# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ; College of Chemistry and Chemical Engineering, Jiangxi Normal University, Nanchang, Jiangxi 330022, P. R. China ; _publ_contact_author_email qyliuchemistry@gmail.com _publ_contact_author_fax +86-791-8120380 _publ_contact_author_phone +86-791-8120380 #TrackingRef '- CdMPTRZ.cif' _publ_contact_author_name 'Qing-Yan Liu' _publ_requested_coeditor_name ? _publ_author_name 'Qing-Yan Liu' # Attachment '- CdMPTRZ.cif' data_Cd(MPTRZ)2 _database_code_depnum_ccdc_archive 'CCDC 780919' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H8 Cd N6 S2' _chemical_formula_weight 340.70 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 Pbcn _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.3271(8) _cell_length_b 10.2322(6) _cell_length_c 8.0646(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1099.73(11) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7058 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 28.22 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 2.341 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.782 _exptl_absorpt_correction_T_max 0.821 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEXII area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9434 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0129 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 28.22 _reflns_number_total 1361 _reflns_number_gt 1299 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^+0.6402P] 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 SHELXL _refine_ls_extinction_coef 0.0263(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1361 _refine_ls_number_parameters 70 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0165 _refine_ls_R_factor_gt 0.0156 _refine_ls_wR_factor_ref 0.0426 _refine_ls_wR_factor_gt 0.0420 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.414738(14) 0.2500 0.02854(8) Uani 1 2 d S . . S1 S 0.64747(3) 0.47795(4) -0.11438(5) 0.03305(11) Uani 1 1 d . . . C1 C 0.60808(10) 0.31982(13) -0.07808(17) 0.0251(3) Uani 1 1 d . . . C2 C 0.58799(14) 0.11011(16) -0.0968(2) 0.0392(4) Uani 1 1 d . . . H2A H 0.5904 0.0249 -0.1368 0.047 Uiso 1 1 calc R . . C3 C 0.68258(15) 0.21445(19) -0.3334(2) 0.0447(4) Uani 1 1 d . . . H3A H 0.6852 0.1271 -0.3765 0.067 Uiso 1 1 calc R . . H3B H 0.7496 0.2459 -0.3156 0.067 Uiso 1 1 calc R . . H3C H 0.6489 0.2702 -0.4113 0.067 Uiso 1 1 calc R . . N1 N 0.54590(12) 0.14383(13) 0.04226(19) 0.0402(3) Uani 1 1 d . . . N2 N 0.55877(10) 0.27828(12) 0.05436(16) 0.0309(3) Uani 1 1 d . . . N3 N 0.62788(10) 0.21469(12) -0.17622(16) 0.0305(3) 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 0.03639(12) 0.02351(11) 0.02570(11) 0.000 0.00135(5) 0.000 S1 0.0345(2) 0.02735(19) 0.0373(2) 0.00533(14) -0.00525(15) -0.00503(14) C1 0.0240(6) 0.0257(6) 0.0254(6) 0.0006(5) -0.0007(5) 0.0023(5) C2 0.0497(10) 0.0254(7) 0.0426(9) -0.0025(7) 0.0095(8) 0.0015(7) C3 0.0516(10) 0.0482(10) 0.0342(9) -0.0007(7) 0.0159(8) 0.0108(8) N1 0.0514(9) 0.0257(6) 0.0434(8) -0.0011(6) 0.0135(7) -0.0045(6) N2 0.0367(7) 0.0250(6) 0.0311(6) -0.0016(5) 0.0072(5) -0.0019(5) N3 0.0348(7) 0.0277(6) 0.0291(6) -0.0006(5) 0.0060(5) 0.0052(5) _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 2.2477(13) 3_655 ? Cd1 N2 2.2477(13) . ? Cd1 S1 2.5029(4) 7_566 ? Cd1 S1 2.5029(4) 5_665 ? S1 C1 1.7260(14) . ? S1 Cd1 2.5029(4) 5_665 ? C1 N2 1.3242(18) . ? C1 N3 1.3613(18) . ? C2 N1 1.301(2) . ? C2 N3 1.356(2) . ? C2 H2A 0.9300 . ? C3 N3 1.462(2) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? N1 N2 1.3898(18) . ? 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 103.20(6) 3_655 . ? N2 Cd1 S1 103.85(4) 3_655 7_566 ? N2 Cd1 S1 107.79(4) . 7_566 ? N2 Cd1 S1 107.79(4) 3_655 5_665 ? N2 Cd1 S1 103.85(4) . 5_665 ? S1 Cd1 S1 127.957(18) 7_566 5_665 ? C1 S1 Cd1 104.27(5) . 5_665 ? N2 C1 N3 108.15(12) . . ? N2 C1 S1 126.06(11) . . ? N3 C1 S1 125.68(11) . . ? N1 C2 N3 111.54(14) . . ? N1 C2 H2A 124.2 . . ? N3 C2 H2A 124.2 . . ? N3 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 N1 N2 105.66(13) . . ? C1 N2 N1 108.81(12) . . ? C1 N2 Cd1 122.67(10) . . ? N1 N2 Cd1 128.40(10) . . ? C2 N3 C1 105.84(13) . . ? C2 N3 C3 127.14(14) . . ? C1 N3 C3 127.01(14) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.22 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.305 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.054 #---end data_Cd(MPTRZ)Br _database_code_depnum_ccdc_archive 'CCDC 780920' #TrackingRef '- CdMPTRZ.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H4 Br Cd N3 S' _chemical_formula_weight 306.46 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' 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.5428(9) _cell_length_b 6.9491(5) _cell_length_c 10.3800(8) _cell_angle_alpha 90.00 _cell_angle_beta 116.3210(10) _cell_angle_gamma 90.00 _cell_volume 746.28(10) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4257 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 28.23 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 8.473 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.134 _exptl_absorpt_correction_T_max 0.251 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEXII area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6743 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 28.29 _reflns_number_total 1834 _reflns_number_gt 1660 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0318P)^2^+0.6615P] 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 1834 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0610 _refine_ls_wR_factor_gt 0.0595 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.619417(19) 0.23701(3) 0.04169(3) 0.03602(9) Uani 1 1 d . . . Br1 Br 0.83978(3) 0.11770(5) 0.07461(4) 0.04875(11) Uani 1 1 d . . . S1 S 0.56566(8) 0.02903(11) 0.21526(9) 0.03832(18) Uani 1 1 d . . . N1 N 0.6740(2) -0.4615(3) 0.1349(3) 0.0324(5) Uani 1 1 d . . . N2 N 0.5864(2) -0.3144(3) 0.1096(3) 0.0294(5) Uani 1 1 d . . . C1 C 0.6438(3) -0.1778(4) 0.2057(3) 0.0271(5) Uani 1 1 d . . . N3 N 0.7667(2) -0.2335(3) 0.2928(3) 0.0314(5) Uani 1 1 d . . . C2 C 0.7808(3) -0.4093(4) 0.2453(3) 0.0342(6) Uani 1 1 d . . . H2B H 0.8560 -0.4826 0.2854 0.041 Uiso 1 1 calc R . . C3 C 0.8635(3) -0.1266(5) 0.4132(4) 0.0454(8) Uani 1 1 d . . . H3A H 0.8277 -0.0060 0.4231 0.068 Uiso 1 1 calc R . . H3B H 0.9374 -0.1032 0.3959 0.068 Uiso 1 1 calc R . . H3C H 0.8893 -0.2001 0.4998 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02266(12) 0.02263(11) 0.05437(16) -0.00297(8) 0.00946(10) 0.00072(7) Br1 0.03360(18) 0.0474(2) 0.0700(3) 0.00785(15) 0.02720(17) 0.00777(13) S1 0.0349(4) 0.0350(3) 0.0493(4) -0.0001(3) 0.0225(3) 0.0088(3) N1 0.0294(12) 0.0221(10) 0.0397(13) -0.0003(9) 0.0099(10) -0.0002(9) N2 0.0243(11) 0.0228(10) 0.0372(13) 0.0008(9) 0.0101(10) -0.0031(8) C1 0.0239(12) 0.0252(12) 0.0339(14) 0.0019(10) 0.0143(11) -0.0009(9) N3 0.0250(12) 0.0267(11) 0.0368(12) -0.0045(9) 0.0087(10) 0.0003(8) C2 0.0304(14) 0.0250(12) 0.0415(16) -0.0014(11) 0.0108(12) 0.0037(10) C3 0.0335(16) 0.0418(17) 0.0457(18) -0.0136(14) 0.0038(13) -0.0006(12) _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 2.256(2) 3_655 ? Cd1 N1 2.277(2) 1_565 ? Cd1 Br1 2.5501(4) . ? Cd1 S1 2.5906(9) . ? S1 C1 1.723(3) . ? N1 C2 1.309(4) . ? N1 N2 1.378(3) . ? N1 Cd1 2.277(2) 1_545 ? N2 C1 1.322(4) . ? N2 Cd1 2.256(2) 3_655 ? C1 N3 1.357(4) . ? N3 C2 1.354(3) . ? N3 C3 1.457(4) . ? C2 H2B 0.9300 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? 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 N1 94.82(8) 3_655 1_565 ? N2 Cd1 Br1 148.27(6) 3_655 . ? N1 Cd1 Br1 99.84(6) 1_565 . ? N2 Cd1 S1 96.55(6) 3_655 . ? N1 Cd1 S1 108.91(7) 1_565 . ? Br1 Cd1 S1 104.931(19) . . ? C1 S1 Cd1 97.62(9) . . ? C2 N1 N2 106.8(2) . . ? C2 N1 Cd1 127.08(18) . 1_545 ? N2 N1 Cd1 124.08(17) . 1_545 ? C1 N2 N1 108.0(2) . . ? C1 N2 Cd1 112.02(17) . 3_655 ? N1 N2 Cd1 140.01(18) . 3_655 ? N2 C1 N3 108.9(2) . . ? N2 C1 S1 122.8(2) . . ? N3 C1 S1 128.2(2) . . ? C1 N3 C2 105.9(2) . . ? C1 N3 C3 127.2(2) . . ? C2 N3 C3 127.0(3) . . ? N1 C2 N3 110.5(2) . . ? N1 C2 H2B 124.8 . . ? N3 C2 H2B 124.8 . . ? N3 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.863 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.098 #---end data_Cd(MPTRZ)I _database_code_depnum_ccdc_archive 'CCDC 780921' #TrackingRef '- CdMPTRZ.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H4 Cd I N3 S' _chemical_formula_weight 353.47 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.9989(8) _cell_length_b 10.3114(12) _cell_length_c 12.9438(12) _cell_angle_alpha 90.00 _cell_angle_beta 118.441(5) _cell_angle_gamma 90.00 _cell_volume 821.39(15) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4463 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 28.32 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.858 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 6.593 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.622 _exptl_absorpt_correction_T_max 0.715 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEXII area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7523 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 28.36 _reflns_number_total 2057 _reflns_number_gt 1871 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0317P)^2^+0.4094P] 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 SHELXL _refine_ls_extinction_coef 0.0073(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2057 _refine_ls_number_parameters 83 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0610 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 0.33312(3) -0.06563(2) -0.40588(2) 0.03030(10) Uani 1 1 d . . . I1 I 0.43580(4) -0.08900(3) -0.17830(2) 0.04781(11) Uani 1 1 d . . . S1 S 0.01585(13) -0.20065(9) -0.54712(8) 0.0375(2) Uani 1 1 d . . . N1 N -0.3719(4) -0.1481(3) -0.4153(2) 0.0318(5) Uani 1 1 d . . . N2 N -0.2883(4) -0.1153(3) -0.4898(2) 0.0297(5) Uani 1 1 d . . . N3 N -0.1159(4) -0.2862(3) -0.3891(2) 0.0321(6) Uani 1 1 d . . . C1 C -0.1338(4) -0.1989(3) -0.4728(3) 0.0267(6) Uani 1 1 d . . . C2 C -0.2657(5) -0.2503(3) -0.3570(3) 0.0354(7) Uani 1 1 d . . . H2B H -0.2898 -0.2928 -0.3009 0.042 Uiso 1 1 calc R . . C3 C 0.0316(7) -0.3967(4) -0.3449(4) 0.0516(10) Uani 1 1 d . . . H3A H 0.0171 -0.4374 -0.2823 0.077 Uiso 1 1 calc R . . H3B H 0.1785 -0.3674 -0.3161 0.077 Uiso 1 1 calc R . . H3C H -0.0037 -0.4580 -0.4072 0.077 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02552(13) 0.03644(15) 0.03167(15) 0.00608(9) 0.01583(11) 0.00171(8) I1 0.05391(17) 0.05843(18) 0.03312(15) 0.01049(10) 0.02237(13) 0.01596(11) S1 0.0319(4) 0.0502(5) 0.0368(4) -0.0077(4) 0.0215(4) -0.0072(3) N1 0.0298(12) 0.0334(14) 0.0369(14) 0.0046(11) 0.0198(11) 0.0021(11) N2 0.0263(11) 0.0321(13) 0.0346(14) 0.0030(11) 0.0177(11) -0.0005(10) N3 0.0287(12) 0.0314(13) 0.0382(15) 0.0064(11) 0.0176(12) 0.0055(11) C1 0.0234(12) 0.0279(14) 0.0284(15) -0.0014(11) 0.0119(12) -0.0030(11) C2 0.0328(15) 0.0394(18) 0.0404(19) 0.0099(14) 0.0227(15) 0.0039(13) C3 0.048(2) 0.042(2) 0.074(3) 0.0188(19) 0.037(2) 0.0181(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N2 2.236(3) 3_554 ? Cd1 N1 2.289(2) 1_655 ? Cd1 S1 2.5189(9) . ? Cd1 I1 2.6899(4) . ? S1 C1 1.727(3) . ? N1 C2 1.303(4) . ? N1 N2 1.388(3) . ? N1 Cd1 2.289(2) 1_455 ? N2 C1 1.317(4) . ? N2 Cd1 2.236(3) 3_554 ? N3 C2 1.351(4) . ? N3 C1 1.368(4) . ? N3 C3 1.458(4) . ? C2 H2B 0.9300 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? 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 N1 98.55(9) 3_554 1_655 ? N2 Cd1 S1 101.61(7) 3_554 . ? N1 Cd1 S1 105.17(7) 1_655 . ? N2 Cd1 I1 128.58(7) 3_554 . ? N1 Cd1 I1 104.34(7) 1_655 . ? S1 Cd1 I1 115.39(2) . . ? C1 S1 Cd1 98.56(10) . . ? C2 N1 N2 106.6(2) . . ? C2 N1 Cd1 123.4(2) . 1_455 ? N2 N1 Cd1 129.52(19) . 1_455 ? C1 N2 N1 108.0(2) . . ? C1 N2 Cd1 120.99(18) . 3_554 ? N1 N2 Cd1 129.70(19) . 3_554 ? C2 N3 C1 105.7(2) . . ? C2 N3 C3 127.0(3) . . ? C1 N3 C3 127.3(3) . . ? N2 C1 N3 108.7(2) . . ? N2 C1 S1 125.6(2) . . ? N3 C1 S1 125.7(2) . . ? N1 C2 N3 110.9(3) . . ? N1 C2 H2B 124.6 . . ? N3 C2 H2B 124.6 . . ? N3 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.822 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.134 #---end data_Cd(MPTRZ)(m-Br) _database_code_depnum_ccdc_archive 'CCDC 780922' #TrackingRef '- CdMPTRZ.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H4 Br Cd N3 S' _chemical_formula_weight 306.46 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' 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 Pbcn _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.8254(5) _cell_length_b 7.8337(3) _cell_length_c 17.8083(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1510.20(11) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5525 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 28.27 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 8.374 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.341 _exptl_absorpt_correction_T_max 0.392 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEXII area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13242 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 28.34 _reflns_number_total 1881 _reflns_number_gt 1684 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0299P)^2^+1.3198P] 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 SHELXL _refine_ls_extinction_coef 0.0071(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1881 _refine_ls_number_parameters 83 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0540 _refine_ls_wR_factor_gt 0.0522 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 0.177604(19) 0.18079(2) 0.671498(11) 0.02379(9) Uani 1 1 d . . . Br1 Br 0.30419(3) -0.02868(4) 0.584126(17) 0.03495(11) Uani 1 1 d . . . S1 S -0.05243(7) 0.18772(9) 0.63890(4) 0.02853(16) Uani 1 1 d . . . N2 N -0.1540(2) -0.0343(3) 0.73905(12) 0.0231(4) Uani 1 1 d . . . N3 N -0.0884(2) -0.1612(3) 0.63748(12) 0.0250(5) Uani 1 1 d . . . C1 C -0.0993(3) -0.0081(3) 0.67325(13) 0.0217(5) Uani 1 1 d . . . C2 C -0.1370(3) -0.2782(4) 0.68395(16) 0.0266(6) Uani 1 1 d . . . H2B H -0.1409 -0.3945 0.6737 0.032 Uiso 1 1 calc R . . C3 C -0.0428(3) -0.1904(4) 0.56115(16) 0.0388(8) Uani 1 1 d . . . H3A H -0.0445 -0.3104 0.5503 0.058 Uiso 1 1 calc R . . H3B H 0.0405 -0.1490 0.5571 0.058 Uiso 1 1 calc R . . H3C H -0.0944 -0.1308 0.5260 0.058 Uiso 1 1 calc R . . N1 N -0.1781(2) -0.2073(3) 0.74539(13) 0.0251(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 0.02664(13) 0.01746(12) 0.02728(12) 0.00027(7) -0.00207(7) -0.00165(7) Br1 0.0479(2) 0.02188(16) 0.03513(17) 0.00490(12) 0.01321(12) 0.00930(12) S1 0.0257(4) 0.0253(4) 0.0345(4) 0.0092(3) 0.0010(3) -0.0010(3) N2 0.0244(11) 0.0199(11) 0.0249(11) 0.0005(9) 0.0019(9) -0.0035(9) N3 0.0234(12) 0.0274(12) 0.0242(11) -0.0043(9) 0.0021(9) -0.0024(9) C1 0.0202(13) 0.0227(12) 0.0222(12) 0.0005(9) -0.0017(9) -0.0023(10) C2 0.0281(14) 0.0196(13) 0.0321(14) -0.0027(10) 0.0024(11) -0.0043(11) C3 0.0457(19) 0.0432(19) 0.0273(14) -0.0070(13) 0.0102(13) -0.0045(15) N1 0.0276(13) 0.0202(11) 0.0275(11) 0.0010(9) 0.0036(9) -0.0035(9) _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 2.324(2) 6_667 ? Cd1 N2 2.333(2) 3_556 ? Cd1 S1 2.5575(8) . ? Cd1 Br1 2.6441(4) . ? Cd1 Br1 2.7640(4) 8_665 ? S1 C1 1.727(3) . ? N2 C1 1.329(3) . ? N2 N1 1.385(3) . ? N2 Cd1 2.333(2) 3_556 ? N3 C2 1.343(4) . ? N3 C1 1.363(3) . ? N3 C3 1.464(3) . ? C2 N1 1.305(4) . ? C2 H2B 0.9300 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? N1 Cd1 2.324(2) 6_557 ? Br1 Cd1 2.7640(4) 8_655 ? 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 84.90(8) 6_667 3_556 ? N1 Cd1 S1 142.30(6) 6_667 . ? N2 Cd1 S1 93.66(6) 3_556 . ? N1 Cd1 Br1 105.10(6) 6_667 . ? N2 Cd1 Br1 90.59(6) 3_556 . ? S1 Cd1 Br1 112.59(2) . . ? N1 Cd1 Br1 89.99(6) 6_667 8_665 ? N2 Cd1 Br1 170.74(6) 3_556 8_665 ? S1 Cd1 Br1 85.652(17) . 8_665 ? Br1 Cd1 Br1 98.209(12) . 8_665 ? C1 S1 Cd1 100.78(10) . . ? C1 N2 N1 107.9(2) . . ? C1 N2 Cd1 122.64(18) . 3_556 ? N1 N2 Cd1 129.10(17) . 3_556 ? C2 N3 C1 106.2(2) . . ? C2 N3 C3 126.7(2) . . ? C1 N3 C3 126.9(2) . . ? N2 C1 N3 108.3(2) . . ? N2 C1 S1 125.5(2) . . ? N3 C1 S1 126.17(19) . . ? N1 C2 N3 111.1(2) . . ? N1 C2 H2B 124.5 . . ? N3 C2 H2B 124.5 . . ? N3 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 N1 N2 106.5(2) . . ? C2 N1 Cd1 127.03(19) . 6_557 ? N2 N1 Cd1 123.20(16) . 6_557 ? Cd1 Br1 Cd1 102.515(12) . 8_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.015 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.114 #---end data_Cd(MPTRZ)(m-Cl) _database_code_depnum_ccdc_archive 'CCDC 780923' #TrackingRef '- CdMPTRZ.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H4 Cd Cl N3 S' _chemical_formula_weight 262.00 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 Orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.813(2) _cell_length_b 7.6106(16) _cell_length_c 17.770(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1462.3(5) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3688 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 28.92 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 3.548 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.238 _exptl_absorpt_correction_T_max 0.461 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8344 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 29.06 _reflns_number_total 1841 _reflns_number_gt 1594 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0242P)^2^+0.8183P] 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 SHELXL _refine_ls_extinction_coef 0.00141(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1841 _refine_ls_number_parameters 83 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0214 _refine_ls_wR_factor_ref 0.0519 _refine_ls_wR_factor_gt 0.0492 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 0.178551(16) 0.17230(2) 0.670668(10) 0.02452(8) Uani 1 1 d . . . S1 S -0.05098(6) 0.18389(8) 0.63715(4) 0.02963(15) Uani 1 1 d . . . N2 N -0.15154(18) -0.0436(3) 0.73800(11) 0.0238(4) Uani 1 1 d . . . N3 N -0.08622(18) -0.1758(3) 0.63650(12) 0.0265(4) Uani 1 1 d . . . C1 C -0.0972(2) -0.0175(3) 0.67206(13) 0.0235(5) Uani 1 1 d . . . C2 C -0.1346(3) -0.2955(3) 0.68362(15) 0.0297(5) Uani 1 1 d . . . H2B H -0.1388 -0.4153 0.6736 0.036 Uiso 1 1 calc R . . C3 C -0.0396(3) -0.2070(4) 0.55993(15) 0.0412(7) Uani 1 1 d . . . H3A H -0.0417 -0.3306 0.5492 0.062 Uiso 1 1 calc R . . H3B H 0.0439 -0.1652 0.5562 0.062 Uiso 1 1 calc R . . H3C H -0.0906 -0.1456 0.5244 0.062 Uiso 1 1 calc R . . N1 N -0.17482(17) -0.2221(3) 0.74524(12) 0.0251(4) Uani 1 1 d . . . Cl1 Cl 0.29574(7) -0.04261(8) 0.58955(4) 0.03716(17) 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 0.02844(12) 0.01982(11) 0.02530(12) 0.00043(7) -0.00171(6) -0.00151(6) S1 0.0280(3) 0.0287(3) 0.0321(3) 0.0086(3) 0.0009(3) -0.0007(2) N2 0.0266(10) 0.0225(10) 0.0223(10) -0.0010(8) 0.0023(8) -0.0017(8) N3 0.0281(10) 0.0301(12) 0.0214(10) -0.0043(8) 0.0020(8) -0.0023(8) C1 0.0213(11) 0.0260(12) 0.0232(11) 0.0008(9) -0.0010(9) -0.0016(9) C2 0.0315(13) 0.0246(13) 0.0329(14) -0.0036(10) 0.0034(11) -0.0032(10) C3 0.0507(17) 0.0463(17) 0.0268(14) -0.0110(12) 0.0112(12) -0.0046(13) N1 0.0285(11) 0.0212(10) 0.0257(11) 0.0000(8) 0.0021(8) -0.0028(8) Cl1 0.0531(4) 0.0252(3) 0.0331(3) 0.0047(3) 0.0131(3) 0.0101(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.322(2) 6_667 ? Cd1 N2 2.328(2) 3_556 ? Cd1 Cl1 2.5216(7) . ? Cd1 S1 2.5538(8) . ? Cd1 Cl1 2.6196(8) 8_665 ? S1 C1 1.727(2) . ? N2 C1 1.326(3) . ? N2 N1 1.387(3) . ? N2 Cd1 2.328(2) 3_556 ? N3 C2 1.343(3) . ? N3 C1 1.366(3) . ? N3 C3 1.470(3) . ? C2 N1 1.304(3) . ? C2 H2B 0.9300 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? N1 Cd1 2.322(2) 6_557 ? Cl1 Cd1 2.6196(8) 8_655 ? 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 83.19(7) 6_667 3_556 ? N1 Cd1 Cl1 104.43(6) 6_667 . ? N2 Cd1 Cl1 90.21(5) 3_556 . ? N1 Cd1 S1 143.28(5) 6_667 . ? N2 Cd1 S1 93.73(5) 3_556 . ? Cl1 Cd1 S1 112.17(3) . . ? N1 Cd1 Cl1 89.71(6) 6_667 8_665 ? N2 Cd1 Cl1 168.98(5) 3_556 8_665 ? Cl1 Cd1 Cl1 99.75(3) . 8_665 ? S1 Cd1 Cl1 86.92(2) . 8_665 ? C1 S1 Cd1 99.59(8) . . ? C1 N2 N1 108.01(19) . . ? C1 N2 Cd1 124.46(16) . 3_556 ? N1 N2 Cd1 127.14(14) . 3_556 ? C2 N3 C1 106.0(2) . . ? C2 N3 C3 126.9(2) . . ? C1 N3 C3 126.9(2) . . ? N2 C1 N3 108.4(2) . . ? N2 C1 S1 125.35(19) . . ? N3 C1 S1 126.28(17) . . ? N1 C2 N3 111.3(2) . . ? N1 C2 H2B 124.4 . . ? N3 C2 H2B 124.4 . . ? N3 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 N1 N2 106.32(19) . . ? C2 N1 Cd1 128.31(17) . 6_557 ? N2 N1 Cd1 121.50(14) . 6_557 ? Cd1 Cl1 Cd1 106.02(3) . 8_655 ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 29.06 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.512 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.094 #---end data_Cd3(OH)2(MPTRZ)4 _database_code_depnum_ccdc_archive 'CCDC 780924' #TrackingRef '- CdMPTRZ.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H18 Cd3 N12 O2 S4' _chemical_formula_weight 827.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.8059(4) _cell_length_b 9.6914(5) _cell_length_c 9.7577(5) _cell_angle_alpha 90.5700(10) _cell_angle_beta 109.6640(10) _cell_angle_gamma 94.7980(10) _cell_volume 603.45(6) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4429 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 28.22 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 398 _exptl_absorpt_coefficient_mu 3.002 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.612 _exptl_absorpt_correction_T_max 0.716 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEXII area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5646 _diffrn_reflns_av_R_equivalents 0.0128 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 28.25 _reflns_number_total 2889 _reflns_number_gt 2724 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0308P)^2^+0.4271P] 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 2889 _refine_ls_number_parameters 155 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0206 _refine_ls_R_factor_gt 0.0193 _refine_ls_wR_factor_ref 0.0516 _refine_ls_wR_factor_gt 0.0509 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 0.5000 0.02031(6) Uani 1 2 d S . . Cd2 Cd 0.49649(2) 0.179757(15) 0.495165(16) 0.02231(6) Uani 1 1 d . . . S1 S -0.29952(10) -0.25015(8) 0.75766(7) 0.03866(15) Uani 1 1 d . . . S2 S 0.44710(9) 0.32829(7) 0.70117(7) 0.03587(15) Uani 1 1 d . . . O1 O 0.3453(2) -0.00579(15) 0.56895(16) 0.0222(3) Uani 1 1 d D . . H1 H 0.366(5) -0.002(3) 0.6638(13) 0.046(9) Uiso 1 1 d D . . N1 N 0.2350(3) -0.0288(3) 0.8363(2) 0.0390(5) Uani 1 1 d . . . N2 N 0.0345(3) -0.0744(2) 0.7407(2) 0.0267(4) Uani 1 1 d . . . N3 N 0.0723(3) -0.1580(2) 0.9547(2) 0.0297(4) Uani 1 1 d . . . N4 N -0.1614(3) 0.29879(19) 0.5696(2) 0.0238(4) Uani 1 1 d . . . N5 N 0.0249(3) 0.24217(19) 0.5806(2) 0.0227(4) Uani 1 1 d . . . N6 N 0.0982(3) 0.44961(18) 0.6869(2) 0.0242(4) Uani 1 1 d . . . C1 C -0.0600(3) -0.1535(2) 0.8142(2) 0.0229(4) Uani 1 1 d . . . C2 C 0.2508(4) -0.0811(3) 0.9612(3) 0.0396(6) Uani 1 1 d . . . H2A H 0.3694 -0.0676 1.0442 0.047 Uiso 1 1 calc R . . C3 C 0.0331(5) -0.2345(4) 1.0717(3) 0.0458(7) Uani 1 1 d . . . H3A H -0.1063 -0.2801 1.0373 0.069 Uiso 1 1 calc R . . H3B H 0.0476 -0.1715 1.1518 0.069 Uiso 1 1 calc R . . H3C H 0.1324 -0.3023 1.1034 0.069 Uiso 1 1 calc R . . C4 C 0.1806(3) 0.3354(2) 0.6519(2) 0.0221(4) Uani 1 1 d . . . C5 C -0.1119(3) 0.4219(2) 0.6333(3) 0.0264(4) Uani 1 1 d . . . H5A H -0.2078 0.4820 0.6406 0.032 Uiso 1 1 calc R . . C6 C 0.2147(4) 0.5738(3) 0.7716(3) 0.0396(6) Uani 1 1 d . . . H6A H 0.1181 0.6374 0.7800 0.059 Uiso 1 1 calc R . . H6B H 0.3042 0.6171 0.7235 0.059 Uiso 1 1 calc R . . H6C H 0.2982 0.5485 0.8670 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01280(10) 0.02417(11) 0.02429(11) 0.00027(8) 0.00668(8) 0.00199(8) Cd2 0.01376(8) 0.02325(9) 0.02916(9) -0.00078(6) 0.00657(6) 0.00072(6) S1 0.0224(3) 0.0494(4) 0.0362(3) 0.0141(3) 0.0018(2) -0.0079(3) S2 0.0139(2) 0.0444(3) 0.0461(3) -0.0211(3) 0.0077(2) -0.0018(2) O1 0.0143(7) 0.0267(8) 0.0263(7) -0.0011(6) 0.0082(6) 0.0012(5) N1 0.0259(10) 0.0541(14) 0.0292(10) 0.0017(9) 0.0032(8) -0.0139(10) N2 0.0222(9) 0.0323(10) 0.0229(9) 0.0014(7) 0.0052(7) -0.0023(7) N3 0.0252(9) 0.0408(11) 0.0213(9) 0.0035(8) 0.0056(7) 0.0008(8) N4 0.0139(8) 0.0261(9) 0.0311(9) -0.0007(7) 0.0073(7) 0.0019(7) N5 0.0144(8) 0.0247(9) 0.0290(9) -0.0043(7) 0.0080(7) -0.0003(6) N6 0.0181(8) 0.0223(9) 0.0332(10) -0.0045(7) 0.0110(7) -0.0021(7) C1 0.0200(10) 0.0263(10) 0.0212(10) 0.0008(7) 0.0054(8) 0.0032(8) C2 0.0269(12) 0.0575(17) 0.0258(11) -0.0008(10) 0.0011(9) -0.0098(11) C3 0.0405(15) 0.070(2) 0.0273(12) 0.0164(12) 0.0117(11) 0.0044(14) C4 0.0176(9) 0.0253(10) 0.0239(10) -0.0039(7) 0.0088(8) -0.0014(8) C5 0.0185(10) 0.0260(11) 0.0358(12) -0.0002(8) 0.0108(9) 0.0020(8) C6 0.0305(13) 0.0285(12) 0.0574(17) -0.0163(11) 0.0143(12) -0.0061(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 O1 2.2220(14) 2_556 ? Cd1 O1 2.2220(14) . ? Cd1 N2 2.4044(19) 2_556 ? Cd1 N2 2.4044(19) . ? Cd1 N5 2.4420(17) 2_556 ? Cd1 N5 2.4420(17) . ? Cd1 Cd2 3.6850(2) . ? Cd1 Cd2 3.6850(2) 2_556 ? Cd1 H1 2.47(3) . ? Cd2 O1 2.2417(15) . ? Cd2 O1 2.2649(14) 2_656 ? Cd2 N4 2.3825(18) 1_655 ? Cd2 S1 2.5118(7) 2_556 ? Cd2 S2 2.5891(6) . ? Cd2 Cd2 3.4903(3) 2_656 ? S1 C1 1.723(2) . ? S1 Cd2 2.5118(7) 2_556 ? S2 C4 1.720(2) . ? O1 Cd2 2.2649(14) 2_656 ? O1 H1 0.888(10) . ? N1 C2 1.300(4) . ? N1 N2 1.401(3) . ? N2 C1 1.324(3) . ? N3 C2 1.353(3) . ? N3 C1 1.367(3) . ? N3 C3 1.453(3) . ? N4 C5 1.304(3) . ? N4 N5 1.395(2) . ? N4 Cd2 2.3825(18) 1_455 ? N5 C4 1.324(3) . ? N6 C5 1.349(3) . ? N6 C4 1.372(3) . ? N6 C6 1.463(3) . ? C2 H2A 0.9300 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C5 H5A 0.9300 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? 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 O1 180.0 2_556 . ? O1 Cd1 N2 85.59(6) 2_556 2_556 ? O1 Cd1 N2 94.41(6) . 2_556 ? O1 Cd1 N2 94.41(6) 2_556 . ? O1 Cd1 N2 85.59(6) . . ? N2 Cd1 N2 180.0 2_556 . ? O1 Cd1 N5 93.60(5) 2_556 2_556 ? O1 Cd1 N5 86.40(5) . 2_556 ? N2 Cd1 N5 90.84(6) 2_556 2_556 ? N2 Cd1 N5 89.16(6) . 2_556 ? O1 Cd1 N5 86.40(5) 2_556 . ? O1 Cd1 N5 93.60(5) . . ? N2 Cd1 N5 89.16(6) 2_556 . ? N2 Cd1 N5 90.84(6) . . ? N5 Cd1 N5 180.00(9) 2_556 . ? O1 Cd1 Cd2 145.47(4) 2_556 . ? O1 Cd1 Cd2 34.53(4) . . ? N2 Cd1 Cd2 69.43(5) 2_556 . ? N2 Cd1 Cd2 110.57(5) . . ? N5 Cd1 Cd2 109.69(4) 2_556 . ? N5 Cd1 Cd2 70.31(4) . . ? O1 Cd1 Cd2 34.53(4) 2_556 2_556 ? O1 Cd1 Cd2 145.47(4) . 2_556 ? N2 Cd1 Cd2 110.57(5) 2_556 2_556 ? N2 Cd1 Cd2 69.43(5) . 2_556 ? N5 Cd1 Cd2 70.31(4) 2_556 2_556 ? N5 Cd1 Cd2 109.69(4) . 2_556 ? Cd2 Cd1 Cd2 180.0 . 2_556 ? O1 Cd1 H1 159.0(4) 2_556 . ? O1 Cd1 H1 21.0(4) . . ? N2 Cd1 H1 114.0(5) 2_556 . ? N2 Cd1 H1 66.0(5) . . ? N5 Cd1 H1 93.5(7) 2_556 . ? N5 Cd1 H1 86.5(7) . . ? Cd2 Cd1 H1 47.4(6) . . ? Cd2 Cd1 H1 132.6(6) 2_556 . ? O1 Cd2 O1 78.48(6) . 2_656 ? O1 Cd2 N4 135.45(6) . 1_655 ? O1 Cd2 N4 83.84(6) 2_656 1_655 ? O1 Cd2 S1 114.61(4) . 2_556 ? O1 Cd2 S1 97.33(4) 2_656 2_556 ? N4 Cd2 S1 107.96(5) 1_655 2_556 ? O1 Cd2 S2 89.20(4) . . ? O1 Cd2 S2 148.13(4) 2_656 . ? N4 Cd2 S2 84.76(5) 1_655 . ? S1 Cd2 S2 114.49(3) 2_556 . ? O1 Cd2 Cd2 39.48(4) . 2_656 ? O1 Cd2 Cd2 39.00(4) 2_656 2_656 ? N4 Cd2 Cd2 112.83(4) 1_655 2_656 ? S1 Cd2 Cd2 110.507(19) 2_556 2_656 ? S2 Cd2 Cd2 122.826(19) . 2_656 ? O1 Cd2 Cd1 34.18(4) . . ? O1 Cd2 Cd1 102.38(4) 2_656 . ? N4 Cd2 Cd1 162.60(5) 1_655 . ? S1 Cd2 Cd1 87.552(15) 2_556 . ? S2 Cd2 Cd1 81.527(14) . . ? Cd2 Cd2 Cd1 66.907(5) 2_656 . ? C1 S1 Cd2 107.12(8) . 2_556 ? C4 S2 Cd2 104.83(7) . . ? Cd1 O1 Cd2 111.29(6) . . ? Cd1 O1 Cd2 123.84(7) . 2_656 ? Cd2 O1 Cd2 101.52(6) . 2_656 ? Cd1 O1 H1 95(2) . . ? Cd2 O1 H1 113(2) . . ? Cd2 O1 H1 112(2) 2_656 . ? C2 N1 N2 106.6(2) . . ? C1 N2 N1 107.55(18) . . ? C1 N2 Cd1 142.83(15) . . ? N1 N2 Cd1 109.23(14) . . ? C2 N3 C1 105.9(2) . . ? C2 N3 C3 126.9(2) . . ? C1 N3 C3 127.2(2) . . ? C5 N4 N5 107.51(17) . . ? C5 N4 Cd2 124.54(14) . 1_455 ? N5 N4 Cd2 126.80(13) . 1_455 ? C4 N5 N4 107.11(17) . . ? C4 N5 Cd1 134.89(14) . . ? N4 N5 Cd1 117.43(12) . . ? C5 N6 C4 106.24(18) . . ? C5 N6 C6 126.81(19) . . ? C4 N6 C6 126.89(19) . . ? N2 C1 N3 108.82(19) . . ? N2 C1 S1 130.83(16) . . ? N3 C1 S1 120.24(17) . . ? N1 C2 N3 111.1(2) . . ? N1 C2 H2A 124.4 . . ? N3 C2 H2A 124.4 . . ? N3 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N5 C4 N6 108.81(18) . . ? N5 C4 S2 129.97(16) . . ? N6 C4 S2 121.22(16) . . ? N4 C5 N6 110.33(18) . . ? N4 C5 H5A 124.8 . . ? N6 C5 H5A 124.8 . . ? N6 C6 H6A 109.5 . . ? N6 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N6 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N1 0.888(10) 2.16(2) 2.953(3) 148(3) . _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.542 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.102 #---end