# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Yu Hui' _publ_contact_author_email jiehuiyu@yahoo.com.cn _publ_author_name 'Yu Hui' data_1 _database_code_depnum_ccdc_archive 'CCDC 892524' #TrackingRef '- 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H28 Cd Cl2 N4 S2' _chemical_formula_weight 511.83 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' 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 5.8919(12) _cell_length_b 11.934(2) _cell_length_c 16.684(3) _cell_angle_alpha 73.06(3) _cell_angle_beta 87.16(3) _cell_angle_gamma 76.67(3) _cell_volume 1091.8(4) _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 0.254 _exptl_crystal_size_mid 0.221 _exptl_crystal_size_min 0.185 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 1.441 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.700 _exptl_absorpt_correction_T_max 0.766 _exptl_absorpt_process_details ; Process-auto, 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 10647 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4914 _reflns_number_gt 4336 _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^)+(0.0709P)^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 CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4914 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.1132 _refine_ls_wR_factor_gt 0.1067 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.175 _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 0.77812(3) 0.625696(17) 0.709076(12) 0.03525(10) Uani 1 1 d . . . Cl1 Cl 0.81352(14) 0.77751(8) 0.56588(5) 0.0507(2) Uani 1 1 d . . . Cl2 Cl 0.73726(14) 0.46865(9) 0.85210(5) 0.0593(2) Uani 1 1 d . . . S1 S 0.43124(16) 0.79746(10) 0.75028(10) 0.0783(4) Uani 1 1 d . . . N4 N 0.4963(4) 0.5599(2) 0.65249(17) 0.0444(6) Uani 1 1 d . . . N1 N 0.3107(4) 0.7832(2) 0.49434(15) 0.0415(5) Uani 1 1 d . . . H1A H 0.1669 0.7814 0.5149 0.080 Uiso 1 1 calc R . . H1B H 0.4117 0.7565 0.5381 0.080 Uiso 1 1 calc R . . N2 N 0.2763(4) 1.3818(2) -0.10830(15) 0.0437(6) Uani 1 1 d . . . H2A H 0.3611 1.4325 -0.1388 0.080 Uiso 1 1 calc R . . H2B H 0.1266 1.4116 -0.1257 0.080 Uiso 1 1 calc R . . N3 N 0.0677(4) 0.6795(3) 0.76853(18) 0.0503(7) Uani 1 1 d . . . S2 S 0.11839(14) 0.45252(7) 0.66387(6) 0.0473(2) Uani 1 1 d . . . C1 C 0.3689(6) 0.6993(3) 0.44147(19) 0.0487(7) Uani 1 1 d . . . H1D H 0.3395 0.6217 0.4725 0.058 Uiso 1 1 calc R . . H1C H 0.5333 0.6879 0.4283 0.058 Uiso 1 1 calc R . . C2 C 0.2247(6) 0.7481(3) 0.36096(18) 0.0448(7) Uani 1 1 d . . . H2D H 0.0617 0.7506 0.3741 0.054 Uiso 1 1 calc R . . H2C H 0.2728 0.6945 0.3262 0.054 Uiso 1 1 calc R . . C3 C 0.2517(5) 0.8733(2) 0.31259(18) 0.0361(6) Uani 1 1 d . . . H3A H 0.4186 0.8685 0.3027 0.043 Uiso 1 1 calc R . . C4 C 0.1744(6) 0.9552(3) 0.36911(18) 0.0473(7) Uani 1 1 d . . . H4B H 0.1908 1.0359 0.3395 0.057 Uiso 1 1 calc R . . H4C H 0.0110 0.9590 0.3822 0.057 Uiso 1 1 calc R . . C5 C 0.3172(7) 0.9101(3) 0.4496(2) 0.0515(8) Uani 1 1 d . . . H5A H 0.4775 0.9155 0.4371 0.062 Uiso 1 1 calc R . . H5B H 0.2568 0.9606 0.4856 0.062 Uiso 1 1 calc R . . C6 C 0.3595(7) 1.2619(3) -0.12357(19) 0.0529(8) Uani 1 1 d . . . H6A H 0.5258 1.2337 -0.1116 0.063 Uiso 1 1 calc R . . H6B H 0.3335 1.2695 -0.1820 0.063 Uiso 1 1 calc R . . C7 C 0.2322(7) 1.1716(3) -0.06887(18) 0.0494(7) Uani 1 1 d . . . H7A H 0.2936 1.0937 -0.0780 0.059 Uiso 1 1 calc R . . H7B H 0.0680 1.1962 -0.0847 0.059 Uiso 1 1 calc R . . C8 C 0.2579(5) 1.1606(3) 0.02383(17) 0.0402(6) Uani 1 1 d . . . H8A H 0.4249 1.1352 0.0382 0.048 Uiso 1 1 calc R . . C9 C 0.1696(6) 1.2843(3) 0.03627(18) 0.0438(7) Uani 1 1 d . . . H9A H 0.0038 1.3111 0.0232 0.053 Uiso 1 1 calc R . . H9B H 0.1915 1.2791 0.0946 0.053 Uiso 1 1 calc R . . C10 C 0.2945(6) 1.3757(3) -0.01826(19) 0.0470(7) Uani 1 1 d . . . H10A H 0.2269 1.4542 -0.0109 0.056 Uiso 1 1 calc R . . H10B H 0.4576 1.3539 -0.0012 0.056 Uiso 1 1 calc R . . C11 C 0.1280(6) 0.9215(3) 0.22729(18) 0.0416(6) Uani 1 1 d . . . H11A H -0.0387 0.9447 0.2350 0.050 Uiso 1 1 calc R . . H11B H 0.1558 0.8582 0.2000 0.050 Uiso 1 1 calc R . . C12 C 0.2118(6) 1.0298(3) 0.17098(17) 0.0441(7) Uani 1 1 d . . . H12A H 0.1526 1.0980 0.1925 0.053 Uiso 1 1 calc R . . H12B H 0.3808 1.0122 0.1747 0.053 Uiso 1 1 calc R . . C13 C 0.1397(6) 1.0654(3) 0.07969(18) 0.0453(7) Uani 1 1 d . . . H13A H -0.0280 1.0959 0.0746 0.054 Uiso 1 1 calc R . . H13B H 0.1773 0.9944 0.0600 0.054 Uiso 1 1 calc R . . C14 C 0.2189(5) 0.7272(3) 0.76040(19) 0.0400(6) Uani 1 1 d . . . C15 C 0.3393(5) 0.5160(2) 0.65846(16) 0.0310(5) 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 0.02547(14) 0.04065(14) 0.04011(14) -0.00812(9) -0.00064(9) -0.01264(9) Cl1 0.0426(4) 0.0503(4) 0.0522(4) 0.0009(3) -0.0021(4) -0.0160(3) Cl2 0.0350(4) 0.0772(6) 0.0498(4) 0.0091(4) 0.0035(4) -0.0170(4) S1 0.0359(4) 0.0587(6) 0.1604(12) -0.0586(7) 0.0188(6) -0.0191(4) N4 0.0324(12) 0.0494(15) 0.0564(15) -0.0201(12) 0.0047(12) -0.0140(11) N1 0.0409(13) 0.0403(13) 0.0373(11) -0.0043(10) -0.0025(11) -0.0054(10) N2 0.0356(12) 0.0459(14) 0.0422(12) -0.0009(10) 0.0039(11) -0.0103(10) N3 0.0331(13) 0.0741(19) 0.0599(16) -0.0392(15) 0.0108(12) -0.0206(13) S2 0.0363(4) 0.0424(4) 0.0739(5) -0.0275(4) 0.0116(4) -0.0181(3) C1 0.061(2) 0.0344(15) 0.0398(14) -0.0035(12) -0.0025(14) 0.0012(13) C2 0.064(2) 0.0305(14) 0.0401(14) -0.0086(11) -0.0023(14) -0.0117(13) C3 0.0386(14) 0.0323(13) 0.0360(12) -0.0070(10) 0.0005(12) -0.0085(11) C4 0.065(2) 0.0309(14) 0.0420(15) -0.0085(12) -0.0105(15) -0.0038(13) C5 0.071(2) 0.0389(16) 0.0455(15) -0.0105(13) -0.0089(16) -0.0142(15) C6 0.062(2) 0.0510(18) 0.0383(14) -0.0087(13) 0.0091(15) -0.0060(15) C7 0.069(2) 0.0420(17) 0.0367(14) -0.0113(12) -0.0012(15) -0.0111(15) C8 0.0433(16) 0.0407(15) 0.0330(13) -0.0052(11) -0.0041(12) -0.0086(12) C9 0.0510(17) 0.0435(16) 0.0382(14) -0.0116(12) 0.0083(13) -0.0153(13) C10 0.0527(18) 0.0477(17) 0.0440(15) -0.0137(13) 0.0064(14) -0.0182(14) C11 0.0509(17) 0.0363(14) 0.0368(13) -0.0069(11) -0.0032(13) -0.0123(12) C12 0.0583(19) 0.0402(15) 0.0333(13) -0.0057(11) -0.0023(13) -0.0159(13) C13 0.0547(18) 0.0424(16) 0.0382(14) -0.0047(12) -0.0070(14) -0.0168(14) C14 0.0254(12) 0.0506(17) 0.0511(16) -0.0270(14) 0.0011(12) -0.0066(11) C15 0.0288(12) 0.0300(12) 0.0342(12) -0.0104(10) -0.0002(10) -0.0051(10) _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 2.314(3) 1_655 ? Cd1 N4 2.335(3) . ? Cd1 Cl1 2.5762(12) . ? Cd1 Cl2 2.6095(12) . ? Cd1 S1 2.7571(13) . ? Cd1 S2 2.7763(12) 1_655 ? S1 C14 1.636(3) . ? N4 C15 1.151(4) . ? N1 C5 1.490(4) . ? N1 C1 1.492(4) . ? N2 C10 1.491(4) . ? N2 C6 1.492(4) . ? N3 C14 1.146(4) . ? N3 Cd1 2.314(3) 1_455 ? S2 C15 1.636(3) . ? S2 Cd1 2.7763(12) 1_455 ? C1 C2 1.515(4) . ? C2 C3 1.518(4) . ? C3 C11 1.523(4) . ? C3 C4 1.530(4) . ? C4 C5 1.511(4) . ? C6 C7 1.513(5) . ? C7 C8 1.526(4) . ? C8 C9 1.520(4) . ? C8 C13 1.526(4) . ? C9 C10 1.511(4) . ? C11 C12 1.529(4) . ? C12 C13 1.511(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 N3 Cd1 N4 176.74(9) 1_655 . ? N3 Cd1 Cl1 92.14(9) 1_655 . ? N4 Cd1 Cl1 90.09(8) . . ? N3 Cd1 Cl2 89.29(9) 1_655 . ? N4 Cd1 Cl2 88.46(8) . . ? Cl1 Cd1 Cl2 178.46(3) . . ? N3 Cd1 S1 92.76(7) 1_655 . ? N4 Cd1 S1 89.64(7) . . ? Cl1 Cd1 S1 89.39(5) . . ? Cl2 Cd1 S1 91.13(5) . . ? N3 Cd1 S2 88.88(7) 1_655 1_655 ? N4 Cd1 S2 88.75(7) . 1_655 ? Cl1 Cd1 S2 89.94(4) . 1_655 ? Cl2 Cd1 S2 89.51(4) . 1_655 ? S1 Cd1 S2 178.25(3) . 1_655 ? C14 S1 Cd1 98.05(10) . . ? C15 N4 Cd1 152.2(2) . . ? C5 N1 C1 114.5(2) . . ? C10 N2 C6 112.6(2) . . ? C14 N3 Cd1 149.3(3) . 1_455 ? C15 S2 Cd1 98.51(9) . 1_455 ? N1 C1 C2 111.0(2) . . ? C1 C2 C3 111.7(3) . . ? C2 C3 C11 113.6(3) . . ? C2 C3 C4 107.9(2) . . ? C11 C3 C4 113.3(2) . . ? C5 C4 C3 111.5(3) . . ? N1 C5 C4 111.2(3) . . ? N2 C6 C7 110.7(2) . . ? C6 C7 C8 111.7(3) . . ? C9 C8 C7 108.5(2) . . ? C9 C8 C13 113.4(2) . . ? C7 C8 C13 112.0(3) . . ? C10 C9 C8 112.1(2) . . ? N2 C10 C9 110.9(3) . . ? C3 C11 C12 112.1(3) . . ? C13 C12 C11 115.2(3) . . ? C12 C13 C8 113.3(3) . . ? N3 C14 S1 178.5(3) . . ? N4 C15 S2 178.0(3) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.578 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.130 # Attachment '- 2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 892525' #TrackingRef '- 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 Br2 Cd N4 S2' _chemical_formula_weight 572.62 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 7.3432(15) _cell_length_b 9.2378(18) _cell_length_c 14.238(3) _cell_angle_alpha 103.57(3) _cell_angle_beta 99.86(3) _cell_angle_gamma 98.14(3) _cell_volume 908.2(3) _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 YELLOW _exptl_crystal_size_max 0.523 _exptl_crystal_size_mid 0.214 _exptl_crystal_size_min 0.171 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.094 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 5.834 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.232 _exptl_absorpt_correction_T_max 0.369 _exptl_absorpt_process_details ; Process-auto, 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 8925 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4126 _reflns_number_gt 3458 _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^)+(0.0391P)^2^+0.7805P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4126 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _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 0.34122(4) 0.46385(3) 0.36317(2) 0.03832(10) Uani 1 1 d . . . Br1 Br 0.24860(7) 0.71914(5) 0.35101(3) 0.04395(13) Uani 1 1 d . . . Br2 Br 0.70045(6) 0.46690(5) 0.42858(3) 0.03853(12) Uani 1 1 d . . . S1 S 0.1258(2) 0.21983(13) 0.36938(9) 0.0539(3) Uani 1 1 d . . . S2 S 0.38355(19) 0.14043(13) 0.04321(9) 0.0491(3) Uani 1 1 d . . . N1 N 0.6686(5) 1.0805(4) 0.4051(3) 0.0448(9) Uani 1 1 d . . . H1A H 0.6571 1.1574 0.4498 0.054 Uiso 1 1 calc R . . N2 N 0.8479(5) 0.2343(4) -0.0399(3) 0.0464(9) Uani 1 1 d . . . H2A H 0.8651 0.1607 -0.0851 0.056 Uiso 1 1 calc R . . N3 N 0.1007(6) -0.0008(4) 0.1925(3) 0.0535(10) Uani 1 1 d . . . N4 N 0.3535(6) 0.3691(4) 0.2026(3) 0.0526(10) Uani 1 1 d . . . C1 C 0.6088(7) 1.0747(5) 0.3103(4) 0.0525(12) Uani 1 1 d . . . H1B H 0.5545 1.1525 0.2931 0.063 Uiso 1 1 calc R . . C2 C 0.6274(7) 0.9554(5) 0.2390(3) 0.0475(10) Uani 1 1 d . . . H2B H 0.5864 0.9520 0.1729 0.057 Uiso 1 1 calc R . . C3 C 0.7063(6) 0.8387(5) 0.2631(3) 0.0382(9) Uani 1 1 d . . . C4 C 0.7663(6) 0.8480(5) 0.3631(3) 0.0442(10) Uani 1 1 d . . . H4B H 0.8201 0.7714 0.3823 0.053 Uiso 1 1 calc R . . C5 C 0.7451(7) 0.9712(5) 0.4328(3) 0.0446(10) Uani 1 1 d . . . H5A H 0.7844 0.9783 0.4996 0.053 Uiso 1 1 calc R . . C6 C 0.7759(7) 0.3477(5) -0.0665(4) 0.0480(11) Uani 1 1 d . . . H6A H 0.7446 0.3465 -0.1329 0.058 Uiso 1 1 calc R . . C7 C 0.7491(6) 0.4658(5) 0.0055(4) 0.0456(10) Uani 1 1 d . . . H7A H 0.6986 0.5448 -0.0122 0.055 Uiso 1 1 calc R . . C8 C 0.7966(6) 0.4681(5) 0.1044(3) 0.0418(10) Uani 1 1 d . . . C9 C 0.8697(6) 0.3469(5) 0.1275(3) 0.0463(10) Uani 1 1 d . . . H9A H 0.9022 0.3444 0.1930 0.056 Uiso 1 1 calc R . . C10 C 0.8934(6) 0.2317(5) 0.0537(4) 0.0469(11) Uani 1 1 d . . . H10A H 0.9421 0.1505 0.0692 0.056 Uiso 1 1 calc R . . C11 C 0.7254(7) 0.7145(5) 0.1805(4) 0.0483(11) Uani 1 1 d . . . H11A H 0.6994 0.7284 0.1173 0.058 Uiso 1 1 calc R . . C12 C 0.7750(6) 0.5884(5) 0.1883(4) 0.0456(10) Uani 1 1 d . . . H12A H 0.7987 0.5723 0.2510 0.055 Uiso 1 1 calc R . . C13 C 0.1132(6) 0.0913(5) 0.2641(3) 0.0398(9) Uani 1 1 d . . . C14 C 0.3656(6) 0.2728(5) 0.1364(3) 0.0366(8) 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 0.04752(18) 0.03005(16) 0.03356(17) 0.00295(12) 0.00514(13) 0.00834(13) Br1 0.0587(3) 0.0377(2) 0.0374(2) 0.00909(17) 0.00914(19) 0.0185(2) Br2 0.0448(2) 0.0367(2) 0.0330(2) 0.00559(16) 0.00854(17) 0.00992(18) S1 0.0772(8) 0.0390(6) 0.0376(6) -0.0020(5) 0.0229(6) -0.0070(6) S2 0.0685(7) 0.0408(6) 0.0397(6) 0.0052(5) 0.0219(5) 0.0120(6) N1 0.051(2) 0.0344(18) 0.044(2) -0.0036(15) 0.0113(17) 0.0138(17) N2 0.0430(19) 0.0351(18) 0.049(2) -0.0121(16) 0.0111(17) 0.0054(16) N3 0.071(3) 0.038(2) 0.047(2) -0.0020(17) 0.023(2) 0.0020(19) N4 0.070(3) 0.045(2) 0.034(2) -0.0008(17) 0.0085(19) 0.005(2) C1 0.058(3) 0.040(2) 0.058(3) 0.009(2) 0.007(2) 0.017(2) C2 0.054(3) 0.049(3) 0.036(2) 0.0064(19) 0.005(2) 0.012(2) C3 0.0348(19) 0.035(2) 0.036(2) -0.0035(17) 0.0081(17) -0.0001(17) C4 0.048(2) 0.030(2) 0.055(3) 0.0094(19) 0.013(2) 0.0090(19) C5 0.053(2) 0.045(2) 0.029(2) 0.0028(18) 0.0057(19) 0.007(2) C6 0.050(2) 0.049(3) 0.041(2) 0.010(2) 0.010(2) 0.001(2) C7 0.045(2) 0.035(2) 0.059(3) 0.016(2) 0.009(2) 0.009(2) C8 0.038(2) 0.034(2) 0.051(3) 0.0022(18) 0.0133(19) 0.0052(18) C9 0.050(2) 0.046(2) 0.036(2) 0.0044(19) 0.0013(19) 0.007(2) C10 0.045(2) 0.037(2) 0.052(3) 0.0051(19) -0.002(2) 0.010(2) C11 0.054(3) 0.042(2) 0.042(3) 0.002(2) 0.006(2) 0.010(2) C12 0.045(2) 0.039(2) 0.048(3) 0.0047(19) 0.010(2) 0.003(2) C13 0.044(2) 0.0300(19) 0.044(2) 0.0069(18) 0.0148(19) 0.0030(18) C14 0.040(2) 0.039(2) 0.030(2) 0.0112(17) 0.0042(17) 0.0048(18) _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 N4 2.271(4) . ? Cd1 Br1 2.5806(7) . ? Cd1 S1 2.5931(15) . ? Cd1 Br2 2.6367(9) . ? Cd1 Br2 2.9615(8) 2_666 ? Br2 Cd1 2.9615(8) 2_666 ? S1 C13 1.659(4) . ? S2 C14 1.618(4) . ? N1 C5 1.327(6) . ? N1 C1 1.333(6) . ? N2 C10 1.323(6) . ? N2 C6 1.340(6) . ? N3 C13 1.144(5) . ? N4 C14 1.160(5) . ? C1 C2 1.352(6) . ? C2 C3 1.377(6) . ? C3 C4 1.395(6) . ? C3 C11 1.479(6) . ? C4 C5 1.370(6) . ? C6 C7 1.373(6) . ? C7 C8 1.386(7) . ? C8 C9 1.390(6) . ? C8 C12 1.476(6) . ? C9 C10 1.363(6) . ? C11 C12 1.291(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 N4 Cd1 Br1 98.62(11) . . ? N4 Cd1 S1 93.43(12) . . ? Br1 Cd1 S1 128.02(4) . . ? N4 Cd1 Br2 93.49(12) . . ? Br1 Cd1 Br2 117.05(3) . . ? S1 Cd1 Br2 112.37(4) . . ? N4 Cd1 Br2 170.21(11) . 2_666 ? Br1 Cd1 Br2 89.33(3) . 2_666 ? S1 Cd1 Br2 77.11(4) . 2_666 ? Br2 Cd1 Br2 87.91(3) . 2_666 ? Cd1 Br2 Cd1 92.09(3) . 2_666 ? C13 S1 Cd1 106.50(15) . . ? C5 N1 C1 122.0(4) . . ? C10 N2 C6 122.2(4) . . ? C14 N4 Cd1 152.8(4) . . ? N1 C1 C2 119.8(4) . . ? C1 C2 C3 120.9(4) . . ? C2 C3 C4 117.8(4) . . ? C2 C3 C11 117.3(4) . . ? C4 C3 C11 124.9(4) . . ? C5 C4 C3 119.3(4) . . ? N1 C5 C4 120.2(4) . . ? N2 C6 C7 119.1(4) . . ? C6 C7 C8 120.5(4) . . ? C7 C8 C9 117.8(4) . . ? C7 C8 C12 125.6(4) . . ? C9 C8 C12 116.7(4) . . ? C10 C9 C8 119.8(4) . . ? N2 C10 C9 120.6(4) . . ? C12 C11 C3 125.9(5) . . ? C11 C12 C8 124.4(5) . . ? N3 C13 S1 177.7(4) . . ? N4 C14 S2 179.1(4) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.020 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.120 # Attachment '- 3.CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 892526' #TrackingRef '- 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H10 Cd2 Cl0 N8 S8' _chemical_formula_weight 795.60 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' 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 5.8896(12) _cell_length_b 13.286(3) _cell_length_c 17.001(3) _cell_angle_alpha 85.77(3) _cell_angle_beta 81.61(3) _cell_angle_gamma 87.58(3) _cell_volume 1311.8(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 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.014 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 2.281 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.734 _exptl_absorpt_correction_T_max 0.796 _exptl_absorpt_process_details ; Process-auto, 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 12902 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.45 _reflns_number_total 5910 _reflns_number_gt 4818 _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^)+(0.0211P)^2^+3.2722P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5910 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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 -0.85776(5) 0.14060(2) 0.44822(2) 0.03302(9) Uani 1 1 d . . . Cd2 Cd -1.11662(5) 0.63140(2) -0.033438(18) 0.02811(8) Uani 1 1 d . . . S1 S -0.56358(19) 0.16874(11) 0.31326(7) 0.0429(3) Uani 1 1 d . . . S2 S -0.84109(17) -0.06755(8) 0.41643(7) 0.0322(2) Uani 1 1 d . . . S3 S -0.8288(2) 0.32132(9) 0.49538(8) 0.0457(3) Uani 1 1 d . . . S4 S -1.45009(18) 0.62001(9) 0.10013(7) 0.0362(2) Uani 1 1 d . . . S5 S -0.83096(17) 0.65680(9) -0.16740(7) 0.0356(2) Uani 1 1 d . . . S6 S -1.1053(2) 0.81164(9) 0.01921(8) 0.0422(3) Uani 1 1 d . . . S7 S -1.0739(2) 0.66428(10) 0.22731(8) 0.0433(3) Uani 1 1 d . . . S8 S -1.1722(2) 0.79944(10) 0.27163(8) 0.0442(3) Uani 1 1 d . . . N1 N -0.1546(6) 0.1632(3) 0.3784(2) 0.0429(10) Uani 1 1 d . . . N2 N -0.4062(6) -0.1057(3) 0.4629(2) 0.0404(9) Uani 1 1 d . . . N3 N -1.1953(9) 0.4254(4) 0.4346(3) 0.0687(15) Uani 1 1 d . . . N4 N -1.8296(5) 0.5538(3) 0.0403(2) 0.0301(7) Uani 1 1 d . . . N5 N -0.4040(6) 0.6551(3) -0.1125(2) 0.0371(9) Uani 1 1 d . . . N6 N -0.6788(8) 0.8835(4) -0.0529(3) 0.0628(13) Uani 1 1 d . . . N7 N -0.5356(7) 0.5190(4) 0.3606(3) 0.0560(13) Uani 1 1 d . . . H7A H -0.4315 0.4892 0.3853 0.067 Uiso 1 1 calc R . . N8 N -0.7049(7) 1.0334(3) 0.1419(2) 0.0459(10) Uani 1 1 d . . . H8A H -0.6173 1.0797 0.1178 0.055 Uiso 1 1 calc R . . C1 C -0.5935(9) 0.6147(5) 0.3728(3) 0.0533(13) Uani 1 1 d . . . H1A H -0.5214 0.6483 0.4080 0.064 Uiso 1 1 calc R . . C2 C -0.7572(8) 0.6646(3) 0.3346(3) 0.0372(10) Uani 1 1 d . . . H2A H -0.7960 0.7320 0.3426 0.045 Uiso 1 1 calc R . . C3 C -0.8642(7) 0.6127(3) 0.2836(2) 0.0320(9) Uani 1 1 d . . . C4 C -0.7999(10) 0.5122(4) 0.2723(3) 0.0480(12) Uani 1 1 d . . . H4A H -0.8701 0.4758 0.2384 0.058 Uiso 1 1 calc R . . C5 C -0.6336(10) 0.4683(4) 0.3115(3) 0.0559(15) Uani 1 1 d . . . H5A H -0.5878 0.4015 0.3038 0.067 Uiso 1 1 calc R . . C6 C -0.9050(9) 1.0596(4) 0.1833(3) 0.0467(12) Uani 1 1 d . . . H6A H -0.9487 1.1275 0.1858 0.056 Uiso 1 1 calc R . . C7 C -1.0463(8) 0.9881(4) 0.2220(3) 0.0407(11) Uani 1 1 d . . . H7B H -1.1857 1.0070 0.2511 0.049 Uiso 1 1 calc R . . C8 C -0.9823(7) 0.8871(3) 0.2179(2) 0.0335(9) Uani 1 1 d . . . C9 C -0.7726(8) 0.8610(4) 0.1735(3) 0.0389(10) Uani 1 1 d . . . H9A H -0.7261 0.7936 0.1690 0.047 Uiso 1 1 calc R . . C10 C -0.6373(8) 0.9365(4) 0.1368(3) 0.0451(11) Uani 1 1 d . . . H10A H -0.4957 0.9203 0.1079 0.054 Uiso 1 1 calc R . . C11 C -0.3253(7) 0.1664(3) 0.3527(2) 0.0318(9) Uani 1 1 d . . . C12 C -0.5855(7) -0.0905(3) 0.4447(2) 0.0281(8) Uani 1 1 d . . . C13 C -1.0446(9) 0.3822(4) 0.4587(3) 0.0440(11) Uani 1 1 d . . . C14 C -1.6704(6) 0.5824(3) 0.0639(2) 0.0262(8) Uani 1 1 d . . . C15 C -0.5809(7) 0.6560(3) -0.1341(2) 0.0296(9) Uani 1 1 d . . . C16 C -0.8532(8) 0.8533(4) -0.0233(3) 0.0407(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 0.02365(15) 0.03528(17) 0.04156(19) 0.00025(13) -0.01148(13) 0.00120(12) Cd2 0.02007(14) 0.03087(16) 0.03411(17) 0.00058(12) -0.00706(11) -0.00294(11) S1 0.0262(5) 0.0677(8) 0.0361(6) -0.0005(6) -0.0101(5) -0.0039(5) S2 0.0274(5) 0.0346(5) 0.0368(6) -0.0017(4) -0.0129(4) 0.0002(4) S3 0.0455(7) 0.0364(6) 0.0586(8) -0.0070(6) -0.0181(6) 0.0036(5) S4 0.0263(5) 0.0505(7) 0.0336(6) -0.0090(5) -0.0041(4) -0.0104(5) S5 0.0221(5) 0.0527(7) 0.0329(6) 0.0011(5) -0.0082(4) -0.0036(5) S6 0.0398(6) 0.0376(6) 0.0488(7) -0.0092(5) -0.0004(5) -0.0066(5) S7 0.0469(7) 0.0448(7) 0.0422(7) -0.0045(5) -0.0176(5) -0.0065(5) S8 0.0343(6) 0.0474(7) 0.0468(7) 0.0042(5) 0.0033(5) 0.0039(5) N1 0.0277(19) 0.056(3) 0.046(2) 0.0024(19) -0.0111(17) -0.0016(17) N2 0.0298(19) 0.044(2) 0.050(2) -0.0078(18) -0.0151(17) 0.0092(17) N3 0.068(3) 0.058(3) 0.080(4) 0.006(3) -0.020(3) 0.020(3) N4 0.0237(16) 0.0344(19) 0.0330(19) -0.0008(15) -0.0068(14) -0.0050(14) N5 0.0250(18) 0.050(2) 0.037(2) 0.0015(17) -0.0073(15) -0.0011(16) N6 0.055(3) 0.058(3) 0.075(3) -0.005(3) -0.003(2) -0.023(2) N7 0.044(2) 0.065(3) 0.051(3) 0.023(2) 0.000(2) 0.016(2) N8 0.054(3) 0.043(2) 0.042(2) 0.0051(18) -0.0115(19) -0.014(2) C1 0.045(3) 0.068(4) 0.048(3) 0.004(3) -0.014(2) -0.002(3) C2 0.040(2) 0.035(2) 0.037(2) -0.0013(19) -0.009(2) -0.0012(19) C3 0.035(2) 0.034(2) 0.025(2) 0.0003(17) 0.0012(17) -0.0039(18) C4 0.070(3) 0.032(2) 0.039(3) -0.003(2) 0.003(2) -0.002(2) C5 0.071(4) 0.039(3) 0.048(3) 0.008(2) 0.014(3) 0.013(3) C6 0.053(3) 0.036(3) 0.052(3) -0.003(2) -0.015(2) 0.007(2) C7 0.042(2) 0.042(3) 0.037(3) -0.007(2) -0.005(2) 0.010(2) C8 0.033(2) 0.040(2) 0.027(2) -0.0016(18) -0.0076(17) 0.0022(18) C9 0.036(2) 0.040(2) 0.040(3) -0.003(2) -0.0007(19) 0.0032(19) C10 0.039(3) 0.055(3) 0.041(3) -0.006(2) -0.002(2) -0.002(2) C11 0.027(2) 0.037(2) 0.030(2) 0.0013(18) -0.0021(17) 0.0014(17) C12 0.033(2) 0.0241(19) 0.028(2) -0.0057(16) -0.0054(17) 0.0018(16) C13 0.046(3) 0.036(2) 0.048(3) 0.001(2) -0.002(2) 0.000(2) C14 0.0231(18) 0.030(2) 0.0245(19) 0.0011(16) -0.0002(15) -0.0001(16) C15 0.025(2) 0.036(2) 0.027(2) 0.0008(17) 0.0001(16) -0.0011(17) C16 0.045(3) 0.036(2) 0.045(3) -0.003(2) -0.014(2) -0.009(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 N1 2.250(4) 1_455 ? Cd1 N2 2.331(4) 2_456 ? Cd1 S3 2.6067(14) . ? Cd1 S1 2.6785(15) . ? Cd1 S2 2.8296(15) 2_356 ? Cd1 S2 2.8516(13) . ? Cd2 N5 2.308(4) 1_455 ? Cd2 N4 2.402(3) 1_655 ? Cd2 N4 2.507(4) 2_265 ? Cd2 S6 2.6244(14) . ? Cd2 S5 2.6357(14) . ? Cd2 S4 2.7765(14) . ? S1 C11 1.639(4) . ? S2 C12 1.656(4) . ? S2 Cd1 2.8296(15) 2_356 ? S3 C13 1.652(5) . ? S4 C14 1.626(4) . ? S5 C15 1.652(4) . ? S6 C16 1.652(5) . ? S7 C3 1.757(4) . ? S7 S8 2.028(2) . ? S8 C8 1.759(5) . ? N1 C11 1.152(5) . ? N1 Cd1 2.250(4) 1_655 ? N2 C12 1.149(5) . ? N2 Cd1 2.331(4) 2_456 ? N3 C13 1.145(6) . ? N4 C14 1.161(5) . ? N4 Cd2 2.402(3) 1_455 ? N4 Cd2 2.507(4) 2_265 ? N5 C15 1.153(5) . ? N5 Cd2 2.308(4) 1_655 ? N6 C16 1.150(6) . ? N7 C5 1.318(8) . ? N7 C1 1.327(7) . ? N8 C6 1.329(6) . ? N8 C10 1.337(6) . ? C1 C2 1.363(7) . ? C2 C3 1.380(6) . ? C3 C4 1.393(6) . ? C4 C5 1.352(8) . ? C6 C7 1.357(7) . ? C7 C8 1.382(6) . ? C8 C9 1.395(6) . ? C9 C10 1.364(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 N1 Cd1 N2 170.67(14) 1_455 2_456 ? N1 Cd1 S3 101.09(12) 1_455 . ? N2 Cd1 S3 80.75(10) 2_456 . ? N1 Cd1 S1 89.97(11) 1_455 . ? N2 Cd1 S1 98.97(10) 2_456 . ? S3 Cd1 S1 95.81(5) . . ? N1 Cd1 S2 90.15(11) 1_455 2_356 ? N2 Cd1 S2 80.55(10) 2_456 2_356 ? S3 Cd1 S2 96.03(5) . 2_356 ? S1 Cd1 S2 167.91(4) . 2_356 ? N1 Cd1 S2 88.26(12) 1_455 . ? N2 Cd1 S2 89.62(10) 2_456 . ? S3 Cd1 S2 170.33(4) . . ? S1 Cd1 S2 86.55(5) . . ? S2 Cd1 S2 81.37(5) 2_356 . ? N5 Cd2 N4 162.34(13) 1_455 1_655 ? N5 Cd2 N4 85.82(13) 1_455 2_265 ? N4 Cd2 N4 76.66(13) 1_655 2_265 ? N5 Cd2 S6 101.27(11) 1_455 . ? N4 Cd2 S6 96.20(9) 1_655 . ? N4 Cd2 S6 162.68(8) 2_265 . ? N5 Cd2 S5 85.62(9) 1_455 . ? N4 Cd2 S5 94.13(9) 1_655 . ? N4 Cd2 S5 96.87(9) 2_265 . ? S6 Cd2 S5 99.40(5) . . ? N5 Cd2 S4 89.10(9) 1_455 . ? N4 Cd2 S4 91.97(9) 1_655 . ? N4 Cd2 S4 86.26(9) 2_265 . ? S6 Cd2 S4 78.15(5) . . ? S5 Cd2 S4 173.64(4) . . ? C11 S1 Cd1 98.20(15) . . ? C12 S2 Cd1 102.48(15) . 2_356 ? C12 S2 Cd1 94.33(14) . . ? Cd1 S2 Cd1 98.63(5) 2_356 . ? C13 S3 Cd1 101.75(19) . . ? C14 S4 Cd2 102.09(14) . . ? C15 S5 Cd2 101.51(14) . . ? C16 S6 Cd2 103.68(18) . . ? C3 S7 S8 105.77(16) . . ? C8 S8 S7 105.54(16) . . ? C11 N1 Cd1 169.3(4) . 1_655 ? C12 N2 Cd1 155.6(4) . 2_456 ? C14 N4 Cd2 134.6(3) . 1_455 ? C14 N4 Cd2 120.8(3) . 2_265 ? Cd2 N4 Cd2 103.34(13) 1_455 2_265 ? C15 N5 Cd2 161.9(3) . 1_655 ? C5 N7 C1 121.7(5) . . ? C6 N8 C10 121.2(4) . . ? N7 C1 C2 120.8(5) . . ? C1 C2 C3 118.5(5) . . ? C2 C3 C4 119.2(4) . . ? C2 C3 S7 125.3(3) . . ? C4 C3 S7 115.4(4) . . ? C5 C4 C3 118.8(5) . . ? N7 C5 C4 120.9(5) . . ? N8 C6 C7 120.6(5) . . ? C6 C7 C8 119.8(4) . . ? C7 C8 C9 118.8(4) . . ? C7 C8 S8 116.9(3) . . ? C9 C8 S8 124.3(4) . . ? C10 C9 C8 118.5(4) . . ? N8 C10 C9 121.1(5) . . ? N1 C11 S1 177.9(4) . . ? N2 C12 S2 178.7(4) . . ? N3 C13 S3 178.7(5) . . ? N4 C14 S4 177.9(4) . . ? N5 C15 S5 178.5(4) . . ? N6 C16 S6 179.2(5) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.800 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.109 # Attachment '- 4.CIF' data_4 _database_code_depnum_ccdc_archive 'CCDC 892527' #TrackingRef '- 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 Br2 Cd N4 S4' _chemical_formula_weight 610.70 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ORTHORHOMBIC _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 10.999(2) _cell_length_b 16.628(3) _cell_length_c 5.1034(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 933.4(3) _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 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 5.899 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.469 _exptl_absorpt_correction_T_max 0.554 _exptl_absorpt_process_details ; Process-auto, 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 8781 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2125 _reflns_number_gt 2017 _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^)+(0.0160P)^2^+0.0271P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(7) _refine_ls_number_reflns 2125 _refine_ls_number_parameters 105 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0219 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0420 _refine_ls_wR_factor_gt 0.0414 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _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 0.5000 0.5000 0.21026(5) 0.03740(8) Uani 1 2 d S . . S1 S 0.43691(7) 0.04470(4) 0.07735(13) 0.04438(17) Uani 1 1 d . . . S2 S 0.66335(6) 0.42336(4) 0.46540(14) 0.03984(16) Uani 1 1 d . . . Br1 Br 0.62538(2) 0.599996(18) -0.06427(6) 0.04831(9) Uani 1 1 d . . . C1 C 0.6208(3) 0.16259(19) 0.6462(6) 0.0500(7) Uani 1 1 d . . . H1A H 0.6878 0.1563 0.7555 0.060 Uiso 1 1 calc R . . C2 C 0.5926(2) 0.10387(17) 0.4683(5) 0.0409(6) Uani 1 1 d . . . H2A H 0.6399 0.0577 0.4549 0.049 Uiso 1 1 calc R . . C3 C 0.4922(2) 0.11473(14) 0.3089(4) 0.0327(5) Uani 1 1 d . . . C4 C 0.4244(2) 0.18541(16) 0.3286(5) 0.0383(6) Uani 1 1 d . . . H4A H 0.3576 0.1939 0.2203 0.046 Uiso 1 1 calc R . . C5 C 0.4574(2) 0.24163(18) 0.5083(6) 0.0477(7) Uani 1 1 d . . . H5A H 0.4134 0.2892 0.5225 0.057 Uiso 1 1 calc R . . C6 C 0.6778(2) 0.35221(15) 0.2388(5) 0.0339(5) Uani 1 1 d . . . N1 N 0.5525(2) 0.22884(16) 0.6638(5) 0.0486(6) Uani 1 1 d . . . H1B H 0.5706 0.2644 0.7796 0.058 Uiso 1 1 calc R . . N2 N 0.6866(2) 0.30163(15) 0.0877(5) 0.0469(6) 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 0.02953(11) 0.02730(13) 0.05537(16) 0.000 0.000 0.00161(10) S1 0.0589(4) 0.0328(4) 0.0415(4) -0.0014(3) -0.0155(4) -0.0004(3) S2 0.0425(3) 0.0373(4) 0.0397(3) -0.0033(3) -0.0062(3) 0.0060(3) Br1 0.03985(14) 0.04484(17) 0.06025(18) 0.01432(14) -0.00040(14) -0.00678(12) C1 0.0438(15) 0.060(2) 0.0460(15) 0.0059(14) -0.0102(14) -0.0162(15) C2 0.0372(12) 0.0416(16) 0.0440(14) 0.0028(13) -0.0045(12) -0.0004(11) C3 0.0361(11) 0.0293(12) 0.0327(11) 0.0028(9) 0.0017(14) -0.0040(10) C4 0.0339(12) 0.0327(15) 0.0483(15) -0.0013(11) -0.0040(12) -0.0021(10) C5 0.0479(14) 0.0355(16) 0.0597(18) -0.0065(13) 0.0079(16) -0.0024(11) C6 0.0289(11) 0.0349(14) 0.0381(14) 0.0053(12) 0.0015(11) 0.0021(10) N1 0.0578(14) 0.0474(15) 0.0405(12) -0.0107(11) 0.0064(12) -0.0207(12) N2 0.0456(12) 0.0486(15) 0.0465(14) -0.0071(13) -0.0027(12) 0.0063(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 S2 2.5589(7) 2_665 ? Cd1 S2 2.5589(7) . ? Cd1 Br1 2.5748(4) 2_665 ? Cd1 Br1 2.5748(4) . ? S1 C3 1.767(2) . ? S1 S1 2.0337(15) 2_655 ? S2 C6 1.662(3) . ? C1 N1 1.336(4) . ? C1 C2 1.369(4) . ? C2 C3 1.384(4) . ? C3 C4 1.395(4) . ? C4 C5 1.359(4) . ? C5 N1 1.330(3) . ? C6 N2 1.145(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 S2 Cd1 S2 118.83(3) 2_665 . ? S2 Cd1 Br1 102.85(2) 2_665 2_665 ? S2 Cd1 Br1 109.35(2) . 2_665 ? S2 Cd1 Br1 109.35(2) 2_665 . ? S2 Cd1 Br1 102.85(2) . . ? Br1 Cd1 Br1 114.07(2) 2_665 . ? C3 S1 S1 104.29(9) . 2_655 ? C6 S2 Cd1 93.87(8) . . ? N1 C1 C2 120.3(3) . . ? C1 C2 C3 118.5(3) . . ? C2 C3 C4 119.6(2) . . ? C2 C3 S1 125.6(2) . . ? C4 C3 S1 114.80(19) . . ? C5 C4 C3 119.0(3) . . ? N1 C5 C4 120.2(3) . . ? N2 C6 S2 178.1(2) . . ? C5 N1 C1 122.3(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.295 _refine_diff_density_min -0.650 _refine_diff_density_rms 0.107 # Attachment '- 5.CIF' data_5 _database_code_depnum_ccdc_archive 'CCDC 892528' #TrackingRef '- 5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H9 Cd N5 S5' _chemical_formula_weight 508.01 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' Cd Cd -0.8075 1.2024 '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 TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4933(17) _cell_length_b 10.509(2) _cell_length_c 11.826(2) _cell_angle_alpha 81.38(3) _cell_angle_beta 73.21(3) _cell_angle_gamma 70.39(3) _cell_volume 950.3(3) _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 BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.472 _exptl_crystal_size_mid 0.271 _exptl_crystal_size_min 0.245 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 1.703 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.581 _exptl_absorpt_correction_T_max 0.659 _exptl_absorpt_process_details ; Process-auto, 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 9346 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4282 _reflns_number_gt 3811 _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^)+(0.0254P)^2^+0.4286P] 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 4282 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0669 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _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 0.31451(2) 0.300378(18) 0.545377(16) 0.04072(7) Uani 1 1 d . . . S1 S 0.46955(13) 0.10764(8) 0.70118(7) 0.0658(2) Uani 1 1 d . . . S2 S -0.00795(9) 0.28649(7) 0.65909(7) 0.05423(19) Uani 1 1 d . . . S3 S 0.24436(11) 0.48921(7) 0.70033(6) 0.05406(18) Uani 1 1 d . . . S4 S 0.22351(13) 0.08200(9) 0.02204(7) 0.0651(2) Uani 1 1 d . . . S5 S 0.22610(12) 0.27327(9) -0.04006(7) 0.0599(2) Uani 1 1 d . . . N1 N 0.6218(3) -0.1222(2) 0.57060(19) 0.0454(5) Uani 1 1 d . . . N2 N -0.1915(3) 0.5510(2) 0.5994(2) 0.0519(6) Uani 1 1 d . . . N3 N 0.4427(3) 0.6484(3) 0.5625(3) 0.0596(7) Uani 1 1 d . . . N4 N 0.1241(3) 0.1789(2) 0.2385(2) 0.0447(5) Uani 1 1 d . . . N5 N 0.3987(3) 0.2709(3) 0.11659(19) 0.0522(6) Uani 1 1 d . . . C1 C 0.0955(4) 0.1028(3) 0.1696(3) 0.0491(6) Uani 1 1 d . . . C2 C -0.0288(4) 0.0395(3) 0.2166(3) 0.0601(8) Uani 1 1 d . . . H2A H -0.0522 -0.0122 0.1699 0.072 Uiso 1 1 calc R . . C3 C -0.1185(4) 0.0535(3) 0.3339(3) 0.0614(8) Uani 1 1 d . . . H3A H -0.2014 0.0097 0.3669 0.074 Uiso 1 1 calc R . . C4 C -0.0862(3) 0.1318(3) 0.4023(3) 0.0539(7) Uani 1 1 d . . . H4B H -0.1464 0.1414 0.4814 0.065 Uiso 1 1 calc R . . C5 C 0.0363(3) 0.1956(3) 0.3517(2) 0.0468(6) Uani 1 1 d . . . H5B H 0.0582 0.2505 0.3962 0.056 Uiso 1 1 calc R . . C6 C 0.4066(4) 0.2865(3) 0.0008(2) 0.0495(6) Uani 1 1 d . . . C7 C 0.5413(5) 0.3169(4) -0.0833(3) 0.0646(9) Uani 1 1 d . . . H7A H 0.5439 0.3256 -0.1632 0.078 Uiso 1 1 calc R . . C8 C 0.6723(5) 0.3340(4) -0.0465(3) 0.0694(9) Uani 1 1 d . . . H8A H 0.7642 0.3558 -0.1013 0.083 Uiso 1 1 calc R . . C9 C 0.6656(4) 0.3184(4) 0.0725(3) 0.0622(8) Uani 1 1 d . . . H9A H 0.7527 0.3294 0.0994 0.075 Uiso 1 1 calc R . . C10 C 0.5277(4) 0.2863(4) 0.1503(3) 0.0609(8) Uani 1 1 d . . . H10A H 0.5240 0.2749 0.2305 0.073 Uiso 1 1 calc R . . C11 C 0.5603(3) -0.0263(2) 0.6224(2) 0.0368(5) Uani 1 1 d . . . C12 C -0.1160(3) 0.4424(3) 0.6237(2) 0.0408(5) Uani 1 1 d . . . C13 C 0.3636(3) 0.5807(3) 0.6180(3) 0.0453(6) Uani 1 1 d . . . H4A H 0.207(3) 0.209(3) 0.210(2) 0.036(7) 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 0.04266(11) 0.03108(10) 0.04474(11) -0.00584(7) -0.00985(8) -0.00627(7) S1 0.0958(6) 0.0422(4) 0.0551(4) -0.0176(3) -0.0395(4) 0.0077(4) S2 0.0522(4) 0.0350(3) 0.0575(4) 0.0060(3) 0.0027(3) -0.0083(3) S3 0.0716(5) 0.0437(4) 0.0458(4) -0.0063(3) -0.0104(3) -0.0188(3) S4 0.0894(6) 0.0581(5) 0.0550(4) -0.0130(4) -0.0141(4) -0.0314(4) S5 0.0777(5) 0.0628(5) 0.0452(4) 0.0036(3) -0.0232(4) -0.0260(4) N1 0.0502(12) 0.0359(11) 0.0455(11) -0.0052(9) -0.0179(10) -0.0017(9) N2 0.0424(11) 0.0472(14) 0.0522(13) 0.0051(10) -0.0059(10) -0.0047(10) N3 0.0450(13) 0.0454(14) 0.0823(18) -0.0174(13) -0.0041(13) -0.0107(11) N4 0.0413(12) 0.0467(13) 0.0478(12) 0.0019(10) -0.0141(10) -0.0156(10) N5 0.0598(14) 0.0637(16) 0.0355(11) -0.0032(10) -0.0067(10) -0.0267(12) C1 0.0558(16) 0.0393(14) 0.0555(15) 0.0015(12) -0.0218(13) -0.0145(12) C2 0.0682(19) 0.0444(16) 0.078(2) 0.0054(14) -0.0301(17) -0.0243(14) C3 0.0535(17) 0.0486(17) 0.079(2) 0.0150(15) -0.0167(16) -0.0204(13) C4 0.0414(14) 0.0499(17) 0.0579(17) 0.0111(13) -0.0119(13) -0.0050(12) C5 0.0388(13) 0.0487(15) 0.0471(14) 0.0017(11) -0.0126(11) -0.0066(11) C6 0.0648(17) 0.0443(15) 0.0387(13) -0.0042(11) -0.0107(13) -0.0175(13) C7 0.084(2) 0.073(2) 0.0365(14) -0.0027(14) -0.0037(15) -0.0342(18) C8 0.073(2) 0.080(2) 0.0517(17) -0.0067(16) 0.0044(16) -0.0345(18) C9 0.0604(18) 0.073(2) 0.0568(17) -0.0073(15) -0.0110(15) -0.0264(16) C10 0.0699(19) 0.078(2) 0.0419(14) -0.0026(14) -0.0131(14) -0.0327(17) C11 0.0409(12) 0.0332(12) 0.0353(11) 0.0012(9) -0.0160(10) -0.0062(9) C12 0.0398(12) 0.0419(14) 0.0354(12) -0.0021(10) -0.0011(10) -0.0131(10) C13 0.0410(13) 0.0383(14) 0.0554(15) -0.0141(12) -0.0160(12) -0.0027(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 N3 2.278(3) 2_666 ? Cd1 N1 2.311(2) 2_656 ? Cd1 N2 2.366(2) 2_566 ? Cd1 S3 2.7049(11) . ? Cd1 S2 2.7226(11) . ? Cd1 S1 2.7792(13) . ? S1 C11 1.641(2) . ? S2 C12 1.646(3) . ? S3 C13 1.643(3) . ? S4 C1 1.771(3) . ? S4 S5 2.0391(13) . ? S5 C6 1.787(3) . ? N1 C11 1.144(3) . ? N1 Cd1 2.311(2) 2_656 ? N2 C12 1.146(3) . ? N2 Cd1 2.366(2) 2_566 ? N3 C13 1.147(4) . ? N3 Cd1 2.278(3) 2_666 ? N4 C5 1.336(3) . ? N4 C1 1.342(4) . ? N4 H4A 0.83(3) . ? N5 C10 1.333(4) . ? N5 C6 1.340(3) . ? C1 C2 1.374(4) . ? C2 C3 1.379(5) . ? C2 H2A 0.9300 . ? C3 C4 1.373(5) . ? C3 H3A 0.9300 . ? C4 C5 1.370(4) . ? C4 H4B 0.9300 . ? C5 H5B 0.9300 . ? C6 C7 1.375(4) . ? C7 C8 1.377(5) . ? C7 H7A 0.9300 . ? C8 C9 1.379(5) . ? C8 H8A 0.9300 . ? C9 C10 1.372(4) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cd1 N1 91.21(9) 2_666 2_656 ? N3 Cd1 N2 82.66(10) 2_666 2_566 ? N1 Cd1 N2 88.90(8) 2_656 2_566 ? N3 Cd1 S3 91.41(7) 2_666 . ? N1 Cd1 S3 173.95(6) 2_656 . ? N2 Cd1 S3 96.84(7) 2_566 . ? N3 Cd1 S2 169.16(7) 2_666 . ? N1 Cd1 S2 93.73(7) 2_656 . ? N2 Cd1 S2 87.79(7) 2_566 . ? S3 Cd1 S2 84.62(4) . . ? N3 Cd1 S1 96.71(8) 2_666 . ? N1 Cd1 S1 86.00(6) 2_656 . ? N2 Cd1 S1 174.85(6) 2_566 . ? S3 Cd1 S1 88.28(3) . . ? S2 Cd1 S1 93.26(4) . . ? C11 S1 Cd1 102.05(9) . . ? C12 S2 Cd1 97.23(10) . . ? C13 S3 Cd1 98.79(9) . . ? C1 S4 S5 103.69(11) . . ? C6 S5 S4 102.73(11) . . ? C11 N1 Cd1 166.7(2) . 2_656 ? C12 N2 Cd1 146.2(2) . 2_566 ? C13 N3 Cd1 156.3(2) . 2_666 ? C5 N4 C1 122.5(3) . . ? C5 N4 H4A 120.1(19) . . ? C1 N4 H4A 117.0(19) . . ? C10 N5 C6 117.8(3) . . ? N4 C1 C2 119.2(3) . . ? N4 C1 S4 119.2(2) . . ? C2 C1 S4 121.6(2) . . ? C1 C2 C3 119.1(3) . . ? C1 C2 H2A 120.4 . . ? C3 C2 H2A 120.4 . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C5 C4 C3 118.8(3) . . ? C5 C4 H4B 120.6 . . ? C3 C4 H4B 120.6 . . ? N4 C5 C4 120.0(3) . . ? N4 C5 H5B 120.0 . . ? C4 C5 H5B 120.0 . . ? N5 C6 C7 122.8(3) . . ? N5 C6 S5 116.3(2) . . ? C7 C6 S5 120.8(2) . . ? C6 C7 C8 118.5(3) . . ? C6 C7 H7A 120.7 . . ? C8 C7 H7A 120.7 . . ? C7 C8 C9 119.2(3) . . ? C7 C8 H8A 120.4 . . ? C9 C8 H8A 120.4 . . ? C10 C9 C8 118.5(3) . . ? C10 C9 H9A 120.7 . . ? C8 C9 H9A 120.7 . . ? N5 C10 C9 123.1(3) . . ? N5 C10 H10A 118.4 . . ? C9 C10 H10A 118.4 . . ? N1 C11 S1 177.8(2) . . ? N2 C12 S2 179.8(3) . . ? N3 C13 S3 177.6(2) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.673 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.074