Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Thomas C. W. Mak' 'Song-Lin Li' 'Hai-Tao Wu' _publ_contact_author_name 'Prof Thomas C. W. Mak' _publ_contact_author_address ; Department of Chemistry The Chinese University of Hong Kong Shatin, New Territories Hong Kong SAR 852 CHINA ; _publ_contact_author_email TCWMAK@CUHK.EDU.HK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Pyridiniodithioacetate and its first stable metal complex ; data_p21c _database_code_CSD 121647 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '\a-pyridinium dithioacetate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H7 N S2' _chemical_formula_weight 169.26 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' _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 10.440(2) _cell_length_b 7.787(2) _cell_length_c 10.037(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.89(3) _cell_angle_gamma 90.00 _cell_volume 806.2(3) _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 prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 352 _exptl_absorpt_coefficient_mu 0.580 _exptl_absorpt_correction_type ABSCOR _exptl_absorpt_correction_T_min 0.715 _exptl_absorpt_correction_T_max 1.216 _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 'rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'IP Rigaku' _diffrn_measurement_method IP _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2380 _diffrn_reflns_av_R_equivalents 0.0949 _diffrn_reflns_av_sigmaI/netI 0.0838 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.62 _reflns_number_total 1430 _reflns_number_gt 1320 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAXIS Rigaku' _computing_cell_refinement 'BIOTEX Rigaku' _computing_data_reduction 'BIOTEX Rigaku' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _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^)+(0.1135P)^2^+0.2381P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.10(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1430 _refine_ls_number_parameters 92 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.1884 _refine_ls_wR_factor_gt 0.1835 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 C1 C 0.2080(3) -0.0529(4) 0.7955(3) 0.0659(8) Uani 1 1 d . . . H1A H 0.2091 0.0582 0.8296 0.079 Uiso 1 1 calc R . . C2 C 0.1233(3) -0.1704(4) 0.8318(3) 0.0720(9) Uani 1 1 d . . . H2A H 0.0659 -0.1391 0.8897 0.086 Uiso 1 1 calc R . . C3 C 0.1225(4) -0.3334(4) 0.7836(4) 0.0774(10) Uani 1 1 d . . . H3A H 0.0658 -0.4145 0.8094 0.093 Uiso 1 1 calc R . . C4 C 0.2065(4) -0.3776(5) 0.6962(4) 0.0829(10) Uani 1 1 d . . . H4A H 0.2068 -0.4886 0.6620 0.099 Uiso 1 1 calc R . . C5 C 0.2895(3) -0.2565(4) 0.6602(4) 0.0698(8) Uani 1 1 d . . . H5A H 0.3459 -0.2851 0.6005 0.084 Uiso 1 1 calc R . . N1 N 0.2903(2) -0.0972(3) 0.7100(2) 0.0573(7) Uani 1 1 d . . . C6 C 0.3810(3) 0.0330(4) 0.6723(4) 0.0715(9) Uani 1 1 d . . . H6B H 0.4480 -0.0253 0.6325 0.086 Uiso 1 1 calc R . . H6A H 0.4227 0.0893 0.7538 0.086 Uiso 1 1 calc R . . C7 C 0.3200(3) 0.1704(3) 0.5739(3) 0.0547(7) Uani 1 1 d . . . S1 S 0.43094(8) 0.31161(11) 0.53718(9) 0.0720(4) Uani 1 1 d . . . S2 S 0.16097(8) 0.17311(10) 0.51976(9) 0.0673(4) 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 C1 0.0755(19) 0.0589(17) 0.0661(18) -0.0040(13) 0.0197(15) -0.0013(14) C2 0.0720(19) 0.086(2) 0.0614(18) 0.0070(15) 0.0205(15) -0.0056(15) C3 0.076(2) 0.072(2) 0.085(2) 0.0205(17) 0.0123(17) -0.0147(15) C4 0.098(3) 0.0495(17) 0.099(3) -0.0042(17) 0.010(2) -0.0048(16) C5 0.0741(18) 0.0648(19) 0.073(2) -0.0014(15) 0.0203(15) 0.0081(15) N1 0.0581(13) 0.0543(13) 0.0609(14) 0.0055(10) 0.0139(11) -0.0035(10) C6 0.0602(16) 0.0709(19) 0.083(2) 0.0191(16) 0.0097(15) -0.0120(14) C7 0.0654(16) 0.0478(14) 0.0539(15) -0.0018(10) 0.0184(13) -0.0026(11) S1 0.0693(6) 0.0644(6) 0.0857(7) 0.0132(4) 0.0222(5) -0.0126(3) S2 0.0620(6) 0.0628(6) 0.0774(7) 0.0070(3) 0.0119(4) -0.0036(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 C1 N1 1.349(3) . ? C1 C2 1.361(4) . ? C2 C3 1.358(5) . ? C3 C4 1.377(5) . ? C4 C5 1.366(5) . ? C5 N1 1.338(4) . ? N1 C6 1.476(4) . ? C6 C7 1.527(4) . ? C7 S2 1.665(3) . ? C7 S1 1.679(3) . ? 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 C1 C2 120.2(3) . . ? C3 C2 C1 120.1(3) . . ? C2 C3 C4 119.4(3) . . ? C5 C4 C3 119.2(3) . . ? N1 C5 C4 120.6(3) . . ? C5 N1 C1 120.5(3) . . ? C5 N1 C6 120.6(3) . . ? C1 N1 C6 119.0(3) . . ? N1 C6 C7 115.3(2) . . ? C6 C7 S2 121.0(2) . . ? C6 C7 S1 111.6(2) . . ? S2 C7 S1 127.38(18) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.62 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.350 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.071 data_pytcd _database_code_CSD 121648 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H14 Cd Cl2 N2 S4' _chemical_formula_weight 521.81 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' 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 13.301(3) _cell_length_b 8.209(6) _cell_length_c 18.014(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.860(10) _cell_angle_gamma 90.00 _cell_volume 1924.9(15) _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 prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.801 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 1.844 _exptl_absorpt_correction_type '\y scans' _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 1.00 _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 'Siemens P4' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 120 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6649 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 30.00 _reflns_number_total 5347 _reflns_number_gt 3584 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _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^)+(0.0378P)^2^+2.3502P] 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 5347 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 0.71785(3) 0.21709(4) 0.786636(17) 0.03996(10) Uani 1 1 d . . . S1 S 0.51370(12) 0.1534(3) 0.77945(8) 0.0817(6) Uani 1 1 d . . . S2 S 0.59841(10) 0.22597(17) 0.64556(7) 0.0514(3) Uani 1 1 d . . . S3 S 0.84057(10) 0.45793(15) 0.79264(6) 0.0453(3) Uani 1 1 d . . . S4 S 0.86074(10) 0.35674(16) 0.63659(6) 0.0472(3) Uani 1 1 d . . . Cl1 Cl 0.72742(12) 0.28451(15) 0.92851(6) 0.0566(3) Uani 1 1 d . . . Cl2 Cl 0.79305(10) -0.05870(14) 0.79224(7) 0.0529(3) Uani 1 1 d . . . N1 N 0.3783(3) 0.2277(5) 0.5629(2) 0.0387(8) Uani 1 1 d . . . N2 N 0.9420(3) 0.7088(4) 0.63725(18) 0.0372(8) Uani 1 1 d . . . C7 C 0.4998(3) 0.1813(5) 0.6868(2) 0.0392(9) Uani 1 1 d . . . C6 C 0.3913(4) 0.1621(6) 0.6404(2) 0.0456(11) Uani 1 1 d . . . H6B H 0.3736 0.0485 0.6376 0.080 Uiso 1 1 d R . . H6A H 0.3446 0.2171 0.6660 0.080 Uiso 1 1 d R . . C1 C 0.3581(4) 0.3863(6) 0.5510(3) 0.0476(11) Uani 1 1 d . . . H1A H 0.3480 0.4533 0.5925 0.080 Uiso 1 1 d R . . C2 C 0.3523(4) 0.4532(7) 0.4814(3) 0.0554(13) Uani 1 1 d . . . H2A H 0.3367 0.5669 0.4735 0.080 Uiso 1 1 d R . . C3 C 0.3680(4) 0.3568(7) 0.4218(3) 0.0536(12) Uani 1 1 d . . . H3A H 0.3644 0.4031 0.3724 0.080 Uiso 1 1 d R . . C4 C 0.3891(4) 0.1952(6) 0.4346(3) 0.0531(12) Uani 1 1 d . . . H4A H 0.4002 0.1266 0.3938 0.080 Uiso 1 1 d R . . C5 C 0.3939(4) 0.1307(6) 0.5053(3) 0.0471(11) Uani 1 1 d . . . H5A H 0.4085 0.0171 0.5145 0.080 Uiso 1 1 d R . . C14 C 0.8819(3) 0.4803(5) 0.7100(2) 0.0327(8) Uani 1 1 d . . . C13 C 0.9504(4) 0.6298(6) 0.7122(2) 0.0425(10) Uani 1 1 d . . . H13B H 0.9316 0.7081 0.7465 0.080 Uiso 1 1 d R . . H13A H 1.0206 0.5990 0.7314 0.080 Uiso 1 1 d R . . C8 C 0.9971(4) 0.6528(6) 0.5887(3) 0.0480(11) Uani 1 1 d . . . H8A H 1.0448 0.5650 0.6034 0.080 Uiso 1 1 d R . . C9 C 0.9859(5) 0.7217(8) 0.5177(3) 0.0685(17) Uani 1 1 d . . . H9A H 1.0249 0.6816 0.4822 0.080 Uiso 1 1 d R . . C10 C 0.9165(6) 0.8477(9) 0.4975(3) 0.076(2) Uani 1 1 d . . . H10A H 0.9058 0.8945 0.4477 0.080 Uiso 1 1 d R . . C11 C 0.8650(5) 0.9065(7) 0.5494(3) 0.0677(17) Uani 1 1 d . . . H11A H 0.8194 0.9974 0.5366 0.080 Uiso 1 1 d R . . C12 C 0.8768(4) 0.8347(6) 0.6191(3) 0.0503(11) Uani 1 1 d . . . H12A H 0.8398 0.8755 0.6557 0.080 Uiso 1 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 0.04644(19) 0.03388(17) 0.04163(17) -0.00155(13) 0.01388(13) 0.00141(15) S1 0.0605(9) 0.1452(17) 0.0435(7) 0.0234(9) 0.0199(6) 0.0225(10) S2 0.0454(6) 0.0606(8) 0.0493(6) 0.0109(6) 0.0125(5) -0.0117(6) S3 0.0637(7) 0.0410(6) 0.0360(5) -0.0040(4) 0.0217(5) -0.0134(5) S4 0.0579(7) 0.0475(7) 0.0398(5) -0.0106(5) 0.0184(5) -0.0143(6) Cl1 0.0901(10) 0.0418(6) 0.0446(6) -0.0038(5) 0.0295(6) -0.0055(6) Cl2 0.0592(7) 0.0335(6) 0.0730(8) -0.0041(5) 0.0302(6) 0.0036(5) N1 0.0368(18) 0.0377(19) 0.0427(18) 0.0008(16) 0.0110(15) -0.0003(16) N2 0.0419(19) 0.0353(19) 0.0358(16) 0.0010(15) 0.0109(14) -0.0081(16) C7 0.043(2) 0.036(2) 0.041(2) 0.0043(17) 0.0138(18) 0.0058(18) C6 0.046(3) 0.053(3) 0.040(2) 0.007(2) 0.0147(19) -0.003(2) C1 0.058(3) 0.040(3) 0.046(2) -0.0026(19) 0.015(2) 0.006(2) C2 0.073(4) 0.043(3) 0.053(3) 0.007(2) 0.019(3) 0.010(3) C3 0.062(3) 0.058(3) 0.045(2) 0.008(2) 0.021(2) 0.007(3) C4 0.062(3) 0.054(3) 0.047(3) -0.007(2) 0.021(2) 0.009(2) C5 0.050(3) 0.041(3) 0.053(3) -0.004(2) 0.017(2) 0.004(2) C14 0.034(2) 0.034(2) 0.0307(17) 0.0040(15) 0.0087(16) 0.0024(16) C13 0.049(3) 0.048(3) 0.0304(19) 0.0029(18) 0.0079(18) -0.012(2) C8 0.056(3) 0.043(3) 0.050(2) -0.004(2) 0.022(2) -0.009(2) C9 0.089(5) 0.077(4) 0.048(3) -0.005(3) 0.032(3) -0.028(4) C10 0.095(5) 0.077(4) 0.050(3) 0.024(3) -0.001(3) -0.041(4) C11 0.067(4) 0.055(4) 0.072(4) 0.028(3) -0.006(3) -0.010(3) C12 0.041(3) 0.045(3) 0.063(3) 0.006(2) 0.006(2) -0.005(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 Cl2 2.4688(19) . ? Cd1 S3 2.5519(17) . ? Cd1 Cl1 2.5925(12) . ? Cd1 S2 2.7070(13) . ? Cd1 S1 2.7421(18) . ? S1 C7 1.657(4) . ? S2 C7 1.675(5) . ? S3 C14 1.699(4) . ? S4 C14 1.645(4) . ? N1 C1 1.338(6) . ? N1 C5 1.356(6) . ? N1 C6 1.474(5) . ? N2 C8 1.333(6) . ? N2 C12 1.345(6) . ? N2 C13 1.482(5) . ? C7 C6 1.520(6) . ? C1 C2 1.355(6) . ? C2 C3 1.383(7) . ? C3 C4 1.366(7) . ? C4 C5 1.369(7) . ? C14 C13 1.523(6) . ? C8 C9 1.379(7) . ? C9 C10 1.384(10) . ? C10 C11 1.356(9) . ? C11 C12 1.367(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 Cl2 Cd1 S3 117.29(6) . . ? Cl2 Cd1 Cl1 102.60(4) . . ? S3 Cd1 Cl1 83.77(4) . . ? Cl2 Cd1 S2 102.58(5) . . ? S3 Cd1 S2 105.41(4) . . ? Cl1 Cd1 S2 145.10(5) . . ? Cl2 Cd1 S1 102.48(6) . . ? S3 Cd1 S1 140.19(6) . . ? Cl1 Cd1 S1 86.26(5) . . ? S2 Cd1 S1 64.94(4) . . ? C7 S1 Cd1 85.73(17) . . ? C7 S2 Cd1 86.54(16) . . ? C14 S3 Cd1 111.49(15) . . ? C1 N1 C5 120.4(4) . . ? C1 N1 C6 119.2(4) . . ? C5 N1 C6 120.2(4) . . ? C8 N2 C12 121.3(4) . . ? C8 N2 C13 119.9(4) . . ? C12 N2 C13 118.8(4) . . ? C6 C7 S1 115.9(3) . . ? C6 C7 S2 121.3(3) . . ? S1 C7 S2 122.8(3) . . ? N1 C6 C7 113.4(4) . . ? N1 C1 C2 120.9(4) . . ? C1 C2 C3 119.8(5) . . ? C4 C3 C2 118.9(5) . . ? C3 C4 C5 120.0(5) . . ? N1 C5 C4 120.0(5) . . ? C13 C14 S4 121.3(3) . . ? C13 C14 S3 111.4(3) . . ? S4 C14 S3 127.2(3) . . ? N2 C13 C14 113.3(3) . . ? N2 C8 C9 119.8(5) . . ? C8 C9 C10 119.3(6) . . ? C11 C10 C9 119.3(5) . . ? C10 C11 C12 120.1(6) . . ? N2 C12 C11 120.1(5) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.755 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.100