# 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 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Srinivasan Natarajan' _publ_contact_author_email SNATARAJAN@SSCU.IISC.ERNET.IN _publ_section_title ; Synthesis, Structure, Transformation Studies and Heterogeneous Catalytic Behavior of Inorganic-Organic Hybrid Cadmium Thiosulfate Compounds ; loop_ _publ_author_name 'Srinivasan Natarajan' 'Giridhar Madras' 'Avijit Kumar Paul' # Attachment 'CIF_Files.txt' data_Compound(1) _database_code_depnum_ccdc_archive 'CCDC 697711' _chemical_name_systematic ; ? ; _chemical_name_common 'Cadmium thiosulfate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H16 Cd N2 O7 S2' _chemical_formula_weight 452.75 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 P21/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 7.1760(13) _cell_length_b 10.5145(18) _cell_length_c 20.899(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.300(3) _cell_angle_gamma 90.00 _cell_volume 1556.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3160 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 26.37 _exptl_crystal_description 'Rod like' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.924 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 1.705 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7720 _exptl_absorpt_correction_T_max 0.9046 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12147 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3160 _reflns_number_gt 2855 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1999) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0379P)^2^+2.3594P] 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 (Two hydrogen atoms of O200 could not be located) ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3160 _refine_ls_number_parameters 223 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0823 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _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 Cd1 Cd 1.00956(4) 0.22394(2) 0.256995(11) 0.02859(10) Uani 1 1 d . . . N1 N 0.9949(4) 0.3274(3) 0.35423(13) 0.0333(7) Uani 1 1 d . . . N2 N 1.0373(5) 0.1292(3) 0.15846(13) 0.0339(7) Uani 1 1 d . . . O1 O 1.1316(4) 0.4077(3) 0.21671(14) 0.0452(7) Uani 1 1 d D . . O2 O 1.3302(4) 0.1987(3) 0.29919(17) 0.0528(8) Uani 1 1 d D . . O3 O 1.0228(4) 0.0196(2) 0.30576(15) 0.0486(7) Uani 1 1 d . . . O4 O 0.7034(5) 0.0207(4) 0.3194(3) 0.1051(18) Uani 1 1 d . . . O5 O 0.9295(9) -0.0757(5) 0.39916(17) 0.128(2) Uani 1 1 d . . . S1 S 0.84845(14) -0.22166(9) 0.28609(5) 0.0389(2) Uani 1 1 d . . . S2 S 0.87712(14) -0.05207(9) 0.33161(4) 0.0369(2) Uani 1 1 d . . . C1 C 0.9752(6) 0.4535(4) 0.35413(17) 0.0392(9) Uani 1 1 d . . . H1 H 0.9595 0.4959 0.3146 0.047 Uiso 1 1 calc R . . C2 C 0.9769(6) 0.5240(3) 0.40991(16) 0.0366(8) Uani 1 1 d . . . H2 H 0.9635 0.6119 0.4075 0.044 Uiso 1 1 calc R . . C3 C 0.9987(5) 0.4638(3) 0.46937(15) 0.0276(7) Uani 1 1 d . . . C4 C 1.0159(7) 0.3330(4) 0.46913(18) 0.0461(10) Uani 1 1 d . . . H4 H 1.0279 0.2877 0.5078 0.055 Uiso 1 1 calc R . . C5 C 1.0153(7) 0.2699(4) 0.41122(19) 0.0469(11) Uani 1 1 d . . . H5 H 1.0301 0.1820 0.4123 0.056 Uiso 1 1 calc R . . C6 C 1.0370(9) 0.2022(4) 0.1064(2) 0.0662(16) Uani 1 1 d . . . H6 H 1.0465 0.2897 0.1125 0.079 Uiso 1 1 calc R . . C7 C 1.0233(9) 0.1559(4) 0.04398(19) 0.0639(15) Uani 1 1 d . . . H7 H 1.0241 0.2114 0.0094 0.077 Uiso 1 1 calc R . . C8 C 1.0084(5) 0.0268(3) 0.03346(15) 0.0289(7) Uani 1 1 d . . . C9 C 1.0096(6) -0.0490(4) 0.08693(17) 0.0379(9) Uani 1 1 d . . . H9 H 1.0002 -0.1368 0.0822 0.045 Uiso 1 1 calc R . . C10 C 1.0248(6) 0.0052(3) 0.14817(16) 0.0367(8) Uani 1 1 d . . . H10 H 1.0262 -0.0484 0.1837 0.044 Uiso 1 1 calc R . . O100 O 1.4641(13) 0.1158(6) 0.4204(3) 0.120(2) Uani 1 1 d . . . O200 O 0.7690(9) 0.0119(6) 0.5058(3) 0.147(2) Uani 1 1 d . . . H1A H 1.253(3) 0.437(5) 0.212(2) 0.074(16) Uiso 1 1 d D . . H1B H 1.024(4) 0.459(4) 0.203(2) 0.064(15) Uiso 1 1 d D . . H2A H 1.423(8) 0.206(7) 0.272(3) 0.13(3) Uiso 1 1 d D . . H2B H 1.379(9) 0.162(6) 0.3400(17) 0.12(3) Uiso 1 1 d D . . H102 H 1.346(8) 0.050(6) 0.427(3) 0.070(18) Uiso 1 1 d . . . H101 H 1.555(11) 0.069(8) 0.429(4) 0.12(3) 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 Cd1 0.04319(17) 0.02437(15) 0.01922(14) -0.00602(9) 0.00814(10) -0.00043(10) N1 0.0462(18) 0.0304(15) 0.0232(14) -0.0072(12) 0.0056(12) 0.0025(13) N2 0.0520(19) 0.0300(15) 0.0204(14) -0.0071(11) 0.0075(13) 0.0026(13) O1 0.0509(18) 0.0351(15) 0.0510(17) 0.0056(12) 0.0123(14) -0.0090(13) O2 0.0432(17) 0.060(2) 0.056(2) 0.0133(16) 0.0106(15) 0.0028(14) O3 0.0589(18) 0.0304(14) 0.0611(18) -0.0012(13) 0.0239(15) -0.0089(13) O4 0.053(2) 0.060(2) 0.208(5) -0.061(3) 0.037(3) -0.0008(18) O5 0.263(7) 0.093(3) 0.0299(19) -0.010(2) 0.029(3) -0.068(4) S1 0.0381(5) 0.0280(5) 0.0517(6) -0.0063(4) 0.0109(4) -0.0038(4) S2 0.0480(6) 0.0343(5) 0.0316(5) -0.0074(4) 0.0158(4) -0.0118(4) C1 0.060(2) 0.037(2) 0.0199(17) -0.0041(14) 0.0050(16) 0.0104(18) C2 0.056(2) 0.0288(18) 0.0254(17) -0.0052(14) 0.0068(16) 0.0110(16) C3 0.0318(18) 0.0292(17) 0.0222(16) -0.0067(13) 0.0049(13) -0.0011(14) C4 0.087(3) 0.0273(19) 0.0241(18) -0.0022(15) 0.0090(19) 0.001(2) C5 0.085(3) 0.0267(19) 0.030(2) -0.0066(15) 0.011(2) 0.001(2) C6 0.147(5) 0.025(2) 0.029(2) -0.0054(16) 0.019(3) -0.001(2) C7 0.140(5) 0.030(2) 0.0240(19) -0.0034(16) 0.019(2) -0.001(3) C8 0.0363(19) 0.0313(18) 0.0193(16) -0.0059(13) 0.0048(13) 0.0035(14) C9 0.058(2) 0.0288(18) 0.0257(18) -0.0055(14) 0.0037(16) 0.0034(17) C10 0.058(2) 0.0324(19) 0.0194(16) -0.0017(14) 0.0047(15) 0.0054(17) O100 0.195(7) 0.084(4) 0.072(3) 0.000(3) -0.008(4) 0.038(5) O200 0.189(7) 0.135(5) 0.113(5) 0.024(4) 0.009(4) 0.003(5) _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 N1 2.322(3) . ? Cd1 N2 2.325(3) . ? Cd1 O1 2.334(3) . ? Cd1 O2 2.342(3) . ? Cd1 O3 2.374(3) . ? Cd1 S1 2.6439(11) 2_655 ? N1 C5 1.322(5) . ? N1 C1 1.333(5) . ? N2 C10 1.323(5) . ? N2 C6 1.330(5) . ? O1 H1A 0.946(10) . ? O1 H1B 0.945(10) . ? O2 H2A 0.948(10) . ? O2 H2B 0.947(10) . ? O3 S2 1.461(3) . ? O4 S2 1.450(4) . ? O5 S2 1.423(4) . ? S1 S2 2.0160(13) . ? S1 Cd1 2.6439(11) 2_645 ? C1 C2 1.380(5) . ? C1 H1 0.9300 . ? C2 C3 1.381(5) . ? C2 H2 0.9300 . ? C3 C4 1.381(5) . ? C3 C3 1.487(6) 3_766 ? C4 C5 1.379(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.381(5) . ? C6 H6 0.9300 . ? C7 C8 1.376(5) . ? C7 H7 0.9300 . ? C8 C9 1.371(5) . ? C8 C8 1.494(6) 3_755 ? C9 C10 1.389(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? O100 H102 1.12(6) . ? O100 H101 0.81(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 N1 Cd1 N2 176.60(11) . . ? N1 Cd1 O1 90.02(11) . . ? N2 Cd1 O1 86.80(11) . . ? N1 Cd1 O2 84.50(12) . . ? N2 Cd1 O2 93.75(12) . . ? O1 Cd1 O2 80.02(11) . . ? N1 Cd1 O3 93.03(10) . . ? N2 Cd1 O3 89.38(10) . . ? O1 Cd1 O3 155.92(11) . . ? O2 Cd1 O3 76.51(11) . . ? N1 Cd1 S1 91.02(8) . 2_655 ? N2 Cd1 S1 90.50(8) . 2_655 ? O1 Cd1 S1 95.66(8) . 2_655 ? O2 Cd1 S1 173.75(9) . 2_655 ? O3 Cd1 S1 108.15(8) . 2_655 ? C5 N1 C1 116.9(3) . . ? C5 N1 Cd1 124.1(2) . . ? C1 N1 Cd1 119.0(2) . . ? C10 N2 C6 116.4(3) . . ? C10 N2 Cd1 123.6(2) . . ? C6 N2 Cd1 119.2(2) . . ? Cd1 O1 H1A 135(3) . . ? Cd1 O1 H1B 104(3) . . ? H1A O1 H1B 120(4) . . ? Cd1 O2 H2A 120(5) . . ? Cd1 O2 H2B 125(4) . . ? H2A O2 H2B 113(6) . . ? S2 O3 Cd1 130.08(18) . . ? S2 S1 Cd1 111.81(5) . 2_645 ? O5 S2 O4 110.4(4) . . ? O5 S2 O3 111.5(3) . . ? O4 S2 O3 108.0(2) . . ? O5 S2 S1 107.7(2) . . ? O4 S2 S1 111.34(17) . . ? O3 S2 S1 107.81(12) . . ? N1 C1 C2 123.1(3) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 119.9(3) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 116.8(3) . . ? C2 C3 C3 121.6(4) . 3_766 ? C4 C3 C3 121.6(4) . 3_766 ? C5 C4 C3 119.6(4) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 C5 C4 123.7(4) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? N2 C6 C7 124.0(4) . . ? N2 C6 H6 118.0 . . ? C7 C6 H6 118.0 . . ? C8 C7 C6 119.4(4) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C9 C8 C7 116.9(3) . . ? C9 C8 C8 122.2(4) . 3_755 ? C7 C8 C8 120.9(4) . 3_755 ? C8 C9 C10 120.1(3) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? N2 C10 C9 123.2(3) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? H102 O100 H101 101(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.913 _refine_diff_density_min -0.999 _refine_diff_density_rms 0.112 #####END##### data_Compound(2) _database_code_depnum_ccdc_archive 'CCDC 697712' _chemical_name_systematic ; ? ; _chemical_name_common 'Cadmium thiosulfate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H12 Cd N3 O3 S2' _chemical_formula_weight 458.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.628(2) _cell_length_b 15.081(2) _cell_length_c 17.362(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.076(3) _cell_angle_gamma 90.00 _cell_volume 3160.8(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3729 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 28.08 _exptl_crystal_description 'Plate like' _exptl_crystal_colour 'Color less' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.928 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 1.665 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8252 _exptl_absorpt_correction_T_max 0.8646 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13654 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.08 _reflns_number_total 3729 _reflns_number_gt 3172 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1999) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0277P)^2^+3.3819P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3729 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0700 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.002 _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 0.5000 0.495876(18) 0.2500 0.02168(9) Uani 1 2 d S . . Cd2 Cd 0.5000 1.01410(2) 0.7500 0.02664(9) Uani 1 2 d S . . O1 O 0.1804(2) 1.00778(16) 0.74475(16) 0.0457(6) Uani 1 1 d . . . O2 O 0.1417(2) 1.03308(17) 0.60204(16) 0.0510(7) Uani 1 1 d . . . O3 O 0.29037(18) 0.93567(14) 0.67241(13) 0.0361(5) Uani 1 1 d . . . N1 N 0.5770(2) 0.39060(16) 0.35082(15) 0.0267(5) Uani 1 1 d . . . N2 N 0.5388(2) 0.61678(16) 0.34332(15) 0.0278(6) Uani 1 1 d . . . N3 N 0.5248(2) 0.92307(16) 0.64955(15) 0.0297(6) Uani 1 1 d . . . S1 S 0.33694(7) 1.11724(6) 0.69911(7) 0.0493(3) Uani 1 1 d . . . S2 S 0.22616(6) 1.01478(5) 0.67656(5) 0.02896(18) Uani 1 1 d . . . C1 C 0.5958(2) 0.40626(18) 0.42944(17) 0.0253(6) Uani 1 1 d . . . H1 H 0.5610 0.4547 0.4448 0.030 Uiso 1 1 calc R . . C2 C 0.6638(2) 0.35441(18) 0.48890(18) 0.0256(6) Uani 1 1 d . . . H2 H 0.6766 0.3697 0.5428 0.031 Uiso 1 1 calc R . . C3 C 0.7135(2) 0.27920(18) 0.46853(17) 0.0230(6) Uani 1 1 d . . . C4 C 0.6908(3) 0.26135(19) 0.38681(18) 0.0293(7) Uani 1 1 d . . . H4 H 0.7193 0.2106 0.3698 0.035 Uiso 1 1 calc R . . C5 C 0.6260(3) 0.3189(2) 0.33114(18) 0.0307(7) Uani 1 1 d . . . H5 H 0.6157 0.3074 0.2768 0.037 Uiso 1 1 calc R . . C6 C 0.4616(3) 0.6804(2) 0.33174(18) 0.0315(7) Uani 1 1 d . . . H6 H 0.4035 0.6798 0.2842 0.038 Uiso 1 1 calc R . . C7 C 0.4641(3) 0.7461(2) 0.3864(2) 0.0319(7) Uani 1 1 d . . . H7 H 0.4103 0.7903 0.3744 0.038 Uiso 1 1 calc R . . C8 C 0.5465(3) 0.74742(18) 0.45992(19) 0.0256(7) Uani 1 1 d . . . C9 C 0.6288(3) 0.68300(19) 0.47115(19) 0.0304(7) Uani 1 1 d . . . H9 H 0.6874 0.6816 0.5184 0.037 Uiso 1 1 calc R . . C10 C 0.6220(3) 0.62140(19) 0.41118(19) 0.0303(7) Uani 1 1 d . . . H10 H 0.6792 0.5805 0.4187 0.036 Uiso 1 1 calc R . . C11 C 0.4609(3) 0.9340(2) 0.57361(19) 0.0315(7) Uani 1 1 d . . . H11 H 0.4088 0.9794 0.5628 0.038 Uiso 1 1 calc R . . C12 C 0.4685(3) 0.88131(19) 0.51092(19) 0.0305(7) Uani 1 1 d . . . H12 H 0.4241 0.8930 0.4589 0.037 Uiso 1 1 calc R . . C13 C 0.5423(2) 0.81069(19) 0.52483(18) 0.0264(6) Uani 1 1 d . . . C14 C 0.6082(3) 0.7994(2) 0.60351(19) 0.0382(8) Uani 1 1 d . . . H14 H 0.6595 0.7534 0.6163 0.046 Uiso 1 1 calc R . . C15 C 0.5974(3) 0.8565(2) 0.6627(2) 0.0393(8) Uani 1 1 d . . . H15 H 0.6435 0.8482 0.7148 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02436(17) 0.02018(14) 0.01839(16) 0.000 0.00299(12) 0.000 Cd2 0.02745(18) 0.02807(16) 0.02579(18) 0.000 0.00996(13) 0.000 O1 0.0360(15) 0.0625(17) 0.0448(16) -0.0129(12) 0.0215(12) -0.0064(11) O2 0.0326(14) 0.0573(16) 0.0513(17) 0.0089(13) -0.0061(12) 0.0026(12) O3 0.0417(13) 0.0345(12) 0.0317(13) -0.0041(10) 0.0100(11) 0.0068(10) N1 0.0278(14) 0.0282(12) 0.0233(13) 0.0061(10) 0.0063(11) 0.0056(10) N2 0.0310(14) 0.0275(13) 0.0248(14) -0.0016(10) 0.0081(11) -0.0012(10) N3 0.0294(15) 0.0314(13) 0.0288(15) -0.0047(11) 0.0093(12) -0.0014(11) S1 0.0288(5) 0.0308(4) 0.0812(8) 0.0069(4) 0.0052(5) -0.0016(3) S2 0.0221(4) 0.0315(4) 0.0323(4) -0.0015(3) 0.0066(3) 0.0015(3) C1 0.0254(16) 0.0248(14) 0.0263(16) 0.0030(12) 0.0084(13) 0.0047(11) C2 0.0304(17) 0.0245(14) 0.0211(15) 0.0023(12) 0.0060(13) 0.0019(12) C3 0.0215(15) 0.0218(13) 0.0234(16) 0.0047(12) 0.0033(12) 0.0010(11) C4 0.0336(18) 0.0277(15) 0.0236(17) -0.0006(12) 0.0036(14) 0.0080(12) C5 0.0359(18) 0.0319(16) 0.0214(16) 0.0026(13) 0.0038(13) 0.0065(13) C6 0.0326(18) 0.0378(17) 0.0225(16) -0.0023(13) 0.0055(13) 0.0032(13) C7 0.0317(18) 0.0354(17) 0.0276(18) -0.0021(13) 0.0073(14) 0.0046(13) C8 0.0265(16) 0.0255(14) 0.0260(17) -0.0012(11) 0.0099(13) -0.0043(11) C9 0.0309(17) 0.0296(15) 0.0283(17) -0.0035(13) 0.0048(14) -0.0008(13) C10 0.0301(17) 0.0274(15) 0.0329(18) -0.0014(13) 0.0083(14) 0.0023(12) C11 0.0309(18) 0.0305(16) 0.0325(18) -0.0010(13) 0.0086(14) 0.0036(13) C12 0.0346(18) 0.0307(16) 0.0239(16) -0.0002(12) 0.0050(13) 0.0003(13) C13 0.0284(16) 0.0279(15) 0.0240(16) -0.0035(12) 0.0095(13) -0.0056(12) C14 0.040(2) 0.0406(18) 0.0305(19) -0.0068(15) 0.0043(15) 0.0112(15) C15 0.044(2) 0.0452(19) 0.0242(17) -0.0055(14) 0.0025(15) 0.0077(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.307(2) 8_565 ? Cd1 O1 2.307(2) 7_566 ? Cd1 N1 2.352(2) 2_655 ? Cd1 N1 2.352(2) . ? Cd1 N2 2.392(2) . ? Cd1 N2 2.392(2) 2_655 ? Cd2 N3 2.312(2) . ? Cd2 N3 2.312(2) 2_656 ? Cd2 S1 2.5243(10) 2_656 ? Cd2 S1 2.5243(9) . ? O1 S2 1.466(3) . ? O1 Cd1 2.307(2) 7_566 ? O2 S2 1.442(2) . ? O3 S2 1.456(2) . ? N1 C1 1.336(4) . ? N1 C5 1.339(4) . ? N2 C10 1.330(4) . ? N2 C6 1.340(4) . ? N3 C15 1.333(4) . ? N3 C11 1.339(4) . ? S1 S2 2.0436(12) . ? C1 C2 1.377(4) . ? C1 H1 0.9300 . ? C2 C3 1.391(4) . ? C2 H2 0.9300 . ? C3 C4 1.389(4) . ? C3 C3 1.493(5) 7_656 ? C4 C5 1.376(4) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.367(4) . ? C6 H6 0.9300 . ? C7 C8 1.390(4) . ? C7 H7 0.9300 . ? C8 C9 1.394(4) . ? C8 C13 1.490(4) . ? C9 C10 1.379(4) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.374(4) . ? C11 H11 0.9300 . ? C12 C13 1.389(4) . ? C12 H12 0.9300 . ? C13 C14 1.385(4) . ? C14 C15 1.378(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O1 177.26(12) 8_565 7_566 ? O1 Cd1 N1 98.74(9) 8_565 2_655 ? O1 Cd1 N1 79.39(8) 7_566 2_655 ? O1 Cd1 N1 79.39(8) 8_565 . ? O1 Cd1 N1 98.74(9) 7_566 . ? N1 Cd1 N1 95.08(12) 2_655 . ? O1 Cd1 N2 92.10(9) 8_565 . ? O1 Cd1 N2 89.99(9) 7_566 . ? N1 Cd1 N2 167.50(8) 2_655 . ? N1 Cd1 N2 93.02(9) . . ? O1 Cd1 N2 89.99(9) 8_565 2_655 ? O1 Cd1 N2 92.10(9) 7_566 2_655 ? N1 Cd1 N2 93.02(9) 2_655 2_655 ? N1 Cd1 N2 167.50(8) . 2_655 ? N2 Cd1 N2 80.69(12) . 2_655 ? N3 Cd2 N3 107.15(13) . 2_656 ? N3 Cd2 S1 110.65(7) . 2_656 ? N3 Cd2 S1 112.28(7) 2_656 2_656 ? N3 Cd2 S1 112.28(7) . . ? N3 Cd2 S1 110.65(7) 2_656 . ? S1 Cd2 S1 103.92(4) 2_656 . ? S2 O1 Cd1 131.44(16) . 7_566 ? C1 N1 C5 116.6(2) . . ? C1 N1 Cd1 123.47(19) . . ? C5 N1 Cd1 118.45(19) . . ? C10 N2 C6 116.5(3) . . ? C10 N2 Cd1 126.26(19) . . ? C6 N2 Cd1 116.7(2) . . ? C15 N3 C11 116.5(3) . . ? C15 N3 Cd2 123.8(2) . . ? C11 N3 Cd2 119.6(2) . . ? S2 S1 Cd2 92.48(4) . . ? O2 S2 O3 112.87(15) . . ? O2 S2 O1 112.03(16) . . ? O3 S2 O1 109.77(14) . . ? O2 S2 S1 108.17(12) . . ? O3 S2 S1 105.61(10) . . ? O1 S2 S1 108.05(11) . . ? N1 C1 C2 123.4(3) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 120.1(3) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 116.4(3) . . ? C4 C3 C3 122.1(3) . 7_656 ? C2 C3 C3 121.5(3) . 7_656 ? C5 C4 C3 119.8(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N1 C5 C4 123.7(3) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? N2 C6 C7 123.2(3) . . ? N2 C6 H6 118.4 . . ? C7 C6 H6 118.4 . . ? C6 C7 C8 120.4(3) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C9 116.4(3) . . ? C7 C8 C13 121.3(3) . . ? C9 C8 C13 122.1(3) . . ? C10 C9 C8 119.0(3) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? N2 C10 C9 124.2(3) . . ? N2 C10 H10 117.9 . . ? C9 C10 H10 117.9 . . ? N3 C11 C12 123.2(3) . . ? N3 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C11 C12 C13 120.4(3) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 116.3(3) . . ? C14 C13 C8 121.5(3) . . ? C12 C13 C8 122.1(3) . . ? C15 C14 C13 119.7(3) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? N3 C15 C14 123.8(3) . . ? N3 C15 H15 118.1 . . ? C14 C15 H15 118.1 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 28.08 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.631 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.093 #####END##### data_Compound(3) _database_code_depnum_ccdc_archive 'CCDC 697713' _chemical_name_systematic ; ? ; _chemical_name_common 'Cadmium thiosulfate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H20 Cd2 N5 O6 S4' _chemical_formula_weight 839.50 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 P21/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 11.0343(17) _cell_length_b 15.894(2) _cell_length_c 15.823(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.969(3) _cell_angle_gamma 90.00 _cell_volume 2773.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6541 _cell_measurement_theta_min 1.82 _cell_measurement_theta_max 28.08 _exptl_crystal_description Rectangular _exptl_crystal_colour 'Light yellow' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.011 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1652 _exptl_absorpt_coefficient_mu 1.887 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7781 _exptl_absorpt_correction_T_max 0.8637 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23968 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 28.08 _reflns_number_total 6541 _reflns_number_gt 5120 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1999) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+2.1270P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6541 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0646 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 Cd1 Cd 0.32384(2) 0.242892(14) 0.264343(15) 0.02961(7) Uani 1 1 d . . . Cd2 Cd 0.78152(2) 0.248022(14) 0.272605(15) 0.03088(7) Uani 1 1 d . . . N1 N 0.3359(3) 0.15263(17) 0.15293(17) 0.0325(7) Uani 1 1 d . . . N2 N 0.2827(3) 0.35675(17) 0.17188(17) 0.0328(7) Uani 1 1 d . . . S1 S 0.52821(9) 0.30082(5) 0.31550(6) 0.0377(2) Uani 1 1 d . . . S2 S 0.55748(8) 0.19332(5) 0.38771(5) 0.0308(2) Uani 1 1 d . . . S4 S 0.04496(8) 0.16348(5) 0.28754(5) 0.0316(2) Uani 1 1 d . . . S3 S 0.15917(10) 0.23449(8) 0.36303(7) 0.0545(3) Uani 1 1 d . . . N3 N 0.7154(3) 0.14780(16) 0.17693(17) 0.0320(7) Uani 1 1 d . . . N4 N 0.8669(2) 0.34986(16) 0.35961(16) 0.0269(6) Uani 1 1 d . . . O1 O 0.6864(2) 0.17642(18) 0.37933(17) 0.0511(7) Uani 1 1 d . . . O2 O 0.9309(2) 0.16016(16) 0.33210(16) 0.0456(7) Uani 1 1 d . . . N5 N 0.7812(3) 0.34731(15) 0.16157(16) 0.0279(6) Uani 1 1 d . . . O3 O 0.5283(3) 0.21022(18) 0.47369(15) 0.0528(8) Uani 1 1 d . . . O4 O 0.4817(2) 0.12943(15) 0.34821(16) 0.0479(7) Uani 1 1 d . . . O5 O 0.0973(3) 0.08229(19) 0.2788(2) 0.0779(11) Uani 1 1 d . . . O6 O 0.0243(3) 0.2061(2) 0.20818(18) 0.0710(10) Uani 1 1 d . . . C15 C 0.6619(3) 0.1669(2) 0.1021(2) 0.0323(8) Uani 1 1 d . . . H15 H 0.6374 0.2222 0.0926 0.039 Uiso 1 1 calc R . . C16 C 0.6686(3) -0.03633(19) -0.01916(19) 0.0254(7) Uani 1 1 d . . . C6 C 0.1581(3) 0.4574(2) 0.0977(2) 0.0357(8) Uani 1 1 d . . . H3 H 0.0843 0.4855 0.0933 0.043 Uiso 1 1 calc R . . C8 C 0.2345(3) 0.53588(19) -0.0289(2) 0.0270(7) Uani 1 1 d . . . C24 C 0.8535(3) 0.3426(2) 0.0956(2) 0.0316(8) Uani 1 1 d . . . H25 H 0.9108 0.2997 0.0950 0.038 Uiso 1 1 calc R . . C19 C 0.8933(3) 0.3309(2) 0.4402(2) 0.0332(8) Uani 1 1 d . . . H10 H 0.8748 0.2772 0.4592 0.040 Uiso 1 1 calc R . . C14 C 0.6415(3) 0.10919(19) 0.0388(2) 0.0300(8) Uani 1 1 d . . . H16 H 0.6034 0.1256 -0.0118 0.036 Uiso 1 1 calc R . . C21 C 0.9739(3) 0.46803(19) 0.47068(19) 0.0248(7) Uani 1 1 d . . . C5 C 0.2491(3) 0.47533(19) 0.0422(2) 0.0285(7) Uani 1 1 d . . . C7 C 0.1781(3) 0.3975(2) 0.1596(2) 0.0378(9) Uani 1 1 d . . . H2 H 0.1148 0.3848 0.1948 0.045 Uiso 1 1 calc R . . C12 C 0.7271(3) 0.0054(2) 0.1300(2) 0.0387(9) Uani 1 1 d . . . H17 H 0.7485 -0.0500 0.1423 0.046 Uiso 1 1 calc R . . C11 C 0.7440(4) 0.0672(2) 0.1902(2) 0.0410(9) Uani 1 1 d . . . H14 H 0.7771 0.0520 0.2428 0.049 Uiso 1 1 calc R . . C13 C 0.6777(3) 0.02617(19) 0.0504(2) 0.0254(7) Uani 1 1 d . . . C18 C 0.6191(3) -0.0169(2) -0.0985(2) 0.0351(8) Uani 1 1 d . . . H21 H 0.5864 0.0363 -0.1085 0.042 Uiso 1 1 calc R . . C20 C 0.9467(3) 0.3867(2) 0.4968(2) 0.0330(8) Uani 1 1 d . . . H11 H 0.9644 0.3701 0.5522 0.040 Uiso 1 1 calc R . . C25 C 0.7041(3) 0.4120(2) 0.1619(2) 0.0330(8) Uani 1 1 d . . . H24 H 0.6540 0.4173 0.2076 0.040 Uiso 1 1 calc R . . C9 C 0.3059(3) 0.5292(2) -0.0992(2) 0.0340(8) Uani 1 1 d . . . H8 H 0.3602 0.4848 -0.1035 0.041 Uiso 1 1 calc R . . C10 C 0.1523(3) 0.6023(2) -0.0284(2) 0.0310(8) Uani 1 1 d . . . H7 H 0.1018 0.6094 0.0168 0.037 Uiso 1 1 calc R . . C1 C 0.2887(4) 0.1716(2) 0.0771(2) 0.0547(12) Uani 1 1 d . . . H23 H 0.2556 0.2249 0.0690 0.066 Uiso 1 1 calc R . . C4 C 0.3573(4) 0.4330(2) 0.0551(2) 0.0458(10) Uani 1 1 d . . . H5 H 0.4216 0.4433 0.0201 0.055 Uiso 1 1 calc R . . C3 C 0.3699(4) 0.3757(2) 0.1196(2) 0.0461(10) Uani 1 1 d . . . H1 H 0.4441 0.3485 0.1270 0.055 Uiso 1 1 calc R . . C2 C 0.3820(3) 0.0757(2) 0.1626(2) 0.0345(8) Uani 1 1 d . . . H22 H 0.4164 0.0609 0.2150 0.041 Uiso 1 1 calc R . . C23 C 0.8964(3) 0.4266(2) 0.3341(2) 0.0365(9) Uani 1 1 d . . . H9 H 0.8807 0.4405 0.2777 0.044 Uiso 1 1 calc R . . C17 C 0.7141(4) -0.1167(2) -0.0100(2) 0.0517(12) Uani 1 1 d . . . H19 H 0.7469 -0.1340 0.0421 0.062 Uiso 1 1 calc R . . C22 C 0.9489(3) 0.4866(2) 0.3862(2) 0.0356(9) Uani 1 1 d . . . H13 H 0.9675 0.5394 0.3649 0.043 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 0.03518(15) 0.02819(13) 0.02532(13) -0.00208(10) -0.00094(10) -0.00103(10) Cd2 0.04710(17) 0.02306(12) 0.02194(13) -0.00050(10) -0.00670(11) -0.00875(11) N1 0.0419(18) 0.0306(15) 0.0247(15) -0.0050(12) -0.0030(13) 0.0024(13) N2 0.0366(18) 0.0324(15) 0.0293(16) 0.0037(12) -0.0005(13) 0.0021(13) S1 0.0404(6) 0.0323(5) 0.0399(5) 0.0070(4) -0.0044(4) -0.0054(4) S2 0.0327(5) 0.0341(4) 0.0253(5) 0.0019(3) -0.0031(4) -0.0078(4) S4 0.0315(5) 0.0340(4) 0.0293(5) -0.0057(4) -0.0013(4) 0.0020(4) S3 0.0378(6) 0.0855(8) 0.0407(6) -0.0302(6) 0.0082(5) -0.0179(5) N3 0.0413(18) 0.0287(14) 0.0254(15) -0.0028(12) -0.0062(13) -0.0030(13) N4 0.0316(16) 0.0254(13) 0.0233(15) -0.0017(11) -0.0030(12) -0.0044(11) O1 0.0335(15) 0.0674(19) 0.0522(18) 0.0244(14) -0.0006(13) 0.0047(13) O2 0.0376(15) 0.0488(15) 0.0511(17) -0.0079(13) 0.0117(13) -0.0125(12) N5 0.0395(17) 0.0232(13) 0.0205(14) 0.0009(11) -0.0046(12) -0.0033(12) O3 0.074(2) 0.0590(18) 0.0259(15) -0.0007(12) 0.0076(13) -0.0145(15) O4 0.0607(18) 0.0410(14) 0.0411(16) 0.0001(12) -0.0096(13) -0.0218(13) O5 0.076(2) 0.062(2) 0.094(3) -0.0403(18) -0.0230(19) 0.0348(17) O6 0.083(2) 0.087(2) 0.0415(18) 0.0214(17) -0.0168(16) -0.0238(19) C15 0.036(2) 0.0232(15) 0.036(2) -0.0048(14) -0.0087(16) 0.0010(14) C16 0.0265(18) 0.0256(16) 0.0240(17) -0.0021(13) -0.0006(14) -0.0049(13) C6 0.033(2) 0.0366(19) 0.037(2) 0.0078(16) 0.0015(17) 0.0054(15) C8 0.0318(19) 0.0261(16) 0.0228(17) -0.0002(13) -0.0025(14) -0.0029(13) C24 0.039(2) 0.0284(17) 0.0277(19) -0.0028(14) -0.0007(16) 0.0065(15) C19 0.050(2) 0.0234(16) 0.0266(19) -0.0002(14) 0.0007(16) -0.0060(15) C14 0.032(2) 0.0282(16) 0.0287(19) 0.0010(14) -0.0068(15) 0.0011(14) C21 0.0242(18) 0.0251(16) 0.0249(18) -0.0037(13) -0.0002(14) -0.0053(13) C5 0.036(2) 0.0245(15) 0.0247(18) 0.0007(13) -0.0021(15) 0.0006(14) C7 0.038(2) 0.042(2) 0.034(2) 0.0056(16) 0.0069(17) -0.0015(17) C12 0.059(3) 0.0242(17) 0.032(2) -0.0010(14) -0.0107(18) -0.0012(16) C11 0.066(3) 0.0274(17) 0.028(2) 0.0019(15) -0.0148(18) 0.0007(17) C13 0.0246(18) 0.0267(15) 0.0249(17) -0.0019(13) 0.0006(14) -0.0067(13) C18 0.051(2) 0.0238(16) 0.0304(19) 0.0000(14) -0.0057(17) 0.0041(15) C20 0.051(2) 0.0266(16) 0.0215(18) -0.0004(13) -0.0052(16) -0.0046(15) C25 0.040(2) 0.0345(18) 0.0248(18) -0.0002(14) 0.0030(15) -0.0003(16) C9 0.038(2) 0.0322(18) 0.032(2) 0.0037(15) 0.0036(16) 0.0062(15) C10 0.036(2) 0.0333(18) 0.0237(18) -0.0014(14) 0.0021(15) 0.0042(15) C1 0.093(3) 0.0312(19) 0.038(2) -0.0059(17) -0.023(2) 0.021(2) C4 0.035(2) 0.053(2) 0.050(3) 0.022(2) 0.0107(19) 0.0082(18) C3 0.036(2) 0.053(2) 0.049(3) 0.0198(19) 0.0039(19) 0.0138(18) C2 0.046(2) 0.0331(18) 0.0238(18) 0.0003(14) -0.0083(16) 0.0024(16) C23 0.052(2) 0.0324(18) 0.0244(18) 0.0022(14) -0.0129(16) -0.0138(16) C17 0.092(3) 0.0328(19) 0.029(2) -0.0030(16) -0.021(2) 0.016(2) C22 0.052(2) 0.0258(16) 0.0282(19) 0.0022(14) -0.0088(17) -0.0142(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.280(3) . ? Cd1 N2 2.361(3) . ? Cd1 S3 2.4398(11) . ? Cd1 S1 2.5422(10) . ? Cd2 N3 2.299(3) . ? Cd2 N4 2.305(2) . ? Cd2 O1 2.318(3) . ? Cd2 O2 2.334(3) . ? Cd2 N5 2.361(3) . ? Cd2 S1 3.0179(11) . ? N1 C1 1.326(4) . ? N1 C2 1.331(4) . ? N2 C3 1.325(4) . ? N2 C7 1.333(4) . ? S1 S2 2.0745(12) . ? S2 O3 1.434(3) . ? S2 O4 1.444(2) . ? S2 O1 1.458(3) . ? S4 O5 1.422(3) . ? S4 O6 1.438(3) . ? S4 O2 1.464(3) 1_455 ? S4 S3 2.0459(13) . ? N3 C11 1.334(4) . ? N3 C15 1.339(4) . ? N4 C23 1.329(4) . ? N4 C19 1.332(4) . ? O2 S4 1.464(3) 1_655 ? N5 C25 1.334(4) . ? N5 C24 1.338(4) . ? C15 C14 1.372(4) . ? C15 H15 0.9300 . ? C16 C17 1.379(5) . ? C16 C18 1.386(4) . ? C16 C13 1.483(4) . ? C6 C7 1.377(5) . ? C6 C5 1.386(5) . ? C6 H3 0.9300 . ? C8 C9 1.389(5) . ? C8 C10 1.392(4) . ? C8 C5 1.485(4) . ? C24 C10 1.376(4) 3_665 ? C24 H25 0.9300 . ? C19 C20 1.378(4) . ? C19 H10 0.9300 . ? C14 C13 1.389(4) . ? C14 H16 0.9300 . ? C21 C22 1.388(4) . ? C21 C20 1.394(4) . ? C21 C21 1.479(6) 3_766 ? C5 C4 1.379(5) . ? C7 H2 0.9300 . ? C12 C11 1.376(5) . ? C12 C13 1.395(4) . ? C12 H17 0.9300 . ? C11 H14 0.9300 . ? C18 C2 1.380(4) 3_655 ? C18 H21 0.9300 . ? C20 H11 0.9300 . ? C25 C9 1.365(4) 3_665 ? C25 H24 0.9300 . ? C9 C25 1.365(4) 3_665 ? C9 H8 0.9300 . ? C10 C24 1.376(4) 3_665 ? C10 H7 0.9300 . ? C1 C17 1.374(5) 3_655 ? C1 H23 0.9300 . ? C4 C3 1.371(5) . ? C4 H5 0.9300 . ? C3 H1 0.9300 . ? C2 C18 1.380(4) 3_655 ? C2 H22 0.9300 . ? C23 C22 1.375(4) . ? C23 H9 0.9300 . ? C17 C1 1.374(5) 3_655 ? C17 H19 0.9300 . ? C22 H13 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N2 91.04(10) . . ? N1 Cd1 S3 121.66(8) . . ? N2 Cd1 S3 107.88(8) . . ? N1 Cd1 S1 113.54(8) . . ? N2 Cd1 S1 93.97(7) . . ? S3 Cd1 S1 119.21(3) . . ? N3 Cd2 N4 173.59(10) . . ? N3 Cd2 O1 89.89(10) . . ? N4 Cd2 O1 95.48(10) . . ? N3 Cd2 O2 93.15(9) . . ? N4 Cd2 O2 84.88(9) . . ? O1 Cd2 O2 75.15(9) . . ? N3 Cd2 N5 88.90(9) . . ? N4 Cd2 N5 88.01(9) . . ? O1 Cd2 N5 151.78(9) . . ? O2 Cd2 N5 133.07(9) . . ? N3 Cd2 S1 93.74(8) . . ? N4 Cd2 S1 91.89(7) . . ? O1 Cd2 S1 61.73(7) . . ? O2 Cd2 S1 136.26(6) . . ? N5 Cd2 S1 90.21(7) . . ? C1 N1 C2 116.7(3) . . ? C1 N1 Cd1 121.7(2) . . ? C2 N1 Cd1 121.4(2) . . ? C3 N2 C7 116.2(3) . . ? C3 N2 Cd1 115.7(2) . . ? C7 N2 Cd1 127.6(2) . . ? S2 S1 Cd1 89.81(4) . . ? S2 S1 Cd2 76.52(4) . . ? Cd1 S1 Cd2 130.24(4) . . ? O3 S2 O4 113.38(16) . . ? O3 S2 O1 111.87(17) . . ? O4 S2 O1 112.52(17) . . ? O3 S2 S1 109.42(13) . . ? O4 S2 S1 105.30(11) . . ? O1 S2 S1 103.63(11) . . ? O5 S4 O6 113.2(2) . . ? O5 S4 O2 111.89(19) . 1_455 ? O6 S4 O2 108.94(18) . 1_455 ? O5 S4 S3 108.25(14) . . ? O6 S4 S3 109.04(14) . . ? O2 S4 S3 105.13(11) 1_455 . ? S4 S3 Cd1 96.54(5) . . ? C11 N3 C15 116.9(3) . . ? C11 N3 Cd2 119.6(2) . . ? C15 N3 Cd2 123.0(2) . . ? C23 N4 C19 116.7(3) . . ? C23 N4 Cd2 124.3(2) . . ? C19 N4 Cd2 119.0(2) . . ? S2 O1 Cd2 116.33(14) . . ? S4 O2 Cd2 113.02(15) 1_655 . ? C25 N5 C24 116.3(3) . . ? C25 N5 Cd2 119.8(2) . . ? C24 N5 Cd2 123.9(2) . . ? N3 C15 C14 123.4(3) . . ? N3 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? C17 C16 C18 115.6(3) . . ? C17 C16 C13 121.8(3) . . ? C18 C16 C13 122.4(3) . . ? C7 C6 C5 119.4(3) . . ? C7 C6 H3 120.3 . . ? C5 C6 H3 120.3 . . ? C9 C8 C10 116.7(3) . . ? C9 C8 C5 120.5(3) . . ? C10 C8 C5 122.8(3) . . ? N5 C24 C10 123.6(3) . 3_665 ? N5 C24 H25 118.2 . . ? C10 C24 H25 118.2 3_665 . ? N4 C19 C20 123.5(3) . . ? N4 C19 H10 118.2 . . ? C20 C19 H10 118.2 . . ? C15 C14 C13 120.0(3) . . ? C15 C14 H16 120.0 . . ? C13 C14 H16 120.0 . . ? C22 C21 C20 116.5(3) . . ? C22 C21 C21 121.2(4) . 3_766 ? C20 C21 C21 122.3(4) . 3_766 ? C4 C5 C6 116.6(3) . . ? C4 C5 C8 119.9(3) . . ? C6 C5 C8 123.5(3) . . ? N2 C7 C6 123.8(3) . . ? N2 C7 H2 118.1 . . ? C6 C7 H2 118.1 . . ? C11 C12 C13 119.7(3) . . ? C11 C12 H17 120.2 . . ? C13 C12 H17 120.2 . . ? N3 C11 C12 123.4(3) . . ? N3 C11 H14 118.3 . . ? C12 C11 H14 118.3 . . ? C14 C13 C12 116.4(3) . . ? C14 C13 C16 121.8(3) . . ? C12 C13 C16 121.7(3) . . ? C2 C18 C16 120.5(3) 3_655 . ? C2 C18 H21 119.7 3_655 . ? C16 C18 H21 119.7 . . ? C19 C20 C21 119.7(3) . . ? C19 C20 H11 120.2 . . ? C21 C20 H11 120.2 . . ? N5 C25 C9 124.1(3) . 3_665 ? N5 C25 H24 117.9 . . ? C9 C25 H24 117.9 3_665 . ? C25 C9 C8 119.7(3) 3_665 . ? C25 C9 H8 120.1 3_665 . ? C8 C9 H8 120.1 . . ? C24 C10 C8 119.5(3) 3_665 . ? C24 C10 H7 120.3 3_665 . ? C8 C10 H7 120.3 . . ? N1 C1 C17 123.6(3) . 3_655 ? N1 C1 H23 118.2 . . ? C17 C1 H23 118.2 3_655 . ? C3 C4 C5 119.9(4) . . ? C3 C4 H5 120.0 . . ? C5 C4 H5 120.0 . . ? N2 C3 C4 123.9(4) . . ? N2 C3 H1 118.0 . . ? C4 C3 H1 118.0 . . ? N1 C2 C18 123.0(3) . 3_655 ? N1 C2 H22 118.5 . . ? C18 C2 H22 118.5 3_655 . ? N4 C23 C22 123.9(3) . . ? N4 C23 H9 118.1 . . ? C22 C23 H9 118.1 . . ? C1 C17 C16 120.6(3) 3_655 . ? C1 C17 H19 119.7 3_655 . ? C16 C17 H19 119.7 . . ? C23 C22 C21 119.7(3) . . ? C23 C22 H13 120.2 . . ? C21 C22 H13 120.2 . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 28.08 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.534 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.087 #####END##### data_Compound(1) _database_code_depnum_ccdc_archive 'CCDC 727266' _chemical_name_systematic ; ? ; _chemical_name_common '1D-Cadmium thiosulfate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H28 Cd N2 Na2 O16 S4' _chemical_formula_weight 718.85 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 6.9673(2) _cell_length_b 14.1333(4) _cell_length_c 14.3657(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.0350(10) _cell_angle_gamma 90.00 _cell_volume 1372.37(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7626 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 30.67 _exptl_crystal_description 'Plate like' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 1.198 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8696 _exptl_absorpt_correction_T_max 0.9537 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14333 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 30.67 _reflns_number_total 7626 _reflns_number_gt 6881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1999) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0501P)^2^+6.0399P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0043(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(1) _refine_ls_number_reflns 7626 _refine_ls_number_parameters 311 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1687 _refine_ls_wR_factor_gt 0.1632 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.061 _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 Cd1 Cd 0.66254(5) 0.59483(5) 0.00000(3) 0.02943(12) Uani 1 1 d D . . Na1 Na 0.7461(7) 0.8431(3) 0.4935(3) 0.0451(10) Uani 1 1 d . . . Na2 Na 0.2514(7) 0.8435(3) 0.5055(2) 0.0419(9) Uani 1 1 d . . . N1 N 0.4232(14) 0.7027(7) 0.0014(7) 0.052(2) Uani 1 1 d D A . N2 N 0.4184(9) 0.4845(5) -0.0004(6) 0.0371(19) Uani 1 1 d D A . O1 O 0.6349(7) 0.5924(9) -0.3353(3) 0.0522(13) Uani 1 1 d . A . O6 O 0.9698(8) 0.5876(8) 0.3354(3) 0.0485(14) Uani 1 1 d . A . O7 O 0.9963(13) 0.7272(6) 0.4934(6) 0.0480(19) Uani 1 1 d . . . O8 O 1.0042(14) 0.9584(6) 0.5142(6) 0.0462(18) Uani 1 1 d . . . O9 O 0.5023(12) 0.7258(6) 0.5096(6) 0.0488(19) Uani 1 1 d . . . O10 O 0.4895(14) 0.9575(6) 0.4889(5) 0.0467(19) Uani 1 1 d . . . O11 O 0.825(3) 0.8534(14) 0.6704(7) 0.115(6) Uani 1 1 d . . . O12 O 0.6145(17) 0.8427(8) 0.3182(5) 0.076(3) Uani 1 1 d . . . O13 O 0.2891(16) 0.8454(10) 0.6773(7) 0.083(3) Uani 1 1 d . . . O14 O 0.163(2) 0.8550(13) 0.3360(7) 0.091(4) Uani 1 1 d . . . C1 C 0.3608(13) 0.7669(8) -0.0625(6) 0.051(2) Uani 1 1 d . . . H1 H 0.4340 0.7782 -0.1075 0.061 Uiso 1 1 calc R A . C2 C 0.3304(16) 0.7000(8) 0.0820(8) 0.059(2) Uani 1 1 d . . . H2 H 0.3811 0.6618 0.1349 0.071 Uiso 1 1 calc R A . C3 C 0.4222(12) 0.4258(8) 0.0623(6) 0.050(2) Uani 1 1 d . . . H3 H 0.5396 0.4177 0.1089 0.060 Uiso 1 1 calc R A . C4 C 0.2627(13) 0.3713(7) 0.0680(6) 0.050(2) Uani 1 1 d . A . H4 H 0.2753 0.3308 0.1201 0.060 Uiso 1 1 calc R . . C5 C 0.0878(13) 0.3735(6) 0.0016(5) 0.0284(16) Uani 1 1 d . . . C6 C 0.0865(13) 0.4339(8) -0.0767(7) 0.059(3) Uani 1 1 d . A . H6 H -0.0257 0.4363 -0.1272 0.070 Uiso 1 1 calc R . . C7 C 0.2471(15) 0.4894(9) -0.0802(7) 0.060(3) Uani 1 1 d . . . H7 H 0.2451 0.5288 -0.1323 0.072 Uiso 1 1 calc R A . C8 C -0.0884(14) 0.3154(7) 0.0018(6) 0.0330(18) Uani 1 1 d . . . C9 C 0.1634(12) 0.7562(8) 0.0779(7) 0.054(2) Uani 1 1 d . . . H9 H 0.1011 0.7546 0.1283 0.064 Uiso 1 1 calc R . . C10 C 0.1922(14) 0.8199(7) -0.0682(6) 0.0488(19) Uani 1 1 d . . . H10 H 0.1494 0.8601 -0.1203 0.059 Uiso 1 1 calc R . . S3 S 0.5687(2) 0.5942(2) -0.24673(9) 0.0368(3) Uani 1 1 d D . . S4 S 0.8174(2) 0.5939(2) 0.24668(9) 0.0386(3) Uani 1 1 d D . . S1A S 0.7752(4) 0.5380(2) -0.14124(19) 0.0349(6) Uiso 0.70 1 d PD A 1 S1B S 0.8026(7) 0.6335(4) -0.1397(3) 0.0225(9) Uiso 0.30 1 d PD A 1 O2A O 0.586(4) 0.4896(7) -0.2383(19) 0.056(6) Uiso 0.30 1 d PD A 1 O2B O 0.5395(17) 0.6968(6) -0.2243(8) 0.055(2) Uiso 0.70 1 d PD A 1 O3A O 0.3794(17) 0.6269(13) -0.2414(13) 0.031(4) Uiso 0.30 1 d PD A 1 O3B O 0.3813(13) 0.5491(8) -0.2516(9) 0.059(3) Uiso 0.70 1 d PD A 1 S2A S 0.9295(5) 0.5386(2) 0.1414(2) 0.0418(7) Uiso 0.70 1 d PD A 2 S2B S 0.9193(8) 0.6361(4) 0.1399(3) 0.0234(10) Uiso 0.30 1 d PD A 2 O5A O 0.834(3) 0.4898(7) 0.2363(15) 0.043(4) Uiso 0.30 1 d PD A 2 O5B O 0.7635(17) 0.6963(6) 0.2249(8) 0.057(2) Uiso 0.70 1 d PD A 2 O4A O 0.6151(15) 0.6216(12) 0.2417(13) 0.034(4) Uiso 0.30 1 d PD A 2 O4B O 0.6392(12) 0.5471(7) 0.2509(7) 0.048(2) Uiso 0.70 1 d PD A 2 O100 O 0.0156(8) 0.5910(9) 0.6348(4) 0.0545(13) Uani 1 1 d . B 2 O200 O 0.3825(9) 0.5939(9) 0.3656(4) 0.0607(17) Uani 1 1 d . C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02680(17) 0.0315(2) 0.02990(18) -0.0011(2) 0.00666(12) 0.0014(3) Na1 0.038(2) 0.037(2) 0.057(2) 0.002(2) 0.0044(18) -0.0044(16) Na2 0.043(2) 0.040(2) 0.046(2) -0.0009(19) 0.0182(17) 0.0077(17) N1 0.059(6) 0.043(5) 0.065(6) -0.002(4) 0.037(5) -0.007(4) N2 0.014(3) 0.021(3) 0.071(5) -0.001(3) 0.000(3) -0.010(2) O1 0.049(2) 0.074(4) 0.033(2) 0.016(4) 0.0097(18) 0.007(5) O6 0.049(2) 0.062(4) 0.031(2) -0.009(3) 0.0039(18) -0.016(4) O7 0.049(5) 0.039(4) 0.054(4) 0.003(3) 0.008(4) -0.007(3) O8 0.059(5) 0.032(4) 0.051(4) -0.006(3) 0.019(4) 0.006(3) O9 0.045(4) 0.038(4) 0.063(5) -0.006(3) 0.012(4) 0.006(3) O10 0.066(5) 0.027(3) 0.045(4) 0.012(3) 0.007(4) -0.005(3) O11 0.179(16) 0.105(10) 0.050(5) -0.024(6) 0.009(7) -0.015(10) O12 0.111(8) 0.071(5) 0.040(3) -0.006(4) 0.005(4) -0.003(6) O13 0.082(6) 0.091(6) 0.060(5) 0.013(5) -0.016(4) 0.005(6) O14 0.101(9) 0.109(9) 0.059(5) 0.003(6) 0.013(6) -0.006(7) C1 0.045(4) 0.069(6) 0.043(4) 0.013(4) 0.020(3) -0.002(4) C2 0.066(6) 0.063(6) 0.059(5) 0.017(5) 0.033(5) 0.009(5) C3 0.031(3) 0.068(6) 0.046(4) -0.001(4) 0.002(3) -0.016(4) C4 0.049(4) 0.051(5) 0.047(4) 0.011(3) 0.006(3) -0.022(4) C5 0.028(4) 0.015(3) 0.036(4) 0.002(2) -0.003(3) -0.003(3) C6 0.038(4) 0.075(7) 0.056(5) 0.018(5) -0.001(4) -0.028(4) C7 0.049(5) 0.081(7) 0.047(4) 0.012(4) 0.003(4) -0.030(5) C8 0.033(5) 0.030(4) 0.041(5) 0.000(3) 0.019(4) -0.001(3) C9 0.037(4) 0.076(7) 0.055(5) 0.021(4) 0.024(3) 0.009(4) C10 0.050(4) 0.055(5) 0.047(4) 0.013(4) 0.022(4) 0.001(4) S3 0.0339(6) 0.0483(8) 0.0260(5) -0.0050(11) 0.0029(4) -0.0121(12) S4 0.0395(7) 0.0513(9) 0.0254(5) 0.0003(11) 0.0088(5) 0.0185(12) O100 0.043(2) 0.064(4) 0.053(3) 0.002(5) 0.004(2) 0.002(5) O200 0.054(3) 0.083(5) 0.047(3) 0.008(5) 0.016(2) -0.035(5) _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 N1 2.263(7) . ? Cd1 N2 2.307(5) . ? Cd1 S2B 2.416(5) . ? Cd1 S1A 2.480(3) . ? Cd1 S1B 2.496(5) . ? Cd1 S2A 2.527(3) . ? Na1 O8 2.391(10) . ? Na1 O7 2.393(10) . ? Na1 O10 2.399(10) . ? Na1 O9 2.425(10) . ? Na1 O12 2.462(8) . ? Na1 O11 2.471(11) . ? Na1 Na2 3.483(4) 1_655 ? Na1 Na2 3.492(4) . ? Na2 O10 2.366(9) . ? Na2 O14 2.368(11) . ? Na2 O8 2.392(9) 1_455 ? Na2 O7 2.396(10) 1_455 ? Na2 O9 2.403(9) . ? Na2 O13 2.417(10) . ? Na2 Na1 3.483(4) 1_455 ? N1 C1 1.289(13) . ? N1 C2 1.456(12) . ? N2 C3 1.220(13) . ? N2 C7 1.442(12) . ? O1 S3 1.456(5) . ? O6 S4 1.450(5) . ? O7 Na2 2.396(10) 1_655 ? O8 Na2 2.392(9) 1_655 ? C1 C10 1.379(13) . ? C1 H1 0.9300 . ? C2 C9 1.398(14) . ? C2 H2 0.9300 . ? C3 C4 1.371(11) . ? C3 H3 0.9300 . ? C4 C5 1.353(11) . ? C4 H4 0.9300 . ? C5 C6 1.410(12) . ? C5 C8 1.477(7) . ? C6 C7 1.378(11) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C10 1.330(11) 2_545 ? C8 C9 1.413(13) 2_545 ? C9 C8 1.413(13) 2 ? C9 H9 0.9300 . ? C10 C8 1.330(11) 2 ? C10 H10 0.9300 . ? S3 O3A 1.417(9) . ? S3 O3B 1.439(8) . ? S3 O2A 1.485(10) . ? S3 O2B 1.510(8) . ? S3 S1A 1.984(3) . ? S3 S1B 2.028(5) . ? S4 O4B 1.421(7) . ? S4 O4A 1.448(9) . ? S4 O5A 1.486(9) . ? S4 O5B 1.508(8) . ? S4 S2B 1.934(5) . ? S4 S2A 2.021(4) . ? S1A S1B 1.362(6) . ? S1A O2A 1.80(3) . ? S1B O2B 2.135(12) . ? O2A O3B 1.63(3) . ? O2B O3A 1.47(2) . ? O3A O3B 1.111(18) . ? S2A S2B 1.380(6) . ? S2A O5A 1.79(2) . ? S2B O5B 2.008(12) . ? O5A O4B 1.64(2) . ? O5B O4A 1.538(19) . ? O4A O4B 1.068(19) . ? 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 N1 Cd1 N2 84.9(2) . . ? N1 Cd1 S2B 103.2(3) . . ? N2 Cd1 S2B 124.2(2) . . ? N1 Cd1 S1A 127.3(3) . . ? N2 Cd1 S1A 99.1(2) . . ? S2B Cd1 S1A 116.20(15) . . ? N1 Cd1 S1B 107.0(3) . . ? N2 Cd1 S1B 125.3(2) . . ? S2B Cd1 S1B 105.13(16) . . ? S1A Cd1 S1B 31.78(14) . . ? N1 Cd1 S2A 127.2(3) . . ? N2 Cd1 S2A 100.8(2) . . ? S2B Cd1 S2A 32.33(14) . . ? S1A Cd1 S2A 103.80(10) . . ? S1B Cd1 S2A 111.10(13) . . ? O8 Na1 O7 86.6(3) . . ? O8 Na1 O10 94.4(3) . . ? O7 Na1 O10 178.2(3) . . ? O8 Na1 O9 167.8(3) . . ? O7 Na1 O9 93.4(3) . . ? O10 Na1 O9 85.9(3) . . ? O8 Na1 O12 102.2(4) . . ? O7 Na1 O12 95.1(4) . . ? O10 Na1 O12 83.3(4) . . ? O9 Na1 O12 90.0(4) . . ? O8 Na1 O11 81.9(5) . . ? O7 Na1 O11 93.5(5) . . ? O10 Na1 O11 88.1(5) . . ? O9 Na1 O11 85.9(5) . . ? O12 Na1 O11 170.7(6) . . ? O8 Na1 Na2 43.3(2) . 1_655 ? O7 Na1 Na2 43.4(2) . 1_655 ? O10 Na1 Na2 137.5(2) . 1_655 ? O9 Na1 Na2 136.0(2) . 1_655 ? O12 Na1 Na2 99.9(3) . 1_655 ? O11 Na1 Na2 88.8(5) . 1_655 ? O8 Na1 Na2 135.6(2) . . ? O7 Na1 Na2 136.8(2) . . ? O10 Na1 Na2 42.5(2) . . ? O9 Na1 Na2 43.4(2) . . ? O12 Na1 Na2 85.6(3) . . ? O11 Na1 Na2 85.7(5) . . ? Na2 Na1 Na2 174.50(13) 1_655 . ? O10 Na2 O14 82.1(4) . . ? O10 Na2 O8 94.3(3) . 1_455 ? O14 Na2 O8 89.8(5) . 1_455 ? O10 Na2 O7 170.3(3) . 1_455 ? O14 Na2 O7 88.2(5) . 1_455 ? O8 Na2 O7 86.5(4) 1_455 1_455 ? O10 Na2 O9 87.1(4) . . ? O14 Na2 O9 94.5(5) . . ? O8 Na2 O9 175.6(3) 1_455 . ? O7 Na2 O9 92.8(3) 1_455 . ? O10 Na2 O13 101.0(4) . . ? O14 Na2 O13 170.3(5) . . ? O8 Na2 O13 80.8(4) 1_455 . ? O7 Na2 O13 88.7(4) 1_455 . ? O9 Na2 O13 94.8(4) . . ? O10 Na2 Na1 136.2(3) . 1_455 ? O14 Na2 Na1 86.7(4) . 1_455 ? O8 Na2 Na1 43.3(2) 1_455 1_455 ? O7 Na2 Na1 43.3(2) 1_455 1_455 ? O9 Na2 Na1 136.1(3) . 1_455 ? O13 Na2 Na1 84.8(3) . 1_455 ? O10 Na2 Na1 43.2(2) . . ? O14 Na2 Na1 87.8(4) . . ? O8 Na2 Na1 137.3(3) 1_455 . ? O7 Na2 Na1 135.9(3) 1_455 . ? O9 Na2 Na1 43.9(2) . . ? O13 Na2 Na1 100.7(3) . . ? Na1 Na2 Na1 174.50(13) 1_455 . ? C1 N1 C2 116.5(8) . . ? C1 N1 Cd1 126.2(7) . . ? C2 N1 Cd1 117.4(7) . . ? C3 N2 C7 119.0(6) . . ? C3 N2 Cd1 125.0(6) . . ? C7 N2 Cd1 115.9(6) . . ? Na1 O7 Na2 93.3(3) . 1_655 ? Na1 O8 Na2 93.5(3) . 1_655 ? Na2 O9 Na1 92.7(3) . . ? Na2 O10 Na1 94.3(3) . . ? N1 C1 C10 124.1(8) . . ? N1 C1 H1 117.9 . . ? C10 C1 H1 117.9 . . ? C9 C2 N1 118.5(9) . . ? C9 C2 H2 120.7 . . ? N1 C2 H2 120.7 . . ? N2 C3 C4 123.6(8) . . ? N2 C3 H3 118.2 . . ? C4 C3 H3 118.2 . . ? C5 C4 C3 123.4(8) . . ? C5 C4 H4 118.3 . . ? C3 C4 H4 118.3 . . ? C4 C5 C6 114.0(8) . . ? C4 C5 C8 126.4(6) . . ? C6 C5 C8 119.6(6) . . ? C7 C6 C5 121.7(8) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C6 C7 N2 117.8(8) . . ? C6 C7 H7 121.1 . . ? N2 C7 H7 121.1 . . ? C10 C8 C9 116.8(9) 2_545 2_545 ? C10 C8 C5 124.9(7) 2_545 . ? C9 C8 C5 118.1(6) 2_545 . ? C2 C9 C8 120.7(8) . 2 ? C2 C9 H9 119.7 . . ? C8 C9 H9 119.7 2 . ? C8 C10 C1 122.3(8) 2 . ? C8 C10 H10 118.8 2 . ? C1 C10 H10 118.8 . . ? O3A S3 O3B 45.8(8) . . ? O3A S3 O1 123.3(8) . . ? O3B S3 O1 115.2(6) . . ? O3A S3 O2A 112.2(13) . . ? O3B S3 O2A 67.5(11) . . ? O1 S3 O2A 91.0(12) . . ? O3A S3 O2B 60.0(9) . . ? O3B S3 O2B 105.6(7) . . ? O1 S3 O2B 106.9(7) . . ? O2A S3 O2B 161.9(11) . . ? O3A S3 S1A 127.0(8) . . ? O3B S3 S1A 109.9(5) . . ? O1 S3 S1A 109.6(3) . . ? O2A S3 S1A 60.7(10) . . ? O2B S3 S1A 109.3(4) . . ? O3A S3 S1B 117.2(8) . . ? O3B S3 S1B 135.3(5) . . ? O1 S3 S1B 107.5(3) . . ? O2A S3 S1B 100.1(10) . . ? O2B S3 S1B 72.5(5) . . ? S1A S3 S1B 39.67(18) . . ? O4B S4 O4A 43.7(8) . . ? O4B S4 O6 113.3(5) . . ? O4A S4 O6 123.8(8) . . ? O4B S4 O5A 68.5(10) . . ? O4A S4 O5A 111.1(11) . . ? O6 S4 O5A 88.2(9) . . ? O4B S4 O5B 106.2(6) . . ? O4A S4 O5B 62.6(8) . . ? O6 S4 O5B 109.5(6) . . ? O5A S4 O5B 161.9(9) . . ? O4B S4 S2B 132.1(4) . . ? O4A S4 S2B 114.7(7) . . ? O6 S4 S2B 112.6(3) . . ? O5A S4 S2B 100.0(8) . . ? O5B S4 S2B 70.1(5) . . ? O4B S4 S2A 110.6(5) . . ? O4A S4 S2A 128.0(7) . . ? O6 S4 S2A 107.5(3) . . ? O5A S4 S2A 59.3(8) . . ? O5B S4 S2A 109.7(4) . . ? S2B S4 S2A 40.77(17) . . ? S1B S1A O2A 117.5(5) . . ? S1B S1A S3 71.9(3) . . ? O2A S1A S3 45.9(4) . . ? S1B S1A Cd1 74.8(3) . . ? O2A S1A Cd1 116.0(9) . . ? S3 S1A Cd1 100.42(12) . . ? S1A S1B S3 68.4(3) . . ? S1A S1B O2B 107.9(4) . . ? S3 S1B O2B 42.4(2) . . ? S1A S1B Cd1 73.5(3) . . ? S3 S1B Cd1 98.65(19) . . ? O2B S1B Cd1 95.8(4) . . ? S3 O2A O3B 54.9(7) . . ? S3 O2A S1A 73.5(8) . . ? O3B O2A S1A 110.5(11) . . ? O3A O2B S3 56.8(5) . . ? O3A O2B S1B 109.1(8) . . ? S3 O2B S1B 65.0(4) . . ? O3B O3A S3 68.2(7) . . ? O3B O3A O2B 131.0(10) . . ? S3 O3A O2B 63.2(6) . . ? O3A O3B S3 66.1(7) . . ? O3A O3B O2A 122.3(11) . . ? S3 O3B O2A 57.6(7) . . ? S2B S2A O5A 111.6(5) . . ? S2B S2A S4 66.2(3) . . ? O5A S2A S4 45.4(3) . . ? S2B S2A Cd1 69.4(3) . . ? O5A S2A Cd1 113.3(7) . . ? S4 S2A Cd1 97.89(14) . . ? S2A S2B S4 73.0(3) . . ? S2A S2B O5B 116.5(5) . . ? S4 S2B O5B 44.9(3) . . ? S2A S2B Cd1 78.3(3) . . ? S4 S2B Cd1 104.2(2) . . ? O5B S2B Cd1 102.0(4) . . ? S4 O5A O4B 53.9(6) . . ? S4 O5A S2A 75.4(7) . . ? O4B O5A S2A 112.3(9) . . ? S4 O5B O4A 56.8(5) . . ? S4 O5B S2B 64.9(4) . . ? O4A O5B S2B 106.8(8) . . ? O4B O4A S4 66.8(7) . . ? O4B O4A O5B 127.1(10) . . ? S4 O4A O5B 60.6(6) . . ? O4A O4B S4 69.5(7) . . ? O4A O4B O5A 125.6(11) . . ? S4 O4B O5A 57.6(6) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 30.67 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 1.662 _refine_diff_density_min -1.604 _refine_diff_density_rms 0.155 #####END##### data_Compound(2) _database_code_depnum_ccdc_archive 'CCDC 727267' _chemical_name_systematic ; ? ; _chemical_name_common '1D-Cadmium thiosulfate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H68 Cd2 N12 O20 S8' _chemical_formula_weight 1758.42 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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 13.420(3) _cell_length_b 17.361(4) _cell_length_c 15.840(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.228(3) _cell_angle_gamma 90.00 _cell_volume 3560.8(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8352 _cell_measurement_theta_min 1.96 _cell_measurement_theta_max 28.07 _exptl_crystal_description 'Block like' _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 0.911 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8985 _exptl_absorpt_correction_T_max 0.9225 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37720 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.07 _reflns_number_total 8352 _reflns_number_gt 5371 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction Saint _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1999) and CAMERON (Watkin et al.,1993)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0661P)^2^+15.5599P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8352 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1060 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.1814 _refine_ls_wR_factor_gt 0.1585 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 Cd1 Cd 0.7500 0.72100(3) 0.2500 0.03254(16) Uani 1 2 d S . . Cd2 Cd 0.2500 0.22024(3) 0.2500 0.03365(16) Uani 1 2 d S . . S1 S 0.65816(14) 0.76471(11) 0.35834(10) 0.0582(5) Uani 1 1 d . . . S2 S 0.34938(15) 0.26632(11) 0.14720(11) 0.0596(5) Uani 1 1 d . . . S3 S 0.55243(15) 0.82366(13) 0.26584(11) 0.0647(6) Uani 1 1 d . . . S4 S 0.4690(3) 0.2993(2) 0.24836(15) 0.1175(13) Uani 1 1 d . . . N1 N 0.6556(4) 0.6284(3) 0.1523(3) 0.0412(11) Uani 1 1 d . . . N2 N 0.1556(4) 0.1290(3) 0.1531(3) 0.0379(10) Uani 1 1 d . . . O1 O 0.5615(5) 0.7956(4) 0.1826(3) 0.0826(17) Uani 1 1 d . . . O6 O 0.4250(5) 0.3064(4) 0.3235(3) 0.0891(19) Uani 1 1 d . . . N5 N 0.3802(4) 0.7403(3) 0.9592(5) 0.0605(15) Uani 1 1 d . . . N4 N 0.5026(4) 0.8648(3) 0.9520(4) 0.0570(14) Uani 1 1 d . . . H4B H 0.4615 0.8266 0.9512 0.068 Uiso 1 1 calc R . . C3 C 0.5331(4) 0.5263(3) 0.0321(3) 0.0328(11) Uani 1 1 d . . . C2 C 0.5771(5) 0.5917(3) 0.0060(4) 0.0459(14) Uani 1 1 d . . . H2 H 0.5657 0.6027 -0.0532 0.055 Uiso 1 1 calc R . . C13 C 0.7033(4) 1.0539(3) 0.9602(4) 0.0430(13) Uani 1 1 d . . . C25 C 0.2558(4) 0.6125(3) 0.9663(4) 0.0427(13) Uani 1 1 d . . . C16 C 0.6333(4) 0.9868(3) 0.9562(4) 0.0425(13) Uani 1 1 d . . . C9C C 0.0534(5) 0.0152(4) 0.1217(4) 0.0499(16) Uani 1 1 d . . . H9 H 0.0267 -0.0277 0.1434 0.060 Uiso 1 1 calc R . . C7 C 0.0767(5) 0.0915(3) 0.0058(4) 0.0434(14) Uani 1 1 d . . . H7 H 0.0661 0.1021 -0.0535 0.052 Uiso 1 1 calc R . . C8 C 0.0328(4) 0.0273(3) 0.0324(3) 0.0334(11) Uani 1 1 d . . . C4 C 0.5524(6) 0.5145(4) 0.1208(4) 0.0600(19) Uani 1 1 d . . . H4 H 0.5254 0.4717 0.1422 0.072 Uiso 1 1 calc R . . O3 O 0.4547(4) 0.8114(6) 0.2817(5) 0.124(3) Uani 1 1 d . . . C6 C 0.1362(5) 0.1398(4) 0.0673(4) 0.0476(15) Uani 1 1 d . . . H6 H 0.1647 0.1829 0.0477 0.057 Uiso 1 1 calc R . . N3 N 0.8345(5) 1.1786(3) 0.9674(5) 0.0652(16) Uani 1 1 d . . . O5 O 0.5182(6) 0.3615(4) 0.2268(4) 0.102(2) Uani 1 1 d . . . C17 C 0.5399(5) 0.9811(4) 0.8921(4) 0.0514(15) Uani 1 1 d . . . H17 H 0.5202 1.0192 0.8498 0.062 Uiso 1 1 calc R . . N6 N 0.0752(6) 0.4136(3) 0.9728(5) 0.0681(17) Uani 1 1 d . . . C27 C 0.2153(6) 0.4939(4) 1.0392(5) 0.0621(19) Uani 1 1 d . . . H27 H 0.2716 0.5038 1.0865 0.074 Uiso 1 1 calc R . . O2 O 0.5800(7) 0.9070(3) 0.2766(4) 0.117(3) Uani 1 1 d . . . C20 C 0.6592(5) 0.9287(3) 1.0190(4) 0.0470(14) Uani 1 1 d . . . H20 H 0.7209 0.9308 1.0627 0.056 Uiso 1 1 calc R . . C26 C 0.1916(5) 0.5436(3) 0.9687(4) 0.0436(13) Uani 1 1 d . . . C10 C 0.1134(5) 0.0668(4) 0.1777(4) 0.0531(17) Uani 1 1 d . . . H10 H 0.1255 0.0577 0.2374 0.064 Uiso 1 1 calc R . . C15 C 0.8306(5) 1.1410(4) 1.0403(5) 0.0599(18) Uani 1 1 d . . . H15 H 0.8724 1.1578 1.0936 0.072 Uiso 1 1 calc R . . C19 C 0.5923(5) 0.8689(4) 1.0149(5) 0.0554(17) Uani 1 1 d . . . H19 H 0.6089 0.8299 1.0565 0.066 Uiso 1 1 calc R . . C1 C 0.6371(5) 0.6400(3) 0.0671(4) 0.0447(14) Uani 1 1 d . . . H1 H 0.6660 0.6830 0.0477 0.054 Uiso 1 1 calc R . . C30 C 0.1071(5) 0.5265(4) 0.9005(5) 0.0573(17) Uani 1 1 d . . . H30 H 0.0886 0.5586 0.8519 0.069 Uiso 1 1 calc R . . C22 C 0.3136(5) 0.6485(4) 1.0414(5) 0.0542(16) Uani 1 1 d . . . H22 H 0.3110 0.6303 1.0960 0.065 Uiso 1 1 calc R . . C5 C 0.6127(6) 0.5673(4) 0.1780(4) 0.063(2) Uani 1 1 d . . . H5 H 0.6234 0.5591 0.2378 0.075 Uiso 1 1 calc R . . C12 C 0.7071(5) 1.0934(4) 0.8859(5) 0.0558(16) Uani 1 1 d . . . H12 H 0.6648 1.0786 0.8319 0.067 Uiso 1 1 calc R . . C23 C 0.2622(6) 0.6445(4) 0.8876(5) 0.0593(18) Uani 1 1 d . . . H23 H 0.2242 0.6235 0.8349 0.071 Uiso 1 1 calc R . . C29 C 0.0506(6) 0.4616(4) 0.9051(5) 0.0659(19) Uani 1 1 d . . . H29 H -0.0069 0.4507 0.8592 0.079 Uiso 1 1 calc R . . C11 C 0.7737(6) 1.1551(4) 0.8912(5) 0.067(2) Uani 1 1 d . . . H11 H 0.7761 1.1808 0.8403 0.080 Uiso 1 1 calc R . . C24 C 0.3244(6) 0.7068(4) 0.8878(5) 0.067(2) Uani 1 1 d . . . H24 H 0.3276 0.7268 0.8341 0.080 Uiso 1 1 calc R . . C28 C 0.1551(8) 0.4295(5) 1.0393(6) 0.079(2) Uani 1 1 d . . . H28 H 0.1711 0.3966 1.0873 0.095 Uiso 1 1 calc R . . C21 C 0.3745(5) 0.7106(4) 1.0357(5) 0.0615(19) Uani 1 1 d . . . H21 H 0.4134 0.7330 1.0871 0.074 Uiso 1 1 calc R . . C18 C 0.4774(5) 0.9184(4) 0.8921(5) 0.0593(17) Uani 1 1 d . . . H18 H 0.4159 0.9140 0.8485 0.071 Uiso 1 1 calc R . . C14 C 0.7676(5) 1.0789(4) 1.0393(5) 0.0534(16) Uani 1 1 d . . . H14 H 0.7678 1.0536 1.0911 0.064 Uiso 1 1 calc R . . O4 O 0.5541(7) 0.2311(6) 0.2641(8) 0.181(5) Uani 1 1 d . . . H4A H 0.5718 0.2237 0.2190 0.271 Uiso 1 1 calc R . . O100 O -0.0355(5) 0.3013(3) 1.0085(4) 0.0918(19) Uani 1 1 d . . . O300 O 0.7500 0.9840(5) 0.2500 0.121(4) Uani 1 2 d S . . O200 O 0.2500 0.8583(8) 0.7500 0.175(6) Uani 1 2 d S . . O400 O 0.8585(10) 0.3432(6) 0.7768(7) 0.193(5) Uani 1 1 d . . . O500 O 0.3562(11) 0.4570(16) 1.2382(7) 0.46(2) 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 0.0417(3) 0.0278(3) 0.0274(3) 0.000 0.0078(2) 0.000 Cd2 0.0407(3) 0.0306(3) 0.0291(3) 0.000 0.0083(2) 0.000 S1 0.0623(10) 0.0783(12) 0.0355(8) 0.0064(8) 0.0154(7) 0.0315(9) S2 0.0663(11) 0.0752(12) 0.0390(8) -0.0022(8) 0.0169(8) -0.0249(9) S3 0.0658(11) 0.0916(15) 0.0386(8) 0.0108(9) 0.0171(8) 0.0435(11) S4 0.131(2) 0.172(3) 0.0509(12) -0.0109(15) 0.0256(14) -0.102(2) N1 0.047(3) 0.040(3) 0.036(3) -0.005(2) 0.009(2) -0.011(2) N2 0.047(3) 0.035(2) 0.031(2) -0.0036(19) 0.008(2) -0.009(2) O1 0.092(4) 0.115(5) 0.037(3) -0.005(3) 0.011(3) 0.022(4) O6 0.115(5) 0.108(5) 0.046(3) -0.011(3) 0.023(3) -0.034(4) N5 0.048(3) 0.049(3) 0.088(5) 0.003(3) 0.024(3) -0.005(3) N4 0.055(3) 0.040(3) 0.086(4) -0.001(3) 0.035(3) -0.010(3) C3 0.039(3) 0.026(3) 0.034(3) -0.003(2) 0.010(2) 0.001(2) C2 0.063(4) 0.042(3) 0.032(3) 0.002(2) 0.012(3) -0.015(3) C13 0.038(3) 0.036(3) 0.056(4) 0.005(3) 0.015(3) 0.003(2) C25 0.038(3) 0.038(3) 0.054(4) 0.004(3) 0.016(3) 0.008(2) C16 0.040(3) 0.043(3) 0.049(3) 0.000(3) 0.021(3) 0.003(3) C9C 0.067(4) 0.043(3) 0.034(3) 0.009(3) 0.002(3) -0.027(3) C7 0.060(4) 0.040(3) 0.029(3) 0.001(2) 0.009(3) -0.018(3) C8 0.034(3) 0.038(3) 0.027(3) -0.002(2) 0.006(2) -0.009(2) C4 0.081(5) 0.063(4) 0.033(3) 0.000(3) 0.010(3) -0.033(4) O3 0.051(3) 0.222(9) 0.102(5) 0.046(5) 0.027(3) 0.047(5) C6 0.059(4) 0.046(3) 0.035(3) 0.000(3) 0.009(3) -0.021(3) N3 0.051(3) 0.046(3) 0.098(5) 0.002(3) 0.019(3) -0.010(3) O5 0.122(5) 0.097(5) 0.075(4) 0.008(3) 0.006(4) -0.059(4) C17 0.048(4) 0.049(4) 0.060(4) 0.012(3) 0.018(3) 0.005(3) N6 0.083(5) 0.042(3) 0.090(5) 0.000(3) 0.042(4) -0.008(3) C27 0.057(4) 0.058(4) 0.073(5) 0.023(4) 0.019(4) 0.004(3) O2 0.208(8) 0.046(3) 0.105(5) 0.004(3) 0.053(5) 0.064(4) C20 0.049(3) 0.038(3) 0.053(4) 0.003(3) 0.012(3) 0.002(3) C26 0.044(3) 0.037(3) 0.054(4) 0.000(3) 0.022(3) 0.001(3) C10 0.076(5) 0.053(4) 0.026(3) -0.001(3) 0.006(3) -0.025(3) C15 0.043(4) 0.055(4) 0.076(5) -0.004(4) 0.007(3) 0.000(3) C19 0.064(4) 0.041(3) 0.065(4) 0.010(3) 0.025(4) -0.001(3) C1 0.067(4) 0.031(3) 0.033(3) 0.001(2) 0.009(3) -0.015(3) C30 0.055(4) 0.054(4) 0.060(4) 0.006(3) 0.010(3) -0.010(3) C22 0.048(4) 0.058(4) 0.057(4) 0.001(3) 0.013(3) -0.003(3) C5 0.086(5) 0.069(5) 0.029(3) 0.002(3) 0.008(3) -0.039(4) C12 0.050(4) 0.055(4) 0.061(4) 0.007(3) 0.013(3) -0.003(3) C23 0.077(5) 0.044(4) 0.055(4) 0.006(3) 0.015(4) -0.014(3) C29 0.063(5) 0.055(4) 0.078(5) -0.006(4) 0.015(4) -0.012(4) C11 0.065(5) 0.060(5) 0.076(5) 0.019(4) 0.021(4) -0.007(4) C24 0.073(5) 0.060(4) 0.069(5) 0.008(4) 0.023(4) -0.012(4) C28 0.094(6) 0.069(5) 0.084(6) 0.024(5) 0.040(5) 0.003(5) C21 0.046(4) 0.061(4) 0.077(5) -0.014(4) 0.015(3) -0.009(3) C18 0.045(4) 0.063(4) 0.069(5) 0.004(4) 0.012(3) -0.007(3) C14 0.046(3) 0.052(4) 0.060(4) 0.000(3) 0.009(3) -0.004(3) O4 0.099(6) 0.222(12) 0.216(11) 0.060(9) 0.033(7) 0.073(7) O100 0.103(5) 0.072(4) 0.096(4) 0.010(3) 0.019(4) -0.036(3) O300 0.141(9) 0.064(6) 0.127(8) 0.000 -0.021(7) 0.000 O200 0.207(14) 0.115(10) 0.154(12) 0.000 -0.039(11) 0.000 O400 0.257(13) 0.148(9) 0.173(10) -0.028(8) 0.057(9) -0.026(9) O500 0.239(15) 1.01(5) 0.090(8) 0.126(17) -0.052(8) -0.34(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 Cd1 N1 2.357(4) . ? Cd1 N1 2.357(4) 2_655 ? Cd1 S1 2.4801(16) . ? Cd1 S1 2.4801(16) 2_655 ? Cd2 N2 2.334(4) . ? Cd2 N2 2.334(4) 2 ? Cd2 S2 2.4922(17) 2 ? Cd2 S2 2.4922(17) . ? S1 S3 2.029(2) . ? S2 S4 2.030(3) . ? S3 O3 1.414(6) . ? S3 O1 1.441(5) . ? S3 O2 1.491(7) . ? S4 O5 1.354(6) . ? S4 O6 1.465(6) . ? S4 O4 1.619(9) . ? N1 C1 1.321(7) . ? N1 C5 1.322(7) . ? N2 C10 1.324(7) . ? N2 C6 1.329(7) . ? N5 C24 1.317(10) . ? N5 C21 1.338(10) . ? N4 C18 1.309(9) . ? N4 C19 1.348(9) . ? N4 H4B 0.8600 . ? C3 C4 1.375(8) . ? C3 C2 1.391(7) . ? C3 C3 1.478(10) 3_665 ? C2 C1 1.371(8) . ? C2 H2 0.9300 . ? C13 C12 1.375(9) . ? C13 C14 1.391(9) . ? C13 C16 1.488(8) . ? C25 C22 1.386(9) . ? C25 C23 1.387(9) . ? C25 C26 1.481(8) . ? C16 C17 1.394(9) . ? C16 C20 1.394(8) . ? C9C C10 1.364(8) . ? C9C C8 1.386(7) . ? C9C H9 0.9300 . ? C7 C6 1.371(8) . ? C7 C8 1.377(7) . ? C7 H7 0.9300 . ? C8 C8 1.502(10) 3 ? C4 C5 1.389(9) . ? C4 H4 0.9300 . ? C6 H6 0.9300 . ? N3 C11 1.331(10) . ? N3 C15 1.339(9) . ? C17 C18 1.373(9) . ? C17 H17 0.9300 . ? N6 C28 1.320(11) . ? N6 C29 1.329(10) . ? C27 C28 1.378(11) . ? C27 C26 1.381(9) . ? C27 H27 0.9300 . ? C20 C19 1.364(9) . ? C20 H20 0.9300 . ? C26 C30 1.378(9) . ? C10 H10 0.9300 . ? C15 C14 1.368(9) . ? C15 H15 0.9300 . ? C19 H19 0.9300 . ? C1 H1 0.9300 . ? C30 C29 1.370(9) . ? C30 H30 0.9300 . ? C22 C21 1.370(9) . ? C22 H22 0.9300 . ? C5 H5 0.9300 . ? C12 C11 1.383(10) . ? C12 H12 0.9300 . ? C23 C24 1.367(9) . ? C23 H23 0.9300 . ? C29 H29 0.9300 . ? C11 H11 0.9300 . ? C24 H24 0.9300 . ? C28 H28 0.9300 . ? C21 H21 0.9300 . ? C18 H18 0.9300 . ? C14 H14 0.9300 . ? O4 H4A 0.8200 . ? 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 N1 Cd1 N1 94.0(2) . 2_655 ? N1 Cd1 S1 112.58(13) . . ? N1 Cd1 S1 91.91(12) 2_655 . ? N1 Cd1 S1 91.91(12) . 2_655 ? N1 Cd1 S1 112.58(13) 2_655 2_655 ? S1 Cd1 S1 144.37(10) . 2_655 ? N2 Cd2 N2 94.5(2) . 2 ? N2 Cd2 S2 110.86(12) . 2 ? N2 Cd2 S2 94.57(12) 2 2 ? N2 Cd2 S2 94.57(12) . . ? N2 Cd2 S2 110.86(12) 2 . ? S2 Cd2 S2 142.55(10) 2 . ? S3 S1 Cd1 92.01(7) . . ? S4 S2 Cd2 91.31(9) . . ? O3 S3 O1 114.6(5) . . ? O3 S3 O2 109.9(5) . . ? O1 S3 O2 110.8(4) . . ? O3 S3 S1 107.5(3) . . ? O1 S3 S1 106.2(2) . . ? O2 S3 S1 107.5(3) . . ? O5 S4 O6 117.8(5) . . ? O5 S4 O4 104.5(5) . . ? O6 S4 O4 110.7(5) . . ? O5 S4 S2 111.2(3) . . ? O6 S4 S2 105.1(3) . . ? O4 S4 S2 107.1(5) . . ? C1 N1 C5 117.2(5) . . ? C1 N1 Cd1 119.4(4) . . ? C5 N1 Cd1 123.2(4) . . ? C10 N2 C6 115.6(5) . . ? C10 N2 Cd2 124.1(4) . . ? C6 N2 Cd2 120.2(4) . . ? C24 N5 C21 116.9(6) . . ? C18 N4 C19 120.6(6) . . ? C18 N4 H4B 119.7 . . ? C19 N4 H4B 119.7 . . ? C4 C3 C2 116.4(5) . . ? C4 C3 C3 122.0(6) . 3_665 ? C2 C3 C3 121.6(6) . 3_665 ? C1 C2 C3 120.4(5) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C12 C13 C14 117.5(6) . . ? C12 C13 C16 121.3(6) . . ? C14 C13 C16 121.2(6) . . ? C22 C25 C23 116.0(6) . . ? C22 C25 C26 122.7(6) . . ? C23 C25 C26 121.3(6) . . ? C17 C16 C20 118.4(6) . . ? C17 C16 C13 121.6(6) . . ? C20 C16 C13 120.0(6) . . ? C10 C9C C8 119.3(5) . . ? C10 C9C H9 120.3 . . ? C8 C9C H9 120.3 . . ? C6 C7 C8 119.5(5) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C7 C8 C9C 116.7(5) . . ? C7 C8 C8 121.6(6) . 3 ? C9C C8 C8 121.7(6) . 3 ? C3 C4 C5 119.3(6) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N2 C6 C7 124.2(5) . . ? N2 C6 H6 117.9 . . ? C7 C6 H6 117.9 . . ? C11 N3 C15 118.6(6) . . ? C18 C17 C16 119.3(6) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C28 N6 C29 119.4(7) . . ? C28 C27 C26 119.8(8) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C19 C20 C16 118.6(6) . . ? C19 C20 H20 120.7 . . ? C16 C20 H20 120.7 . . ? C30 C26 C27 117.8(6) . . ? C30 C26 C25 121.2(6) . . ? C27 C26 C25 121.0(6) . . ? N2 C10 C9C 124.7(5) . . ? N2 C10 H10 117.7 . . ? C9C C10 H10 117.7 . . ? N3 C15 C14 122.6(7) . . ? N3 C15 H15 118.7 . . ? C14 C15 H15 118.7 . . ? N4 C19 C20 121.6(6) . . ? N4 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? N1 C1 C2 123.0(5) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C29 C30 C26 119.3(7) . . ? C29 C30 H30 120.4 . . ? C26 C30 H30 120.4 . . ? C21 C22 C25 120.5(7) . . ? C21 C22 H22 119.8 . . ? C25 C22 H22 119.8 . . ? N1 C5 C4 123.6(6) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? C13 C12 C11 120.2(7) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C24 C23 C25 119.8(7) . . ? C24 C23 H23 120.1 . . ? C25 C23 H23 120.1 . . ? N6 C29 C30 122.3(7) . . ? N6 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? N3 C11 C12 121.7(7) . . ? N3 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? N5 C24 C23 124.1(7) . . ? N5 C24 H24 118.0 . . ? C23 C24 H24 118.0 . . ? N6 C28 C27 121.5(8) . . ? N6 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? N5 C21 C22 122.7(7) . . ? N5 C21 H21 118.6 . . ? C22 C21 H21 118.6 . . ? N4 C18 C17 121.4(7) . . ? N4 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C15 C14 C13 119.4(7) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? S4 O4 H4A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 28.07 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 3.522 _refine_diff_density_min -2.159 _refine_diff_density_rms 0.121 #####END##### data_Compound(6) _database_code_depnum_ccdc_archive 'CCDC 727268' _chemical_name_systematic ; ? ; _chemical_name_common '3D-Cadmium sulphate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H26 Cd2 N4 O13 S2' _chemical_formula_weight 819.28 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 C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 24.5534(6) _cell_length_b 9.7877(2) _cell_length_c 13.5716(3) _cell_angle_alpha 90.00 _cell_angle_beta 120.579(2) _cell_angle_gamma 90.00 _cell_volume 2807.96(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8579 _cell_measurement_theta_min 1.74 _cell_measurement_theta_max 30.57 _exptl_crystal_description 'Block like' _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.914 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 1.733 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8596 _exptl_absorpt_correction_T_max 0.8738 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30229 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 30.57 _reflns_number_total 8579 _reflns_number_gt 6599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1999) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0762P)^2^+7.0806P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(4) _refine_ls_number_reflns 8579 _refine_ls_number_parameters 365 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1435 _refine_ls_wR_factor_gt 0.1311 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 Cd1 Cd 0.246597(16) 0.39001(5) 0.10180(3) 0.03131(11) Uani 1 1 d . . . Cd2 Cd 0.256156(16) 0.89774(5) 0.35669(3) 0.03058(11) Uani 1 1 d . . . S1 S 0.18480(7) 0.57331(16) 0.22368(14) 0.0314(3) Uani 1 1 d . . . S2 S 0.30894(7) 0.05026(17) 0.18811(15) 0.0338(3) Uani 1 1 d . . . N1 N 0.1497(2) 0.2900(6) 0.0045(4) 0.0270(11) Uani 1 1 d . . . N2 N 0.3431(2) 0.4894(5) 0.2170(5) 0.0318(12) Uani 1 1 d . . . N3 N -0.1589(2) 0.0017(6) -0.2626(5) 0.0324(12) Uani 1 1 d . . . N4 N 0.6466(3) 0.7931(7) 0.5300(5) 0.0401(14) Uani 1 1 d . . . O1 O 0.2958(2) 0.3112(5) 0.0021(5) 0.0451(12) Uani 1 1 d . . . O2 O 0.2013(3) 0.5864(8) 0.1329(6) 0.0691(18) Uani 1 1 d . . . O3 O 0.2871(2) 0.1838(5) 0.2122(5) 0.0410(12) Uani 1 1 d . . . O4 O 0.2079(2) 0.5454(5) -0.0679(4) 0.0435(11) Uani 1 1 d . . . O5 O 0.2127(3) 0.6854(6) 0.3040(7) 0.076(2) Uani 1 1 d . . . O6 O 0.2734(3) -0.0601(5) 0.2058(5) 0.0446(13) Uani 1 1 d . . . O7 O 0.2338(3) 0.8689(7) 0.5048(5) 0.0685(19) Uani 1 1 d . . . O8 O 0.3011(3) 1.1172(8) 0.4279(9) 0.106(4) Uani 1 1 d . . . O9 O 0.2132(5) 0.4465(7) 0.2769(8) 0.104(3) Uani 1 1 d . . . O10 O 0.1172(3) 0.5746(8) 0.1683(7) 0.076(2) Uani 1 1 d . . . O11 O 0.3766(2) 0.0327(7) 0.2641(6) 0.0617(17) Uani 1 1 d . . . C1 C 0.1406(3) 0.1561(7) 0.0031(5) 0.0306(13) Uani 1 1 d . . . H1 H 0.1759 0.0996 0.0388 0.037 Uiso 1 1 calc R . . C2 C 0.0806(3) 0.0955(7) -0.0492(5) 0.0259(12) Uani 1 1 d . . . H2 H 0.0764 0.0011 -0.0483 0.031 Uiso 1 1 calc R . . C3 C 0.0270(2) 0.1794(6) -0.1030(5) 0.0220(11) Uani 1 1 d . . . C4 C 0.0368(3) 0.3178(7) -0.1035(6) 0.0344(15) Uani 1 1 d . . . H4 H 0.0023 0.3761 -0.1410 0.041 Uiso 1 1 calc R . . C5 C 0.0980(3) 0.3720(7) -0.0485(6) 0.0330(15) Uani 1 1 d . . . H5 H 0.1034 0.4661 -0.0481 0.040 Uiso 1 1 calc R . . C6 C -0.0379(3) 0.1193(6) -0.1599(5) 0.0246(12) Uani 1 1 d . . . C7 C -0.0920(3) 0.1986(7) -0.2033(5) 0.0296(13) Uani 1 1 d . . . H7 H -0.0881 0.2932 -0.1976 0.036 Uiso 1 1 calc R . . C8 C -0.1511(3) 0.1415(7) -0.2543(6) 0.0322(14) Uani 1 1 d . . . H8 H -0.1865 0.1979 -0.2838 0.039 Uiso 1 1 calc R . . C9 C 0.3509(3) 0.6235(7) 0.2328(5) 0.0299(13) Uani 1 1 d . . . H9 H 0.3150 0.6780 0.2045 0.036 Uiso 1 1 calc R . . C10 C 0.4078(3) 0.6850(7) 0.2873(5) 0.0293(13) Uani 1 1 d . . . H10 H 0.4100 0.7799 0.2905 0.035 Uiso 1 1 calc R . . C11 C 0.4633(2) 0.6096(6) 0.3387(5) 0.0246(12) Uani 1 1 d . . . C12 C 0.4562(3) 0.4662(7) 0.3271(7) 0.0432(19) Uani 1 1 d . . . H12 H 0.4916 0.4098 0.3606 0.052 Uiso 1 1 calc R . . C13 C 0.3964(3) 0.4107(9) 0.2657(7) 0.0445(19) Uani 1 1 d . . . H13 H 0.3922 0.3163 0.2573 0.053 Uiso 1 1 calc R . . C14 C 0.5284(3) 0.6730(7) 0.4025(5) 0.0277(13) Uani 1 1 d . . . C15 C 0.5352(3) 0.8111(7) 0.4206(7) 0.045(2) Uani 1 1 d . . . H15 H 0.4997 0.8669 0.3916 0.054 Uiso 1 1 calc R . . C16 C 0.5815(2) 0.5932(7) 0.4500(5) 0.0291(13) Uani 1 1 d . . . H16 H 0.5788 0.4988 0.4408 0.035 Uiso 1 1 calc R . . C17 C -0.1077(3) -0.0753(7) -0.2188(7) 0.0428(19) Uani 1 1 d . . . H17 H -0.1127 -0.1697 -0.2227 0.051 Uiso 1 1 calc R . . C18 C -0.0463(3) -0.0222(7) -0.1669(7) 0.0387(17) Uani 1 1 d . . . H18 H -0.0115 -0.0803 -0.1375 0.046 Uiso 1 1 calc R . . C19 C 0.6411(3) 0.6597(7) 0.5141(6) 0.0341(14) Uani 1 1 d . . . H19 H 0.6777 0.6070 0.5461 0.041 Uiso 1 1 calc R . . C20 C 0.5932(3) 0.8658(7) 0.4800(8) 0.055(3) Uani 1 1 d . . . H20 H 0.5965 0.9604 0.4869 0.066 Uiso 1 1 calc R . . O100 O 0.4283(6) 0.2441(13) 0.0467(11) 0.136(4) Uani 1 1 d . . . O200 O 0.4827(7) 0.1349(18) 0.2653(13) 0.184(6) 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 Cd1 0.01607(17) 0.0292(2) 0.0382(2) -0.0011(3) 0.00617(15) -0.0068(2) Cd2 0.01820(17) 0.0337(2) 0.0322(2) 0.0036(3) 0.00732(14) 0.0089(2) S1 0.0270(7) 0.0269(7) 0.0339(7) -0.0025(6) 0.0109(6) -0.0007(6) S2 0.0259(7) 0.0251(7) 0.0465(9) 0.0036(7) 0.0155(7) 0.0022(6) N1 0.016(2) 0.029(3) 0.026(2) -0.003(2) 0.0039(19) -0.0058(19) N2 0.016(2) 0.023(3) 0.044(3) -0.007(2) 0.006(2) -0.0064(19) N3 0.018(2) 0.031(3) 0.041(3) -0.004(2) 0.010(2) -0.010(2) N4 0.026(3) 0.046(4) 0.037(3) -0.006(3) 0.008(2) -0.011(3) O1 0.042(3) 0.038(3) 0.050(3) -0.004(2) 0.020(2) 0.000(2) O2 0.065(4) 0.076(5) 0.082(5) -0.014(4) 0.049(4) -0.008(3) O3 0.037(3) 0.022(2) 0.056(3) 0.006(2) 0.019(2) 0.0020(19) O4 0.054(3) 0.031(2) 0.055(3) 0.001(2) 0.034(3) 0.003(2) O5 0.051(4) 0.048(4) 0.088(5) -0.036(4) 0.006(3) 0.005(3) O6 0.059(3) 0.031(3) 0.051(3) 0.002(2) 0.033(3) -0.009(2) O7 0.085(5) 0.070(5) 0.051(3) -0.002(3) 0.035(3) 0.017(4) O8 0.040(4) 0.066(5) 0.152(8) -0.051(5) 0.006(4) 0.010(3) O9 0.115(7) 0.043(4) 0.096(6) -0.008(4) 0.012(5) 0.005(4) O10 0.036(3) 0.089(5) 0.107(6) -0.050(5) 0.039(4) -0.021(3) O11 0.026(3) 0.059(4) 0.083(4) 0.007(3) 0.015(3) 0.005(3) C1 0.018(3) 0.031(3) 0.033(3) 0.001(3) 0.006(2) -0.004(2) C2 0.014(2) 0.025(3) 0.034(3) -0.001(2) 0.010(2) -0.005(2) C3 0.011(2) 0.029(3) 0.022(2) -0.003(2) 0.0056(19) -0.003(2) C4 0.017(3) 0.028(3) 0.046(4) 0.002(3) 0.007(3) -0.002(2) C5 0.024(3) 0.024(4) 0.041(3) -0.006(3) 0.009(2) -0.008(2) C6 0.023(3) 0.021(3) 0.027(3) -0.003(2) 0.010(2) -0.007(2) C7 0.020(3) 0.028(3) 0.033(3) -0.001(2) 0.008(2) -0.008(2) C8 0.016(3) 0.036(3) 0.035(3) 0.001(3) 0.006(2) -0.002(2) C9 0.022(3) 0.036(3) 0.028(3) 0.001(3) 0.009(2) 0.003(2) C10 0.030(3) 0.025(3) 0.029(3) -0.002(2) 0.012(2) -0.001(2) C11 0.015(2) 0.027(3) 0.024(3) -0.004(2) 0.005(2) -0.007(2) C12 0.021(3) 0.029(4) 0.058(5) -0.002(3) 0.004(3) -0.006(3) C13 0.020(3) 0.030(4) 0.062(4) -0.010(4) 0.006(3) -0.005(3) C14 0.023(3) 0.033(3) 0.021(3) 0.000(2) 0.006(2) -0.008(2) C15 0.026(3) 0.027(4) 0.061(5) 0.008(3) 0.006(3) -0.004(3) C16 0.013(2) 0.033(3) 0.034(3) -0.009(2) 0.006(2) -0.007(2) C17 0.023(3) 0.030(5) 0.062(5) -0.006(3) 0.011(3) -0.007(2) C18 0.020(3) 0.030(4) 0.059(5) -0.007(3) 0.014(3) -0.006(2) C19 0.022(3) 0.034(4) 0.038(3) -0.008(3) 0.010(3) -0.006(3) C20 0.028(3) 0.024(4) 0.078(6) 0.005(3) 0.001(3) -0.005(3) O100 0.129(9) 0.125(9) 0.150(11) 0.010(8) 0.067(8) -0.041(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.273(5) . ? Cd1 N2 2.289(5) . ? Cd1 O1 2.356(6) . ? Cd1 O2 2.364(7) . ? Cd1 O3 2.407(5) . ? Cd1 O4 2.509(5) . ? Cd2 O5 2.279(6) . ? Cd2 N3 2.295(5) 2_565 ? Cd2 N4 2.320(5) 2_656 ? Cd2 O6 2.329(5) 1_565 ? Cd2 O7 2.355(7) . ? Cd2 O8 2.383(7) . ? S1 O9 1.427(8) . ? S1 O10 1.433(6) . ? S1 O5 1.449(6) . ? S1 O2 1.486(7) . ? S2 O11 1.454(5) . ? S2 O4 1.466(6) 4_545 ? S2 O6 1.483(5) . ? S2 O3 1.510(5) . ? N1 C1 1.328(8) . ? N1 C5 1.358(8) . ? N2 C9 1.328(8) . ? N2 C13 1.364(9) . ? N3 C17 1.320(8) . ? N3 C8 1.378(9) . ? N3 Cd2 2.295(5) 2_545 ? N4 C19 1.319(9) . ? N4 C20 1.334(9) . ? N4 Cd2 2.320(5) 2_656 ? O4 S2 1.466(6) 4 ? O6 Cd2 2.329(5) 1_545 ? C1 C2 1.401(8) . ? C1 H1 0.9300 . ? C2 C3 1.400(8) . ? C2 H2 0.9300 . ? C3 C4 1.377(9) . ? C3 C6 1.493(7) . ? C4 C5 1.397(8) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.385(9) . ? C6 C18 1.395(8) . ? C7 C8 1.369(8) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.346(9) . ? C9 H9 0.9300 . ? C10 C11 1.385(8) . ? C10 H10 0.9300 . ? C11 C12 1.413(9) . ? C11 C14 1.511(7) . ? C12 C13 1.380(9) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C16 1.368(9) . ? C14 C15 1.369(9) . ? C15 C20 1.340(9) . ? C15 H15 0.9300 . ? C16 C19 1.424(8) . ? C16 H16 0.9300 . ? C17 C18 1.400(9) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N2 173.8(2) . . ? N1 Cd1 O1 102.47(19) . . ? N2 Cd1 O1 82.9(2) . . ? N1 Cd1 O2 90.3(2) . . ? N2 Cd1 O2 87.1(2) . . ? O1 Cd1 O2 142.6(2) . . ? N1 Cd1 O3 88.79(18) . . ? N2 Cd1 O3 88.57(18) . . ? O1 Cd1 O3 85.00(19) . . ? O2 Cd1 O3 130.8(2) . . ? N1 Cd1 O4 86.14(18) . . ? N2 Cd1 O4 98.4(2) . . ? O1 Cd1 O4 74.71(18) . . ? O2 Cd1 O4 71.2(2) . . ? O3 Cd1 O4 157.45(18) . . ? O5 Cd2 N3 92.4(2) . 2_565 ? O5 Cd2 N4 88.0(2) . 2_656 ? N3 Cd2 N4 173.6(2) 2_565 2_656 ? O5 Cd2 O6 98.7(3) . 1_565 ? N3 Cd2 O6 92.0(2) 2_565 1_565 ? N4 Cd2 O6 94.3(2) 2_656 1_565 ? O5 Cd2 O7 83.3(3) . . ? N3 Cd2 O7 84.2(2) 2_565 . ? N4 Cd2 O7 89.4(2) 2_656 . ? O6 Cd2 O7 175.8(2) 1_565 . ? O5 Cd2 O8 174.6(4) . . ? N3 Cd2 O8 87.8(2) 2_565 . ? N4 Cd2 O8 91.2(2) 2_656 . ? O6 Cd2 O8 86.7(3) 1_565 . ? O7 Cd2 O8 91.3(3) . . ? O9 S1 O10 114.2(5) . . ? O9 S1 O5 110.8(4) . . ? O10 S1 O5 111.5(4) . . ? O9 S1 O2 103.1(6) . . ? O10 S1 O2 107.2(4) . . ? O5 S1 O2 109.5(5) . . ? O11 S2 O4 111.1(4) . 4_545 ? O11 S2 O6 110.7(4) . . ? O4 S2 O6 107.5(3) 4_545 . ? O11 S2 O3 110.7(4) . . ? O4 S2 O3 109.8(3) 4_545 . ? O6 S2 O3 107.0(3) . . ? C1 N1 C5 118.0(5) . . ? C1 N1 Cd1 123.6(4) . . ? C5 N1 Cd1 118.2(4) . . ? C9 N2 C13 117.2(6) . . ? C9 N2 Cd1 123.0(4) . . ? C13 N2 Cd1 119.7(4) . . ? C17 N3 C8 118.0(5) . . ? C17 N3 Cd2 118.7(4) . 2_545 ? C8 N3 Cd2 123.2(4) . 2_545 ? C19 N4 C20 117.0(6) . . ? C19 N4 Cd2 122.0(5) . 2_656 ? C20 N4 Cd2 121.0(5) . 2_656 ? S1 O2 Cd1 115.4(4) . . ? S2 O3 Cd1 132.1(3) . . ? S2 O4 Cd1 143.3(3) 4 . ? S1 O5 Cd2 153.3(6) . . ? S2 O6 Cd2 131.1(3) . 1_545 ? N1 C1 C2 123.5(6) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 118.9(6) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C4 C3 C2 117.3(5) . . ? C4 C3 C6 122.0(5) . . ? C2 C3 C6 120.7(5) . . ? C3 C4 C5 121.0(6) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? N1 C5 C4 121.3(6) . . ? N1 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C7 C6 C18 116.8(6) . . ? C7 C6 C3 122.6(5) . . ? C18 C6 C3 120.5(5) . . ? C8 C7 C6 121.8(6) . . ? C8 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C7 C8 N3 120.9(6) . . ? C7 C8 H8 119.5 . . ? N3 C8 H8 119.5 . . ? N2 C9 C10 123.7(6) . . ? N2 C9 H9 118.2 . . ? C10 C9 H9 118.2 . . ? C9 C10 C11 121.2(6) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C12 116.1(5) . . ? C10 C11 C14 123.5(5) . . ? C12 C11 C14 120.4(5) . . ? C13 C12 C11 119.4(7) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? N2 C13 C12 122.3(7) . . ? N2 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C16 C14 C15 118.6(6) . . ? C16 C14 C11 120.9(5) . . ? C15 C14 C11 120.4(6) . . ? C20 C15 C14 119.9(7) . . ? C20 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C14 C16 C19 117.7(6) . . ? C14 C16 H16 121.2 . . ? C19 C16 H16 121.2 . . ? N3 C17 C18 123.3(6) . . ? N3 C17 H17 118.3 . . ? C18 C17 H17 118.3 . . ? C6 C18 C17 119.1(6) . . ? C6 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? N4 C19 C16 122.7(6) . . ? N4 C19 H19 118.7 . . ? C16 C19 H19 118.7 . . ? N4 C20 C15 124.1(7) . . ? N4 C20 H20 117.9 . . ? C15 C20 H20 117.9 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.57 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.740 _refine_diff_density_min -0.838 _refine_diff_density_rms 0.157 #####END##### data_Compound(7) _database_code_depnum_ccdc_archive 'CCDC 727269' _chemical_name_systematic ; ? ; _chemical_name_common '3D-Cadmium sulphate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Cd N2 O4 S' _chemical_formula_weight 364.64 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 Tetragonal _symmetry_space_group_name_H-M P-421m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' 'y+1/2, x+1/2, z' '-y+1/2, -x+1/2, z' '-y, x, -z' 'y, -x, -z' _cell_length_a 6.8212(7) _cell_length_b 6.8212(7) _cell_length_c 11.838(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 550.81(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 627 _cell_measurement_theta_min 1.72 _cell_measurement_theta_max 26.30 _exptl_crystal_description 'Plate like' _exptl_crystal_colour 'Yellowish White' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 356 _exptl_absorpt_coefficient_mu 2.179 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8450 _exptl_absorpt_correction_T_max 0.8804 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4320 _diffrn_reflns_av_R_equivalents 0.1463 _diffrn_reflns_av_sigmaI/netI 0.0632 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.30 _reflns_number_total 627 _reflns_number_gt 579 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1999) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0275P)^2^+0.4698P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(3) _refine_ls_number_reflns 627 _refine_ls_number_parameters 57 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 1.185 _refine_ls_restrained_S_all 1.185 _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 0.5000 0.0000 0.46021(6) 0.0141(2) Uani 1 4 d S . . O1 O 0.4853(19) -0.3305(7) 0.4280(3) 0.0536(18) Uani 1 1 d . . . N1 N 0.5000 0.0000 0.6588(7) 0.028(3) Uani 1 4 d S . . N2 N 0.5000 0.0000 0.2579(7) 0.0173(19) Uani 1 4 d S . . C1 C 0.6138(13) 0.1138(13) 0.7155(9) 0.059(4) Uani 1 2 d S . . H1 H 0.6973 0.1973 0.6762 0.070 Uiso 1 2 calc SR . . C2 C 0.6174(13) 0.1174(13) 0.8337(8) 0.064(4) Uani 1 2 d S . . H2 H 0.7023 0.2023 0.8708 0.076 Uiso 1 2 calc SR . . C3 C 0.5000 0.0000 0.8937(9) 0.026(3) Uani 1 4 d S . . C4 C 0.3837(11) -0.1163(11) 0.1997(8) 0.052(4) Uani 1 2 d S . . H4 H 0.3001 -0.1999 0.2387 0.062 Uiso 1 2 calc SR . . C5 C 0.3806(13) -0.1194(13) 0.0821(8) 0.054(4) Uani 1 2 d S . . H5 H 0.2957 -0.2043 0.0448 0.065 Uiso 1 2 calc SR . . C6 C 0.5000 0.0000 0.0211(7) 0.022(3) Uani 1 4 d S . . S1 S 0.5000 -0.5000 0.5000 0.0153(5) Uani 1 4 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 0.0145(3) 0.0145(3) 0.0132(3) 0.000 0.000 -0.0039(11) O1 0.121(6) 0.015(2) 0.025(2) 0.0023(15) -0.008(5) 0.012(6) N1 0.037(5) 0.037(5) 0.010(4) 0.000 0.000 0.020(18) N2 0.016(3) 0.016(3) 0.020(4) 0.000 0.000 0.010(16) C1 0.073(7) 0.073(7) 0.030(6) 0.001(4) 0.001(4) -0.052(8) C2 0.087(7) 0.087(7) 0.018(5) -0.002(4) -0.002(4) -0.055(9) C3 0.031(5) 0.031(5) 0.016(5) 0.000 0.000 0.020(19) C4 0.067(6) 0.067(6) 0.021(5) 0.002(3) 0.002(3) -0.055(8) C5 0.070(6) 0.070(6) 0.023(5) -0.008(3) -0.008(3) -0.046(8) C6 0.026(4) 0.026(4) 0.012(5) 0.000 0.000 0.012(18) S1 0.0132(7) 0.0132(7) 0.0194(10) 0.000 0.000 0.000 _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 2.289(5) 6 ? Cd1 O1 2.289(5) . ? Cd1 O1 2.289(5) 5_545 ? Cd1 O1 2.289(5) 2_655 ? Cd1 N1 2.350(8) . ? Cd1 N2 2.395(8) . ? O1 S1 1.440(4) . ? N1 C1 1.286(12) . ? N1 C1 1.286(12) 2_655 ? N2 C4 1.317(11) . ? N2 C4 1.317(11) 2_655 ? C1 C2 1.400(14) . ? C1 H1 0.9300 . ? C2 C3 1.337(13) . ? C2 H2 0.9300 . ? C3 C2 1.337(13) 2_655 ? C3 C6 1.508(13) 1_556 ? C4 C5 1.392(14) . ? C4 H4 0.9300 . ? C5 C6 1.359(13) . ? C5 H5 0.9300 . ? C6 C5 1.359(13) 2_655 ? C6 C3 1.508(13) 1_554 ? S1 O1 1.440(4) 2_645 ? S1 O1 1.440(4) 8_656 ? S1 O1 1.440(4) 7_546 ? 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 93.3(6) 6 . ? O1 Cd1 O1 160.81(18) 6 5_545 ? O1 Cd1 O1 83.5(6) . 5_545 ? O1 Cd1 O1 83.5(6) 6 2_655 ? O1 Cd1 O1 160.81(18) . 2_655 ? O1 Cd1 O1 93.3(6) 5_545 2_655 ? O1 Cd1 N1 99.59(9) 6 . ? O1 Cd1 N1 99.59(9) . . ? O1 Cd1 N1 99.59(9) 5_545 . ? O1 Cd1 N1 99.59(9) 2_655 . ? O1 Cd1 N2 80.41(9) 6 . ? O1 Cd1 N2 80.41(9) . . ? O1 Cd1 N2 80.41(9) 5_545 . ? O1 Cd1 N2 80.41(9) 2_655 . ? N1 Cd1 N2 180.000(1) . . ? S1 O1 Cd1 133.6(2) . . ? C1 N1 C1 117.1(12) . 2_655 ? C1 N1 Cd1 121.5(6) . . ? C1 N1 Cd1 121.5(6) 2_655 . ? C4 N2 C4 116.8(11) . 2_655 ? C4 N2 Cd1 121.6(5) . . ? C4 N2 Cd1 121.6(5) 2_655 . ? N1 C1 C2 122.9(11) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 120.7(11) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C2 115.8(12) 2_655 . ? C2 C3 C6 122.1(6) 2_655 1_556 ? C2 C3 C6 122.1(6) . 1_556 ? N2 C4 C5 122.8(10) . . ? N2 C4 H4 118.6 . . ? C5 C4 H4 118.6 . . ? C6 C5 C4 120.8(11) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C5 115.8(11) 2_655 . ? C5 C6 C3 122.1(5) 2_655 1_554 ? C5 C6 C3 122.1(5) . 1_554 ? O1 S1 O1 110.52(16) 2_645 8_656 ? O1 S1 O1 107.4(3) 2_645 . ? O1 S1 O1 110.52(16) 8_656 . ? O1 S1 O1 110.52(16) 2_645 7_546 ? O1 S1 O1 107.4(3) 8_656 7_546 ? O1 S1 O1 110.52(16) . 7_546 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.355 _refine_diff_density_min -1.197 _refine_diff_density_rms 0.168