# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jose Sordo' _publ_contact_author_email QIJSORDO@USC.ES _publ_section_title ; Chemical and in vitro study of the potential of 3-aryl-2-sulfanylpropenoic acids and their Zn(II) complexes as protective agents against cadmium toxicity ; loop_ _publ_author_name 'Jose Sordo' 'Jose Casas' 'E Castellano' 'Maria D Couce' 'M Garcia-Vega' ; A.Sanchez ; 'Angeles Sanchez-Gonzalez' 'J M Varela' 'E M Vazquez Lopez' # Attachment 'Mat_dep.cif' data_H2pspa _database_code_depnum_ccdc_archive 'CCDC 741227' ################ # CCDC 741227 # ################ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H8 O2 S' _chemical_formula_weight 180.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.3072(10) _cell_length_b 16.4712(10) _cell_length_c 8.717(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.303(10) _cell_angle_gamma 90.00 _cell_volume 884.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .150 _exptl_crystal_size_mid .125 _exptl_crystal_size_min .050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_absorpt_coefficient_mu 2.890 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.5013 _exptl_absorpt_correction_T_max 0.7532 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _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 1219 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 5.37 _diffrn_reflns_theta_max 54.94 _reflns_number_total 1104 _reflns_number_gt 879 _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^)+(0.0529P)^2^+0.3163P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1104 _refine_ls_number_parameters 114 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1180 _refine_ls_wR_factor_gt 0.1090 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.30152(13) 0.61637(6) 0.14158(11) 0.0853(4) Uani 1 1 d . . . O1 O 0.1752(3) 0.54005(15) 0.4131(3) 0.0776(7) Uani 1 1 d . . . O2 O -0.1770(3) 0.52655(16) 0.3124(3) 0.0779(7) Uani 1 1 d . . . C1 C 0.0207(5) 0.54883(19) 0.3037(4) 0.0641(8) Uani 1 1 d . . . C2 C 0.0403(5) 0.58526(19) 0.1533(4) 0.0619(8) Uani 1 1 d . . . C3 C -0.1366(5) 0.59250(19) 0.0374(4) 0.0629(8) Uani 1 1 d . . . H3 H -0.2624 0.5726 0.0633 0.076 Uiso 1 1 calc R . . C4 C -0.1703(5) 0.62558(18) -0.1215(4) 0.0607(8) Uani 1 1 d . . . C5 C -0.3782(5) 0.6218(2) -0.2139(4) 0.0724(9) Uani 1 1 d . . . H5 H -0.4877 0.5977 -0.1732 0.087 Uiso 1 1 calc R . . C6 C -0.4273(6) 0.6524(3) -0.3639(4) 0.0899(11) Uani 1 1 d . . . H6 H -0.5688 0.6495 -0.4224 0.108 Uiso 1 1 calc R . . C7 C -0.2689(7) 0.6871(2) -0.4273(5) 0.0894(11) Uani 1 1 d . . . H7 H -0.3010 0.7074 -0.5292 0.107 Uiso 1 1 calc R . . C8 C -0.0626(6) 0.6917(2) -0.3389(5) 0.0877(11) Uani 1 1 d . . . H8 H 0.0458 0.7154 -0.3814 0.105 Uiso 1 1 calc R . . C9 C -0.0122(5) 0.6619(2) -0.1880(4) 0.0752(9) Uani 1 1 d . . . H9 H 0.1292 0.6660 -0.1298 0.090 Uiso 1 1 calc R . . H2 H -0.169(7) 0.502(2) 0.414(5) 0.116(14) Uiso 1 1 d . . . HS H 0.3982 0.5877 0.2799 0.107(11) Uiso 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 S1 0.0475(6) 0.1159(8) 0.0948(7) 0.0108(6) 0.0203(4) -0.0079(4) O1 0.0505(14) 0.1081(18) 0.0724(15) 0.0054(13) 0.0091(11) -0.0067(11) O2 0.0495(14) 0.1111(19) 0.0733(16) 0.0112(14) 0.0135(11) -0.0061(12) C1 0.0490(19) 0.071(2) 0.073(2) -0.0052(16) 0.0156(17) 0.0013(15) C2 0.0460(17) 0.072(2) 0.070(2) -0.0020(16) 0.0176(15) 0.0004(15) C3 0.0485(18) 0.071(2) 0.072(2) -0.0035(16) 0.0191(16) 0.0005(15) C4 0.0524(19) 0.0615(18) 0.071(2) -0.0031(15) 0.0194(15) 0.0028(14) C5 0.060(2) 0.081(2) 0.076(2) 0.0036(18) 0.0139(17) -0.0055(16) C6 0.077(2) 0.103(3) 0.083(3) 0.007(2) 0.0013(19) -0.010(2) C7 0.100(3) 0.084(2) 0.082(2) 0.013(2) 0.013(2) -0.009(2) C8 0.084(3) 0.091(3) 0.094(3) 0.018(2) 0.031(2) -0.008(2) C9 0.0601(19) 0.081(2) 0.086(2) 0.012(2) 0.0197(17) -0.0007(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 S1 C2 1.749(3) . ? O1 C1 1.218(4) . ? O2 C1 1.317(4) . ? C1 C2 1.471(4) . ? C2 C3 1.341(4) . ? C3 C4 1.462(4) . ? C4 C5 1.386(4) . ? C4 C9 1.390(4) . ? C5 C6 1.373(5) . ? C6 C7 1.367(5) . ? C7 C8 1.365(5) . ? C8 C9 1.376(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 122.1(3) . . ? O1 C1 C2 122.8(3) . . ? O2 C1 C2 115.1(3) . . ? C3 C2 C1 119.6(3) . . ? C3 C2 S1 124.9(2) . . ? C1 C2 S1 115.5(2) . . ? C2 C3 C4 132.6(3) . . ? C5 C4 C9 116.8(3) . . ? C5 C4 C3 117.6(3) . . ? C9 C4 C3 125.6(3) . . ? C6 C5 C4 122.0(3) . . ? C7 C6 C5 120.2(3) . . ? C8 C7 C6 119.0(4) . . ? C7 C8 C9 121.2(3) . . ? C8 C9 C4 120.8(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 O1 C1 C2 C3 179.5(3) . . . . ? O2 C1 C2 C3 -0.8(4) . . . . ? O1 C1 C2 S1 -0.5(4) . . . . ? O2 C1 C2 S1 179.1(2) . . . . ? C1 C2 C3 C4 179.6(3) . . . . ? S1 C2 C3 C4 -0.3(5) . . . . ? C2 C3 C4 C5 178.5(3) . . . . ? C2 C3 C4 C9 -2.5(6) . . . . ? C9 C4 C5 C6 -0.2(5) . . . . ? C3 C4 C5 C6 178.9(3) . . . . ? C4 C5 C6 C7 0.8(6) . . . . ? C5 C6 C7 C8 -0.8(6) . . . . ? C6 C7 C8 C9 0.1(6) . . . . ? C7 C8 C9 C4 0.5(6) . . . . ? C5 C4 C9 C8 -0.4(5) . . . . ? C3 C4 C9 C8 -179.4(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A S1 HS O1 1.32 2.154(2) 2.937(2) 113.33(7) . O2 H2 O1 0.97(5) 1.67(5) 2.630(3) 176(4) 3_566 S1 HS O2 1.32 2.819(2) 3.624(2) 117.68(6) 1_655 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 54.94 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.175 _refine_diff_density_min -0.187 _refine_diff_density_rms 0.037 #=== data_1 _database_code_depnum_ccdc_archive 'CCDC 741228' ################ # CCDC 741228 # ################ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H44 N2 O4 S2 Zn' _chemical_formula_weight 626.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 14.9443(10) _cell_length_b 15.826(3) _cell_length_c 27.464(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6495.3(15) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .250 _exptl_crystal_size_mid .065 _exptl_crystal_size_min .026 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 2.527 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.7672 _exptl_absorpt_correction_T_max 0.9363 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6379 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.1186 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 69.94 _reflns_number_total 6117 _reflns_number_gt 2543 _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^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6117 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1635 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.1100 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 0.10826(4) 0.16339(3) 0.597711(18) 0.04093(15) Uani 1 1 d . . . S1 S 0.13400(7) 0.12700(8) 0.67651(4) 0.0463(3) Uani 1 1 d . . . S2 S 0.01446(7) 0.12144(7) 0.53792(4) 0.0428(3) Uani 1 1 d . . . O11 O 0.23698(18) 0.14052(18) 0.58209(9) 0.0449(8) Uani 1 1 d . . . O12 O 0.35480(18) 0.07081(19) 0.60936(10) 0.0501(8) Uani 1 1 d . . . O21 O 0.06526(18) 0.28297(17) 0.58908(9) 0.0427(7) Uani 1 1 d . . . O22 O -0.04133(17) 0.35859(17) 0.55450(9) 0.0441(7) Uani 1 1 d . . . C11 C 0.2836(3) 0.1090(3) 0.61679(14) 0.0385(10) Uani 1 1 d . . . C12 C 0.2499(3) 0.1198(3) 0.66803(14) 0.0380(9) Uani 1 1 d . . . C13 C 0.3121(3) 0.1224(3) 0.70406(14) 0.0432(11) Uani 1 1 d . . . H13 H 0.3704 0.1180 0.6926 0.052 Uiso 1 1 calc R . . C14 C 0.30711(19) 0.13061(19) 0.75723(7) 0.0436(11) Uani 1 1 d G . . C15 C 0.22803(15) 0.1448(2) 0.78259(10) 0.0667(16) Uani 1 1 d G . . H15 H 0.1746 0.1518 0.7657 0.080 Uiso 1 1 calc R . . C16 C 0.22883(17) 0.1485(2) 0.83315(10) 0.0808(18) Uani 1 1 d G . . H16 H 0.1759 0.1580 0.8501 0.097 Uiso 1 1 calc R . . C17 C 0.3087(2) 0.1380(2) 0.85836(7) 0.0675(15) Uani 1 1 d G . . H17 H 0.3093 0.1405 0.8922 0.081 Uiso 1 1 calc R . . C18 C 0.38780(17) 0.1238(2) 0.83300(10) 0.0679(14) Uani 1 1 d G . . H18 H 0.4412 0.1168 0.8499 0.081 Uiso 1 1 calc R . . C19 C 0.38699(15) 0.1201(2) 0.78244(10) 0.0583(13) Uani 1 1 d G . . H19 H 0.4399 0.1106 0.7655 0.070 Uiso 1 1 calc R . . C21 C 0.0050(3) 0.2935(3) 0.55613(13) 0.0344(9) Uani 1 1 d . . . C22 C -0.0051(2) 0.2255(2) 0.51832(13) 0.0313(9) Uani 1 1 d . . . C23 C -0.0219(2) 0.2511(3) 0.47197(13) 0.0368(10) Uani 1 1 d . . . H23 H -0.0367 0.3080 0.4689 0.044 Uiso 1 1 calc R . . C24 C -0.02077(18) 0.20385(18) 0.42572(7) 0.0376(10) Uani 1 1 d G . . C25 C -0.02118(18) 0.11621(17) 0.42240(8) 0.0476(11) Uani 1 1 d G . . H25 H -0.0268 0.0836 0.4504 0.057 Uiso 1 1 calc R . . C26 C -0.0132(2) 0.07732(15) 0.37723(11) 0.0559(13) Uani 1 1 d G . . H26 H -0.0135 0.0187 0.3750 0.067 Uiso 1 1 calc R . . C27 C -0.0049(2) 0.1261(2) 0.33538(8) 0.0682(15) Uani 1 1 d G . . H27 H 0.0004 0.1000 0.3052 0.082 Uiso 1 1 calc R . . C28 C -0.0045(2) 0.2137(2) 0.33869(8) 0.0645(15) Uani 1 1 d G . . H28 H 0.0011 0.2463 0.3107 0.077 Uiso 1 1 calc R . . C29 C -0.0124(2) 0.25260(14) 0.38386(10) 0.0526(12) Uani 1 1 d G . . H29 H -0.0121 0.3112 0.3861 0.063 Uiso 1 1 calc R . . N1 N 0.2934(2) 0.0942(2) 0.48393(12) 0.0390(8) Uani 1 1 d . . . H1A H 0.2877 0.1063 0.5158 0.047 Uiso 1 1 calc R . . H1B H 0.3477 0.1126 0.4744 0.047 Uiso 1 1 calc R . . C111 C 0.2909(3) -0.0005(3) 0.47811(16) 0.0461(11) Uani 1 1 d . . . H111 H 0.2878 -0.0139 0.4433 0.055 Uiso 1 1 calc R . . C112 C 0.2086(3) -0.0357(3) 0.5029(2) 0.0719(16) Uani 1 1 d . . . H11A H 0.2054 -0.0955 0.4975 0.108 Uiso 1 1 calc R . . H11B H 0.1562 -0.0090 0.4898 0.108 Uiso 1 1 calc R . . H11C H 0.2120 -0.0248 0.5373 0.108 Uiso 1 1 calc R . . C113 C 0.3763(3) -0.0365(3) 0.4984(2) 0.0685(15) Uani 1 1 d . . . H11D H 0.4264 -0.0134 0.4810 0.103 Uiso 1 1 calc R . . H11E H 0.3758 -0.0968 0.4948 0.103 Uiso 1 1 calc R . . H11F H 0.3811 -0.0222 0.5322 0.103 Uiso 1 1 calc R . . C114 C 0.2235(3) 0.1433(3) 0.45639(15) 0.0447(11) Uani 1 1 d . . . H114 H 0.1642 0.1233 0.4663 0.054 Uiso 1 1 calc R . . C115 C 0.2325(3) 0.2352(3) 0.47032(17) 0.0658(15) Uani 1 1 d . . . H11G H 0.1877 0.2677 0.4536 0.099 Uiso 1 1 calc R . . H11H H 0.2908 0.2552 0.4614 0.099 Uiso 1 1 calc R . . H11I H 0.2245 0.2411 0.5048 0.099 Uiso 1 1 calc R . . C116 C 0.2337(3) 0.1300(3) 0.40226(16) 0.0744(16) Uani 1 1 d . . . H11J H 0.2235 0.0716 0.3946 0.112 Uiso 1 1 calc R . . H11K H 0.2931 0.1457 0.3925 0.112 Uiso 1 1 calc R . . H11L H 0.1909 0.1644 0.3853 0.112 Uiso 1 1 calc R . . N2 N 0.3990(2) -0.0864(2) 0.65584(11) 0.0429(8) Uani 1 1 d . . . H2A H 0.4183 -0.1125 0.6287 0.051 Uiso 1 1 calc R . . H2B H 0.3788 -0.0351 0.6469 0.051 Uiso 1 1 calc R . . C211 C 0.3206(3) -0.1358(3) 0.67517(17) 0.0558(13) Uani 1 1 d . . . H211 H 0.3402 -0.1944 0.6798 0.067 Uiso 1 1 calc R . . C212 C 0.2873(4) -0.1033(3) 0.72375(19) 0.0877(19) Uani 1 1 d . . . H21A H 0.3343 -0.1077 0.7475 0.132 Uiso 1 1 calc R . . H21B H 0.2369 -0.1363 0.7341 0.132 Uiso 1 1 calc R . . H21C H 0.2698 -0.0452 0.7205 0.132 Uiso 1 1 calc R . . C213 C 0.2478(3) -0.1360(3) 0.6365(2) 0.0829(18) Uani 1 1 d . . . H21D H 0.2731 -0.1522 0.6058 0.124 Uiso 1 1 calc R . . H21E H 0.2224 -0.0804 0.6339 0.124 Uiso 1 1 calc R . . H21F H 0.2019 -0.1755 0.6455 0.124 Uiso 1 1 calc R . . C214 C 0.4783(3) -0.0733(3) 0.68841(16) 0.0523(12) Uani 1 1 d . . . H214 H 0.4581 -0.0475 0.7189 0.063 Uiso 1 1 calc R . . C215 C 0.5418(3) -0.0139(3) 0.66330(19) 0.0757(17) Uani 1 1 d . . . H21G H 0.5927 -0.0041 0.6838 0.114 Uiso 1 1 calc R . . H21H H 0.5120 0.0387 0.6569 0.114 Uiso 1 1 calc R . . H21I H 0.5612 -0.0385 0.6331 0.114 Uiso 1 1 calc R . . C216 C 0.5214(4) -0.1582(3) 0.69965(17) 0.0780(17) Uani 1 1 d . . . H21J H 0.5708 -0.1500 0.7215 0.117 Uiso 1 1 calc R . . H21K H 0.5426 -0.1833 0.6700 0.117 Uiso 1 1 calc R . . H21L H 0.4781 -0.1948 0.7145 0.117 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 0.0428(3) 0.0456(3) 0.0343(3) 0.0010(3) -0.0077(3) 0.0064(3) S1 0.0421(6) 0.0623(7) 0.0346(5) 0.0047(5) -0.0029(5) 0.0010(5) S2 0.0495(6) 0.0400(6) 0.0390(5) 0.0008(5) -0.0107(5) -0.0015(5) O11 0.0452(17) 0.054(2) 0.0351(14) 0.0026(13) -0.0016(13) 0.0074(15) O12 0.0469(17) 0.057(2) 0.0467(18) -0.0056(15) 0.0026(14) 0.0141(15) O21 0.0453(16) 0.0452(18) 0.0375(16) -0.0090(13) -0.0139(13) 0.0071(14) O22 0.0440(17) 0.0423(19) 0.0459(16) -0.0097(14) -0.0092(13) 0.0135(14) C11 0.041(2) 0.037(3) 0.038(2) -0.0044(19) -0.005(2) -0.003(2) C12 0.043(2) 0.033(2) 0.038(2) 0.001(2) -0.004(2) 0.003(2) C13 0.039(2) 0.053(3) 0.038(2) -0.002(2) -0.0057(19) 0.001(2) C14 0.048(3) 0.043(3) 0.040(2) 0.001(2) -0.009(2) -0.001(2) C15 0.050(3) 0.103(5) 0.047(3) -0.004(3) -0.010(2) 0.003(3) C16 0.067(4) 0.132(6) 0.043(3) -0.014(3) -0.003(2) -0.007(4) C17 0.090(4) 0.078(4) 0.034(3) -0.010(2) -0.012(3) 0.000(3) C18 0.069(3) 0.086(4) 0.049(3) -0.010(3) -0.025(3) 0.009(3) C19 0.050(3) 0.077(4) 0.048(3) -0.011(3) -0.017(2) 0.009(3) C21 0.035(2) 0.038(2) 0.030(2) -0.0037(18) 0.0025(18) 0.001(2) C22 0.023(2) 0.037(2) 0.034(2) -0.0029(18) 0.0003(16) 0.0005(17) C23 0.032(2) 0.042(2) 0.036(2) -0.0006(19) -0.0051(18) 0.003(2) C24 0.032(2) 0.052(3) 0.028(2) 0.001(2) -0.0048(18) -0.002(2) C25 0.052(3) 0.048(3) 0.042(2) -0.003(2) -0.002(2) -0.005(3) C26 0.068(3) 0.053(3) 0.047(3) -0.010(2) -0.006(3) -0.002(3) C27 0.087(4) 0.078(4) 0.040(3) -0.010(3) 0.004(3) 0.014(3) C28 0.082(4) 0.076(4) 0.036(3) 0.004(2) 0.002(3) 0.009(3) C29 0.068(3) 0.052(3) 0.038(2) 0.001(2) -0.004(2) 0.005(3) N1 0.0342(18) 0.039(2) 0.0440(19) -0.0012(17) 0.0085(16) 0.0016(16) C111 0.047(3) 0.037(3) 0.054(3) -0.007(2) 0.001(2) 0.002(2) C112 0.047(3) 0.049(3) 0.120(5) 0.004(3) 0.014(3) -0.008(3) C113 0.048(3) 0.042(3) 0.115(4) 0.008(3) -0.007(3) 0.006(2) C114 0.034(2) 0.048(3) 0.052(3) 0.008(2) 0.0006(19) 0.004(2) C115 0.078(4) 0.047(3) 0.073(4) 0.009(3) 0.015(3) 0.017(3) C116 0.080(4) 0.091(4) 0.053(3) 0.002(3) -0.019(3) 0.014(3) N2 0.046(2) 0.042(2) 0.0414(19) -0.0037(16) -0.0017(17) 0.0067(18) C211 0.058(3) 0.046(3) 0.064(3) 0.003(2) 0.012(3) 0.000(2) C212 0.107(5) 0.069(4) 0.087(4) -0.002(3) 0.049(4) -0.008(4) C213 0.044(3) 0.083(4) 0.122(5) -0.007(4) -0.009(3) -0.007(3) C214 0.057(3) 0.057(3) 0.043(3) -0.016(2) -0.012(2) 0.010(3) C215 0.054(3) 0.080(4) 0.093(4) -0.010(3) -0.010(3) -0.002(3) C216 0.087(4) 0.083(4) 0.064(3) 0.000(3) -0.030(3) 0.027(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 Zn O11 2.004(3) . ? Zn O21 2.012(3) . ? Zn S2 2.2588(11) . ? Zn S1 2.2722(12) . ? S1 C12 1.751(4) . ? S2 C22 1.757(4) . ? O11 C11 1.282(4) . ? O12 C11 1.240(4) . ? O21 C21 1.287(4) . ? O22 C21 1.242(4) . ? C11 C12 1.505(5) . ? C12 C13 1.358(5) . ? C13 C14 1.468(4) . ? C14 C15 1.3900 . ? C14 C19 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C21 C22 1.503(5) . ? C22 C23 1.359(5) . ? C23 C24 1.474(4) . ? C24 C25 1.3900 . ? C24 C29 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? N1 C114 1.506(5) . ? N1 C111 1.507(5) . ? C111 C113 1.503(6) . ? C111 C112 1.513(6) . ? C114 C116 1.509(6) . ? C114 C115 1.509(6) . ? N2 C214 1.499(5) . ? N2 C211 1.506(5) . ? C211 C212 1.514(6) . ? C211 C213 1.520(6) . ? C214 C215 1.503(6) . ? C214 C216 1.522(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Zn O21 116.82(12) . . ? O11 Zn S2 112.77(8) . . ? O21 Zn S2 89.58(8) . . ? O11 Zn S1 89.75(8) . . ? O21 Zn S1 113.86(8) . . ? S2 Zn S1 136.29(5) . . ? C12 S1 Zn 93.28(13) . . ? C22 S2 Zn 92.88(12) . . ? C11 O11 Zn 115.7(3) . . ? C21 O21 Zn 115.3(2) . . ? O12 C11 O11 122.3(4) . . ? O12 C11 C12 119.8(4) . . ? O11 C11 C12 117.9(4) . . ? C13 C12 C11 117.1(4) . . ? C13 C12 S1 125.3(3) . . ? C11 C12 S1 117.6(3) . . ? C12 C13 C14 133.9(4) . . ? C15 C14 C19 120.0 . . ? C15 C14 C13 123.8(2) . . ? C19 C14 C13 116.2(2) . . ? C16 C15 C14 120.0 . . ? C15 C16 C17 120.0 . . ? C16 C17 C18 120.0 . . ? C17 C18 C19 120.0 . . ? C18 C19 C14 120.0 . . ? O22 C21 O21 121.5(4) . . ? O22 C21 C22 120.9(3) . . ? O21 C21 C22 117.6(3) . . ? C23 C22 C21 116.9(3) . . ? C23 C22 S2 126.7(3) . . ? C21 C22 S2 116.3(3) . . ? C22 C23 C24 130.8(4) . . ? C25 C24 C29 120.0 . . ? C25 C24 C23 124.2(2) . . ? C29 C24 C23 115.6(2) . . ? C26 C25 C24 120.0 . . ? C27 C26 C25 120.0 . . ? C26 C27 C28 120.0 . . ? C29 C28 C27 120.0 . . ? C28 C29 C24 120.0 . . ? C114 N1 C111 116.3(3) . . ? C113 C111 N1 108.5(4) . . ? C113 C111 C112 112.5(4) . . ? N1 C111 C112 109.8(3) . . ? N1 C114 C116 110.7(3) . . ? N1 C114 C115 108.0(3) . . ? C116 C114 C115 112.0(4) . . ? C214 N2 C211 118.5(3) . . ? N2 C211 C212 112.9(4) . . ? N2 C211 C213 108.2(4) . . ? C212 C211 C213 112.4(4) . . ? N2 C214 C215 108.2(4) . . ? N2 C214 C216 109.5(4) . . ? C215 C214 C216 112.2(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Zn S1 C12 7.72(16) . . . . ? O21 Zn S1 C12 -111.72(16) . . . . ? S2 Zn S1 C12 131.47(14) . . . . ? O11 Zn S2 C22 -105.34(15) . . . . ? O21 Zn S2 C22 13.76(14) . . . . ? S1 Zn S2 C22 139.05(13) . . . . ? O21 Zn O11 C11 122.5(3) . . . . ? S2 Zn O11 C11 -135.8(3) . . . . ? S1 Zn O11 C11 5.6(3) . . . . ? O11 Zn O21 C21 115.8(3) . . . . ? S2 Zn O21 C21 0.3(3) . . . . ? S1 Zn O21 C21 -141.6(2) . . . . ? Zn O11 C11 O12 159.8(3) . . . . ? Zn O11 C11 C12 -20.5(5) . . . . ? O12 C11 C12 C13 28.5(6) . . . . ? O11 C11 C12 C13 -151.1(4) . . . . ? O12 C11 C12 S1 -150.8(3) . . . . ? O11 C11 C12 S1 29.5(5) . . . . ? Zn S1 C12 C13 160.7(4) . . . . ? Zn S1 C12 C11 -20.0(3) . . . . ? C11 C12 C13 C14 -178.9(4) . . . . ? S1 C12 C13 C14 0.4(7) . . . . ? C12 C13 C14 C15 -5.3(7) . . . . ? C12 C13 C14 C19 172.3(4) . . . . ? C19 C14 C15 C16 0.0 . . . . ? C13 C14 C15 C16 177.5(3) . . . . ? C14 C15 C16 C17 0.0 . . . . ? C15 C16 C17 C18 0.0 . . . . ? C16 C17 C18 C19 0.0 . . . . ? C17 C18 C19 C14 0.0 . . . . ? C15 C14 C19 C18 0.0 . . . . ? C13 C14 C19 C18 -177.7(3) . . . . ? Zn O21 C21 O22 163.4(3) . . . . ? Zn O21 C21 C22 -18.9(4) . . . . ? O22 C21 C22 C23 36.4(5) . . . . ? O21 C21 C22 C23 -141.3(4) . . . . ? O22 C21 C22 S2 -148.1(3) . . . . ? O21 C21 C22 S2 34.1(4) . . . . ? Zn S2 C22 C23 147.8(3) . . . . ? Zn S2 C22 C21 -27.1(3) . . . . ? C21 C22 C23 C24 168.6(4) . . . . ? S2 C22 C23 C24 -6.3(6) . . . . ? C22 C23 C24 C25 15.6(6) . . . . ? C22 C23 C24 C29 -159.8(4) . . . . ? C29 C24 C25 C26 0.0 . . . . ? C23 C24 C25 C26 -175.2(3) . . . . ? C24 C25 C26 C27 0.0 . . . . ? C25 C26 C27 C28 0.0 . . . . ? C26 C27 C28 C29 0.0 . . . . ? C27 C28 C29 C24 0.0 . . . . ? C25 C24 C29 C28 0.0 . . . . ? C23 C24 C29 C28 175.6(3) . . . . ? C114 N1 C111 C113 167.3(4) . . . . ? C114 N1 C111 C112 -69.4(5) . . . . ? C111 N1 C114 C116 -61.7(5) . . . . ? C111 N1 C114 C115 175.3(3) . . . . ? C214 N2 C211 C212 51.9(5) . . . . ? C214 N2 C211 C213 177.0(4) . . . . ? C211 N2 C214 C215 -173.2(4) . . . . ? C211 N2 C214 C216 64.3(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1B O22 0.90 1.90 2.788(4) 171.1 6_666 N2 H2B O12 0.90 2.00 2.873(4) 163.1 . N2 H2A O21 0.90 2.00 2.814(4) 150.6 2_545 N1 H1A O11 0.90 2.05 2.918(4) 163.2 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 69.94 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.449 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.070 #=== data_2 _database_code_depnum_ccdc_archive 'CCDC 741229' ################ # CCDC 741229 # ################ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H42 Cl2 N2 O4 S2 Zn' _chemical_formula_weight 695.05 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 14.415(2) _cell_length_b 7.7905(11) _cell_length_c 17.9381(18) _cell_angle_alpha 90.00 _cell_angle_beta 120.395(8) _cell_angle_gamma 90.00 _cell_volume 1737.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .37 _exptl_crystal_size_mid .06 _exptl_crystal_size_min .04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 1.015 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.569198 _exptl_absorpt_correction_T_max 1.000000 _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 '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 9349 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.1298 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.07 _reflns_number_total 3882 _reflns_number_gt 1933 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3882 _refine_ls_number_parameters 186 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1375 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1084 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 0.875 _refine_ls_restrained_S_all 0.875 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.0000 0.68310(8) 0.2500 0.0402(2) Uani 1 2 d S . . Cl Cl 0.49899(10) 0.7656(2) 0.64100(9) 0.1032(5) Uani 1 1 d . . . S1 S 0.16513(8) 0.57174(15) 0.33519(6) 0.0546(3) Uani 1 1 d . . . O1 O 0.02200(19) 0.8310(3) 0.34911(14) 0.0448(6) Uani 1 1 d . . . O2 O 0.1250(2) 0.8953(4) 0.48626(17) 0.0722(9) Uani 1 1 d . . . C1 C 0.1087(3) 0.8103(5) 0.4228(2) 0.0430(9) Uani 1 1 d . . . C2 C 0.1890(3) 0.6774(5) 0.4298(2) 0.0393(9) Uani 1 1 d . . . C3 C 0.2748(3) 0.6485(5) 0.5081(2) 0.0469(10) Uani 1 1 d . . . H3 H 0.2806 0.7190 0.5521 0.056 Uiso 1 1 calc R . . C4 C 0.3601(3) 0.5221(6) 0.5340(2) 0.0468(10) Uani 1 1 d . . . C5 C 0.4667(4) 0.5605(6) 0.5967(3) 0.0632(13) Uani 1 1 d . . . C6 C 0.5486(4) 0.4442(9) 0.6215(3) 0.0872(18) Uani 1 1 d . . . H6 H 0.6188 0.4748 0.6619 0.105 Uiso 1 1 calc R . . C7 C 0.5260(5) 0.2812(9) 0.5860(4) 0.0904(19) Uani 1 1 d . . . H7 H 0.5811 0.2020 0.6017 0.108 Uiso 1 1 calc R . . C8 C 0.4222(5) 0.2373(6) 0.5277(3) 0.0767(15) Uani 1 1 d . . . H8 H 0.4061 0.1262 0.5058 0.092 Uiso 1 1 calc R . . C9 C 0.3415(4) 0.3564(6) 0.5014(3) 0.0604(12) Uani 1 1 d . . . H9 H 0.2718 0.3250 0.4601 0.072 Uiso 1 1 calc R . . N N 0.1457(2) 0.9810(4) 0.13963(18) 0.0414(8) Uani 1 1 d . . . H111 H 0.1321 1.0134 0.0869 0.050 Uiso 1 1 calc R . . H112 H 0.0841 0.9385 0.1332 0.050 Uiso 1 1 calc R . . C11 C 0.1728(4) 1.1394(5) 0.1941(3) 0.0570(12) Uani 1 1 d . . . H11 H 0.2367 1.1931 0.1982 0.068 Uiso 1 1 calc R . . C12 C 0.1960(4) 1.0950(6) 0.2844(3) 0.0792(15) Uani 1 1 d . . . H12A H 0.2572 1.0202 0.3118 0.119 Uiso 1 1 calc R . . H12B H 0.1346 1.0385 0.2807 0.119 Uiso 1 1 calc R . . H12C H 0.2107 1.1983 0.3178 0.119 Uiso 1 1 calc R . . C13 C 0.0784(5) 1.2610(6) 0.1481(3) 0.0895(17) Uani 1 1 d . . . H13A H 0.0674 1.2879 0.0920 0.134 Uiso 1 1 calc R . . H13B H 0.0930 1.3646 0.1812 0.134 Uiso 1 1 calc R . . H13C H 0.0149 1.2076 0.1420 0.134 Uiso 1 1 calc R . . C14 C 0.2254(3) 0.8369(5) 0.1690(3) 0.0551(11) Uani 1 1 d . . . H14 H 0.2388 0.7960 0.2253 0.066 Uiso 1 1 calc R . . C15 C 0.1757(4) 0.6931(5) 0.1041(3) 0.0793(15) Uani 1 1 d . . . H15A H 0.1101 0.6570 0.1008 0.119 Uiso 1 1 calc R . . H15B H 0.2249 0.5981 0.1219 0.119 Uiso 1 1 calc R . . H15C H 0.1607 0.7327 0.0484 0.119 Uiso 1 1 calc R . . C16 C 0.3305(3) 0.8979(6) 0.1784(3) 0.0778(15) Uani 1 1 d . . . H16A H 0.3600 0.9875 0.2209 0.117 Uiso 1 1 calc R . . H16B H 0.3179 0.9411 0.1239 0.117 Uiso 1 1 calc R . . H16C H 0.3802 0.8038 0.1964 0.117 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 0.0371(4) 0.0502(4) 0.0271(4) 0.000 0.0118(3) 0.000 Cl 0.0594(9) 0.1402(14) 0.0798(10) -0.0404(9) 0.0129(7) -0.0093(8) S1 0.0493(7) 0.0688(8) 0.0329(6) -0.0101(5) 0.0114(5) 0.0181(6) O1 0.0435(16) 0.0540(17) 0.0305(14) -0.0046(13) 0.0141(12) 0.0126(13) O2 0.078(2) 0.089(2) 0.0368(17) -0.0195(16) 0.0193(16) 0.0236(17) C1 0.040(2) 0.052(3) 0.034(2) 0.001(2) 0.0167(19) 0.003(2) C2 0.038(2) 0.047(2) 0.030(2) -0.0055(19) 0.0158(17) 0.003(2) C3 0.046(2) 0.060(3) 0.027(2) -0.0016(19) 0.0135(18) 0.004(2) C4 0.044(3) 0.065(3) 0.031(2) 0.010(2) 0.020(2) 0.013(2) C5 0.045(3) 0.097(4) 0.042(3) 0.006(3) 0.018(2) 0.014(3) C6 0.057(3) 0.146(6) 0.051(3) 0.016(4) 0.021(3) 0.028(4) C7 0.078(4) 0.130(6) 0.072(4) 0.046(4) 0.045(4) 0.060(4) C8 0.099(5) 0.070(4) 0.071(4) 0.021(3) 0.050(3) 0.035(3) C9 0.067(3) 0.065(3) 0.048(3) 0.014(2) 0.027(2) 0.018(3) N 0.0446(19) 0.046(2) 0.0320(18) 0.0007(15) 0.0180(15) -0.0084(16) C11 0.070(3) 0.044(3) 0.046(3) -0.008(2) 0.021(2) -0.017(2) C12 0.119(4) 0.067(3) 0.038(3) -0.013(2) 0.030(3) -0.009(3) C13 0.137(5) 0.048(3) 0.075(4) -0.003(3) 0.047(4) 0.012(3) C14 0.058(3) 0.061(3) 0.050(3) 0.011(2) 0.030(2) 0.010(3) C15 0.099(4) 0.051(3) 0.108(4) -0.015(3) 0.067(4) -0.007(3) C16 0.054(3) 0.105(4) 0.073(4) -0.004(3) 0.032(3) -0.006(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 O1 2.004(2) . ? Zn O1 2.004(2) 2 ? Zn S1 2.2523(11) 2 ? Zn S1 2.2524(11) . ? Cl C5 1.740(5) . ? S1 C2 1.756(3) . ? O1 C1 1.290(4) . ? O2 C1 1.232(4) . ? C1 C2 1.510(5) . ? C2 C3 1.340(5) . ? C3 C4 1.456(5) . ? C4 C9 1.386(5) . ? C4 C5 1.401(5) . ? C5 C6 1.371(6) . ? C6 C7 1.384(7) . ? C7 C8 1.366(7) . ? C8 C9 1.372(6) . ? N C11 1.498(4) . ? N C14 1.499(5) . ? C11 C13 1.515(6) . ? C11 C12 1.519(5) . ? C14 C15 1.510(5) . ? C14 C16 1.513(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn O1 109.84(14) . 2 ? O1 Zn S1 117.50(8) . 2 ? O1 Zn S1 88.91(7) 2 2 ? O1 Zn S1 88.91(7) . . ? O1 Zn S1 117.50(8) 2 . ? S1 Zn S1 134.69(7) 2 . ? C2 S1 Zn 95.64(12) . . ? C1 O1 Zn 118.3(2) . . ? O2 C1 O1 120.8(4) . . ? O2 C1 C2 120.8(3) . . ? O1 C1 C2 118.3(3) . . ? C3 C2 C1 117.6(3) . . ? C3 C2 S1 124.1(3) . . ? C1 C2 S1 118.3(3) . . ? C2 C3 C4 129.1(3) . . ? C9 C4 C5 115.9(4) . . ? C9 C4 C3 122.9(4) . . ? C5 C4 C3 121.2(4) . . ? C6 C5 C4 122.3(5) . . ? C6 C5 Cl 118.1(4) . . ? C4 C5 Cl 119.6(4) . . ? C5 C6 C7 119.6(5) . . ? C8 C7 C6 119.6(5) . . ? C7 C8 C9 120.2(5) . . ? C8 C9 C4 122.4(5) . . ? C11 N C14 119.2(3) . . ? N C11 C13 107.1(3) . . ? N C11 C12 110.6(3) . . ? C13 C11 C12 112.0(4) . . ? N C14 C15 107.7(3) . . ? N C14 C16 110.5(3) . . ? C15 C14 C16 112.1(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N H111 O2 0.90 1.89 2.785(4) 170.2 4_575 N H112 O1 0.90 1.91 2.784(4) 164.7 2 _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 28.07 _diffrn_measured_fraction_theta_full 0.919 _refine_diff_density_max 0.695 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.061 #=== data_3 _database_code_depnum_ccdc_archive 'CCDC 741230' ################ # CCDC 741230 # ################ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H40 N2 O4 S4 Zn' _chemical_formula_weight 638.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 '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' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.0680(10) _cell_length_b 15.065(2) _cell_length_c 16.045(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.822(10) _cell_angle_gamma 90.00 _cell_volume 3134.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .10 _exptl_crystal_size_mid .10 _exptl_crystal_size_min .06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 3.841 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.8677 _exptl_absorpt_correction_T_max 0.9972 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAC4' _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 6119 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 69.99 _reflns_number_total 5897 _reflns_number_gt 3846 _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^)+(0.0504P)^2^+0.1206P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5897 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.0953 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 0.69287(3) 0.09090(3) 0.90697(3) 0.03968(12) Uani 1 1 d . . . S1 S 0.86269(6) 0.10179(5) 0.99541(6) 0.04662(19) Uani 1 1 d . . . S2 S 0.55477(6) 0.00687(5) 0.89418(5) 0.04344(18) Uani 1 1 d . . . S3 S 1.08760(7) 0.14457(7) 1.01337(7) 0.0627(3) Uani 1 1 d . . . S4 S 0.31477(7) -0.01267(6) 0.83692(6) 0.0548(2) Uani 1 1 d . . . O11 O 0.67347(15) 0.22052(14) 0.92878(15) 0.0430(5) Uani 1 1 d . . . O12 O 0.75104(17) 0.33562(14) 1.01361(15) 0.0497(5) Uani 1 1 d . . . O21 O 0.67234(15) 0.05963(14) 0.77813(14) 0.0429(5) Uani 1 1 d . . . O22 O 0.59349(17) -0.03680(14) 0.67005(15) 0.0455(5) Uani 1 1 d . . . C11 C 0.7548(2) 0.2622(2) 0.98086(19) 0.0377(6) Uani 1 1 d . . . C12 C 0.8567(2) 0.21810(19) 0.99836(18) 0.0374(6) Uani 1 1 d . . . C13 C 0.9383(2) 0.2708(2) 1.0125(2) 0.0437(7) Uani 1 1 d . . . H13 H 0.9266 0.3308 1.0184 0.052 Uiso 1 1 calc R . . C14 C 1.0416(2) 0.2495(2) 1.0201(2) 0.0472(7) Uani 1 1 d . . . C15 C 1.1176(3) 0.3118(3) 1.0314(3) 0.0595(9) Uani 1 1 d . . . H15 H 1.1087 0.3723 1.0375 0.071 Uiso 1 1 calc R . . C16 C 1.2098(3) 0.2746(4) 1.0327(3) 0.0744(13) Uani 1 1 d . . . H16 H 1.2677 0.3080 1.0389 0.089 Uiso 1 1 calc R . . C17 C 1.2057(3) 0.1863(4) 1.0242(3) 0.0784(14) Uani 1 1 d . . . H17 H 1.2603 0.1515 1.0242 0.094 Uiso 1 1 calc R . . C21 C 0.5994(2) 0.00426(18) 0.73871(19) 0.0344(6) Uani 1 1 d . . . C22 C 0.5183(2) -0.00659(17) 0.77773(19) 0.0346(6) Uani 1 1 d . . . C23 C 0.4207(2) -0.02165(19) 0.7181(2) 0.0407(7) Uani 1 1 d . . . H23 H 0.4135 -0.0327 0.6589 0.049 Uiso 1 1 calc R . . C24 C 0.3258(2) -0.02293(19) 0.7338(2) 0.0416(7) Uani 1 1 d . . . C25 C 0.2294(3) -0.0287(2) 0.6653(3) 0.0534(8) Uani 1 1 d . . . H25 H 0.2187 -0.0348 0.6046 0.064 Uiso 1 1 calc R . . C26 C 0.1487(3) -0.0242(3) 0.6966(3) 0.0687(11) Uani 1 1 d . . . H26 H 0.0792 -0.0268 0.6588 0.082 Uiso 1 1 calc R . . C27 C 0.1826(3) -0.0159(3) 0.7862(3) 0.0663(11) Uani 1 1 d . . . H27 H 0.1395 -0.0122 0.8178 0.080 Uiso 1 1 calc R . . N1 N 0.81319(18) 0.39661(16) 1.19502(16) 0.0386(5) Uani 1 1 d . . . H1A H 0.7918 0.3735 1.1390 0.046 Uiso 1 1 calc R . . H1B H 0.7567 0.4159 1.2029 0.046 Uiso 1 1 calc R . . C111 C 0.8596(3) 0.3222(2) 1.2614(2) 0.0507(8) Uani 1 1 d . . . H111 H 0.8762 0.3454 1.3226 0.061 Uiso 1 1 calc R . . C112 C 0.7773(4) 0.2521(2) 1.2429(3) 0.0786(13) Uani 1 1 d . . . H11J H 0.8005 0.2073 1.2890 0.118 Uiso 1 1 calc R . . H11K H 0.7637 0.2254 1.1850 0.118 Uiso 1 1 calc R . . H11L H 0.7153 0.2788 1.2427 0.118 Uiso 1 1 calc R . . C113 C 0.9578(3) 0.2874(3) 1.2562(3) 0.0785(13) Uani 1 1 d . . . H11D H 0.9851 0.2405 1.2996 0.118 Uiso 1 1 calc R . . H11E H 1.0074 0.3345 1.2692 0.118 Uiso 1 1 calc R . . H11F H 0.9433 0.2648 1.1966 0.118 Uiso 1 1 calc R . . C114 C 0.8785(3) 0.4759(2) 1.1979(2) 0.0481(8) Uani 1 1 d . . . H114 H 0.9410 0.4560 1.1904 0.058 Uiso 1 1 calc R . . C115 C 0.8180(3) 0.5355(3) 1.1194(3) 0.0690(11) Uani 1 1 d . . . H11G H 0.8590 0.5863 1.1191 0.104 Uiso 1 1 calc R . . H11H H 0.7559 0.5546 1.1255 0.104 Uiso 1 1 calc R . . H11I H 0.8007 0.5033 1.0638 0.104 Uiso 1 1 calc R . . C116 C 0.9094(3) 0.5222(3) 1.2882(3) 0.0711(12) Uani 1 1 d . . . H11A H 0.9502 0.5736 1.2891 0.107 Uiso 1 1 calc R . . H11B H 0.9490 0.4823 1.3356 0.107 Uiso 1 1 calc R . . H11C H 0.8486 0.5401 1.2973 0.107 Uiso 1 1 calc R . . N2 N 0.47369(18) 0.29288(15) 0.89102(16) 0.0361(5) Uani 1 1 d . . . H2A H 0.5413 0.2831 0.9052 0.043 Uiso 1 1 calc R . . H2B H 0.4597 0.3481 0.8680 0.043 Uiso 1 1 calc R . . C211 C 0.4548(3) 0.2905(2) 0.9769(2) 0.0420(7) Uani 1 1 d . . . H211 H 0.3805 0.2961 0.9613 0.050 Uiso 1 1 calc R . . C212 C 0.4902(4) 0.2032(2) 1.0241(3) 0.0769(14) Uani 1 1 d . . . H21J H 0.4722 0.2001 1.0760 0.115 Uiso 1 1 calc R . . H21K H 0.5636 0.1982 1.0431 0.115 Uiso 1 1 calc R . . H21L H 0.4572 0.1555 0.9834 0.115 Uiso 1 1 calc R . . C213 C 0.5078(3) 0.3687(2) 1.0342(2) 0.0618(10) Uani 1 1 d . . . H21G H 0.4980 0.3669 1.0902 0.093 Uiso 1 1 calc R . . H21H H 0.4791 0.4227 1.0026 0.093 Uiso 1 1 calc R . . H21I H 0.5802 0.3665 1.0465 0.093 Uiso 1 1 calc R . . C214 C 0.4134(2) 0.2281(2) 0.8177(2) 0.0443(7) Uani 1 1 d . . . H214 H 0.4298 0.1677 0.8417 0.053 Uiso 1 1 calc R . . C215 C 0.2988(3) 0.2426(3) 0.7883(3) 0.0671(11) Uani 1 1 d . . . H21D H 0.2622 0.2017 0.7408 0.101 Uiso 1 1 calc R . . H21E H 0.2819 0.3023 0.7667 0.101 Uiso 1 1 calc R . . H21F H 0.2794 0.2331 0.8388 0.101 Uiso 1 1 calc R . . C216 C 0.4494(3) 0.2389(3) 0.7408(2) 0.0595(9) Uani 1 1 d . . . H21A H 0.5229 0.2320 0.7634 0.089 Uiso 1 1 calc R . . H21B H 0.4309 0.2969 0.7147 0.089 Uiso 1 1 calc R . . H21C H 0.4172 0.1947 0.6955 0.089 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 0.0386(2) 0.0362(2) 0.0439(2) -0.00700(17) 0.01565(17) -0.00479(16) S1 0.0387(4) 0.0415(4) 0.0523(4) 0.0026(3) 0.0096(3) 0.0019(3) S2 0.0493(4) 0.0417(4) 0.0441(4) -0.0013(3) 0.0234(3) -0.0101(3) S3 0.0471(5) 0.0728(6) 0.0686(6) 0.0127(5) 0.0230(4) 0.0119(4) S4 0.0542(5) 0.0560(5) 0.0661(5) -0.0035(4) 0.0364(4) -0.0048(4) O11 0.0321(10) 0.0414(11) 0.0524(12) -0.0096(9) 0.0131(9) 0.0000(8) O12 0.0548(13) 0.0438(12) 0.0549(13) -0.0201(10) 0.0259(11) -0.0028(10) O21 0.0401(11) 0.0443(11) 0.0488(12) -0.0112(10) 0.0221(10) -0.0139(9) O22 0.0536(13) 0.0408(11) 0.0503(13) -0.0134(10) 0.0291(11) -0.0108(10) C11 0.0398(15) 0.0406(15) 0.0358(14) -0.0043(12) 0.0180(12) -0.0035(12) C12 0.0384(15) 0.0414(15) 0.0300(14) -0.0042(12) 0.0108(12) -0.0014(12) C13 0.0398(16) 0.0462(17) 0.0434(17) -0.0057(13) 0.0143(13) -0.0056(13) C14 0.0413(16) 0.059(2) 0.0396(16) 0.0043(15) 0.0138(13) -0.0057(15) C15 0.0452(19) 0.072(2) 0.061(2) 0.0022(19) 0.0210(17) -0.0133(17) C16 0.0363(19) 0.116(4) 0.070(3) 0.012(3) 0.0190(18) -0.009(2) C17 0.038(2) 0.128(4) 0.071(3) 0.025(3) 0.0224(19) 0.020(2) C21 0.0370(14) 0.0270(13) 0.0415(15) -0.0007(11) 0.0176(12) 0.0003(11) C22 0.0393(15) 0.0241(12) 0.0452(16) -0.0034(11) 0.0216(13) -0.0029(11) C23 0.0427(16) 0.0352(15) 0.0478(17) -0.0056(13) 0.0217(14) -0.0035(12) C24 0.0419(16) 0.0345(14) 0.0525(18) 0.0000(13) 0.0228(14) -0.0029(12) C25 0.0403(17) 0.057(2) 0.065(2) 0.0079(17) 0.0228(16) 0.0040(15) C26 0.0374(18) 0.078(3) 0.096(3) 0.014(2) 0.033(2) 0.0063(18) C27 0.054(2) 0.065(2) 0.097(3) 0.003(2) 0.048(2) 0.0016(18) N1 0.0407(13) 0.0379(13) 0.0399(13) -0.0042(10) 0.0184(11) -0.0028(10) C111 0.066(2) 0.0455(18) 0.0420(17) 0.0026(14) 0.0224(16) 0.0105(16) C112 0.117(4) 0.039(2) 0.093(3) 0.006(2) 0.056(3) -0.003(2) C113 0.077(3) 0.091(3) 0.065(3) 0.008(2) 0.025(2) 0.037(2) C114 0.0464(18) 0.0474(18) 0.060(2) -0.0085(15) 0.0304(16) -0.0123(14) C115 0.093(3) 0.050(2) 0.073(3) 0.0089(19) 0.041(2) -0.008(2) C116 0.074(3) 0.067(3) 0.067(3) -0.019(2) 0.021(2) -0.030(2) N2 0.0401(13) 0.0318(12) 0.0413(13) 0.0028(10) 0.0211(11) 0.0042(10) C211 0.0516(18) 0.0403(16) 0.0437(16) -0.0014(13) 0.0290(14) 0.0003(13) C212 0.149(4) 0.042(2) 0.064(2) 0.0160(18) 0.068(3) 0.010(2) C213 0.092(3) 0.047(2) 0.0488(19) -0.0061(16) 0.030(2) -0.0095(19) C214 0.0518(18) 0.0362(15) 0.0439(17) -0.0029(13) 0.0173(14) 0.0017(13) C215 0.049(2) 0.082(3) 0.065(2) -0.016(2) 0.0167(18) -0.009(2) C216 0.069(2) 0.069(2) 0.0426(18) -0.0063(17) 0.0230(17) 0.0104(19) _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 O11 2.021(2) . ? Zn O21 2.029(2) . ? Zn S2 2.2605(8) . ? Zn S1 2.2622(9) . ? S1 C12 1.756(3) . ? S2 C22 1.747(3) . ? S3 C17 1.721(4) . ? S3 C14 1.726(4) . ? S4 C27 1.717(4) . ? S4 C24 1.727(3) . ? O11 C11 1.288(3) . ? O12 C11 1.235(4) . ? O21 C21 1.283(3) . ? O22 C21 1.238(3) . ? C11 C12 1.504(4) . ? C12 C13 1.341(4) . ? C13 C14 1.447(4) . ? C14 C15 1.381(5) . ? C15 C16 1.406(6) . ? C16 C17 1.336(7) . ? C21 C22 1.507(4) . ? C22 C23 1.354(4) . ? C23 C24 1.452(4) . ? C24 C25 1.378(5) . ? C25 C26 1.411(5) . ? C26 C27 1.334(6) . ? N1 C114 1.497(4) . ? N1 C111 1.509(4) . ? C111 C113 1.510(5) . ? C111 C112 1.510(5) . ? C114 C115 1.512(5) . ? C114 C116 1.513(5) . ? N2 C211 1.501(3) . ? N2 C214 1.511(4) . ? C211 C213 1.503(4) . ? C211 C212 1.504(4) . ? C214 C215 1.510(5) . ? C214 C216 1.514(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 O11 Zn O21 115.18(9) . . ? O11 Zn S2 112.82(6) . . ? O21 Zn S2 89.98(6) . . ? O11 Zn S1 90.12(6) . . ? O21 Zn S1 110.75(6) . . ? S2 Zn S1 139.36(3) . . ? C12 S1 Zn 92.27(10) . . ? C22 S2 Zn 92.72(9) . . ? C17 S3 C14 91.7(2) . . ? C27 S4 C24 91.56(18) . . ? C11 O11 Zn 115.92(18) . . ? C21 O21 Zn 115.07(18) . . ? O12 C11 O11 122.6(3) . . ? O12 C11 C12 120.8(3) . . ? O11 C11 C12 116.7(3) . . ? C13 C12 C11 117.5(3) . . ? C13 C12 S1 123.3(2) . . ? C11 C12 S1 119.2(2) . . ? C12 C13 C14 130.4(3) . . ? C15 C14 C13 124.1(3) . . ? C15 C14 S3 110.0(3) . . ? C13 C14 S3 125.9(3) . . ? C14 C15 C16 113.1(4) . . ? C17 C16 C15 113.1(4) . . ? C16 C17 S3 112.0(3) . . ? O22 C21 O21 121.9(3) . . ? O22 C21 C22 121.0(2) . . ? O21 C21 C22 117.1(2) . . ? C23 C22 C21 116.6(3) . . ? C23 C22 S2 124.8(2) . . ? C21 C22 S2 118.4(2) . . ? C22 C23 C24 129.0(3) . . ? C25 C24 C23 123.3(3) . . ? C25 C24 S4 110.1(2) . . ? C23 C24 S4 126.6(3) . . ? C24 C25 C26 113.0(4) . . ? C27 C26 C25 112.8(4) . . ? C26 C27 S4 112.5(3) . . ? C114 N1 C111 118.6(3) . . ? N1 C111 C113 112.0(3) . . ? N1 C111 C112 106.9(3) . . ? C113 C111 C112 113.2(3) . . ? N1 C114 C115 107.9(3) . . ? N1 C114 C116 110.0(3) . . ? C115 C114 C116 112.6(3) . . ? C211 N2 C214 117.0(2) . . ? N2 C211 C213 108.7(3) . . ? N2 C211 C212 110.0(3) . . ? C213 C211 C212 112.9(3) . . ? C215 C214 N2 111.0(3) . . ? C215 C214 C216 112.6(3) . . ? N2 C214 C216 107.5(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 O11 Zn S1 C12 -11.22(12) . . . . ? O21 Zn S1 C12 105.89(12) . . . . ? S2 Zn S1 C12 -137.94(10) . . . . ? O11 Zn S2 C22 107.42(11) . . . . ? O21 Zn S2 C22 -10.06(11) . . . . ? S1 Zn S2 C22 -133.00(10) . . . . ? O21 Zn O11 C11 -113.7(2) . . . . ? S2 Zn O11 C11 144.88(19) . . . . ? S1 Zn O11 C11 -0.6(2) . . . . ? O11 Zn O21 C21 -119.0(2) . . . . ? S2 Zn O21 C21 -3.6(2) . . . . ? S1 Zn O21 C21 140.61(18) . . . . ? Zn O11 C11 O12 -165.9(2) . . . . ? Zn O11 C11 C12 15.8(3) . . . . ? O12 C11 C12 C13 -29.5(4) . . . . ? O11 C11 C12 C13 148.8(3) . . . . ? O12 C11 C12 S1 152.7(2) . . . . ? O11 C11 C12 S1 -29.0(4) . . . . ? Zn S1 C12 C13 -154.5(3) . . . . ? Zn S1 C12 C11 23.1(2) . . . . ? C11 C12 C13 C14 -171.6(3) . . . . ? S1 C12 C13 C14 6.1(5) . . . . ? C12 C13 C14 C15 177.4(3) . . . . ? C12 C13 C14 S3 -0.7(5) . . . . ? C17 S3 C14 C15 -0.7(3) . . . . ? C17 S3 C14 C13 177.6(3) . . . . ? C13 C14 C15 C16 -177.2(3) . . . . ? S3 C14 C15 C16 1.1(4) . . . . ? C14 C15 C16 C17 -1.0(5) . . . . ? C15 C16 C17 S3 0.4(5) . . . . ? C14 S3 C17 C16 0.2(4) . . . . ? Zn O21 C21 O22 -162.4(2) . . . . ? Zn O21 C21 C22 19.7(3) . . . . ? O22 C21 C22 C23 -33.0(4) . . . . ? O21 C21 C22 C23 145.0(3) . . . . ? O22 C21 C22 S2 150.4(2) . . . . ? O21 C21 C22 S2 -31.7(3) . . . . ? Zn S2 C22 C23 -153.2(2) . . . . ? Zn S2 C22 C21 23.2(2) . . . . ? C21 C22 C23 C24 -170.9(3) . . . . ? S2 C22 C23 C24 5.5(5) . . . . ? C22 C23 C24 C25 172.0(3) . . . . ? C22 C23 C24 S4 -4.9(5) . . . . ? C27 S4 C24 C25 -0.2(3) . . . . ? C27 S4 C24 C23 177.0(3) . . . . ? C23 C24 C25 C26 -176.9(3) . . . . ? S4 C24 C25 C26 0.3(4) . . . . ? C24 C25 C26 C27 -0.4(5) . . . . ? C25 C26 C27 S4 0.2(5) . . . . ? C24 S4 C27 C26 0.0(3) . . . . ? C114 N1 C111 C113 -55.4(4) . . . . ? C114 N1 C111 C112 -179.8(3) . . . . ? C111 N1 C114 C115 174.4(3) . . . . ? C111 N1 C114 C116 -62.4(4) . . . . ? C214 N2 C211 C213 -170.8(3) . . . . ? C214 N2 C211 C212 65.2(4) . . . . ? C211 N2 C214 C215 59.7(4) . . . . ? C211 N2 C214 C216 -176.8(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1B O21 0.90 2.03 2.862(3) 153.6 4_566 N1 H1A O12 0.90 1.95 2.847(3) 173.5 . N2 H2A O11 0.90 1.99 2.852(3) 161.0 . N2 H2B O22 0.90 1.89 2.778(3) 167.1 2_656 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 69.99 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.239 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.061 #=== data_4 _database_code_depnum_ccdc_archive 'CCDC 741231' ################ # CCDC 741231 # ################ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H40 N2 O6 S2 Zn' _chemical_formula_weight 606.09 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 9.0837(11) _cell_length_b 12.8696(15) _cell_length_c 14.8088(17) _cell_angle_alpha 69.626(2) _cell_angle_beta 75.541(2) _cell_angle_gamma 81.680(2) _cell_volume 1568.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 0.954 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.578501 _exptl_absorpt_correction_T_max 1.000000 _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 '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 7703 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.04 _reflns_number_total 5756 _reflns_number_gt 3704 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5756 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0837 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 0.866 _refine_ls_restrained_S_all 0.866 _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 0.88190(4) 0.51978(2) 0.18957(2) 0.05170(11) Uani 1 1 d . . . S1 S 0.89204(9) 0.70308(5) 0.10048(5) 0.0576(2) Uani 1 1 d . . . O11 O 0.7836(2) 0.49669(14) 0.09224(13) 0.0567(5) Uani 1 1 d . . . O12 O 0.6749(2) 0.57762(15) -0.03447(14) 0.0643(5) Uani 1 1 d . . . O13 O 0.8412(3) 0.94772(19) -0.20515(15) 0.1047(9) Uani 1 1 d . . . C11 C 0.7539(3) 0.5824(2) 0.0215(2) 0.0485(7) Uani 1 1 d . . . C12 C 0.8156(3) 0.6915(2) 0.00722(18) 0.0440(6) Uani 1 1 d . . . C13 C 0.8100(3) 0.7733(2) -0.07863(19) 0.0527(7) Uani 1 1 d . . . H13 H 0.7675 0.7556 -0.1220 0.063 Uiso 1 1 calc R . . C14 C 0.8601(3) 0.8835(2) -0.1127(2) 0.0571(7) Uani 1 1 d . . . C15 C 0.8987(5) 1.0483(3) -0.2230(3) 0.1091(15) Uani 1 1 d . . . H15 H 0.9019 1.1078 -0.2812 0.131 Uiso 1 1 calc R . . C16 C 0.9479(5) 1.0491(3) -0.1481(3) 0.0922(12) Uani 1 1 d . . . H16 H 0.9896 1.1080 -0.1427 0.111 Uiso 1 1 calc R . . C17 C 0.9252(4) 0.9423(2) -0.0761(2) 0.0670(9) Uani 1 1 d . . . H17 H 0.9510 0.9178 -0.0147 0.080 Uiso 1 1 calc R . . S2 S 1.03860(8) 0.38225(6) 0.26441(5) 0.0589(2) Uani 1 1 d . . . O21 O 0.7245(2) 0.48351(14) 0.31891(12) 0.0518(5) Uani 1 1 d . . . O22 O 0.6520(2) 0.35645(17) 0.46384(14) 0.0771(6) Uani 1 1 d . . . O23 O 1.0574(3) 0.08417(18) 0.54375(16) 0.0925(7) Uani 1 1 d . . . C21 C 0.7489(3) 0.3925(2) 0.38694(19) 0.0487(7) Uani 1 1 d . . . C22 C 0.9021(3) 0.33057(19) 0.37291(17) 0.0422(6) Uani 1 1 d . . . C23 C 0.9274(3) 0.2384(2) 0.44721(19) 0.0510(7) Uani 1 1 d . . . H23 H 0.8466 0.2192 0.5014 0.061 Uiso 1 1 calc R . . C24 C 1.0626(4) 0.1658(2) 0.4538(2) 0.0574(7) Uani 1 1 d . . . C25 C 1.1926(6) 0.0247(3) 0.5363(4) 0.1104(16) Uani 1 1 d . . . H25 H 1.2192 -0.0365 0.5870 0.133 Uiso 1 1 calc R . . C26 C 1.2826(5) 0.0639(3) 0.4483(4) 0.0996(13) Uani 1 1 d . . . H26 H 1.3807 0.0370 0.4263 0.120 Uiso 1 1 calc R . . C27 C 1.1977(4) 0.1554(2) 0.3948(3) 0.0708(9) Uani 1 1 d . . . H27 H 1.2303 0.2004 0.3299 0.085 Uiso 1 1 calc R . . N3 N 0.3771(2) 0.34443(16) 0.59505(15) 0.0519(6) Uani 1 1 d . . . H3A H 0.3541 0.4053 0.6138 0.062 Uiso 1 1 calc R . . H3B H 0.4643 0.3557 0.5489 0.062 Uiso 1 1 calc R . . C31 C 0.2538(4) 0.3369(2) 0.5467(2) 0.0655(8) Uani 1 1 d . . . H31 H 0.2764 0.2697 0.5277 0.079 Uiso 1 1 calc R . . C32 C 0.2571(4) 0.4357(3) 0.4547(2) 0.0864(11) Uani 1 1 d . . . H32A H 0.3563 0.4376 0.4122 0.130 Uiso 1 1 calc R . . H32B H 0.2350 0.5025 0.4720 0.130 Uiso 1 1 calc R . . H32C H 0.1822 0.4301 0.4212 0.130 Uiso 1 1 calc R . . C33 C 0.1001(4) 0.3278(3) 0.6182(3) 0.0948(11) Uani 1 1 d . . . H33A H 0.1042 0.2639 0.6757 0.142 Uiso 1 1 calc R . . H33B H 0.0233 0.3203 0.5869 0.142 Uiso 1 1 calc R . . H33C H 0.0755 0.3934 0.6372 0.142 Uiso 1 1 calc R . . C34 C 0.4083(4) 0.2485(2) 0.6828(2) 0.0673(8) Uani 1 1 d . . . H34 H 0.3150 0.2366 0.7346 0.081 Uiso 1 1 calc R . . C35 C 0.4542(5) 0.1437(2) 0.6556(3) 0.1049(13) Uani 1 1 d . . . H35A H 0.3740 0.1272 0.6319 0.157 Uiso 1 1 calc R . . H35B H 0.4722 0.0831 0.7126 0.157 Uiso 1 1 calc R . . H35C H 0.5456 0.1542 0.6048 0.157 Uiso 1 1 calc R . . C36 C 0.5292(4) 0.2784(3) 0.7205(3) 0.0938(11) Uani 1 1 d . . . H36A H 0.4953 0.3444 0.7381 0.141 Uiso 1 1 calc R . . H36B H 0.6209 0.2915 0.6701 0.141 Uiso 1 1 calc R . . H36C H 0.5490 0.2185 0.7775 0.141 Uiso 1 1 calc R . . N4 N 0.6050(3) 0.32745(16) 0.07662(15) 0.0556(6) Uani 1 1 d . . . H4A H 0.5136 0.3537 0.0619 0.067 Uiso 1 1 calc R . . H4B H 0.6574 0.3866 0.0652 0.067 Uiso 1 1 calc R . . C41 C 0.6875(4) 0.2677(2) 0.0057(2) 0.0681(8) Uani 1 1 d . . . H41 H 0.7923 0.2477 0.0149 0.082 Uiso 1 1 calc R . . C42 C 0.6921(4) 0.3472(3) -0.0985(2) 0.0861(10) Uani 1 1 d . . . H42A H 0.7427 0.4119 -0.1081 0.129 Uiso 1 1 calc R . . H42B H 0.5900 0.3687 -0.1082 0.129 Uiso 1 1 calc R . . H42C H 0.7465 0.3111 -0.1451 0.129 Uiso 1 1 calc R . . C43 C 0.6116(4) 0.1616(3) 0.0244(3) 0.0980(12) Uani 1 1 d . . . H43A H 0.6119 0.1132 0.0905 0.147 Uiso 1 1 calc R . . H43B H 0.6668 0.1250 -0.0216 0.147 Uiso 1 1 calc R . . H43C H 0.5085 0.1800 0.0161 0.147 Uiso 1 1 calc R . . C44 C 0.5786(3) 0.2643(2) 0.1854(2) 0.0629(8) Uani 1 1 d . . . H44 H 0.5145 0.2030 0.1997 0.075 Uiso 1 1 calc R . . C45 C 0.4930(4) 0.3423(3) 0.2400(2) 0.0737(9) Uani 1 1 d . . . H45A H 0.3993 0.3703 0.2186 0.111 Uiso 1 1 calc R . . H45B H 0.5542 0.4031 0.2264 0.111 Uiso 1 1 calc R . . H45C H 0.4713 0.3030 0.3096 0.111 Uiso 1 1 calc R . . C46 C 0.7290(4) 0.2157(3) 0.2150(3) 0.0939(11) Uani 1 1 d . . . H46A H 0.7775 0.1661 0.1791 0.141 Uiso 1 1 calc R . . H46B H 0.7105 0.1757 0.2845 0.141 Uiso 1 1 calc R . . H46C H 0.7941 0.2747 0.2001 0.141 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 0.0559(2) 0.04917(18) 0.04813(19) -0.01004(15) -0.01419(15) -0.00664(15) S1 0.0769(6) 0.0497(4) 0.0505(4) -0.0101(3) -0.0236(4) -0.0158(4) O11 0.0686(14) 0.0491(10) 0.0551(11) -0.0105(9) -0.0206(10) -0.0157(9) O12 0.0604(14) 0.0745(13) 0.0694(13) -0.0230(11) -0.0286(11) -0.0148(10) O13 0.169(3) 0.0825(16) 0.0559(14) 0.0023(13) -0.0375(16) -0.0281(16) C11 0.0405(17) 0.0571(16) 0.0493(16) -0.0203(14) -0.0047(13) -0.0089(13) C12 0.0378(16) 0.0507(14) 0.0426(15) -0.0153(12) -0.0056(12) -0.0045(12) C13 0.0562(19) 0.0595(17) 0.0453(15) -0.0163(14) -0.0144(14) -0.0085(14) C14 0.071(2) 0.0523(16) 0.0418(16) -0.0075(13) -0.0126(14) -0.0042(14) C15 0.175(5) 0.055(2) 0.072(3) 0.0106(19) -0.016(3) -0.027(2) C16 0.136(4) 0.061(2) 0.076(2) -0.0200(19) -0.009(2) -0.026(2) C17 0.104(3) 0.0478(16) 0.0477(17) -0.0096(14) -0.0169(17) -0.0150(16) S2 0.0456(5) 0.0636(4) 0.0509(4) -0.0057(3) -0.0024(3) 0.0019(3) O21 0.0508(12) 0.0507(10) 0.0520(11) -0.0183(9) -0.0086(9) 0.0019(8) O22 0.0599(15) 0.0920(15) 0.0558(12) -0.0129(11) 0.0097(11) 0.0013(11) O23 0.124(2) 0.0688(14) 0.0718(15) 0.0022(12) -0.0408(15) 0.0068(14) C21 0.0475(18) 0.0575(16) 0.0468(16) -0.0256(14) -0.0058(14) -0.0070(13) C22 0.0408(16) 0.0474(14) 0.0397(14) -0.0166(12) -0.0054(12) -0.0061(11) C23 0.0551(19) 0.0512(15) 0.0436(15) -0.0125(13) -0.0070(13) -0.0071(13) C24 0.073(2) 0.0453(15) 0.0566(18) -0.0123(14) -0.0252(17) -0.0039(15) C25 0.149(5) 0.060(2) 0.135(4) -0.019(3) -0.089(4) 0.027(3) C26 0.100(3) 0.073(3) 0.141(4) -0.046(3) -0.056(3) 0.027(2) C27 0.068(2) 0.0568(18) 0.085(2) -0.0210(17) -0.023(2) 0.0097(16) N3 0.0531(15) 0.0509(12) 0.0540(14) -0.0247(11) -0.0054(11) -0.0019(10) C31 0.065(2) 0.070(2) 0.078(2) -0.0411(18) -0.0196(18) -0.0051(16) C32 0.096(3) 0.097(2) 0.083(2) -0.036(2) -0.043(2) 0.004(2) C33 0.061(2) 0.127(3) 0.110(3) -0.054(3) -0.010(2) -0.027(2) C34 0.080(2) 0.0594(18) 0.0534(18) -0.0146(15) -0.0036(17) -0.0044(16) C35 0.147(4) 0.054(2) 0.106(3) -0.022(2) -0.025(3) 0.004(2) C36 0.114(3) 0.089(2) 0.083(3) -0.024(2) -0.046(2) 0.014(2) N4 0.0567(16) 0.0501(13) 0.0598(15) -0.0124(12) -0.0155(12) -0.0111(11) C41 0.058(2) 0.0706(19) 0.077(2) -0.0316(18) -0.0064(17) -0.0022(15) C42 0.085(3) 0.107(3) 0.070(2) -0.037(2) -0.0100(19) -0.005(2) C43 0.098(3) 0.082(2) 0.124(3) -0.059(2) 0.000(2) -0.016(2) C44 0.070(2) 0.0591(17) 0.0558(18) -0.0040(15) -0.0187(16) -0.0208(16) C45 0.074(2) 0.092(2) 0.0559(19) -0.0221(18) -0.0078(16) -0.0238(18) C46 0.102(3) 0.083(2) 0.091(3) -0.005(2) -0.049(2) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn O11 1.9950(17) . ? Zn O21 2.0330(17) . ? Zn S2 2.2539(8) . ? Zn S1 2.2692(7) . ? S1 C12 1.750(3) . ? O11 C11 1.280(3) . ? O12 C11 1.245(3) . ? O13 C14 1.370(3) . ? O13 C15 1.380(4) . ? C11 C12 1.515(3) . ? C12 C13 1.346(3) . ? C13 C14 1.431(4) . ? C14 C17 1.339(4) . ? C15 C16 1.299(4) . ? C16 C17 1.421(4) . ? S2 C22 1.750(2) . ? O21 C21 1.285(3) . ? O22 C21 1.240(3) . ? O23 C25 1.351(5) . ? O23 C24 1.375(3) . ? C21 C22 1.504(3) . ? C22 C23 1.346(3) . ? C23 C24 1.433(4) . ? C24 C27 1.337(4) . ? C25 C26 1.324(5) . ? C26 C27 1.415(4) . ? N3 C31 1.501(3) . ? N3 C34 1.503(3) . ? C31 C32 1.503(4) . ? C31 C33 1.519(4) . ? C34 C36 1.498(4) . ? C34 C35 1.513(4) . ? N4 C41 1.503(3) . ? N4 C44 1.505(3) . ? C41 C42 1.520(4) . ? C41 C43 1.526(4) . ? C44 C45 1.514(4) . ? C44 C46 1.520(4) . ? 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 O11 Zn O21 105.74(7) . . ? O11 Zn S2 118.72(6) . . ? O21 Zn S2 88.64(5) . . ? O11 Zn S1 89.70(5) . . ? O21 Zn S1 115.03(5) . . ? S2 Zn S1 137.39(3) . . ? C12 S1 Zn 94.33(8) . . ? C11 O11 Zn 117.48(16) . . ? C14 O13 C15 105.7(3) . . ? O12 C11 O11 121.4(2) . . ? O12 C11 C12 120.0(2) . . ? O11 C11 C12 118.6(2) . . ? C13 C12 C11 116.8(2) . . ? C13 C12 S1 124.33(19) . . ? C11 C12 S1 118.88(19) . . ? C12 C13 C14 129.2(3) . . ? C17 C14 O13 108.9(2) . . ? C17 C14 C13 135.4(3) . . ? O13 C14 C13 115.7(3) . . ? C16 C15 O13 111.3(3) . . ? C15 C16 C17 106.5(3) . . ? C14 C17 C16 107.5(3) . . ? C22 S2 Zn 95.15(9) . . ? C21 O21 Zn 117.07(16) . . ? C25 O23 C24 106.1(3) . . ? O22 C21 O21 122.0(3) . . ? O22 C21 C22 119.7(2) . . ? O21 C21 C22 118.2(2) . . ? C23 C22 C21 117.1(2) . . ? C23 C22 S2 123.4(2) . . ? C21 C22 S2 119.48(18) . . ? C22 C23 C24 128.5(3) . . ? C27 C24 O23 108.8(3) . . ? C27 C24 C23 136.9(3) . . ? O23 C24 C23 114.3(3) . . ? C26 C25 O23 111.8(4) . . ? C25 C26 C27 105.4(4) . . ? C24 C27 C26 108.0(3) . . ? C31 N3 C34 118.7(2) . . ? N3 C31 C32 108.5(2) . . ? N3 C31 C33 110.6(2) . . ? C32 C31 C33 112.8(3) . . ? C36 C34 N3 108.4(2) . . ? C36 C34 C35 111.9(3) . . ? N3 C34 C35 110.6(2) . . ? C41 N4 C44 118.5(2) . . ? N4 C41 C42 108.2(2) . . ? N4 C41 C43 111.2(2) . . ? C42 C41 C43 111.8(3) . . ? N4 C44 C45 107.9(2) . . ? N4 C44 C46 110.4(2) . . ? C45 C44 C46 113.0(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3B O22 0.90 1.85 2.741(3) 171.2 . N4 H4B O11 0.90 2.14 2.999(3) 159.4 . N4 H4B O12 0.90 2.39 3.140(3) 140.8 . N3 H3A O21 0.90 1.97 2.857(2) 167.2 2_666 N4 H4A O12 0.90 1.88 2.777(3) 173.7 2_665 _diffrn_measured_fraction_theta_max 0.760 _diffrn_reflns_theta_full 28.04 _diffrn_measured_fraction_theta_full 0.760 _refine_diff_density_max 0.373 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.042 #=== data_5 _database_code_depnum_ccdc_archive 'CCDC 741232' ################ # CCDC 741232 # ################ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H44 Cd N2 O4 S2' _chemical_formula_weight 673.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 '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' Cd Cd 0.1185 4.6533 '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 13.901(2) _cell_length_b 9.9576(17) _cell_length_c 25.286(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.500(10) _cell_angle_gamma 90.00 _cell_volume 3477.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .45 _exptl_crystal_size_mid .40 _exptl_crystal_size_min .13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 6.410 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.0978 _exptl_absorpt_correction_T_max 0.4972 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _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 6874 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 70.21 _reflns_number_total 6586 _reflns_number_gt 5290 _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^)+(0.0657P)^2^+2.7246P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00256(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6586 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1189 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Cd Cd 0.382252(19) 0.51209(3) 0.029723(10) 0.06283(13) Uani 1 1 d . . . S1 S 0.36601(7) 0.41286(16) 0.11467(4) 0.0872(4) Uani 1 1 d . . . S2 S 0.40776(6) 0.49345(8) -0.06516(3) 0.0551(2) Uani 1 1 d . . . O11 O 0.2127(2) 0.4837(4) 0.02527(13) 0.0969(12) Uani 1 1 d . . . O12 O 0.0893(2) 0.4031(8) 0.06209(17) 0.165(2) Uani 1 1 d . . . C11 C 0.1775(3) 0.4267(7) 0.06332(18) 0.0943(15) Uani 1 1 d . . . C12 C 0.2429(3) 0.3821(5) 0.11105(15) 0.0723(10) Uani 1 1 d . . . C13 C 0.2015(4) 0.3197(6) 0.1501(2) 0.0952(14) Uani 1 1 d . . . H13 H 0.1351 0.3071 0.1424 0.114 Uiso 1 1 calc R . . C14 C 0.2413(3) 0.2679(4) 0.20246(13) 0.1047(17) Uani 1 1 d G . . C15 C 0.3358(3) 0.2881(5) 0.22550(16) 0.129(2) Uani 1 1 d G . . H15 H 0.3791 0.3358 0.2072 0.155 Uiso 1 1 calc R . . C16 C 0.3655(4) 0.2371(6) 0.27586(17) 0.166(3) Uani 1 1 d G . . H16 H 0.4287 0.2506 0.2913 0.200 Uiso 1 1 calc R . . C17 C 0.3008(5) 0.1658(6) 0.30319(14) 0.200(5) Uani 1 1 d G . . H17 H 0.3207 0.1316 0.3369 0.240 Uiso 1 1 calc R . . C18 C 0.2063(5) 0.1455(5) 0.2802(2) 0.191(5) Uani 1 1 d G . . H18 H 0.1630 0.0978 0.2984 0.229 Uiso 1 1 calc R . . C19 C 0.1765(3) 0.1966(5) 0.2298(2) 0.150(3) Uani 1 1 d G . . H19 H 0.1133 0.1830 0.2144 0.180 Uiso 1 1 calc R . . O21 O 0.3948(2) 0.7311(3) 0.01102(11) 0.0797(8) Uani 1 1 d . . . O22 O 0.4322(3) 0.8850(3) -0.04510(14) 0.1014(10) Uani 1 1 d . . . C21 C 0.4107(3) 0.7680(4) -0.03480(17) 0.0698(9) Uani 1 1 d . . . C22 C 0.4002(2) 0.6657(3) -0.08024(13) 0.0571(8) Uani 1 1 d . . . C23 C 0.3836(3) 0.7159(4) -0.12963(15) 0.0693(9) Uani 1 1 d . . . H23 H 0.3807 0.8091 -0.1309 0.083 Uiso 1 1 calc R . . C24 C 0.3692(2) 0.6523(3) -0.18147(9) 0.0765(11) Uani 1 1 d G . . C25 C 0.3218(3) 0.7296(3) -0.22213(14) 0.1108(18) Uani 1 1 d G . . H25 H 0.3008 0.8157 -0.2150 0.133 Uiso 1 1 calc R . . C26 C 0.3058(3) 0.6784(5) -0.27351(11) 0.153(3) Uani 1 1 d G . . H26 H 0.2741 0.7301 -0.3007 0.183 Uiso 1 1 calc R . . C27 C 0.3373(4) 0.5497(5) -0.28421(9) 0.155(3) Uani 1 1 d G . . H27 H 0.3266 0.5154 -0.3186 0.186 Uiso 1 1 calc R . . C28 C 0.3847(3) 0.4724(4) -0.24354(13) 0.124(2) Uani 1 1 d G . . H28 H 0.4057 0.3863 -0.2507 0.149 Uiso 1 1 calc R . . C29 C 0.4007(3) 0.5236(3) -0.19217(11) 0.0883(13) Uani 1 1 d G . . H29 H 0.4324 0.4719 -0.1650 0.106 Uiso 1 1 calc R . . N1 N 0.4198(3) 0.9610(4) 0.08032(15) 0.0864(11) Uani 1 1 d . . . H1A H 0.4638 1.0222 0.0726 0.104 Uiso 1 1 calc R . . H1B H 0.4146 0.9004 0.0537 0.104 Uiso 1 1 calc R . . C111 C 0.3246(5) 1.0311(7) 0.0792(3) 0.122(2) Uani 1 1 d . . . H111 H 0.3294 1.0998 0.1071 0.146 Uiso 1 1 calc R . . C112 C 0.3023(6) 1.0974(8) 0.0266(3) 0.152(3) Uani 1 1 d . . . H11A H 0.2922 1.0304 -0.0007 0.228 Uiso 1 1 calc R . . H11B H 0.3555 1.1540 0.0199 0.228 Uiso 1 1 calc R . . H11C H 0.2449 1.1508 0.0268 0.228 Uiso 1 1 calc R . . C113 C 0.2450(6) 0.9333(11) 0.0889(4) 0.188(4) Uani 1 1 d . . . H11D H 0.1838 0.9788 0.0846 0.282 Uiso 1 1 calc R . . H11E H 0.2570 0.8982 0.1243 0.282 Uiso 1 1 calc R . . H11F H 0.2439 0.8609 0.0637 0.282 Uiso 1 1 calc R . . C114 C 0.4603(5) 0.8900(6) 0.1301(2) 0.1136(19) Uani 1 1 d . . . H114 H 0.4194 0.8118 0.1350 0.136 Uiso 1 1 calc R . . C115 C 0.5590(6) 0.8415(6) 0.1226(3) 0.138(3) Uani 1 1 d . . . H11G H 0.5826 0.7848 0.1519 0.208 Uiso 1 1 calc R . . H11H H 0.6016 0.9170 0.1211 0.208 Uiso 1 1 calc R . . H11I H 0.5565 0.7915 0.0900 0.208 Uiso 1 1 calc R . . C116 C 0.4599(7) 0.9806(7) 0.1784(2) 0.149(3) Uani 1 1 d . . . H11J H 0.3944 1.0034 0.1833 0.223 Uiso 1 1 calc R . . H11K H 0.4955 1.0611 0.1730 0.223 Uiso 1 1 calc R . . H11L H 0.4896 0.9346 0.2094 0.223 Uiso 1 1 calc R . . N2 N 0.9146(3) 0.5071(6) 0.06951(19) 0.128(3) Uani 1 1 d . . . H2A H 0.8843 0.5110 0.0361 0.154 Uiso 1 1 calc R . . H2B H 0.9737 0.4717 0.0679 0.154 Uiso 1 1 calc R . . C211 C 0.9260(5) 0.6520(9) 0.0922(3) 0.136(3) Uani 1 1 d . . . H211 H 0.9547 0.6468 0.1294 0.163 Uiso 1 1 calc R . . C212 C 0.8305(6) 0.7130(10) 0.0906(3) 0.171(4) Uani 1 1 d . . . H21A H 0.8369 0.8038 0.1033 0.256 Uiso 1 1 calc R . . H21B H 0.7919 0.6626 0.1128 0.256 Uiso 1 1 calc R . . H21C H 0.7997 0.7127 0.0546 0.256 Uiso 1 1 calc R . . C213 C 0.9998(6) 0.7234(11) 0.0588(4) 0.193(4) Uani 1 1 d . . . H21D H 1.0103 0.8140 0.0712 0.290 Uiso 1 1 calc R . . H21E H 0.9742 0.7245 0.0220 0.290 Uiso 1 1 calc R . . H21F H 1.0602 0.6756 0.0629 0.290 Uiso 1 1 calc R . . C214 C 0.8607(3) 0.4203(10) 0.1008(2) 0.123(3) Uani 1 1 d . . . H214 H 0.7940 0.4529 0.1001 0.148 Uiso 1 1 calc R . . C215 C 0.9075(4) 0.4093(10) 0.1583(2) 0.154(3) Uani 1 1 d . . . H21G H 0.8698 0.3503 0.1778 0.232 Uiso 1 1 calc R . . H21H H 0.9102 0.4966 0.1745 0.232 Uiso 1 1 calc R . . H21I H 0.9719 0.3742 0.1587 0.232 Uiso 1 1 calc R . . C216 C 0.8617(6) 0.2763(9) 0.0701(3) 0.153(3) Uani 1 1 d . . . H21J H 0.8347 0.2083 0.0909 0.230 Uiso 1 1 calc R . . H21K H 0.9271 0.2529 0.0652 0.230 Uiso 1 1 calc R . . H21L H 0.8238 0.2831 0.0360 0.230 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 Cd 0.06107(19) 0.0722(2) 0.05675(18) -0.00008(11) 0.01330(12) 0.00626(11) S1 0.0555(5) 0.1515(11) 0.0544(5) 0.0136(6) 0.0055(4) 0.0026(6) S2 0.0551(4) 0.0582(5) 0.0520(4) -0.0014(3) 0.0059(3) 0.0028(3) O11 0.0559(16) 0.170(4) 0.0645(17) 0.0188(18) 0.0044(13) 0.0165(17) O12 0.0485(18) 0.327(8) 0.118(3) 0.041(4) 0.0086(18) 0.005(3) C11 0.045(2) 0.170(5) 0.069(2) 0.002(3) 0.0096(18) 0.004(3) C12 0.056(2) 0.104(3) 0.0583(19) -0.004(2) 0.0147(16) 0.001(2) C13 0.082(3) 0.119(4) 0.089(3) -0.004(3) 0.029(2) -0.007(3) C14 0.148(5) 0.093(3) 0.081(3) 0.012(3) 0.049(3) -0.001(3) C15 0.156(6) 0.147(6) 0.082(3) 0.028(4) 0.003(4) -0.018(5) C16 0.254(10) 0.160(7) 0.082(4) 0.036(4) 0.003(5) 0.009(7) C17 0.372(17) 0.133(7) 0.100(5) 0.034(5) 0.049(8) 0.026(9) C18 0.315(15) 0.140(7) 0.133(7) 0.049(6) 0.091(8) -0.025(8) C19 0.206(8) 0.125(5) 0.132(5) 0.025(4) 0.081(5) -0.007(5) O21 0.110(2) 0.0641(16) 0.0643(15) -0.0083(13) 0.0047(14) 0.0110(14) O22 0.137(3) 0.0595(17) 0.108(2) -0.0087(16) 0.019(2) -0.0113(17) C21 0.071(2) 0.061(2) 0.076(2) -0.0058(18) 0.0019(19) 0.0053(17) C22 0.0503(17) 0.0591(19) 0.0614(19) 0.0000(15) 0.0046(14) 0.0005(14) C23 0.067(2) 0.069(2) 0.071(2) 0.0112(18) 0.0046(18) -0.0014(18) C24 0.069(2) 0.094(3) 0.064(2) 0.017(2) 0.0004(18) -0.011(2) C25 0.123(4) 0.128(5) 0.077(3) 0.027(3) -0.010(3) -0.002(4) C26 0.194(7) 0.177(7) 0.076(4) 0.041(4) -0.035(4) -0.025(6) C27 0.219(9) 0.182(7) 0.057(3) 0.006(4) -0.017(4) -0.049(7) C28 0.178(7) 0.125(5) 0.068(3) -0.014(3) 0.006(4) -0.028(4) C29 0.102(4) 0.105(4) 0.056(2) -0.003(2) 0.002(2) -0.010(3) N1 0.116(3) 0.075(2) 0.069(2) -0.0116(18) 0.014(2) -0.003(2) C111 0.134(6) 0.121(5) 0.113(5) -0.033(4) 0.023(4) 0.023(4) C112 0.162(7) 0.156(7) 0.131(6) -0.040(5) -0.015(5) 0.065(5) C113 0.133(7) 0.208(9) 0.235(11) -0.040(9) 0.073(7) -0.033(7) C114 0.174(6) 0.089(4) 0.076(3) 0.005(3) 0.005(3) -0.027(4) C115 0.186(7) 0.092(4) 0.126(5) 0.003(4) -0.029(5) 0.025(4) C116 0.222(10) 0.151(6) 0.072(4) -0.012(3) 0.009(5) -0.034(5) N2 0.059(2) 0.251(8) 0.072(3) 0.041(3) -0.0016(19) -0.010(3) C211 0.127(6) 0.192(8) 0.087(4) -0.019(4) -0.001(4) -0.043(5) C212 0.135(7) 0.228(10) 0.150(7) -0.056(7) 0.016(5) -0.003(7) C213 0.170(8) 0.213(10) 0.202(9) 0.006(8) 0.048(7) -0.071(7) C214 0.051(2) 0.228(8) 0.092(3) 0.060(5) 0.014(2) 0.006(4) C215 0.099(4) 0.272(10) 0.094(4) 0.068(5) 0.016(3) 0.014(5) C216 0.142(6) 0.167(7) 0.151(7) 0.045(6) 0.016(5) 0.011(6) _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 Cd O21 2.243(3) . ? Cd O11 2.363(3) . ? Cd S1 2.3980(11) . ? Cd S2 2.4716(9) . ? Cd S2 2.9554(10) 3_665 ? Cd Cd 3.7613(7) 3_665 ? S1 C12 1.730(4) . ? S2 C22 1.758(4) . ? S2 Cd 2.9554(10) 3_665 ? O11 C11 1.262(6) . ? O12 C11 1.246(5) . ? C11 C12 1.494(6) . ? C12 C13 1.350(6) . ? C13 C14 1.468(6) . ? C14 C15 1.3900 . ? C14 C19 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? O21 C21 1.259(5) . ? O22 C21 1.238(5) . ? C21 C22 1.530(5) . ? C22 C23 1.341(5) . ? C23 C24 1.449(5) . ? C24 C25 1.3900 . ? C24 C29 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? N1 C111 1.493(8) . ? N1 C114 1.496(6) . ? C111 C112 1.484(9) . ? C111 C113 1.515(11) . ? C114 C115 1.487(9) . ? C114 C116 1.520(8) . ? N2 C214 1.439(7) . ? N2 C211 1.554(9) . ? C211 C212 1.457(10) . ? C211 C213 1.571(10) . ? C214 C215 1.527(7) . ? C214 C216 1.632(11) . ? 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 O21 Cd O11 101.95(12) . . ? O21 Cd S1 127.37(8) . . ? O11 Cd S1 78.40(8) . . ? O21 Cd S2 81.10(7) . . ? O11 Cd S2 101.34(8) . . ? S1 Cd S2 151.27(4) . . ? O21 Cd S2 89.12(8) . 3_665 ? O11 Cd S2 163.23(8) . 3_665 ? S1 Cd S2 84.88(3) . 3_665 ? S2 Cd S2 92.73(3) . 3_665 ? O21 Cd Cd 83.47(8) . 3_665 ? O11 Cd Cd 151.82(8) . 3_665 ? S1 Cd Cd 120.40(3) . 3_665 ? S2 Cd Cd 51.70(2) . 3_665 ? S2 Cd Cd 41.023(19) 3_665 3_665 ? C12 S1 Cd 102.62(14) . . ? C22 S2 Cd 97.22(12) . . ? C22 S2 Cd 96.69(11) . 3_665 ? Cd S2 Cd 87.27(3) . 3_665 ? C11 O11 Cd 119.2(3) . . ? O12 C11 O11 122.1(4) . . ? O12 C11 C12 118.1(4) . . ? O11 C11 C12 119.8(4) . . ? C13 C12 C11 117.2(4) . . ? C13 C12 S1 122.9(4) . . ? C11 C12 S1 119.8(3) . . ? C12 C13 C14 132.3(4) . . ? C15 C14 C19 120.0 . . ? C15 C14 C13 124.6(3) . . ? C19 C14 C13 115.4(3) . . ? C14 C15 C16 120.0 . . ? C17 C16 C15 120.0 . . ? C18 C17 C16 120.0 . . ? C19 C18 C17 120.0 . . ? C18 C19 C14 120.0 . . ? C21 O21 Cd 120.2(2) . . ? O22 C21 O21 122.7(4) . . ? O22 C21 C22 118.2(4) . . ? O21 C21 C22 119.1(3) . . ? C23 C22 C21 116.3(3) . . ? C23 C22 S2 124.4(3) . . ? C21 C22 S2 119.2(3) . . ? C22 C23 C24 132.2(4) . . ? C25 C24 C29 120.0 . . ? C25 C24 C23 115.6(3) . . ? C29 C24 C23 124.4(3) . . ? C24 C25 C26 120.0 . . ? C25 C26 C27 120.0 . . ? C28 C27 C26 120.0 . . ? C29 C28 C27 120.0 . . ? C28 C29 C24 120.0 . . ? C111 N1 C114 119.0(5) . . ? C112 C111 N1 108.7(5) . . ? C112 C111 C113 110.4(8) . . ? N1 C111 C113 111.0(7) . . ? C115 C114 N1 108.1(5) . . ? C115 C114 C116 112.4(6) . . ? N1 C114 C116 111.1(5) . . ? C214 N2 C211 113.1(6) . . ? C212 C211 N2 108.7(6) . . ? C212 C211 C213 116.4(9) . . ? N2 C211 C213 105.5(6) . . ? N2 C214 C215 112.0(5) . . ? N2 C214 C216 103.4(5) . . ? C215 C214 C216 111.4(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1B O21 0.90 2.00 2.880(5) 163.9 . N1 H1B O22 0.90 2.54 3.284(5) 140.0 . N1 H1A O22 0.90 1.91 2.791(6) 165.0 3_675 N2 H2A O11 0.90 1.94 2.815(5) 163.9 3_665 N2 H2B O12 0.90 1.77 2.667(7) 177.9 1_655 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 70.21 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.658 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.067 #=== data_6 _database_code_depnum_ccdc_archive 'CCDC 741233' ################ # CCDC 741233 # ################ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H42 Cd Cl2 N2 O4 S2' _chemical_formula_weight 742.08 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.482(3) _cell_length_b 14.585(3) _cell_length_c 17.589(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.630(4) _cell_angle_gamma 90.00 _cell_volume 3441.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .27 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.946 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.740103 _exptl_absorpt_correction_T_max 1.000000 _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 '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 15605 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.1937 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 26.18 _reflns_number_total 6415 _reflns_number_gt 1830 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1041P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6415 _refine_ls_number_parameters 362 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.3081 _refine_ls_R_factor_gt 0.0804 _refine_ls_wR_factor_ref 0.2553 _refine_ls_wR_factor_gt 0.1783 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd 0.57465(7) 0.06472(7) 0.07911(5) 0.1114(5) Uani 1 1 d . . . S2 S 0.3921(2) 0.0536(2) 0.05543(16) 0.1011(10) Uani 1 1 d . . . Cl2 Cl 0.1692(3) 0.3646(3) 0.0666(3) 0.1769(18) Uani 1 1 d . . . O21 O 0.5454(7) 0.1839(6) 0.0002(4) 0.112(3) Uani 1 1 d . . . O22 O 0.4369(6) 0.2716(7) -0.0673(5) 0.124(3) Uani 1 1 d . . . C21 C 0.4588(12) 0.2079(9) -0.0201(7) 0.102(5) Uani 1 1 d . . . C22 C 0.3685(11) 0.1596(8) 0.0117(6) 0.095(4) Uani 1 1 d . . . C23 C 0.2828(11) 0.2049(9) 0.0080(7) 0.105(4) Uani 1 1 d . . . H23 H 0.2814 0.2582 -0.0210 0.125 Uiso 1 1 calc R . . C24 C 0.1914(11) 0.1855(13) 0.0413(7) 0.108(4) Uani 1 1 d . . . C25 C 0.1343(13) 0.2512(11) 0.0709(9) 0.127(5) Uani 1 1 d . . . C26 C 0.0503(14) 0.2328(17) 0.1063(10) 0.151(7) Uani 1 1 d . . . H26 H 0.0139 0.2799 0.1259 0.181 Uiso 1 1 calc R . . C27 C 0.0214(12) 0.143(2) 0.1119(10) 0.155(7) Uani 1 1 d . . . H27 H -0.0342 0.1291 0.1370 0.186 Uiso 1 1 calc R . . C28 C 0.0738(15) 0.0755(12) 0.0811(10) 0.147(6) Uani 1 1 d . . . H28 H 0.0524 0.0151 0.0838 0.177 Uiso 1 1 calc R . . C29 C 0.1559(13) 0.0946(13) 0.0466(9) 0.137(5) Uani 1 1 d . . . H29 H 0.1903 0.0470 0.0258 0.164 Uiso 1 1 calc R . . Cl1 Cl 1.0275(5) 0.0683(5) 0.3592(5) 0.283(4) Uani 1 1 d . . . S1 S 0.7390(4) 0.0198(6) 0.1239(3) 0.270(4) Uani 1 1 d . . . O11 O 0.5919(7) 0.1286(6) 0.2030(5) 0.122(3) Uani 1 1 d . . . O12 O 0.6893(10) 0.1494(9) 0.3090(7) 0.214(6) Uani 1 1 d . . . C11 C 0.6727(14) 0.1168(9) 0.2443(9) 0.116(5) Uani 1 1 d . . . C12 C 0.7498(12) 0.0589(10) 0.2147(7) 0.119(5) Uani 1 1 d . . . C13 C 0.8335(15) 0.0338(9) 0.2622(9) 0.123(5) Uani 1 1 d . . . H13 H 0.8371 0.0609 0.3102 0.148 Uiso 1 1 calc R . . C14 C 0.9171(14) -0.0269(16) 0.2513(12) 0.126(5) Uani 1 1 d . . . C15 C 1.003(2) -0.0154(18) 0.2935(13) 0.183(9) Uani 1 1 d . . . C16 C 1.087(3) -0.075(2) 0.2889(19) 0.210(13) Uani 1 1 d . . . H16 H 1.1458 -0.0673 0.3209 0.252 Uiso 1 1 calc R . . C17 C 1.079(2) -0.140(3) 0.2397(19) 0.229(16) Uani 1 1 d . . . H17 H 1.1344 -0.1757 0.2328 0.274 Uiso 1 1 calc R . . C18 C 0.994(2) -0.1570(16) 0.1980(14) 0.202(10) Uani 1 1 d . . . H18 H 0.9868 -0.2088 0.1670 0.242 Uiso 1 1 calc R . . C19 C 0.9098(16) -0.0935(19) 0.2013(14) 0.171(8) Uani 1 1 d . . . H19 H 0.8522 -0.1005 0.1681 0.206 Uiso 1 1 calc R . . N1 N 0.4369(8) 0.2203(7) 0.2746(5) 0.107(3) Uani 1 1 d . . . H1A H 0.4901 0.1911 0.2589 0.129 Uiso 1 1 calc R . . H1B H 0.4434 0.2186 0.3260 0.129 Uiso 1 1 calc R . . C31 C 0.4429(15) 0.3168(13) 0.2516(12) 0.176(7) Uani 1 1 d . . . H31 H 0.3863 0.3506 0.2687 0.211 Uiso 1 1 calc R . . C32 C 0.5429(17) 0.3569(11) 0.2922(10) 0.231(10) Uani 1 1 d . . . H32A H 0.5469 0.4212 0.2812 0.346 Uiso 1 1 calc R . . H32B H 0.5985 0.3258 0.2737 0.346 Uiso 1 1 calc R . . H32C H 0.5443 0.3481 0.3464 0.346 Uiso 1 1 calc R . . C33 C 0.4450(16) 0.3297(12) 0.1699(11) 0.223(10) Uani 1 1 d . . . H33A H 0.4662 0.3910 0.1601 0.335 Uiso 1 1 calc R . . H33B H 0.3796 0.3197 0.1446 0.335 Uiso 1 1 calc R . . H33C H 0.4908 0.2868 0.1511 0.335 Uiso 1 1 calc R . . C34 C 0.3495(11) 0.1680(13) 0.2484(9) 0.136(5) Uani 1 1 d . . . H34 H 0.3460 0.1643 0.1925 0.163 Uiso 1 1 calc R . . C35 C 0.2543(11) 0.2144(13) 0.2692(9) 0.191(8) Uani 1 1 d . . . H35A H 0.2656 0.2791 0.2752 0.287 Uiso 1 1 calc R . . H35B H 0.2358 0.1892 0.3162 0.287 Uiso 1 1 calc R . . H35C H 0.2016 0.2040 0.2293 0.287 Uiso 1 1 calc R . . C36 C 0.3575(12) 0.0765(11) 0.2781(12) 0.191(8) Uani 1 1 d . . . H36A H 0.4218 0.0683 0.3059 0.286 Uiso 1 1 calc R . . H36B H 0.3495 0.0335 0.2366 0.286 Uiso 1 1 calc R . . H36C H 0.3065 0.0665 0.3116 0.286 Uiso 1 1 calc R . . N2 N 0.6949(8) 0.1960(8) 0.4565(6) 0.130(4) Uani 1 1 d D . . H2A H 0.6920 0.1837 0.4061 0.156 Uiso 1 1 calc R . . H2B H 0.6411 0.2302 0.4640 0.156 Uiso 1 1 calc R . . C41 C 0.7859(13) 0.2527(17) 0.4776(16) 0.223(10) Uani 1 1 d DU . . H41 H 0.7921 0.2692 0.5319 0.268 Uiso 1 1 calc R . . C42 C 0.7736(15) 0.3337(14) 0.4290(14) 0.242(12) Uani 1 1 d U . . H42A H 0.7189 0.3697 0.4436 0.364 Uiso 1 1 calc R . . H42B H 0.7601 0.3151 0.3767 0.364 Uiso 1 1 calc R . . H42C H 0.8335 0.3696 0.4348 0.364 Uiso 1 1 calc R . . C43 C 0.8807(14) 0.2012(18) 0.4554(14) 0.284(11) Uani 1 1 d U . . H43A H 0.8952 0.1506 0.4896 0.426 Uiso 1 1 calc R . . H43B H 0.9363 0.2426 0.4590 0.426 Uiso 1 1 calc R . . H43C H 0.8688 0.1788 0.4040 0.426 Uiso 1 1 calc R . . C44 C 0.6871(19) 0.1069(16) 0.4982(15) 0.2545(15) Uani 1 1 d DU . . H44 H 0.7474 0.0727 0.4894 0.305 Uiso 1 1 calc R . . C45 C 0.683(3) 0.104(2) 0.5677(17) 0.354(12) Uani 1 1 d U . . H45A H 0.7415 0.1316 0.5932 0.531 Uiso 1 1 calc R . . H45B H 0.6778 0.0417 0.5837 0.531 Uiso 1 1 calc R . . H45C H 0.6249 0.1376 0.5802 0.531 Uiso 1 1 calc R . . C46 C 0.603(2) 0.0533(19) 0.4590(16) 0.354(12) Uani 1 1 d U . . H46A H 0.6227 0.0293 0.4118 0.531 Uiso 1 1 calc R . . H46B H 0.5462 0.0923 0.4487 0.531 Uiso 1 1 calc R . . H46C H 0.5868 0.0035 0.4912 0.531 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 Cd 0.1306(9) 0.1241(9) 0.0808(7) 0.0113(6) 0.0165(5) 0.0389(6) S2 0.119(3) 0.104(3) 0.084(2) 0.0122(18) 0.0267(18) 0.0338(19) Cl2 0.168(4) 0.130(4) 0.236(5) -0.011(3) 0.041(3) 0.059(3) O21 0.117(7) 0.121(7) 0.100(6) 0.030(5) 0.024(5) 0.035(5) O22 0.119(7) 0.140(8) 0.119(7) 0.034(6) 0.037(5) 0.034(5) C21 0.156(15) 0.091(10) 0.062(8) 0.009(7) 0.020(9) 0.060(10) C22 0.120(11) 0.103(10) 0.068(8) 0.003(6) 0.038(8) 0.013(8) C23 0.106(10) 0.121(11) 0.093(9) 0.021(7) 0.038(8) 0.038(9) C24 0.113(12) 0.118(13) 0.093(10) 0.019(9) 0.013(9) 0.050(11) C25 0.131(13) 0.136(16) 0.115(11) 0.015(9) 0.020(10) 0.058(12) C26 0.121(15) 0.20(2) 0.146(14) 0.020(13) 0.070(11) 0.068(13) C27 0.101(12) 0.23(2) 0.143(14) 0.068(16) 0.049(10) 0.045(16) C28 0.129(13) 0.150(15) 0.171(15) 0.033(12) 0.062(12) 0.033(13) C29 0.131(14) 0.137(18) 0.151(14) 0.028(10) 0.056(11) 0.040(11) Cl1 0.214(6) 0.298(8) 0.310(8) -0.021(6) -0.108(6) -0.052(5) S1 0.196(5) 0.496(11) 0.110(4) -0.072(5) -0.017(4) 0.189(6) O11 0.129(8) 0.137(8) 0.100(7) -0.020(5) 0.005(6) 0.037(6) O12 0.286(15) 0.220(13) 0.127(9) -0.084(9) -0.026(9) 0.094(10) C11 0.166(16) 0.089(10) 0.094(12) -0.008(8) 0.023(11) 0.046(10) C12 0.118(11) 0.139(13) 0.095(10) 0.022(9) -0.010(9) 0.025(10) C13 0.151(15) 0.084(10) 0.141(14) -0.025(9) 0.041(12) -0.028(9) C14 0.110(16) 0.169(19) 0.101(13) 0.034(11) 0.030(13) -0.005(14) C15 0.135(17) 0.20(2) 0.20(2) 0.072(17) -0.038(18) -0.047(18) C16 0.18(3) 0.20(3) 0.25(4) 0.06(2) 0.00(2) -0.02(2) C17 0.11(2) 0.34(5) 0.24(4) 0.08(3) 0.08(2) 0.00(3) C18 0.18(2) 0.19(2) 0.25(3) 0.026(18) 0.12(2) 0.00(2) C19 0.155(18) 0.22(2) 0.155(19) 0.033(17) 0.080(15) 0.030(19) N1 0.167(11) 0.060(8) 0.100(8) -0.018(6) 0.035(7) 0.013(7) C31 0.25(2) 0.104(16) 0.18(2) -0.020(13) 0.017(16) -0.022(13) C32 0.43(3) 0.117(15) 0.155(16) 0.006(12) 0.093(19) -0.098(18) C33 0.40(3) 0.156(16) 0.112(14) 0.025(11) -0.008(17) 0.025(16) C34 0.129(13) 0.143(15) 0.134(13) -0.066(11) 0.004(10) -0.029(12) C35 0.127(13) 0.30(2) 0.150(15) -0.025(14) 0.030(11) 0.058(14) C36 0.183(16) 0.092(13) 0.30(2) -0.037(14) 0.051(14) -0.047(11) N2 0.122(9) 0.141(10) 0.129(9) -0.036(8) 0.023(7) -0.011(8) C41 0.100(12) 0.28(3) 0.28(3) -0.104(19) 0.000(16) -0.044(16) C42 0.23(2) 0.185(19) 0.35(3) -0.127(16) 0.19(2) -0.098(13) C43 0.143(16) 0.40(3) 0.32(3) -0.12(2) 0.041(17) -0.016(17) C44 0.267 0.240 0.250 0.08(2) -0.01(2) 0.113(15) C45 0.41(3) 0.36(3) 0.293(10) 0.13(2) 0.03(2) -0.084(18) C46 0.41(3) 0.36(3) 0.293(10) 0.13(2) 0.03(2) -0.084(18) _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 Cd O21 2.235(8) . ? Cd O11 2.361(9) . ? Cd S1 2.370(4) . ? Cd S2 2.461(3) . ? Cd S2 2.998(3) 3_655 ? Cd Cd 3.776(2) 3_655 ? S2 C22 1.743(12) . ? S2 Cd 2.998(3) 3_655 ? Cl2 C25 1.723(16) . ? O21 C21 1.237(13) . ? O22 C21 1.262(12) . ? C21 C22 1.557(17) . ? C22 C23 1.326(14) . ? C23 C24 1.443(16) . ? C24 C25 1.364(17) . ? C24 C29 1.416(17) . ? C25 C26 1.371(19) . ? C26 C27 1.37(2) . ? C27 C28 1.36(2) . ? C28 C29 1.342(17) . ? Cl1 C15 1.69(2) . ? S1 C12 1.687(14) . ? O11 C11 1.260(15) . ? O12 C11 1.233(15) . ? C11 C12 1.474(18) . ? C12 C13 1.386(18) . ? C13 C14 1.46(2) . ? C14 C19 1.31(2) . ? C14 C15 1.33(2) . ? C15 C16 1.44(3) . ? C16 C17 1.28(3) . ? C17 C18 1.33(3) . ? C18 C19 1.47(2) . ? N1 C34 1.442(14) . ? N1 C31 1.469(18) . ? C31 C33 1.45(2) . ? C31 C32 1.58(2) . ? C34 C36 1.434(19) . ? C34 C35 1.526(17) . ? N2 C41 1.496(14) . ? N2 C44 1.502(16) . ? C41 C42 1.46(3) . ? C41 C43 1.57(3) . ? C44 C45 1.23(3) . ? C44 C46 1.49(3) . ? 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 O21 Cd O11 105.2(3) . . ? O21 Cd S1 121.6(3) . . ? O11 Cd S1 78.3(3) . . ? O21 Cd S2 80.4(2) . . ? O11 Cd S2 100.9(2) . . ? S1 Cd S2 157.7(2) . . ? O21 Cd S2 89.3(2) . 3_655 ? O11 Cd S2 161.3(2) . 3_655 ? S1 Cd S2 84.04(13) . 3_655 ? S2 Cd S2 93.03(9) . 3_655 ? O21 Cd Cd 83.2(2) . 3_655 ? O11 Cd Cd 151.0(2) . 3_655 ? S1 Cd Cd 121.35(16) . 3_655 ? S2 Cd Cd 52.43(7) . 3_655 ? S2 Cd Cd 40.60(6) 3_655 3_655 ? C22 S2 Cd 98.8(5) . . ? C22 S2 Cd 101.4(4) . 3_655 ? Cd S2 Cd 86.97(9) . 3_655 ? C21 O21 Cd 120.2(9) . . ? O21 C21 O22 123.4(15) . . ? O21 C21 C22 121.2(12) . . ? O22 C21 C22 115.4(12) . . ? C23 C22 C21 117.7(11) . . ? C23 C22 S2 125.7(11) . . ? C21 C22 S2 116.4(10) . . ? C22 C23 C24 131.1(13) . . ? C25 C24 C29 115.2(15) . . ? C25 C24 C23 123.7(18) . . ? C29 C24 C23 121.1(14) . . ? C24 C25 C26 123.9(16) . . ? C24 C25 Cl2 119.3(16) . . ? C26 C25 Cl2 116.7(16) . . ? C27 C26 C25 118.3(17) . . ? C28 C27 C26 120.2(18) . . ? C29 C28 C27 120.8(18) . . ? C28 C29 C24 121.5(15) . . ? C12 S1 Cd 102.3(6) . . ? C11 O11 Cd 118.6(9) . . ? O12 C11 O11 123.2(14) . . ? O12 C11 C12 118.5(15) . . ? O11 C11 C12 118.3(14) . . ? C13 C12 C11 119.9(13) . . ? C13 C12 S1 118.1(12) . . ? C11 C12 S1 122.0(11) . . ? C12 C13 C14 132.4(16) . . ? C19 C14 C15 118(2) . . ? C19 C14 C13 122(2) . . ? C15 C14 C13 120(3) . . ? C14 C15 C16 123(3) . . ? C14 C15 Cl1 125(3) . . ? C16 C15 Cl1 112(2) . . ? C17 C16 C15 118(4) . . ? C16 C17 C18 122(4) . . ? C17 C18 C19 119(3) . . ? C14 C19 C18 119(2) . . ? C34 N1 C31 118.9(13) . . ? C33 C31 N1 113.8(15) . . ? C33 C31 C32 107.5(17) . . ? N1 C31 C32 107.3(15) . . ? C36 C34 N1 110.2(14) . . ? C36 C34 C35 111.1(15) . . ? N1 C34 C35 111.7(13) . . ? C41 N2 C44 116.9(16) . . ? C42 C41 N2 104.9(17) . . ? C42 C41 C43 107(2) . . ? N2 C41 C43 110.0(17) . . ? C45 C44 C46 110(3) . . ? C45 C44 N2 122(3) . . ? C46 C44 N2 108.4(17) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O11 0.90 1.99 2.873(12) 168.1 . N2 H2A O12 0.90 1.78 2.675(15) 175.0 . N1 H1B O22 0.90 1.89 2.782(13) 169.9 4_566 N2 H2B O21 0.90 1.95 2.833(13) 166.4 4_566 _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 26.18 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.541 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.072