.3(3) . . ? O1 C1 Zn1 45.8(2) . . ? C2 C1 Zn1 162.0(5) . . ? C15 C20 C19 121.1(4) . . ? C15 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C1 O1 Zn1 105.7(4) . . ? C18 C19 C20 120.0(4) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C5 C6 C7 120.8(5) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C2 C7 C6 119.7(5) . . ? C2 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C16 C15 C20 117.8(4) . . ? C16 C15 C14 122.3(4) . . ? C20 C15 C14 120.0(4) . . ? C26 N2 C25 117.0(4) . . ? C26 N2 Zn1 119.0(3) . . ? C25 N2 Zn1 121.6(3) . . ? C15 C16 C17 121.5(5) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C3 C2 C7 119.5(4) . . ? C3 C2 C1 119.1(5) . . ? C7 C2 C1 121.3(5) . . ? C3 C4 C5 118.7(4) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C2 C3 C4 121.4(5) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C6 C5 C4 119.9(4) . . ? C6 C5 S1 125.1(4) . . ? C4 C5 S1 115.0(4) . . ? C17 C18 C19 118.0(4) . . ? C17 C18 S2 118.0(4) . . ? C19 C18 S2 123.9(4) . . ? N2 C25 C24 122.1(4) . . ? N2 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? C23 C22 C26 117.5(4) . . ? C23 C22 C21 122.6(5) . . ? C26 C22 C21 119.8(5) . . ? C16 C17 C18 121.5(5) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C22 C21 S2 106.8(4) . . ? C22 C21 H21A 110.4 . . ? S2 C21 H21A 110.4 . . ? C22 C21 H21B 110.4 . . ? S2 C21 H21B 110.4 . . ? H21A C21 H21B 108.6 . . ? N2 C26 C22 124.2(5) . . ? N2 C26 H26 117.9 . . ? C22 C26 H26 117.9 . . ? C25 C24 C23 119.8(5) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C22 C23 C24 119.2(5) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.399 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.070 # Attachment '2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 643831' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H20 N2 O4 S2 Zn' _chemical_formula_weight 553.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.3416(19) _cell_length_b 20.947(4) _cell_length_c 12.521(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.04(3) _cell_angle_gamma 90.00 _cell_volume 2426.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4600 _cell_measurement_theta_min 1.9086 _cell_measurement_theta_max 27.8644 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 1.221 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7923 _exptl_absorpt_correction_T_max 0.7923 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 14744 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4266 _reflns_number_gt 3572 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+2.4052P] 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 geom _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0014(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4266 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1304 _refine_ls_wR_factor_gt 0.1226 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _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 0.73375(5) 0.13638(2) 0.94069(4) 0.0367(2) Uani 1 1 d . . . C1 C 0.5096(5) 0.2285(2) 0.9291(4) 0.0428(11) Uani 1 1 d . . . C2 C 0.3586(5) 0.2484(2) 0.8873(3) 0.0387(10) Uani 1 1 d . . . C3 C 0.3045(6) 0.3069(2) 0.9168(5) 0.0636(16) Uani 1 1 d . . . H3 H 0.3645 0.3352 0.9592 0.076 Uiso 1 1 calc R . . C4 C 0.1620(6) 0.3227(3) 0.8832(5) 0.0698(18) Uani 1 1 d . . . H4 H 0.1272 0.3618 0.9039 0.084 Uiso 1 1 calc R . . C5 C 0.0703(5) 0.2825(2) 0.8202(4) 0.0446(12) Uani 1 1 d . . . C6 C 0.1234(5) 0.2246(2) 0.7918(4) 0.0556(14) Uani 1 1 d . . . H6 H 0.0632 0.1962 0.7497 0.067 Uiso 1 1 calc R . . C7 C 0.2653(5) 0.2086(2) 0.8256(4) 0.0548(14) Uani 1 1 d . . . H7 H 0.2990 0.1691 0.8058 0.066 Uiso 1 1 calc R . . C8 C -0.1860(5) 0.2515(2) 0.6878(4) 0.0524(13) Uani 1 1 d . . . H8A H -0.1191 0.2449 0.6362 0.063 Uiso 1 1 calc R . . H8B H -0.2027 0.2107 0.7206 0.063 Uiso 1 1 calc R . . C9 C 0.7806(6) 0.0283(3) 1.0983(5) 0.0620(15) Uani 1 1 d . . . H9 H 0.8695 0.0259 1.0731 0.074 Uiso 1 1 calc R . . C10 C 0.7541(6) -0.0128(3) 1.1789(4) 0.0625(15) Uani 1 1 d . . . H10 H 0.8250 -0.0417 1.2073 0.075 Uiso 1 1 calc R . . C11 C 0.6239(5) -0.0115(2) 1.2176(4) 0.0442(11) Uani 1 1 d . . . C12 C 0.5269(6) 0.0329(3) 1.1727(5) 0.0729(18) Uani 1 1 d . . . H12 H 0.4372 0.0361 1.1964 0.087 Uiso 1 1 calc R . . C13 C 0.5603(6) 0.0730(3) 1.0930(5) 0.0689(17) Uani 1 1 d . . . H13 H 0.4915 0.1028 1.0645 0.083 Uiso 1 1 calc R . . C14 C 0.5842(6) -0.0580(2) 1.3002(4) 0.0530(13) Uani 1 1 d . . . H14A H 0.5203 -0.0897 1.2628 0.064 Uiso 1 1 calc R . . H14B H 0.5292 -0.0350 1.3480 0.064 Uiso 1 1 calc R . . C15 C 1.0401(5) 0.1443(2) 1.0206(4) 0.0519(13) Uani 1 1 d . . . H15 H 1.0395 0.1061 0.9829 0.062 Uiso 1 1 calc R . . C16 C 1.1678(5) 0.1656(2) 1.0759(4) 0.0532(13) Uani 1 1 d . . . H16 H 1.2513 0.1414 1.0761 0.064 Uiso 1 1 calc R . . C17 C 1.1741(5) 0.2226(2) 1.1314(4) 0.0409(11) Uani 1 1 d . . . C18 C 1.0456(5) 0.2546(2) 1.1300(4) 0.0546(14) Uani 1 1 d . . . H18 H 1.0436 0.2926 1.1681 0.066 Uiso 1 1 calc R . . C19 C 0.9194(5) 0.2313(2) 1.0730(4) 0.0498(13) Uani 1 1 d . . . H19 H 0.8344 0.2545 1.0724 0.060 Uiso 1 1 calc R . . C20 C 0.8324(5) 0.0500(2) 0.7977(4) 0.0414(11) Uani 1 1 d . . . C21 C 0.8205(5) 0.0177(2) 0.6904(3) 0.0377(10) Uani 1 1 d . . . C22 C 0.7569(6) 0.0466(2) 0.5970(4) 0.0532(14) Uani 1 1 d . . . H22 H 0.7305 0.0893 0.5985 0.064 Uiso 1 1 calc R . . C23 C 0.7313(7) 0.0134(2) 0.5009(4) 0.0623(16) Uani 1 1 d . . . H23 H 0.6891 0.0340 0.4386 0.075 Uiso 1 1 calc R . . C24 C 0.7679(5) -0.0501(2) 0.4968(4) 0.0439(11) Uani 1 1 d . . . C25 C 0.8390(6) -0.0789(2) 0.5892(4) 0.0492(12) Uani 1 1 d . . . H25 H 0.8696 -0.1211 0.5867 0.059 Uiso 1 1 calc R . . C26 C 0.8642(5) -0.0455(2) 0.6843(4) 0.0499(13) Uani 1 1 d . . . H26 H 0.9113 -0.0655 0.7457 0.060 Uiso 1 1 calc R . . N1 N 0.6855(4) 0.07151(18) 1.0544(3) 0.0434(9) Uani 1 1 d . . . N2 N 0.9159(4) 0.17644(18) 1.0187(3) 0.0376(9) Uani 1 1 d . . . O1 O 0.5500(4) 0.17565(17) 0.8929(3) 0.0599(10) Uani 1 1 d . . . O2 O 0.5843(4) 0.2599(2) 0.9972(4) 0.0923(15) Uani 1 1 d . . . O3 O 0.7668(4) 0.10393(15) 0.8000(2) 0.0478(8) Uani 1 1 d . . . O4 O 0.8995(4) 0.02484(18) 0.8777(3) 0.0641(11) Uani 1 1 d . . . S1 S -0.11054(14) 0.30678(7) 0.78952(12) 0.0640(4) Uani 1 1 d . . . S2 S 0.72909(18) -0.09945(6) 1.38234(10) 0.0605(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0231(3) 0.0458(3) 0.0381(3) -0.0073(2) -0.0063(2) 0.0044(2) C1 0.030(3) 0.052(3) 0.043(3) -0.001(2) -0.007(2) 0.005(2) C2 0.025(2) 0.046(3) 0.042(2) -0.002(2) -0.0067(18) 0.004(2) C3 0.046(3) 0.047(3) 0.087(4) -0.017(3) -0.026(3) 0.007(3) C4 0.046(3) 0.043(3) 0.110(5) -0.025(3) -0.027(3) 0.017(3) C5 0.031(3) 0.047(3) 0.051(3) -0.005(2) -0.010(2) 0.012(2) C6 0.037(3) 0.056(3) 0.066(3) -0.023(3) -0.020(2) 0.009(2) C7 0.032(3) 0.057(3) 0.070(3) -0.026(3) -0.015(2) 0.019(2) C8 0.031(3) 0.053(3) 0.067(3) 0.009(3) -0.015(2) 0.004(2) C9 0.042(3) 0.073(4) 0.073(4) 0.017(3) 0.018(3) 0.018(3) C10 0.050(3) 0.069(4) 0.070(4) 0.023(3) 0.011(3) 0.014(3) C11 0.043(3) 0.051(3) 0.038(3) -0.010(2) 0.003(2) -0.005(2) C12 0.040(3) 0.093(5) 0.092(4) 0.030(4) 0.029(3) 0.027(3) C13 0.046(3) 0.079(4) 0.086(4) 0.028(3) 0.024(3) 0.027(3) C14 0.056(3) 0.059(3) 0.043(3) -0.005(2) 0.004(2) -0.010(3) C15 0.030(3) 0.061(3) 0.061(3) -0.022(3) -0.007(2) 0.007(2) C16 0.023(2) 0.063(3) 0.070(3) -0.020(3) -0.008(2) 0.009(2) C17 0.025(2) 0.050(3) 0.045(3) -0.003(2) -0.0043(19) -0.003(2) C18 0.036(3) 0.048(3) 0.074(4) -0.027(3) -0.011(2) 0.001(2) C19 0.031(3) 0.050(3) 0.065(3) -0.014(3) -0.008(2) 0.003(2) C20 0.028(2) 0.051(3) 0.044(3) -0.012(2) -0.001(2) -0.002(2) C21 0.038(3) 0.040(3) 0.036(2) -0.007(2) 0.0071(19) 0.000(2) C22 0.085(4) 0.030(3) 0.043(3) -0.004(2) 0.003(3) 0.004(3) C23 0.108(5) 0.039(3) 0.038(3) 0.001(2) 0.004(3) 0.007(3) C24 0.057(3) 0.040(3) 0.036(3) -0.004(2) 0.012(2) -0.002(2) C25 0.058(3) 0.039(3) 0.047(3) -0.006(2) -0.003(2) 0.006(2) C26 0.058(3) 0.050(3) 0.038(3) 0.001(2) -0.004(2) 0.012(3) N1 0.031(2) 0.053(2) 0.045(2) -0.0015(19) 0.0005(17) 0.0065(18) N2 0.0239(19) 0.048(2) 0.039(2) -0.0053(17) -0.0025(15) 0.0006(17) O1 0.037(2) 0.066(2) 0.070(2) -0.0189(19) -0.0127(17) 0.0196(18) O2 0.044(2) 0.087(3) 0.131(4) -0.040(3) -0.040(2) 0.015(2) O3 0.055(2) 0.0444(19) 0.0428(18) -0.0124(15) 0.0028(15) 0.0068(17) O4 0.067(3) 0.078(3) 0.043(2) -0.0117(18) -0.0097(18) 0.024(2) S1 0.0351(7) 0.0784(10) 0.0713(9) -0.0198(8) -0.0173(6) 0.0247(7) S2 0.0893(11) 0.0465(8) 0.0419(7) -0.0099(6) -0.0040(7) 0.0025(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.922(3) . ? Zn1 O3 1.953(3) . ? Zn1 N2 2.022(3) . ? Zn1 N1 2.063(4) . ? C1 O2 1.216(6) . ? C1 O1 1.273(5) . ? C1 C2 1.494(6) . ? C2 C7 1.366(6) . ? C2 C3 1.393(6) . ? C3 C4 1.380(7) . ? C3 H3 0.9300 . ? C4 C5 1.370(7) . ? C4 H4 0.9300 . ? C5 C6 1.376(6) . ? C5 S1 1.755(4) . ? C6 C7 1.375(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C17 1.498(6) 4_465 ? C8 S1 1.792(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N1 1.331(6) . ? C9 C10 1.376(7) . ? C9 H9 0.9300 . ? C10 C11 1.371(7) . ? C10 H10 0.9300 . ? C11 C12 1.363(7) . ? C11 C14 1.505(7) . ? C12 C13 1.373(7) . ? C12 H12 0.9300 . ? C13 N1 1.327(6) . ? C13 H13 0.9300 . ? C14 S2 1.804(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N2 1.339(6) . ? C15 C16 1.367(6) . ? C15 H15 0.9300 . ? C16 C17 1.378(6) . ? C16 H16 0.9300 . ? C17 C18 1.373(6) . ? C17 C8 1.498(6) 4_766 ? C18 C19 1.379(6) . ? C18 H18 0.9300 . ? C19 N2 1.333(6) . ? C19 H19 0.9300 . ? C20 O4 1.223(5) . ? C20 O3 1.287(5) . ? C20 C21 1.495(6) . ? C21 C22 1.376(6) . ? C21 C26 1.391(6) . ? C22 C23 1.382(7) . ? C22 H22 0.9300 . ? C23 C24 1.375(6) . ? C23 H23 0.9300 . ? C24 C25 1.389(6) . ? C24 S2 1.763(4) 1_554 ? C25 C26 1.373(6) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? S2 C24 1.763(5) 1_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O3 96.64(15) . . ? O1 Zn1 N2 128.85(15) . . ? O3 Zn1 N2 110.59(14) . . ? O1 Zn1 N1 102.98(16) . . ? O3 Zn1 N1 118.08(14) . . ? N2 Zn1 N1 100.97(15) . . ? O2 C1 O1 123.4(4) . . ? O2 C1 C2 121.0(4) . . ? O1 C1 C2 115.5(4) . . ? C7 C2 C3 117.4(4) . . ? C7 C2 C1 121.6(4) . . ? C3 C2 C1 120.8(4) . . ? C4 C3 C2 120.1(5) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 121.7(5) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 118.2(4) . . ? C4 C5 S1 116.9(4) . . ? C6 C5 S1 124.8(4) . . ? C7 C6 C5 120.1(4) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C2 C7 C6 122.4(4) . . ? C2 C7 H7 118.8 . . ? C6 C7 H7 118.8 . . ? C17 C8 S1 109.3(3) 4_465 . ? C17 C8 H8A 109.8 4_465 . ? S1 C8 H8A 109.8 . . ? C17 C8 H8B 109.8 4_465 . ? S1 C8 H8B 109.8 . . ? H8A C8 H8B 108.3 . . ? N1 C9 C10 123.4(5) . . ? N1 C9 H9 118.3 . . ? C10 C9 H9 118.3 . . ? C11 C10 C9 120.4(5) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 C10 116.1(5) . . ? C12 C11 C14 120.7(5) . . ? C10 C11 C14 123.1(5) . . ? C11 C12 C13 120.7(5) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? N1 C13 C12 123.5(5) . . ? N1 C13 H13 118.3 . . ? C12 C13 H13 118.3 . . ? C11 C14 S2 117.8(4) . . ? C11 C14 H14A 107.9 . . ? S2 C14 H14A 107.9 . . ? C11 C14 H14B 107.9 . . ? S2 C14 H14B 107.9 . . ? H14A C14 H14B 107.2 . . ? N2 C15 C16 122.6(5) . . ? N2 C15 H15 118.7 . . ? C16 C15 H15 118.7 . . ? C15 C16 C17 120.7(5) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C18 C17 C16 116.2(4) . . ? C18 C17 C8 122.1(4) . 4_766 ? C16 C17 C8 121.7(4) . 4_766 ? C17 C18 C19 121.1(4) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? N2 C19 C18 121.8(4) . . ? N2 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? O4 C20 O3 123.5(4) . . ? O4 C20 C21 120.4(4) . . ? O3 C20 C21 116.2(4) . . ? C22 C21 C26 117.8(4) . . ? C22 C21 C20 122.3(4) . . ? C26 C21 C20 119.6(4) . . ? C21 C22 C23 121.4(4) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C24 C23 C22 120.3(5) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 118.8(4) . . ? C23 C24 S2 124.9(4) . 1_554 ? C25 C24 S2 116.2(4) . 1_554 ? C26 C25 C24 120.3(4) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C21 121.1(4) . . ? C25 C26 H26 119.4 . . ? C21 C26 H26 119.4 . . ? C13 N1 C9 115.9(4) . . ? C13 N1 Zn1 121.6(3) . . ? C9 N1 Zn1 122.3(3) . . ? C19 N2 C15 117.7(4) . . ? C19 N2 Zn1 124.3(3) . . ? C15 N2 Zn1 118.0(3) . . ? C1 O1 Zn1 123.9(3) . . ? C20 O3 Zn1 117.5(3) . . ? C5 S1 C8 103.8(2) . . ? C24 S2 C14 103.5(2) 1_556 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.450 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.068 # Attachment '1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 647989' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H60 N6 O12 S6 Zn3' _chemical_formula_weight 1661.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.382(2) _cell_length_b 12.958(3) _cell_length_c 15.276(3) _cell_angle_alpha 105.77(3) _cell_angle_beta 107.50(3) _cell_angle_gamma 101.88(3) _cell_volume 1791.2(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6236 _cell_measurement_theta_min 1.8321 _cell_measurement_theta_max 27.8884 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 1.240 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7895 _exptl_absorpt_correction_T_max 0.7895 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 18526 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0399 _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 -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6329 _reflns_number_gt 5817 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+0.6297P] 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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6329 _refine_ls_number_parameters 475 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.002 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 0.22398(3) 0.10077(2) 0.462959(18) 0.01383(8) Uani 1 1 d . . . Zn2 Zn 0.5000 0.0000 0.5000 0.01210(9) Uani 1 2 d S . . S1 S 0.19382(7) -0.42250(5) -0.03150(5) 0.02912(16) Uani 1 1 d . . . S2 S 0.29847(7) -0.08204(5) 0.97884(4) 0.02519(15) Uani 1 1 d . . . S3 S 0.96897(6) 0.69991(5) 0.75209(4) 0.01967(14) Uani 1 1 d . . . N1 N 0.4066(2) -0.53968(18) -0.14884(16) 0.0332(5) Uani 1 1 d . . . N2 N 0.07354(19) 0.18261(15) 0.47111(14) 0.0164(4) Uani 1 1 d . . . N3 N 0.2108(2) 0.17393(18) 1.03743(15) 0.0313(5) Uani 1 1 d . . . O1 O 0.32808(16) 0.00955(12) 0.38393(11) 0.0165(3) Uani 1 1 d . . . O2 O 0.09612(17) -0.04226(13) 0.32649(11) 0.0223(4) Uani 1 1 d . . . O3 O 0.23252(16) 0.05800(13) 0.57668(11) 0.0191(4) Uani 1 1 d . . . O4 O 0.38420(15) 0.24237(12) 0.49846(11) 0.0155(3) Uani 1 1 d . . . O5 O 0.63216(16) 0.05523(12) 0.43622(11) 0.0181(4) Uani 1 1 d . . . O6 O 0.46494(16) -0.16694(12) 0.42103(10) 0.0161(3) Uani 1 1 d . . . C1 C 0.2080(2) -0.05629(18) 0.31798(16) 0.0165(5) Uani 1 1 d . . . C2 C 0.2052(2) -0.14536(18) 0.23134(16) 0.0156(5) Uani 1 1 d . . . C3 C 0.0781(2) -0.22563(19) 0.16192(17) 0.0211(5) Uani 1 1 d . . . H3 H -0.0075 -0.2238 0.1689 0.025 Uiso 1 1 calc R . . C4 C 0.0790(3) -0.3082(2) 0.08261(17) 0.0233(5) Uani 1 1 d . . . H4 H -0.0062 -0.3618 0.0368 0.028 Uiso 1 1 calc R . . C5 C 0.2061(3) -0.31161(19) 0.07083(16) 0.0203(5) Uani 1 1 d . . . C6 C 0.3330(2) -0.23033(18) 0.13908(16) 0.0169(5) Uani 1 1 d . . . H6 H 0.4184 -0.2313 0.1316 0.020 Uiso 1 1 calc R . . C7 C 0.3315(2) -0.14782(18) 0.21839(16) 0.0151(5) Uani 1 1 d . . . H7 H 0.4164 -0.0933 0.2636 0.018 Uiso 1 1 calc R . . C8 C 0.3674(3) -0.3856(2) -0.03951(18) 0.0267(6) Uani 1 1 d . . . H8A H 0.4008 -0.3056 -0.0280 0.032 Uiso 1 1 calc R . . H8B H 0.4357 -0.4023 0.0094 0.032 Uiso 1 1 calc R . . C9 C 0.3513(3) -0.4549(2) -0.14189(18) 0.0236(6) Uani 1 1 d . . . C10 C 0.2831(3) -0.4285(2) -0.22164(18) 0.0268(6) Uani 1 1 d . . . H10 H 0.2441 -0.3698 -0.2136 0.032 Uiso 1 1 calc R . . C11 C 0.2741(3) -0.4914(2) -0.31395(19) 0.0308(6) Uani 1 1 d . . . H11 H 0.2305 -0.4747 -0.3688 0.037 Uiso 1 1 calc R . . C12 C 0.3310(3) -0.5790(2) -0.32286(19) 0.0309(6) Uani 1 1 d . . . H12 H 0.3268 -0.6227 -0.3837 0.037 Uiso 1 1 calc R . . C13 C 0.3939(3) -0.6001(2) -0.23967(19) 0.0359(7) Uani 1 1 d . . . H13 H 0.4303 -0.6604 -0.2465 0.043 Uiso 1 1 calc R . . C14 C 0.0329(2) 0.24171(18) 0.41305(16) 0.0159(5) Uani 1 1 d . . . C15 C -0.0450(2) 0.31265(19) 0.43334(18) 0.0223(5) Uani 1 1 d . . . H15 H -0.0683 0.3555 0.3946 0.027 Uiso 1 1 calc R . . C16 C -0.0884(3) 0.3202(2) 0.51138(19) 0.0262(6) Uani 1 1 d . . . H16 H -0.1408 0.3680 0.5257 0.031 Uiso 1 1 calc R . . C17 C -0.0527(3) 0.2558(2) 0.56770(19) 0.0255(6) Uani 1 1 d . . . H17 H -0.0834 0.2572 0.6192 0.031 Uiso 1 1 calc R . . C18 C 0.0294(2) 0.18912(19) 0.54605(18) 0.0207(5) Uani 1 1 d . . . H18 H 0.0553 0.1469 0.5849 0.025 Uiso 1 1 calc R . . C19 C 0.2993(2) -0.00636(18) 0.60581(16) 0.0162(5) Uani 1 1 d . . . C20 C 0.2942(2) -0.02298(18) 0.69765(16) 0.0158(5) Uani 1 1 d . . . C21 C 0.2308(2) 0.0356(2) 0.75293(17) 0.0206(5) Uani 1 1 d . . . H21 H 0.1879 0.0852 0.7315 0.025 Uiso 1 1 calc R . . C22 C 0.2297(2) 0.0218(2) 0.83963(17) 0.0210(5) Uani 1 1 d . . . H22 H 0.1878 0.0627 0.8763 0.025 Uiso 1 1 calc R . . C23 C 0.2921(2) -0.05378(19) 0.87150(16) 0.0185(5) Uani 1 1 d . . . C24 C 0.3575(3) -0.11206(19) 0.81645(17) 0.0215(5) Uani 1 1 d . . . H24 H 0.4009 -0.1615 0.8379 0.026 Uiso 1 1 calc R . . C25 C 0.3587(2) -0.09719(19) 0.73078(17) 0.0187(5) Uani 1 1 d . . . H25 H 0.4025 -0.1367 0.6948 0.022 Uiso 1 1 calc R . . C26 C 0.1686(3) -0.0250(2) 1.01559(17) 0.0257(6) Uani 1 1 d . . . H26A H 0.0902 -0.0340 0.9571 0.031 Uiso 1 1 calc R . . H26B H 0.1310 -0.0682 1.0503 0.031 Uiso 1 1 calc R . . C27 C 0.2302(2) 0.0986(2) 1.08092(17) 0.0221(5) Uani 1 1 d . . . C28 C 0.3059(3) 0.1307(2) 1.18112(18) 0.0258(6) Uani 1 1 d . . . H28 H 0.3151 0.0763 1.2096 0.031 Uiso 1 1 calc R . . C29 C 0.3673(3) 0.2440(2) 1.23805(19) 0.0304(6) Uani 1 1 d . . . H29 H 0.4182 0.2670 1.3053 0.037 Uiso 1 1 calc R . . C30 C 0.3520(3) 0.3223(2) 1.1936(2) 0.0327(6) Uani 1 1 d . . . H30 H 0.3940 0.3992 1.2296 0.039 Uiso 1 1 calc R . . C31 C 0.2721(3) 0.2834(2) 1.0936(2) 0.0352(7) Uani 1 1 d . . . H31 H 0.2604 0.3364 1.0639 0.042 Uiso 1 1 calc R . . C32 C 0.5060(2) 0.24675(18) 0.55468(15) 0.0141(5) Uani 1 1 d . . . C33 C 0.6223(2) 0.35795(18) 0.59857(16) 0.0138(5) Uani 1 1 d . . . C34 C 0.7344(2) 0.38361(18) 0.68689(16) 0.0155(5) Uani 1 1 d . . . H34 H 0.7387 0.3304 0.7171 0.019 Uiso 1 1 calc R . . C35 C 0.8395(2) 0.48702(18) 0.73015(17) 0.0179(5) Uani 1 1 d . . . H35 H 0.9135 0.5030 0.7893 0.021 Uiso 1 1 calc R . . C36 C 0.8351(2) 0.56789(18) 0.68555(16) 0.0150(5) Uani 1 1 d . . . C37 C 0.7257(2) 0.54125(18) 0.59538(16) 0.0164(5) Uani 1 1 d . . . H37 H 0.7238 0.5930 0.5635 0.020 Uiso 1 1 calc R . . C38 C 0.6196(2) 0.43772(18) 0.55332(16) 0.0153(5) Uani 1 1 d . . . H38 H 0.5457 0.4214 0.4940 0.018 Uiso 1 1 calc R . . C39 C 0.9252(2) 0.78090(18) 0.67538(16) 0.0168(5) Uani 1 1 d . . . H39A H 0.8232 0.7672 0.6523 0.020 Uiso 1 1 calc R . . H39B H 0.9703 0.8603 0.7157 0.020 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 0.01520(14) 0.01412(15) 0.01660(15) 0.00716(11) 0.00849(12) 0.00755(11) Zn2 0.01403(19) 0.01134(19) 0.01425(19) 0.00525(15) 0.00766(16) 0.00625(15) S1 0.0287(4) 0.0257(4) 0.0220(3) -0.0045(3) 0.0114(3) 0.0011(3) S2 0.0341(4) 0.0280(4) 0.0181(3) 0.0123(3) 0.0117(3) 0.0106(3) S3 0.0191(3) 0.0162(3) 0.0193(3) 0.0079(2) 0.0017(3) 0.0027(2) N1 0.0441(14) 0.0314(13) 0.0296(13) 0.0096(10) 0.0156(11) 0.0221(11) N2 0.0135(10) 0.0142(10) 0.0230(11) 0.0073(8) 0.0086(9) 0.0041(8) N3 0.0383(14) 0.0344(14) 0.0277(12) 0.0133(11) 0.0170(11) 0.0145(11) O1 0.0203(9) 0.0137(8) 0.0145(8) 0.0046(7) 0.0052(7) 0.0060(7) O2 0.0208(9) 0.0249(9) 0.0238(9) 0.0061(7) 0.0113(8) 0.0118(7) O3 0.0223(9) 0.0246(9) 0.0209(9) 0.0142(7) 0.0127(7) 0.0137(7) O4 0.0145(8) 0.0136(8) 0.0192(8) 0.0057(7) 0.0066(7) 0.0060(6) O5 0.0223(9) 0.0177(9) 0.0251(9) 0.0124(7) 0.0165(8) 0.0104(7) O6 0.0230(9) 0.0113(8) 0.0149(8) 0.0051(7) 0.0067(7) 0.0074(7) C1 0.0240(13) 0.0154(12) 0.0170(12) 0.0115(10) 0.0096(11) 0.0096(10) C2 0.0200(12) 0.0152(12) 0.0135(11) 0.0076(10) 0.0051(10) 0.0077(10) C3 0.0181(13) 0.0245(13) 0.0212(13) 0.0087(11) 0.0076(11) 0.0068(10) C4 0.0195(13) 0.0228(13) 0.0177(13) 0.0023(10) 0.0023(11) 0.0004(10) C5 0.0272(14) 0.0191(13) 0.0148(12) 0.0056(10) 0.0089(11) 0.0068(10) C6 0.0194(12) 0.0195(12) 0.0152(12) 0.0078(10) 0.0087(10) 0.0073(10) C7 0.0175(12) 0.0147(12) 0.0124(11) 0.0069(9) 0.0040(10) 0.0031(9) C8 0.0271(14) 0.0275(14) 0.0236(14) 0.0038(11) 0.0114(12) 0.0096(11) C9 0.0231(13) 0.0230(14) 0.0228(13) 0.0044(11) 0.0088(11) 0.0083(11) C10 0.0263(14) 0.0284(14) 0.0251(14) 0.0051(11) 0.0097(12) 0.0131(12) C11 0.0281(15) 0.0407(17) 0.0225(14) 0.0079(12) 0.0080(12) 0.0159(13) C12 0.0302(15) 0.0316(15) 0.0239(14) -0.0013(12) 0.0108(12) 0.0099(12) C13 0.0495(19) 0.0318(16) 0.0327(16) 0.0067(13) 0.0194(15) 0.0257(14) C14 0.0122(11) 0.0112(11) 0.0209(12) 0.0046(10) 0.0044(10) 0.0009(9) C15 0.0210(13) 0.0196(13) 0.0320(14) 0.0134(11) 0.0112(12) 0.0106(10) C16 0.0226(13) 0.0222(14) 0.0423(16) 0.0122(12) 0.0179(12) 0.0148(11) C17 0.0241(14) 0.0286(14) 0.0349(15) 0.0145(12) 0.0204(12) 0.0127(11) C18 0.0207(13) 0.0207(13) 0.0275(13) 0.0126(11) 0.0130(11) 0.0087(10) C19 0.0125(11) 0.0148(12) 0.0215(12) 0.0072(10) 0.0075(10) 0.0017(9) C20 0.0125(11) 0.0164(12) 0.0172(12) 0.0066(10) 0.0056(10) 0.0014(9) C21 0.0171(12) 0.0266(14) 0.0228(13) 0.0116(11) 0.0088(11) 0.0107(10) C22 0.0212(13) 0.0276(14) 0.0181(12) 0.0091(11) 0.0109(11) 0.0091(11) C23 0.0169(12) 0.0206(13) 0.0143(12) 0.0066(10) 0.0041(10) 0.0004(10) C24 0.0248(13) 0.0191(13) 0.0234(13) 0.0123(11) 0.0077(11) 0.0087(11) C25 0.0196(12) 0.0189(12) 0.0203(13) 0.0081(10) 0.0089(11) 0.0076(10) C26 0.0250(14) 0.0329(15) 0.0208(13) 0.0113(11) 0.0119(12) 0.0054(11) C27 0.0200(13) 0.0286(14) 0.0231(13) 0.0110(11) 0.0140(11) 0.0069(11) C28 0.0257(14) 0.0316(15) 0.0245(14) 0.0123(12) 0.0119(12) 0.0113(12) C29 0.0266(15) 0.0382(16) 0.0239(14) 0.0045(12) 0.0096(12) 0.0139(13) C30 0.0298(15) 0.0275(15) 0.0409(17) 0.0049(13) 0.0192(14) 0.0102(12) C31 0.0427(17) 0.0333(16) 0.0430(18) 0.0187(14) 0.0254(15) 0.0184(14) C32 0.0192(12) 0.0142(12) 0.0120(11) 0.0030(9) 0.0104(10) 0.0072(10) C33 0.0156(12) 0.0129(11) 0.0170(12) 0.0041(9) 0.0100(10) 0.0084(9) C34 0.0212(12) 0.0151(12) 0.0179(12) 0.0109(10) 0.0107(11) 0.0098(10) C35 0.0161(12) 0.0194(13) 0.0169(12) 0.0074(10) 0.0024(10) 0.0071(10) C36 0.0148(11) 0.0135(12) 0.0166(12) 0.0045(10) 0.0058(10) 0.0055(9) C37 0.0179(12) 0.0156(12) 0.0205(12) 0.0091(10) 0.0095(10) 0.0079(10) C38 0.0137(11) 0.0173(12) 0.0150(11) 0.0051(10) 0.0042(10) 0.0080(9) C39 0.0187(12) 0.0105(11) 0.0214(12) 0.0068(10) 0.0060(10) 0.0061(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 Zn1 O3 1.9451(15) . ? Zn1 O4 2.0219(17) . ? Zn1 N2 2.0753(19) . ? Zn1 O1 2.1347(16) . ? Zn1 O2 2.183(2) . ? Zn1 C1 2.503(2) . ? Zn2 O5 2.0305(15) 2_656 ? Zn2 O5 2.0305(15) . ? Zn2 O6 2.0640(16) 2_656 ? Zn2 O6 2.0640(16) . ? Zn2 O1 2.1569(17) 2_656 ? Zn2 O1 2.1569(17) . ? S1 C5 1.763(2) . ? S1 C8 1.817(3) . ? S2 C23 1.760(2) . ? S2 C26 1.822(2) . ? S3 C36 1.766(2) . ? S3 C39 1.796(2) . ? N1 C9 1.335(3) . ? N1 C13 1.346(3) . ? N2 C18 1.344(3) . ? N2 C14 1.352(3) . ? N3 C27 1.337(3) . ? N3 C31 1.338(3) . ? O1 C1 1.279(3) . ? O2 C1 1.251(3) . ? O3 C19 1.276(3) . ? O4 C32 1.277(3) . ? O5 C19 1.249(3) 2_656 ? O6 C32 1.252(2) 2_656 ? C1 C2 1.489(3) . ? C2 C7 1.389(3) . ? C2 C3 1.393(3) . ? C3 C4 1.385(3) . ? C3 H3 0.9300 . ? C4 C5 1.393(3) . ? C4 H4 0.9300 . ? C5 C6 1.392(3) . ? C6 C7 1.387(3) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.516(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.382(3) . ? C10 C11 1.388(3) . ? C10 H10 0.9300 . ? C11 C12 1.377(4) . ? C11 H11 0.9300 . ? C12 C13 1.371(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.377(3) . ? C14 C39 1.513(3) 2_666 ? C15 C16 1.383(3) . ? C15 H15 0.9300 . ? C16 C17 1.379(3) . ? C16 H16 0.9300 . ? C17 C18 1.378(3) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 O5 1.249(3) 2_656 ? C19 C20 1.490(3) . ? C20 C21 1.383(3) . ? C20 C25 1.398(3) . ? C21 C22 1.386(3) . ? C21 H21 0.9300 . ? C22 C23 1.395(3) . ? C22 H22 0.9300 . ? C23 C24 1.396(3) . ? C24 C25 1.377(3) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.516(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.389(3) . ? C28 C29 1.381(4) . ? C28 H28 0.9300 . ? C29 C30 1.375(4) . ? C29 H29 0.9300 . ? C30 C31 1.387(4) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 O6 1.252(2) 2_656 ? C32 C33 1.502(3) . ? C33 C38 1.391(3) . ? C33 C34 1.392(3) . ? C34 C35 1.380(3) . ? C34 H34 0.9300 . ? C35 C36 1.398(3) . ? C35 H35 0.9300 . ? C36 C37 1.395(3) . ? C37 C38 1.387(3) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C14 1.513(3) 2_666 ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O4 111.46(7) . . ? O3 Zn1 N2 95.36(7) . . ? O4 Zn1 N2 95.25(7) . . ? O3 Zn1 O1 109.08(6) . . ? O4 Zn1 O1 87.67(6) . . ? N2 Zn1 O1 152.43(7) . . ? O3 Zn1 O2 110.97(7) . . ? O4 Zn1 O2 133.38(7) . . ? N2 Zn1 O2 99.19(7) . . ? O1 Zn1 O2 60.72(6) . . ? O3 Zn1 C1 113.52(7) . . ? O4 Zn1 C1 112.20(7) . . ? N2 Zn1 C1 126.91(8) . . ? O1 Zn1 C1 30.74(7) . . ? O2 Zn1 C1 29.98(7) . . ? O5 Zn2 O5 180.0 2_656 . ? O5 Zn2 O6 92.12(7) 2_656 2_656 ? O5 Zn2 O6 87.88(7) . 2_656 ? O5 Zn2 O6 87.88(7) 2_656 . ? O5 Zn2 O6 92.12(7) . . ? O6 Zn2 O6 180.00(4) 2_656 . ? O5 Zn2 O1 87.63(6) 2_656 2_656 ? O5 Zn2 O1 92.37(6) . 2_656 ? O6 Zn2 O1 91.39(7) 2_656 2_656 ? O6 Zn2 O1 88.61(7) . 2_656 ? O5 Zn2 O1 92.37(6) 2_656 . ? O5 Zn2 O1 87.63(6) . . ? O6 Zn2 O1 88.61(7) 2_656 . ? O6 Zn2 O1 91.39(7) . . ? O1 Zn2 O1 180.0 2_656 . ? C5 S1 C8 104.78(12) . . ? C23 S2 C26 105.00(11) . . ? C36 S3 C39 103.06(11) . . ? C9 N1 C13 116.2(2) . . ? C18 N2 C14 118.68(19) . . ? C18 N2 Zn1 117.71(15) . . ? C14 N2 Zn1 123.00(15) . . ? C27 N3 C31 117.4(2) . . ? C1 O1 Zn1 90.73(13) . . ? C1 O1 Zn2 137.73(14) . . ? Zn1 O1 Zn2 102.51(7) . . ? C1 O2 Zn1 89.31(14) . . ? C19 O3 Zn1 126.55(14) . . ? C32 O4 Zn1 115.32(14) . . ? C19 O5 Zn2 130.71(14) 2_656 . ? C32 O6 Zn2 133.09(14) 2_656 . ? O2 C1 O1 119.2(2) . . ? O2 C1 C2 121.7(2) . . ? O1 C1 C2 119.1(2) . . ? O2 C1 Zn1 60.71(12) . . ? O1 C1 Zn1 58.53(11) . . ? C2 C1 Zn1 176.81(16) . . ? C7 C2 C3 119.1(2) . . ? C7 C2 C1 119.5(2) . . ? C3 C2 C1 121.4(2) . . ? C4 C3 C2 120.1(2) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.6(2) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C4 C5 C6 119.4(2) . . ? C4 C5 S1 116.36(19) . . ? C6 C5 S1 124.25(19) . . ? C7 C6 C5 119.7(2) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C2 121.0(2) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? C9 C8 S1 107.41(17) . . ? C9 C8 H8A 110.2 . . ? S1 C8 H8A 110.2 . . ? C9 C8 H8B 110.2 . . ? S1 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? N1 C9 C10 123.5(2) . . ? N1 C9 C8 116.3(2) . . ? C10 C9 C8 120.1(2) . . ? C9 C10 C11 118.7(2) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C12 C11 C10 118.8(2) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C13 C12 C11 118.2(2) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? N1 C13 C12 124.6(2) . . ? N1 C13 H13 117.7 . . ? C12 C13 H13 117.7 . . ? N2 C14 C15 121.0(2) . . ? N2 C14 C39 114.58(19) . 2_666 ? C15 C14 C39 124.4(2) . 2_666 ? C14 C15 C16 119.9(2) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 119.0(2) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C16 C17 C18 118.5(2) . . ? C16 C17 H17 120.7 . . ? C18 C17 H17 120.7 . . ? N2 C18 C17 122.7(2) . . ? N2 C18 H18 118.6 . . ? C17 C18 H18 118.6 . . ? O5 C19 O3 125.2(2) 2_656 . ? O5 C19 C20 118.36(19) 2_656 . ? O3 C19 C20 116.47(19) . . ? C21 C20 C25 118.8(2) . . ? C21 C20 C19 121.8(2) . . ? C25 C20 C19 119.4(2) . . ? C20 C21 C22 121.5(2) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C21 C22 C23 119.5(2) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C22 C23 C24 119.1(2) . . ? C22 C23 S2 125.26(18) . . ? C24 C23 S2 115.59(17) . . ? C25 C24 C23 120.8(2) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C20 120.3(2) . . ? C24 C25 H25 119.9 . . ? C20 C25 H25 119.9 . . ? C27 C26 S2 113.02(17) . . ? C27 C26 H26A 109.0 . . ? S2 C26 H26A 109.0 . . ? C27 C26 H26B 109.0 . . ? S2 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? N3 C27 C28 122.3(2) . . ? N3 C27 C26 117.1(2) . . ? C28 C27 C26 120.6(2) . . ? C29 C28 C27 119.4(2) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C30 C29 C28 118.9(3) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? C29 C30 C31 118.1(3) . . ? C29 C30 H30 120.9 . . ? C31 C30 H30 120.9 . . ? N3 C31 C30 123.8(3) . . ? N3 C31 H31 118.1 . . ? C30 C31 H31 118.1 . . ? O6 C32 O4 125.3(2) 2_656 . ? O6 C32 C33 117.30(19) 2_656 . ? O4 C32 C33 117.37(19) . . ? C38 C33 C34 118.7(2) . . ? C38 C33 C32 121.2(2) . . ? C34 C33 C32 120.08(19) . . ? C35 C34 C33 120.9(2) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C36 120.3(2) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C37 C36 C35 119.0(2) . . ? C37 C36 S3 124.97(17) . . ? C35 C36 S3 115.94(17) . . ? C38 C37 C36 120.1(2) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C33 120.9(2) . . ? C37 C38 H38 119.5 . . ? C33 C38 H38 119.5 . . ? C14 C39 S3 116.60(15) 2_666 . ? C14 C39 H39A 108.1 2_666 . ? S3 C39 H39A 108.1 . . ? C14 C39 H39B 108.1 2_666 . ? S3 C39 H39B 108.1 . . ? H39A C39 H39B 107.3 . . ? 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 O3 Zn1 N2 C18 2.47(17) . . . . ? O4 Zn1 N2 C18 -109.72(17) . . . . ? O1 Zn1 N2 C18 155.23(15) . . . . ? O2 Zn1 N2 C18 114.76(17) . . . . ? C1 Zn1 N2 C18 127.35(16) . . . . ? O3 Zn1 N2 C14 173.47(17) . . . . ? O4 Zn1 N2 C14 61.28(18) . . . . ? O1 Zn1 N2 C14 -33.8(3) . . . . ? O2 Zn1 N2 C14 -74.25(17) . . . . ? C1 Zn1 N2 C14 -61.66(19) . . . . ? O3 Zn1 O1 C1 104.16(13) . . . . ? O4 Zn1 O1 C1 -143.91(12) . . . . ? N2 Zn1 O1 C1 -47.0(2) . . . . ? O2 Zn1 O1 C1 0.26(12) . . . . ? O3 Zn1 O1 Zn2 -35.38(8) . . . . ? O4 Zn1 O1 Zn2 76.55(7) . . . . ? N2 Zn1 O1 Zn2 173.45(11) . . . . ? O2 Zn1 O1 Zn2 -139.28(8) . . . . ? C1 Zn1 O1 Zn2 -139.54(14) . . . . ? O5 Zn2 O1 C1 -56.1(2) 2_656 . . . ? O5 Zn2 O1 C1 123.9(2) . . . . ? O6 Zn2 O1 C1 -148.2(2) 2_656 . . . ? O6 Zn2 O1 C1 31.8(2) . . . . ? O1 Zn2 O1 C1 35(100) 2_656 . . . ? O5 Zn2 O1 Zn1 49.19(7) 2_656 . . . ? O5 Zn2 O1 Zn1 -130.81(7) . . . . ? O6 Zn2 O1 Zn1 -42.87(7) 2_656 . . . ? O6 Zn2 O1 Zn1 137.13(7) . . . . ? O1 Zn2 O1 Zn1 141(100) 2_656 . . . ? O3 Zn1 O2 C1 -101.01(13) . . . . ? O4 Zn1 O2 C1 53.30(15) . . . . ? N2 Zn1 O2 C1 159.59(13) . . . . ? O1 Zn1 O2 C1 -0.27(12) . . . . ? O4 Zn1 O3 C19 -89.55(18) . . . . ? N2 Zn1 O3 C19 172.65(18) . . . . ? O1 Zn1 O3 C19 5.61(19) . . . . ? O2 Zn1 O3 C19 70.67(18) . . . . ? C1 Zn1 O3 C19 38.3(2) . . . . ? O3 Zn1 O4 C32 43.20(15) . . . . ? N2 Zn1 O4 C32 141.07(14) . . . . ? O1 Zn1 O4 C32 -66.41(14) . . . . ? O2 Zn1 O4 C32 -111.03(15) . . . . ? C1 Zn1 O4 C32 -85.39(15) . . . . ? O5 Zn2 O5 C19 88(100) 2_656 . . 2_656 ? O6 Zn2 O5 C19 158.74(19) 2_656 . . 2_656 ? O6 Zn2 O5 C19 -21.26(19) . . . 2_656 ? O1 Zn2 O5 C19 67.4(2) 2_656 . . 2_656 ? O1 Zn2 O5 C19 -112.6(2) . . . 2_656 ? O5 Zn2 O6 C32 -64.89(19) 2_656 . . 2_656 ? O5 Zn2 O6 C32 115.11(19) . . . 2_656 ? O6 Zn2 O6 C32 59(100) 2_656 . . 2_656 ? O1 Zn2 O6 C32 22.79(19) 2_656 . . 2_656 ? O1 Zn2 O6 C32 -157.21(19) . . . 2_656 ? Zn1 O2 C1 O1 0.4(2) . . . . ? Zn1 O2 C1 C2 -177.54(18) . . . . ? Zn1 O1 C1 O2 -0.5(2) . . . . ? Zn2 O1 C1 O2 109.2(2) . . . . ? Zn1 O1 C1 C2 177.59(17) . . . . ? Zn2 O1 C1 C2 -72.8(3) . . . . ? Zn2 O1 C1 Zn1 109.64(19) . . . . ? O3 Zn1 C1 O2 91.52(13) . . . . ? O4 Zn1 C1 O2 -140.99(12) . . . . ? N2 Zn1 C1 O2 -25.51(16) . . . . ? O1 Zn1 C1 O2 179.5(2) . . . . ? O3 Zn1 C1 O1 -88.03(13) . . . . ? O4 Zn1 C1 O1 39.47(13) . . . . ? N2 Zn1 C1 O1 154.95(11) . . . . ? O2 Zn1 C1 O1 -179.5(2) . . . . ? O3 Zn1 C1 C2 -130(3) . . . . ? O4 Zn1 C1 C2 -2(3) . . . . ? N2 Zn1 C1 C2 113(3) . . . . ? O1 Zn1 C1 C2 -42(3) . . . . ? O2 Zn1 C1 C2 139(3) . . . . ? O2 C1 C2 C7 171.2(2) . . . . ? O1 C1 C2 C7 -6.8(3) . . . . ? Zn1 C1 C2 C7 34(3) . . . . ? O2 C1 C2 C3 -7.8(3) . . . . ? O1 C1 C2 C3 174.17(19) . . . . ? Zn1 C1 C2 C3 -146(3) . . . . ? C7 C2 C3 C4 1.6(3) . . . . ? C1 C2 C3 C4 -179.4(2) . . . . ? C2 C3 C4 C5 -0.4(4) . . . . ? C3 C4 C5 C6 -0.7(4) . . . . ? C3 C4 C5 S1 178.63(18) . . . . ? C8 S1 C5 C4 168.40(19) . . . . ? C8 S1 C5 C6 -12.3(2) . . . . ? C4 C5 C6 C7 0.7(3) . . . . ? S1 C5 C6 C7 -178.60(16) . . . . ? C5 C6 C7 C2 0.5(3) . . . . ? C3 C2 C7 C6 -1.6(3) . . . . ? C1 C2 C7 C6 179.31(19) . . . . ? C5 S1 C8 C9 -162.28(17) . . . . ? C13 N1 C9 C10 0.4(4) . . . . ? C13 N1 C9 C8 -179.1(2) . . . . ? S1 C8 C9 N1 -107.1(2) . . . . ? S1 C8 C9 C10 73.4(3) . . . . ? N1 C9 C10 C11 -1.6(4) . . . . ? C8 C9 C10 C11 178.0(2) . . . . ? C9 C10 C11 C12 1.2(4) . . . . ? C10 C11 C12 C13 0.1(4) . . . . ? C9 N1 C13 C12 1.0(4) . . . . ? C11 C12 C13 N1 -1.3(4) . . . . ? C18 N2 C14 C15 3.9(3) . . . . ? Zn1 N2 C14 C15 -167.01(17) . . . . ? C18 N2 C14 C39 -173.8(2) . . . 2_666 ? Zn1 N2 C14 C39 15.3(3) . . . 2_666 ? N2 C14 C15 C16 -3.0(3) . . . . ? C39 C14 C15 C16 174.4(2) 2_666 . . . ? C14 C15 C16 C17 -0.1(4) . . . . ? C15 C16 C17 C18 2.3(4) . . . . ? C14 N2 C18 C17 -1.7(3) . . . . ? Zn1 N2 C18 C17 169.72(19) . . . . ? C16 C17 C18 N2 -1.4(4) . . . . ? Zn1 O3 C19 O5 -2.0(3) . . . 2_656 ? Zn1 O3 C19 C20 177.74(14) . . . . ? O5 C19 C20 C21 174.4(2) 2_656 . . . ? O3 C19 C20 C21 -5.3(3) . . . . ? O5 C19 C20 C25 -3.6(3) 2_656 . . . ? O3 C19 C20 C25 176.6(2) . . . . ? C25 C20 C21 C22 -0.2(3) . . . . ? C19 C20 C21 C22 -178.3(2) . . . . ? C20 C21 C22 C23 -0.9(4) . . . . ? C21 C22 C23 C24 1.6(3) . . . . ? C21 C22 C23 S2 -179.38(18) . . . . ? C26 S2 C23 C22 15.3(2) . . . . ? C26 S2 C23 C24 -165.64(18) . . . . ? C22 C23 C24 C25 -1.2(3) . . . . ? S2 C23 C24 C25 179.68(18) . . . . ? C23 C24 C25 C20 0.1(4) . . . . ? C21 C20 C25 C24 0.6(3) . . . . ? C19 C20 C25 C24 178.7(2) . . . . ? C23 S2 C26 C27 -87.54(19) . . . . ? C31 N3 C27 C28 2.5(4) . . . . ? C31 N3 C27 C26 -176.2(2) . . . . ? S2 C26 C27 N3 96.8(2) . . . . ? S2 C26 C27 C28 -81.8(2) . . . . ? N3 C27 C28 C29 -2.0(4) . . . . ? C26 C27 C28 C29 176.6(2) . . . . ? C27 C28 C29 C30 -0.1(4) . . . . ? C28 C29 C30 C31 1.6(4) . . . . ? C27 N3 C31 C30 -0.9(4) . . . . ? C29 C30 C31 N3 -1.1(4) . . . . ? Zn1 O4 C32 O6 8.6(3) . . . 2_656 ? Zn1 O4 C32 C33 -168.73(13) . . . . ? O6 C32 C33 C38 157.44(19) 2_656 . . . ? O4 C32 C33 C38 -25.1(3) . . . . ? O6 C32 C33 C34 -23.5(3) 2_656 . . . ? O4 C32 C33 C34 153.99(19) . . . . ? C38 C33 C34 C35 1.5(3) . . . . ? C32 C33 C34 C35 -177.6(2) . . . . ? C33 C34 C35 C36 -0.2(3) . . . . ? C34 C35 C36 C37 -1.9(3) . . . . ? C34 C35 C36 S3 176.00(17) . . . . ? C39 S3 C36 C37 -0.1(2) . . . . ? C39 S3 C36 C35 -177.91(17) . . . . ? C35 C36 C37 C38 2.9(3) . . . . ? S3 C36 C37 C38 -174.86(17) . . . . ? C36 C37 C38 C33 -1.7(3) . . . . ? C34 C33 C38 C37 -0.5(3) . . . . ? C32 C33 C38 C37 178.54(19) . . . . ? C36 S3 C39 C14 -78.38(19) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.283 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.060