# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Jie-Hui Yu' _publ_contact_author_email JIEHUIYU@YAHOO.COM.CN _publ_section_title ; Organically templated chained chlorocadmates and cadmium-chloro thiocyanates ; loop_ _publ_author_name 'Yu Hui' 'Qin Hou' 'Xumei Wang' 'Qing-Feng Yang' 'Ling Ye' 'Jie-Hui Yu' # Attachment '3.CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 688441' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H16 Cd Cl3 N3 O2 S' _chemical_formula_weight 401.02 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9957(4) _cell_length_b 9.7477(6) _cell_length_c 10.7688(8) _cell_angle_alpha 63.248(4) _cell_angle_beta 69.699(4) _cell_angle_gamma 87.997(4) _cell_volume 695.52(8) _cell_formula_units_Z 2 _cell_measurement_temperature 253(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description columnar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.915 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 2.282 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 253(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 'Siements SMART CCD' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 5091 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 28.33 _reflns_number_total 3439 _reflns_number_gt 2689 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3439 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.0980 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 0.51801(4) 0.79368(3) 0.49713(4) 0.02793(12) Uani 1 1 d . . . Cl1 Cl 0.60655(15) 0.94013(14) 0.20882(12) 0.0339(2) Uani 1 1 d . . . Cl2 Cl 0.40965(15) 0.64979(12) 0.78793(13) 0.0340(2) Uani 1 1 d . . . Cl3 Cl 0.26844(13) 0.98690(11) 0.51649(11) 0.0250(2) Uani 1 1 d . . . OW1 O 0.5196(6) 0.3136(6) 0.8683(4) 0.0409(9) Uani 1 1 d . . . H13 H 0.493(10) 0.264(8) 0.839(8) 0.07(2) Uiso 1 1 d . . . H14 H 0.488(14) 0.374(12) 0.852(11) 0.13(5) Uiso 1 1 d . . . OW2 O 0.1216(8) 0.6779(7) 0.1319(5) 0.0633(14) Uani 1 1 d . . . H15 H 0.215(11) 0.685(9) 0.128(8) 0.07(3) Uiso 1 1 d . . . H16 H 0.055(11) 0.666(10) 0.194(9) 0.09(3) Uiso 1 1 d . . . C1 C 0.1730(7) 0.2706(5) 0.2080(6) 0.0365(11) Uani 1 1 d . . . H1A H 0.2462 0.3599 0.1897 0.044 Uiso 1 1 calc R . . H1B H 0.0948 0.2194 0.3130 0.044 Uiso 1 1 calc R . . C2 C 0.0609(6) 0.3231(5) 0.1129(6) 0.0374(11) Uani 1 1 d . . . H2A H -0.0198 0.3900 0.1404 0.045 Uiso 1 1 calc R . . H2B H 0.1390 0.3830 0.0086 0.045 Uiso 1 1 calc R . . C3 C 0.0671(6) 0.0732(6) 0.1058(6) 0.0376(11) Uani 1 1 d . . . H3A H 0.1450 0.1179 0.0010 0.045 Uiso 1 1 calc R . . H3B H -0.0095 -0.0171 0.1297 0.045 Uiso 1 1 calc R . . C4 C 0.1811(6) 0.0238(5) 0.2012(6) 0.0376(11) Uani 1 1 d . . . H4A H 0.1038 -0.0312 0.3062 0.045 Uiso 1 1 calc R . . H4B H 0.2599 -0.0462 0.1776 0.045 Uiso 1 1 calc R . . C5 C 0.2649(6) 0.5042(5) 0.5201(5) 0.0313(9) Uani 1 1 d . . . S1 S 0.17802(16) 0.34818(14) 0.52996(16) 0.0401(3) Uani 1 1 d . . . N1 N -0.0468(5) 0.1888(5) 0.1314(5) 0.0320(9) Uani 1 1 d . . . H5 H -0.130(8) 0.148(6) 0.210(7) 0.049(18) Uiso 1 1 d . . . H6 H -0.083(8) 0.218(7) 0.071(7) 0.051(19) Uiso 1 1 d . . . N2 N 0.2911(5) 0.1619(4) 0.1732(5) 0.0295(8) Uani 1 1 d . . . H11 H 0.353(9) 0.217(8) 0.076(7) 0.07(2) Uiso 1 1 d . . . H12 H 0.349(7) 0.136(5) 0.226(5) 0.029(13) Uiso 1 1 d . . . N3 N 0.3248(6) 0.6166(5) 0.5083(6) 0.0501(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03019(19) 0.02471(17) 0.03118(19) -0.01518(13) -0.01101(13) 0.00371(12) Cl1 0.0303(6) 0.0456(6) 0.0315(6) -0.0226(5) -0.0118(5) 0.0091(5) Cl2 0.0281(6) 0.0309(5) 0.0332(6) -0.0082(5) -0.0096(5) 0.0034(4) Cl3 0.0258(5) 0.0252(5) 0.0240(5) -0.0116(4) -0.0093(4) 0.0036(4) OW1 0.050(2) 0.039(2) 0.038(2) -0.0198(18) -0.0193(18) 0.0078(18) OW2 0.042(3) 0.101(4) 0.033(2) -0.018(2) -0.016(2) 0.009(3) C1 0.036(3) 0.034(2) 0.049(3) -0.025(2) -0.020(2) 0.008(2) C2 0.027(2) 0.032(2) 0.045(3) -0.010(2) -0.014(2) 0.0034(19) C3 0.026(2) 0.061(3) 0.048(3) -0.042(3) -0.017(2) 0.010(2) C4 0.031(3) 0.035(2) 0.055(3) -0.024(2) -0.020(2) 0.0092(19) C5 0.028(2) 0.030(2) 0.037(3) -0.017(2) -0.0105(19) 0.0064(18) S1 0.0289(6) 0.0367(6) 0.0632(9) -0.0312(6) -0.0159(6) 0.0050(5) N1 0.022(2) 0.044(2) 0.026(2) -0.0126(18) -0.0096(18) 0.0031(17) N2 0.026(2) 0.034(2) 0.031(2) -0.0125(17) -0.0173(18) 0.0061(16) N3 0.047(3) 0.045(3) 0.067(3) -0.035(2) -0.019(2) -0.002(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 N3 2.291(4) . ? Cd1 Cl1 2.5949(12) . ? Cd1 Cl2 2.6024(12) . ? Cd1 Cl3 2.7038(10) 2_676 ? Cd1 Cl3 2.7157(10) . ? Cd1 S1 2.7460(12) 2_666 ? Cl3 Cd1 2.7038(10) 2_676 ? C1 N2 1.482(6) . ? C1 C2 1.499(6) . ? C2 N1 1.490(6) . ? C3 N1 1.486(6) . ? C3 C4 1.514(6) . ? C4 N2 1.487(6) . ? C5 N3 1.147(6) . ? C5 S1 1.638(5) . ? S1 Cd1 2.7460(12) 2_666 ? 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 N3 Cd1 Cl1 88.73(13) . . ? N3 Cd1 Cl2 89.61(13) . . ? Cl1 Cd1 Cl2 176.60(4) . . ? N3 Cd1 Cl3 176.79(12) . 2_676 ? Cl1 Cd1 Cl3 90.84(3) . 2_676 ? Cl2 Cd1 Cl3 90.65(3) . 2_676 ? N3 Cd1 Cl3 93.50(12) . . ? Cl1 Cd1 Cl3 87.74(3) . . ? Cl2 Cd1 Cl3 89.40(3) . . ? Cl3 Cd1 Cl3 83.31(3) 2_676 . ? N3 Cd1 S1 99.75(12) . 2_666 ? Cl1 Cd1 S1 91.65(4) . 2_666 ? Cl2 Cd1 S1 91.55(4) . 2_666 ? Cl3 Cd1 S1 83.44(3) 2_676 2_666 ? Cl3 Cd1 S1 166.73(3) . 2_666 ? Cd1 Cl3 Cd1 96.69(3) 2_676 . ? N2 C1 C2 110.3(4) . . ? N1 C2 C1 111.4(4) . . ? N1 C3 C4 111.2(4) . . ? N2 C4 C3 110.2(4) . . ? N3 C5 S1 177.5(5) . . ? C5 S1 Cd1 97.41(16) . 2_666 ? C3 N1 C2 112.2(4) . . ? C1 N2 C4 110.4(4) . . ? C5 N3 Cd1 161.2(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 OW2 H15 OW1 0.73(8) 2.14(8) 2.872(7) 175(8) 2_666 N1 H6 OW2 0.74(6) 2.09(6) 2.809(6) 167(6) 2_565 N2 H11 OW1 0.88(7) 1.95(7) 2.821(6) 170(6) 1_554 OW1 H13 Cl1 0.76(8) 2.48(8) 3.230(5) 169(7) 2_666 OW1 H14 Cl2 0.61(10) 2.57(10) 3.168(5) 169(13) . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.296 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.134 # Attachment '4.CIF' data_4 _database_code_depnum_ccdc_archive 'CCDC 688442' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H30 Cd3 Cl8 N6 O S2' _chemical_formula_weight 983.36 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3087(17) _cell_length_b 13.661(3) _cell_length_c 15.298(3) _cell_angle_alpha 113.89(3) _cell_angle_beta 96.41(3) _cell_angle_gamma 102.12(3) _cell_volume 1514.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.278 _exptl_crystal_size_mid 0.243 _exptl_crystal_size_min 0.138 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 2.953 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3571 _exptl_absorpt_correction_T_max 0.5 _exptl_absorpt_process_details ;Higashi, T.(1995).Program for Absorption Correction. Rigaku Corporation, Tokyo,Japan. ; _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method w _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14892 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6790 _reflns_number_gt 5896 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+5.2667P] 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 6790 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0876 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.022 _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 -0.35631(4) 0.66480(3) 0.42267(2) 0.02755(8) Uani 1 1 d . . . Cd2 Cd -0.45640(4) 0.54353(3) 0.13544(2) 0.03134(9) Uani 1 1 d . . . Cd3 Cd -0.40263(4) 0.83294(3) 0.05066(2) 0.02947(9) Uani 1 1 d . . . Cl1 Cl -0.35508(14) 0.85907(9) 0.44325(8) 0.0321(2) Uani 1 1 d . . . Cl2 Cl -0.62522(13) 0.58846(9) 0.27555(8) 0.0282(2) Uani 1 1 d . . . Cl3 Cl -0.19678(13) 0.59824(9) 0.27339(7) 0.0279(2) Uani 1 1 d . . . Cl4 Cl -0.38543(14) 0.76617(9) 0.17942(8) 0.0311(2) Uani 1 1 d . . . Cl5 Cl -0.72056(17) 0.49258(13) 0.00025(9) 0.0471(3) Uani 1 1 d . . . Cl6 Cl -0.47805(16) 0.67212(9) -0.11401(9) 0.0369(3) Uani 1 1 d . . . Cl7 Cl -0.60723(16) 0.93989(11) 0.08006(9) 0.0403(3) Uani 1 1 d . . . Cl8 Cl -0.11064(14) 0.93732(9) 0.06973(9) 0.0320(2) Uani 1 1 d . . . S1 S 0.1716(2) 0.92682(14) 0.64535(13) 0.0560(4) Uani 1 1 d . . . S2 S -0.47960(19) 0.28636(11) 0.42140(11) 0.0424(3) Uani 1 1 d . . . N1 N -0.0560(5) 0.1934(3) 0.1291(3) 0.0336(9) Uani 1 1 d . . . N2 N 0.0093(5) 0.3863(3) 0.2595(3) 0.0325(8) Uani 1 1 d . . . N3 N 0.0586(5) -0.1010(3) 0.2815(3) 0.0270(8) Uani 1 1 d . . . N4 N 0.3044(5) -0.1711(3) 0.3038(3) 0.0285(8) Uani 1 1 d . . . N5 N -0.0802(5) 0.7422(4) 0.5338(3) 0.0287(8) Uani 1 1 d . . . N6 N -0.3936(6) 0.4910(4) 0.4131(3) 0.0416(10) Uani 1 1 d . . . C1 C -0.0273(7) 0.2725(4) 0.0841(4) 0.0389(11) Uani 1 1 d . . . H1A H -0.1200 0.2499 0.0291 0.047 Uiso 1 1 calc R . . H1B H 0.0762 0.2727 0.0604 0.047 Uiso 1 1 calc R . . C2 C -0.0152(6) 0.3884(4) 0.1620(3) 0.0338(10) Uani 1 1 d . . . H2A H 0.0791 0.4430 0.1607 0.041 Uiso 1 1 calc R . . H2B H -0.1177 0.4086 0.1499 0.041 Uiso 1 1 calc R . . C3 C -0.1998(6) 0.2043(4) 0.1790(4) 0.0416(12) Uani 1 1 d . . . H3A H -0.2269 0.1461 0.2003 0.050 Uiso 1 1 calc R . . H3B H -0.2987 0.1970 0.1341 0.050 Uiso 1 1 calc R . . C4 C -0.1496(6) 0.3182(5) 0.2669(4) 0.0392(11) Uani 1 1 d . . . H4A H -0.2383 0.3545 0.2674 0.047 Uiso 1 1 calc R . . H4B H -0.1318 0.3102 0.3271 0.047 Uiso 1 1 calc R . . C5 C 0.0997(6) 0.2163(4) 0.2020(4) 0.0383(11) Uani 1 1 d . . . H5B H 0.1894 0.1975 0.1686 0.046 Uiso 1 1 calc R . . H5C H 0.0771 0.1714 0.2371 0.046 Uiso 1 1 calc R . . C6 C 0.1524(6) 0.3392(4) 0.2731(4) 0.0356(10) Uani 1 1 d . . . H6A H 0.1783 0.3485 0.3399 0.043 Uiso 1 1 calc R . . H6B H 0.2524 0.3778 0.2604 0.043 Uiso 1 1 calc R . . C7 C 0.1987(6) -0.2436(4) 0.2031(3) 0.0357(11) Uani 1 1 d . . . H7A H 0.1705 -0.3211 0.1914 0.043 Uiso 1 1 calc R . . H7B H 0.2604 -0.2361 0.1549 0.043 Uiso 1 1 calc R . . C8 C 0.0390(6) -0.2080(4) 0.1941(3) 0.0324(10) Uani 1 1 d . . . H8A H 0.0200 -0.1982 0.1348 0.039 Uiso 1 1 calc R . . H8B H -0.0572 -0.2649 0.1905 0.039 Uiso 1 1 calc R . . C9 C 0.0652(6) -0.1193(4) 0.3717(3) 0.0317(10) Uani 1 1 d . . . H9A H -0.0426 -0.1664 0.3684 0.038 Uiso 1 1 calc R . . H9B H 0.0890 -0.0486 0.4293 0.038 Uiso 1 1 calc R . . C10 C 0.2035(7) -0.1751(5) 0.3782(4) 0.0393(11) Uani 1 1 d . . . H10A H 0.2758 -0.1364 0.4434 0.047 Uiso 1 1 calc R . . H10B H 0.1541 -0.2519 0.3652 0.047 Uiso 1 1 calc R . . C11 C 0.2152(6) -0.0154(4) 0.2931(4) 0.0338(10) Uani 1 1 d . . . H11A H 0.2207 0.0562 0.3456 0.041 Uiso 1 1 calc R . . H11B H 0.2152 -0.0071 0.2330 0.041 Uiso 1 1 calc R . . C12 C 0.3666(6) -0.0543(4) 0.3168(4) 0.0312(10) Uani 1 1 d . . . H12A H 0.4422 -0.0513 0.2735 0.037 Uiso 1 1 calc R . . H12B H 0.4281 -0.0060 0.3838 0.037 Uiso 1 1 calc R . . C13 C 0.0073(9) 0.8077(7) 0.5727(5) 0.0531(17) Uani 1 1 d . . . C14 C -0.4311(6) 0.4068(4) 0.4162(3) 0.0291(9) Uani 1 1 d . . . OW1 O 0.0870(8) 0.5654(5) 0.4328(4) 0.0713(18) Uani 1 1 d . . . H33 H 0.039(7) 0.454(5) 0.304(4) 0.044(16) Uiso 1 1 d . . . H32 H -0.081(7) 0.128(5) 0.081(4) 0.045(16) Uiso 1 1 d . . . H31 H -0.008(6) -0.072(4) 0.280(4) 0.026(13) Uiso 1 1 d . . . H30 H 0.388(7) -0.200(5) 0.311(4) 0.044(16) Uiso 1 1 d . . . H51 H 0.162(13) 0.604(8) 0.458(8) 0.10(4) Uiso 1 1 d . . . H50 H 0.008(12) 0.579(8) 0.448(7) 0.09(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 0.03077(17) 0.02394(16) 0.02602(16) 0.01069(13) 0.00316(13) 0.00614(12) Cd2 0.03806(18) 0.03008(18) 0.02117(16) 0.00858(13) 0.00331(13) 0.00744(14) Cd3 0.02712(16) 0.03094(18) 0.02832(17) 0.01170(14) 0.00770(13) 0.00607(13) Cl1 0.0349(5) 0.0241(5) 0.0303(5) 0.0079(4) 0.0015(4) 0.0057(4) Cl2 0.0281(5) 0.0241(5) 0.0277(5) 0.0095(4) 0.0038(4) 0.0032(4) Cl3 0.0297(5) 0.0270(5) 0.0245(5) 0.0093(4) 0.0051(4) 0.0079(4) Cl4 0.0353(5) 0.0317(5) 0.0331(5) 0.0177(5) 0.0131(5) 0.0128(4) Cl5 0.0448(7) 0.0617(9) 0.0277(6) 0.0132(6) 0.0059(5) 0.0152(6) Cl6 0.0460(6) 0.0248(5) 0.0316(6) 0.0067(4) 0.0050(5) 0.0073(5) Cl7 0.0415(6) 0.0480(7) 0.0373(6) 0.0185(5) 0.0137(5) 0.0223(5) Cl8 0.0297(5) 0.0237(5) 0.0421(6) 0.0140(5) 0.0119(5) 0.0058(4) S1 0.0438(8) 0.0523(9) 0.0660(10) 0.0205(8) 0.0120(7) 0.0132(7) S2 0.0548(8) 0.0297(6) 0.0496(8) 0.0197(6) 0.0250(6) 0.0139(6) N1 0.040(2) 0.0203(19) 0.035(2) 0.0066(17) 0.0098(18) 0.0072(16) N2 0.041(2) 0.024(2) 0.0259(19) 0.0055(16) 0.0041(17) 0.0095(17) N3 0.0234(17) 0.0253(19) 0.035(2) 0.0114(16) 0.0099(16) 0.0152(15) N4 0.0240(18) 0.033(2) 0.0290(19) 0.0131(16) 0.0055(15) 0.0088(15) N5 0.030(2) 0.028(2) 0.0227(19) 0.0059(16) -0.0010(16) 0.0114(17) N6 0.058(3) 0.036(2) 0.046(3) 0.024(2) 0.029(2) 0.021(2) C1 0.054(3) 0.031(3) 0.031(2) 0.013(2) 0.013(2) 0.011(2) C2 0.043(3) 0.025(2) 0.031(2) 0.0118(19) 0.004(2) 0.0090(19) C3 0.032(2) 0.040(3) 0.052(3) 0.022(3) 0.010(2) 0.005(2) C4 0.038(3) 0.047(3) 0.036(3) 0.017(2) 0.019(2) 0.017(2) C5 0.036(2) 0.033(3) 0.052(3) 0.021(2) 0.011(2) 0.014(2) C6 0.032(2) 0.034(3) 0.039(3) 0.018(2) 0.001(2) 0.0082(19) C7 0.036(2) 0.030(2) 0.029(2) 0.0013(19) 0.0009(19) 0.0110(19) C8 0.033(2) 0.031(2) 0.028(2) 0.0079(19) 0.0004(19) 0.0149(19) C9 0.029(2) 0.033(2) 0.034(2) 0.013(2) 0.0173(19) 0.0100(18) C10 0.041(3) 0.054(3) 0.031(2) 0.028(2) 0.008(2) 0.012(2) C11 0.041(3) 0.025(2) 0.038(3) 0.015(2) 0.013(2) 0.0081(19) C12 0.024(2) 0.030(2) 0.037(2) 0.012(2) 0.0090(19) 0.0049(17) C13 0.069(4) 0.083(5) 0.060(4) 0.056(4) 0.043(4) 0.060(4) C14 0.031(2) 0.034(2) 0.028(2) 0.0143(19) 0.0154(18) 0.0139(18) OW1 0.060(3) 0.070(4) 0.045(3) -0.015(2) -0.011(2) 0.036(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 N6 2.270(4) . ? Cd1 N5 2.435(4) . ? Cd1 Cl1 2.5404(13) . ? Cd1 Cl2 2.6728(16) . ? Cd1 Cl3 2.7017(14) . ? Cd1 S2 2.7952(16) 2_466 ? Cd2 Cl3 2.5875(15) . ? Cd2 Cl5 2.5998(17) . ? Cd2 Cl5 2.6212(15) 2_465 ? Cd2 Cl2 2.6278(13) . ? Cd2 Cl4 2.7482(14) . ? Cd2 Cl6 2.7545(14) 2_465 ? Cd3 Cl7 2.4306(14) . ? Cd3 Cl8 2.4611(14) . ? Cd3 Cl6 2.4804(17) . ? Cd3 Cl4 2.4860(12) . ? Cl5 Cd2 2.6211(15) 2_465 ? Cl6 Cd2 2.7545(14) 2_465 ? S1 C13 1.736(9) . ? S2 C14 1.647(5) . ? S2 Cd1 2.7952(16) 2_466 ? N1 C3 1.489(6) . ? N1 C1 1.494(6) . ? N1 C5 1.496(7) . ? N2 C4 1.492(6) . ? N2 C2 1.494(6) . ? N2 C6 1.499(6) . ? N3 C8 1.490(6) . ? N3 C11 1.495(6) . ? N3 C9 1.497(6) . ? N4 C7 1.491(6) . ? N4 C12 1.492(6) . ? N4 C10 1.498(6) . ? N5 C13 0.939(8) . ? N6 C14 1.148(6) . ? C1 C2 1.522(6) . ? C3 C4 1.520(7) . ? C5 C6 1.516(7) . ? C7 C8 1.517(6) . ? C9 C10 1.522(7) . ? C11 C12 1.527(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 N6 Cd1 N5 94.82(17) . . ? N6 Cd1 Cl1 171.34(11) . . ? N5 Cd1 Cl1 89.63(11) . . ? N6 Cd1 Cl2 90.22(13) . . ? N5 Cd1 Cl2 168.45(10) . . ? Cl1 Cd1 Cl2 86.79(5) . . ? N6 Cd1 Cl3 86.47(11) . . ? N5 Cd1 Cl3 87.58(10) . . ? Cl1 Cd1 Cl3 101.16(5) . . ? Cl2 Cd1 Cl3 82.35(4) . . ? N6 Cd1 S2 87.79(11) . 2_466 ? N5 Cd1 S2 91.83(10) . 2_466 ? Cl1 Cd1 S2 84.65(5) . 2_466 ? Cl2 Cd1 S2 98.75(5) . 2_466 ? Cl3 Cd1 S2 174.15(4) . 2_466 ? Cl3 Cd2 Cl5 178.42(4) . . ? Cl3 Cd2 Cl5 93.23(4) . 2_465 ? Cl5 Cd2 Cl5 88.07(5) . 2_465 ? Cl3 Cd2 Cl2 85.45(4) . . ? Cl5 Cd2 Cl2 93.23(4) . . ? Cl5 Cd2 Cl2 177.55(4) 2_465 . ? Cl3 Cd2 Cl4 86.84(5) . . ? Cl5 Cd2 Cl4 92.23(6) . . ? Cl5 Cd2 Cl4 91.52(5) 2_465 . ? Cl2 Cd2 Cl4 86.36(4) . . ? Cl3 Cd2 Cl6 88.59(5) . 2_465 ? Cl5 Cd2 Cl6 92.23(6) . 2_465 ? Cl5 Cd2 Cl6 93.40(5) 2_465 2_465 ? Cl2 Cd2 Cl6 88.63(5) . 2_465 ? Cl4 Cd2 Cl6 173.47(4) . 2_465 ? Cl7 Cd3 Cl8 116.22(5) . . ? Cl7 Cd3 Cl6 113.72(5) . . ? Cl8 Cd3 Cl6 105.83(6) . . ? Cl7 Cd3 Cl4 106.26(5) . . ? Cl8 Cd3 Cl4 104.44(5) . . ? Cl6 Cd3 Cl4 109.93(4) . . ? Cd2 Cl2 Cd1 95.74(4) . . ? Cd2 Cl3 Cd1 96.00(4) . . ? Cd3 Cl4 Cd2 122.40(5) . . ? Cd2 Cl5 Cd2 91.93(5) . 2_465 ? Cd3 Cl6 Cd2 121.09(5) . 2_465 ? C14 S2 Cd1 101.45(16) . 2_466 ? C3 N1 C1 110.8(4) . . ? C3 N1 C5 109.3(4) . . ? C1 N1 C5 109.9(4) . . ? C4 N2 C2 109.4(4) . . ? C4 N2 C6 110.1(4) . . ? C2 N2 C6 110.8(4) . . ? C8 N3 C11 110.6(4) . . ? C8 N3 C9 110.0(4) . . ? C11 N3 C9 109.8(4) . . ? C7 N4 C12 109.8(4) . . ? C7 N4 C10 109.9(4) . . ? C12 N4 C10 110.6(4) . . ? C13 N5 Cd1 144.9(5) . . ? C14 N6 Cd1 169.5(4) . . ? N1 C1 C2 108.1(4) . . ? N2 C2 C1 107.9(4) . . ? N1 C3 C4 108.5(4) . . ? N2 C4 C3 108.1(4) . . ? N1 C5 C6 108.3(4) . . ? N2 C6 C5 108.1(4) . . ? N4 C7 C8 108.5(4) . . ? N3 C8 C7 108.6(4) . . ? N3 C9 C10 108.4(3) . . ? N4 C10 C9 108.2(4) . . ? N3 C11 C12 108.0(4) . . ? N4 C12 C11 108.7(4) . . ? N5 C13 S1 178.6(6) . . ? N6 C14 S2 178.5(5) . . ? 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 H31 S1 0.75(5) 2.59(5) 3.287(4) 155(5) 2_566 N4 H30 Cl1 0.89(6) 2.51(6) 3.190(4) 134(5) 1_645 N2 H33 OW1 0.85(6) 1.88(6) 2.671(6) 154(6) . N1 H32 Cl8 0.86(6) 2.49(6) 3.152(4) 134(5) 1_545 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.792 _refine_diff_density_min -1.048 _refine_diff_density_rms 0.137 # Attachment '2.cif' data_y _database_code_depnum_ccdc_archive 'CCDC 688443' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H16 Cd2 Cl6 N2 O' _chemical_formula_weight 569.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 7.5685(15) _cell_length_b 20.604(4) _cell_length_c 10.448(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.89(3) _cell_angle_gamma 90.00 _cell_volume 1574.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description columnar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.447 _exptl_crystal_size_mid 0.248 _exptl_crystal_size_min 0.194 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 3.703 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3186 _exptl_absorpt_correction_T_max 0.5 _exptl_absorpt_process_details ;Higashi, T.(1995).Program for Absorption Correction. Rigaku Corporation, Tokyo,Japan. ; _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method w _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15363 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3610 _reflns_number_gt 3390 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+1.4808P] 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 3610 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0196 _refine_ls_wR_factor_ref 0.0489 _refine_ls_wR_factor_gt 0.0483 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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 0.54900(2) 0.409218(8) 0.020156(17) 0.02425(5) Uani 1 1 d . . . Cd2 Cd 0.93428(2) 0.431543(9) -0.132290(17) 0.02599(6) Uani 1 1 d . . . Cl1 Cl 0.61532(8) 0.32877(3) 0.20665(6) 0.02756(12) Uani 1 1 d . . . Cl2 Cl 0.22697(8) 0.36173(3) -0.09685(7) 0.03223(14) Uani 1 1 d . . . Cl3 Cl 0.55915(8) 0.49931(3) -0.15537(6) 0.02817(12) Uani 1 1 d . . . Cl4 Cl 0.71650(8) 0.33386(3) -0.11953(6) 0.02818(12) Uani 1 1 d . . . Cl5 Cl 0.92785(8) 0.45132(3) 0.11545(6) 0.02740(12) Uani 1 1 d . . . Cl6 Cl 0.84937(9) 0.43128(3) -0.37908(6) 0.03113(13) Uani 1 1 d . . . C3 C 0.2687(5) 0.41578(14) 0.5594(3) 0.0431(7) Uani 1 1 d . . . H3A H 0.3531 0.4199 0.6463 0.052 Uiso 1 1 calc R . . H3B H 0.1793 0.4504 0.5486 0.052 Uiso 1 1 calc R . . C4 C 0.3721(4) 0.42025(14) 0.4521(3) 0.0397(7) Uani 1 1 d . . . H4A H 0.3061 0.4477 0.3802 0.048 Uiso 1 1 calc R . . H4B H 0.4924 0.4388 0.4883 0.048 Uiso 1 1 calc R . . C5 C 0.3164(4) 0.29926(14) 0.5902(3) 0.0335(6) Uani 1 1 d . . . H5A H 0.2601 0.2569 0.5707 0.040 Uiso 1 1 calc R . . H5B H 0.3703 0.3021 0.6849 0.040 Uiso 1 1 calc R . . C6 C 0.4627(3) 0.30852(13) 0.5157(3) 0.0309(5) Uani 1 1 d . . . H6A H 0.5723 0.3267 0.5742 0.037 Uiso 1 1 calc R . . H6B H 0.4937 0.2671 0.4830 0.037 Uiso 1 1 calc R . . H1 H 0.105(5) 0.3515(17) 0.595(3) 0.039(9) Uiso 1 1 d . . . H2 H 0.463(5) 0.3567(19) 0.356(4) 0.052(11) Uiso 1 1 d . . . N1 N 0.1755(3) 0.35159(11) 0.5470(2) 0.0259(4) Uani 1 1 d . . . N2 N 0.3891(3) 0.35354(11) 0.4027(2) 0.0290(5) Uani 1 1 d . . . C1 C 0.0707(4) 0.34009(18) 0.4081(3) 0.0423(7) Uani 1 1 d . . . H1A H -0.0064 0.3772 0.3751 0.051 Uiso 1 1 calc R . . H1B H -0.0067 0.3022 0.4033 0.051 Uiso 1 1 calc R . . C2 C 0.2068(4) 0.32956(18) 0.3251(3) 0.0416(7) Uani 1 1 d . . . H2A H 0.2139 0.2838 0.3052 0.050 Uiso 1 1 calc R . . H2B H 0.1681 0.3531 0.2423 0.050 Uiso 1 1 calc R . . OW1 O 0.9344(4) 0.23433(15) 1.1412(4) 0.0513(6) Uani 1 1 d . . . H3 H 0.909(12) 0.234(4) 1.188(9) 0.16(4) Uiso 1 1 d . . . H4 H 0.880(8) 0.261(3) 1.096(6) 0.10(2) 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 0.02882(10) 0.02148(9) 0.02480(9) 0.00118(6) 0.01118(7) 0.00175(6) Cd2 0.02862(10) 0.02563(10) 0.02521(9) -0.00214(7) 0.00966(7) -0.00413(7) Cl1 0.0305(3) 0.0294(3) 0.0258(3) 0.0051(2) 0.0129(2) 0.0053(2) Cl2 0.0232(3) 0.0290(3) 0.0422(3) -0.0043(3) 0.0042(2) 0.0012(2) Cl3 0.0363(3) 0.0251(3) 0.0249(3) 0.0006(2) 0.0112(2) 0.0032(2) Cl4 0.0313(3) 0.0245(3) 0.0323(3) -0.0066(2) 0.0148(2) -0.0048(2) Cl5 0.0307(3) 0.0264(3) 0.0248(3) 0.0009(2) 0.0065(2) -0.0056(2) Cl6 0.0328(3) 0.0357(3) 0.0257(3) 0.0002(2) 0.0089(2) 0.0070(2) C3 0.0558(19) 0.0272(14) 0.0533(19) -0.0123(13) 0.0268(16) -0.0042(13) C4 0.0384(15) 0.0263(13) 0.0595(19) 0.0075(13) 0.0219(14) 0.0016(11) C5 0.0355(13) 0.0339(14) 0.0319(13) 0.0097(11) 0.0101(11) 0.0067(11) C6 0.0269(12) 0.0309(13) 0.0355(13) 0.0076(11) 0.0092(10) 0.0090(10) N1 0.0235(10) 0.0321(11) 0.0252(10) 0.0006(8) 0.0120(8) 0.0026(8) N2 0.0286(11) 0.0347(12) 0.0286(11) 0.0060(9) 0.0163(9) 0.0082(9) C1 0.0210(12) 0.069(2) 0.0321(14) 0.0004(14) -0.0015(11) -0.0026(13) C2 0.0390(15) 0.061(2) 0.0207(12) -0.0061(12) 0.0010(11) 0.0049(14) OW1 0.0375(12) 0.0502(15) 0.0674(18) -0.0076(13) 0.0154(12) 0.0118(11) _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 Cl1 2.5087(7) . ? Cd1 Cl3 2.6100(7) 3_665 ? Cd1 Cl2 2.6193(9) . ? Cd1 Cl3 2.6244(7) . ? Cd1 Cl4 2.6644(8) . ? Cd1 Cl5 2.9152(9) . ? Cd2 Cl6 2.4920(9) . ? Cd2 Cl2 2.5869(8) 1_655 ? Cd2 Cl5 2.6173(8) 3_765 ? Cd2 Cl4 2.6263(7) . ? Cd2 Cl5 2.6331(8) . ? Cl2 Cd2 2.5869(8) 1_455 ? Cl3 Cd1 2.6100(7) 3_665 ? Cl5 Cd2 2.6173(8) 3_765 ? C3 N1 1.489(3) . ? C3 C4 1.527(4) . ? C4 N2 1.485(4) . ? C5 N1 1.502(3) . ? C5 C6 1.521(4) . ? C6 N2 1.492(3) . ? N1 C1 1.483(3) . ? N2 C2 1.494(4) . ? C1 C2 1.522(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 Cl1 Cd1 Cl3 94.86(2) . 3_665 ? Cl1 Cd1 Cl2 95.29(3) . . ? Cl3 Cd1 Cl2 97.97(3) 3_665 . ? Cl1 Cd1 Cl3 166.95(2) . . ? Cl3 Cd1 Cl3 86.39(3) 3_665 . ? Cl2 Cd1 Cl3 97.41(3) . . ? Cl1 Cd1 Cl4 90.69(3) . . ? Cl3 Cd1 Cl4 167.65(2) 3_665 . ? Cl2 Cd1 Cl4 92.48(3) . . ? Cl3 Cd1 Cl4 85.75(3) . . ? Cl1 Cd1 Cl5 87.04(3) . . ? Cl3 Cd1 Cl5 91.03(2) 3_665 . ? Cl2 Cd1 Cl5 170.46(2) . . ? Cl3 Cd1 Cl5 79.94(3) . . ? Cl4 Cd1 Cl5 78.22(2) . . ? Cl6 Cd2 Cl2 97.50(3) . 1_655 ? Cl6 Cd2 Cl5 93.66(2) . 3_765 ? Cl2 Cd2 Cl5 101.02(2) 1_655 3_765 ? Cl6 Cd2 Cl4 93.01(3) . . ? Cl2 Cd2 Cl4 95.29(3) 1_655 . ? Cl5 Cd2 Cl4 161.40(2) 3_765 . ? Cl6 Cd2 Cl5 162.27(2) . . ? Cl2 Cd2 Cl5 100.18(3) 1_655 . ? Cl5 Cd2 Cl5 84.20(2) 3_765 . ? Cl4 Cd2 Cl5 84.16(3) . . ? Cd2 Cl2 Cd1 121.26(3) 1_455 . ? Cd1 Cl3 Cd1 93.61(3) 3_665 . ? Cd2 Cl4 Cd1 88.54(2) . . ? Cd2 Cl5 Cd2 95.80(2) 3_765 . ? Cd2 Cl5 Cd1 129.61(2) 3_765 . ? Cd2 Cl5 Cd1 83.29(3) . . ? N1 C3 C4 108.1(2) . . ? N2 C4 C3 107.8(2) . . ? N1 C5 C6 108.1(2) . . ? N2 C6 C5 108.1(2) . . ? C1 N1 C3 110.5(2) . . ? C1 N1 C5 109.8(2) . . ? C3 N1 C5 109.1(2) . . ? C4 N2 C6 110.4(2) . . ? C4 N2 C2 110.1(2) . . ? C6 N2 C2 109.2(2) . . ? N1 C1 C2 108.1(2) . . ? N2 C2 C1 108.1(2) . . ? 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 N2 H2 Cl1 0.83(4) 2.25(4) 3.031(2) 159(4) . N1 H1 Cl6 0.82(4) 2.60(3) 3.219(2) 133(3) 1_456 OW1 H4 Cl4 0.77(6) 2.73(6) 3.470(4) 164(6) 1_556 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.453 _refine_diff_density_min -0.865 _refine_diff_density_rms 0.145 # Attachment '1.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 704584' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H16 Cd2 Cl6 N2 O2' _chemical_formula_weight 561.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 6.803(3) _cell_length_b 11.084(5) _cell_length_c 10.664(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.066(4) _cell_angle_gamma 90.00 _cell_volume 768.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description columnar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.257 _exptl_crystal_size_mid 0.244 _exptl_crystal_size_min 0.211 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 3.795 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 P4 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5593 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0453 _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 -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 4.19 _diffrn_reflns_theta_max 26.05 _reflns_number_total 1374 _reflns_number_gt 1183 _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1374 _refine_ls_number_parameters 81 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0655 _refine_ls_wR_factor_gt 0.0638 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.28745(4) 0.49769(2) 0.08806(3) 0.02261(13) Uani 1 1 d . . . Cl1 Cl 0.29235(14) 0.39549(8) 0.30253(9) 0.0319(2) Uani 1 1 d . . . Cl2 Cl 0.61368(12) 0.36497(8) 0.08731(9) 0.0261(2) Uani 1 1 d . . . Cl3 Cl -0.03265(12) 0.62604(7) 0.09482(8) 0.0244(2) Uani 1 1 d . . . OW1 O 0.5164(4) 0.6424(2) 0.2347(2) 0.0296(6) Uani 1 1 d . . . C1 C -0.0262(6) 0.6140(3) 0.4333(4) 0.0296(8) Uani 1 1 d . . . H1C H -0.1322 0.6512 0.4644 0.036 Uiso 1 1 calc R . . H1D H 0.0104 0.6701 0.3739 0.036 Uiso 1 1 calc R . . C2 C 0.1623(6) 0.5887(3) 0.5495(4) 0.0295(8) Uani 1 1 d . . . H2A H 0.2726 0.5572 0.5184 0.035 Uiso 1 1 calc R . . H2B H 0.2094 0.6628 0.5971 0.035 Uiso 1 1 calc R . . N1 N -0.1074(5) 0.5012(3) 0.3617(3) 0.0285(7) Uani 1 1 d . . . H1B H -0.227(7) 0.526(3) 0.293(4) 0.023(10) Uiso 1 1 d . . . H1A H -0.021(10) 0.486(4) 0.297(7) 0.060(17) 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 0.01853(17) 0.02628(18) 0.0230(2) 0.00152(9) 0.00603(12) -0.00059(9) Cl1 0.0356(5) 0.0336(5) 0.0310(5) 0.0101(4) 0.0168(4) 0.0109(4) Cl2 0.0238(4) 0.0284(4) 0.0280(5) 0.0042(3) 0.0107(3) 0.0030(3) Cl3 0.0232(4) 0.0227(4) 0.0266(5) -0.0020(3) 0.0065(3) 0.0009(3) OW1 0.0292(13) 0.0286(14) 0.0288(14) -0.0004(11) 0.0048(10) -0.0045(10) C1 0.034(2) 0.0247(18) 0.026(2) -0.0003(15) 0.0017(15) -0.0025(15) C2 0.0255(18) 0.0300(19) 0.030(2) -0.0074(15) 0.0028(15) -0.0024(15) N1 0.0280(17) 0.0360(19) 0.0178(18) -0.0037(12) 0.0008(14) 0.0024(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 OW1 2.453(3) . ? Cd1 Cl1 2.5438(13) . ? Cd1 Cl3 2.5894(11) 3_565 ? Cd1 Cl3 2.6199(12) . ? Cd1 Cl2 2.6468(12) 3_665 ? Cd1 Cl2 2.6646(12) . ? Cl2 Cd1 2.6468(12) 3_665 ? Cl3 Cd1 2.5894(11) 3_565 ? C1 N1 1.484(5) . ? C1 C2 1.525(5) . ? C2 N1 1.495(5) 3_566 ? N1 C2 1.495(5) 3_566 ? 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 OW1 Cd1 Cl1 83.09(7) . . ? OW1 Cd1 Cl3 170.46(6) . 3_565 ? Cl1 Cd1 Cl3 105.70(4) . 3_565 ? OW1 Cd1 Cl3 90.28(7) . . ? Cl1 Cd1 Cl3 90.50(3) . . ? Cl3 Cd1 Cl3 86.00(4) 3_565 . ? OW1 Cd1 Cl2 80.14(7) . 3_665 ? Cl1 Cd1 Cl2 162.26(3) . 3_665 ? Cl3 Cd1 Cl2 91.45(4) 3_565 3_665 ? Cl3 Cd1 Cl2 95.32(3) . 3_665 ? OW1 Cd1 Cl2 89.38(7) . . ? Cl1 Cd1 Cl2 88.03(3) . . ? Cl3 Cd1 Cl2 94.56(4) 3_565 . ? Cl3 Cd1 Cl2 178.52(3) . . ? Cl2 Cd1 Cl2 86.03(4) 3_665 . ? Cd1 Cl2 Cd1 93.97(4) 3_665 . ? Cd1 Cl3 Cd1 94.00(4) 3_565 . ? N1 C1 C2 111.1(3) . . ? N1 C2 C1 109.3(3) 3_566 . ? C1 N1 C2 111.1(3) . 3_566 ? 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 N1 H1A Cl1 1.05(7) 2.34(6) 3.190(4) 138(5) . N1 H1B OW1 0.96(4) 2.11(4) 2.966(4) 147(4) 1_455 C1 H1C Cl3 0.97 2.82 3.364(4) 116.5 4_576 C2 H2B Cl3 0.97 2.86 3.517(4) 126.1 4_576 _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.901 _refine_diff_density_max 0.558 _refine_diff_density_min -1.254 _refine_diff_density_rms 0.125 # Attachment '6.CIF' data_6 _database_code_depnum_ccdc_archive 'CCDC 711977' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H13 Cl N4 S2 Zn' _chemical_formula_weight 330.16 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' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca 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' '-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 10.839(2) _cell_length_b 12.536(3) _cell_length_c 18.910(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2569.4(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.474 _exptl_crystal_size_mid 0.255 _exptl_crystal_size_min 0.221 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 2.422 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2702 _exptl_absorpt_correction_T_max 0.5 _exptl_absorpt_process_details ;Higashi, T.(1995).Program for Absorption Correction. Rigaku Corporation, Tokyo,Japan. ; _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method w _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22749 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_sigmaI/netI 0.0690 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2941 _reflns_number_gt 2337 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+3.8669P] 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 2941 _refine_ls_number_parameters 149 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1186 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _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 Zn1 Zn 0.76966(4) -0.37904(3) 0.35684(2) 0.02837(15) Uani 1 1 d . . . S1 S 0.44094(11) -0.13371(10) 0.37258(8) 0.0544(3) Uani 1 1 d . . . S2 S 0.70821(11) -0.57863(9) 0.56142(6) 0.0457(3) Uani 1 1 d . . . Cl1 Cl 0.76985(9) -0.45988(8) 0.25268(5) 0.0369(2) Uani 1 1 d . . . N1 N 0.9199(3) -0.2753(2) 0.36082(14) 0.0241(6) Uani 1 1 d . . . N2 N 1.0944(3) -0.1418(2) 0.36626(16) 0.0309(7) Uani 1 1 d . . . N3 N 0.7761(3) -0.4711(3) 0.44040(18) 0.0428(8) Uani 1 1 d . . . N4 N 0.6233(3) -0.2881(3) 0.37058(19) 0.0448(9) Uani 1 1 d . . . C1 C 0.8779(4) -0.1695(3) 0.3356(2) 0.0386(9) Uani 1 1 d . . . H1A H 0.8080 -0.1464 0.3637 0.046 Uiso 1 1 calc R . . H1B H 0.8511 -0.1753 0.2868 0.046 Uiso 1 1 calc R . . C2 C 0.9805(4) -0.0867(3) 0.3408(3) 0.0416(10) Uani 1 1 d . . . H2A H 0.9952 -0.0547 0.2949 0.050 Uiso 1 1 calc R . . H2B H 0.9572 -0.0307 0.3736 0.050 Uiso 1 1 calc R . . C3 C 0.9659(4) -0.2657(3) 0.4344(2) 0.0414(10) Uani 1 1 d . . . H3A H 0.9935 -0.3349 0.4509 0.050 Uiso 1 1 calc R . . H3B H 0.8995 -0.2419 0.4649 0.050 Uiso 1 1 calc R . . C4 C 1.0727(4) -0.1863(3) 0.4382(2) 0.0402(9) Uani 1 1 d . . . H4A H 1.0527 -0.1293 0.4709 0.048 Uiso 1 1 calc R . . H4B H 1.1465 -0.2219 0.4550 0.048 Uiso 1 1 calc R . . C5 C 1.0235(3) -0.3111(3) 0.3159(2) 0.0376(9) Uani 1 1 d . . . H5A H 0.9944 -0.3216 0.2678 0.045 Uiso 1 1 calc R . . H5B H 1.0543 -0.3788 0.3332 0.045 Uiso 1 1 calc R . . C6 C 1.1279(3) -0.2289(3) 0.3160(2) 0.0361(9) Uani 1 1 d . . . H6A H 1.2045 -0.2624 0.3307 0.043 Uiso 1 1 calc R . . H6B H 1.1392 -0.2001 0.2689 0.043 Uiso 1 1 calc R . . C7 C 0.7499(3) -0.5155(3) 0.4905(2) 0.0307(8) Uani 1 1 d . . . C8 C 0.5461(4) -0.2244(3) 0.3718(2) 0.0360(9) Uani 1 1 d . . . H1C H 1.160(4) -0.097(3) 0.368(2) 0.039(12) 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 Zn1 0.0284(3) 0.0293(2) 0.0274(2) 0.00020(16) 0.00277(15) -0.00302(16) S1 0.0391(6) 0.0535(7) 0.0707(8) 0.0002(6) 0.0003(5) 0.0118(5) S2 0.0659(7) 0.0367(6) 0.0344(5) 0.0099(4) 0.0100(5) 0.0086(5) Cl1 0.0424(5) 0.0376(5) 0.0308(5) -0.0051(4) -0.0010(4) -0.0004(4) N1 0.0275(15) 0.0229(14) 0.0218(14) -0.0029(11) 0.0008(11) 0.0009(11) N2 0.0258(16) 0.0296(16) 0.0372(17) -0.0053(13) -0.0013(12) -0.0034(12) N3 0.052(2) 0.044(2) 0.0322(18) 0.0030(15) 0.0005(15) -0.0021(16) N4 0.034(2) 0.050(2) 0.050(2) -0.0003(17) 0.0083(15) 0.0058(16) C1 0.028(2) 0.030(2) 0.058(3) 0.0041(18) -0.0069(17) 0.0009(15) C2 0.035(2) 0.027(2) 0.063(3) 0.0087(19) -0.0054(18) 0.0011(16) C3 0.051(2) 0.049(2) 0.0238(19) -0.0004(17) -0.0037(16) -0.0150(19) C4 0.045(2) 0.044(2) 0.031(2) -0.0047(17) -0.0070(16) -0.0067(18) C5 0.030(2) 0.036(2) 0.047(2) -0.0156(18) 0.0128(16) -0.0050(15) C6 0.0283(19) 0.038(2) 0.042(2) -0.0093(17) 0.0066(15) -0.0034(15) C7 0.0340(19) 0.0264(18) 0.0317(19) -0.0047(15) -0.0047(14) 0.0022(14) C8 0.031(2) 0.047(2) 0.0300(19) -0.0009(17) 0.0043(15) -0.0037(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 Zn1 N3 1.958(4) . ? Zn1 N4 1.971(4) . ? Zn1 N1 2.085(3) . ? Zn1 Cl1 2.2150(10) . ? S1 C8 1.610(4) . ? S2 C7 1.622(4) . ? N1 C5 1.478(4) . ? N1 C1 1.481(5) . ? N1 C3 1.483(4) . ? N2 C4 1.489(5) . ? N2 C6 1.493(5) . ? N2 C2 1.494(5) . ? N3 C7 1.135(5) . ? N4 C8 1.157(5) . ? C1 C2 1.524(5) . ? C3 C4 1.527(5) . ? C5 C6 1.530(5) . ? 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 N3 Zn1 N4 105.28(15) . . ? N3 Zn1 N1 108.10(13) . . ? N4 Zn1 N1 105.22(14) . . ? N3 Zn1 Cl1 116.61(11) . . ? N4 Zn1 Cl1 112.50(11) . . ? N1 Zn1 Cl1 108.47(8) . . ? C5 N1 C1 108.7(3) . . ? C5 N1 C3 107.9(3) . . ? C1 N1 C3 109.4(3) . . ? C5 N1 Zn1 112.5(2) . . ? C1 N1 Zn1 107.9(2) . . ? C3 N1 Zn1 110.3(2) . . ? C4 N2 C6 110.2(3) . . ? C4 N2 C2 109.7(3) . . ? C6 N2 C2 109.6(3) . . ? C7 N3 Zn1 162.5(3) . . ? C8 N4 Zn1 169.8(3) . . ? N1 C1 C2 111.4(3) . . ? N2 C2 C1 108.0(3) . . ? N1 C3 C4 110.6(3) . . ? N2 C4 C3 108.7(3) . . ? N1 C5 C6 110.9(3) . . ? N2 C6 C5 108.3(3) . . ? N3 C7 S2 178.4(4) . . ? N4 C8 S1 178.6(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 N2 H1C S2 0.90(5) 2.63(4) 3.321(3) 134(4) 4_546 N2 H1C Cl1 0.90(5) 2.96(4) 3.525(3) 122(3) 3_755 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.762 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.124