Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author 'Prof Xiao-Ming Chen' _publ_contact_author_address ; Chen, Xiao-Ming School of Chemistry and Chemical Engineering Zhongshan University Guangzhou, 510275 P. R. China ; _publ_contact_author_phone '86-20-84113986' _publ_contact_author_fax '86-20-84112245' _publ_contact_author_email cescxm@zsu.edu.cn _publ_requested_joiurnal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir, Please consider this CIF submission as supplementary data for a paper submitted to J. Chem. Soc., Dalton Trans. Xiao-Ming Chen ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_Cambridge 186 _journal_name_full 'J. Chem. Soc., Dalton Trans.' _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Syntheses and crystal structures of four metal-organic co-ordination networks constructed from cadmium(II) thiocyanate and nicotinic derivatives with hydrogen bonds ; loop_ _publ_author_name _publ_author_address 'Yang,Guang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Zhu, Huai-Gang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Liang, Bing-Hua' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Chen, Xiao-Ming' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; #============================================================ data_Complex_1 _database_code_CSD 152859 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H15 Cd N5 O6 S2' _chemical_formula_weight 597.89 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 7.305(5) _cell_length_b 11.625(5) _cell_length_c 14.837(5) _cell_angle_alpha 109.05(5) _cell_angle_beta 102.49(5) _cell_angle_gamma 94.14(5) _cell_volume 1148.8(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 1.180 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.787 _exptl_absorpt_correction_T_max 0.923 _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 R3m _diffrn_measurement_method /w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6165 _diffrn_reflns_av_R_equivalents 0.0085 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 29.94 _reflns_number_total 6147 _reflns_number_gt 4473 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL Version 5 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.4358P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6147 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.5000 0.5000 0.5000 0.03144(9) Uani 1 d S . . Cd2 Cd 0.5000 0.0000 0.5000 0.03122(9) Uani 1 d S . . S1 S 0.73983(15) 0.35825(8) 0.41662(8) 0.0548(3) Uani 1 d . . . S2 S 0.19419(11) 0.11654(7) 0.52977(6) 0.03664(17) Uani 1 d . . . O1 O 0.4444(3) 0.4807(3) 0.87281(17) 0.0535(7) Uani 1 d . . . O2 O 0.7216(3) 0.5374(2) 0.98654(16) 0.0488(6) Uani 1 d . . . O3 O 0.4049(3) 0.1700(2) 0.88425(16) 0.0482(6) Uani 1 d . . . O4 O 0.6706(3) 0.2668(2) 1.00110(16) 0.0478(6) Uani 1 d . . . O5 O 0.4264(4) 0.1058(3) 1.1130(2) 0.0783(10) Uani 1 d . . . H5A H 0.5019 0.1159 1.0790 0.080 Uiso 1 d R . . O6 O 0.2261(4) 0.1720(3) 1.01116(19) 0.0563(7) Uani 1 d . . . N1 N 0.6209(4) 0.1350(3) 0.4347(2) 0.0484(7) Uani 1 d . . . N2 N 0.3142(4) 0.3399(3) 0.5111(2) 0.0477(7) Uani 1 d . . . N3 N 0.6892(4) 0.5247(3) 0.65938(19) 0.0414(6) Uani 1 d . . . N4 N 0.6667(4) 0.1279(3) 0.66098(18) 0.0371(6) Uani 1 d . . . N5 N -0.2024(4) 0.1183(3) 1.1363(2) 0.0406(6) Uani 1 d . . . C1 C 0.6689(4) 0.2276(3) 0.4280(2) 0.0344(7) Uani 1 d . . . C2 C 0.2671(4) 0.2486(3) 0.5202(2) 0.0313(6) Uani 1 d . . . C3 C 0.8785(5) 0.5489(3) 0.6800(2) 0.0448(8) Uani 1 d . . . H3A H 0.9340 0.5567 0.6311 0.067 Uiso 1 d R . . C4 C 0.9957(5) 0.5628(3) 0.7710(3) 0.0478(9) Uani 1 d . . . H4 H 1.1268 0.5798 0.7826 0.072 Uiso 1 d R . . C5 C 0.9150(5) 0.5515(3) 0.8442(2) 0.0431(8) Uani 1 d . . . H5 H 0.9906 0.5596 0.9057 0.065 Uiso 1 d R . . C6 C 0.7180(4) 0.5275(3) 0.8242(2) 0.0348(6) Uani 1 d . . . C7 C 0.6114(4) 0.5145(3) 0.7311(2) 0.0383(7) Uani 1 d . . . H7 H 0.4800 0.4980 0.7177 0.057 Uiso 1 d R . . C8 C 0.6239(5) 0.5159(3) 0.9012(2) 0.0368(7) Uani 1 d . . . C9 C 0.8499(5) 0.1742(3) 0.6826(2) 0.0430(8) Uani 1 d . . . H9 H 0.9070 0.1664 0.6310 0.064 Uiso 1 d R . . C10 C 0.9580(5) 0.2334(3) 0.7774(3) 0.0473(8) Uani 1 d . . . H10 H 1.0857 0.2637 0.7894 0.071 Uiso 1 d R . . C11 C 0.8738(5) 0.2476(3) 0.8549(2) 0.0423(8) Uani 1 d . . . H11 H 0.9441 0.2864 0.9199 0.063 Uiso 1 d R . . C12 C 0.6815(4) 0.2019(3) 0.8332(2) 0.0322(6) Uani 1 d . . . C13 C 0.5848(4) 0.1424(3) 0.7356(2) 0.0338(6) Uani 1 d . . . H13 H 0.4569 0.1112 0.7211 0.051 Uiso 1 d R . . C14 C 0.5852(4) 0.2166(3) 0.9154(2) 0.0350(7) Uani 1 d . . . C15 C -0.1673(5) 0.1010(3) 1.2228(2) 0.0442(8) Uani 1 d . . . H15 H -0.2666 0.0914 1.2510 0.066 Uiso 1 d R . . C16 C 0.0141(5) 0.0972(4) 1.2700(2) 0.0493(9) Uani 1 d . . . C17 C 0.1597(5) 0.1089(3) 1.2260(2) 0.0428(8) Uani 1 d . . . H17 H 0.2832 0.1055 1.2570 0.064 Uiso 1 d R . . C18 C 0.1220(4) 0.1252(3) 1.1356(2) 0.0324(6) Uani 1 d . . . C19 C -0.0617(4) 0.1306(3) 1.0931(2) 0.0396(7) Uani 1 d . . . H19 H -0.0898 0.1430 1.0331 0.059 Uiso 1 d R . . C20 C 0.2742(4) 0.1374(3) 1.0827(2) 0.0415(8) Uani 1 d . . . H1 H 0.4044 0.4734 0.9195 0.050 Uiso 1 d . . . H3 H 0.3501 0.1834 0.9352 0.050 Uiso 1 d . . . H16 H 0.0541 0.0938 1.3381 0.050 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 0.03763(18) 0.03144(17) 0.02912(16) 0.01387(13) 0.01264(13) 0.00131(13) Cd2 0.03958(18) 0.03112(17) 0.02732(16) 0.01251(13) 0.01406(13) 0.00488(13) S1 0.0660(6) 0.0378(5) 0.0824(7) 0.0266(5) 0.0534(6) 0.0118(4) S2 0.0363(4) 0.0357(4) 0.0484(5) 0.0220(3) 0.0206(4) 0.0064(3) O1 0.0409(13) 0.088(2) 0.0345(12) 0.0236(13) 0.0160(10) 0.0005(13) O2 0.0479(14) 0.0711(17) 0.0299(12) 0.0221(12) 0.0097(10) 0.0049(12) O3 0.0367(12) 0.0749(18) 0.0326(12) 0.0152(11) 0.0162(10) 0.0004(12) O4 0.0449(13) 0.0650(16) 0.0287(12) 0.0112(11) 0.0091(10) 0.0051(12) O5 0.0324(14) 0.140(3) 0.095(2) 0.067(2) 0.0378(15) 0.0307(16) O6 0.0474(14) 0.087(2) 0.0572(16) 0.0401(15) 0.0322(13) 0.0205(14) N1 0.0598(19) 0.0432(17) 0.0603(19) 0.0279(15) 0.0349(16) 0.0152(14) N2 0.0472(17) 0.0375(16) 0.064(2) 0.0209(14) 0.0231(15) 0.0024(13) N3 0.0383(14) 0.0568(18) 0.0323(14) 0.0201(13) 0.0110(11) 0.0001(13) N4 0.0343(13) 0.0469(16) 0.0291(13) 0.0093(11) 0.0133(11) 0.0039(12) N5 0.0286(13) 0.0541(17) 0.0409(15) 0.0138(13) 0.0160(11) 0.0094(12) C1 0.0376(16) 0.0364(17) 0.0357(16) 0.0143(13) 0.0185(13) 0.0097(13) C2 0.0276(14) 0.0342(16) 0.0353(16) 0.0131(13) 0.0132(12) 0.0045(12) C3 0.0379(17) 0.060(2) 0.0398(18) 0.0187(16) 0.0170(14) -0.0020(16) C4 0.0343(17) 0.061(2) 0.047(2) 0.0191(17) 0.0099(15) -0.0011(16) C5 0.0393(18) 0.053(2) 0.0347(17) 0.0153(15) 0.0063(14) 0.0030(15) C6 0.0388(16) 0.0391(17) 0.0296(15) 0.0142(13) 0.0122(13) 0.0051(13) C7 0.0357(16) 0.051(2) 0.0330(16) 0.0185(14) 0.0139(13) 0.0030(14) C8 0.0422(17) 0.0411(18) 0.0310(15) 0.0154(13) 0.0127(13) 0.0067(14) C9 0.0369(17) 0.054(2) 0.0410(18) 0.0150(16) 0.0207(14) 0.0035(15) C10 0.0297(16) 0.059(2) 0.049(2) 0.0120(17) 0.0150(15) -0.0016(15) C11 0.0362(17) 0.048(2) 0.0357(17) 0.0074(14) 0.0069(14) 0.0007(14) C12 0.0347(15) 0.0351(16) 0.0280(14) 0.0102(12) 0.0114(12) 0.0067(12) C13 0.0318(15) 0.0398(17) 0.0299(15) 0.0107(13) 0.0117(12) 0.0019(13) C14 0.0363(16) 0.0407(17) 0.0314(15) 0.0134(13) 0.0128(13) 0.0097(13) C15 0.0428(18) 0.051(2) 0.0426(18) 0.0121(15) 0.0270(15) 0.0046(15) C16 0.055(2) 0.063(2) 0.0339(17) 0.0202(16) 0.0135(16) 0.0068(18) C17 0.0340(17) 0.055(2) 0.0398(18) 0.0181(16) 0.0061(14) 0.0094(15) C18 0.0277(14) 0.0379(16) 0.0362(15) 0.0147(13) 0.0142(12) 0.0079(12) C19 0.0321(16) 0.057(2) 0.0360(16) 0.0197(15) 0.0144(13) 0.0134(14) C20 0.0283(16) 0.053(2) 0.0434(18) 0.0131(15) 0.0166(14) 0.0052(14) _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 N2 2.294(3) . ? Cd1 N2 2.294(3) 2_666 ? Cd1 N3 2.381(3) 2_666 ? Cd1 N3 2.381(3) . ? Cd1 S1 2.7090(19) 2_666 ? Cd1 S1 2.7090(19) . ? Cd2 N1 2.311(3) 2_656 ? Cd2 N1 2.311(3) . ? Cd2 N4 2.358(3) . ? Cd2 N4 2.358(3) 2_656 ? Cd2 S2 2.7375(19) 2_656 ? Cd2 S2 2.7375(19) . ? S1 C1 1.642(3) . ? S2 C2 1.649(3) . ? O1 C8 1.279(4) . ? O1 O2 2.686(3) 2_667 ? O2 C8 1.246(4) . ? O3 C14 1.309(4) . ? O3 O6 2.508(3) . ? O4 C14 1.211(4) . ? O5 C20 1.234(4) . ? O5 N5 2.645(4) 1_655 ? O6 C20 1.244(4) . ? N1 C1 1.150(4) . ? N2 C2 1.150(4) . ? N3 C3 1.338(4) . ? N3 C7 1.343(4) . ? N4 C9 1.335(4) . ? N4 C13 1.338(4) . ? N5 C15 1.336(4) . ? N5 C19 1.346(4) . ? C3 C4 1.385(5) . ? C4 C5 1.381(5) . ? C5 C6 1.392(5) . ? C6 C7 1.384(4) . ? C6 C8 1.491(4) . ? C9 C10 1.372(5) . ? C10 C11 1.388(4) . ? C11 C12 1.394(4) . ? C12 C13 1.382(4) . ? C12 C14 1.504(4) . ? C15 C16 1.370(5) . ? C16 C17 1.383(5) . ? C17 C18 1.387(4) . ? C18 C19 1.369(4) . ? C18 C20 1.517(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 N2 180.0 . 2_666 ? N2 Cd1 N3 92.70(12) . 2_666 ? N2 Cd1 N3 87.30(12) 2_666 2_666 ? N2 Cd1 N3 87.30(12) . . ? N2 Cd1 N3 92.70(12) 2_666 . ? N3 Cd1 N3 180.0 2_666 . ? N2 Cd1 S1 85.11(9) . 2_666 ? N2 Cd1 S1 94.89(9) 2_666 2_666 ? N3 Cd1 S1 89.90(9) 2_666 2_666 ? N3 Cd1 S1 90.10(9) . 2_666 ? N2 Cd1 S1 94.89(9) . . ? N2 Cd1 S1 85.11(9) 2_666 . ? N3 Cd1 S1 90.10(9) 2_666 . ? N3 Cd1 S1 89.90(9) . . ? S1 Cd1 S1 180.0 2_666 . ? N1 Cd2 N1 180.0 2_656 . ? N1 Cd2 N4 89.04(11) 2_656 . ? N1 Cd2 N4 90.96(11) . . ? N1 Cd2 N4 90.96(11) 2_656 2_656 ? N1 Cd2 N4 89.04(11) . 2_656 ? N4 Cd2 N4 180.0 . 2_656 ? N1 Cd2 S2 94.15(8) 2_656 2_656 ? N1 Cd2 S2 85.85(8) . 2_656 ? N4 Cd2 S2 92.10(9) . 2_656 ? N4 Cd2 S2 87.90(9) 2_656 2_656 ? N1 Cd2 S2 85.85(8) 2_656 . ? N1 Cd2 S2 94.15(8) . . ? N4 Cd2 S2 87.90(9) . . ? N4 Cd2 S2 92.10(9) 2_656 . ? S2 Cd2 S2 180.0 2_656 . ? C1 S1 Cd1 100.24(12) . . ? C2 S2 Cd2 99.49(11) . . ? C8 O1 O2 115.4(2) . 2_667 ? C14 O3 O6 117.8(2) . . ? C20 O5 N5 150.8(3) . 1_655 ? C20 O6 O3 127.2(2) . . ? C1 N1 Cd2 158.4(3) . . ? C2 N2 Cd1 161.6(3) . . ? C3 N3 C7 117.7(3) . . ? C3 N3 Cd1 120.5(2) . . ? C7 N3 Cd1 121.8(2) . . ? C9 N4 C13 118.0(3) . . ? C9 N4 Cd2 121.7(2) . . ? C13 N4 Cd2 119.7(2) . . ? C15 N5 C19 121.0(3) . . ? N1 C1 S1 178.7(3) . . ? N2 C2 S2 178.1(3) . . ? N3 C3 C4 123.0(3) . . ? C5 C4 C3 119.0(3) . . ? C4 C5 C6 118.7(3) . . ? C7 C6 C5 118.6(3) . . ? C7 C6 C8 120.7(3) . . ? C5 C6 C8 120.7(3) . . ? N3 C7 C6 123.0(3) . . ? O2 C8 O1 124.3(3) . . ? O2 C8 C6 119.6(3) . . ? O1 C8 C6 116.1(3) . . ? N4 C9 C10 123.1(3) . . ? C9 C10 C11 119.0(3) . . ? C10 C11 C12 118.5(3) . . ? C13 C12 C11 118.4(3) . . ? C13 C12 C14 121.7(3) . . ? C11 C12 C14 119.9(3) . . ? N4 C13 C12 123.0(3) . . ? O4 C14 O3 124.9(3) . . ? O4 C14 C12 121.8(3) . . ? O3 C14 C12 113.3(3) . . ? N5 C15 C16 120.4(3) . . ? C15 C16 C17 119.1(3) . . ? C16 C17 C18 120.2(3) . . ? C19 C18 C17 117.8(3) . . ? C19 C18 C20 119.2(3) . . ? C17 C18 C20 123.0(3) . . ? N5 C19 C18 121.5(3) . . ? O5 C20 O6 128.4(3) . . ? O5 C20 C18 115.8(3) . . ? O6 C20 C18 115.7(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O2 0.83 1.86 2.686(3) 170.7 2_667 O3 H3 O6 0.91 1.62 2.508(3) 165.6 . O5 H5A N5 0.85 2.14 2.645(4) 118.0 1_655 _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 29.94 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.656 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.076 #=========================end data_Complex_2 _database_code_CSD 152860 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H14 Cd N6 O3 S2' _chemical_formula_weight 490.83 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 24.290(12) _cell_length_b 9.863(4) _cell_length_c 7.617(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.67 _cell_angle_gamma 90.00 _cell_volume 1822.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description polyhedra _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.789 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 1.455 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.642 _exptl_absorpt_correction_T_max 0.694 _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 'Siemens R3m' _diffrn_measurement_method \w-scan _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 2025 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 26.98 _reflns_number_total 1981 _reflns_number_gt 1581 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL Version 5 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+5.7409P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0013(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1981 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.2500 0.2500 0.0000 0.03175(16) Uani 1 d S . . S1 S 0.31536(5) 0.20530(12) 0.30118(15) 0.0456(3) Uani 1 d . . . C1 C 0.28275(15) 0.0727(4) 0.3769(5) 0.0322(8) Uani 1 d . . . N1 N 0.26086(16) -0.0221(3) 0.4299(5) 0.0445(8) Uani 1 d . . . N2 N 0.16960(13) 0.1970(4) 0.1454(4) 0.0350(7) Uani 1 d . . . C2 C 0.15309(17) 0.0681(4) 0.1521(5) 0.0398(9) Uani 1 d . . . H2 H 0.1749 -0.0001 0.0984 0.080 Uiso 1 d R . . C3 C 0.10605(18) 0.0291(4) 0.2337(6) 0.0465(10) Uani 1 d . . . H3 H 0.0957 -0.0648 0.2377 0.080 Uiso 1 d R . . C4 C 0.07458(17) 0.1264(4) 0.3109(5) 0.0418(10) Uani 1 d . . . H4 H 0.0417 0.1015 0.3680 0.080 Uiso 1 d R . . C5 C 0.09102(15) 0.2615(4) 0.3056(5) 0.0340(8) Uani 1 d . . . C6 C 0.13881(16) 0.2912(4) 0.2223(5) 0.0366(8) Uani 1 d . . . H6 H 0.1504 0.3841 0.2177 0.080 Uiso 1 d R . . C7 C 0.05604(17) 0.3657(5) 0.3906(5) 0.0409(9) Uani 1 d . . . O1 O 0.01579(13) 0.3292(3) 0.4717(5) 0.0579(9) Uani 1 d . . . N3 N 0.06868(15) 0.4954(4) 0.3763(5) 0.0526(10) Uani 1 d . . . H3NA H 0.1006 0.5275 0.3309 0.050 Uiso 1 d R . . H3NB H 0.0470 0.5632 0.4198 0.050 Uiso 1 d R . . O1W O 0.0000 0.1555(8) 0.7500 0.110(2) Uiso 1 d S . . H1WB H -0.0059 0.2064 0.8534 0.080 Uiso 1 d 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 0.0344(2) 0.0251(2) 0.0370(2) 0.00005(16) 0.01387(14) 0.00448(16) S1 0.0512(6) 0.0369(5) 0.0480(6) 0.0129(5) -0.0059(5) -0.0154(5) C1 0.0355(19) 0.0286(18) 0.0327(18) 0.0021(15) 0.0041(15) 0.0029(15) N1 0.054(2) 0.0308(18) 0.050(2) 0.0075(16) 0.0142(17) -0.0043(16) N2 0.0376(18) 0.0323(16) 0.0360(16) 0.0019(13) 0.0112(14) 0.0055(14) C2 0.040(2) 0.036(2) 0.044(2) -0.0002(17) 0.0107(17) 0.0055(17) C3 0.043(2) 0.034(2) 0.064(3) -0.003(2) 0.016(2) 0.0005(18) C4 0.035(2) 0.049(3) 0.042(2) 0.0002(19) 0.0113(17) 0.0012(18) C5 0.0322(18) 0.037(2) 0.0334(17) -0.0011(16) 0.0080(14) 0.0041(16) C6 0.0328(19) 0.036(2) 0.042(2) -0.0021(16) 0.0132(16) 0.0039(16) C7 0.032(2) 0.050(3) 0.042(2) -0.0066(18) 0.0114(17) 0.0068(18) O1 0.0491(18) 0.055(2) 0.072(2) -0.0080(17) 0.0342(16) 0.0024(15) N3 0.045(2) 0.041(2) 0.074(3) -0.0092(18) 0.0302(19) 0.0057(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.328(3) 6 ? Cd1 N1 2.328(3) 4 ? Cd1 N2 2.349(3) 7 ? Cd1 N2 2.349(3) . ? Cd1 S1 2.7637(14) 7 ? Cd1 S1 2.7637(14) . ? S1 C1 1.647(4) . ? C1 N1 1.158(5) . ? N1 Cd1 2.328(3) 4_545 ? N2 C2 1.335(5) . ? N2 C6 1.344(5) . ? C2 C3 1.381(6) . ? C3 C4 1.375(6) . ? C4 C5 1.392(6) . ? C5 C6 1.380(5) . ? C5 C7 1.499(5) . ? C7 O1 1.234(5) . ? C7 N3 1.322(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N1 180.0 6 4 ? N1 Cd1 N2 90.07(12) 6 7 ? N1 Cd1 N2 89.93(13) 4 7 ? N1 Cd1 N2 89.93(13) 6 . ? N1 Cd1 N2 90.07(13) 4 . ? N2 Cd1 N2 180.0 7 . ? N1 Cd1 S1 91.75(10) 6 7 ? N1 Cd1 S1 88.25(10) 4 7 ? N2 Cd1 S1 91.79(9) 7 7 ? N2 Cd1 S1 88.21(9) . 7 ? N1 Cd1 S1 88.25(10) 6 . ? N1 Cd1 S1 91.75(10) 4 . ? N2 Cd1 S1 88.21(9) 7 . ? N2 Cd1 S1 91.79(9) . . ? S1 Cd1 S1 180.0 7 . ? C1 S1 Cd1 98.64(14) . . ? N1 C1 S1 178.5(4) . . ? C1 N1 Cd1 156.7(3) . 4_545 ? C2 N2 C6 117.9(3) . . ? C2 N2 Cd1 119.2(2) . . ? C6 N2 Cd1 122.9(3) . . ? N2 C2 C3 122.6(4) . . ? C4 C3 C2 119.1(4) . . ? C3 C4 C5 119.3(4) . . ? C6 C5 C4 117.7(4) . . ? C6 C5 C7 124.0(4) . . ? C4 C5 C7 118.3(3) . . ? N2 C6 C5 123.4(4) . . ? O1 C7 N3 121.0(4) . . ? O1 C7 C5 119.6(4) . . ? N3 C7 C5 119.3(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3NB O1 0.92 2.06 2.960(4) 164.2 5_566 O1W H1WB O1 0.95 1.82 2.766(6) 170.3 2_556 _diffrn_measured_fraction_theta_max 0.471 _diffrn_reflns_theta_full 26.98 _diffrn_measured_fraction_theta_full 0.471 _refine_diff_density_max 0.450 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.087 #==========================end data_CdinaSCN (3) _database_code_CSD 152861 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 Cd N6 O2 S2' _chemical_formula_weight 472.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.786(10) _cell_length_b 9.667(4) _cell_length_c 8.112(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.62 _cell_angle_gamma 90.00 _cell_volume 880.9(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.783 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 1.497 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.658 _exptl_absorpt_correction_T_max 0.981 _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 'Siemens R3m' _diffrn_measurement_method \w-scan _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 1359 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0141 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 29.98 _reflns_number_total 1193 _reflns_number_gt 1041 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+1.0368P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.069(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1193 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0781 _refine_ls_wR_factor_gt 0.0750 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.0000 0.0000 0.0000 0.0292(4) Uani 1 d S . . S1 S -0.14309(10) -0.04246(12) -0.3331(2) 0.0468(7) Uani 1 d . . . O1 O -0.5356(3) 0.2810(3) 0.1474(6) 0.0571(15) Uani 1 d . . . N1 N -0.0257(3) -0.2654(3) -0.4312(7) 0.0416(15) Uani 1 d . . . N2 N -0.1680(2) 0.0607(3) 0.0794(6) 0.0267(15) Uani 1 d . . . N3 N -0.54886(17) 0.0702(2) 0.2575(4) 0.0473(18) Uani 1 d . . . H1N H -0.5364 0.0004 0.2590 0.050 Uiso 1 d R . . H2N H -0.6051 0.1177 0.2916 0.050 Uiso 1 d R . . C1 C -0.07291(17) -0.1732(2) -0.3889(4) 0.0299(16) Uani 1 d R . . C2 C -0.22022(17) 0.1857(2) 0.0376(4) 0.0343(16) Uani 1 d R . . H2 H -0.1844 0.2517 -0.0199 0.080 Uiso 1 d R . . C3 C -0.3255(3) 0.2193(4) 0.0734(7) 0.0326(17) Uani 1 d . . . H3 H -0.3613 0.3083 0.0403 0.080 Uiso 1 d R . . C4 C -0.3790(3) 0.1246(3) 0.1533(7) 0.0241(16) Uani 1 d . . . C5 C -0.3225(4) -0.0010(3) 0.2016(10) 0.045(3) Uani 1 d . . . H5 H -0.3539 -0.0663 0.2656 0.080 Uiso 1 d R . . C6 C -0.2178(4) -0.0280(4) 0.1627(9) 0.043(2) Uani 1 d . . . H6 H -0.1789 -0.1153 0.1969 0.080 Uiso 1 d R . . C7 C -0.4947(3) 0.1646(4) 0.1869(7) 0.039(2) Uani 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 0.03021(19) 0.02510(19) 0.0390(10) 0.0015(2) 0.0205(2) 0.00109(11) S1 0.0493(5) 0.0435(5) 0.043(2) -0.0102(8) 0.0070(7) 0.0173(4) O1 0.0515(15) 0.0432(14) 0.089(5) 0.002(2) 0.039(2) 0.0141(13) N1 0.0507(17) 0.0315(14) 0.052(5) -0.005(2) 0.030(2) -0.0003(13) N2 0.0310(12) 0.0310(14) 0.025(5) 0.0021(19) 0.0185(17) 0.0027(10) N3 0.0431(16) 0.0398(17) 0.073(6) -0.007(2) 0.038(2) 0.0013(13) C1 0.0404(16) 0.0282(14) 0.023(5) 0.000(2) 0.012(2) -0.0028(13) C2 0.0366(16) 0.0324(15) 0.040(5) 0.006(2) 0.020(2) 0.0032(13) C3 0.0388(16) 0.0310(14) 0.032(5) 0.002(2) 0.017(2) 0.0079(13) C4 0.0302(14) 0.0324(14) 0.014(5) -0.003(2) 0.0138(18) 0.0004(12) C5 0.047(2) 0.0335(17) 0.068(9) 0.007(2) 0.037(3) 0.0044(14) C6 0.047(2) 0.0355(17) 0.058(7) 0.016(3) 0.035(3) 0.0132(15) C7 0.0335(16) 0.0376(17) 0.049(6) -0.009(3) 0.019(2) 0.0012(13) _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 N2 2.334(4) 3 ? Cd1 N2 2.334(4) . ? Cd1 N1 2.376(3) 2_554 ? Cd1 N1 2.376(3) 4_556 ? Cd1 S1 2.749(2) . ? Cd1 S1 2.749(2) 3 ? S1 C1 1.647(3) . ? O1 C7 1.228(5) . ? N1 C1 1.157(4) . ? N1 Cd1 2.376(3) 2_544 ? N2 C6 1.333(6) . ? N2 C2 1.352(3) . ? N3 C7 1.338(5) . ? C2 C3 1.396(4) . ? C3 C4 1.380(6) . ? C4 C5 1.383(5) . ? C4 C7 1.520(5) . ? C5 C6 1.387(7) . ? 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 N2 Cd1 N2 180.0 3 . ? N2 Cd1 N1 89.78(12) 3 2_554 ? N2 Cd1 N1 90.22(12) . 2_554 ? N2 Cd1 N1 90.22(12) 3 4_556 ? N2 Cd1 N1 89.78(12) . 4_556 ? N1 Cd1 N1 180.0 2_554 4_556 ? N2 Cd1 S1 90.59(11) 3 . ? N2 Cd1 S1 89.41(11) . . ? N1 Cd1 S1 89.74(12) 2_554 . ? N1 Cd1 S1 90.26(12) 4_556 . ? N2 Cd1 S1 89.41(11) 3 3 ? N2 Cd1 S1 90.59(11) . 3 ? N1 Cd1 S1 90.26(12) 2_554 3 ? N1 Cd1 S1 89.74(12) 4_556 3 ? S1 Cd1 S1 180.0 . 3 ? C1 S1 Cd1 100.08(11) . . ? C1 N1 Cd1 155.8(3) . 2_544 ? C6 N2 C2 117.7(3) . . ? C6 N2 Cd1 121.3(2) . . ? C2 N2 Cd1 121.0(2) . . ? N1 C1 S1 178.5(3) . . ? N2 C2 C3 121.5(3) . . ? C4 C3 C2 120.3(3) . . ? C3 C4 C5 117.8(4) . . ? C3 C4 C7 118.5(3) . . ? C5 C4 C7 123.6(4) . . ? C4 C5 C6 119.0(5) . . ? N2 C6 C5 123.6(4) . . ? O1 C7 N3 122.5(4) . . ? O1 C7 C4 119.3(4) . . ? N3 C7 C4 118.3(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H1N O1 0.69 2.33 2.989(4) 162.3 2_445 _diffrn_measured_fraction_theta_max 0.440 _diffrn_reflns_theta_full 29.98 _diffrn_measured_fraction_theta_full 0.440 _refine_diff_density_max 0.505 _refine_diff_density_min -0.821 _refine_diff_density_rms 0.068 #=========================end data_Complex_4 _database_code_CSD 152862 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H6 Cd N2 O3 S' _chemical_formula_weight 310.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.052(2) _cell_length_b 14.763(8) _cell_length_c 11.423(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.26 _cell_angle_gamma 90.00 _cell_volume 1017.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description prism _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.027 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 2.332 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.630 _exptl_absorpt_correction_T_max 0.697 _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 'Siemens R3m' _diffrn_measurement_method \w-scan _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 3223 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 30.00 _reflns_number_total 2972 _reflns_number_gt 2398 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+0.1537P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0075(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2972 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1121 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.16848(4) 0.013642(19) 0.28654(2) 0.03056(12) Uani 1 d . . . S1 S 0.40523(19) -0.08932(10) 0.16185(12) 0.0572(4) Uani 1 d . . . C1 C 0.6503(7) -0.0644(3) 0.2277(4) 0.0368(8) Uani 1 d . . . N1 N 0.8226(6) -0.0499(3) 0.2716(4) 0.0490(9) Uani 1 d . . . N2 N 0.0370(6) 0.1200(2) 0.1455(3) 0.0373(7) Uani 1 d . . . C2 C 0.1526(7) 0.1471(3) 0.0565(4) 0.0412(9) Uani 1 d . . . H2A H 0.2874 0.1156 0.0434 0.080 Uiso 1 d R . . C3 C 0.0869(7) 0.2181(3) -0.0174(4) 0.0420(10) Uani 1 d . . . H3A H 0.1761 0.2368 -0.0791 0.080 Uiso 1 d R . . C4 C -0.1144(6) 0.2624(3) 0.0002(3) 0.0310(7) Uani 1 d . . . C5 C -0.2371(7) 0.2327(3) 0.0912(4) 0.0348(8) Uani 1 d . . . H5A H -0.3762 0.2605 0.1049 0.080 Uiso 1 d R . . C6 C -0.1535(7) 0.1621(3) 0.1620(4) 0.0387(9) Uani 1 d . . . H6A H -0.2367 0.1422 0.2256 0.080 Uiso 1 d R . . C7 C -0.1946(7) 0.3404(3) -0.0764(3) 0.0335(8) Uani 1 d . . . O1 O -0.0562(5) 0.3851(2) -0.1308(3) 0.0418(7) Uani 1 d . . . O2 O -0.3989(5) 0.3588(2) -0.0839(3) 0.0395(6) Uani 1 d . . . O1W O 0.2156(6) -0.0683(3) 0.4566(3) 0.0532(9) Uani 1 d . . . H1W H 0.2391 -0.0226 0.5146 0.080 Uiso 1 d R . . H2W H 0.3375 -0.0745 0.4971 0.080 Uiso 1 d 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 0.02782(16) 0.03220(18) 0.03106(17) -0.00047(10) -0.00184(10) 0.00026(10) S1 0.0315(5) 0.0761(9) 0.0630(8) -0.0383(7) -0.0033(5) 0.0030(5) C1 0.0316(19) 0.035(2) 0.044(2) -0.0022(16) 0.0062(16) 0.0013(15) N1 0.0346(19) 0.048(2) 0.064(3) 0.003(2) -0.0003(17) -0.0049(17) N2 0.0369(17) 0.0377(18) 0.0373(17) 0.0040(14) 0.0016(14) 0.0036(14) C2 0.038(2) 0.043(2) 0.043(2) 0.0055(18) 0.0080(17) 0.0106(18) C3 0.037(2) 0.046(2) 0.044(2) 0.0101(18) 0.0114(17) 0.0090(18) C4 0.0310(18) 0.0333(19) 0.0281(17) 0.0014(14) -0.0018(14) 0.0007(14) C5 0.0318(18) 0.036(2) 0.0365(19) 0.0031(15) 0.0039(15) 0.0051(15) C6 0.038(2) 0.046(2) 0.0331(19) 0.0041(17) 0.0073(16) 0.0075(17) C7 0.0348(19) 0.036(2) 0.0293(17) 0.0010(15) -0.0017(14) 0.0010(15) O1 0.0338(15) 0.0429(17) 0.0485(17) 0.0143(13) 0.0023(12) 0.0010(12) O2 0.0333(14) 0.0431(16) 0.0417(15) 0.0050(12) 0.0005(12) 0.0046(12) O1W 0.0414(18) 0.070(2) 0.0467(17) 0.0252(17) -0.0036(14) 0.0000(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 O1W 2.288(3) . ? Cd1 N1 2.289(4) 1_455 ? Cd1 N2 2.346(3) . ? Cd1 O1 2.381(3) 4_666 ? Cd1 O2 2.448(3) 4_666 ? Cd1 S1 2.5875(14) . ? Cd1 C7 2.754(4) 4_666 ? S1 C1 1.654(4) . ? C1 N1 1.143(5) . ? N1 Cd1 2.289(4) 1_655 ? N2 C6 1.335(5) . ? N2 C2 1.338(5) . ? C2 C3 1.386(6) . ? C3 C4 1.410(6) . ? C4 C5 1.392(5) . ? C4 C7 1.505(5) . ? C5 C6 1.391(6) . ? C7 O2 1.263(5) . ? C7 O1 1.265(5) . ? C7 Cd1 2.754(4) 4_565 ? O1 Cd1 2.381(3) 4_565 ? O2 Cd1 2.448(3) 4_565 ? 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 O1W Cd1 N1 84.38(14) . 1_455 ? O1W Cd1 N2 162.05(13) . . ? N1 Cd1 N2 87.80(14) 1_455 . ? O1W Cd1 O1 87.47(13) . 4_666 ? N1 Cd1 O1 153.67(14) 1_455 4_666 ? N2 Cd1 O1 92.51(12) . 4_666 ? O1W Cd1 O2 84.77(13) . 4_666 ? N1 Cd1 O2 99.66(13) 1_455 4_666 ? N2 Cd1 O2 80.64(12) . 4_666 ? O1 Cd1 O2 54.58(10) 4_666 4_666 ? O1W Cd1 S1 96.76(11) . . ? N1 Cd1 S1 105.00(12) 1_455 . ? N2 Cd1 S1 100.87(10) . . ? O1 Cd1 S1 100.79(8) 4_666 . ? O2 Cd1 S1 155.32(7) 4_666 . ? O1W Cd1 C7 85.27(14) . 4_666 ? N1 Cd1 C7 126.72(14) 1_455 4_666 ? N2 Cd1 C7 86.52(13) . 4_666 ? O1 Cd1 C7 27.30(11) 4_666 4_666 ? O2 Cd1 C7 27.29(10) 4_666 4_666 ? S1 Cd1 C7 128.09(9) . 4_666 ? C1 S1 Cd1 97.67(15) . . ? N1 C1 S1 177.5(4) . . ? C1 N1 Cd1 155.3(4) . 1_655 ? C6 N2 C2 118.3(4) . . ? C6 N2 Cd1 117.8(3) . . ? C2 N2 Cd1 123.5(3) . . ? N2 C2 C3 123.1(4) . . ? C2 C3 C4 118.4(4) . . ? C5 C4 C3 118.3(4) . . ? C5 C4 C7 120.6(3) . . ? C3 C4 C7 121.1(4) . . ? C6 C5 C4 118.6(4) . . ? N2 C6 C5 123.2(4) . . ? O2 C7 O1 122.4(4) . . ? O2 C7 C4 118.4(4) . . ? O1 C7 C4 119.2(3) . . ? O2 C7 Cd1 62.7(2) . 4_565 ? O1 C7 Cd1 59.7(2) . 4_565 ? C4 C7 Cd1 178.3(3) . 4_565 ? C7 O1 Cd1 93.0(2) . 4_565 ? C7 O2 Cd1 90.0(2) . 4_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H2W O1 0.85 2.03 2.842(4) 159.1 2_545 _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.569 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.143 #==================================end