# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 913195' #TrackingRef '1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H12 Cd N6 O6 S3' _chemical_formula_weight 496.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pcca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 17.523(4) _cell_length_b 5.8825(17) _cell_length_c 17.164(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1769.2(7) _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 block _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 1.865 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.625 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.850 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 3741 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 23.30 _reflns_number_total 1275 _reflns_number_gt 1184 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMAR' _computing_cell_refinement 'Bruker SMAR' _computing_data_reduction 'Bruker SMAR' _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^)+(0.0800P)^2^+5.2501P] 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 1275 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1251 _refine_ls_wR_factor_gt 0.1225 _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 0.5000 0.0000 0.0000 0.0325(3) Uani 1 2 d S . . S1 S 0.48713(8) -0.2483(2) -0.13279(8) 0.0414(4) Uani 1 1 d . . . S2 S 0.7500 -0.5000 0.00400(8) 0.0276(5) Uani 1 2 d S . . O1 O 0.76882(19) -0.3047(5) 0.05405(16) 0.0335(8) Uani 1 1 d . . . O2 O 0.68479(18) -0.4423(6) -0.04579(17) 0.0349(8) Uani 1 1 d . . . OW1 O 0.6308(2) 0.0039(7) -0.0237(3) 0.0460(10) Uani 1 1 d . . . N1 N 0.7047(2) -0.2816(6) 0.1946(2) 0.0339(9) Uani 1 1 d . . . H1B H 0.7240 -0.2955 0.1488 0.041 Uiso 1 1 calc R . . N2 N 0.6809(2) -0.3399(7) 0.3158(2) 0.0361(10) Uani 1 1 d . . . H2B H 0.6817 -0.3983 0.3617 0.043 Uiso 1 1 calc R . . N3 N 0.4872(3) -0.6909(7) -0.0770(3) 0.0463(12) Uani 1 1 d . . . C1 C 0.6512(3) -0.1271(10) 0.2160(3) 0.0482(14) Uani 1 1 d . . . H1C H 0.6287 -0.0181 0.1842 0.058 Uiso 1 1 calc R . . C2 C 0.6366(3) -0.1621(10) 0.2927(3) 0.0496(14) Uani 1 1 d . . . H2C H 0.6028 -0.0802 0.3236 0.060 Uiso 1 1 calc R . . C3 C 0.7223(3) -0.4075(10) 0.2560(2) 0.0303(11) Uani 1 1 d . . . C4 C 0.4871(3) -0.5090(8) -0.0984(3) 0.0310(12) Uani 1 1 d . . . H02 H 0.652(5) -0.121(16) -0.008(4) 0.09(3) Uiso 1 1 d . . . H01 H 0.662(5) 0.096(15) -0.003(4) 0.08(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 0.0353(4) 0.0207(4) 0.0414(5) 0.00845(19) -0.00197(19) 0.00077(17) S1 0.0636(9) 0.0224(7) 0.0380(8) 0.0100(5) -0.0060(6) -0.0007(5) S2 0.0353(12) 0.0330(12) 0.0144(9) 0.000 0.000 0.0004(6) O1 0.0488(19) 0.0305(17) 0.0211(15) -0.0040(13) 0.0054(14) -0.0105(15) O2 0.0405(19) 0.0425(18) 0.0217(16) -0.0042(14) -0.0063(14) 0.0080(15) OW1 0.039(2) 0.039(2) 0.060(2) -0.0036(18) -0.004(2) -0.0011(17) N1 0.045(2) 0.035(2) 0.0214(19) 0.0032(16) 0.0024(16) 0.0097(18) N2 0.045(2) 0.047(2) 0.0173(18) 0.0049(17) 0.0026(17) 0.0131(19) N3 0.079(3) 0.019(2) 0.041(3) 0.005(2) -0.009(2) 0.000(2) C1 0.054(3) 0.054(3) 0.036(3) 0.002(3) -0.006(2) 0.021(3) C2 0.051(3) 0.060(4) 0.038(3) -0.005(3) 0.007(2) 0.027(3) C3 0.037(3) 0.038(3) 0.016(2) -0.0026(18) -0.0013(17) 0.008(3) C4 0.038(3) 0.026(3) 0.029(3) 0.0011(19) -0.004(2) -0.0008(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 N3 2.259(4) 5_645 ? Cd1 N3 2.259(4) 1_565 ? Cd1 OW1 2.328(4) 5_655 ? Cd1 OW1 2.328(4) . ? Cd1 S1 2.7164(14) . ? Cd1 S1 2.7164(14) 5_655 ? S1 C4 1.643(5) . ? S2 O2 1.467(3) . ? S2 O2 1.467(3) 2_645 ? S2 O1 1.472(3) . ? S2 O1 1.472(3) 2_645 ? N1 C3 1.325(6) . ? N1 C1 1.357(7) . ? N2 C3 1.318(6) . ? N2 C2 1.362(7) . ? N3 C4 1.132(6) . ? N3 Cd1 2.259(4) 1_545 ? C1 C2 1.356(8) . ? C3 C3 1.457(11) 2_645 ? 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 N3 180.0(3) 5_645 1_565 ? N3 Cd1 OW1 89.26(16) 5_645 5_655 ? N3 Cd1 OW1 90.74(16) 1_565 5_655 ? N3 Cd1 OW1 90.74(16) 5_645 . ? N3 Cd1 OW1 89.26(16) 1_565 . ? OW1 Cd1 OW1 180.0(2) 5_655 . ? N3 Cd1 S1 93.82(12) 5_645 . ? N3 Cd1 S1 86.18(12) 1_565 . ? OW1 Cd1 S1 93.43(11) 5_655 . ? OW1 Cd1 S1 86.57(11) . . ? N3 Cd1 S1 86.18(12) 5_645 5_655 ? N3 Cd1 S1 93.82(12) 1_565 5_655 ? OW1 Cd1 S1 86.57(11) 5_655 5_655 ? OW1 Cd1 S1 93.43(11) . 5_655 ? S1 Cd1 S1 180.00(8) . 5_655 ? C4 S1 Cd1 101.6(2) . . ? O2 S2 O2 108.7(3) . 2_645 ? O2 S2 O1 109.51(18) . . ? O2 S2 O1 110.26(18) 2_645 . ? O2 S2 O1 110.26(18) . 2_645 ? O2 S2 O1 109.51(18) 2_645 2_645 ? O1 S2 O1 108.6(2) . 2_645 ? C3 N1 C1 108.7(4) . . ? C3 N2 C2 108.6(4) . . ? C4 N3 Cd1 162.1(4) . 1_545 ? C2 C1 N1 106.9(4) . . ? C1 C2 N2 107.0(4) . . ? N2 C3 N1 108.8(5) . . ? N2 C3 C3 126.3(3) . 2_645 ? N1 C3 C3 124.9(3) . 2_645 ? N3 C4 S1 177.9(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.401 _refine_diff_density_min -1.347 _refine_diff_density_rms 0.202 data_2 _database_code_depnum_ccdc_archive 'CCDC 913196' #TrackingRef '2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H40 Br0 Cd2 Cl0 N12 O14 S6' _chemical_formula_weight 1089.88 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' 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' _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 6.7918(3) _cell_length_b 11.1504(7) _cell_length_c 12.7737(9) _cell_angle_alpha 88.191(4) _cell_angle_beta 89.623(4) _cell_angle_gamma 84.908(4) _cell_volume 963.06(10) _cell_formula_units_Z 1 _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 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.879 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 1.505 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.835 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 4673 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 23.28 _reflns_number_total 2763 _reflns_number_gt 2695 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMAR' _computing_cell_refinement 'Bruker SMAR' _computing_data_reduction 'Bruker SMAR' _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^)+(0.0470P)^2^+0.8236P] 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 2763 _refine_ls_number_parameters 256 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0743 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 -0.10949(3) 0.421083(18) 0.217706(16) 0.02610(12) Uani 1 1 d . . . S1 S -0.06599(15) 0.64927(8) 0.16166(6) 0.0372(2) Uani 1 1 d . . . S2 S -0.17647(13) -0.01685(8) 0.24977(7) 0.0371(2) Uani 1 1 d . . . S3 S 0.27016(11) 0.33105(6) 0.38964(6) 0.02205(18) Uani 1 1 d . . . N1 N 0.6903(4) 0.1178(2) 0.8776(2) 0.0284(6) Uani 1 1 d . . . N2 N 0.6904(4) -0.0592(2) 0.7836(2) 0.0243(6) Uani 1 1 d . . . N3 N 0.6385(4) 0.1295(2) 0.6990(2) 0.0277(6) Uani 1 1 d . . . N4 N 0.7659(5) 0.2569(3) 0.5180(2) 0.0272(6) Uani 1 1 d . . . H04 H 0.648(6) 0.287(3) 0.485(3) 0.035(9) Uiso 1 1 d . . . H02 H 0.853(6) 0.276(3) 0.493(3) 0.024(10) Uiso 1 1 d . . . N5 N -0.1685(5) 0.2317(3) 0.2674(2) 0.0423(7) Uani 1 1 d . . . N6 N 0.0244(5) 0.6382(3) -0.0521(2) 0.0412(7) Uani 1 1 d . . . O1 O 0.2137(3) 0.3819(2) 0.28400(17) 0.0328(5) Uani 1 1 d . . . O2 O 0.4424(3) 0.3887(2) 0.42608(18) 0.0346(5) Uani 1 1 d . . . O3 O 0.3214(5) 0.2016(2) 0.3852(2) 0.0520(7) Uani 1 1 d . . . O4 O 0.1070(3) 0.3572(2) 0.46347(19) 0.0414(6) Uani 1 1 d . . . OW1 O 0.4951(4) 0.6613(3) 0.0243(2) 0.0576(8) Uani 1 1 d . . . OW2 O -0.4478(3) 0.4482(2) 0.16233(19) 0.0396(6) Uani 1 1 d . . . OW3 O -0.2451(3) 0.5137(2) 0.36494(18) 0.0348(5) Uani 1 1 d . . . C1 C 0.6221(5) 0.2612(3) 0.6970(3) 0.0334(7) Uani 1 1 d . . . H1B H 0.6405 0.2893 0.7671 0.040 Uiso 1 1 calc R . . H1C H 0.4915 0.2920 0.6733 0.040 Uiso 1 1 calc R . . C2 C 0.7766(5) 0.3070(3) 0.6243(3) 0.0337(7) Uani 1 1 d . . . H2B H 0.7577 0.3943 0.6188 0.040 Uiso 1 1 calc R . . H2C H 0.9068 0.2849 0.6534 0.040 Uiso 1 1 calc R . . C3 C 0.7773(6) 0.1237(3) 0.5241(3) 0.0396(8) Uani 1 1 d . . . H3C H 0.9052 0.0922 0.5513 0.048 Uiso 1 1 calc R . . H3D H 0.7633 0.0929 0.4547 0.048 Uiso 1 1 calc R . . C4 C 0.6156(6) 0.0825(3) 0.5948(3) 0.0392(9) Uani 1 1 d . . . H4C H 0.4873 0.1116 0.5666 0.047 Uiso 1 1 calc R . . H4D H 0.6238 -0.0048 0.5990 0.047 Uiso 1 1 calc R . . C5 C 0.6729(4) 0.0627(3) 0.7862(2) 0.0228(6) Uani 1 1 d . . . C6 C 0.7318(5) -0.1279(3) 0.8706(3) 0.0312(7) Uani 1 1 d . . . H7A H 0.7439 -0.2114 0.8670 0.037 Uiso 1 1 calc R . . C7 C 0.7557(5) -0.0757(3) 0.9630(3) 0.0379(8) Uani 1 1 d . . . H8A H 0.7861 -0.1209 1.0241 0.045 Uiso 1 1 calc R . . C8 C 0.7323(5) 0.0494(3) 0.9619(3) 0.0351(8) Uani 1 1 d . . . H9A H 0.7473 0.0874 1.0248 0.042 Uiso 1 1 calc R . . C9 C -0.0110(5) 0.6402(3) 0.0362(3) 0.0274(7) Uani 1 1 d . . . C10 C -0.1722(5) 0.1288(3) 0.2584(2) 0.0287(7) Uani 1 1 d . . . H011 H 0.676(5) -0.091(3) 0.734(3) 0.020(9) 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 0.02786(16) 0.02716(17) 0.02276(16) 0.00137(10) 0.00100(10) -0.00042(10) S1 0.0598(6) 0.0312(5) 0.0220(4) -0.0004(3) -0.0002(4) -0.0116(4) S2 0.0373(5) 0.0325(5) 0.0424(5) -0.0038(4) -0.0008(4) -0.0067(4) S3 0.0242(4) 0.0218(4) 0.0204(4) -0.0002(3) -0.0016(3) -0.0031(3) N1 0.0337(14) 0.0285(14) 0.0225(14) -0.0016(11) 0.0007(11) -0.0005(11) N2 0.0279(14) 0.0233(14) 0.0220(14) -0.0009(12) -0.0019(11) -0.0032(11) N3 0.0410(15) 0.0220(13) 0.0209(13) 0.0016(10) -0.0034(11) -0.0066(11) N4 0.0254(15) 0.0341(16) 0.0224(14) 0.0047(11) 0.0017(12) -0.0060(13) N5 0.0524(19) 0.0361(19) 0.0389(18) 0.0031(14) 0.0051(14) -0.0087(14) N6 0.058(2) 0.0334(16) 0.0298(19) 0.0046(12) 0.0079(14) 0.0046(14) O1 0.0281(11) 0.0417(13) 0.0275(12) 0.0082(10) -0.0036(9) 0.0002(10) O2 0.0249(11) 0.0423(13) 0.0379(13) 0.0015(10) -0.0044(10) -0.0113(10) O3 0.092(2) 0.0253(13) 0.0374(15) -0.0039(11) -0.0206(14) 0.0057(13) O4 0.0291(12) 0.0653(17) 0.0321(13) -0.0084(11) 0.0072(10) -0.0150(11) OW1 0.0556(17) 0.0565(18) 0.0597(18) -0.0154(14) -0.0156(14) 0.0063(14) OW2 0.0322(12) 0.0474(15) 0.0394(14) 0.0017(11) -0.0028(10) -0.0057(11) OW3 0.0364(13) 0.0400(13) 0.0293(12) -0.0092(10) 0.0069(10) -0.0074(10) C1 0.045(2) 0.0250(17) 0.0286(17) 0.0043(13) 0.0056(14) 0.0036(14) C2 0.048(2) 0.0249(16) 0.0297(17) -0.0006(13) -0.0015(15) -0.0128(15) C3 0.063(2) 0.0324(18) 0.0220(17) -0.0034(14) -0.0021(16) 0.0069(16) C4 0.069(3) 0.0275(17) 0.0228(17) 0.0036(13) -0.0119(16) -0.0162(17) C5 0.0199(14) 0.0246(16) 0.0236(16) 0.0018(12) 0.0015(11) -0.0008(11) C6 0.0344(17) 0.0256(16) 0.0322(18) 0.0054(13) 0.0004(14) 0.0027(13) C7 0.049(2) 0.0362(19) 0.0256(18) 0.0075(14) -0.0024(15) 0.0085(16) C8 0.0417(19) 0.0392(19) 0.0237(17) -0.0020(14) -0.0008(14) 0.0013(15) C9 0.0307(16) 0.0224(16) 0.029(2) 0.0045(12) -0.0001(13) -0.0026(12) C10 0.0289(16) 0.037(2) 0.0204(16) 0.0034(13) 0.0022(12) -0.0070(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N5 2.255(3) . ? Cd1 N6 2.291(3) 2_565 ? Cd1 OW3 2.320(2) . ? Cd1 O1 2.357(2) . ? Cd1 OW2 2.399(2) . ? Cd1 S1 2.6626(9) . ? S1 C9 1.647(3) . ? S2 C10 1.634(4) . ? S3 O3 1.457(3) . ? S3 O4 1.466(2) . ? S3 O2 1.469(2) . ? S3 O1 1.486(2) . ? N1 C8 1.318(4) . ? N1 C5 1.348(4) . ? N2 C6 1.347(4) . ? N2 C5 1.355(4) . ? N2 H011 0.75(4) . ? N3 C5 1.331(4) . ? N3 C4 1.460(4) . ? N3 C1 1.461(4) . ? N4 C3 1.480(4) . ? N4 C2 1.490(4) . ? N4 H04 0.94(4) . ? N4 H02 0.72(4) . ? N5 C10 1.160(4) . ? N6 C9 1.153(4) . ? N6 Cd1 2.291(3) 2_565 ? C1 C2 1.509(5) . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 C4 1.511(6) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C6 C7 1.350(5) . ? C6 H7A 0.9300 . ? C7 C8 1.389(5) . ? C7 H8A 0.9300 . ? C8 H9A 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 N5 Cd1 N6 91.40(11) . 2_565 ? N5 Cd1 OW3 96.53(10) . . ? N6 Cd1 OW3 166.77(10) 2_565 . ? N5 Cd1 O1 88.64(10) . . ? N6 Cd1 O1 94.25(10) 2_565 . ? OW3 Cd1 O1 96.51(8) . . ? N5 Cd1 OW2 86.82(10) . . ? N6 Cd1 OW2 88.52(10) 2_565 . ? OW3 Cd1 OW2 81.38(8) . . ? O1 Cd1 OW2 174.74(7) . . ? N5 Cd1 S1 176.05(9) . . ? N6 Cd1 S1 90.43(8) 2_565 . ? OW3 Cd1 S1 81.04(6) . . ? O1 Cd1 S1 94.71(6) . . ? OW2 Cd1 S1 89.73(6) . . ? C9 S1 Cd1 102.53(11) . . ? O3 S3 O4 110.55(17) . . ? O3 S3 O2 109.08(16) . . ? O4 S3 O2 108.28(14) . . ? O3 S3 O1 110.29(14) . . ? O4 S3 O1 109.75(14) . . ? O2 S3 O1 108.85(14) . . ? C8 N1 C5 117.7(3) . . ? C6 N2 C5 121.4(3) . . ? C6 N2 H011 117(3) . . ? C5 N2 H011 121(3) . . ? C5 N3 C4 125.1(3) . . ? C5 N3 C1 123.0(3) . . ? C4 N3 C1 111.9(2) . . ? C3 N4 C2 110.8(3) . . ? C3 N4 H04 110(2) . . ? C2 N4 H04 110(2) . . ? C3 N4 H02 109(3) . . ? C2 N4 H02 103(3) . . ? H04 N4 H02 114(4) . . ? C10 N5 Cd1 156.1(3) . . ? C9 N6 Cd1 164.3(3) . 2_565 ? S3 O1 Cd1 126.71(13) . . ? N3 C1 C2 109.8(3) . . ? N3 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? N3 C1 H1C 109.7 . . ? C2 C1 H1C 109.7 . . ? H1B C1 H1C 108.2 . . ? N4 C2 C1 111.6(3) . . ? N4 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? N4 C2 H2C 109.3 . . ? C1 C2 H2C 109.3 . . ? H2B C2 H2C 108.0 . . ? N4 C3 C4 110.0(3) . . ? N4 C3 H3C 109.7 . . ? C4 C3 H3C 109.7 . . ? N4 C3 H3D 109.7 . . ? C4 C3 H3D 109.7 . . ? H3C C3 H3D 108.2 . . ? N3 C4 C3 109.0(3) . . ? N3 C4 H4C 109.9 . . ? C3 C4 H4C 109.9 . . ? N3 C4 H4D 109.9 . . ? C3 C4 H4D 109.9 . . ? H4C C4 H4D 108.3 . . ? N3 C5 N1 119.1(3) . . ? N3 C5 N2 120.8(3) . . ? N1 C5 N2 120.1(3) . . ? N2 C6 C7 120.0(3) . . ? N2 C6 H7A 120.0 . . ? C7 C6 H7A 120.0 . . ? C6 C7 C8 116.4(3) . . ? C6 C7 H8A 121.8 . . ? C8 C7 H8A 121.8 . . ? N1 C8 C7 124.3(3) . . ? N1 C8 H9A 117.9 . . ? C7 C8 H9A 117.9 . . ? N6 C9 S1 177.5(3) . . ? N5 C10 S2 178.2(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.739 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.147 data_3 _database_code_depnum_ccdc_archive 'CCDC 913197' #TrackingRef '3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H20 Cd3 N14 S12' _chemical_formula_weight 1298.52 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' _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 5.7788(3) _cell_length_b 10.8811(8) _cell_length_c 17.8852(8) _cell_angle_alpha 88.857(4) _cell_angle_beta 86.001(3) _cell_angle_gamma 89.661(4) _cell_volume 1121.64(11) _cell_formula_units_Z 1 _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 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.922 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 634 _exptl_absorpt_coefficient_mu 2.011 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.767 _exptl_absorpt_correction_T_max 0.802 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 5398 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 23.24 _reflns_number_total 3215 _reflns_number_gt 2942 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMAR' _computing_cell_refinement 'Bruker SMAR' _computing_data_reduction 'Bruker SMAR' _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^)+(0.0353P)^2^+0.3861P] 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 3215 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0617 _refine_ls_wR_factor_gt 0.0601 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 0.5000 0.0000 0.5000 0.02899(11) Uani 1 2 d S . . Cd2 Cd 0.62032(4) -0.35086(2) 0.926618(14) 0.03733(10) Uani 1 1 d . . . N1 N 1.0435(6) -0.1952(3) 0.76797(18) 0.0576(9) Uani 1 1 d . . . N2 N 1.2938(5) -0.2439(3) 0.96362(17) 0.0440(7) Uani 1 1 d . . . N3 N -0.0538(5) -0.4670(3) 0.91253(16) 0.0392(7) Uani 1 1 d . . . N4 N 0.7528(7) -0.3603(3) 0.48983(19) 0.0591(9) Uani 1 1 d . . . N5 N 1.1912(5) 0.0648(3) 0.42899(14) 0.0348(6) Uani 1 1 d . . . N6 N -0.6053(5) -1.0325(3) 0.78671(16) 0.0415(7) Uani 1 1 d . . . H6A H -0.7103 -1.0872 0.7828 0.050 Uiso 1 1 calc R . . N7 N -0.0852(5) -0.4757(3) 0.61734(16) 0.0458(8) Uani 1 1 d . . . H7A H -0.0881 -0.4218 0.5815 0.055 Uiso 1 1 calc R . . S1 S 0.61732(16) -0.32174(9) 0.78012(5) 0.0444(2) Uani 1 1 d . . . S2 S 0.84331(14) -0.14727(8) 0.96460(5) 0.0416(2) Uani 1 1 d . . . S3 S 0.39409(13) -0.57006(7) 0.91443(5) 0.03385(19) Uani 1 1 d . . . S4 S 0.69098(15) -0.15739(8) 0.39349(4) 0.0388(2) Uani 1 1 d . . . S5 S 0.75514(14) 0.18167(8) 0.43326(5) 0.0439(2) Uani 1 1 d . . . S6 S -0.06481(18) -0.74474(9) 0.80950(5) 0.0479(2) Uani 1 1 d . . . C1 C 0.0862(6) -0.4716(3) 0.66467(19) 0.0439(9) Uani 1 1 d . . . H1A H 0.2001 -0.4115 0.6584 0.053 Uiso 1 1 calc R . . C2 C 0.0910(6) -0.5558(3) 0.72144(18) 0.0399(8) Uani 1 1 d . . . H2A H 0.2090 -0.5536 0.7542 0.048 Uiso 1 1 calc R . . C3 C -0.0790(6) -0.6453(3) 0.73106(17) 0.0354(8) Uani 1 1 d . . . C4 C -0.2534(7) -0.6463(3) 0.6814(2) 0.0464(9) Uani 1 1 d . . . H4A H -0.3709 -0.7045 0.6869 0.056 Uiso 1 1 calc R . . C5 C -0.2502(7) -0.5610(3) 0.6246(2) 0.0490(9) Uani 1 1 d . . . H5A H -0.3644 -0.5622 0.5905 0.059 Uiso 1 1 calc R . . C6 C -0.4453(6) -1.0158(3) 0.73029(18) 0.0381(8) Uani 1 1 d . . . H6B H -0.4480 -1.0636 0.6879 0.046 Uiso 1 1 calc R . . C7 C -0.2771(6) -0.9289(3) 0.73420(18) 0.0365(8) Uani 1 1 d . . . H7B H -0.1640 -0.9179 0.6951 0.044 Uiso 1 1 calc R . . C8 C -0.2783(6) -0.8576(3) 0.79756(17) 0.0346(7) Uani 1 1 d . . . C9 C -0.4452(7) -0.8787(3) 0.85654(19) 0.0433(9) Uani 1 1 d . . . H9A H -0.4456 -0.8333 0.9001 0.052 Uiso 1 1 calc R . . C10 C -0.6086(7) -0.9674(3) 0.8491(2) 0.0478(9) Uani 1 1 d . . . H10A H -0.7219 -0.9823 0.8877 0.057 Uiso 1 1 calc R . . C11 C 0.8698(7) -0.2484(3) 0.77331(19) 0.0448(9) Uani 1 1 d . . . C12 C 1.1067(5) -0.2055(3) 0.96442(17) 0.0317(7) Uani 1 1 d . . . C13 C 0.1302(6) -0.5094(3) 0.91421(17) 0.0316(7) Uani 1 1 d . . . C14 C 0.7283(6) -0.2766(3) 0.45050(19) 0.0381(8) Uani 1 1 d . . . C15 C 1.0115(6) 0.1121(3) 0.43073(16) 0.0309(7) 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 0.02345(18) 0.0324(2) 0.03093(18) 0.00059(13) -0.00088(12) -0.00067(13) Cd2 0.02300(15) 0.03633(16) 0.05256(18) -0.00135(11) -0.00200(11) 0.00094(11) N1 0.049(2) 0.065(2) 0.058(2) 0.0012(17) 0.0033(15) -0.0131(18) N2 0.0281(17) 0.0420(18) 0.0626(19) -0.0088(14) -0.0065(13) 0.0006(14) N3 0.0301(16) 0.0417(17) 0.0465(17) -0.0043(13) -0.0076(12) 0.0047(14) N4 0.081(3) 0.045(2) 0.052(2) 0.0044(17) -0.0134(17) 0.0102(18) N5 0.0248(15) 0.0468(17) 0.0329(15) -0.0015(12) -0.0017(11) 0.0005(13) N6 0.0442(17) 0.0310(16) 0.0493(18) 0.0036(13) -0.0029(14) -0.0056(13) N7 0.061(2) 0.0363(17) 0.0392(17) 0.0075(13) 0.0016(15) 0.0101(15) S1 0.0405(5) 0.0450(5) 0.0484(5) 0.0003(4) -0.0075(4) -0.0046(4) S2 0.0252(4) 0.0370(5) 0.0629(6) -0.0115(4) -0.0029(4) 0.0030(4) S3 0.0247(4) 0.0327(5) 0.0444(5) -0.0032(3) -0.0034(3) 0.0019(3) S4 0.0463(5) 0.0384(5) 0.0320(4) -0.0019(4) -0.0041(4) 0.0055(4) S5 0.0276(4) 0.0377(5) 0.0649(6) 0.0147(4) 0.0032(4) 0.0013(4) S6 0.0617(6) 0.0409(5) 0.0432(5) 0.0069(4) -0.0210(4) -0.0162(5) C1 0.050(2) 0.035(2) 0.046(2) -0.0011(16) 0.0043(17) -0.0041(17) C2 0.042(2) 0.040(2) 0.0377(19) -0.0027(15) -0.0042(15) -0.0047(16) C3 0.0416(19) 0.0296(18) 0.0353(18) -0.0044(14) -0.0053(14) -0.0007(15) C4 0.050(2) 0.039(2) 0.052(2) 0.0043(17) -0.0152(17) -0.0063(17) C5 0.058(2) 0.042(2) 0.048(2) 0.0003(17) -0.0172(18) 0.0038(19) C6 0.050(2) 0.0317(19) 0.0332(18) -0.0012(14) -0.0046(15) 0.0002(16) C7 0.0416(19) 0.0364(19) 0.0310(17) 0.0027(14) 0.0000(14) -0.0018(15) C8 0.044(2) 0.0260(18) 0.0346(18) 0.0034(14) -0.0097(15) -0.0012(15) C9 0.062(2) 0.0324(19) 0.0351(19) -0.0044(14) 0.0037(16) 0.0001(17) C10 0.054(2) 0.038(2) 0.048(2) 0.0005(17) 0.0149(17) -0.0015(18) C11 0.050(2) 0.046(2) 0.038(2) 0.0004(16) -0.0019(16) 0.0030(19) C12 0.0292(19) 0.0306(18) 0.0352(18) -0.0048(13) -0.0006(13) -0.0053(15) C13 0.0336(19) 0.0295(18) 0.0324(17) -0.0034(13) -0.0051(13) -0.0046(15) C14 0.040(2) 0.037(2) 0.0384(19) -0.0131(17) -0.0071(15) 0.0047(16) C15 0.0301(19) 0.0351(18) 0.0274(16) 0.0012(13) -0.0009(13) -0.0100(15) _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 N5 2.358(3) 1_455 ? Cd1 N5 2.358(3) 2_756 ? Cd1 S5 2.6835(8) . ? Cd1 S5 2.6835(8) 2_656 ? Cd1 S4 2.7558(8) 2_656 ? Cd1 S4 2.7558(8) . ? Cd2 N3 2.264(3) 1_655 ? Cd2 N2 2.277(3) 1_455 ? Cd2 S1 2.6341(9) . ? Cd2 S2 2.6917(9) . ? Cd2 S3 2.7465(8) . ? Cd2 S3 2.9495(9) 2_647 ? N1 C11 1.158(5) . ? N2 C12 1.156(4) . ? N2 Cd2 2.277(3) 1_655 ? N3 C13 1.159(4) . ? N3 Cd2 2.264(3) 1_455 ? N4 C14 1.154(5) . ? N5 C15 1.155(4) . ? N5 Cd1 2.358(3) 1_655 ? N6 C6 1.331(4) . ? N6 C10 1.333(5) . ? N7 C5 1.332(5) . ? N7 C1 1.348(5) . ? S1 C11 1.663(4) . ? S2 C12 1.645(3) . ? S3 C13 1.658(3) . ? S3 Cd2 2.9495(9) 2_647 ? S4 C14 1.656(4) . ? S5 C15 1.658(3) . ? S6 C3 1.760(3) . ? S6 C8 1.772(3) . ? C1 C2 1.356(5) . ? C2 C3 1.387(5) . ? C3 C4 1.389(5) . ? C4 C5 1.362(5) . ? C6 C7 1.365(5) . ? C7 C8 1.386(5) . ? C8 C9 1.395(5) . ? C9 C10 1.369(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 N5 Cd1 N5 180.00(10) 1_455 2_756 ? N5 Cd1 S5 88.05(7) 1_455 . ? N5 Cd1 S5 91.95(7) 2_756 . ? N5 Cd1 S5 91.95(7) 1_455 2_656 ? N5 Cd1 S5 88.05(7) 2_756 2_656 ? S5 Cd1 S5 180.00(3) . 2_656 ? N5 Cd1 S4 84.88(7) 1_455 2_656 ? N5 Cd1 S4 95.12(7) 2_756 2_656 ? S5 Cd1 S4 91.49(3) . 2_656 ? S5 Cd1 S4 88.51(3) 2_656 2_656 ? N5 Cd1 S4 95.12(7) 1_455 . ? N5 Cd1 S4 84.88(7) 2_756 . ? S5 Cd1 S4 88.51(3) . . ? S5 Cd1 S4 91.49(3) 2_656 . ? S4 Cd1 S4 180.00(2) 2_656 . ? N3 Cd2 N2 169.40(10) 1_655 1_455 ? N3 Cd2 S1 90.47(7) 1_655 . ? N2 Cd2 S1 100.07(8) 1_455 . ? N3 Cd2 S2 94.61(7) 1_655 . ? N2 Cd2 S2 84.43(7) 1_455 . ? S1 Cd2 S2 101.77(3) . . ? N3 Cd2 S3 84.45(7) 1_655 . ? N2 Cd2 S3 94.61(7) 1_455 . ? S1 Cd2 S3 88.43(3) . . ? S2 Cd2 S3 169.78(3) . . ? N3 Cd2 S3 85.60(7) 1_655 2_647 ? N2 Cd2 S3 83.82(8) 1_455 2_647 ? S1 Cd2 S3 169.74(3) . 2_647 ? S2 Cd2 S3 88.01(3) . 2_647 ? S3 Cd2 S3 81.77(3) . 2_647 ? C12 N2 Cd2 160.3(3) . 1_655 ? C13 N3 Cd2 166.6(2) . 1_455 ? C15 N5 Cd1 145.4(2) . 1_655 ? C6 N6 C10 122.3(3) . . ? C5 N7 C1 121.7(3) . . ? C11 S1 Cd2 93.14(12) . . ? C12 S2 Cd2 98.24(11) . . ? C13 S3 Cd2 95.77(11) . . ? C13 S3 Cd2 98.34(11) . 2_647 ? Cd2 S3 Cd2 98.23(3) . 2_647 ? C14 S4 Cd1 97.17(11) . . ? C15 S5 Cd1 98.29(11) . . ? C3 S6 C8 104.54(15) . . ? N7 C1 C2 119.4(3) . . ? C1 C2 C3 120.5(3) . . ? C2 C3 C4 118.5(3) . . ? C2 C3 S6 116.6(3) . . ? C4 C3 S6 124.8(3) . . ? C5 C4 C3 119.2(3) . . ? N7 C5 C4 120.7(3) . . ? N6 C6 C7 120.5(3) . . ? C6 C7 C8 118.7(3) . . ? C7 C8 C9 119.6(3) . . ? C7 C8 S6 122.5(3) . . ? C9 C8 S6 117.8(2) . . ? C10 C9 C8 118.7(3) . . ? N6 C10 C9 120.1(3) . . ? N1 C11 S1 178.6(4) . . ? N2 C12 S2 178.5(3) . . ? N3 C13 S3 178.7(3) . . ? N4 C14 S4 179.3(3) . . ? N5 C15 S5 179.3(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.24 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.412 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.071 data_4 _database_code_depnum_ccdc_archive 'CCDC 913198' #TrackingRef '4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H15 Cd N6 S4' _chemical_formula_weight 544.04 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 orthorhombic _symmetry_space_group_name_H-M P21212 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 20.400(2) _cell_length_b 12.0901(13) _cell_length_c 4.2614(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1051.0(2) _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 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.719 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 542 _exptl_absorpt_coefficient_mu 1.452 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.865 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 5076 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 23.31 _reflns_number_total 1527 _reflns_number_gt 1470 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMAR' _computing_cell_refinement 'Bruker SMAR' _computing_data_reduction 'Bruker SMAR' _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^)+(0.0300P)^2^+0.5014P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.10(4) _refine_ls_number_reflns 1527 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0661 _refine_ls_wR_factor_gt 0.0657 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _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 0.0000 0.0000 0.63890(12) 0.05019(18) Uani 1 2 d S . . S1 S -0.03450(5) 0.16003(9) 0.2592(3) 0.0420(3) Uani 1 1 d . . . S2 S 0.21280(6) 0.13094(10) 1.0599(3) 0.0498(3) Uani 1 1 d . . . N1 N -0.1719(2) 0.1561(4) 0.3326(14) 0.0670(13) Uani 1 1 d . . . N2 N 0.09189(19) 0.0680(3) 0.8161(10) 0.0479(10) Uani 1 1 d . . . N3 N 0.27470(19) -0.0942(4) 0.7401(10) 0.0387(9) Uani 1 1 d . . . C1 C 0.3468(2) 0.0396(3) 0.4730(11) 0.0342(11) Uani 1 1 d . . . H1A H 0.3210 0.0975 0.5464 0.041 Uiso 1 1 calc R . . C2 C 0.4006(2) 0.0600(3) 0.2861(11) 0.0368(11) Uani 1 1 d . . . H2A H 0.4109 0.1326 0.2342 0.044 Uiso 1 1 calc R . . C3 C 0.43990(19) -0.0247(3) 0.1735(9) 0.0287(9) Uani 1 1 d . . . C4 C 0.4247(2) -0.1316(3) 0.2559(10) 0.0356(10) Uani 1 1 d . . . H4A H 0.4511 -0.1891 0.1846 0.043 Uiso 1 1 calc R . . C5 C 0.3707(2) -0.1553(4) 0.4441(10) 0.0352(10) Uani 1 1 d . . . H5A H 0.3608 -0.2280 0.4984 0.042 Uiso 1 1 calc R . . C6 C 0.3321(2) -0.0689(3) 0.5487(10) 0.0295(10) Uani 1 1 d . . . C7 C 0.5000 0.0000 -0.0256(14) 0.0394(14) Uani 1 2 d S . . C8 C -0.1149(3) 0.1566(4) 0.3096(12) 0.0462(12) Uani 1 1 d . . . C9 C 0.1419(2) 0.0936(3) 0.9181(11) 0.0344(10) Uani 1 1 d . . . H07 H 0.493(3) 0.061(3) -0.146(10) 0.047(12) Uiso 1 1 d . . . H03 H 0.261(2) -0.035(4) 0.879(11) 0.038(12) Uiso 1 1 d . . . H02 H 0.281(2) -0.150(4) 0.842(12) 0.043(14) Uiso 1 1 d . . . H01 H 0.239(2) -0.122(4) 0.582(12) 0.049(13) 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 0.0278(2) 0.0449(3) 0.0779(4) 0.000 0.000 -0.0072(2) S1 0.0338(6) 0.0420(6) 0.0503(7) 0.0073(5) 0.0020(6) -0.0058(5) S2 0.0354(6) 0.0500(7) 0.0640(8) -0.0202(6) -0.0095(6) 0.0040(5) N1 0.045(3) 0.062(3) 0.094(4) 0.015(3) 0.012(3) 0.004(2) N2 0.040(2) 0.043(2) 0.061(3) 0.000(2) -0.004(2) -0.0020(18) N3 0.034(2) 0.043(2) 0.039(2) 0.000(2) 0.0020(19) 0.0039(18) C1 0.030(2) 0.034(2) 0.039(3) -0.0037(19) -0.003(2) 0.0098(17) C2 0.037(3) 0.033(2) 0.040(3) 0.005(2) -0.006(2) -0.0026(19) C3 0.029(2) 0.034(3) 0.023(2) -0.0034(18) -0.0087(17) -0.0015(16) C4 0.034(2) 0.039(2) 0.033(2) -0.007(2) 0.004(2) 0.0046(19) C5 0.038(3) 0.031(2) 0.036(2) 0.000(2) 0.002(2) -0.0005(18) C6 0.026(2) 0.038(2) 0.024(2) -0.005(2) -0.0022(19) 0.0009(17) C7 0.043(3) 0.046(4) 0.029(3) 0.000 0.000 -0.006(4) C8 0.049(3) 0.035(2) 0.054(3) 0.005(2) 0.002(3) 0.001(2) C9 0.034(3) 0.032(2) 0.037(3) -0.003(2) 0.000(2) 0.0038(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N2 2.182(4) . ? Cd1 N2 2.182(4) 2 ? Cd1 S1 2.6186(12) . ? Cd1 S1 2.6186(12) 2 ? S1 C8 1.654(5) . ? S2 C9 1.631(5) . ? N1 C8 1.168(6) . ? N2 C9 1.152(6) . ? N3 C6 1.459(6) . ? N3 H03 0.97(5) . ? N3 H02 0.81(5) . ? N3 H01 1.06(5) . ? C1 C2 1.379(6) . ? C1 C6 1.385(6) . ? C1 H1A 0.9300 . ? C2 C3 1.386(6) . ? C2 H2A 0.9300 . ? C3 C4 1.374(6) . ? C3 C7 1.521(5) . ? C4 C5 1.393(6) . ? C4 H4A 0.9300 . ? C5 C6 1.383(6) . ? C5 H5A 0.9300 . ? C7 C3 1.521(5) 2_655 ? C7 H07 0.91(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 N2 139.5(2) . 2 ? N2 Cd1 S1 99.57(11) . . ? N2 Cd1 S1 105.16(11) 2 . ? N2 Cd1 S1 105.16(11) . 2 ? N2 Cd1 S1 99.57(11) 2 2 ? S1 Cd1 S1 103.67(6) . 2 ? C8 S1 Cd1 99.63(17) . . ? C9 N2 Cd1 173.4(4) . . ? C6 N3 H03 115(3) . . ? C6 N3 H02 110(3) . . ? H03 N3 H02 109(4) . . ? C6 N3 H01 106(3) . . ? H03 N3 H01 115(4) . . ? H02 N3 H01 101(4) . . ? C2 C1 C6 118.5(4) . . ? C2 C1 H1A 120.8 . . ? C6 C1 H1A 120.8 . . ? C1 C2 C3 121.9(4) . . ? C1 C2 H2A 119.0 . . ? C3 C2 H2A 119.0 . . ? C4 C3 C2 118.4(4) . . ? C4 C3 C7 120.6(3) . . ? C2 C3 C7 120.9(3) . . ? C3 C4 C5 121.3(4) . . ? C3 C4 H4A 119.4 . . ? C5 C4 H4A 119.4 . . ? C6 C5 C4 118.7(4) . . ? C6 C5 H5A 120.6 . . ? C4 C5 H5A 120.6 . . ? C5 C6 C1 121.1(4) . . ? C5 C6 N3 118.7(4) . . ? C1 C6 N3 120.2(4) . . ? C3 C7 C3 112.2(4) 2_655 . ? C3 C7 H07 106(3) 2_655 . ? C3 C7 H07 111(3) . . ? N1 C8 S1 177.1(5) . . ? N2 C9 S2 179.4(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.381 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.059 data_5 _database_code_depnum_ccdc_archive 'CCDC 913199' #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Cd2 N6 O4 S5' _chemical_formula_weight 691.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M c2/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.6880(16) _cell_length_b 5.8675(3) _cell_length_c 19.9244(15) _cell_angle_alpha 90.00 _cell_angle_beta 115.730(9) _cell_angle_gamma 90.00 _cell_volume 2178.8(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 BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 2.463 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.752 _exptl_absorpt_correction_T_max 0.801 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 5839 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.11 _reflns_number_total 1931 _reflns_number_gt 1643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMAR' _computing_cell_refinement 'Bruker SMAR' _computing_data_reduction 'Bruker SMAR' _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^)+(0.0281P)^2^+1.6083P] 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 1931 _refine_ls_number_parameters 173 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.069 _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 -0.550477(13) 0.87581(4) -0.111638(12) 0.03488(11) Uani 1 1 d . . . S1 S -0.67189(5) 0.63617(14) -0.18914(5) 0.0445(2) Uani 1 1 d . A . S2 S -0.42724(4) 1.12182(12) -0.01709(5) 0.03525(19) Uani 1 1 d . . . S3 S -0.5000 0.98963(18) -0.2500 0.0440(3) Uani 1 2 d S . . N1 N -0.61614(15) 0.1976(5) -0.14705(18) 0.0476(8) Uani 1 1 d . . . N2 N -0.47767(15) 1.5605(4) -0.06951(16) 0.0393(7) Uani 1 1 d . . . N3 N -0.38941(15) 1.5168(5) -0.17489(16) 0.0465(7) Uani 1 1 d . . . H3A H -0.4108 1.4146 -0.2108 0.080 Uiso 1 1 calc . . . H3B H -0.3793 1.6409 -0.1942 0.080 Uiso 1 1 calc . . . H3C H -0.4185 1.5537 -0.1543 0.080 Uiso 1 1 calc . . . C1 C -0.63863(17) 0.3765(5) -0.16395(19) 0.0356(7) Uani 1 1 d . . . C2 C -0.45797(17) 1.3818(5) -0.04755(18) 0.0331(7) Uani 1 1 d . . . C3 C -0.25325(17) 1.7822(6) -0.06992(19) 0.0430(8) Uani 1 1 d . . . H3 H -0.2553 1.8057 -0.1170 0.080 Uiso 1 1 calc . . . C4 C -0.28411(15) 1.5881(5) -0.05583(18) 0.0344(7) Uani 1 1 d . . . C5 C -0.28045(17) 1.5600(6) 0.01407(19) 0.0422(8) Uani 1 1 d . . . H5 H -0.3012 1.4316 0.0241 0.080 Uiso 1 1 calc . . . C6 C -0.32214(18) 1.4190(5) -0.1173(2) 0.0431(8) Uani 1 1 d . . . H6A H -0.2909 1.3756 -0.1399 0.080 Uiso 1 1 calc . . . H6B H -0.3332 1.2829 -0.0966 0.080 Uiso 1 1 calc . . . O1 O -0.5143(5) 0.8367(12) -0.2017(4) 0.0399(17) Uani 0.50 1 d P A 1 O2 O -0.5000 1.225(3) -0.2500 0.041(7) Uani 0.50 2 d SP A 1 O3 O -0.4221(9) 0.961(3) -0.1758(8) 0.047(5) Uani 0.25 1 d P A 1 O4 O -0.5515(7) 0.917(2) -0.2271(7) 0.040(3) Uani 0.25 1 d P . 2 O5 O -0.5093(16) 1.229(2) -0.2277(15) 0.021(4) Uani 0.25 1 d PU . 2 O6 O -0.4830(8) 0.917(3) -0.1792(7) 0.039(3) Uani 0.25 1 d P A 2 O7 O -0.4113(8) 0.971(3) -0.2064(8) 0.043(3) Uani 0.25 1 d P . 2 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 0.05028(17) 0.02335(15) 0.03479(16) 0.00102(9) 0.02200(11) 0.00212(10) S1 0.0478(5) 0.0275(4) 0.0530(6) 0.0040(4) 0.0170(4) 0.0043(4) S2 0.0438(4) 0.0255(4) 0.0421(5) 0.0011(3) 0.0239(4) 0.0010(3) S3 0.0855(9) 0.0196(6) 0.0460(7) 0.000 0.0463(7) 0.000 N1 0.0503(18) 0.0256(15) 0.063(2) 0.0021(14) 0.0203(15) 0.0009(13) N2 0.0506(17) 0.0236(14) 0.0492(18) 0.0025(12) 0.0268(14) 0.0002(12) N3 0.0443(16) 0.0349(16) 0.0463(17) -0.0040(14) 0.0066(13) -0.0041(13) C1 0.0382(17) 0.0310(19) 0.0399(19) -0.0039(15) 0.0190(14) -0.0085(15) C2 0.0387(17) 0.0306(18) 0.0366(18) -0.0071(14) 0.0224(14) -0.0086(14) C3 0.0384(18) 0.050(2) 0.039(2) 0.0039(16) 0.0149(15) -0.0096(16) C4 0.0273(15) 0.0310(17) 0.0388(18) 0.0010(13) 0.0088(13) 0.0003(12) C5 0.0393(18) 0.0395(19) 0.042(2) 0.0071(15) 0.0121(15) -0.0121(14) C6 0.0393(18) 0.0353(18) 0.044(2) -0.0019(15) 0.0082(15) 0.0002(14) O1 0.064(6) 0.031(4) 0.037(4) -0.001(3) 0.033(4) -0.008(3) O2 0.045(7) 0.029(5) 0.07(2) 0.000 0.050(11) 0.000 O3 0.059(12) 0.037(6) 0.016(7) 0.004(6) -0.012(6) 0.004(6) O4 0.048(7) 0.037(7) 0.045(9) -0.010(5) 0.030(7) -0.005(5) O5 0.036(10) 0.015(5) 0.029(8) -0.002(4) 0.030(6) 0.003(4) O6 0.042(9) 0.053(9) 0.027(7) 0.008(5) 0.019(6) 0.011(6) O7 0.032(6) 0.038(6) 0.040(10) 0.003(7) -0.003(8) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.236(7) . ? Cd1 N1 2.253(3) 1_565 ? Cd1 N2 2.302(3) 1_545 ? Cd1 O4 2.303(12) . ? Cd1 O6 2.335(12) . ? Cd1 S1 2.7024(10) . ? Cd1 S2 2.7960(9) 5_475 ? Cd1 S2 2.8217(9) . ? S1 C1 1.657(3) . ? S2 C2 1.663(3) . ? S2 Cd1 2.7960(9) 5_475 ? S3 O6 1.366(11) 2_454 ? S3 O6 1.366(11) . ? S3 O2 1.384(15) . ? S3 O4 1.397(11) . ? S3 O4 1.397(11) 2_454 ? S3 O1 1.437(6) . ? S3 O1 1.437(6) 2_454 ? S3 O5 1.511(11) . ? S3 O5 1.511(11) 2_454 ? S3 O3 1.656(15) . ? S3 O3 1.656(15) 2_454 ? S3 O7 1.659(15) . ? N1 C1 1.138(4) . ? N1 Cd1 2.253(3) 1_545 ? N2 C2 1.141(4) . ? N2 Cd1 2.302(3) 1_565 ? N3 C6 1.482(4) . ? N3 H3A 0.8900 . ? N3 H3B 0.8900 . ? N3 H3C 0.8900 . ? C3 C5 1.381(5) 7_485 ? C3 C4 1.393(4) . ? C3 H3 0.9300 . ? C4 C5 1.372(5) . ? C4 C6 1.506(4) . ? C5 C3 1.381(5) 7_485 ? C5 H5 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? O4 O7 1.251(19) 2_454 ? O4 O6 1.321(17) . ? O5 O5 1.11(4) 2_454 ? O6 O7 1.815(17) . ? O7 O4 1.251(19) 2_454 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 N1 101.6(2) . 1_565 ? O1 Cd1 N2 79.4(2) . 1_545 ? N1 Cd1 N2 176.29(10) 1_565 1_545 ? O1 Cd1 O4 21.6(3) . . ? N1 Cd1 O4 81.8(4) 1_565 . ? N2 Cd1 O4 99.7(4) 1_545 . ? O1 Cd1 O6 19.2(3) . . ? N1 Cd1 O6 99.4(3) 1_565 . ? N2 Cd1 O6 80.3(3) 1_545 . ? O4 Cd1 O6 33.1(4) . . ? O1 Cd1 S1 92.3(2) . . ? N1 Cd1 S1 88.43(7) 1_565 . ? N2 Cd1 S1 95.11(7) 1_545 . ? O4 Cd1 S1 83.1(3) . . ? O6 Cd1 S1 111.4(4) . . ? O1 Cd1 S2 169.3(2) . 5_475 ? N1 Cd1 S2 88.05(8) 1_565 5_475 ? N2 Cd1 S2 90.68(7) 1_545 5_475 ? O4 Cd1 S2 169.0(4) . 5_475 ? O6 Cd1 S2 155.0(4) . 5_475 ? S1 Cd1 S2 92.54(3) . 5_475 ? O1 Cd1 S2 93.9(2) . . ? N1 Cd1 S2 91.58(8) 1_565 . ? N2 Cd1 S2 84.78(7) 1_545 . ? O4 Cd1 S2 103.2(3) . . ? O6 Cd1 S2 74.9(4) . . ? S1 Cd1 S2 173.68(3) . . ? S2 Cd1 S2 81.14(3) 5_475 . ? C1 S1 Cd1 98.31(11) . . ? C2 S2 Cd1 98.11(12) . 5_475 ? C2 S2 Cd1 97.71(11) . . ? Cd1 S2 Cd1 98.86(3) 5_475 . ? O6 S3 O6 143.5(13) 2_454 . ? O6 S3 O2 108.3(6) 2_454 . ? O6 S3 O2 108.3(6) . . ? O6 S3 O4 110.5(8) 2_454 . ? O6 S3 O4 57.1(7) . . ? O2 S3 O4 107.9(5) . . ? O6 S3 O4 57.1(7) 2_454 2_454 ? O6 S3 O4 110.5(8) . 2_454 ? O2 S3 O4 107.9(5) . 2_454 ? O4 S3 O4 144.2(10) . 2_454 ? O6 S3 O1 117.4(6) 2_454 . ? O6 S3 O1 31.6(5) . . ? O2 S3 O1 128.6(3) . . ? O4 S3 O1 35.1(5) . . ? O4 S3 O1 115.8(5) 2_454 . ? O6 S3 O1 31.6(5) 2_454 2_454 ? O6 S3 O1 117.4(6) . 2_454 ? O2 S3 O1 128.6(3) . 2_454 ? O4 S3 O1 115.8(5) . 2_454 ? O4 S3 O1 35.1(5) 2_454 2_454 ? O1 S3 O1 102.7(6) . 2_454 ? O6 S3 O5 125.9(12) 2_454 . ? O6 S3 O5 89.8(11) . . ? O2 S3 O5 21.6(7) . . ? O4 S3 O5 88.7(9) . . ? O4 S3 O5 126.5(10) 2_454 . ? O1 S3 O5 107.1(8) . . ? O1 S3 O5 150.1(8) 2_454 . ? O6 S3 O5 89.8(11) 2_454 2_454 ? O6 S3 O5 125.9(12) . 2_454 ? O2 S3 O5 21.6(7) . 2_454 ? O4 S3 O5 126.5(10) . 2_454 ? O4 S3 O5 88.7(9) 2_454 2_454 ? O1 S3 O5 150.1(8) . 2_454 ? O1 S3 O5 107.1(8) 2_454 2_454 ? O5 S3 O5 43.1(15) . 2_454 ? O6 S3 O3 127.2(7) 2_454 . ? O6 S3 O3 48.1(7) . . ? O2 S3 O3 95.8(5) . . ? O4 S3 O3 105.2(7) . . ? O4 S3 O3 71.1(7) 2_454 . ? O1 S3 O3 75.0(6) . . ? O1 S3 O3 97.5(6) 2_454 . ? O5 S3 O3 91.8(13) . . ? O5 S3 O3 99.1(13) 2_454 . ? O6 S3 O3 48.1(7) 2_454 2_454 ? O6 S3 O3 127.2(7) . 2_454 ? O2 S3 O3 95.8(5) . 2_454 ? O4 S3 O3 71.1(7) . 2_454 ? O4 S3 O3 105.2(7) 2_454 2_454 ? O1 S3 O3 97.5(6) . 2_454 ? O1 S3 O3 75.0(6) 2_454 2_454 ? O5 S3 O3 99.1(13) . 2_454 ? O5 S3 O3 91.8(13) 2_454 2_454 ? O3 S3 O3 168.3(11) . 2_454 ? O6 S3 O7 104.5(7) 2_454 . ? O6 S3 O7 73.0(6) . . ? O2 S3 O7 93.8(5) . . ? O4 S3 O7 129.5(7) . . ? O4 S3 O7 47.4(7) 2_454 . ? O1 S3 O7 96.4(5) . . ? O1 S3 O7 78.9(6) 2_454 . ? O5 S3 O7 99.3(13) . . ? O5 S3 O7 87.8(13) 2_454 . ? O3 S3 O7 25.7(5) . . ? O3 S3 O7 152.6(5) 2_454 . ? C1 N1 Cd1 168.2(3) . 1_545 ? C2 N2 Cd1 161.2(3) . 1_565 ? C6 N3 H3A 109.5 . . ? C6 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? C6 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? N1 C1 S1 179.6(4) . . ? N2 C2 S2 177.9(3) . . ? C5 C3 C4 120.1(3) 7_485 . ? C5 C3 H3 120.0 7_485 . ? C4 C3 H3 120.0 . . ? C5 C4 C3 118.4(3) . . ? C5 C4 C6 121.7(3) . . ? C3 C4 C6 119.9(3) . . ? C4 C5 C3 121.6(3) . 7_485 ? C4 C5 H5 119.2 . . ? C3 C5 H5 119.2 7_485 . ? N3 C6 C4 111.0(3) . . ? N3 C6 H6A 109.4 . . ? C4 C6 H6A 109.4 . . ? N3 C6 H6B 109.4 . . ? C4 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? S3 O1 Cd1 135.3(4) . . ? O7 O4 O6 137.6(12) 2_454 . ? O7 O4 S3 77.4(9) 2_454 . ? O6 O4 S3 60.3(7) . . ? O7 O4 Cd1 145.0(13) 2_454 . ? O6 O4 Cd1 74.8(8) . . ? S3 O4 Cd1 132.9(8) . . ? O5 O5 S3 68.4(7) 2_454 . ? O4 O6 S3 62.6(7) . . ? O4 O6 O7 123.0(10) . . ? S3 O6 O7 60.9(6) . . ? O4 O6 Cd1 72.1(8) . . ? S3 O6 Cd1 132.6(8) . . ? O7 O6 Cd1 164.0(10) . . ? O4 O7 S3 55.2(8) 2_454 . ? O4 O7 O6 93.7(10) 2_454 . ? S3 O7 O6 46.0(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.345 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.116