Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Rao, C. N. R.' 'Choudhury, Amitava' 'Paul, Geo' _publ_contact_author_name 'Prof C. N. R. Rao' _publ_contact_author_address ; Chemistry and Physics of Materials Unit Jawaharlal Nehru Centre for Advanced Scientific Research Jakkur, P. O. Bangalore 560 064 INDIA ; _publ_contact_author_email 'CNRRAO@JNCASR.AC.IN' _publ_section_title ; Organically Templated Linear and Layered Cadmium Sulfates ; data_sad _database_code_CSD 185728 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C4 H22 Cd Cl2 N4 O9 S2' _chemical_formula_weight 517.68 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.3207(2) _cell_length_b 10.6852(3) _cell_length_c 21.8939(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1712.61(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4966 _cell_measurement_theta_min 2 _cell_measurement_theta_max 23 _exptl_crystal_description Rod _exptl_crystal_colour Transparent _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.008 _exptl_crystal_density_method ? _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 1.876 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.803809 _exptl_absorpt_correction_T_max 1.000000 _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 'Siemens CCD-diffractometer' _diffrn_measurement_method '\W' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7148 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 23.29 _reflns_number_total 2461 _reflns_number_observed 2265 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART(Siemens,1996)' _computing_cell_refinement 'SAINT(Siemens,1996)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL v5.0' _computing_publication_material 'SHELXTL v5.0' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0158P)^2^+0.8553P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0052(3) _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 _refine_ls_number_reflns 2461 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_obs 0.0240 _refine_ls_wR_factor_all 0.0507 _refine_ls_wR_factor_obs 0.0492 _refine_ls_goodness_of_fit_all 1.051 _refine_ls_goodness_of_fit_obs 1.068 _refine_ls_restrained_S_all 1.051 _refine_ls_restrained_S_obs 1.068 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd1 Cd 0.11164(4) 0.25194(3) -0.003644(14) 0.02650(11) Uani 1 d . . S1 S 0.3644(2) 0.48223(9) 0.08059(5) 0.0225(2) Uani 1 d . . S2 S 0.0608(2) 0.91425(11) 0.22454(5) 0.0294(3) Uani 1 d . . O1 O 0.0254(4) 0.0973(3) -0.0717(2) 0.0439(9) Uani 1 d . . O2 O 0.2012(4) 0.4087(3) 0.06453(15) 0.0414(9) Uani 1 d . . Cl1 Cl 0.3563(2) 0.10123(10) 0.04221(5) 0.0329(3) Uani 1 d . . Cl2 Cl -0.1305(2) 0.17778(10) 0.07824(5) 0.0328(3) Uani 1 d . . O3 O 0.3772(6) 0.5931(3) 0.04335(14) 0.0535(10) Uani 1 d . . O4 O 0.3524(5) 0.5172(3) 0.14456(13) 0.0444(9) Uani 1 d . . O5 O 0.1621(5) 0.8734(3) 0.1713(2) 0.0607(11) Uani 1 d . . O6 O 0.0934(4) 1.0463(3) 0.23859(15) 0.0417(9) Uani 1 d . . O7 O -0.1351(5) 0.8948(3) 0.21289(14) 0.0417(8) Uani 1 d . . O8 O 0.1119(5) 0.8418(3) 0.27901(13) 0.0436(9) Uani 1 d . . O100 O 0.5092(7) 1.3083(5) 0.3871(3) 0.079(2) Uani 1 d . . H21 H 0.5403(99) 1.2477(69) 0.4055(34) 0.096(29) Uiso 1 d . . H22 H 0.5923(103) 1.3484(63) 0.3741(33) 0.096(29) Uiso 1 d . . N1 N 0.1420(7) 1.3372(3) 0.4216(2) 0.0418(11) Uani 1 d . . H1 H 0.1321(7) 1.3788(3) 0.4566(2) 0.063 Uiso 1 calc R . H2 H 0.0562(7) 1.3633(3) 0.3958(2) 0.063 Uiso 1 calc R . H3 H 0.2518(7) 1.3510(3) 0.4054(2) 0.063 Uiso 1 calc R . C1 C 0.1189(9) 1.2017(4) 0.4330(2) 0.0356(12) Uani 1 d . . H4 H -0.0001(9) 1.1864(4) 0.4511(2) 0.043 Uiso 1 calc R . H5 H 0.2114(9) 1.1732(4) 0.4615(2) 0.043 Uiso 1 calc R . C2 C 0.1356(8) 1.1307(4) 0.3739(2) 0.0329(11) Uani 1 d . . H6 H 0.0354(8) 1.1537(4) 0.3471(2) 0.040 Uiso 1 calc R . H7 H 0.2487(8) 1.1539(4) 0.3538(2) 0.040 Uiso 1 calc R . N2 N 0.1330(5) 0.9942(3) 0.3837(2) 0.0271(8) Uani 1 d . . H8 H 0.1431(5) 0.9552(3) 0.3480(2) 0.041 Uiso 1 calc R . H9 H 0.0284(5) 0.9724(3) 0.4015(2) 0.041 Uiso 1 calc R . H10 H 0.2260(5) 0.9726(3) 0.4077(2) 0.041 Uiso 1 calc R . N3 N 0.2526(5) 1.2353(4) 0.1790(2) 0.0354(10) Uani 1 d . . H11 H 0.1961(5) 1.3085(4) 0.1836(2) 0.053 Uiso 1 calc R . H12 H 0.1842(5) 1.1747(4) 0.1950(2) 0.053 Uiso 1 calc R . H13 H 0.2701(5) 1.2204(4) 0.1395(2) 0.053 Uiso 1 calc R . C3 C 0.4299(6) 1.2391(5) 0.2104(2) 0.0478(13) Uani 1 d . . H14 H 0.5032(6) 1.3062(5) 0.1934(2) 0.057 Uiso 1 calc R . H15 H 0.4105(6) 1.2569(5) 0.2534(2) 0.057 Uiso 1 calc R . C4 C 0.5287(7) 1.1208(5) 0.2043(3) 0.0465(14) Uani 1 d . . H16 H 0.5582(7) 1.1069(5) 0.1617(3) 0.056 Uiso 1 calc R . H17 H 0.4509(7) 1.0527(5) 0.2178(3) 0.056 Uiso 1 calc R . N4 N 0.6988(5) 1.1210(4) 0.2407(2) 0.0354(10) Uani 1 d . . H18 H 0.7558(5) 1.0480(4) 0.2361(2) 0.053 Uiso 1 calc R . H19 H 0.6718(5) 1.1324(4) 0.2799(2) 0.053 Uiso 1 calc R . H20 H 0.7711(5) 1.1826(4) 0.2279(2) 0.053 Uiso 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 0.0188(2) 0.0306(2) 0.0301(2) -0.00572(14) 0.00034(13) -0.00037(15) S1 0.0224(6) 0.0241(5) 0.0210(5) -0.0024(4) 0.0010(5) -0.0008(5) S2 0.0309(7) 0.0306(6) 0.0268(6) -0.0013(5) 0.0017(5) -0.0010(5) O1 0.023(2) 0.050(2) 0.059(2) -0.030(2) 0.009(2) -0.009(2) O2 0.023(2) 0.043(2) 0.059(2) -0.024(2) 0.006(2) -0.005(2) Cl1 0.0275(6) 0.0308(6) 0.0404(6) 0.0042(5) 0.0004(6) 0.0005(6) Cl2 0.0247(6) 0.0439(6) 0.0299(6) 0.0015(5) 0.0001(6) 0.0001(6) O3 0.092(3) 0.036(2) 0.033(2) 0.010(2) -0.002(2) -0.007(2) O4 0.065(2) 0.045(2) 0.023(2) -0.0082(15) 0.004(2) 0.001(2) O5 0.059(3) 0.082(3) 0.041(2) -0.018(2) 0.025(2) -0.005(2) O6 0.048(2) 0.033(2) 0.044(2) 0.0002(15) -0.003(2) -0.011(2) O7 0.033(2) 0.037(2) 0.055(2) -0.004(2) -0.008(2) -0.004(2) O8 0.061(3) 0.036(2) 0.035(2) -0.002(2) -0.012(2) 0.011(2) O100 0.050(3) 0.053(3) 0.133(5) 0.031(3) 0.010(3) -0.004(3) N1 0.059(3) 0.037(2) 0.030(2) -0.005(2) 0.002(3) 0.007(3) C1 0.047(3) 0.032(2) 0.028(2) -0.002(2) 0.000(3) -0.005(3) C2 0.048(3) 0.027(2) 0.024(2) 0.003(2) -0.001(2) -0.003(3) N2 0.023(2) 0.030(2) 0.028(2) 0.001(2) -0.005(2) -0.005(2) N3 0.030(2) 0.037(2) 0.039(2) 0.007(2) -0.003(2) 0.005(2) C3 0.034(3) 0.043(3) 0.066(3) 0.014(3) -0.006(2) 0.003(3) C4 0.034(3) 0.048(3) 0.057(4) 0.004(3) -0.005(3) -0.001(3) N4 0.032(2) 0.040(2) 0.034(2) 0.009(2) -0.002(2) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.312(3) . ? Cd1 O2 2.338(3) . ? Cd1 Cl1 2.5827(11) 4_455 ? Cd1 Cl2 2.6069(12) 4 ? Cd1 Cl1 2.6092(11) . ? Cd1 Cl2 2.6425(12) . ? S1 O3 1.441(3) . ? S1 O4 1.452(3) . ? S1 O1 1.466(3) 4 ? S1 O2 1.472(3) . ? S2 O5 1.450(3) . ? S2 O6 1.464(3) . ? S2 O8 1.470(3) . ? S2 O7 1.471(4) . ? O1 S1 1.466(3) 4_455 ? Cl1 Cd1 2.5827(11) 4 ? Cl2 Cd1 2.6069(12) 4_455 ? O100 H21 0.80(7) . ? O100 H22 0.80(7) . ? N1 C1 1.479(5) . ? N1 H1 0.89 . ? N1 H2 0.89 . ? N1 H3 0.89 . ? C1 C2 1.507(6) . ? C1 H4 0.97 . ? C1 H5 0.97 . ? C2 N2 1.474(5) . ? C2 H6 0.97 . ? C2 H7 0.97 . ? N2 H8 0.89 . ? N2 H9 0.89 . ? N2 H10 0.89 . ? N3 C3 1.469(6) . ? N3 H11 0.89 . ? N3 H12 0.89 . ? N3 H13 0.89 . ? C3 C4 1.462(7) . ? C3 H14 0.97 . ? C3 H15 0.97 . ? C4 N4 1.478(6) . ? C4 H16 0.97 . ? C4 H17 0.97 . ? N4 H18 0.89 . ? N4 H19 0.89 . ? N4 H20 0.89 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O2 179.46(11) . . ? O1 Cd1 Cl1 91.49(9) . 4_455 ? O2 Cd1 Cl1 88.65(8) . 4_455 ? O1 Cd1 Cl2 90.01(8) . 4 ? O2 Cd1 Cl2 89.45(8) . 4 ? Cl1 Cd1 Cl2 98.30(4) 4_455 4 ? O1 Cd1 Cl1 89.66(9) . . ? O2 Cd1 Cl1 90.24(9) . . ? Cl1 Cd1 Cl1 176.01(3) 4_455 . ? Cl2 Cd1 Cl1 85.51(4) 4 . ? O1 Cd1 Cl2 92.26(9) . . ? O2 Cd1 Cl2 88.27(8) . . ? Cl1 Cd1 Cl2 85.32(4) 4_455 . ? Cl2 Cd1 Cl2 175.67(4) 4 . ? Cl1 Cd1 Cl2 90.82(4) . . ? O3 S1 O4 109.7(2) . . ? O3 S1 O1 110.4(2) . 4 ? O4 S1 O1 109.1(2) . 4 ? O3 S1 O2 110.9(2) . . ? O4 S1 O2 108.6(2) . . ? O1 S1 O2 108.1(2) 4 . ? O5 S2 O6 112.1(2) . . ? O5 S2 O8 111.4(2) . . ? O6 S2 O8 107.2(2) . . ? O5 S2 O7 108.4(2) . . ? O6 S2 O7 109.3(2) . . ? O8 S2 O7 108.3(2) . . ? S1 O1 Cd1 136.0(2) 4_455 . ? S1 O2 Cd1 139.7(2) . . ? Cd1 Cl1 Cd1 89.78(3) 4 . ? Cd1 Cl2 Cd1 88.53(3) 4_455 . ? H21 O100 H22 113.6(77) . . ? C1 N1 H1 109.5(2) . . ? C1 N1 H2 109.5(3) . . ? H1 N1 H2 109.5 . . ? C1 N1 H3 109.5(4) . . ? H1 N1 H3 109.5 . . ? H2 N1 H3 109.5 . . ? N1 C1 C2 109.8(3) . . ? N1 C1 H4 109.7(4) . . ? C2 C1 H4 109.7(3) . . ? N1 C1 H5 109.7(3) . . ? C2 C1 H5 109.7(3) . . ? H4 C1 H5 108.2 . . ? N2 C2 C1 111.8(3) . . ? N2 C2 H6 109.3(3) . . ? C1 C2 H6 109.3(3) . . ? N2 C2 H7 109.3(3) . . ? C1 C2 H7 109.3(3) . . ? H6 C2 H7 107.9 . . ? C2 N2 H8 109.5(2) . . ? C2 N2 H9 109.5(3) . . ? H8 N2 H9 109.5 . . ? C2 N2 H10 109.5(3) . . ? H8 N2 H10 109.5 . . ? H9 N2 H10 109.5 . . ? C3 N3 H11 109.5(3) . . ? C3 N3 H12 109.5(3) . . ? H11 N3 H12 109.5 . . ? C3 N3 H13 109.5(3) . . ? H11 N3 H13 109.5 . . ? H12 N3 H13 109.5 . . ? C4 C3 N3 111.7(5) . . ? C4 C3 H14 109.3(3) . . ? N3 C3 H14 109.3(3) . . ? C4 C3 H15 109.3(3) . . ? N3 C3 H15 109.3(3) . . ? H14 C3 H15 107.9 . . ? C3 C4 N4 111.5(4) . . ? C3 C4 H16 109.3(3) . . ? N4 C4 H16 109.3(3) . . ? C3 C4 H17 109.3(3) . . ? N4 C4 H17 109.3(3) . . ? H16 C4 H17 108.0 . . ? C4 N4 H18 109.5(3) . . ? C4 N4 H19 109.5(3) . . ? H18 N4 H19 109.5 . . ? C4 N4 H20 109.5(3) . . ? H18 N4 H20 109.5 . . ? H19 N4 H20 109.5 . . ? _refine_diff_density_max 0.518 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.077 #===END data_try _database_code_CSD 185729 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C1.50 H3.50 Br0.50 Cd0.25 N0.50 O S0.25' _chemical_formula_weight 120.62 _chemical_melting_point ? _chemical_compound_source ? 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' 'Br' 'Br' -0.2901 2.4595 '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 Orthorhombic _symmetry_space_group_name_H-M Cmcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 9.7782(9) _cell_length_b 17.300(2) _cell_length_c 7.5504(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1277.3(2) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2393 _cell_measurement_theta_min 2 _cell_measurement_theta_max 23 _exptl_crystal_description Plate-like _exptl_crystal_colour Transparent _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.509 _exptl_crystal_density_method ? _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 8.130 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.496220 _exptl_absorpt_correction_T_max 1.000000 _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 'Siemens CCD-diffractometer' _diffrn_measurement_method '\W' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2636 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 23.27 _reflns_number_total 533 _reflns_number_observed 508 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART(Siemens,1996)' _computing_cell_refinement 'SAINT(Siemens,1996)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL v5.0' _computing_publication_material 'SHELXTL v5.0' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+1.8302P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0431(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 533 _refine_ls_number_parameters 53 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_obs 0.0233 _refine_ls_wR_factor_all 0.0600 _refine_ls_wR_factor_obs 0.0588 _refine_ls_goodness_of_fit_all 1.089 _refine_ls_goodness_of_fit_obs 1.096 _refine_ls_restrained_S_all 1.089 _refine_ls_restrained_S_obs 1.096 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd1 Cd 0.0000 0.0000 0.0000 0.0267(3) Uani 1 d S . S1 S 0.0000 -0.17203(9) 0.2500 0.0196(4) Uani 1 d S . O1 O 0.0317(8) -0.1245(3) 0.0947(6) 0.042(3) Uani 0.50 d P . Br1 Br 0.19703(5) 0.03566(3) 0.2500 0.0343(3) Uani 1 d S . O2 O -0.1164(4) -0.2229(3) 0.2500 0.075(2) Uani 1 d S . N1 N 0.6249(4) -0.1795(3) 0.2500 0.0364(11) Uani 1 d S . H1 H 0.7180(4) -0.1798(3) 0.2500 0.044 Uiso 1 calc SR . C1 C 0.5772(4) -0.1390(2) 0.0886(6) 0.0479(10) Uani 1 d . . H2 H 0.6112(4) -0.1652(2) -0.0161(6) 0.057 Uiso 1 calc R . H3 H 0.6112(4) -0.0864(2) 0.0876(6) 0.057 Uiso 1 calc R . C2 C 0.5753(6) -0.2611(3) 0.2500 0.0406(13) Uani 1 d S . H4 H 0.6090(6) -0.2878(3) 0.1459 0.049 Uiso 0.50 calc PR . H5 H 0.6090(6) -0.2878(3) 0.3541 0.049 Uiso 0.50 calc PR . 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 0.0426(4) 0.0186(4) 0.0188(4) 0.0011(2) 0.000 0.000 S1 0.0216(8) 0.0148(8) 0.0224(9) 0.000 0.000 0.000 O1 0.081(9) 0.021(2) 0.025(2) 0.003(2) 0.013(3) 0.007(3) Br1 0.0373(4) 0.0391(5) 0.0267(4) 0.000 0.000 -0.0054(2) O2 0.027(2) 0.069(3) 0.128(5) 0.000 0.000 -0.018(2) N1 0.019(2) 0.050(3) 0.040(3) 0.000 0.000 -0.009(2) C1 0.063(2) 0.044(2) 0.037(2) 0.008(2) 0.009(2) -0.016(2) C2 0.044(3) 0.029(3) 0.049(3) 0.000 0.000 0.011(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 O1 2.291(5) . ? Cd1 O1 2.291(5) 4 ? Cd1 O1 2.291(4) 9 ? Cd1 O1 2.291(4) 12 ? Cd1 Br1 2.7669(4) 11 ? Cd1 Br1 2.7669(4) . ? Cd1 Br1 2.7669(4) 3 ? Cd1 Br1 2.7669(4) 9 ? S1 O2 1.440(5) 3 ? S1 O2 1.440(5) . ? S1 O1 1.465(5) 10_556 ? S1 O1 1.465(5) 3 ? S1 O1 1.465(5) 12 ? S1 O1 1.465(5) . ? O1 O1 0.62(2) 12 ? Br1 Cd1 2.7669(4) 2 ? N1 C1 1.481(5) . ? N1 C1 1.481(5) 10_556 ? N1 C2 1.494(8) . ? C1 C1 1.511(8) 12_655 ? C2 C2 1.472(13) 3_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O1 164.4(4) . 4 ? O1 Cd1 O1 180.0 . 9 ? O1 Cd1 O1 15.6(4) 4 9 ? O1 Cd1 O1 15.6(4) . 12 ? O1 Cd1 O1 180.0 4 12 ? O1 Cd1 O1 164.4(4) 9 12 ? O1 Cd1 Br1 84.8(2) . 11 ? O1 Cd1 Br1 84.4(2) 4 11 ? O1 Cd1 Br1 95.2(2) 9 11 ? O1 Cd1 Br1 95.6(2) 12 11 ? O1 Cd1 Br1 84.4(2) . . ? O1 Cd1 Br1 84.8(2) 4 . ? O1 Cd1 Br1 95.6(2) 9 . ? O1 Cd1 Br1 95.2(2) 12 . ? Br1 Cd1 Br1 91.73(2) 11 . ? O1 Cd1 Br1 95.2(2) . 3 ? O1 Cd1 Br1 95.6(2) 4 3 ? O1 Cd1 Br1 84.8(2) 9 3 ? O1 Cd1 Br1 84.4(2) 12 3 ? Br1 Cd1 Br1 180.0 11 3 ? Br1 Cd1 Br1 88.27(2) . 3 ? O1 Cd1 Br1 95.6(2) . 9 ? O1 Cd1 Br1 95.2(2) 4 9 ? O1 Cd1 Br1 84.4(2) 9 9 ? O1 Cd1 Br1 84.8(2) 12 9 ? Br1 Cd1 Br1 88.27(2) 11 9 ? Br1 Cd1 Br1 180.0 . 9 ? Br1 Cd1 Br1 91.73(2) 3 9 ? O2 S1 O2 104.5(4) 3 . ? O2 S1 O1 100.1(3) 3 10_556 ? O2 S1 O1 120.7(3) . 10_556 ? O2 S1 O1 120.7(3) 3 3 ? O2 S1 O1 100.1(3) . 3 ? O1 S1 O1 24.5(6) 10_556 3 ? O2 S1 O1 120.7(3) 3 12 ? O2 S1 O1 100.1(3) . 12 ? O1 S1 O1 111.8(4) 10_556 12 ? O1 S1 O1 106.3(4) 3 12 ? O2 S1 O1 100.1(3) 3 . ? O2 S1 O1 120.7(3) . . ? O1 S1 O1 106.3(4) 10_556 . ? O1 S1 O1 111.8(4) 3 . ? O1 S1 O1 24.5(6) 12 . ? O1 O1 S1 77.8(3) 12 . ? O1 O1 Cd1 82.2(2) 12 . ? S1 O1 Cd1 138.4(3) . . ? Cd1 Br1 Cd1 86.03(2) . 2 ? C1 N1 C1 110.8(5) . 10_556 ? C1 N1 C2 110.1(3) . . ? C1 N1 C2 110.1(3) 10_556 . ? N1 C1 C1 108.4(2) . 12_655 ? C2 C2 N1 109.0(3) 3_655 . ? _refine_diff_density_max 1.197 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.127 #===END data_try2 _database_code_CSD 185730 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C1.50 H3.50 Cd0.25 Cl0.50 N0.50 O S0.25' _chemical_formula_weight 98.39 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 9.7138(10) _cell_length_b 16.922(2) _cell_length_c 7.3872(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1214.3(2) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2246 _cell_measurement_theta_min 2 _cell_measurement_theta_max 23 _exptl_crystal_description Rod _exptl_crystal_colour Transparent _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.153 _exptl_crystal_density_method ? _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 2.410 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.544957 _exptl_absorpt_correction_T_max 1.000000 _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 'Siemens CCD-diffractometer' _diffrn_measurement_method '\W' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2520 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 23.26 _reflns_number_total 510 _reflns_number_observed 478 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART(Siemens,1996)' _computing_cell_refinement 'SAINT(Siemens,1996)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL v5.0' _computing_publication_material 'SHELXTL v5.0' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+2.4096P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0534(26) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 510 _refine_ls_number_parameters 53 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0260 _refine_ls_R_factor_obs 0.0249 _refine_ls_wR_factor_all 0.0663 _refine_ls_wR_factor_obs 0.0657 _refine_ls_goodness_of_fit_all 1.171 _refine_ls_goodness_of_fit_obs 1.203 _refine_ls_restrained_S_all 1.171 _refine_ls_restrained_S_obs 1.203 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd1 Cd 0.0000 0.0000 0.0000 0.0279(4) Uani 1 d S . S1 S 0.0000 -0.17494(9) 0.2500 0.0232(5) Uani 1 d S . O1 O 0.0351(9) -0.1268(3) 0.0917(6) 0.054(4) Uani 0.50 d P . Cl1 Cl 0.18541(13) 0.03361(9) 0.2500 0.0400(5) Uani 1 d S . O2 O -0.1164(5) -0.2273(4) 0.2500 0.090(2) Uani 1 d S . N1 N 0.6262(4) -0.1717(3) 0.2500 0.0409(11) Uani 1 d S . H1 H 0.7199(4) -0.1722(3) 0.2500 0.049 Uiso 1 calc SR . C1 C 0.5760(6) -0.2547(4) 0.2500 0.0482(15) Uani 1 d S . H2 H 0.6099(6) -0.2820(4) 0.1436 0.058 Uiso 0.50 calc PR . H3 H 0.6099(6) -0.2820(4) 0.3564 0.058 Uiso 0.50 calc PR . C2 C 0.5780(4) -0.1301(3) 0.0850(6) 0.0508(11) Uani 1 d . . H4 H 0.6122(4) -0.1567(3) -0.0222(6) 0.061 Uiso 1 calc R . H5 H 0.6121(4) -0.0762(3) 0.0843(6) 0.061 Uiso 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 0.0409(5) 0.0227(5) 0.0200(5) 0.0010(2) 0.000 0.000 S1 0.0264(9) 0.0179(8) 0.0255(9) 0.000 0.000 0.000 O1 0.108(11) 0.024(2) 0.031(2) 0.002(2) 0.019(3) 0.010(3) Cl1 0.0370(8) 0.0527(9) 0.0303(8) 0.000 0.000 -0.0064(6) O2 0.035(3) 0.091(4) 0.143(5) 0.000 0.000 -0.022(3) N1 0.022(2) 0.056(3) 0.045(3) 0.000 0.000 -0.006(2) C1 0.054(3) 0.037(3) 0.054(4) 0.000 0.000 0.015(3) C2 0.059(2) 0.053(3) 0.040(2) 0.010(2) 0.010(2) -0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.275(5) 9 ? Cd1 O1 2.275(5) 4 ? Cd1 O1 2.275(5) . ? Cd1 O1 2.275(5) 12 ? Cd1 Cl1 2.6415(9) 3 ? Cd1 Cl1 2.6415(9) 9 ? Cd1 Cl1 2.6415(9) . ? Cd1 Cl1 2.6416(9) 11 ? S1 O2 1.437(5) . ? S1 O2 1.437(5) 3 ? S1 O1 1.466(5) 3 ? S1 O1 1.466(5) 12 ? S1 O1 1.466(5) 10_556 ? S1 O1 1.466(5) . ? O1 O1 0.68(2) 12 ? Cl1 Cd1 2.6415(9) 2 ? N1 C2 1.484(5) 10_556 ? N1 C2 1.484(5) . ? N1 C1 1.486(8) . ? N1 H1 0.91 . ? C1 C1 1.476(13) 3_655 ? C1 H2 0.97 . ? C1 H3 0.97 . ? C2 C2 1.515(9) 12_655 ? C2 H4 0.97 . ? C2 H5 0.97 . ? 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 17.3(4) 9 4 ? O1 Cd1 O1 180.0 9 . ? O1 Cd1 O1 162.7(4) 4 . ? O1 Cd1 O1 162.8(4) 9 12 ? O1 Cd1 O1 180.0 4 12 ? O1 Cd1 O1 17.2(4) . 12 ? O1 Cd1 Cl1 84.4(2) 9 3 ? O1 Cd1 Cl1 96.2(2) 4 3 ? O1 Cd1 Cl1 95.6(2) . 3 ? O1 Cd1 Cl1 83.8(2) 12 3 ? O1 Cd1 Cl1 83.8(2) 9 9 ? O1 Cd1 Cl1 95.6(2) 4 9 ? O1 Cd1 Cl1 96.2(2) . 9 ? O1 Cd1 Cl1 84.4(2) 12 9 ? Cl1 Cd1 Cl1 94.03(4) 3 9 ? O1 Cd1 Cl1 96.2(2) 9 . ? O1 Cd1 Cl1 84.4(2) 4 . ? O1 Cd1 Cl1 83.8(2) . . ? O1 Cd1 Cl1 95.6(2) 12 . ? Cl1 Cd1 Cl1 85.97(4) 3 . ? Cl1 Cd1 Cl1 180.0 9 . ? O1 Cd1 Cl1 95.6(2) 9 11 ? O1 Cd1 Cl1 83.8(2) 4 11 ? O1 Cd1 Cl1 84.4(2) . 11 ? O1 Cd1 Cl1 96.2(2) 12 11 ? Cl1 Cd1 Cl1 180.0 3 11 ? Cl1 Cd1 Cl1 85.97(4) 9 11 ? Cl1 Cd1 Cl1 94.03(4) . 11 ? O2 S1 O2 103.8(5) . 3 ? O2 S1 O1 99.2(3) . 3 ? O2 S1 O1 121.8(3) 3 3 ? O2 S1 O1 99.2(3) . 12 ? O2 S1 O1 121.8(3) 3 12 ? O1 S1 O1 105.8(4) 3 12 ? O2 S1 O1 121.8(3) . 10_556 ? O2 S1 O1 99.2(3) 3 10_556 ? O1 S1 O1 26.9(7) 3 10_556 ? O1 S1 O1 112.4(4) 12 10_556 ? O2 S1 O1 121.8(3) . . ? O2 S1 O1 99.2(3) 3 . ? O1 S1 O1 112.4(4) 3 . ? O1 S1 O1 26.9(7) 12 . ? O1 S1 O1 105.8(4) 10_556 . ? O1 O1 S1 76.5(3) 12 . ? O1 O1 Cd1 81.4(2) 12 . ? S1 O1 Cd1 136.6(4) . . ? Cd1 Cl1 Cd1 88.72(4) 2 . ? C2 N1 C2 110.5(5) 10_556 . ? C2 N1 C1 110.2(3) 10_556 . ? C2 N1 C1 110.2(3) . . ? C2 N1 H1 108.7(2) 10_556 . ? C2 N1 H1 108.7(2) . . ? C1 N1 H1 108.7(3) . . ? C1 C1 N1 109.2(3) 3_655 . ? C1 C1 H2 109.845(3) 3_655 . ? N1 C1 H2 109.85(14) . . ? C1 C1 H3 109.846(3) 3_655 . ? N1 C1 H3 109.85(14) . . ? H2 C1 H3 108.3 . . ? N1 C2 C2 108.4(2) . 12_655 ? N1 C2 H4 110.0(2) . . ? C2 C2 H4 110.011(3) 12_655 . ? N1 C2 H5 110.0(2) . . ? C2 C2 H5 110.011(3) 12_655 . ? H4 C2 H5 108.4 . . ? _refine_diff_density_max 0.737 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.125 #===END data_sad2 _database_code_CSD 185731 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C3 H16 Cd2 N2 O14 S3' _chemical_formula_weight 625.16 _chemical_melting_point ? _chemical_compound_source ? 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3802(4) _cell_length_b 8.6579(5) _cell_length_c 11.3254(6) _cell_angle_alpha 84.926(2) _cell_angle_beta 72.414(2) _cell_angle_gamma 75.741(2) _cell_volume 759.09(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2078 _cell_measurement_theta_min 2 _cell_measurement_theta_max 23 _exptl_crystal_description Plate _exptl_crystal_colour Transparent _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.735 _exptl_crystal_density_method ? _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 3.292 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.586679 _exptl_absorpt_correction_T_max 1.000000 _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 'Siemens CCD-diffractometer' _diffrn_measurement_method '\W' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3176 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0690 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 23.30 _reflns_number_total 2150 _reflns_number_observed 1675 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART(Siemens,1996)' _computing_cell_refinement 'SAINT(Siemens,1996)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL v5.0' _computing_publication_material 'SHELXTL v5.0' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0101(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2150 _refine_ls_number_parameters 234 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_obs 0.0360 _refine_ls_wR_factor_all 0.0855 _refine_ls_wR_factor_obs 0.0809 _refine_ls_goodness_of_fit_all 0.949 _refine_ls_goodness_of_fit_obs 1.034 _refine_ls_restrained_S_all 0.949 _refine_ls_restrained_S_obs 1.034 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd1 Cd 0.04055(7) 0.78235(6) 0.36952(5) 0.0178(2) Uani 1 d . . Cd2 Cd -0.45088(7) 0.27003(6) 0.39015(5) 0.0181(2) Uani 1 d . . S1 S -0.2033(2) 0.4922(2) 0.4455(2) 0.0151(4) Uani 1 d . . S2 S -0.2614(2) 0.3026(2) 0.1198(2) 0.0191(5) Uani 1 d . . S3 S -0.3086(2) 0.0084(2) 0.5806(2) 0.0157(4) Uani 1 d . . O1 O 0.1034(6) 0.6693(6) 0.5391(4) 0.0218(12) Uani 1 d . . O2 O 0.1803(6) 0.9803(6) 0.3566(5) 0.0268(13) Uani 1 d . . O3 O -0.2220(6) 0.9481(6) 0.4532(5) 0.0266(13) Uani 1 d . . O4 O -0.0893(6) 0.5823(6) 0.3578(5) 0.0230(12) Uani 1 d . . O5 O 0.2702(9) 0.6442(8) 0.2170(7) 0.043(2) Uani 1 d . . O6 O -0.0342(8) 0.8814(7) 0.1898(5) 0.0245(13) Uani 1 d . . O7 O -0.4214(6) 0.1681(6) 0.5726(5) 0.0220(12) Uani 1 d . . O8 O -0.3406(6) 0.4841(6) 0.3913(5) 0.0208(12) Uani 1 d . . O9 O -0.7211(6) 0.4275(6) 0.4333(4) 0.0230(12) Uani 1 d . . O10 O -0.5871(6) 0.0968(6) 0.3441(5) 0.0224(12) Uani 1 d . . O11 O -0.2168(7) 0.1848(6) 0.2173(5) 0.0309(14) Uani 1 d . . O12 O -0.4370(6) 0.3928(6) 0.1757(5) 0.0312(14) Uani 1 d . . O13 O -0.1429(7) 0.4073(7) 0.0881(5) 0.0377(15) Uani 1 d . . O14 O -0.2527(7) 0.2158(6) 0.0114(5) 0.0333(15) Uani 1 d . . N1 N -0.3125(8) -0.2729(8) 0.1927(6) 0.030(2) Uani 1 d . . H1 H -0.3882(8) -0.2645(8) 0.2677(6) 0.045 Uiso 1 calc R . H2 H -0.2133(8) -0.2578(8) 0.1975(6) 0.045 Uiso 1 calc R . H3 H -0.2955(8) -0.3695(8) 0.1634(6) 0.045 Uiso 1 calc R . C1 C -0.3795(10) -0.1514(9) 0.1089(7) 0.026(2) Uani 1 d . . H4 H -0.4002(10) -0.0467(9) 0.1425(7) 0.031 Uiso 1 calc R . H5 H -0.4889(10) -0.1670(9) 0.1058(7) 0.031 Uiso 1 calc R . C2 C -0.2585(10) -0.1567(9) -0.0215(7) 0.027(2) Uani 1 d . . H6 H -0.2917(10) -0.0573(9) -0.0642(7) 0.032 Uiso 1 calc R . H7 H -0.1428(10) -0.1654(9) -0.0172(7) 0.032 Uiso 1 calc R . C3 C -0.2576(11) -0.2929(10) -0.0957(7) 0.033(2) Uani 1 d . . H8 H -0.2272(11) -0.3928(10) -0.0529(7) 0.039 Uiso 1 calc R . H9 H -0.3718(11) -0.2826(10) -0.1038(7) 0.039 Uiso 1 calc R . N2 N -0.1334(8) -0.2941(8) -0.2197(6) 0.029(2) Uani 1 d . . H10 H -0.1344(8) -0.3752(8) -0.2624(6) 0.044 Uiso 1 calc R . H11 H -0.0285(8) -0.3049(8) -0.2123(6) 0.044 Uiso 1 calc R . H12 H -0.1623(8) -0.2030(8) -0.2594(6) 0.044 Uiso 1 calc R . H13 H 0.3582(95) 0.5587(88) 0.2226(63) 0.016(20) Uiso 1 d . . H14 H 0.2577(139) 0.6727(135) 0.1535(106) 0.070(42) Uiso 1 d . . H16 H 0.0544(174) 0.8465(153) 0.0980(140) 0.151(58) Uiso 1 d . . H17 H -0.1049(93) 0.9717(92) 0.2003(65) 0.015(21) Uiso 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 0.0208(4) 0.0181(4) 0.0147(3) 0.0000(2) -0.0031(3) -0.0075(3) Cd2 0.0195(4) 0.0198(4) 0.0143(3) -0.0013(2) -0.0012(3) -0.0077(3) S1 0.0159(10) 0.0160(10) 0.0118(10) -0.0034(8) -0.0006(8) -0.0041(8) S2 0.0202(11) 0.0186(10) 0.0148(10) 0.0007(8) -0.0023(8) -0.0015(9) S3 0.0166(10) 0.0151(10) 0.0158(10) -0.0008(8) -0.0029(8) -0.0063(9) O1 0.024(3) 0.018(3) 0.018(3) -0.003(2) -0.004(2) 0.002(2) O2 0.030(3) 0.026(3) 0.032(3) 0.008(3) -0.015(3) -0.014(3) O3 0.026(3) 0.030(3) 0.018(3) -0.003(2) 0.000(2) -0.002(3) O4 0.023(3) 0.022(3) 0.023(3) -0.004(2) -0.001(2) -0.010(2) O5 0.031(4) 0.043(4) 0.033(4) 0.005(3) 0.003(3) 0.015(3) O6 0.026(3) 0.020(3) 0.022(3) -0.001(2) -0.007(3) 0.005(3) O7 0.023(3) 0.017(3) 0.020(3) 0.000(2) -0.002(2) 0.002(2) O8 0.023(3) 0.023(3) 0.022(3) -0.001(2) -0.011(2) -0.009(2) O9 0.021(3) 0.029(3) 0.016(3) -0.007(2) -0.002(2) -0.002(2) O10 0.028(3) 0.020(3) 0.020(3) 0.001(2) -0.004(2) -0.012(2) O11 0.041(3) 0.022(3) 0.017(3) 0.002(2) 0.000(3) 0.005(3) O12 0.017(3) 0.043(4) 0.027(3) -0.012(3) -0.007(3) 0.009(3) O13 0.038(4) 0.036(4) 0.040(4) 0.006(3) -0.004(3) -0.022(3) O14 0.042(4) 0.034(4) 0.020(3) -0.007(3) -0.002(3) -0.007(3) N1 0.037(4) 0.037(4) 0.016(4) 0.003(3) -0.008(3) -0.009(4) C1 0.025(5) 0.023(5) 0.025(5) -0.008(4) -0.003(4) 0.002(4) C2 0.029(5) 0.024(4) 0.027(5) 0.004(4) -0.006(4) -0.008(4) C3 0.037(5) 0.034(5) 0.027(5) 0.003(4) -0.004(4) -0.018(4) N2 0.032(4) 0.030(4) 0.023(4) 0.000(3) -0.005(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.224(5) . ? Cd1 O2 2.274(5) . ? Cd1 O3 2.286(5) . ? Cd1 O4 2.293(5) . ? Cd1 O5 2.311(6) . ? Cd1 O6 2.339(5) . ? Cd2 O7 2.233(5) . ? Cd2 O8 2.268(4) . ? Cd2 O9 2.270(5) . ? Cd2 O10 2.273(4) . ? Cd2 O11 2.334(5) . ? Cd2 O12 2.545(6) . ? Cd2 S2 3.018(2) . ? S1 O1 1.468(5) 2_566 ? S1 O4 1.472(5) . ? S1 O8 1.476(5) . ? S1 O9 1.481(5) 2_466 ? S2 O13 1.451(5) . ? S2 O12 1.461(5) . ? S2 O14 1.469(5) . ? S2 O11 1.504(5) . ? S3 O10 1.458(5) 2_456 ? S3 O3 1.482(5) 1_545 ? S3 O2 1.482(5) 2_566 ? S3 O7 1.483(5) . ? O1 S1 1.468(5) 2_566 ? O2 S3 1.482(5) 2_566 ? O3 S3 1.482(5) 1_565 ? O5 H13 0.92(8) . ? O5 H14 0.77(11) . ? O6 H16 1.10(15) . ? O6 H17 0.85(8) . ? O9 S1 1.481(5) 2_466 ? O10 S3 1.458(5) 2_456 ? N1 C1 1.475(10) . ? N1 H1 0.89 . ? N1 H2 0.89 . ? N1 H3 0.89 . ? C1 C2 1.516(10) . ? C1 H4 0.97 . ? C1 H5 0.97 . ? C2 C3 1.504(10) . ? C2 H6 0.97 . ? C2 H7 0.97 . ? C3 N2 1.473(10) . ? C3 H8 0.97 . ? C3 H9 0.97 . ? N2 H10 0.89 . ? N2 H11 0.89 . ? N2 H12 0.89 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O2 95.0(2) . . ? O1 Cd1 O3 101.2(2) . . ? O2 Cd1 O3 92.4(2) . . ? O1 Cd1 O4 90.4(2) . . ? O2 Cd1 O4 173.3(2) . . ? O3 Cd1 O4 90.5(2) . . ? O1 Cd1 O5 100.8(2) . . ? O2 Cd1 O5 90.2(2) . . ? O3 Cd1 O5 157.5(2) . . ? O4 Cd1 O5 84.9(2) . . ? O1 Cd1 O6 175.0(2) . . ? O2 Cd1 O6 89.9(2) . . ? O3 Cd1 O6 79.4(2) . . ? O4 Cd1 O6 84.6(2) . . ? O5 Cd1 O6 78.2(3) . . ? O7 Cd2 O8 96.3(2) . . ? O7 Cd2 O9 105.4(2) . . ? O8 Cd2 O9 90.8(2) . . ? O7 Cd2 O10 99.8(2) . . ? O8 Cd2 O10 163.4(2) . . ? O9 Cd2 O10 81.1(2) . . ? O7 Cd2 O11 116.0(2) . . ? O8 Cd2 O11 86.9(2) . . ? O9 Cd2 O11 138.6(2) . . ? O10 Cd2 O11 89.7(2) . . ? O7 Cd2 O12 171.0(2) . . ? O8 Cd2 O12 77.3(2) . . ? O9 Cd2 O12 81.3(2) . . ? O10 Cd2 O12 87.1(2) . . ? O11 Cd2 O12 57.9(2) . . ? O7 Cd2 S2 144.08(13) . . ? O8 Cd2 S2 78.29(13) . . ? O9 Cd2 S2 110.16(13) . . ? O10 Cd2 S2 90.89(13) . . ? O11 Cd2 S2 29.24(13) . . ? O12 Cd2 S2 28.89(11) . . ? O1 S1 O4 108.9(3) 2_566 . ? O1 S1 O8 109.7(3) 2_566 . ? O4 S1 O8 107.4(3) . . ? O1 S1 O9 110.1(3) 2_566 2_466 ? O4 S1 O9 110.5(3) . 2_466 ? O8 S1 O9 110.2(3) . 2_466 ? O13 S2 O12 110.5(3) . . ? O13 S2 O14 111.6(3) . . ? O12 S2 O14 110.5(3) . . ? O13 S2 O11 108.8(3) . . ? O12 S2 O11 106.0(3) . . ? O14 S2 O11 109.2(3) . . ? O13 S2 Cd2 117.3(2) . . ? O12 S2 Cd2 57.3(2) . . ? O14 S2 Cd2 130.7(2) . . ? O11 S2 Cd2 49.3(2) . . ? O10 S3 O3 111.6(3) 2_456 1_545 ? O10 S3 O2 107.4(3) 2_456 2_566 ? O3 S3 O2 110.7(3) 1_545 2_566 ? O10 S3 O7 109.0(3) 2_456 . ? O3 S3 O7 108.3(3) 1_545 . ? O2 S3 O7 109.9(3) 2_566 . ? S1 O1 Cd1 128.2(3) 2_566 . ? S3 O2 Cd1 128.9(3) 2_566 . ? S3 O3 Cd1 131.3(3) 1_565 . ? S1 O4 Cd1 136.4(3) . . ? Cd1 O5 H13 130.7(44) . . ? Cd1 O5 H14 108.7(85) . . ? H13 O5 H14 120.1(94) . . ? Cd1 O6 H16 120.8(72) . . ? Cd1 O6 H17 112.6(48) . . ? H16 O6 H17 120.7(87) . . ? S3 O7 Cd2 120.6(3) . . ? S1 O8 Cd2 127.1(3) . . ? S1 O9 Cd2 118.7(3) 2_466 . ? S3 O10 Cd2 133.3(3) 2_456 . ? S2 O11 Cd2 101.5(3) . . ? S2 O12 Cd2 93.8(3) . . ? C1 N1 H1 109.5(4) . . ? C1 N1 H2 109.5(4) . . ? H1 N1 H2 109.5 . . ? C1 N1 H3 109.5(4) . . ? H1 N1 H3 109.5 . . ? H2 N1 H3 109.5 . . ? N1 C1 C2 113.2(6) . . ? N1 C1 H4 108.9(4) . . ? C2 C1 H4 108.9(4) . . ? N1 C1 H5 108.9(4) . . ? C2 C1 H5 108.9(4) . . ? H4 C1 H5 107.8 . . ? C3 C2 C1 113.4(7) . . ? C3 C2 H6 108.9(4) . . ? C1 C2 H6 108.9(4) . . ? C3 C2 H7 108.9(4) . . ? C1 C2 H7 108.9(4) . . ? H6 C2 H7 107.7 . . ? N2 C3 C2 110.5(6) . . ? N2 C3 H8 109.5(4) . . ? C2 C3 H8 109.5(5) . . ? N2 C3 H9 109.5(4) . . ? C2 C3 H9 109.5(4) . . ? H8 C3 H9 108.1 . . ? C3 N2 H10 109.5(4) . . ? C3 N2 H11 109.5(4) . . ? H10 N2 H11 109.5 . . ? C3 N2 H12 109.5(4) . . ? H10 N2 H12 109.5 . . ? H11 N2 H12 109.5 . . ? _refine_diff_density_max 1.038 _refine_diff_density_min -1.199 _refine_diff_density_rms 0.172 #===END