Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Xian-He Bu' _publ_contact_author_address ; Department of Chemistry Nankai University No 94, Weijin Road Tianjin 300071 CHINA ; _publ_contact_author_email BUXH@NANKAI.EDU.CN _publ_section_title ; Novel Cd(II) coordination polymers with flexible disulfoxide ligands: effects of ligand spacers, terminal groups and counter anions on the complex framework formations ; loop_ _publ_author_name 'Xian-He Bu' 'Jian-Rong Li' 'Ruo-Hua Zhang' data_4 _database_code_depnum_ccdc_archive 'CCDC 200618' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H20 Cd N2 O9 S2' _chemical_formula_weight 560.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/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 13.147(4) _cell_length_b 10.163(3) _cell_length_c 16.844(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.095(5) _cell_angle_gamma 90.00 _cell_volume 2173.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.247 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7061 _exptl_absorpt_correction_T_max 0.7886 _exptl_absorpt_process_details SADABS _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 8673 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3785 _reflns_number_gt 2659 _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^)+(0.0545P)^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 3785 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1003 _refine_ls_wR_factor_gt 0.0909 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _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 Cd1 Cd 0.29511(3) 0.23867(3) 0.22987(2) 0.04473(15) Uani 1 1 d . . . N1 N 0.1034(4) 0.0047(4) 0.2562(3) 0.0555(11) Uani 1 1 d . . . N2 N 0.2619(4) 0.2542(4) 0.0519(3) 0.0534(11) Uani 1 1 d . . . O1 O 0.3097(3) 0.2573(3) 0.36609(19) 0.0486(8) Uani 1 1 d . . . O2 O 0.4241(2) 0.0781(3) 0.27167(17) 0.0436(8) Uani 1 1 d . . . O3 O 0.0711(3) -0.1103(3) 0.2643(2) 0.0706(11) Uani 1 1 d . . . O4 O 0.1930(3) 0.0214(3) 0.2453(2) 0.0506(8) Uani 1 1 d . . . O5 O 0.0452(3) 0.0991(4) 0.2580(3) 0.0939(15) Uani 1 1 d . . . O6 O 0.2916(4) 0.1632(3) 0.1012(2) 0.0714(12) Uani 1 1 d . . . O7 O 0.2518(4) 0.3630(4) 0.0808(3) 0.0991(16) Uani 1 1 d . . . O8 O 0.2459(5) 0.2388(4) -0.0208(2) 0.0993(17) Uani 1 1 d . . . O9 O 0.1286(3) 0.3138(4) 0.2056(2) 0.0658(10) Uani 1 1 d . . . S1 S 0.26045(10) 0.36644(12) 0.40447(7) 0.0445(3) Uani 1 1 d . . . S2 S 0.53433(9) 0.11657(11) 0.31999(7) 0.0400(3) Uani 1 1 d . . . C1 C 0.1826(4) 0.1542(5) 0.4702(4) 0.0628(15) Uani 1 1 d . . . H1A H 0.2236 0.1028 0.4449 0.075 Uiso 1 1 calc R . . C2 C 0.1223(5) 0.0964(7) 0.5156(5) 0.090(2) Uani 1 1 d . . . H2A H 0.1214 0.0053 0.5206 0.108 Uiso 1 1 calc R . . C3 C 0.0626(5) 0.1737(9) 0.5544(4) 0.093(2) Uani 1 1 d . . . H3A H 0.0235 0.1348 0.5868 0.112 Uiso 1 1 calc R . . C4 C 0.0614(5) 0.3070(7) 0.5448(4) 0.086(2) Uani 1 1 d . . . H4A H 0.0200 0.3586 0.5697 0.103 Uiso 1 1 calc R . . C5 C 0.1206(5) 0.3653(6) 0.4989(4) 0.0702(16) Uani 1 1 d . . . H5A H 0.1192 0.4562 0.4925 0.084 Uiso 1 1 calc R . . C6 C 0.1820(4) 0.2895(5) 0.4624(3) 0.0478(12) Uani 1 1 d . . . C7 C 0.3651(4) 0.4188(5) 0.4906(3) 0.0509(13) Uani 1 1 d . . . H7A H 0.3375 0.4818 0.5229 0.061 Uiso 1 1 calc R . . H7B H 0.3911 0.3435 0.5254 0.061 Uiso 1 1 calc R . . C8 C 0.4559(4) 0.4812(5) 0.4636(3) 0.0538(13) Uani 1 1 d . . . H8A H 0.4818 0.4196 0.4294 0.065 Uiso 1 1 calc R . . H8B H 0.4308 0.5589 0.4309 0.065 Uiso 1 1 calc R . . C9 C 0.5834(4) -0.0458(5) 0.2043(3) 0.0582(14) Uani 1 1 d . . . H9A H 0.5124 -0.0679 0.1881 0.070 Uiso 1 1 calc R . . C10 C 0.6539(6) -0.1005(7) 0.1651(4) 0.0783(18) Uani 1 1 d . . . H10A H 0.6299 -0.1585 0.1215 0.094 Uiso 1 1 calc R . . C11 C 0.7577(6) -0.0695(7) 0.1902(4) 0.0799(19) Uani 1 1 d . . . H11A H 0.8048 -0.1078 0.1645 0.096 Uiso 1 1 calc R . . C12 C 0.7931(5) 0.0164(7) 0.2524(4) 0.087(2) Uani 1 1 d . . . H12A H 0.8642 0.0383 0.2684 0.105 Uiso 1 1 calc R . . C13 C 0.7248(5) 0.0717(6) 0.2921(4) 0.0730(17) Uani 1 1 d . . . H13A H 0.7497 0.1294 0.3357 0.088 Uiso 1 1 calc R . . C14 C 0.6200(4) 0.0416(5) 0.2673(3) 0.0438(12) Uani 1 1 d . . . C15 C 0.5619(4) 0.0113(5) 0.4087(3) 0.0424(11) Uani 1 1 d . . . H15A H 0.5501 -0.0797 0.3914 0.051 Uiso 1 1 calc R . . H15B H 0.6351 0.0207 0.4389 0.051 Uiso 1 1 calc R . . C16 C 0.4916(4) 0.0464(5) 0.4641(3) 0.0461(12) Uani 1 1 d . . . H16A H 0.5067 0.1357 0.4841 0.055 Uiso 1 1 calc R . . H16B H 0.4185 0.0428 0.4327 0.055 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 Cd1 0.0439(2) 0.0503(2) 0.0384(2) -0.00425(17) 0.00785(15) 0.01331(17) N1 0.055(3) 0.046(3) 0.063(3) -0.005(2) 0.011(2) 0.003(2) N2 0.071(3) 0.045(3) 0.046(3) 0.002(2) 0.018(2) 0.001(2) O1 0.059(2) 0.0445(19) 0.0399(17) -0.0070(15) 0.0083(16) 0.0144(16) O2 0.043(2) 0.0429(18) 0.0411(17) -0.0005(14) 0.0048(15) 0.0042(14) O3 0.065(3) 0.045(2) 0.104(3) -0.002(2) 0.025(2) -0.0146(19) O4 0.036(2) 0.052(2) 0.066(2) -0.0096(17) 0.0161(17) 0.0000(16) O5 0.063(3) 0.053(3) 0.178(5) 0.001(3) 0.053(3) 0.010(2) O6 0.122(4) 0.042(2) 0.050(2) 0.0048(18) 0.019(2) 0.011(2) O7 0.147(5) 0.062(3) 0.082(3) 0.001(2) 0.018(3) 0.024(3) O8 0.168(5) 0.092(3) 0.036(2) 0.005(2) 0.024(3) 0.018(3) O9 0.050(2) 0.055(2) 0.086(3) 0.001(2) 0.005(2) 0.0077(18) S1 0.0496(8) 0.0392(7) 0.0414(7) -0.0063(5) 0.0058(6) 0.0100(6) S2 0.0380(7) 0.0388(6) 0.0437(7) 0.0006(5) 0.0118(5) 0.0024(5) C1 0.056(4) 0.054(3) 0.082(4) -0.003(3) 0.024(3) 0.001(3) C2 0.081(5) 0.069(4) 0.128(6) 0.006(4) 0.039(5) -0.005(4) C3 0.077(5) 0.118(7) 0.093(5) -0.001(5) 0.038(4) -0.019(5) C4 0.075(5) 0.085(5) 0.109(6) -0.027(4) 0.044(4) 0.000(4) C5 0.071(4) 0.066(4) 0.079(4) -0.015(3) 0.029(3) 0.007(3) C6 0.037(3) 0.050(3) 0.051(3) -0.012(2) 0.004(2) 0.005(2) C7 0.055(3) 0.053(3) 0.042(3) -0.009(2) 0.007(2) -0.002(2) C8 0.054(3) 0.055(3) 0.048(3) -0.010(3) 0.006(2) -0.001(3) C9 0.047(3) 0.075(4) 0.054(3) -0.009(3) 0.017(3) 0.001(3) C10 0.086(5) 0.093(5) 0.059(4) -0.011(3) 0.024(4) 0.023(4) C11 0.073(5) 0.100(5) 0.079(4) 0.013(4) 0.042(4) 0.029(4) C12 0.055(4) 0.107(5) 0.113(6) -0.009(5) 0.046(4) 0.000(4) C13 0.054(4) 0.080(4) 0.094(4) -0.017(3) 0.035(3) -0.012(3) C14 0.043(3) 0.044(3) 0.047(3) 0.009(2) 0.016(2) 0.006(2) C15 0.035(3) 0.047(3) 0.044(3) 0.006(2) 0.008(2) 0.011(2) C16 0.046(3) 0.053(3) 0.041(3) 0.003(2) 0.015(2) 0.008(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 Cd1 O9 2.253(4) . ? Cd1 O1 2.260(3) . ? Cd1 O6 2.289(4) . ? Cd1 O3 2.317(4) 2 ? Cd1 O2 2.326(3) . ? Cd1 O4 2.632(3) . ? N1 O5 1.233(5) . ? N1 O4 1.249(5) . ? N1 O3 1.263(5) . ? N2 O8 1.198(5) . ? N2 O7 1.230(5) . ? N2 O6 1.236(5) . ? O1 S1 1.512(3) . ? O2 S2 1.517(3) . ? O3 Cd1 2.317(4) 2_545 ? S1 C6 1.776(5) . ? S1 C7 1.800(5) . ? S2 C14 1.777(5) . ? S2 C15 1.797(4) . ? C1 C2 1.369(8) . ? C1 C6 1.381(7) . ? C2 C3 1.388(9) . ? C3 C4 1.364(11) . ? C4 C5 1.365(8) . ? C5 C6 1.372(7) . ? C7 C8 1.523(7) . ? C8 C8 1.502(9) 3_666 ? C9 C14 1.371(7) . ? C9 C10 1.387(7) . ? C10 C11 1.357(9) . ? C11 C12 1.350(9) . ? C12 C13 1.372(8) . ? C13 C14 1.366(7) . ? C15 C16 1.516(6) . ? C16 C16 1.505(8) 3_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Cd1 O1 88.67(13) . . ? O9 Cd1 O6 99.39(15) . . ? O1 Cd1 O6 164.83(11) . . ? O9 Cd1 O3 118.30(13) . 2 ? O1 Cd1 O3 92.24(13) . 2 ? O6 Cd1 O3 95.15(14) . 2 ? O9 Cd1 O2 152.84(12) . . ? O1 Cd1 O2 83.64(10) . . ? O6 Cd1 O2 83.39(12) . . ? O3 Cd1 O2 88.09(12) 2 . ? O9 Cd1 O4 78.79(12) . . ? O1 Cd1 O4 83.14(11) . . ? O6 Cd1 O4 85.84(12) . . ? O3 Cd1 O4 162.31(11) 2 . ? O2 Cd1 O4 74.46(11) . . ? O5 N1 O4 120.8(4) . . ? O5 N1 O3 119.3(5) . . ? O4 N1 O3 119.9(4) . . ? O8 N2 O7 121.0(5) . . ? O8 N2 O6 122.0(5) . . ? O7 N2 O6 117.0(4) . . ? S1 O1 Cd1 124.28(18) . . ? S2 O2 Cd1 120.06(16) . . ? N1 O3 Cd1 110.2(3) . 2_545 ? N1 O4 Cd1 130.8(3) . . ? N2 O6 Cd1 108.1(3) . . ? O1 S1 C6 106.6(2) . . ? O1 S1 C7 103.8(2) . . ? C6 S1 C7 96.8(2) . . ? O2 S2 C14 105.2(2) . . ? O2 S2 C15 104.5(2) . . ? C14 S2 C15 98.2(2) . . ? C2 C1 C6 119.4(6) . . ? C1 C2 C3 120.1(6) . . ? C4 C3 C2 119.8(7) . . ? C3 C4 C5 120.5(6) . . ? C4 C5 C6 119.9(6) . . ? C5 C6 C1 120.4(5) . . ? C5 C6 S1 119.5(4) . . ? C1 C6 S1 120.1(4) . . ? C8 C7 S1 112.1(3) . . ? C8 C8 C7 111.1(5) 3_666 . ? C14 C9 C10 119.1(5) . . ? C11 C10 C9 120.0(6) . . ? C12 C11 C10 120.6(6) . . ? C11 C12 C13 120.3(6) . . ? C14 C13 C12 119.7(6) . . ? C13 C14 C9 120.3(5) . . ? C13 C14 S2 118.1(4) . . ? C9 C14 S2 121.6(4) . . ? C16 C15 S2 110.4(3) . . ? C16 C16 C15 111.2(5) 3_656 . ? 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 O9 Cd1 O1 S1 -36.7(2) . . . . ? O6 Cd1 O1 S1 -159.3(4) . . . . ? O3 Cd1 O1 S1 81.5(2) 2 . . . ? O2 Cd1 O1 S1 169.4(2) . . . . ? O4 Cd1 O1 S1 -115.6(2) . . . . ? O9 Cd1 O2 S2 -142.1(3) . . . . ? O1 Cd1 O2 S2 -67.65(19) . . . . ? O6 Cd1 O2 S2 120.2(2) . . . . ? O3 Cd1 O2 S2 24.8(2) 2 . . . ? O4 Cd1 O2 S2 -152.3(2) . . . . ? O5 N1 O3 Cd1 -174.8(4) . . . 2_545 ? O4 N1 O3 Cd1 6.3(5) . . . 2_545 ? O5 N1 O4 Cd1 3.1(7) . . . . ? O3 N1 O4 Cd1 -177.9(3) . . . . ? O9 Cd1 O4 N1 -17.5(4) . . . . ? O1 Cd1 O4 N1 72.5(4) . . . . ? O6 Cd1 O4 N1 -117.9(4) . . . . ? O3 Cd1 O4 N1 148.2(5) 2 . . . ? O2 Cd1 O4 N1 157.8(4) . . . . ? O8 N2 O6 Cd1 -174.7(5) . . . . ? O7 N2 O6 Cd1 7.1(6) . . . . ? O9 Cd1 O6 N2 54.2(4) . . . . ? O1 Cd1 O6 N2 175.6(4) . . . . ? O3 Cd1 O6 N2 -65.6(4) 2 . . . ? O2 Cd1 O6 N2 -153.1(4) . . . . ? O4 Cd1 O6 N2 132.1(4) . . . . ? Cd1 O1 S1 C6 124.8(2) . . . . ? Cd1 O1 S1 C7 -133.6(2) . . . . ? Cd1 O2 S2 C14 -129.0(2) . . . . ? Cd1 O2 S2 C15 128.1(2) . . . . ? C6 C1 C2 C3 -1.0(10) . . . . ? C1 C2 C3 C4 2.2(11) . . . . ? C2 C3 C4 C5 -1.6(10) . . . . ? C3 C4 C5 C6 -0.2(10) . . . . ? C4 C5 C6 C1 1.4(9) . . . . ? C4 C5 C6 S1 -178.8(5) . . . . ? C2 C1 C6 C5 -0.8(8) . . . . ? C2 C1 C6 S1 179.5(5) . . . . ? O1 S1 C6 C5 -174.7(4) . . . . ? C7 S1 C6 C5 78.6(5) . . . . ? O1 S1 C6 C1 5.0(5) . . . . ? C7 S1 C6 C1 -101.6(4) . . . . ? O1 S1 C7 C8 65.8(4) . . . . ? C6 S1 C7 C8 174.9(4) . . . . ? S1 C7 C8 C8 -177.6(5) . . . 3_666 ? C14 C9 C10 C11 1.3(9) . . . . ? C9 C10 C11 C12 -1.2(10) . . . . ? C10 C11 C12 C13 1.3(11) . . . . ? C11 C12 C13 C14 -1.4(10) . . . . ? C12 C13 C14 C9 1.5(9) . . . . ? C12 C13 C14 S2 -179.5(5) . . . . ? C10 C9 C14 C13 -1.4(8) . . . . ? C10 C9 C14 S2 179.6(4) . . . . ? O2 S2 C14 C13 172.8(4) . . . . ? C15 S2 C14 C13 -79.6(5) . . . . ? O2 S2 C14 C9 -8.1(5) . . . . ? C15 S2 C14 C9 99.4(4) . . . . ? O2 S2 C15 C16 -67.5(4) . . . . ? C14 S2 C15 C16 -175.7(4) . . . . ? S2 C15 C16 C16 176.2(4) . . . 3_656 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.911 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.090 data_3 _database_code_depnum_ccdc_archive 'CCDC 211358' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Cd(besb)(NO3)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H36 Cd2 N4 O16 S4' _chemical_formula_weight 893.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 10.177(2) _cell_length_b 18.796(4) _cell_length_c 17.661(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.70(3) _cell_angle_gamma 90.00 _cell_volume 3330.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 787 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 22.70 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 1.597 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6459 _exptl_absorpt_correction_T_max 0.7005 _exptl_absorpt_process_details 'SADABS(Bruker/Siemens area detector absorption- V2.03)' _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 15198 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.1060 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 26.46 _reflns_number_total 6784 _reflns_number_gt 3830 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0407P)^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 6784 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1261 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1161 _refine_ls_wR_factor_gt 0.0980 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 Cd1 Cd 0.65999(5) -0.00593(2) 0.32384(3) 0.03747(16) Uani 1 1 d . . . Cd2 Cd 0.83000(5) 0.03917(2) 0.16329(3) 0.03625(16) Uani 1 1 d . . . S1 S 0.45951(19) -0.08838(10) 0.41945(12) 0.0498(5) Uani 1 1 d . . . S2 S 0.58351(17) -0.08084(9) 0.13677(11) 0.0418(5) Uani 1 1 d . . . S3 S 0.90551(17) 0.11666(10) 0.34970(11) 0.0451(5) Uani 1 1 d . . . S4 S 1.02877(19) 0.12103(10) 0.06884(12) 0.0540(5) Uani 1 1 d . . . O1 O 0.4957(5) -0.0807(2) 0.3384(3) 0.0509(13) Uani 1 1 d . . . O2 O 0.6670(4) -0.0330(2) 0.1980(2) 0.0346(11) Uani 1 1 d . . . O3 O 0.8231(5) -0.1042(3) 0.3519(3) 0.0619(15) Uani 1 1 d . . . O4 O 0.9285(6) -0.1206(3) 0.4666(4) 0.0827(19) Uani 1 1 d . . . O5 O 0.7900(6) -0.0331(3) 0.4410(3) 0.0671(16) Uani 1 1 d . . . O6 O 0.5986(6) 0.0885(3) 0.4014(3) 0.0647(16) Uani 1 1 d . . . O7 O 0.4438(7) 0.1644(3) 0.3626(4) 0.097(2) Uani 1 1 d . . . O8 O 0.4963(5) 0.0846(3) 0.2850(4) 0.0690(17) Uani 1 1 d . . . O9 O 0.8236(4) 0.0671(2) 0.2890(2) 0.0354(11) Uani 1 1 d . . . O10 O 0.9898(4) 0.1165(2) 0.1495(3) 0.0508(13) Uani 1 1 d . . . O11 O 0.9999(5) -0.0490(3) 0.2040(3) 0.0614(15) Uani 1 1 d . . . O12 O 1.0433(7) -0.1346(3) 0.1311(4) 0.091(2) Uani 1 1 d . . . O13 O 0.8895(6) -0.0586(3) 0.0905(3) 0.0638(15) Uani 1 1 d . . . O14 O 0.7019(5) 0.0660(3) 0.0449(3) 0.0583(15) Uani 1 1 d . . . O15 O 0.5638(6) 0.1530(3) 0.0160(3) 0.0722(18) Uani 1 1 d . . . O16 O 0.6641(5) 0.1379(3) 0.1326(3) 0.0600(15) Uani 1 1 d . . . N1 N 0.8498(6) -0.0872(4) 0.4200(4) 0.0530(17) Uani 1 1 d . . . N2 N 0.5109(7) 0.1140(3) 0.3488(5) 0.0570(18) Uani 1 1 d . . . N3 N 0.9790(7) -0.0816(3) 0.1421(5) 0.0542(18) Uani 1 1 d . . . N4 N 0.6415(6) 0.1198(3) 0.0640(4) 0.0503(16) Uani 1 1 d . . . C1 C 0.6060(9) -0.2086(5) 0.4456(7) 0.105(4) Uani 1 1 d . . . H1A H 0.6063 -0.2588 0.4557 0.158 Uiso 1 1 calc R . . H1B H 0.6615 -0.1848 0.4874 0.158 Uiso 1 1 calc R . . H1C H 0.6397 -0.2000 0.3989 0.158 Uiso 1 1 calc R . . C2 C 0.4657(7) -0.1806(4) 0.4379(5) 0.063(2) Uani 1 1 d . . . H2A H 0.4313 -0.1901 0.4848 0.076 Uiso 1 1 calc R . . H2B H 0.4095 -0.2052 0.3962 0.076 Uiso 1 1 calc R . . C3 C 0.2841(6) -0.0740(4) 0.4060(5) 0.054(2) Uani 1 1 d . . . H3A H 0.2393 -0.1066 0.3675 0.065 Uiso 1 1 calc R . . H3B H 0.2516 -0.0827 0.4537 0.065 Uiso 1 1 calc R . . C4 C 0.2538(6) 0.0025(4) 0.3800(4) 0.051(2) Uani 1 1 d . . . H4A H 0.2804 0.0099 0.3304 0.061 Uiso 1 1 calc R . . H4B H 0.3051 0.0349 0.4164 0.061 Uiso 1 1 calc R . . C5 C 0.1047(6) 0.0191(3) 0.3741(4) 0.0458(19) Uani 1 1 d . . . H5A H 0.0534 -0.0135 0.3381 0.055 Uiso 1 1 calc R . . H5B H 0.0784 0.0124 0.4239 0.055 Uiso 1 1 calc R . . C6 C 0.7338(7) -0.1969(4) 0.1862(5) 0.069(3) Uani 1 1 d . . . H6A H 0.7358 -0.2434 0.2089 0.104 Uiso 1 1 calc R . . H6B H 0.7942 -0.1662 0.2186 0.104 Uiso 1 1 calc R . . H6C H 0.7600 -0.2002 0.1366 0.104 Uiso 1 1 calc R . . C7 C 0.5946(7) -0.1672(3) 0.1776(5) 0.059(2) Uani 1 1 d . . . H7A H 0.5675 -0.1653 0.2277 0.071 Uiso 1 1 calc R . . H7B H 0.5337 -0.1987 0.1453 0.071 Uiso 1 1 calc R . . C8 C 0.4146(6) -0.0590(4) 0.1412(4) 0.0463(19) Uani 1 1 d . . . H8A H 0.3557 -0.0917 0.1093 0.056 Uiso 1 1 calc R . . H8B H 0.3990 -0.0638 0.1936 0.056 Uiso 1 1 calc R . . C9 C 0.3842(6) 0.0158(3) 0.1140(4) 0.0469(19) Uani 1 1 d . . . H9A H 0.4081 0.0220 0.0635 0.056 Uiso 1 1 calc R . . H9B H 0.4368 0.0489 0.1489 0.056 Uiso 1 1 calc R . . C10 C 0.2372(6) 0.0317(4) 0.1103(4) 0.050(2) Uani 1 1 d . . . H10A H 0.2128 0.0238 0.1604 0.060 Uiso 1 1 calc R . . H10B H 0.1850 -0.0005 0.0742 0.060 Uiso 1 1 calc R . . C11 C 0.8809(8) 0.2404(4) 0.0339(7) 0.100(4) Uani 1 1 d . . . H11A H 0.8802 0.2903 0.0225 0.151 Uiso 1 1 calc R . . H11B H 0.8431 0.2327 0.0795 0.151 Uiso 1 1 calc R . . H11C H 0.8293 0.2153 -0.0083 0.151 Uiso 1 1 calc R . . C12 C 1.0238(8) 0.2131(4) 0.0466(6) 0.070(3) Uani 1 1 d . . . H12A H 1.0765 0.2393 0.0884 0.084 Uiso 1 1 calc R . . H12B H 1.0621 0.2210 0.0006 0.084 Uiso 1 1 calc R . . C13 C 1.2053(6) 0.1080(4) 0.0855(5) 0.054(2) Uani 1 1 d . . . H13A H 1.2405 0.1181 0.0389 0.065 Uiso 1 1 calc R . . H13B H 1.2469 0.1404 0.1253 0.065 Uiso 1 1 calc R . . C14 C 0.7547(8) 0.2318(4) 0.2975(5) 0.080(3) Uani 1 1 d . . . H14A H 0.7511 0.2774 0.2729 0.120 Uiso 1 1 calc R . . H14B H 0.7309 0.2367 0.3476 0.120 Uiso 1 1 calc R . . H14C H 0.6933 0.1999 0.2672 0.120 Uiso 1 1 calc R . . C15 C 0.8965(7) 0.2016(3) 0.3052(5) 0.058(2) Uani 1 1 d . . . H15A H 0.9587 0.2338 0.3357 0.070 Uiso 1 1 calc R . . H15B H 0.9214 0.1976 0.2547 0.070 Uiso 1 1 calc R . . C16 C 1.0747(6) 0.0952(4) 0.3473(5) 0.053(2) Uani 1 1 d . . . H16A H 1.0925 0.1007 0.2954 0.064 Uiso 1 1 calc R . . H16C H 1.1325 0.1277 0.3803 0.064 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 Cd1 0.0355(3) 0.0395(3) 0.0389(3) 0.0006(3) 0.0104(2) 0.0011(2) Cd2 0.0351(3) 0.0375(3) 0.0373(3) -0.0009(2) 0.0096(2) -0.0018(2) S1 0.0424(11) 0.0524(13) 0.0574(14) 0.0060(10) 0.0160(10) 0.0003(9) S2 0.0354(10) 0.0438(11) 0.0463(12) -0.0126(9) 0.0069(9) -0.0083(8) S3 0.0373(10) 0.0528(12) 0.0434(12) -0.0143(9) 0.0022(9) -0.0029(9) S4 0.0440(12) 0.0594(14) 0.0604(15) 0.0095(11) 0.0141(10) -0.0023(10) O1 0.056(3) 0.051(3) 0.049(3) 0.000(2) 0.020(3) 0.001(3) O2 0.029(2) 0.035(3) 0.041(3) -0.010(2) 0.008(2) -0.009(2) O3 0.065(4) 0.066(4) 0.052(4) -0.008(3) 0.005(3) 0.016(3) O4 0.083(4) 0.076(4) 0.078(5) 0.012(4) -0.019(4) 0.025(4) O5 0.078(4) 0.070(4) 0.048(4) -0.005(3) -0.002(3) 0.026(3) O6 0.074(4) 0.069(4) 0.051(4) -0.001(3) 0.014(3) 0.024(3) O7 0.110(5) 0.053(4) 0.135(7) -0.001(4) 0.046(5) 0.041(4) O8 0.067(4) 0.072(4) 0.067(5) -0.001(3) 0.009(3) 0.015(3) O9 0.032(2) 0.036(3) 0.038(3) -0.005(2) 0.004(2) -0.005(2) O10 0.042(3) 0.055(3) 0.059(4) 0.006(3) 0.020(3) -0.003(2) O11 0.061(4) 0.065(4) 0.058(4) -0.004(3) 0.008(3) 0.011(3) O12 0.114(5) 0.052(4) 0.116(6) 0.011(4) 0.045(4) 0.041(4) O13 0.069(4) 0.076(4) 0.048(4) -0.007(3) 0.014(3) 0.021(3) O14 0.071(4) 0.051(3) 0.048(3) -0.013(3) -0.004(3) 0.021(3) O15 0.081(4) 0.057(3) 0.066(4) 0.002(3) -0.025(3) 0.022(3) O16 0.069(4) 0.069(4) 0.039(3) -0.009(3) 0.002(3) 0.004(3) N1 0.043(4) 0.061(5) 0.051(5) 0.004(4) -0.004(4) 0.000(3) N2 0.066(5) 0.035(4) 0.076(6) 0.004(4) 0.029(5) 0.010(4) N3 0.061(5) 0.038(4) 0.072(6) 0.008(4) 0.037(4) 0.001(4) N4 0.047(4) 0.047(4) 0.055(5) 0.005(4) 0.002(4) 0.000(3) C1 0.081(7) 0.068(6) 0.183(12) 0.029(7) 0.066(8) 0.017(5) C2 0.051(5) 0.060(5) 0.081(7) 0.018(5) 0.022(5) 0.006(4) C3 0.038(4) 0.064(5) 0.062(6) 0.010(4) 0.014(4) 0.001(4) C4 0.034(4) 0.067(5) 0.054(5) 0.009(4) 0.013(4) 0.003(4) C5 0.035(4) 0.053(5) 0.048(5) -0.010(4) 0.003(4) -0.004(4) C6 0.058(5) 0.045(5) 0.103(8) -0.017(5) 0.008(5) 0.006(4) C7 0.043(5) 0.043(5) 0.091(7) -0.018(4) 0.008(5) -0.008(4) C8 0.031(4) 0.062(5) 0.044(5) -0.006(4) 0.002(3) -0.008(4) C9 0.034(4) 0.049(5) 0.057(5) -0.006(4) 0.005(4) -0.008(3) C10 0.037(4) 0.061(5) 0.054(5) 0.007(4) 0.009(4) 0.003(4) C11 0.054(6) 0.071(6) 0.180(11) 0.055(7) 0.032(7) 0.011(5) C12 0.056(5) 0.054(5) 0.107(8) 0.028(5) 0.032(5) 0.003(4) C13 0.039(4) 0.064(5) 0.063(6) 0.007(4) 0.016(4) -0.003(4) C14 0.079(7) 0.066(6) 0.090(8) -0.015(5) -0.004(6) 0.021(5) C15 0.060(5) 0.035(4) 0.079(6) -0.014(4) 0.009(5) -0.007(4) C16 0.033(4) 0.063(5) 0.062(6) -0.005(4) 0.003(4) 0.000(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 Cd1 O1 2.231(5) . ? Cd1 O2 2.293(4) . ? Cd1 O5 2.317(5) . ? Cd1 O9 2.320(4) . ? Cd1 O6 2.388(5) . ? Cd1 O8 2.399(5) . ? Cd1 O3 2.477(5) . ? Cd2 O10 2.225(4) . ? Cd2 O9 2.292(4) . ? Cd2 O2 2.305(4) . ? Cd2 O14 2.325(5) . ? Cd2 O13 2.379(5) . ? Cd2 O11 2.416(5) . ? Cd2 O16 2.505(5) . ? S1 O1 1.545(5) . ? S1 C2 1.762(7) . ? S1 C3 1.782(7) . ? S2 O2 1.546(4) . ? S2 C7 1.772(7) . ? S2 C8 1.782(7) . ? S3 O9 1.553(4) . ? S3 C15 1.776(7) . ? S3 C16 1.776(7) . ? S4 O10 1.544(5) . ? S4 C12 1.774(7) . ? S4 C13 1.788(7) . ? O3 N1 1.230(7) . ? O4 N1 1.221(7) . ? O5 N1 1.273(7) . ? O6 N2 1.269(8) . ? O7 N2 1.217(7) . ? O8 N2 1.242(8) . ? O11 N3 1.239(8) . ? O12 N3 1.226(7) . ? O13 N3 1.252(8) . ? O14 N4 1.258(7) . ? O15 N4 1.227(7) . ? O16 N4 1.242(7) . ? C1 C2 1.506(10) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.525(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.535(9) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C16 1.521(8) 1_455 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.506(9) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.501(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.517(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C13 1.520(9) 1_455 ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.522(10) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C10 1.520(9) 1_655 ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.535(10) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C5 1.521(8) 1_655 ? C16 H16A 0.9700 . ? C16 H16C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O2 96.77(16) . . ? O1 Cd1 O5 94.88(19) . . ? O2 Cd1 O5 135.24(18) . . ? O1 Cd1 O9 171.20(16) . . ? O2 Cd1 O9 74.51(14) . . ? O5 Cd1 O9 92.28(18) . . ? O1 Cd1 O6 97.40(18) . . ? O2 Cd1 O6 140.78(17) . . ? O5 Cd1 O6 79.45(19) . . ? O9 Cd1 O6 88.94(17) . . ? O1 Cd1 O8 88.95(18) . . ? O2 Cd1 O8 90.80(19) . . ? O5 Cd1 O8 132.5(2) . . ? O9 Cd1 O8 89.98(17) . . ? O6 Cd1 O8 53.19(19) . . ? O1 Cd1 O3 89.85(17) . . ? O2 Cd1 O3 84.17(17) . . ? O5 Cd1 O3 52.76(18) . . ? O9 Cd1 O3 90.41(16) . . ? O6 Cd1 O3 132.14(19) . . ? O8 Cd1 O3 174.7(2) . . ? O10 Cd2 O9 95.57(16) . . ? O10 Cd2 O2 170.36(16) . . ? O9 Cd2 O2 74.80(14) . . ? O10 Cd2 O14 94.00(19) . . ? O9 Cd2 O14 135.89(17) . . ? O2 Cd2 O14 92.71(17) . . ? O10 Cd2 O13 100.82(19) . . ? O9 Cd2 O13 138.71(17) . . ? O2 Cd2 O13 87.10(17) . . ? O14 Cd2 O13 80.60(19) . . ? O10 Cd2 O11 88.90(17) . . ? O9 Cd2 O11 90.26(18) . . ? O2 Cd2 O11 91.60(16) . . ? O14 Cd2 O11 132.93(19) . . ? O13 Cd2 O11 52.85(18) . . ? O10 Cd2 O16 88.35(17) . . ? O9 Cd2 O16 84.96(16) . . ? O2 Cd2 O16 90.27(16) . . ? O14 Cd2 O16 52.38(16) . . ? O13 Cd2 O16 132.74(19) . . ? O11 Cd2 O16 174.23(18) . . ? O1 S1 C2 104.9(3) . . ? O1 S1 C3 104.6(3) . . ? C2 S1 C3 100.3(3) . . ? O2 S2 C7 104.9(3) . . ? O2 S2 C8 104.8(3) . . ? C7 S2 C8 100.9(3) . . ? O9 S3 C15 104.6(3) . . ? O9 S3 C16 104.9(3) . . ? C15 S3 C16 99.9(4) . . ? O10 S4 C12 104.8(4) . . ? O10 S4 C13 104.3(3) . . ? C12 S4 C13 99.2(3) . . ? S1 O1 Cd1 117.8(3) . . ? S2 O2 Cd1 134.7(2) . . ? S2 O2 Cd2 119.4(2) . . ? Cd1 O2 Cd2 105.58(15) . . ? N1 O3 Cd1 91.8(4) . . ? N1 O5 Cd1 98.3(4) . . ? N2 O6 Cd1 94.7(4) . . ? N2 O8 Cd1 94.9(5) . . ? S3 O9 Cd2 134.9(2) . . ? S3 O9 Cd1 119.8(2) . . ? Cd2 O9 Cd1 105.11(15) . . ? S4 O10 Cd2 116.3(3) . . ? N3 O11 Cd2 93.9(4) . . ? N3 O13 Cd2 95.3(4) . . ? N4 O14 Cd2 99.1(4) . . ? N4 O16 Cd2 90.9(4) . . ? O4 N1 O3 122.5(7) . . ? O4 N1 O5 120.5(7) . . ? O3 N1 O5 117.1(6) . . ? O7 N2 O8 123.0(8) . . ? O7 N2 O6 119.8(8) . . ? O8 N2 O6 117.2(6) . . ? O12 N3 O11 121.6(8) . . ? O12 N3 O13 120.4(8) . . ? O11 N3 O13 117.9(7) . . ? O15 N4 O16 121.8(7) . . ? O15 N4 O14 120.7(7) . . ? O16 N4 O14 117.5(6) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 S1 111.4(6) . . ? C1 C2 H2A 109.4 . . ? S1 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? S1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C4 C3 S1 109.3(5) . . ? C4 C3 H3A 109.8 . . ? S1 C3 H3A 109.8 . . ? C4 C3 H3B 109.8 . . ? S1 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? C3 C4 C5 111.0(6) . . ? C3 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C16 C5 C4 110.9(6) 1_455 . ? C16 C5 H5A 109.5 1_455 . ? C4 C5 H5A 109.5 . . ? C16 C5 H5B 109.5 1_455 . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C6 C7 S2 112.0(5) . . ? C6 C7 H7A 109.2 . . ? S2 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? S2 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C9 C8 S2 110.5(5) . . ? C9 C8 H8A 109.6 . . ? S2 C8 H8A 109.6 . . ? C9 C8 H8B 109.6 . . ? S2 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C8 C9 C10 110.2(6) . . ? C8 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? C8 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C9 C10 C13 111.0(6) . 1_455 ? C9 C10 H10A 109.4 . . ? C13 C10 H10A 109.4 1_455 . ? C9 C10 H10B 109.4 . . ? C13 C10 H10B 109.4 1_455 . ? H10A C10 H10B 108.0 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C11 C12 S4 110.6(5) . . ? C11 C12 H12A 109.5 . . ? S4 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? S4 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C10 C13 S4 109.6(5) 1_655 . ? C10 C13 H13A 109.7 1_655 . ? S4 C13 H13A 109.7 . . ? C10 C13 H13B 109.7 1_655 . ? S4 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C15 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C14 C15 S3 110.4(6) . . ? C14 C15 H15A 109.6 . . ? S3 C15 H15A 109.6 . . ? C14 C15 H15B 109.6 . . ? S3 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? C5 C16 S3 110.5(5) 1_655 . ? C5 C16 H16A 109.5 1_655 . ? S3 C16 H16A 109.5 . . ? C5 C16 H16C 109.5 1_655 . ? S3 C16 H16C 109.5 . . ? H16A C16 H16C 108.1 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.447 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.120 data_1 _database_code_depnum_ccdc_archive 'CCDC 225746' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H48 Cd Cl2 N0 O14 S6' _chemical_formula_weight 1188.49 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' Cl Cl 0.1484 0.1585 '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' 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/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 14.030(5) _cell_length_b 9.517(4) _cell_length_c 20.476(8) _cell_angle_alpha 90.00 _cell_angle_beta 108.790(6) _cell_angle_gamma 90.00 _cell_volume 2588.4(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 851 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 26.14 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.829 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7601 _exptl_absorpt_correction_T_max 0.8517 _exptl_absorpt_process_details SADABS _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 10546 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4588 _reflns_number_gt 3443 _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^)+(0.0642P)^2^+0.1229P] 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 4588 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.1011 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.5000 0.5000 0.5000 0.03965(13) Uani 1 2 d S . . S1 S 0.70112(8) 0.28597(9) 0.54254(5) 0.0550(3) Uani 1 1 d . . . S2 S 0.36727(8) 0.23393(10) 0.53834(5) 0.0543(3) Uani 1 1 d . . . S3 S 0.56927(9) 0.58462(11) 0.66637(5) 0.0645(3) Uani 1 1 d . . . O1 O 0.5978(2) 0.3133(3) 0.49132(14) 0.0656(7) Uani 1 1 d . . . O2 O 0.3740(2) 0.3404(3) 0.48537(13) 0.0599(7) Uani 1 1 d . . . O3 O 0.5538(2) 0.4625(3) 0.61578(13) 0.0577(7) Uani 1 1 d . . . C1 C 0.7775(3) 0.2301(3) 0.49255(19) 0.0497(9) Uani 1 1 d . . . C2 C 0.8787(3) 0.2073(4) 0.5263(2) 0.0641(11) Uani 1 1 d . . . H2A H 0.9061 0.2209 0.5737 0.077 Uiso 1 1 calc R . . C3 C 0.9377(4) 0.1641(5) 0.4882(3) 0.0841(14) Uani 1 1 d . . . H3A H 1.0060 0.1484 0.5101 0.101 Uiso 1 1 calc R . . C4 C 0.8974(5) 0.1434(5) 0.4181(4) 0.0978(18) Uani 1 1 d . . . H4A H 0.9380 0.1129 0.3929 0.117 Uiso 1 1 calc R . . C5 C 0.7966(5) 0.1683(5) 0.3856(3) 0.0898(16) Uani 1 1 d . . . H5A H 0.7694 0.1552 0.3382 0.108 Uiso 1 1 calc R . . C6 C 0.7352(4) 0.2125(4) 0.4225(2) 0.0654(11) Uani 1 1 d . . . H6A H 0.6672 0.2299 0.4006 0.078 Uiso 1 1 calc R . . C7 C 0.6895(3) 0.1242(4) 0.5844(2) 0.0632(11) Uani 1 1 d . . . H7A H 0.7565 0.0924 0.6109 0.076 Uiso 1 1 calc R . . H7B H 0.6536 0.1433 0.6168 0.076 Uiso 1 1 calc R . . C8 C 0.6360(3) 0.0053(4) 0.5374(2) 0.0623(11) Uani 1 1 d . . . H8A H 0.5854 0.0454 0.4976 0.075 Uiso 1 1 calc R . . H8B H 0.6014 -0.0519 0.5619 0.075 Uiso 1 1 calc R . . C9 C 0.2716(3) 0.2952(4) 0.5717(2) 0.0608(11) Uani 1 1 d . . . C10 C 0.2639(4) 0.2286(6) 0.6302(2) 0.0841(15) Uani 1 1 d . . . H10A H 0.3073 0.1557 0.6509 0.101 Uiso 1 1 calc R . . C11 C 0.1910(5) 0.2730(9) 0.6564(3) 0.112(2) Uani 1 1 d . . . H11A H 0.1825 0.2274 0.6943 0.134 Uiso 1 1 calc R . . C12 C 0.1316(5) 0.3813(8) 0.6278(4) 0.111(2) Uani 1 1 d . . . H12A H 0.0839 0.4123 0.6472 0.133 Uiso 1 1 calc R . . C13 C 0.1396(5) 0.4470(6) 0.5712(4) 0.124(3) Uani 1 1 d . . . H13A H 0.0974 0.5221 0.5522 0.149 Uiso 1 1 calc R . . C14 C 0.2108(4) 0.4028(5) 0.5411(3) 0.0951(18) Uani 1 1 d . . . H14A H 0.2161 0.4457 0.5016 0.114 Uiso 1 1 calc R . . C15 C 0.2957(3) 0.0894(4) 0.4879(2) 0.0570(10) Uani 1 1 d . . . H15A H 0.2650 0.0352 0.5160 0.068 Uiso 1 1 calc R . . H15B H 0.2423 0.1262 0.4487 0.068 Uiso 1 1 calc R . . C16 C 0.6937(4) 0.6460(6) 0.6815(2) 0.0815(15) Uani 1 1 d . . . C17 C 0.7133(5) 0.7894(6) 0.6920(2) 0.107(2) Uani 1 1 d . . . H17A H 0.6630 0.8517 0.6935 0.128 Uiso 1 1 calc R . . C18 C 0.8091(8) 0.8359(11) 0.7002(4) 0.168(5) Uani 1 1 d . . . H18A H 0.8252 0.9300 0.7101 0.201 Uiso 1 1 calc R . . C19 C 0.8810(8) 0.7454(17) 0.6940(6) 0.193(7) Uani 1 1 d . . . H19A H 0.9436 0.7805 0.6956 0.232 Uiso 1 1 calc R . . C20 C 0.8635(6) 0.6055(12) 0.6854(4) 0.153(4) Uani 1 1 d . . . H20A H 0.9147 0.5447 0.6840 0.184 Uiso 1 1 calc R . . C21 C 0.7682(5) 0.5539(8) 0.6788(3) 0.1001(17) Uani 1 1 d . . . H21A H 0.7548 0.4583 0.6727 0.120 Uiso 1 1 calc R . . C22 C 0.5898(4) 0.4975(5) 0.7491(2) 0.0728(13) Uani 1 1 d . . . H22A H 0.6483 0.4370 0.7587 0.087 Uiso 1 1 calc R . . H22B H 0.6035 0.5678 0.7852 0.087 Uiso 1 1 calc R . . C23 C 0.5000 0.4109(7) 0.7500 0.0706(17) Uani 1 2 d S . . H23A H 0.517(7) 0.341(9) 0.792(4) 0.085 Uiso 0.50 1 d P . . Cl1 Cl 1.0000 0.15978(16) 0.7500 0.0669(4) Uani 1 2 d S . . O4 O 0.9190(4) 0.2425(6) 0.7168(2) 0.161(2) Uani 1 1 d . . . O5 O 1.0204(4) 0.0765(4) 0.6990(2) 0.1217(14) Uani 1 1 d . . . Cl2 Cl 0.5000 0.0169(2) 0.2500 0.1548(15) Uani 1 2 d S . . O6 O 0.5418(9) 0.1439(9) 0.2676(8) 0.207(7) Uani 0.67 1 d P . . O7 O 0.4267(10) -0.0599(8) 0.2700(6) 0.166(4) Uani 0.67 1 d P . . O8 O 0.5442(16) -0.0038(16) 0.3140(11) 0.385(16) Uani 0.67 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0449(2) 0.02727(19) 0.0468(2) 0.00336(15) 0.01478(16) -0.00214(15) S1 0.0663(7) 0.0366(5) 0.0583(6) -0.0060(4) 0.0149(5) 0.0073(4) S2 0.0584(6) 0.0432(5) 0.0577(6) 0.0062(4) 0.0133(5) -0.0137(4) S3 0.0793(8) 0.0605(7) 0.0466(6) -0.0014(5) 0.0104(5) -0.0015(5) O1 0.0680(18) 0.0458(15) 0.0754(18) -0.0064(14) 0.0126(15) 0.0176(13) O2 0.0646(18) 0.0540(15) 0.0591(16) 0.0090(13) 0.0169(14) -0.0229(13) O3 0.0688(18) 0.0511(14) 0.0476(15) 0.0063(11) 0.0108(13) -0.0048(13) C1 0.062(2) 0.0325(18) 0.055(2) -0.0002(16) 0.0192(19) 0.0026(17) C2 0.062(3) 0.048(2) 0.075(3) -0.005(2) 0.012(2) 0.001(2) C3 0.080(4) 0.066(3) 0.114(4) 0.001(3) 0.043(3) 0.011(3) C4 0.123(5) 0.075(3) 0.123(5) -0.004(3) 0.079(5) 0.008(3) C5 0.128(5) 0.084(4) 0.069(3) 0.004(3) 0.049(3) 0.007(3) C6 0.078(3) 0.053(2) 0.063(3) 0.005(2) 0.020(2) 0.004(2) C7 0.084(3) 0.052(2) 0.061(3) 0.005(2) 0.034(2) 0.008(2) C8 0.061(3) 0.055(2) 0.075(3) 0.008(2) 0.027(2) -0.002(2) C9 0.073(3) 0.042(2) 0.070(3) -0.009(2) 0.026(2) -0.023(2) C10 0.093(4) 0.096(4) 0.065(3) -0.002(3) 0.027(3) -0.024(3) C11 0.113(5) 0.150(6) 0.090(4) -0.030(4) 0.056(4) -0.043(5) C12 0.101(5) 0.099(5) 0.158(7) -0.046(5) 0.077(5) -0.038(4) C13 0.128(6) 0.059(3) 0.213(8) -0.007(4) 0.093(6) -0.003(4) C14 0.107(4) 0.051(3) 0.153(5) 0.013(3) 0.076(4) -0.004(3) C15 0.057(2) 0.042(2) 0.071(3) -0.0040(18) 0.020(2) -0.0142(18) C16 0.098(4) 0.094(4) 0.041(2) -0.006(2) 0.005(2) -0.038(3) C17 0.150(6) 0.090(4) 0.053(3) 0.011(3) -0.005(3) -0.029(4) C18 0.202(10) 0.174(9) 0.068(4) 0.041(5) -0.038(6) -0.136(8) C19 0.126(8) 0.32(2) 0.103(6) 0.052(9) -0.013(6) -0.118(10) C20 0.085(5) 0.264(12) 0.095(5) 0.001(6) 0.006(4) -0.062(6) C21 0.081(4) 0.136(5) 0.071(3) -0.022(3) 0.009(3) -0.029(4) C22 0.079(3) 0.089(3) 0.046(2) 0.006(2) 0.013(2) 0.001(3) C23 0.083(5) 0.066(4) 0.062(4) 0.000 0.022(4) 0.000 Cl1 0.0725(10) 0.0652(9) 0.0672(9) 0.000 0.0280(8) 0.000 O4 0.152(4) 0.222(6) 0.112(3) 0.045(3) 0.047(3) 0.103(4) O5 0.185(4) 0.102(3) 0.103(3) -0.013(2) 0.081(3) 0.011(3) Cl2 0.1010(19) 0.0557(13) 0.229(4) 0.000 -0.057(2) 0.000 O6 0.29(2) 0.137(6) 0.227(17) -0.092(10) 0.123(15) -0.080(8) O7 0.260(12) 0.078(4) 0.163(8) -0.014(5) 0.074(8) -0.051(6) O8 0.28(2) 0.254(18) 0.48(4) 0.20(2) -0.08(2) 0.049(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O3 2.273(3) 3_666 ? Cd1 O3 2.273(3) . ? Cd1 O2 2.277(2) 3_666 ? Cd1 O2 2.277(2) . ? Cd1 O1 2.286(3) . ? Cd1 O1 2.286(3) 3_666 ? S1 O1 1.513(3) . ? S1 C1 1.785(4) . ? S1 C7 1.794(4) . ? S2 O2 1.509(3) . ? S2 C9 1.789(4) . ? S2 C15 1.817(4) . ? S3 O3 1.525(3) . ? S3 C16 1.771(5) . ? S3 C22 1.823(4) . ? C1 C6 1.374(5) . ? C1 C2 1.381(5) . ? C2 C3 1.371(6) . ? C3 C4 1.378(8) . ? C4 C5 1.376(8) . ? C5 C6 1.382(6) . ? C7 C8 1.518(6) . ? C8 C15 1.522(5) 3_656 ? C9 C14 1.351(7) . ? C9 C10 1.388(6) . ? C10 C11 1.367(7) . ? C11 C12 1.336(9) . ? C12 C13 1.352(9) . ? C13 C14 1.397(7) . ? C15 C8 1.522(5) 3_656 ? C16 C21 1.378(8) . ? C16 C17 1.395(7) . ? C17 C18 1.373(10) . ? C18 C19 1.363(15) . ? C19 C20 1.355(15) . ? C20 C21 1.390(8) . ? C22 C23 1.511(6) . ? C23 C22 1.511(6) 2_656 ? Cl1 O4 1.369(4) 2_756 ? Cl1 O4 1.369(4) . ? Cl1 O5 1.412(4) 2_756 ? Cl1 O5 1.412(4) . ? Cl2 O8 1.272(18) . ? Cl2 O8 1.272(18) 2_655 ? Cl2 O6 1.341(8) . ? Cl2 O6 1.341(8) 2_655 ? Cl2 O7 1.425(10) 2_655 ? Cl2 O7 1.425(10) . ? O6 O6 1.16(2) 2_655 ? O6 O8 1.692(19) . ? O7 O8 1.691(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cd1 O3 180.000(1) 3_666 . ? O3 Cd1 O2 90.88(9) 3_666 3_666 ? O3 Cd1 O2 89.12(9) . 3_666 ? O3 Cd1 O2 89.12(9) 3_666 . ? O3 Cd1 O2 90.88(9) . . ? O2 Cd1 O2 180.00(9) 3_666 . ? O3 Cd1 O1 92.67(10) 3_666 . ? O3 Cd1 O1 87.33(10) . . ? O2 Cd1 O1 93.95(11) 3_666 . ? O2 Cd1 O1 86.05(11) . . ? O3 Cd1 O1 87.33(10) 3_666 3_666 ? O3 Cd1 O1 92.67(10) . 3_666 ? O2 Cd1 O1 86.05(11) 3_666 3_666 ? O2 Cd1 O1 93.95(11) . 3_666 ? O1 Cd1 O1 180.00(14) . 3_666 ? O1 S1 C1 105.78(17) . . ? O1 S1 C7 105.31(19) . . ? C1 S1 C7 100.49(17) . . ? O2 S2 C9 106.50(18) . . ? O2 S2 C15 104.52(17) . . ? C9 S2 C15 96.82(18) . . ? O3 S3 C16 106.7(2) . . ? O3 S3 C22 103.29(19) . . ? C16 S3 C22 97.8(2) . . ? S1 O1 Cd1 122.99(15) . . ? S2 O2 Cd1 125.37(15) . . ? S3 O3 Cd1 121.06(15) . . ? C6 C1 C2 122.1(4) . . ? C6 C1 S1 119.8(3) . . ? C2 C1 S1 118.0(3) . . ? C3 C2 C1 118.3(4) . . ? C2 C3 C4 121.0(5) . . ? C5 C4 C3 119.5(5) . . ? C4 C5 C6 120.8(5) . . ? C1 C6 C5 118.2(5) . . ? C8 C7 S1 116.1(3) . . ? C7 C8 C15 114.9(4) . 3_656 ? C14 C9 C10 122.2(5) . . ? C14 C9 S2 120.6(4) . . ? C10 C9 S2 117.2(4) . . ? C11 C10 C9 118.2(6) . . ? C12 C11 C10 120.4(6) . . ? C11 C12 C13 121.4(6) . . ? C12 C13 C14 120.5(6) . . ? C9 C14 C13 117.3(6) . . ? C8 C15 S2 110.4(3) 3_656 . ? C21 C16 C17 120.9(6) . . ? C21 C16 S3 120.0(4) . . ? C17 C16 S3 119.0(5) . . ? C18 C17 C16 118.1(8) . . ? C19 C18 C17 120.7(10) . . ? C20 C19 C18 121.6(11) . . ? C19 C20 C21 119.2(11) . . ? C16 C21 C20 119.3(8) . . ? C23 C22 S3 112.2(3) . . ? C22 C23 C22 113.8(6) . 2_656 ? O4 Cl1 O4 109.8(6) 2_756 . ? O4 Cl1 O5 106.8(3) 2_756 2_756 ? O4 Cl1 O5 110.9(3) . 2_756 ? O4 Cl1 O5 110.9(3) 2_756 . ? O4 Cl1 O5 106.8(3) . . ? O5 Cl1 O5 111.7(4) 2_756 . ? O8 Cl2 O8 162.2(16) . 2_655 ? O8 Cl2 O6 80.6(10) . . ? O8 Cl2 O6 116.2(11) 2_655 . ? O8 Cl2 O6 116.2(11) . 2_655 ? O8 Cl2 O6 80.6(10) 2_655 2_655 ? O6 Cl2 O6 51.4(10) . 2_655 ? O8 Cl2 O7 93.4(9) . 2_655 ? O8 Cl2 O7 77.4(9) 2_655 2_655 ? O6 Cl2 O7 104.2(8) . 2_655 ? O6 Cl2 O7 132.8(8) 2_655 2_655 ? O8 Cl2 O7 77.4(9) . . ? O8 Cl2 O7 93.4(9) 2_655 . ? O6 Cl2 O7 132.8(8) . . ? O6 Cl2 O7 104.2(8) 2_655 . ? O7 Cl2 O7 118.3(8) 2_655 . ? O6 O6 Cl2 64.3(5) 2_655 . ? O6 O6 O8 100.4(13) 2_655 . ? Cl2 O6 O8 47.9(8) . . ? Cl2 O7 O8 47.2(8) . . ? Cl2 O8 O7 55.4(8) . . ? Cl2 O8 O6 51.5(7) . . ? O7 O8 O6 97.1(9) . . ? 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 C1 S1 O1 Cd1 -139.54(18) . . . . ? C7 S1 O1 Cd1 114.6(2) . . . . ? O3 Cd1 O1 S1 140.5(2) 3_666 . . . ? O3 Cd1 O1 S1 -39.5(2) . . . . ? O2 Cd1 O1 S1 49.4(2) 3_666 . . . ? O2 Cd1 O1 S1 -130.6(2) . . . . ? O1 Cd1 O1 S1 -123(100) 3_666 . . . ? C9 S2 O2 Cd1 105.9(2) . . . . ? C15 S2 O2 Cd1 -152.28(19) . . . . ? O3 Cd1 O2 S2 165.0(2) 3_666 . . . ? O3 Cd1 O2 S2 -15.0(2) . . . . ? O2 Cd1 O2 S2 54(100) 3_666 . . . ? O1 Cd1 O2 S2 72.2(2) . . . . ? O1 Cd1 O2 S2 -107.8(2) 3_666 . . . ? C16 S3 O3 Cd1 -87.2(2) . . . . ? C22 S3 O3 Cd1 170.3(2) . . . . ? O3 Cd1 O3 S3 -175(100) 3_666 . . . ? O2 Cd1 O3 S3 52.22(19) 3_666 . . . ? O2 Cd1 O3 S3 -127.78(19) . . . . ? O1 Cd1 O3 S3 146.22(19) . . . . ? O1 Cd1 O3 S3 -33.78(19) 3_666 . . . ? O1 S1 C1 C6 -3.8(3) . . . . ? C7 S1 C1 C6 105.5(3) . . . . ? O1 S1 C1 C2 175.5(3) . . . . ? C7 S1 C1 C2 -75.1(3) . . . . ? C6 C1 C2 C3 -0.8(6) . . . . ? S1 C1 C2 C3 179.9(3) . . . . ? C1 C2 C3 C4 -0.2(7) . . . . ? C2 C3 C4 C5 0.8(8) . . . . ? C3 C4 C5 C6 -0.6(8) . . . . ? C2 C1 C6 C5 1.1(6) . . . . ? S1 C1 C6 C5 -179.6(3) . . . . ? C4 C5 C6 C1 -0.4(7) . . . . ? O1 S1 C7 C8 46.7(3) . . . . ? C1 S1 C7 C8 -63.0(4) . . . . ? S1 C7 C8 C15 89.8(4) . . . 3_656 ? O2 S2 C9 C14 10.7(4) . . . . ? C15 S2 C9 C14 -96.6(4) . . . . ? O2 S2 C9 C10 -168.6(3) . . . . ? C15 S2 C9 C10 84.0(4) . . . . ? C14 C9 C10 C11 1.1(7) . . . . ? S2 C9 C10 C11 -179.6(4) . . . . ? C9 C10 C11 C12 -2.6(9) . . . . ? C10 C11 C12 C13 2.2(10) . . . . ? C11 C12 C13 C14 -0.1(11) . . . . ? C10 C9 C14 C13 0.9(8) . . . . ? S2 C9 C14 C13 -178.4(4) . . . . ? C12 C13 C14 C9 -1.4(9) . . . . ? O2 S2 C15 C8 82.0(3) . . . 3_656 ? C9 S2 C15 C8 -168.9(3) . . . 3_656 ? O3 S3 C16 C21 -31.0(4) . . . . ? C22 S3 C16 C21 75.4(4) . . . . ? O3 S3 C16 C17 145.3(4) . . . . ? C22 S3 C16 C17 -108.2(4) . . . . ? C21 C16 C17 C18 -0.5(8) . . . . ? S3 C16 C17 C18 -176.8(4) . . . . ? C16 C17 C18 C19 3.9(12) . . . . ? C17 C18 C19 C20 -5.7(17) . . . . ? C18 C19 C20 C21 3.8(16) . . . . ? C17 C16 C21 C20 -1.3(8) . . . . ? S3 C16 C21 C20 175.0(4) . . . . ? C19 C20 C21 C16 -0.4(11) . . . . ? O3 S3 C22 C23 -61.4(4) . . . . ? C16 S3 C22 C23 -170.7(4) . . . . ? S3 C22 C23 C22 -71.3(2) . . . 2_656 ? O8 Cl2 O6 O6 -135(2) . . . 2_655 ? O8 Cl2 O6 O6 51(2) 2_655 . . 2_655 ? O7 Cl2 O6 O6 134.0(15) 2_655 . . 2_655 ? O7 Cl2 O6 O6 -72(2) . . . 2_655 ? O8 Cl2 O6 O8 -173.9(6) 2_655 . . . ? O6 Cl2 O6 O8 135(2) 2_655 . . . ? O7 Cl2 O6 O8 -91.2(10) 2_655 . . . ? O7 Cl2 O6 O8 63.0(12) . . . . ? O8 Cl2 O7 O8 164.6(14) 2_655 . . . ? O6 Cl2 O7 O8 -64.3(12) . . . . ? O6 Cl2 O7 O8 -114.3(11) 2_655 . . . ? O7 Cl2 O7 O8 87.1(9) 2_655 . . . ? O8 Cl2 O8 O7 -60.2(5) 2_655 . . . ? O6 Cl2 O8 O7 137.9(9) . . . . ? O6 Cl2 O8 O7 99.8(10) 2_655 . . . ? O7 Cl2 O8 O7 -118.3(9) 2_655 . . . ? O8 Cl2 O8 O6 161.9(7) 2_655 . . . ? O6 Cl2 O8 O6 -38.1(15) 2_655 . . . ? O7 Cl2 O8 O6 103.8(8) 2_655 . . . ? O7 Cl2 O8 O6 -137.9(9) . . . . ? Cl2 O7 O8 O6 31.9(8) . . . . ? O6 O6 O8 Cl2 40.5(16) 2_655 . . . ? O6 O6 O8 O7 7(2) 2_655 . . . ? Cl2 O6 O8 O7 -33.8(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.514 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.073 data_2 _database_code_depnum_ccdc_archive 'CCDC 225747' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H55 Cd Cl5 O14 S6' _chemical_formula_weight 1349.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Trigonal _symmetry_space_group_name_H-M ' P-3 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 10.636(2) _cell_length_b 10.636(2) _cell_length_c 17.934(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1757.1(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 826 _cell_measurement_theta_min 2.2712 _cell_measurement_theta_max 24.1565 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 690 _exptl_absorpt_coefficient_mu 0.729 _exptl_absorpt_correction_type 'Multi-scan ' _exptl_absorpt_correction_T_min 0.8218 _exptl_absorpt_correction_T_max 0.8679 _exptl_absorpt_process_details SADABS _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 3496 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.06 _diffrn_reflns_theta_max 19.97 _reflns_number_total 1043 _reflns_number_gt 979 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0909P)^2^+25.8069P] 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 1043 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_gt 0.0917 _refine_ls_wR_factor_ref 0.2329 _refine_ls_wR_factor_gt 0.2312 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 Cd1 Cd 0.0000 0.0000 0.5000 0.0329(9) Uani 1 6 d S . . Cl1 Cl 0.6667 0.3333 0.6832(3) 0.0499(17) Uani 1 3 d S . . Cl2 Cl 0.8274(15) 0.350(2) 0.9596(7) 0.180(9) Uani 0.50 1 d P . . S1 S 0.2462(4) 0.2481(4) 0.6173(2) 0.0501(12) Uani 1 1 d . . . C1 C 0.0889(17) 0.3157(18) 0.7115(8) 0.064(4) Uani 1 1 d . . . H1A H 0.0280 0.2984 0.6709 0.076 Uiso 1 1 calc R . . C2 C 0.060(2) 0.358(3) 0.7799(11) 0.099(7) Uani 1 1 d . . . H2A H -0.0210 0.3686 0.7860 0.118 Uiso 1 1 calc R . . C3 C 0.152(3) 0.382(3) 0.8369(12) 0.127(9) Uani 1 1 d . . . H3A H 0.1343 0.4136 0.8821 0.152 Uiso 1 1 calc R . . C4 C 0.265(3) 0.364(3) 0.8318(11) 0.111(8) Uani 1 1 d . . . H4A H 0.3240 0.3806 0.8731 0.133 Uiso 1 1 calc R . . C5 C 0.295(2) 0.320(3) 0.7658(11) 0.093(6) Uani 1 1 d . . . H5A H 0.3731 0.3039 0.7620 0.112 Uiso 1 1 calc R . . C6 C 0.2077(16) 0.3005(15) 0.7053(8) 0.052(4) Uani 1 1 d . . . C7 C 0.3769(16) 0.4251(16) 0.5874(8) 0.062(4) Uani 1 1 d . . . H7A H 0.3319 0.4850 0.5857 0.075 Uiso 1 1 calc R . . H7B H 0.4549 0.4675 0.6237 0.075 Uiso 1 1 calc R . . C8 C 0.4417(16) 0.4274(15) 0.5099(8) 0.058(4) Uani 1 1 d . . . H8A H 0.4792 0.3609 0.5100 0.070 Uiso 1 1 calc R . . H8B H 0.3656 0.3942 0.4726 0.070 Uiso 1 1 calc R . . C9 C 0.6667 0.3333 0.926(3) 0.09(2) Uani 0.50 3 d SP . . H9A H 0.6667 0.3333 0.8714 0.106 Uiso 0.50 3 calc SPR . . O1 O 0.1117(9) 0.2071(9) 0.5692(4) 0.045(2) Uani 1 1 d . . . O2 O 0.7781(18) 0.3099(18) 0.6599(13) 0.159(8) Uani 1 1 d . . . O3 O 0.6667 0.3333 0.7554(15) 0.26(3) Uani 1 3 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0327(11) 0.0327(11) 0.0335(14) 0.000 0.000 0.0163(5) Cl1 0.045(2) 0.045(2) 0.060(4) 0.000 0.000 0.0225(12) Cl2 0.120(10) 0.37(3) 0.105(9) 0.068(12) 0.034(8) 0.162(15) S1 0.048(2) 0.050(2) 0.054(2) -0.0003(17) -0.0015(17) 0.0257(19) C1 0.051(10) 0.096(13) 0.048(10) 0.003(9) 0.005(8) 0.040(9) C2 0.089(14) 0.18(2) 0.056(12) -0.016(13) 0.010(12) 0.089(15) C3 0.13(2) 0.18(3) 0.056(14) -0.035(14) 0.011(15) 0.07(2) C4 0.095(17) 0.19(3) 0.065(15) -0.030(14) -0.023(12) 0.082(17) C5 0.067(12) 0.15(2) 0.072(13) -0.006(13) -0.006(11) 0.065(13) C6 0.054(10) 0.057(9) 0.050(9) -0.006(7) -0.005(8) 0.030(8) C7 0.058(10) 0.055(10) 0.066(11) -0.018(8) -0.013(8) 0.021(8) C8 0.050(9) 0.043(8) 0.065(10) -0.008(7) 0.013(8) 0.012(6) C9 0.13(3) 0.13(3) 0.01(3) 0.000 0.000 0.063(17) O1 0.048(6) 0.041(5) 0.049(5) -0.014(4) -0.016(4) 0.024(4) O2 0.097(11) 0.127(13) 0.29(2) 0.001(14) 0.037(13) 0.081(11) O3 0.38(4) 0.38(4) 0.035(16) 0.000 0.000 0.19(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 Cd1 O1 2.277(8) . ? Cd1 O1 2.277(8) 4_556 ? Cd1 O1 2.277(8) 5_556 ? Cd1 O1 2.277(8) 2 ? Cd1 O1 2.277(8) 6_556 ? Cd1 O1 2.277(8) 3 ? Cl1 O3 1.30(3) . ? Cl1 O2 1.392(14) . ? Cl1 O2 1.392(14) 3_665 ? Cl1 O2 1.392(14) 2_655 ? Cl2 C9 1.74(2) . ? S1 O1 1.535(9) . ? S1 C7 1.775(16) . ? S1 C6 1.788(14) . ? C1 C6 1.36(2) . ? C1 C2 1.39(2) . ? C2 C3 1.35(3) . ? C3 C4 1.31(3) . ? C4 C5 1.37(3) . ? C5 C6 1.38(2) . ? C7 C8 1.55(2) . ? C8 C8 1.46(3) 4_666 ? C9 Cl2 1.74(2) 3_665 ? C9 Cl2 1.74(2) 2_655 ? 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 Cd1 O1 180.0(3) . 4_556 ? O1 Cd1 O1 86.9(3) . 5_556 ? O1 Cd1 O1 93.1(3) 4_556 5_556 ? O1 Cd1 O1 93.1(3) . 2 ? O1 Cd1 O1 86.9(3) 4_556 2 ? O1 Cd1 O1 180.000(1) 5_556 2 ? O1 Cd1 O1 86.9(3) . 6_556 ? O1 Cd1 O1 93.1(3) 4_556 6_556 ? O1 Cd1 O1 93.1(3) 5_556 6_556 ? O1 Cd1 O1 86.9(3) 2 6_556 ? O1 Cd1 O1 93.1(3) . 3 ? O1 Cd1 O1 86.9(3) 4_556 3 ? O1 Cd1 O1 86.9(3) 5_556 3 ? O1 Cd1 O1 93.1(3) 2 3 ? O1 Cd1 O1 180.0(3) 6_556 3 ? O3 Cl1 O2 107.4(10) . . ? O3 Cl1 O2 107.4(10) . 3_665 ? O2 Cl1 O2 111.4(9) . 3_665 ? O3 Cl1 O2 107.4(10) . 2_655 ? O2 Cl1 O2 111.4(9) . 2_655 ? O2 Cl1 O2 111.4(9) 3_665 2_655 ? O1 S1 C7 104.8(6) . . ? O1 S1 C6 105.0(6) . . ? C7 S1 C6 96.7(7) . . ? C6 C1 C2 118.7(15) . . ? C3 C2 C1 118.4(18) . . ? C4 C3 C2 123.1(19) . . ? C3 C4 C5 120.1(19) . . ? C4 C5 C6 118.4(17) . . ? C1 C6 C5 121.2(15) . . ? C1 C6 S1 118.8(11) . . ? C5 C6 S1 120.0(13) . . ? C8 C7 S1 113.3(10) . . ? C8 C8 C7 111.8(15) 4_666 . ? Cl2 C9 Cl2 108.6(16) . 3_665 ? Cl2 C9 Cl2 108.6(16) . 2_655 ? Cl2 C9 Cl2 108.6(16) 3_665 2_655 ? S1 O1 Cd1 122.9(5) . . ? 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 C6 C1 C2 C3 0(3) . . . . ? C1 C2 C3 C4 -2(4) . . . . ? C2 C3 C4 C5 1(4) . . . . ? C3 C4 C5 C6 2(4) . . . . ? C2 C1 C6 C5 3(3) . . . . ? C2 C1 C6 S1 -179.5(15) . . . . ? C4 C5 C6 C1 -4(3) . . . . ? C4 C5 C6 S1 178.3(18) . . . . ? O1 S1 C6 C1 -9.1(14) . . . . ? C7 S1 C6 C1 98.2(14) . . . . ? O1 S1 C6 C5 168.8(14) . . . . ? C7 S1 C6 C5 -83.9(16) . . . . ? O1 S1 C7 C8 -73.2(12) . . . . ? C6 S1 C7 C8 179.4(12) . . . . ? S1 C7 C8 C8 -174.7(15) . . . 4_666 ? C7 S1 O1 Cd1 125.8(7) . . . . ? C6 S1 O1 Cd1 -132.9(6) . . . . ? O1 Cd1 O1 S1 63(35) 4_556 . . . ? O1 Cd1 O1 S1 -65.6(4) 5_556 . . . ? O1 Cd1 O1 S1 114.4(4) 2 . . . ? O1 Cd1 O1 S1 -158.9(7) 6_556 . . . ? O1 Cd1 O1 S1 21.1(7) 3 . . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 19.97 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 1.213 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.131 data_5 _database_code_depnum_ccdc_archive 'CCDC 225748' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H54 Cd Cl2 O14 S6' _chemical_formula_weight 942.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Rhombohedral _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 10.313(3) _cell_length_b 10.313(3) _cell_length_c 67.52(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6219(5) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 715 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 21.87 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 1.012 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.8388 _exptl_absorpt_correction_T_max 0.8882 _exptl_absorpt_process_details SADABS _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 7624 _diffrn_reflns_av_R_equivalents 0.0817 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -79 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 24.96 _reflns_number_total 1230 _reflns_number_gt 749 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0514P)^2^+87.0877P] 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 1230 _refine_ls_number_parameters 82 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1106 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1646 _refine_ls_wR_factor_gt 0.1399 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.053 _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 Cd1 Cd 0.0000 0.0000 0.0000 0.0576(5) Uani 1 6 d S . . O1 O 0.2060(7) 0.1248(6) 0.01982(7) 0.0748(17) Uani 1 1 d . . . S1 S 0.2408(3) 0.2682(3) 0.03056(3) 0.0739(7) Uani 1 1 d . . . C1 C 0.3550(12) 0.1684(13) 0.06096(13) 0.098(3) Uani 1 1 d . . . H1A H 0.3547 0.1539 0.0750 0.147 Uiso 1 1 calc R . . H1B H 0.4554 0.2357 0.0566 0.147 Uiso 1 1 calc R . . H1C H 0.3176 0.0738 0.0544 0.147 Uiso 1 1 calc R . . C2 C 0.2576(11) 0.2330(11) 0.05615(11) 0.077(3) Uani 1 1 d . . . H2A H 0.2956 0.3266 0.0633 0.092 Uiso 1 1 calc R . . H2B H 0.1580 0.1653 0.0612 0.092 Uiso 1 1 calc R . . C3 C 0.4299(11) 0.3898(9) 0.02458(7) 0.095(3) Uani 1 1 d D . . H3A H 0.4549 0.4833 0.0311 0.113 Uiso 1 1 calc R A 1 H3B H 0.4842 0.3501 0.0317 0.113 Uiso 1 1 calc R A 1 C4 C 0.507(4) 0.436(3) 0.0045(3) 0.086(14) Uani 0.31(3) 1 d PD . 1 H4A H 0.6119 0.4669 0.0060 0.103 Uiso 0.31(3) 1 calc PR . 1 H4B H 0.4622 0.3508 -0.0044 0.103 Uiso 0.31(3) 1 calc PR . 1 C4' C 0.4220(4) 0.4472(17) 0.00400(13) 0.076(6) Uani 0.69(3) 1 d PD . 2 H4'A H 0.3701 0.3630 -0.0050 0.091 Uiso 0.69(3) 1 calc PR . 2 H4'B H 0.3656 0.4992 0.0047 0.091 Uiso 0.69(3) 1 calc PR . 2 Cl1 Cl 0.3333 0.6667 0.05815(5) 0.0630(9) Uani 1 3 d S . . O2 O 0.3333 0.6667 0.0379(2) 0.175(7) Uani 1 3 d S . . O3 O 0.4566(9) 0.6559(10) 0.06371(15) 0.157(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0687(7) 0.0687(7) 0.0355(6) 0.000 0.000 0.0343(3) O1 0.089(4) 0.068(4) 0.074(3) -0.020(3) -0.026(3) 0.044(4) S1 0.0931(18) 0.0721(15) 0.0656(13) -0.0084(12) -0.0218(12) 0.0481(14) C1 0.106(8) 0.127(10) 0.074(5) 0.031(6) 0.002(5) 0.068(8) C2 0.087(7) 0.079(6) 0.055(5) -0.001(4) 0.005(5) 0.034(6) C3 0.134(10) 0.066(6) 0.054(5) 0.007(4) 0.002(6) 0.028(6) C4 0.09(3) 0.05(2) 0.10(2) 0.004(18) 0.02(2) 0.02(3) C4' 0.088(12) 0.085(13) 0.049(8) -0.005(7) -0.008(7) 0.038(11) Cl1 0.0640(14) 0.0640(14) 0.0611(19) 0.000 0.000 0.0320(7) O2 0.218(12) 0.218(12) 0.088(9) 0.000 0.000 0.109(6) O3 0.104(7) 0.138(7) 0.243(10) 0.003(7) -0.056(7) 0.071(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 Cd1 O1 2.286(5) . ? Cd1 O1 2.286(5) 3 ? Cd1 O1 2.286(5) 2 ? Cd1 O1 2.286(5) 19 ? Cd1 O1 2.286(5) 21 ? Cd1 O1 2.286(5) 20 ? O1 S1 1.521(6) . ? S1 C3 1.758(9) . ? S1 C2 1.792(8) . ? C1 C2 1.493(12) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.523(5) . ? C3 C4' 1.528(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C4 1.521(5) 19_665 ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4' C4' 1.521(5) 19_665 ? C4' H4'A 0.9700 . ? C4' H4'B 0.9700 . ? Cl1 O2 1.369(14) . ? Cl1 O3 1.382(8) 2_665 ? Cl1 O3 1.382(8) 3_565 ? Cl1 O3 1.382(8) . ? 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 Cd1 O1 89.2(2) . 3 ? O1 Cd1 O1 89.2(2) . 2 ? O1 Cd1 O1 89.2(2) 3 2 ? O1 Cd1 O1 180.0(2) . 19 ? O1 Cd1 O1 90.8(2) 3 19 ? O1 Cd1 O1 90.8(2) 2 19 ? O1 Cd1 O1 90.8(2) . 21 ? O1 Cd1 O1 180.0(4) 3 21 ? O1 Cd1 O1 90.8(2) 2 21 ? O1 Cd1 O1 89.2(2) 19 21 ? O1 Cd1 O1 90.8(2) . 20 ? O1 Cd1 O1 90.8(2) 3 20 ? O1 Cd1 O1 180.0(2) 2 20 ? O1 Cd1 O1 89.2(2) 19 20 ? O1 Cd1 O1 89.2(2) 21 20 ? S1 O1 Cd1 121.9(3) . . ? O1 S1 C3 102.8(4) . . ? O1 S1 C2 105.2(4) . . ? C3 S1 C2 100.4(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 S1 117.1(6) . . ? C1 C2 H2A 108.0 . . ? S1 C2 H2A 108.0 . . ? C1 C2 H2B 108.0 . . ? S1 C2 H2B 108.0 . . ? H2A C2 H2B 107.3 . . ? C4 C3 C4' 35.8(8) . . ? C4 C3 S1 130.3(17) . . ? C4' C3 S1 103.3(5) . . ? C4 C3 H3A 104.7 . . ? C4' C3 H3A 93.8 . . ? S1 C3 H3A 104.7 . . ? C4 C3 H3B 104.7 . . ? C4' C3 H3B 140.2 . . ? S1 C3 H3B 104.7 . . ? H3A C3 H3B 105.7 . . ? C4 C4 C3 111.5(5) 19_665 . ? C4 C4 H4A 109.3 19_665 . ? C3 C4 H4A 109.3 . . ? C4 C4 H4B 109.3 19_665 . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C4' C4' C3 111.0(5) 19_665 . ? C4' C4' H4'A 109.4 19_665 . ? C3 C4' H4'A 109.4 . . ? C4' C4' H4'B 109.4 19_665 . ? C3 C4' H4'B 109.4 . . ? H4'A C4' H4'B 108.0 . . ? O2 Cl1 O3 105.8(5) . 2_665 ? O2 Cl1 O3 105.8(5) . 3_565 ? O3 Cl1 O3 112.9(4) 2_665 3_565 ? O2 Cl1 O3 105.8(5) . . ? O3 Cl1 O3 112.9(4) 2_665 . ? O3 Cl1 O3 112.9(4) 3_565 . ? 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 Cd1 O1 S1 -120.5(3) 3 . . . ? O1 Cd1 O1 S1 -31.3(5) 2 . . . ? O1 Cd1 O1 S1 110.3(8) 19 . . . ? O1 Cd1 O1 S1 59.5(3) 21 . . . ? O1 Cd1 O1 S1 148.7(5) 20 . . . ? Cd1 O1 S1 C3 -130.4(4) . . . . ? Cd1 O1 S1 C2 124.9(4) . . . . ? O1 S1 C2 C1 48.8(9) . . . . ? C3 S1 C2 C1 -57.7(9) . . . . ? O1 S1 C3 C4 54.6(9) . . . . ? C2 S1 C3 C4 163.0(8) . . . . ? O1 S1 C3 C4' 81.5(9) . . . . ? C2 S1 C3 C4' -170.1(9) . . . . ? C4' C3 C4 C4 34.9(19) . . . 19_665 ? S1 C3 C4 C4 84(4) . . . 19_665 ? C4 C3 C4' C4' -34.7(19) . . . 19_665 ? S1 C3 C4' C4' -178.6(17) . . . 19_665 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.941 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.089