# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _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 ; The Illustrative use of Thiosulfate in the Formation of New Three-dimensional Hybrid Structures: Synthesis, Structure, Transformation Studies and Sunlight Assisted Photocatalytic Behavior ; 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 450.75 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#####