Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Maria V. Castano' _publ_contact_author_address ; Departamento de Quimica Inorganica University of Santiago de Compostela Facultade de Farmacia Santiago de Compostela Galicia 15782 SPAIN ; _publ_contact_author_email QITOYI@USC.ES _publ_section_title ; Reactions of thiosemicarbazones derived from b-keto amides and b-keto esters with Zn(II) and Cd(II) acetates: Influence of metal, substitution, reagent ratio and temperature on metal-induced cyclization ; loop_ _publ_author_name 'Maria V. Castano' 'Jose S. Casas' 'Maria S. Garcia-Tasende' ; E.Rodriguez-Castellon ; 'Agustin Sanchez' 'Luisa M. Sanjuan' 'Jose Sordo' data_HL3 _database_code_depnum_ccdc_archive 'CCDC 230381' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common HL3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H9 N3 O S' _chemical_formula_weight 171.22 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m 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' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 18.825(4) _cell_length_b 6.9385(14) _cell_length_c 6.1461(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.087(3) _cell_angle_gamma 90.00 _cell_volume 802.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 764 _cell_measurement_theta_min 3,13 _cell_measurement_theta_max 26,34 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0,95 _exptl_crystal_size_mid 0,53 _exptl_crystal_size_min 0,44 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 0.348 _exptl_absorpt_correction_type 'empirical(Sadabs, Sheldrick, 1996)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2519 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0110 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 26.37 _reflns_number_total 890 _reflns_number_gt 760 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction 'BRUKER SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1999)' _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^)+(0.1304P)^2^+0.2184P] 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 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.010(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 890 _refine_ls_number_parameters 68 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1744 _refine_ls_wR_factor_gt 0.1661 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.12575(14) 0.0000 0.9592(4) 0.0507(7) Uani 1 2 d S . . C2 C 0.30775(14) 0.0000 0.8392(4) 0.0483(7) Uani 1 2 d S . . C3 C 0.31375(15) 0.0000 1.0617(4) 0.0562(7) Uani 1 2 d S . . H3 H 0.3560 0.0000 1.1405 0.067 Uiso 1 2 calc SR . . C4 C 0.24496(15) 0.0000 1.1492(4) 0.0515(7) Uani 1 2 d S . . C5 C 0.36468(15) 0.0000 0.6701(5) 0.0679(9) Uani 1 2 d S . . H5A H 0.3591 0.1129 0.5787 0.082 Uiso 0.50 1 calc PR . . H5B H 0.3591 -0.1129 0.5787 0.082 Uiso 0.50 1 calc PR . . C6 C 0.43924(19) 0.0000 0.7671(8) 0.0919(13) Uani 1 2 d S . . H6A H 0.4736 0.0000 0.6519 0.138 Uiso 1 2 calc SR . . H6B H 0.4455 -0.1130 0.8552 0.138 Uiso 0.50 1 calc PR . . H6C H 0.4455 0.1130 0.8552 0.138 Uiso 0.50 1 calc PR . . N1 N 0.09516(14) 0.0000 1.1540(4) 0.0685(8) Uani 1 2 d S . . H1A H 0.1209 0.0000 1.2697 0.082 Uiso 1 2 calc SR . . H1B H 0.0496 0.0000 1.1643 0.082 Uiso 1 2 calc SR . . N2 N 0.19897(11) 0.0000 0.9679(3) 0.0467(6) Uani 1 2 d S . . N3 N 0.23994(11) 0.0000 0.7822(4) 0.0526(6) Uani 1 2 d S . . H3N H 0.2241 0.0000 0.6509 0.063 Uiso 1 2 calc SR . . O1 O 0.22147(13) 0.0000 1.3389(3) 0.0790(8) Uani 1 2 d S . . S1 S 0.08176(4) 0.0000 0.72521(11) 0.0748(5) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0378(13) 0.0829(17) 0.0314(13) 0.000 -0.0002(10) 0.000 C2 0.0390(13) 0.0740(15) 0.0321(13) 0.000 -0.0011(10) 0.000 C3 0.0405(14) 0.097(2) 0.0310(13) 0.000 -0.0068(10) 0.000 C4 0.0446(14) 0.0843(17) 0.0255(13) 0.000 -0.0033(10) 0.000 C5 0.0434(16) 0.119(3) 0.0416(17) 0.000 0.0058(13) 0.000 C6 0.0411(17) 0.164(4) 0.071(2) 0.000 0.0089(16) 0.000 N1 0.0411(13) 0.133(2) 0.0315(13) 0.000 0.0029(10) 0.000 N2 0.0370(11) 0.0806(14) 0.0224(10) 0.000 0.0000(8) 0.000 N3 0.0392(12) 0.0941(16) 0.0244(10) 0.000 0.0018(8) 0.000 O1 0.0563(14) 0.157(2) 0.0235(10) 0.000 0.0009(9) 0.000 S1 0.0364(6) 0.1561(10) 0.0317(5) 0.000 -0.0019(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.329(3) . ? C1 N2 1.379(3) . ? C1 S1 1.659(3) . ? C2 N3 1.323(3) . ? C2 C3 1.372(4) . ? C2 C5 1.494(3) . ? C3 C4 1.403(4) . ? C4 O1 1.248(3) . ? C4 N2 1.410(3) . ? C5 C6 1.524(5) . ? N2 N3 1.379(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 113.5(2) . . ? N1 C1 S1 124.4(2) . . ? N2 C1 S1 122.08(18) . . ? N3 C2 C3 110.0(2) . . ? N3 C2 C5 120.6(2) . . ? C3 C2 C5 129.4(3) . . ? C2 C3 C4 107.9(2) . . ? O1 C4 C3 133.4(3) . . ? O1 C4 N2 121.4(2) . . ? C3 C4 N2 105.2(2) . . ? C2 C5 C6 112.9(3) . . ? N3 N2 C1 121.9(2) . . ? N3 N2 C4 108.10(19) . . ? C1 N2 C4 130.01(19) . . ? C2 N3 N2 108.8(2) . . ? 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 N1 H1A O1 0.86 1.94 2.634(4) 136.9 . N1 H1A S1 0.86 2.90 3.520(3) 130.9 1_556 N1 H1B S1 0.86 2.57 3.413(3) 168.9 5_557 N3 H3N O1 0.86 1.92 2.746(3) 161.1 1_554 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.351 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.078 #========END data_HL5 _database_code_depnum_ccdc_archive 'CCDC 230382' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common HL5 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H9 N3 O S' _chemical_formula_weight 219.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 6.0107(3) _cell_length_b 7.8604(13) _cell_length_c 11.2049(9) _cell_angle_alpha 94.399(12) _cell_angle_beta 100.733(7) _cell_angle_gamma 95.417(11) _cell_volume 515.40(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 21.01 _cell_measurement_theta_max 42.91 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 228 _exptl_absorpt_coefficient_mu 2.599 _exptl_absorpt_correction_type 'empirical(Sadabs, Sheldrick, 1996)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MACH3 Enraf Nonius' _diffrn_measurement_method omega/2-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% ? _diffrn_reflns_number 2270 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _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 4.03 _diffrn_reflns_theta_max 72.99 _reflns_number_total 2065 _reflns_number_gt 1712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4-Express Software (Nonius, 1994)' _computing_cell_refinement 'CAD4-Express Software (Nonius, 1994)' _computing_data_reduction XCAD4 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _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^)+(0.0719P)^2^+0.1424P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2065 _refine_ls_number_parameters 152 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1242 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_restrained_S_all 1.158 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0338(3) 0.1625(3) 0.68710(18) 0.0347(4) Uani 1 1 d . . . C2 C 0.0691(3) 0.2753(3) 1.00171(18) 0.0331(4) Uani 1 1 d . . . C3 C 0.2911(3) 0.3256(3) 0.99645(19) 0.0383(5) Uani 1 1 d . . . C4 C 0.3183(3) 0.2930(3) 0.87489(19) 0.0359(4) Uani 1 1 d . . . C5 C -0.0370(4) 0.2760(3) 1.10962(19) 0.0369(5) Uani 1 1 d . . . C6 C 0.0646(5) 0.3826(3) 1.2141(2) 0.0519(6) Uani 1 1 d . . . H6 H 0.1966 0.4548 1.2145 0.062 Uiso 1 1 calc R . . C7 C -0.0302(7) 0.3812(4) 1.3172(3) 0.0694(9) Uani 1 1 d . . . H7 H 0.0377 0.4525 1.3871 0.083 Uiso 1 1 calc R . . C8 C -0.2263(6) 0.2736(4) 1.3165(3) 0.0723(9) Uani 1 1 d . . . H8 H -0.2910 0.2738 1.3857 0.087 Uiso 1 1 calc R . . C9 C -0.3259(5) 0.1666(4) 1.2143(3) 0.0625(8) Uani 1 1 d . . . H9 H -0.4571 0.0940 1.2147 0.075 Uiso 1 1 calc R . . C10 C -0.2321(4) 0.1662(3) 1.1103(2) 0.0469(5) Uani 1 1 d . . . H10 H -0.2993 0.0929 1.0412 0.056 Uiso 1 1 calc R . . N1 N 0.1982(3) 0.1804(3) 0.62339(18) 0.0453(5) Uani 1 1 d . . . N2 N 0.0996(3) 0.2277(2) 0.80862(15) 0.0333(4) Uani 1 1 d . . . N3 N -0.0490(3) 0.2104(2) 0.88960(15) 0.0348(4) Uani 1 1 d . . . O1 O 0.4896(2) 0.3087(2) 0.82649(15) 0.0476(4) Uani 1 1 d . . . S1 S -0.23137(8) 0.07497(9) 0.63074(5) 0.0494(2) Uani 1 1 d . . . H1A H 0.341(5) 0.219(4) 0.662(3) 0.061(8) Uiso 1 1 d . . . H1B H 0.182(5) 0.127(4) 0.548(3) 0.062(8) Uiso 1 1 d . . . H3 H 0.408(4) 0.367(3) 1.062(2) 0.044(7) Uiso 1 1 d . . . H3N H -0.189(6) 0.224(4) 0.861(3) 0.068(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 C1 0.0285(9) 0.0461(11) 0.0298(10) -0.0032(8) 0.0098(7) 0.0032(8) C2 0.0311(9) 0.0391(10) 0.0294(9) -0.0005(8) 0.0069(7) 0.0064(8) C3 0.0276(9) 0.0511(12) 0.0336(10) -0.0061(9) 0.0041(8) 0.0034(8) C4 0.0234(9) 0.0457(11) 0.0363(10) -0.0058(8) 0.0060(8) 0.0005(8) C5 0.0420(11) 0.0419(11) 0.0309(10) 0.0061(8) 0.0124(8) 0.0132(9) C6 0.0709(17) 0.0499(13) 0.0368(12) 0.0004(10) 0.0164(11) 0.0075(12) C7 0.112(3) 0.0662(17) 0.0370(13) 0.0016(12) 0.0297(15) 0.0170(17) C8 0.107(3) 0.080(2) 0.0498(16) 0.0249(15) 0.0480(17) 0.0340(19) C9 0.0632(16) 0.0776(19) 0.0608(17) 0.0306(15) 0.0337(14) 0.0172(14) C10 0.0433(12) 0.0584(14) 0.0436(12) 0.0126(10) 0.0157(10) 0.0088(10) N1 0.0332(9) 0.0677(13) 0.0341(10) -0.0086(9) 0.0153(8) -0.0057(9) N2 0.0220(7) 0.0478(9) 0.0295(8) -0.0051(7) 0.0094(6) -0.0007(7) N3 0.0243(8) 0.0519(10) 0.0288(8) -0.0013(7) 0.0100(6) 0.0028(7) O1 0.0248(7) 0.0693(10) 0.0464(9) -0.0128(8) 0.0132(6) -0.0044(7) S1 0.0267(3) 0.0808(5) 0.0361(3) -0.0155(3) 0.0087(2) -0.0050(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.326(3) . ? C1 N2 1.388(3) . ? C1 S1 1.663(2) . ? C2 N3 1.358(3) . ? C2 C3 1.369(3) . ? C2 C5 1.468(3) . ? C3 C4 1.409(3) . ? C4 O1 1.251(2) . ? C4 N2 1.412(2) . ? C5 C10 1.391(3) . ? C5 C6 1.390(3) . ? C6 C7 1.381(4) . ? C7 C8 1.383(5) . ? C8 C9 1.370(5) . ? C9 C10 1.386(3) . ? N2 N3 1.392(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 113.95(18) . . ? N1 C1 S1 124.93(17) . . ? N2 C1 S1 121.12(14) . . ? N3 C2 C3 110.27(17) . . ? N3 C2 C5 121.49(18) . . ? C3 C2 C5 128.14(19) . . ? C2 C3 C4 108.24(18) . . ? O1 C4 C3 131.96(19) . . ? O1 C4 N2 122.70(18) . . ? C3 C4 N2 105.31(16) . . ? C10 C5 C6 119.7(2) . . ? C10 C5 C2 120.8(2) . . ? C6 C5 C2 119.5(2) . . ? C7 C6 C5 120.0(3) . . ? C6 C7 C8 119.9(3) . . ? C9 C8 C7 120.4(2) . . ? C8 C9 C10 120.3(3) . . ? C9 C10 C5 119.7(3) . . ? C1 N2 N3 121.14(15) . . ? C1 N2 C4 129.27(16) . . ? N3 N2 C4 108.89(15) . . ? C2 N3 N2 107.09(15) . . ? 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 N3 H3N O1 0.86(3) 2.08(3) 2.924(2) 165(3) 1_455 N1 H1A O1 0.90(3) 1.94(3) 2.664(3) 136(3) . N1 H1B S1 0.89(3) 2.54(3) 3.404(2) 162(3) 2_556 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 72.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.250 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.094 #======END data_[Zn(L4)2]0.5(H2O) _database_code_depnum_ccdc_archive 'CCDC 230383' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Zn(L4)2]0.5(H2O)' _chemical_melting_point ? _chemical_formula_moiety '[Zn(C6H8N3O2S)2]0.5(H2O)' _chemical_formula_sum 'C12 H17 N6 O4.50 S2 Zn' _chemical_formula_weight 446.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, -z+3/4' '-x+1/2, y+1/2, -z+1/4' '-y, -x, -z+1/2' 'y, x, -z' 'y+1/2, -x+1/2, z+3/4' '-y+1/2, x+1/2, z+1/4' _cell_length_a 9.3579(15) _cell_length_b 9.3579(15) _cell_length_c 22.554(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1975.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1019 _cell_measurement_theta_min 3,47 _cell_measurement_theta_max 26,06 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0,31 _exptl_crystal_size_mid 0,25 _exptl_crystal_size_min 0,34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 1.486 _exptl_absorpt_correction_type empirical(Sadabs, _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11298 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 26.33 _reflns_number_total 2025 _reflns_number_gt 1687 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction 'BRUKER SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _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^)+(0.0452P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy atom' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _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 0.01(2) _refine_ls_number_reflns 2025 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.149 _refine_ls_shift/su_max 2.521 _refine_ls_shift/su_mean 0.024 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 Zn1 Zn 0.88879(4) 0.11121(4) 0.7500 0.04191(17) Uani 1 2 d S . . S1 S 1.06512(10) 0.07389(9) 0.67601(4) 0.0469(2) Uani 1 1 d . . . O1 O 1.1768(3) 0.5565(3) 0.67830(12) 0.0656(8) Uani 1 1 d . . . N2 N 1.0617(3) 0.3478(3) 0.70931(11) 0.0357(6) Uani 1 1 d . . . N3 N 0.9604(3) 0.3091(3) 0.75117(12) 0.0369(6) Uani 1 1 d . . . O2 O 0.7879(4) 0.2802(3) 0.83966(16) 0.0822(11) Uani 1 1 d . . . N1 N 1.2138(3) 0.2918(3) 0.63381(15) 0.0502(8) Uani 1 1 d . . . H1A H 1.2381 0.3804 0.6329 0.060 Uiso 1 1 calc R . . H1B H 1.2522 0.2321 0.6096 0.060 Uiso 1 1 calc R . . C2 C 0.9223(4) 0.4279(4) 0.77820(15) 0.0430(8) Uani 1 1 d . . . C5 C 0.8100(5) 0.4229(4) 0.82554(18) 0.0604(11) Uani 1 1 d . . . H5A H 0.8416 0.4752 0.8603 0.072 Uiso 1 1 calc R . . H5B H 0.7221 0.4656 0.8113 0.072 Uiso 1 1 calc R . . C3 C 0.9975(4) 0.5477(4) 0.75655(18) 0.0536(9) Uani 1 1 d . . . H3 H 0.9881 0.6414 0.7697 0.064 Uiso 1 1 calc R . . C1 C 1.1179(4) 0.2475(3) 0.67231(14) 0.0359(7) Uani 1 1 d . . . C4 C 1.0878(4) 0.5000(3) 0.71219(16) 0.0470(9) Uani 1 1 d . . . C6 C 0.6833(7) 0.2598(6) 0.8850(3) 0.110(2) Uani 1 1 d . . . H6A H 0.6726 0.1596 0.8929 0.165 Uiso 1 1 calc R . . H6B H 0.5934 0.2985 0.8721 0.165 Uiso 1 1 calc R . . H6C H 0.7134 0.3078 0.9205 0.165 Uiso 1 1 calc R . . OW O 0.4721(10) 0.5279(10) 0.7500 0.135(6) Uani 0.50 2 d SP . . H1W H 0.532(5) 0.577(5) 0.733(3) 0.000(15) Uiso 0.50 1 d P . . 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 Zn1 0.03334(19) 0.03334(19) 0.0590(3) 0.0058(2) 0.0058(2) -0.0066(2) S1 0.0413(5) 0.0300(5) 0.0693(5) -0.0063(4) 0.0181(4) -0.0019(3) O1 0.0734(19) 0.0338(14) 0.0897(18) 0.0030(14) 0.0362(17) -0.0130(14) N2 0.0332(14) 0.0263(13) 0.0475(14) 0.0008(11) 0.0092(12) -0.0031(11) N3 0.0337(14) 0.0319(14) 0.0449(13) -0.0007(14) 0.0105(14) -0.0027(11) O2 0.096(2) 0.0468(17) 0.104(2) -0.0035(17) 0.063(2) -0.0054(16) N1 0.0533(19) 0.0300(15) 0.0672(19) 0.0006(14) 0.0253(16) -0.0032(13) C2 0.045(2) 0.0313(18) 0.0526(19) -0.0042(15) 0.0069(16) 0.0035(16) C5 0.063(3) 0.047(2) 0.071(2) -0.005(2) 0.025(2) -0.003(2) C3 0.063(2) 0.0297(17) 0.068(2) -0.004(2) 0.014(2) -0.0005(17) C1 0.0262(15) 0.0331(17) 0.0485(18) 0.0029(14) 0.0060(16) 0.0033(13) C4 0.050(2) 0.0275(17) 0.064(2) 0.0018(16) 0.008(2) -0.0005(16) C6 0.132(6) 0.068(3) 0.129(4) -0.011(3) 0.092(4) -0.018(3) OW 0.125(9) 0.125(9) 0.156(15) -0.022(10) -0.022(10) 0.038(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N3 1.969(2) 5_666 ? Zn1 N3 1.969(2) . ? Zn1 S1 2.3727(10) 5_666 ? Zn1 S1 2.3727(10) . ? S1 C1 1.701(3) . ? O1 C4 1.248(4) . ? N2 C1 1.361(4) . ? N2 N3 1.386(3) . ? N2 C4 1.447(4) . ? N3 C2 1.317(4) . ? O2 C5 1.388(5) . ? O2 C6 1.429(5) . ? N1 C1 1.316(4) . ? C2 C3 1.411(5) . ? C2 C5 1.499(5) . ? C3 C4 1.384(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 N3 Zn1 N3 129.78(15) 5_666 . ? N3 Zn1 S1 84.91(8) 5_666 5_666 ? N3 Zn1 S1 126.47(9) . 5_666 ? N3 Zn1 S1 126.47(9) 5_666 . ? N3 Zn1 S1 84.91(8) . . ? S1 Zn1 S1 106.85(5) 5_666 . ? C1 S1 Zn1 95.51(11) . . ? C1 N2 N3 120.2(3) . . ? C1 N2 C4 129.8(3) . . ? N3 N2 C4 110.0(2) . . ? C2 N3 N2 106.3(2) . . ? C2 N3 Zn1 135.1(2) . . ? N2 N3 Zn1 117.97(19) . . ? C5 O2 C6 113.2(3) . . ? N3 C2 C3 112.1(3) . . ? N3 C2 C5 119.5(3) . . ? C3 C2 C5 128.4(3) . . ? O2 C5 C2 107.4(3) . . ? C4 C3 C2 107.4(3) . . ? N1 C1 N2 116.8(3) . . ? N1 C1 S1 122.1(2) . . ? N2 C1 S1 121.1(2) . . ? O1 C4 C3 135.6(3) . . ? O1 C4 N2 120.1(3) . . ? C3 C4 N2 104.3(3) . . ? 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 N1 H1A O1 0.86 2.02 2.694(4) 134.2 . N1 H1A S1 0.86 2.90 3.615(3) 141.3 4_756 N1 H1B O1 0.86 1.97 2.804(4) 163.6 4_746 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.33 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.311 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.061 data_e2cd _database_code_depnum_ccdc_archive 'CCDC 230384' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common e2cd _chemical_melting_point ? _chemical_formula_moiety '[Cd(C6H8N3OS)2(H2O)].2[[CH3)2SO]' _chemical_formula_sum 'C16 H30 Cd N6 O5 S4' _chemical_formula_weight 627.10 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/m 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' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 15.665(3) _cell_length_b 20.270(4) _cell_length_c 8.1761(17) _cell_angle_alpha 90.00 _cell_angle_beta 100.030(3) _cell_angle_gamma 90.00 _cell_volume 2556.5(9) _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 prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.65 _exptl_crystal_size_min 0.63 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 1.219 _exptl_absorpt_correction_type 'multiscan (Sadabs, Sheldrick, 1996)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5924 _diffrn_reflns_av_R_equivalents 0.0158 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.41 _reflns_number_total 2696 _reflns_number_gt 2493 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction 'BRUKER SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'Wingx publication routines (Farrugia, 1999)' _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^)+(0.0423P)^2^+3.1742P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2696 _refine_ls_number_parameters 165 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 C1D C 0.2371(3) 0.5000 0.8676(5) 0.0613(11) Uani 1 2 d S . . H5D1 H 0.2989 0.4971 0.8777 0.092 Uiso 0.50 1 calc PR . . H5D2 H 0.2184 0.4737 0.9524 0.092 Uiso 0.50 1 calc PR . . H5D3 H 0.2207 0.5451 0.8797 0.092 Uiso 0.50 1 calc PR . . C2D C 0.0995(5) 0.4713(5) 0.6440(10) 0.096(3) Uani 0.50 1 d P . . H6D1 H 0.0778 0.4270 0.6383 0.144 Uiso 0.50 1 calc PR . . H6D2 H 0.0775 0.4939 0.5422 0.144 Uiso 0.50 1 calc PR . . H6D3 H 0.0811 0.4939 0.7351 0.144 Uiso 0.50 1 calc PR . . C3D C 0.5392(2) 0.56573(15) 0.2682(5) 0.0606(8) Uani 1 1 d . . . H4D1 H 0.5100 0.6071 0.2430 0.091 Uiso 1 1 calc R . . H4D2 H 0.5876 0.5630 0.2107 0.091 Uiso 1 1 calc R . . H4D3 H 0.5596 0.5627 0.3857 0.091 Uiso 1 1 calc R . . O1D O 0.24418(19) 0.5000 0.5494(3) 0.0557(7) Uani 1 2 d S . . O1W O 0.0000 0.21189(12) 0.0000 0.0454(6) Uani 1 2 d S . . O2D O 0.40248(17) 0.5000 0.3190(4) 0.0574(7) Uani 1 2 d S . . S1D S 0.18699(9) 0.47020(7) 0.66730(17) 0.0458(3) Uani 0.50 1 d P . . S2D S 0.46619(6) 0.5000 0.20360(13) 0.0482(2) Uani 1 2 d S . . H1W H 0.0566 0.1877 -0.0152 0.050 Uiso 1 1 d . . . C1 C 0.19099(14) 0.38062(11) 0.1861(3) 0.0299(4) Uani 1 1 d . . . C2 C 0.16571(14) 0.30045(11) -0.1931(3) 0.0300(4) Uani 1 1 d . . . C3 C 0.25472(14) 0.31023(11) -0.1756(3) 0.0296(4) Uani 1 1 d . . . C4 C 0.28118(13) 0.34003(10) -0.0220(3) 0.0279(4) Uani 1 1 d . . . C5 C 0.10695(16) 0.26969(15) -0.3362(3) 0.0452(6) Uani 1 1 d . . . H5A H 0.0488 0.2688 -0.3137 0.068 Uiso 1 1 calc R . . H5B H 0.1258 0.2254 -0.3520 0.068 Uiso 1 1 calc R . . H5C H 0.1084 0.2950 -0.4349 0.068 Uiso 1 1 calc R . . C6 C 0.31114(16) 0.29415(14) -0.3003(3) 0.0399(5) Uani 1 1 d . . . H6A H 0.2768 0.2737 -0.3957 0.060 Uiso 1 1 calc R . . H6B H 0.3562 0.2644 -0.2517 0.060 Uiso 1 1 calc R . . H6C H 0.3366 0.3340 -0.3336 0.060 Uiso 1 1 calc R . . N1 N 0.25955(13) 0.40691(11) 0.2770(3) 0.0402(5) Uani 1 1 d . . . H1A H 0.3094 0.4033 0.2473 0.048 Uiso 1 1 calc R . . H1B H 0.2548 0.4278 0.3665 0.048 Uiso 1 1 calc R . . N2 N 0.20294(11) 0.34794(9) 0.0451(2) 0.0277(4) Uani 1 1 d . . . N3 N 0.13283(12) 0.32218(9) -0.0641(2) 0.0315(4) Uani 1 1 d . . . O1 O 0.35400(10) 0.35948(9) 0.0548(2) 0.0367(4) Uani 1 1 d . . . S1 S 0.09207(4) 0.38768(4) 0.24458(8) 0.04536(17) Uani 1 1 d . . . Cd1 Cd 0.0000 0.326311(12) 0.0000 0.03391(10) Uani 1 2 d S . . 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 C1D 0.081(3) 0.061(3) 0.041(2) 0.000 0.011(2) 0.000 C2D 0.073(5) 0.144(9) 0.077(5) -0.043(5) 0.035(4) -0.053(5) C3D 0.0478(16) 0.0510(16) 0.085(2) 0.0065(16) 0.0158(16) -0.0065(13) O1D 0.0518(16) 0.077(2) 0.0416(15) 0.000 0.0178(13) 0.000 O1W 0.0290(12) 0.0371(13) 0.0720(18) 0.000 0.0140(11) 0.000 O2D 0.0341(14) 0.0689(19) 0.072(2) 0.000 0.0180(13) 0.000 S1D 0.0555(8) 0.0398(6) 0.0437(7) -0.0015(5) 0.0127(6) -0.0054(6) S2D 0.0335(4) 0.0611(6) 0.0498(5) 0.000 0.0061(4) 0.000 C1 0.0292(10) 0.0312(11) 0.0309(11) -0.0020(8) 0.0097(9) -0.0022(8) C2 0.0277(10) 0.0346(11) 0.0287(10) 0.0012(9) 0.0078(8) -0.0001(9) C3 0.0279(10) 0.0320(10) 0.0303(11) 0.0012(8) 0.0095(9) 0.0012(8) C4 0.0237(10) 0.0287(10) 0.0330(11) 0.0020(8) 0.0097(8) 0.0015(8) C5 0.0344(13) 0.0656(17) 0.0356(13) -0.0118(12) 0.0059(10) -0.0042(11) C6 0.0332(12) 0.0528(14) 0.0368(12) -0.0062(11) 0.0147(10) -0.0005(11) N1 0.0310(10) 0.0528(12) 0.0378(11) -0.0152(9) 0.0090(8) -0.0093(9) N2 0.0203(8) 0.0336(9) 0.0299(9) -0.0035(7) 0.0065(7) -0.0022(7) N3 0.0222(9) 0.0415(10) 0.0315(9) -0.0072(8) 0.0066(7) -0.0034(7) O1 0.0216(7) 0.0461(9) 0.0432(9) -0.0085(8) 0.0077(7) -0.0033(7) S1 0.0299(3) 0.0626(4) 0.0472(4) -0.0216(3) 0.0167(3) -0.0044(3) Cd1 0.02014(13) 0.04228(15) 0.04063(15) 0.000 0.00897(9) 0.000 _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 C1D S1D 1.793(4) . ? C2D S1D 1.350(7) . ? C3D S2D 1.776(3) . ? O1D S1D 1.548(3) 6_565 ? O1D S1D 1.548(3) . ? O1W Cd1 2.319(3) . ? O2D S2D 1.488(3) . ? S1D S1D 1.208(3) 6_565 ? S1D C2D 1.796(7) 6_565 ? S2D C3D 1.776(3) 6_565 ? C1 N1 1.308(3) . ? C1 N2 1.370(3) . ? C1 S1 1.705(2) . ? C2 N3 1.327(3) . ? C2 C3 1.391(3) . ? C2 C5 1.493(3) . ? C3 C4 1.390(3) . ? C3 C6 1.497(3) . ? C4 O1 1.266(3) . ? C4 N2 1.436(3) . ? N2 N3 1.391(3) . ? N3 Cd1 2.2342(18) . ? S1 Cd1 2.5733(7) . ? Cd1 N3 2.2342(18) 2 ? Cd1 S1 2.5733(7) 2 ? 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 S1D O1D S1D 45.93(13) 6_565 . ? S1D S1D C2D 89.0(4) 6_565 . ? S1D S1D O1D 67.03(7) 6_565 . ? C2D S1D O1D 126.1(4) . . ? S1D S1D C1D 70.31(6) 6_565 . ? C2D S1D C1D 113.2(4) . . ? O1D S1D C1D 103.21(19) . . ? S1D S1D C2D 48.7(3) 6_565 6_565 ? C2D S1D C2D 40.3(7) . 6_565 ? O1D S1D C2D 101.0(3) . 6_565 ? C1D S1D C2D 94.5(3) . 6_565 ? O2D S2D C3D 106.27(14) . . ? O2D S2D C3D 106.27(14) . 6_565 ? C3D S2D C3D 97.2(2) . 6_565 ? N1 C1 N2 117.12(19) . . ? N1 C1 S1 120.17(17) . . ? N2 C1 S1 122.71(16) . . ? N3 C2 C3 113.1(2) . . ? N3 C2 C5 119.3(2) . . ? C3 C2 C5 127.6(2) . . ? C4 C3 C2 106.90(19) . . ? C4 C3 C6 126.3(2) . . ? C2 C3 C6 126.8(2) . . ? O1 C4 C3 133.2(2) . . ? O1 C4 N2 122.06(19) . . ? C3 C4 N2 104.70(18) . . ? C1 N2 N3 120.88(17) . . ? C1 N2 C4 128.76(18) . . ? N3 N2 C4 110.10(17) . . ? C2 N3 N2 105.23(17) . . ? C2 N3 Cd1 134.84(15) . . ? N2 N3 Cd1 119.92(13) . . ? C1 S1 Cd1 98.92(8) . . ? N3 Cd1 N3 175.71(10) 2 . ? N3 Cd1 O1W 87.85(5) 2 . ? N3 Cd1 O1W 87.85(5) . . ? N3 Cd1 S1 104.75(5) 2 . ? N3 Cd1 S1 77.38(5) . . ? O1W Cd1 S1 118.910(19) . . ? N3 Cd1 S1 77.38(5) 2 2 ? N3 Cd1 S1 104.75(5) . 2 ? O1W Cd1 S1 118.910(19) . 2 ? S1 Cd1 S1 122.18(4) . 2 ? 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 S1D O1D S1D C2D 70.6(5) 6_565 . . . ? S1D O1D S1D C1D -61.62(14) 6_565 . . . ? S1D O1D S1D C2D 35.7(3) 6_565 . . 6_565 ? N3 C2 C3 C4 0.7(3) . . . . ? C5 C2 C3 C4 -179.6(2) . . . . ? N3 C2 C3 C6 -177.3(2) . . . . ? C5 C2 C3 C6 2.4(4) . . . . ? C2 C3 C4 O1 -179.9(2) . . . . ? C6 C3 C4 O1 -1.9(4) . . . . ? C2 C3 C4 N2 -1.2(2) . . . . ? C6 C3 C4 N2 176.8(2) . . . . ? N1 C1 N2 N3 -175.9(2) . . . . ? S1 C1 N2 N3 4.2(3) . . . . ? N1 C1 N2 C4 -2.4(3) . . . . ? S1 C1 N2 C4 177.68(17) . . . . ? O1 C4 N2 C1 6.1(3) . . . . ? C3 C4 N2 C1 -172.7(2) . . . . ? O1 C4 N2 N3 -179.8(2) . . . . ? C3 C4 N2 N3 1.3(2) . . . . ? C3 C2 N3 N2 0.1(3) . . . . ? C5 C2 N3 N2 -179.6(2) . . . . ? C3 C2 N3 Cd1 178.79(16) . . . . ? C5 C2 N3 Cd1 -1.0(3) . . . . ? C1 N2 N3 C2 173.69(19) . . . . ? C4 N2 N3 C2 -0.9(2) . . . . ? C1 N2 N3 Cd1 -5.2(3) . . . . ? C4 N2 N3 Cd1 -179.80(13) . . . . ? N1 C1 S1 Cd1 178.85(19) . . . . ? N2 C1 S1 Cd1 -1.2(2) . . . . ? C2 N3 Cd1 N3 64.4(2) . . . 2 ? N2 N3 Cd1 N3 -117.06(15) . . . 2 ? C2 N3 Cd1 O1W 64.4(2) . . . . ? N2 N3 Cd1 O1W -117.06(15) . . . . ? C2 N3 Cd1 S1 -175.3(2) . . . . ? N2 N3 Cd1 S1 3.21(14) . . . . ? C2 N3 Cd1 S1 -54.9(2) . . . 2 ? N2 N3 Cd1 S1 123.57(15) . . . 2 ? C1 S1 Cd1 N3 175.22(9) . . . 2 ? C1 S1 Cd1 N3 -0.95(9) . . . . ? C1 S1 Cd1 O1W 79.41(8) . . . . ? C1 S1 Cd1 S1 -100.59(8) . . . 2 ? 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 N1 H1A O2D 0.86 2.45 2.902(3) 113.2 . N1 H1A O1 0.86 2.03 2.711(3) 135.0 . N1 H1B O1D 0.86 2.12 2.961(3) 165.9 . O1W H1W O1 1.04 1.77 2.807(2) 174 7 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.578 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.074 #=====END data_[Cd(L5)2(dmso)]dmso _database_code_depnum_ccdc_archive 'CCDC 230385' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Cd(L5)2(dmso)]dmso' _chemical_melting_point ? _chemical_formula_moiety '[Cd(C10H8N3OS)2(CH3)2SO](CH3)2SO' _chemical_formula_sum 'C24 H28 Cd N6 O4 S4' _chemical_formula_weight 705.16 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.636(3) _cell_length_b 13.317(3) _cell_length_c 20.713(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.174(5) _cell_angle_gamma 90.00 _cell_volume 2933.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 903 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 26.22 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 1.070 _exptl_absorpt_correction_type 'empirical(Sadabs, Sheldrick, 1996)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14594 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0825 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.39 _reflns_number_total 5964 _reflns_number_gt 3540 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction 'BRUKER SHELXTL' _computing_structure_solution 'SHELXS-97(Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _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^)+(0.0576P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy atom' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5964 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0920 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _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 0.12172(3) 0.81112(3) 0.181024(18) 0.03402(13) Uani 1 1 d . . . C1 C -0.1082(4) 0.9699(4) 0.2075(2) 0.0374(12) Uani 1 1 d . . . C1D C -0.1129(7) 0.8205(7) -0.0086(4) 0.112(3) Uani 1 1 d . . . H1D1 H -0.1720 0.8186 0.0258 0.168 Uiso 1 1 calc R . . H1D2 H -0.0993 0.7537 -0.0243 0.168 Uiso 1 1 calc R . . H1D3 H -0.1455 0.8618 -0.0430 0.168 Uiso 1 1 calc R . . C2 C 0.1880(4) 1.0663(4) 0.1761(2) 0.0333(12) Uani 1 1 d . . . C2D C 0.1133(8) 0.8630(9) -0.0548(4) 0.135(4) Uani 1 1 d . . . H2D1 H 0.1976 0.8876 -0.0490 0.202 Uiso 1 1 calc R . . H2D2 H 0.0698 0.9026 -0.0869 0.202 Uiso 1 1 calc R . . H2D3 H 0.1156 0.7942 -0.0686 0.202 Uiso 1 1 calc R . . C3D C 0.6460(8) 0.6178(10) -0.0572(4) 0.155(5) Uani 1 1 d . . . H3D1 H 0.7260 0.5918 -0.0428 0.232 Uiso 1 1 calc R . . H3D2 H 0.6585 0.6789 -0.0809 0.232 Uiso 1 1 calc R . . H3D3 H 0.6047 0.5694 -0.0847 0.232 Uiso 1 1 calc R . . C4 C 0.0178(5) 1.1294(4) 0.2223(2) 0.0357(12) Uani 1 1 d . . . C4D C 0.4173(9) 0.6862(8) -0.0265(4) 0.134(4) Uani 1 1 d . . . H4D1 H 0.3571 0.7032 0.0056 0.200 Uiso 1 1 calc R . . H4D2 H 0.3830 0.6351 -0.0544 0.200 Uiso 1 1 calc R . . H4D3 H 0.4365 0.7447 -0.0515 0.200 Uiso 1 1 calc R . . C5 C 0.3162(5) 1.0521(4) 0.1505(2) 0.0343(12) Uani 1 1 d . . . C6 C 0.4138(5) 1.1126(4) 0.1739(3) 0.0474(14) Uani 1 1 d . . . H6 H 0.3975 1.1629 0.2038 0.057 Uiso 1 1 calc R . . C7 C 0.5348(5) 1.0980(5) 0.1529(3) 0.0611(18) Uani 1 1 d . . . H7 H 0.5997 1.1388 0.1684 0.073 Uiso 1 1 calc R . . C8 C 0.5596(5) 1.0230(5) 0.1090(3) 0.0611(18) Uani 1 1 d . . . H8 H 0.6416 1.0124 0.0958 0.073 Uiso 1 1 calc R . . C9 C 0.4640(5) 0.9640(5) 0.0849(3) 0.0537(16) Uani 1 1 d . . . H9 H 0.4807 0.9141 0.0548 0.064 Uiso 1 1 calc R . . C10 C 0.3428(5) 0.9791(4) 0.1055(2) 0.0431(14) Uani 1 1 d . . . H10 H 0.2780 0.9394 0.0887 0.052 Uiso 1 1 calc R . . C11 C 0.4279(5) 0.7678(4) 0.1907(2) 0.0372(12) Uani 1 1 d . . . C12 C 0.2882(5) 0.9162(4) 0.3052(2) 0.0357(12) Uani 1 1 d . . . C14 C 0.4884(5) 0.8907(4) 0.2780(3) 0.0409(13) Uani 1 1 d . . . C15 C 0.1746(5) 0.9518(4) 0.3372(2) 0.0390(13) Uani 1 1 d . . . C16 C 0.0679(5) 0.8936(5) 0.3405(3) 0.0504(15) Uani 1 1 d . . . H16 H 0.0671 0.8297 0.3223 0.060 Uiso 1 1 calc R . . C17 C -0.0386(6) 0.9294(6) 0.3707(3) 0.072(2) Uani 1 1 d . . . H17 H -0.1109 0.8902 0.3717 0.087 Uiso 1 1 calc R . . C18 C -0.0374(7) 1.0229(6) 0.3993(3) 0.080(2) Uani 1 1 d . . . H18 H -0.1080 1.0458 0.4206 0.096 Uiso 1 1 calc R . . C19 C 0.0672(8) 1.0819(6) 0.3962(3) 0.078(2) Uani 1 1 d . . . H19 H 0.0669 1.1455 0.4148 0.093 Uiso 1 1 calc R . . C110 C 0.1735(6) 1.0478(5) 0.3658(3) 0.0599(17) Uani 1 1 d . . . H110 H 0.2445 1.0884 0.3643 0.072 Uiso 1 1 calc R . . N1 N -0.2026(4) 1.0124(3) 0.2368(2) 0.0468(12) Uani 1 1 d . . . H1A H -0.1959 1.0731 0.2506 0.056 Uiso 1 1 calc R . . H1B H -0.2713 0.9796 0.2421 0.056 Uiso 1 1 calc R . . N2 N -0.0019(3) 1.0289(3) 0.20125(19) 0.0330(10) Uani 1 1 d . . . N3 N 0.1060(3) 0.9898(3) 0.17238(18) 0.0331(10) Uani 1 1 d . . . N11 N 0.5478(4) 0.7581(4) 0.1759(2) 0.0492(12) Uani 1 1 d . . . H11A H 0.6047 0.7896 0.1980 0.059 Uiso 1 1 calc R . . H11B H 0.5688 0.7202 0.1443 0.059 Uiso 1 1 calc R . . N12 N 0.4022(3) 0.8291(3) 0.24154(19) 0.0340(10) Uani 1 1 d . . . N13 N 0.2788(4) 0.8462(3) 0.25960(19) 0.0337(10) Uani 1 1 d . . . O1 O -0.0702(3) 1.1773(3) 0.2486(2) 0.0526(11) Uani 1 1 d . . . O1D O 0.0935(4) 0.7932(3) 0.06152(18) 0.0579(11) Uani 1 1 d . . . O2D O 0.6093(6) 0.7009(6) 0.0530(3) 0.142(3) Uani 1 1 d . . . O11 O 0.6062(3) 0.8831(3) 0.27124(19) 0.0555(11) Uani 1 1 d . . . S1 S -0.11673(13) 0.85102(11) 0.17959(7) 0.0447(4) Uani 1 1 d . . . S1D S 0.03204(19) 0.87140(15) 0.02076(9) 0.0752(6) Uani 1 1 d . . . S2D S 0.5516(2) 0.6425(3) 0.01051(14) 0.1449(13) Uani 1 1 d . . . S11 S 0.31435(13) 0.70507(11) 0.14814(7) 0.0481(4) Uani 1 1 d . . . C3 C 0.1392(5) 1.1518(4) 0.2049(3) 0.0399(13) Uani 1 1 d . . . H3 H 0.1806 1.2126 0.2113 0.048 Uiso 1 1 calc R . . C13 C 0.4121(5) 0.9466(4) 0.3171(2) 0.0444(14) Uani 1 1 d . . . H13 H 0.4384 0.9958 0.3463 0.053 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 0.0254(2) 0.0329(2) 0.0439(2) -0.0012(2) 0.00273(15) -0.00019(18) C1 0.025(3) 0.036(3) 0.051(3) 0.004(3) 0.001(2) 0.000(2) C1D 0.081(6) 0.150(9) 0.103(6) 0.027(6) -0.049(5) -0.035(6) C2 0.027(3) 0.036(3) 0.036(3) 0.007(2) 0.001(2) -0.001(2) C2D 0.115(8) 0.213(11) 0.077(5) 0.062(7) 0.012(5) -0.024(8) C3D 0.079(6) 0.287(14) 0.099(6) -0.098(8) 0.033(5) -0.031(8) C4 0.029(3) 0.030(3) 0.047(3) -0.002(3) 0.003(2) -0.001(2) C4D 0.114(8) 0.206(12) 0.081(6) -0.018(7) -0.003(6) 0.059(8) C5 0.030(3) 0.036(3) 0.038(3) 0.006(2) 0.004(2) 0.002(2) C6 0.035(3) 0.046(4) 0.061(4) -0.006(3) 0.000(3) -0.001(3) C7 0.031(3) 0.072(5) 0.080(4) 0.000(4) 0.003(3) -0.016(3) C8 0.033(3) 0.070(5) 0.081(5) 0.008(4) 0.021(3) 0.002(3) C9 0.051(4) 0.052(4) 0.059(4) 0.001(3) 0.025(3) 0.007(3) C10 0.038(3) 0.046(3) 0.045(3) -0.001(3) 0.010(3) -0.001(3) C11 0.030(3) 0.038(3) 0.043(3) 0.010(3) 0.003(2) 0.003(2) C12 0.032(3) 0.041(3) 0.034(3) 0.007(3) 0.004(2) -0.001(3) C14 0.035(3) 0.042(3) 0.046(3) 0.012(3) -0.002(3) -0.005(3) C15 0.044(3) 0.035(3) 0.038(3) 0.002(3) 0.002(3) 0.006(3) C16 0.051(4) 0.049(4) 0.052(3) -0.002(3) 0.016(3) 0.002(3) C17 0.058(4) 0.088(6) 0.071(4) 0.002(4) 0.028(4) 0.009(4) C18 0.078(5) 0.089(6) 0.073(5) -0.005(5) 0.026(4) 0.041(5) C19 0.094(6) 0.061(5) 0.078(5) -0.028(4) 0.011(5) 0.024(5) C110 0.065(4) 0.053(4) 0.061(4) -0.009(3) 0.001(3) 0.006(4) N1 0.025(2) 0.040(3) 0.076(3) -0.006(3) 0.010(2) -0.003(2) N2 0.022(2) 0.034(2) 0.044(2) 0.000(2) 0.0024(18) 0.0032(19) N3 0.026(2) 0.031(2) 0.042(2) 0.000(2) 0.0035(19) -0.0013(19) N11 0.028(2) 0.067(3) 0.053(3) -0.002(3) 0.008(2) 0.008(2) N12 0.020(2) 0.043(3) 0.039(2) 0.001(2) 0.0025(18) -0.0009(19) N13 0.025(2) 0.039(3) 0.038(2) -0.002(2) 0.0055(19) 0.0008(19) O1 0.034(2) 0.038(2) 0.086(3) -0.013(2) 0.016(2) 0.0006(18) O1D 0.059(3) 0.065(3) 0.049(2) 0.009(2) -0.008(2) 0.007(2) O2D 0.091(4) 0.265(9) 0.069(3) -0.064(5) -0.002(3) 0.042(5) O11 0.027(2) 0.070(3) 0.070(3) 0.006(2) 0.0014(19) -0.013(2) S1 0.0289(7) 0.0370(8) 0.0682(10) -0.0045(7) 0.0029(7) -0.0045(6) S1D 0.0841(14) 0.0745(13) 0.0663(11) 0.0181(10) -0.0172(10) -0.0126(11) S2D 0.0678(16) 0.249(4) 0.118(2) -0.091(2) 0.0014(15) 0.006(2) S11 0.0358(8) 0.0547(10) 0.0541(8) -0.0144(7) 0.0067(7) 0.0038(7) C3 0.034(3) 0.030(3) 0.055(3) -0.003(3) 0.007(3) -0.006(2) C13 0.044(3) 0.048(4) 0.041(3) -0.005(3) -0.006(3) -0.005(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 N13 2.355(4) . ? Cd1 O1 2.374(4) 2_545 ? Cd1 N3 2.392(4) . ? Cd1 O1D 2.499(4) . ? Cd1 S1 2.5908(15) . ? Cd1 S11 2.5910(15) . ? C1 N1 1.312(6) . ? C1 N2 1.385(6) . ? C1 S1 1.687(5) . ? C1D S1D 1.779(7) . ? C2 N3 1.342(6) . ? C2 C3 1.390(7) . ? C2 C5 1.485(6) . ? C2D S1D 1.807(8) . ? C3D S2D 1.773(7) . ? C4 O1 1.266(6) . ? C4 C3 1.381(7) . ? C4 N2 1.421(6) . ? C4D S2D 1.709(9) . ? C5 C10 1.382(7) . ? C5 C6 1.393(7) . ? C6 C7 1.381(7) . ? C7 C8 1.380(8) . ? C8 C9 1.372(8) . ? C9 C10 1.381(7) . ? C11 N11 1.324(6) . ? C11 N12 1.365(6) . ? C11 S11 1.700(5) . ? C12 N13 1.329(6) . ? C12 C13 1.395(7) . ? C12 C15 1.469(7) . ? C14 O11 1.267(6) . ? C14 C13 1.378(7) . ? C14 N12 1.434(6) . ? C15 C16 1.377(7) . ? C15 C110 1.411(7) . ? C16 C17 1.390(8) . ? C17 C18 1.378(10) . ? C18 C19 1.364(10) . ? C19 C110 1.382(9) . ? N2 N3 1.405(5) . ? N12 N13 1.390(5) . ? O1 Cd1 2.374(4) 2 ? O1D S1D 1.484(4) . ? O2D S2D 1.317(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N13 Cd1 O1 83.92(14) . 2_545 ? N13 Cd1 N3 84.37(14) . . ? O1 Cd1 N3 140.94(13) 2_545 . ? N13 Cd1 O1D 140.60(13) . . ? O1 Cd1 O1D 120.77(14) 2_545 . ? N3 Cd1 O1D 90.82(13) . . ? N13 Cd1 S1 130.37(10) . . ? O1 Cd1 S1 85.57(9) 2_545 . ? N3 Cd1 S1 74.24(10) . . ? O1D Cd1 S1 84.87(10) . . ? N13 Cd1 S11 74.70(10) . . ? O1 Cd1 S11 86.89(9) 2_545 . ? N3 Cd1 S11 125.24(10) . . ? O1D Cd1 S11 76.53(10) . . ? S1 Cd1 S11 152.61(5) . . ? N1 C1 N2 115.6(5) . . ? N1 C1 S1 121.8(4) . . ? N2 C1 S1 122.6(4) . . ? N3 C2 C3 113.5(4) . . ? N3 C2 C5 118.9(5) . . ? C3 C2 C5 127.7(5) . . ? O1 C4 C3 135.1(5) . . ? O1 C4 N2 120.1(4) . . ? C3 C4 N2 104.8(4) . . ? C10 C5 C6 118.7(5) . . ? C10 C5 C2 122.2(5) . . ? C6 C5 C2 119.0(5) . . ? C7 C6 C5 120.1(6) . . ? C8 C7 C6 120.1(6) . . ? C9 C8 C7 120.3(5) . . ? C8 C9 C10 119.6(6) . . ? C9 C10 C5 121.1(5) . . ? N11 C11 N12 116.5(5) . . ? N11 C11 S11 120.6(4) . . ? N12 C11 S11 122.8(4) . . ? N13 C12 C13 112.8(5) . . ? N13 C12 C15 119.8(4) . . ? C13 C12 C15 127.5(5) . . ? O11 C14 C13 134.8(5) . . ? O11 C14 N12 121.3(5) . . ? C13 C14 N12 103.9(4) . . ? C16 C15 C110 118.4(5) . . ? C16 C15 C12 121.8(5) . . ? C110 C15 C12 119.8(5) . . ? C15 C16 C17 120.6(6) . . ? C18 C17 C16 120.2(7) . . ? C19 C18 C17 120.1(6) . . ? C18 C19 C110 120.5(7) . . ? C19 C110 C15 120.2(6) . . ? C1 N2 N3 120.3(4) . . ? C1 N2 C4 128.4(4) . . ? N3 N2 C4 111.3(4) . . ? C2 N3 N2 103.3(4) . . ? C2 N3 Cd1 135.0(3) . . ? N2 N3 Cd1 113.1(3) . . ? C11 N12 N13 120.7(4) . . ? C11 N12 C14 127.7(4) . . ? N13 N12 C14 111.2(4) . . ? C12 N13 N12 104.4(4) . . ? C12 N13 Cd1 132.2(3) . . ? N12 N13 Cd1 116.2(3) . . ? C4 O1 Cd1 145.6(3) . 2 ? S1D O1D Cd1 122.6(2) . . ? C1 S1 Cd1 98.21(18) . . ? O1D S1D C1D 107.2(3) . . ? O1D S1D C2D 103.7(4) . . ? C1D S1D C2D 96.2(4) . . ? O2D S2D C4D 118.2(5) . . ? O2D S2D C3D 112.0(4) . . ? C4D S2D C3D 100.9(5) . . ? C11 S11 Cd1 98.81(19) . . ? C4 C3 C2 107.1(5) . . ? C14 C13 C12 107.7(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 N1 H1A O1 0.86 1.93 2.617(6) 136.3 . N1 H1B O11 0.86 1.94 2.770(5) 163.0 1_455 N11 H11A O11 0.86 1.96 2.646(6) 135.6 . N11 H11B O2D 0.86 1.96 2.749(7) 151.2 . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.522 _refine_diff_density_min -1.313 _refine_diff_density_rms 0.104 #====END