# 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_mo_vsh_12_0m _database_code_depnum_ccdc_archive 'CCDC 916533' #TrackingRef 'C1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H6 Cd Cl N3 O3 S' _chemical_formula_weight 372.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 6.6344(12) _cell_length_b 7.794(3) _cell_length_c 10.419(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.716(5) _cell_angle_gamma 90.00 _cell_volume 531.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 503 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 36.03 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 2.501 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5207 _exptl_absorpt_correction_T_max 0.9754 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith MicroMount' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Micorfocus source E025 IuS' _diffrn_source_type 'Bruker APEX DUO' _diffrn_source_power 50 _diffrn_source_current 0.6 _diffrn_source_size '0.2 mm x 0.2 mm fine focus' _diffrn_radiation_monochromator 'Quazar MX Multilayer Optics' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'APEX DUO Kappa 4-axis goniometer' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 14292 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 36.27 _reflns_number_total 5041 _reflns_number_gt 4930 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2011.4-0' _computing_cell_refinement 'Bruker APEX2 v2011.4-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution Sir2011 _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0414P)^2^+0.0123P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration ad _refine_ls_abs_structure_Flack 0.285(18) _refine_ls_number_reflns 5041 _refine_ls_number_parameters 155 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0226 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0648 _refine_ls_wR_factor_gt 0.0572 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.160 _refine_ls_shift/su_max 0.004 _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 0.988195(19) 0.60049(3) 1.005318(12) 0.01056(3) Uani 1 1 d . . . S1 S 1.15784(7) 0.85593(7) 0.74246(4) 0.00968(7) Uani 1 1 d . . . Cl1 Cl 1.25341(7) 0.35728(7) 1.01476(4) 0.01363(8) Uani 1 1 d . . . O3 O 1.3558(2) 0.8478(2) 0.70170(14) 0.0144(2) Uani 1 1 d . . . O1 O 1.1147(3) 0.70749(19) 0.81986(15) 0.0141(3) Uani 1 1 d . . . O2 O 1.1217(3) 1.02016(19) 0.80376(16) 0.0157(3) Uani 1 1 d . . . C1 C 0.9727(3) 0.8465(3) 0.59755(17) 0.0112(3) Uani 1 1 d . . . C2 C 1.0255(3) 0.8866(3) 0.4777(2) 0.0146(3) Uani 1 1 d . . . H2 H 1.1623 0.9170 0.4719 0.017 Uiso 1 1 calc R . . C6 C 0.7738(3) 0.8024(3) 0.6088(2) 0.0180(4) Uani 1 1 d . . . H6 H 0.7396 0.7769 0.6916 0.022 Uiso 1 1 calc R . . C5 C 0.6248(3) 0.7959(3) 0.4974(2) 0.0191(4) Uani 1 1 d . . . H5 H 0.4886 0.7631 0.5030 0.023 Uiso 1 1 calc R . . C4 C 0.6782(3) 0.8384(3) 0.37757(18) 0.0121(3) Uani 1 1 d . . . C3 C 0.8759(3) 0.8819(3) 0.3651(2) 0.0158(3) Uani 1 1 d . . . H3 H 0.9097 0.9080 0.2822 0.019 Uiso 1 1 calc R . . N1 N 0.5170(2) 0.8395(2) 0.26569(15) 0.0124(3) Uani 1 1 d . . . C7 C 0.4304(3) 0.9807(2) 0.2010(2) 0.0130(3) Uani 1 1 d . . . H7 H 0.4814 1.0945 0.2130 0.016 Uiso 1 1 calc R . . N3 N 0.2657(3) 0.9349(2) 0.11970(18) 0.0125(3) Uani 1 1 d . . . N2 N 0.2456(3) 0.7592(2) 0.12956(18) 0.0129(3) Uani 1 1 d . . . C8 C 0.3983(3) 0.7047(2) 0.2172(2) 0.0142(3) Uani 1 1 d . . . H8 H 0.4220 0.5885 0.2427 0.017 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 0.01155(5) 0.00889(5) 0.01048(5) 0.00002(5) -0.00030(3) -0.00126(6) S1 0.00962(17) 0.01092(15) 0.00833(15) 0.00009(14) 0.00101(12) 0.00050(14) Cl1 0.01263(17) 0.01180(15) 0.01662(18) -0.00001(15) 0.00289(13) -0.00045(14) O3 0.0103(6) 0.0191(5) 0.0138(6) 0.0002(6) 0.0024(4) 0.0003(5) O1 0.0172(7) 0.0132(6) 0.0121(6) 0.0029(5) 0.0030(5) -0.0002(5) O2 0.0216(7) 0.0124(5) 0.0134(6) -0.0037(5) 0.0038(6) 0.0012(5) C1 0.0102(7) 0.0133(6) 0.0097(6) 0.0001(6) 0.0009(5) 0.0001(6) C2 0.0110(8) 0.0210(9) 0.0113(7) 0.0021(6) 0.0008(6) -0.0037(6) C6 0.0126(8) 0.0301(9) 0.0114(7) 0.0025(7) 0.0023(6) -0.0019(7) C5 0.0105(8) 0.0339(10) 0.0129(8) 0.0021(7) 0.0020(6) -0.0022(7) C4 0.0104(7) 0.0152(7) 0.0100(6) -0.0008(6) -0.0001(5) -0.0005(6) C3 0.0129(8) 0.0231(9) 0.0111(7) 0.0027(6) 0.0010(6) -0.0021(6) N1 0.0107(6) 0.0130(6) 0.0121(6) 0.0005(5) -0.0016(5) 0.0012(5) C7 0.0116(7) 0.0118(7) 0.0148(8) 0.0003(6) -0.0001(6) -0.0002(6) N3 0.0116(6) 0.0116(6) 0.0133(7) 0.0010(5) -0.0004(6) -0.0005(5) N2 0.0137(7) 0.0095(6) 0.0144(7) 0.0000(5) -0.0010(6) -0.0007(5) C8 0.0146(8) 0.0116(7) 0.0145(8) 0.0008(6) -0.0028(6) 0.0002(6) _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 O2 2.3174(17) 2_747 ? Cd1 N2 2.3185(18) 1_656 ? Cd1 N3 2.3366(18) 2_646 ? Cd1 O1 2.3836(16) . ? Cd1 Cl1 2.5506(8) 2_757 ? Cd1 Cl1 2.5769(8) . ? S1 O3 1.4482(16) . ? S1 O1 1.4658(16) . ? S1 O2 1.4682(16) . ? S1 C1 1.7798(17) . ? Cl1 Cd1 2.5506(8) 2_747 ? O2 Cd1 2.3174(17) 2_757 ? C1 C6 1.387(3) . ? C1 C2 1.389(3) . ? C2 C3 1.403(3) . ? C6 C5 1.393(3) . ? C5 C4 1.394(3) . ? C4 C3 1.382(3) . ? C4 N1 1.443(2) . ? N1 C8 1.358(3) . ? N1 C7 1.366(3) . ? C7 N3 1.314(3) . ? N3 N2 1.381(2) . ? N3 Cd1 2.3366(18) 2_656 ? N2 C8 1.314(3) . ? N2 Cd1 2.3185(17) 1_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 O2 Cd1 N2 88.49(6) 2_747 1_656 ? O2 Cd1 N3 91.59(7) 2_747 2_646 ? N2 Cd1 N3 178.60(7) 1_656 2_646 ? O2 Cd1 O1 174.43(6) 2_747 . ? N2 Cd1 O1 86.50(6) 1_656 . ? N3 Cd1 O1 93.48(6) 2_646 . ? O2 Cd1 Cl1 89.89(4) 2_747 2_757 ? N2 Cd1 Cl1 91.18(5) 1_656 2_757 ? N3 Cd1 Cl1 90.22(5) 2_646 2_757 ? O1 Cd1 Cl1 87.79(4) . 2_757 ? O2 Cd1 Cl1 94.60(4) 2_747 . ? N2 Cd1 Cl1 86.41(5) 1_656 . ? N3 Cd1 Cl1 92.19(5) 2_646 . ? O1 Cd1 Cl1 87.52(4) . . ? Cl1 Cd1 Cl1 174.845(16) 2_757 . ? O3 S1 O1 113.44(10) . . ? O3 S1 O2 112.85(10) . . ? O1 S1 O2 112.80(10) . . ? O3 S1 C1 106.23(9) . . ? O1 S1 C1 105.26(9) . . ? O2 S1 C1 105.37(10) . . ? Cd1 Cl1 Cd1 99.12(3) 2_747 . ? S1 O1 Cd1 148.24(10) . . ? S1 O2 Cd1 135.00(10) . 2_757 ? C6 C1 C2 121.29(16) . . ? C6 C1 S1 117.95(15) . . ? C2 C1 S1 120.74(14) . . ? C1 C2 C3 119.72(19) . . ? C1 C6 C5 119.35(19) . . ? C6 C5 C4 119.06(19) . . ? C3 C4 C5 122.09(17) . . ? C3 C4 N1 120.54(17) . . ? C5 C4 N1 117.35(17) . . ? C4 C3 C2 118.46(19) . . ? C8 N1 C7 105.68(15) . . ? C8 N1 C4 126.90(17) . . ? C7 N1 C4 126.59(17) . . ? N3 C7 N1 109.50(16) . . ? C7 N3 N2 107.57(17) . . ? C7 N3 Cd1 130.69(13) . 2_656 ? N2 N3 Cd1 121.30(14) . 2_656 ? C8 N2 N3 107.39(17) . . ? C8 N2 Cd1 128.62(13) . 1_454 ? N3 N2 Cd1 123.96(14) . 1_454 ? N2 C8 N1 109.84(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Cd1 Cl1 Cd1 63.53(4) 2_747 . . 2_747 ? N2 Cd1 Cl1 Cd1 151.72(5) 1_656 . . 2_747 ? N3 Cd1 Cl1 Cd1 -28.24(5) 2_646 . . 2_747 ? O1 Cd1 Cl1 Cd1 -121.63(4) . . . 2_747 ? Cl1 Cd1 Cl1 Cd1 -146.07(13) 2_757 . . 2_747 ? O3 S1 O1 Cd1 135.62(18) . . . . ? O2 S1 O1 Cd1 5.7(2) . . . . ? C1 S1 O1 Cd1 -108.65(19) . . . . ? O2 Cd1 O1 S1 -34.9(8) 2_747 . . . ? N2 Cd1 O1 S1 -60.86(19) 1_656 . . . ? N3 Cd1 O1 S1 120.54(19) 2_646 . . . ? Cl1 Cd1 O1 S1 30.46(19) 2_757 . . . ? Cl1 Cd1 O1 S1 -147.41(19) . . . . ? O3 S1 O2 Cd1 -130.26(13) . . . 2_757 ? O1 S1 O2 Cd1 -0.06(17) . . . 2_757 ? C1 S1 O2 Cd1 114.24(14) . . . 2_757 ? O3 S1 C1 C6 161.72(18) . . . . ? O1 S1 C1 C6 41.1(2) . . . . ? O2 S1 C1 C6 -78.32(19) . . . . ? O3 S1 C1 C2 -19.9(2) . . . . ? O1 S1 C1 C2 -140.54(19) . . . . ? O2 S1 C1 C2 100.02(19) . . . . ? C6 C1 C2 C3 -0.3(3) . . . . ? S1 C1 C2 C3 -178.59(17) . . . . ? C2 C1 C6 C5 0.9(4) . . . . ? S1 C1 C6 C5 179.21(18) . . . . ? C1 C6 C5 C4 -1.7(4) . . . . ? C6 C5 C4 C3 1.9(4) . . . . ? C6 C5 C4 N1 -176.6(2) . . . . ? C5 C4 C3 C2 -1.4(3) . . . . ? N1 C4 C3 C2 177.13(19) . . . . ? C1 C2 C3 C4 0.5(3) . . . . ? C3 C4 N1 C8 120.5(2) . . . . ? C5 C4 N1 C8 -60.9(3) . . . . ? C3 C4 N1 C7 -71.4(3) . . . . ? C5 C4 N1 C7 107.1(3) . . . . ? C8 N1 C7 N3 1.3(2) . . . . ? C4 N1 C7 N3 -168.83(19) . . . . ? N1 C7 N3 N2 -1.0(2) . . . . ? N1 C7 N3 Cd1 171.22(14) . . . 2_656 ? C7 N3 N2 C8 0.4(2) . . . . ? Cd1 N3 N2 C8 -172.75(15) 2_656 . . . ? C7 N3 N2 Cd1 -178.12(14) . . . 1_454 ? Cd1 N3 N2 Cd1 8.8(2) 2_656 . . 1_454 ? N3 N2 C8 N1 0.4(3) . . . . ? Cd1 N2 C8 N1 178.82(14) 1_454 . . . ? C7 N1 C8 N2 -1.0(2) . . . . ? C4 N1 C8 N2 169.02(19) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 36.27 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.542 _refine_diff_density_min -0.770 _refine_diff_density_rms 0.237 data_30 _database_code_depnum_ccdc_archive 'CCDC 916534' #TrackingRef 'C2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H6 Cd Cl N3 O3 S' _chemical_formula_weight 324.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 6.1479(3) _cell_length_b 7.9347(4) _cell_length_c 8.5948(5) _cell_angle_alpha 94.4470(10) _cell_angle_beta 102.6400(10) _cell_angle_gamma 91.3460(10) _cell_volume 407.52(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 312 _exptl_absorpt_coefficient_mu 3.237 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5637 _exptl_absorpt_correction_T_max 0.8814 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith MicroMount' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Micorfocus source E025 IuS' _diffrn_source_type 'Bruker APEX DUO' _diffrn_source_power 50 _diffrn_source_current 0.6 _diffrn_source_size '0.2 mm x 0.2 mm fine focus' _diffrn_radiation_monochromator 'Quazar MX Multilayer Optics' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'APEX DUO Kappa 4-axis goniometer' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 4273 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0133 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 30.00 _reflns_number_total 4273 _reflns_number_gt 4174 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2011.4-0' _computing_cell_refinement 'Bruker APEX2 v2011.4-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution Sir2011 _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0290P)^2^+0.1908P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4273 _refine_ls_number_parameters 122 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0167 _refine_ls_R_factor_gt 0.0163 _refine_ls_wR_factor_ref 0.0514 _refine_ls_wR_factor_gt 0.0511 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.5000 0.5000 0.5000 0.00698(4) Uani 1 2 d S . . Cd2 Cd 0.5000 1.0000 0.5000 0.00708(4) Uani 1 2 d S . . Cl1 Cl 0.77820(4) 0.75691(4) 0.53278(3) 0.00936(6) Uani 1 1 d . . . S1 S 1.60502(4) 1.22266(4) 1.18096(3) 0.00694(6) Uani 1 1 d . . . N1 N 0.76724(17) 1.18028(13) 0.66317(12) 0.00901(19) Uani 1 1 d . . . N2 N 1.07329(16) 1.28852(13) 0.82196(12) 0.00840(19) Uani 1 1 d . . . N3 N 0.76205(17) 1.35421(13) 0.66615(12) 0.00949(19) Uani 1 1 d . . . O1 O 1.63064(15) 1.07928(12) 1.27985(11) 0.01029(17) Uani 1 1 d . . . O2 O 1.76135(15) 1.22125(13) 1.07579(11) 0.01035(18) Uani 1 1 d . . . O3 O 1.61182(15) 1.38662(11) 1.27278(10) 0.01030(17) Uani 1 1 d . . . C1 C 1.3006(2) 1.30821(18) 0.92230(16) 0.0113(2) Uani 1 1 d . . . H1A H 1.3301 1.4273 0.9674 0.014 Uiso 1 1 calc R . . H1B H 1.4096 1.2812 0.8555 0.014 Uiso 1 1 calc R . . C2 C 1.33123(19) 1.19288(16) 1.05779(14) 0.0092(2) Uani 1 1 d . . . H2A H 1.3063 1.0735 1.0129 0.011 Uiso 1 1 calc R . . H2B H 1.2199 1.2177 1.1231 0.011 Uiso 1 1 calc R . . C3 C 0.9478(2) 1.41595(16) 0.76140(15) 0.0100(2) Uani 1 1 d . . . H3 H 0.9883 1.5330 0.7845 0.012 Uiso 1 1 calc R . . C4 C 0.9563(2) 1.14413(16) 0.75655(14) 0.0096(2) Uani 1 1 d . . . H4 H 1.0040 1.0331 0.7754 0.012 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 0.00739(7) 0.00603(7) 0.00700(7) 0.00091(4) 0.00027(4) 0.00086(4) Cd2 0.00745(7) 0.00589(7) 0.00723(7) 0.00074(4) 0.00017(4) -0.00038(4) Cl1 0.00863(12) 0.00785(14) 0.01149(13) 0.00131(10) 0.00181(9) 0.00034(9) S1 0.00716(12) 0.00708(14) 0.00638(12) 0.00085(10) 0.00098(9) 0.00047(9) N1 0.0095(4) 0.0071(5) 0.0098(4) 0.0012(4) 0.0007(4) 0.0004(4) N2 0.0069(4) 0.0084(5) 0.0089(4) 0.0021(4) -0.0009(3) -0.0002(4) N3 0.0099(4) 0.0070(5) 0.0107(4) 0.0011(4) 0.0004(4) 0.0007(4) O1 0.0111(4) 0.0102(4) 0.0103(4) 0.0046(3) 0.0023(3) 0.0023(3) O2 0.0092(4) 0.0125(5) 0.0099(4) 0.0015(3) 0.0033(3) 0.0002(3) O3 0.0127(4) 0.0083(4) 0.0095(4) -0.0017(3) 0.0027(3) -0.0008(3) C1 0.0077(5) 0.0145(6) 0.0104(5) 0.0042(4) -0.0020(4) -0.0017(4) C2 0.0083(5) 0.0097(6) 0.0088(5) 0.0018(4) 0.0000(4) -0.0003(4) C3 0.0092(5) 0.0090(6) 0.0111(5) 0.0010(4) 0.0003(4) 0.0003(4) C4 0.0087(5) 0.0082(6) 0.0110(5) 0.0012(4) 0.0003(4) 0.0003(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 N3 2.3043(10) 2_676 ? Cd1 N3 2.3043(10) 1_545 ? Cd1 O3 2.3324(9) 2_777 ? Cd1 O3 2.3324(9) 1_444 ? Cd1 Cl1 2.5877(3) . ? Cd1 Cl1 2.5877(3) 2_666 ? Cd2 N1 2.2983(10) 2_676 ? Cd2 N1 2.2983(10) . ? Cd2 O1 2.3339(9) 2_777 ? Cd2 O1 2.3339(9) 1_454 ? Cd2 Cl1 2.5987(3) . ? Cd2 Cl1 2.5987(3) 2_676 ? S1 O2 1.4560(9) . ? S1 O3 1.4631(9) . ? S1 O1 1.4633(9) . ? S1 C2 1.7811(12) . ? N1 C4 1.3116(15) . ? N1 N3 1.3796(15) . ? N2 C4 1.3530(16) . ? N2 C3 1.3532(16) . ? N2 C1 1.4707(15) . ? N3 C3 1.3100(16) . ? N3 Cd1 2.3043(10) 1_565 ? O1 Cd2 2.3339(9) 1_656 ? O3 Cd1 2.3324(9) 1_666 ? C1 C2 1.5187(17) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? 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 2_676 1_545 ? N3 Cd1 O3 92.02(3) 2_676 2_777 ? N3 Cd1 O3 87.98(3) 1_545 2_777 ? N3 Cd1 O3 87.98(3) 2_676 1_444 ? N3 Cd1 O3 92.02(3) 1_545 1_444 ? O3 Cd1 O3 180.0 2_777 1_444 ? N3 Cd1 Cl1 89.37(3) 2_676 . ? N3 Cd1 Cl1 90.63(3) 1_545 . ? O3 Cd1 Cl1 88.21(2) 2_777 . ? O3 Cd1 Cl1 91.79(2) 1_444 . ? N3 Cd1 Cl1 90.63(3) 2_676 2_666 ? N3 Cd1 Cl1 89.37(3) 1_545 2_666 ? O3 Cd1 Cl1 91.79(2) 2_777 2_666 ? O3 Cd1 Cl1 88.21(2) 1_444 2_666 ? Cl1 Cd1 Cl1 180.000(2) . 2_666 ? N1 Cd2 N1 180.00(6) 2_676 . ? N1 Cd2 O1 89.04(3) 2_676 2_777 ? N1 Cd2 O1 90.96(3) . 2_777 ? N1 Cd2 O1 90.96(3) 2_676 1_454 ? N1 Cd2 O1 89.04(3) . 1_454 ? O1 Cd2 O1 180.0 2_777 1_454 ? N1 Cd2 Cl1 90.15(3) 2_676 . ? N1 Cd2 Cl1 89.85(3) . . ? O1 Cd2 Cl1 90.00(2) 2_777 . ? O1 Cd2 Cl1 90.00(2) 1_454 . ? N1 Cd2 Cl1 89.85(3) 2_676 2_676 ? N1 Cd2 Cl1 90.15(3) . 2_676 ? O1 Cd2 Cl1 90.00(2) 2_777 2_676 ? O1 Cd2 Cl1 90.00(2) 1_454 2_676 ? Cl1 Cd2 Cl1 180.000(12) . 2_676 ? Cd1 Cl1 Cd2 99.804(10) . . ? O2 S1 O3 111.56(6) . . ? O2 S1 O1 112.20(5) . . ? O3 S1 O1 113.61(5) . . ? O2 S1 C2 107.53(6) . . ? O3 S1 C2 106.50(6) . . ? O1 S1 C2 104.86(6) . . ? C4 N1 N3 107.24(10) . . ? C4 N1 Cd2 128.92(9) . . ? N3 N1 Cd2 123.57(7) . . ? C4 N2 C3 105.63(10) . . ? C4 N2 C1 128.47(11) . . ? C3 N2 C1 125.52(11) . . ? C3 N3 N1 107.21(10) . . ? C3 N3 Cd1 127.27(9) . 1_565 ? N1 N3 Cd1 124.79(8) . 1_565 ? S1 O1 Cd2 136.34(5) . 1_656 ? S1 O3 Cd1 138.39(5) . 1_666 ? N2 C1 C2 111.24(10) . . ? N2 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N2 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C1 C2 S1 110.55(8) . . ? C1 C2 H2A 109.5 . . ? S1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? S1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? N3 C3 N2 110.00(11) . . ? N3 C3 H3 125.0 . . ? N2 C3 H3 125.0 . . ? N1 C4 N2 109.90(11) . . ? N1 C4 H4 125.0 . . ? N2 C4 H4 125.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cd1 Cl1 Cd2 30.15(3) 2_676 . . . ? N3 Cd1 Cl1 Cd2 -149.85(3) 1_545 . . . ? O3 Cd1 Cl1 Cd2 -61.90(2) 2_777 . . . ? O3 Cd1 Cl1 Cd2 118.10(2) 1_444 . . . ? Cl1 Cd1 Cl1 Cd2 30(100) 2_666 . . . ? N1 Cd2 Cl1 Cd1 -29.35(3) 2_676 . . . ? N1 Cd2 Cl1 Cd1 150.65(3) . . . . ? O1 Cd2 Cl1 Cd1 59.69(2) 2_777 . . . ? O1 Cd2 Cl1 Cd1 -120.31(2) 1_454 . . . ? Cl1 Cd2 Cl1 Cd1 -6(16) 2_676 . . . ? N1 Cd2 N1 C4 124(61) 2_676 . . . ? O1 Cd2 N1 C4 76.64(11) 2_777 . . . ? O1 Cd2 N1 C4 -103.36(11) 1_454 . . . ? Cl1 Cd2 N1 C4 -13.36(10) . . . . ? Cl1 Cd2 N1 C4 166.64(10) 2_676 . . . ? N1 Cd2 N1 N3 -63(61) 2_676 . . . ? O1 Cd2 N1 N3 -110.11(9) 2_777 . . . ? O1 Cd2 N1 N3 69.89(9) 1_454 . . . ? Cl1 Cd2 N1 N3 159.89(9) . . . . ? Cl1 Cd2 N1 N3 -20.11(9) 2_676 . . . ? C4 N1 N3 C3 -0.14(13) . . . . ? Cd2 N1 N3 C3 -174.65(8) . . . . ? C4 N1 N3 Cd1 170.67(8) . . . 1_565 ? Cd2 N1 N3 Cd1 -3.84(13) . . . 1_565 ? O2 S1 O1 Cd2 168.92(7) . . . 1_656 ? O3 S1 O1 Cd2 41.22(9) . . . 1_656 ? C2 S1 O1 Cd2 -74.67(9) . . . 1_656 ? O2 S1 O3 Cd1 -162.98(7) . . . 1_666 ? O1 S1 O3 Cd1 -34.95(10) . . . 1_666 ? C2 S1 O3 Cd1 79.97(9) . . . 1_666 ? C4 N2 C1 C2 -49.14(17) . . . . ? C3 N2 C1 C2 138.92(12) . . . . ? N2 C1 C2 S1 -178.45(9) . . . . ? O2 S1 C2 C1 -47.04(11) . . . . ? O3 S1 C2 C1 72.66(10) . . . . ? O1 S1 C2 C1 -166.62(9) . . . . ? N1 N3 C3 N2 -0.56(14) . . . . ? Cd1 N3 C3 N2 -171.08(8) 1_565 . . . ? C4 N2 C3 N3 1.02(14) . . . . ? C1 N2 C3 N3 174.48(11) . . . . ? N3 N1 C4 N2 0.79(13) . . . . ? Cd2 N1 C4 N2 174.91(8) . . . . ? C3 N2 C4 N1 -1.11(14) . . . . ? C1 N2 C4 N1 -174.31(11) . . . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.559 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.123