Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_Mhmel20fe01 #=================================================================== _journal_coden_Cambridge 186 _audit_creation_date 'August, 2001' _audit_creation_method 'manual method and SHELXL-97' #=================================================================== # SUBMISSION DETAILS _publ_contact_author ; Prof Renzo Cini Department of Chemical and Biosystem Sciences and Technologies University of Siena Via E.Bastianini 12 I-53100 Siena Italy ; _publ_contact_author_email cini@unisi.it _publ_contact_author_fax '39(0577)232004' _publ_contact_author_phone '39(0577)232041' #=============================================================== # PROCESSING SUMMARY (IUCr Office Use Only) #=============================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Synthesis, X-ray Structure and Molecular Modelling Analysis of Cobalt(II), Nickel(II), Zinc(II) and Cadmium(II) Complexes of the Widely Used Anti-inflammatory Drug Meloxicam ; loop_ _publ_author_name _publ_author_address 'Sandra, Defazio' ; Department of Chemical and Biosystem Sciences and Technologies University of Siena Via E.Bastianini 12 I-53100 Siena Italy ; 'Renzo, Cini' ; Department of Chemical and Biosystem Sciences and Technologies University of Siena Via E.Bastianini 12 I-53100 Siena Italy ; ############### # DATA ############### data_vco2 _database_code_CSD 169593 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-bis(O15,N1'-(4-Hydroxy-2-methyl-1,3-thiazol-2-yl)-2H- 1,2-benzothiazine-3-carbox-amide 1,1-Dioxide)trans- bis(O-dimethylsolfoxide)cobalt(II) ; _chemical_name_common ? _chemical_formula_moiety 'C32 H36 Co N6 O10 S6' _chemical_formula_sum 'C32 H36 Co N6 O10 S6' _chemical_formula_weight 915.96 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclin _symmetry_space_group_name_H-M P-1 #nø2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.844(1) _cell_length_b 9.153(3) _cell_length_c 13.914(1) _cell_angle_alpha 79.12(1) _cell_angle_beta 85.74(1) _cell_angle_gamma 81.87(1) _cell_volume 970.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 36 _cell_measurement_theta_min 12 _cell_measurement_theta_max 29.567 _exptl_crystal_description parallelepiped _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 473 _exptl_absorpt_coefficient_mu 0.828 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 Siemens P4 _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4223 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0621 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3413 _reflns_number_gt 2412 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Xscans,Siemens' _computing_cell_refinement 'Xscans,Siemens' _computing_data_reduction 'Xscans,Siemens' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Johson&Burnett; L.J.Farrugia, Glasgow, 1998)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.4360P] 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 3413 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1050 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.0000 0.0000 0.0000 0.0280(2) Uani 1 d S . . S1D S 0.32241(15) 0.16751(13) -0.10705(9) 0.0439(3) Uani 1 d . . . O15 O 0.0837(4) -0.1704(3) 0.11477(18) 0.0317(6) Uani 1 d . . . N1' N 0.0708(5) -0.1552(4) -0.0929(2) 0.0326(8) Uani 1 d . . . N16 N 0.1395(5) -0.3693(4) 0.0327(2) 0.0387(9) Uani 1 d . . . H16 H 0.1536 -0.4657 0.0414 0.046 Uiso 1 calc R . . O1D O 0.2554(4) 0.0581(3) -0.0211(2) 0.0420(7) Uani 1 d . . . C14 C 0.1270(5) -0.3071(4) 0.1154(3) 0.0290(9) Uani 1 d . . . C3 C 0.1715(5) -0.4123(4) 0.2035(3) 0.0309(9) Uani 1 d . . . S3' S 0.21569(17) -0.38969(13) -0.15564(8) 0.0448(3) Uani 1 d . . . S1 S 0.31310(17) -0.41158(13) 0.36437(8) 0.0444(3) Uani 1 d . . . O1 O 0.4728(4) -0.3835(4) 0.3118(2) 0.0573(9) Uani 1 d . . . O17 O 0.2416(4) -0.6275(3) 0.1314(2) 0.0475(8) Uani 1 d . . . N2 N 0.1560(5) -0.3479(4) 0.2908(2) 0.0367(9) Uani 1 d . . . C5' C 0.0883(6) -0.1190(5) -0.1940(3) 0.0360(10) Uani 1 d . . . H5' H 0.0515 -0.0233 -0.2277 0.043 Uiso 1 calc R . . O2 O 0.2716(5) -0.3567(4) 0.4535(2) 0.0673(11) Uani 1 d . . . C2' C 0.1319(5) -0.2950(4) -0.0624(3) 0.0319(9) Uani 1 d . . . C4' C 0.1611(6) -0.2289(5) -0.2407(3) 0.0385(10) Uani 1 d . . . C4 C 0.2260(6) -0.5646(5) 0.2056(3) 0.0355(10) Uani 1 d . . . C10 C 0.2682(5) -0.6620(5) 0.3030(3) 0.0360(10) Uani 1 d . . . C8 C 0.3347(6) -0.6962(5) 0.4744(3) 0.0450(12) Uani 1 d . . . H8 H 0.3569 -0.6556 0.5280 0.054 Uiso 1 calc R . . C13 C -0.0182(7) -0.3288(6) 0.3376(4) 0.0590(14) Uani 1 d . . . H13A H -0.0136 -0.2906 0.3969 0.071 Uiso 1 calc R . . H13B H -0.0616 -0.4239 0.3526 0.071 Uiso 1 calc R . . H13C H -0.0931 -0.2594 0.2938 0.071 Uiso 1 calc R . . C1D C 0.4683(6) 0.2583(5) -0.0555(4) 0.0491(12) Uani 1 d . . . H1D1 H 0.4058 0.3207 -0.0129 0.059 Uiso 1 calc R . . H1D2 H 0.5289 0.3191 -0.1069 0.059 Uiso 1 calc R . . H1D3 H 0.5494 0.1844 -0.0186 0.059 Uiso 1 calc R . . C9 C 0.3050(6) -0.6049(5) 0.3835(3) 0.0386(10) Uani 1 d . . . C5 C 0.2689(6) -0.8166(5) 0.3147(3) 0.0472(12) Uani 1 d . . . H5 H 0.2489 -0.8587 0.2614 0.057 Uiso 1 calc R . . C6' C 0.1956(7) -0.2266(6) -0.3485(3) 0.0581(14) Uani 1 d . . . H6'1 H 0.2482 -0.3240 -0.3589 0.070 Uiso 1 calc R . . H6'2 H 0.2717 -0.1537 -0.3744 0.070 Uiso 1 calc R . . H6'3 H 0.0889 -0.2006 -0.3811 0.070 Uiso 1 calc R . . C6 C 0.2986(7) -0.9077(6) 0.4038(4) 0.0577(14) Uani 1 d . . . H6 H 0.2973 -1.0106 0.4107 0.069 Uiso 1 calc R . . C2D C 0.4770(7) 0.0553(6) -0.1728(4) 0.0652(16) Uani 1 d . . . H2D1 H 0.4180 0.0006 -0.2094 0.078 Uiso 1 calc R . . H2D2 H 0.5492 -0.0138 -0.1274 0.078 Uiso 1 calc R . . H2D3 H 0.5467 0.1191 -0.2170 0.078 Uiso 1 calc R . . C7 C 0.3304(7) -0.8471(6) 0.4830(4) 0.0573(14) Uani 1 d . . . H7 H 0.3493 -0.9096 0.5432 0.069 Uiso 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 Co 0.0283(5) 0.0271(4) 0.0284(4) -0.0058(3) -0.0008(3) -0.0021(3) S1D 0.0345(7) 0.0426(6) 0.0514(7) 0.0017(5) -0.0027(5) -0.0075(5) O15 0.0358(17) 0.0305(15) 0.0283(15) -0.0066(12) -0.0027(13) -0.0002(13) N1' 0.040(2) 0.0296(18) 0.0281(18) -0.0041(14) -0.0009(16) -0.0056(16) N16 0.055(3) 0.0309(19) 0.0296(19) -0.0062(15) -0.0061(17) -0.0012(18) O1D 0.0299(17) 0.0440(17) 0.0493(18) 0.0028(14) 0.0021(14) -0.0119(14) C14 0.023(2) 0.033(2) 0.032(2) -0.0084(17) -0.0002(17) -0.0028(18) C3 0.034(2) 0.032(2) 0.026(2) -0.0048(17) 0.0002(18) -0.0033(19) S3' 0.0598(8) 0.0401(6) 0.0331(6) -0.0125(5) -0.0011(6) 0.0057(6) S1 0.0566(8) 0.0483(7) 0.0301(6) -0.0064(5) -0.0076(5) -0.0109(6) O1 0.053(2) 0.071(2) 0.051(2) 0.0019(17) -0.0092(17) -0.0289(19) O17 0.068(2) 0.0345(16) 0.0378(17) -0.0108(13) -0.0041(16) 0.0061(16) N2 0.048(2) 0.0334(19) 0.0274(18) -0.0066(14) 0.0001(17) -0.0009(17) C5' 0.043(3) 0.035(2) 0.029(2) -0.0046(18) -0.004(2) -0.003(2) O2 0.102(3) 0.067(2) 0.0370(19) -0.0186(17) -0.013(2) -0.005(2) C2' 0.033(2) 0.035(2) 0.029(2) -0.0113(18) -0.0024(18) -0.0032(19) C4' 0.043(3) 0.046(3) 0.028(2) -0.0090(19) -0.001(2) -0.007(2) C4 0.039(3) 0.035(2) 0.031(2) -0.0064(18) -0.001(2) 0.000(2) C10 0.030(2) 0.034(2) 0.039(2) -0.0013(19) 0.001(2) 0.0040(19) C8 0.039(3) 0.059(3) 0.031(2) 0.002(2) -0.003(2) 0.002(2) C13 0.060(4) 0.067(3) 0.044(3) -0.009(2) 0.010(3) 0.006(3) C1D 0.039(3) 0.044(3) 0.062(3) -0.005(2) 0.009(2) -0.010(2) C9 0.031(2) 0.043(3) 0.038(2) -0.002(2) -0.001(2) 0.003(2) C5 0.048(3) 0.042(3) 0.049(3) -0.007(2) -0.004(2) 0.003(2) C6' 0.074(4) 0.066(3) 0.033(3) -0.012(2) 0.008(3) -0.010(3) C6 0.056(3) 0.042(3) 0.066(3) 0.012(3) -0.006(3) -0.002(3) C2D 0.074(4) 0.070(4) 0.055(3) -0.020(3) 0.016(3) -0.024(3) C7 0.055(3) 0.054(3) 0.049(3) 0.016(2) -0.004(3) 0.009(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 Co O15 2.083(3) . yes Co O15 2.083(3) 2 ? Co N1' 2.088(3) 2 ? Co N1' 2.088(3) . yes Co O1D 2.130(3) . yes Co O1D 2.130(3) 2 ? S1D O1D 1.521(3) . yes S1D C1D 1.770(5) . ? S1D C2D 1.789(5) . ? O15 C14 1.248(4) . yes N1' C2' 1.303(5) . yes N1' C5' 1.384(5) . ? N16 C14 1.368(5) . yes N16 C2' 1.371(5) . yes C14 C3 1.440(5) . yes C3 C4 1.394(6) . yes C3 N2 1.438(5) . yes S3' C4' 1.729(4) . ? S3' C2' 1.733(4) . yes S1 O2 1.423(3) . yes S1 O1 1.433(3) . yes S1 N2 1.633(4) . yes S1 C9 1.749(5) . ? O17 C4 1.263(5) . yes N2 C13 1.471(6) . yes C5' C4' 1.337(6) . ? C4' C6' 1.502(6) . ? C4 C10 1.506(6) . ? C10 C9 1.387(6) . ? C10 C5 1.392(6) . ? C8 C7 1.369(7) . ? C8 C9 1.394(6) . ? C5 C6 1.373(6) . ? C6 C7 1.376(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O15 Co O15 180.0 . 2 ? O15 Co N1' 92.86(11) . 2 ? O15 Co N1' 87.14(11) 2 2 ? O15 Co N1' 87.14(11) . . yes O15 Co N1' 92.86(11) 2 . ? N1' Co N1' 180.0 2 . ? O15 Co O1D 88.76(11) . . yes O15 Co O1D 91.24(11) 2 . ? N1' Co O1D 91.56(13) 2 . ? N1' Co O1D 88.44(13) . . yes O15 Co O1D 91.24(11) . 2 ? O15 Co O1D 88.76(11) 2 2 ? N1' Co O1D 88.44(13) 2 2 ? N1' Co O1D 91.56(13) . 2 ? O1D Co O1D 180.0 . 2 ? O1D S1D C1D 104.5(2) . . ? O1D S1D C2D 105.2(2) . . ? C1D S1D C2D 98.0(2) . . ? C14 O15 Co 129.6(2) . . yes C2' N1' C5' 110.6(3) . . yes C2' N1' Co 123.7(3) . . yes C5' N1' Co 124.7(3) . . ? C14 N16 C2' 127.2(3) . . yes S1D O1D Co 125.79(18) . . yes O15 C14 N16 123.2(4) . . yes O15 C14 C3 122.5(3) . . yes N16 C14 C3 114.3(3) . . yes C4 C3 N2 121.8(3) . . yes C4 C3 C14 123.6(4) . . yes N2 C3 C14 114.6(3) . . yes C4' S3' C2' 89.7(2) . . yes O2 S1 O1 118.9(2) . . yes O2 S1 N2 108.6(2) . . yes O1 S1 N2 108.59(19) . . yes O2 S1 C9 110.3(2) . . ? O1 S1 C9 107.6(2) . . ? N2 S1 C9 101.5(2) . . yes C3 N2 C13 116.0(4) . . yes C3 N2 S1 113.8(3) . . yes C13 N2 S1 116.1(3) . . yes C4' C5' N1' 116.5(4) . . ? N1' C2' N16 127.1(4) . . yes N1' C2' S3' 113.9(3) . . yes N16 C2' S3' 119.0(3) . . yes C5' C4' C6' 129.5(4) . . ? C5' C4' S3' 109.2(3) . . yes C6' C4' S3' 121.3(3) . . yes O17 C4 C3 124.6(4) . . yes O17 C4 C10 117.3(4) . . ? C3 C4 C10 118.1(4) . . ? C9 C10 C5 117.5(4) . . ? C9 C10 C4 123.0(4) . . yes C5 C10 C4 119.5(4) . . ? C7 C8 C9 118.3(5) . . ? C10 C9 C8 122.1(4) . . ? C10 C9 S1 116.2(3) . . ? C8 C9 S1 121.8(4) . . ? C6 C5 C10 121.0(5) . . ? C5 C6 C7 120.1(5) . . ? C8 C7 C6 121.0(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.462 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.069 #===END data_v32bdcen _database_code_CSD 169594 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-bis(N1',O15-(4-Hydroxy-2-N-(5-methyl-1,3-thiazol-2-yl)- 2H-1,2-benzothiazine-3-carbox-amide 1,1-Dioxide)-trans- bis(O-dimethylsulfoxide)zinc(II) ; _chemical_name_common ? _chemical_formula_moiety 'C32 H36 N6 O10 S6 Zn' _chemical_formula_sum 'C32 H36 N6 O10 S6 Zn' _chemical_formula_weight 922.40 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 Triclinic _symmetry_space_group_name_H-M P-1 #nø 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.878(4) _cell_length_b 9.127(6) _cell_length_c 13.873(7) _cell_angle_alpha 79.26(4) _cell_angle_beta 85.90(3) _cell_angle_gamma 81.67(4) _cell_volume 968.7(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 6.0 _cell_measurement_theta_max 19.5 _exptl_crystal_description parallelepiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 1.020 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 Siemens P4 _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3650 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0797 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3393 _reflns_number_gt 2246 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS, Siemens' _computing_cell_refinement 'XSCANS, Siemens' _computing_data_reduction 'XSCANS, Siemens' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Johnson&Burnett; L.J.Farrugia, Glasgow, 1998)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0917P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3393 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1040 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1600 _refine_ls_wR_factor_gt 0.1361 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.0000 0.0000 0.0000 0.0291(3) Uani 1 d S . . S1D S 0.32506(19) 0.16871(17) -0.10722(12) 0.0431(4) Uani 1 d . . . O15 O 0.0839(4) -0.1699(4) 0.1153(3) 0.0318(8) Uani 1 d . . . N1' N 0.0704(6) -0.1538(5) -0.0919(3) 0.0305(10) Uani 1 d . . . N16 N 0.1376(6) -0.3697(5) 0.0335(3) 0.0349(11) Uani 1 d . . . H16 H 0.1496 -0.4664 0.0422 0.042 Uiso 1 calc R . . O1D O 0.2590(5) 0.0594(4) -0.0220(3) 0.0424(10) Uani 1 d . . . C14 C 0.1265(6) -0.3056(6) 0.1160(4) 0.0284(11) Uani 1 d . . . C3 C 0.1708(7) -0.4122(6) 0.2041(4) 0.0314(12) Uani 1 d . . . S3' S 0.2150(2) -0.39007(17) -0.15514(11) 0.0432(4) Uani 1 d . . . S1 S 0.3124(2) -0.41297(18) 0.36553(11) 0.0436(4) Uani 1 d . . . O1 O 0.4705(6) -0.3851(6) 0.3125(3) 0.0584(13) Uani 1 d . . . O17 O 0.2386(6) -0.6282(4) 0.1319(3) 0.0452(10) Uani 1 d . . . N2 N 0.1561(6) -0.3485(5) 0.2919(3) 0.0372(11) Uani 1 d . . . C5' C 0.0899(7) -0.1189(7) -0.1934(4) 0.0384(13) Uani 1 d . . . H5' H 0.0544 -0.0227 -0.2273 0.046 Uiso 1 calc R . . O2 O 0.2733(7) -0.3576(5) 0.4545(3) 0.0652(14) Uani 1 d . . . C2' C 0.1312(7) -0.2937(6) -0.0622(4) 0.0333(12) Uani 1 d . . . C4' C 0.1617(8) -0.2289(7) -0.2406(4) 0.0388(14) Uani 1 d . . . C4 C 0.2245(7) -0.5652(6) 0.2066(4) 0.0344(12) Uani 1 d . . . C10 C 0.2669(7) -0.6637(6) 0.3035(4) 0.0361(13) Uani 1 d . . . C8 C 0.3348(7) -0.6968(7) 0.4748(4) 0.0446(15) Uani 1 d . . . H8 H 0.3574 -0.6562 0.5285 0.053 Uiso 1 calc R . . C13 C -0.0179(8) -0.3282(8) 0.3387(5) 0.0549(18) Uani 1 d . . . H13A H -0.0131 -0.2899 0.3982 0.066 Uiso 1 calc R . . H13B H -0.0614 -0.4232 0.3536 0.066 Uiso 1 calc R . . H13C H -0.0923 -0.2583 0.2947 0.066 Uiso 1 calc R . . C1D C 0.4711(7) 0.2588(7) -0.0547(5) 0.0456(15) Uani 1 d . . . H1D1 H 0.4090 0.3214 -0.0120 0.055 Uiso 1 calc R . . H1D2 H 0.5316 0.3195 -0.1060 0.055 Uiso 1 calc R . . H1D3 H 0.5517 0.1841 -0.0178 0.055 Uiso 1 calc R . . C9 C 0.3049(7) -0.6058(7) 0.3842(4) 0.0370(13) Uani 1 d . . . C5 C 0.2667(8) -0.8178(7) 0.3154(5) 0.0455(15) Uani 1 d . . . H5 H 0.2450 -0.8601 0.2622 0.055 Uiso 1 calc R . . C6' C 0.1993(10) -0.2263(9) -0.3481(4) 0.0582(19) Uani 1 d . . . H6'1 H 0.2520 -0.3241 -0.3584 0.070 Uiso 1 calc R . . H6'2 H 0.2757 -0.1537 -0.3728 0.070 Uiso 1 calc R . . H6'3 H 0.0941 -0.1995 -0.3820 0.070 Uiso 1 calc R . . C6 C 0.2980(9) -0.9084(8) 0.4039(5) 0.0554(18) Uani 1 d . . . H6 H 0.2976 -1.0116 0.4106 0.067 Uiso 1 calc R . . C2D C 0.4772(9) 0.0568(9) -0.1739(5) 0.062(2) Uani 1 d . . . H2D1 H 0.4177 0.0021 -0.2105 0.074 Uiso 1 calc R . . H2D2 H 0.5501 -0.0128 -0.1289 0.074 Uiso 1 calc R . . H2D3 H 0.5457 0.1208 -0.2183 0.074 Uiso 1 calc R . . C7 C 0.3300(8) -0.8485(8) 0.4831(5) 0.058(2) Uani 1 d . . . H7 H 0.3489 -0.9114 0.5433 0.070 Uiso 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 Zn 0.0263(5) 0.0299(5) 0.0310(5) -0.0050(4) -0.0004(4) -0.0041(4) S1D 0.0303(8) 0.0447(9) 0.0512(9) 0.0034(7) -0.0038(7) -0.0094(7) O15 0.033(2) 0.027(2) 0.034(2) -0.0052(16) -0.0026(16) 0.0000(16) N1' 0.029(2) 0.035(3) 0.028(2) -0.007(2) -0.0004(19) -0.006(2) N16 0.046(3) 0.032(3) 0.027(2) -0.006(2) -0.003(2) -0.005(2) O1D 0.030(2) 0.044(2) 0.053(3) 0.0011(19) -0.0023(19) -0.0151(18) C14 0.024(3) 0.029(3) 0.031(3) -0.001(2) -0.005(2) -0.002(2) C3 0.031(3) 0.034(3) 0.029(3) -0.006(2) -0.003(2) -0.004(2) S3' 0.0529(10) 0.0424(9) 0.0334(8) -0.0117(7) 0.0002(7) 0.0026(7) S1 0.0531(10) 0.0493(9) 0.0299(8) -0.0050(7) -0.0077(7) -0.0121(7) O1 0.045(3) 0.082(3) 0.051(3) 0.003(2) -0.008(2) -0.031(2) O17 0.059(3) 0.037(2) 0.039(2) -0.0106(18) -0.001(2) 0.001(2) N2 0.041(3) 0.040(3) 0.028(2) -0.005(2) 0.000(2) -0.001(2) C5' 0.043(3) 0.043(3) 0.031(3) -0.004(3) 0.000(3) -0.011(3) O2 0.094(4) 0.067(3) 0.038(3) -0.018(2) -0.015(3) -0.006(3) C2' 0.033(3) 0.043(3) 0.026(3) -0.009(2) -0.002(2) -0.008(3) C4' 0.042(3) 0.043(3) 0.032(3) -0.007(3) -0.001(3) -0.003(3) C4 0.036(3) 0.034(3) 0.033(3) -0.006(2) 0.004(2) -0.007(2) C10 0.026(3) 0.041(3) 0.037(3) 0.000(3) 0.001(2) -0.001(2) C8 0.032(3) 0.061(4) 0.035(3) 0.003(3) -0.002(3) 0.000(3) C13 0.051(4) 0.069(5) 0.036(3) -0.001(3) 0.010(3) 0.003(3) C1D 0.032(3) 0.038(3) 0.065(4) -0.004(3) 0.000(3) -0.008(3) C9 0.027(3) 0.047(3) 0.033(3) 0.000(3) 0.001(2) -0.001(3) C5 0.044(4) 0.034(3) 0.053(4) -0.001(3) -0.008(3) 0.004(3) C6' 0.072(5) 0.069(5) 0.031(3) -0.007(3) 0.011(3) -0.009(4) C6 0.049(4) 0.042(4) 0.066(5) 0.009(3) -0.003(3) -0.001(3) C2D 0.061(5) 0.074(5) 0.053(4) -0.016(4) 0.020(4) -0.021(4) C7 0.042(4) 0.065(5) 0.052(4) 0.023(4) -0.006(3) 0.002(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 Zn N1' 2.060(4) . yes Zn N1' 2.060(4) 2 ? Zn O15 2.081(4) 2 ? Zn O15 2.081(4) . yes Zn O1D 2.173(4) 2 ? Zn O1D 2.173(4) . yes S1D O1D 1.512(4) . yes S1D C1D 1.774(6) . ? S1D C2D 1.782(7) . ? O15 C14 1.235(6) . yes N1' C2' 1.297(7) . yes N1' C5' 1.388(7) . ? N16 C14 1.371(7) . yes N16 C2' 1.380(7) . yes C14 C3 1.443(7) . yes C3 C4 1.394(8) . yes C3 N2 1.436(7) . yes S3' C4' 1.728(6) . ? S3' C2' 1.733(6) . yes S1 O2 1.416(5) . yes S1 O1 1.431(5) . yes S1 N2 1.628(5) . yes S1 C9 1.740(6) . ? O17 C4 1.267(6) . yes N2 C13 1.476(7) . yes C5' C4' 1.335(8) . ? C4' C6' 1.496(8) . ? C4 C10 1.501(8) . ? C10 C5 1.386(8) . ? C10 C9 1.392(8) . ? C8 C7 1.373(9) . ? C8 C9 1.385(8) . ? C5 C6 1.363(9) . ? C6 C7 1.368(10) . ? 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' Zn N1' 180.0 . 2 ? N1' Zn O15 92.65(16) . 2 ? N1' Zn O15 87.35(16) 2 2 ? N1' Zn O15 87.35(16) . . yes N1' Zn O15 92.65(16) 2 . ? O15 Zn O15 180.0 2 . ? N1' Zn O1D 91.82(17) . 2 ? N1' Zn O1D 88.18(17) 2 2 ? O15 Zn O1D 88.97(15) 2 2 ? O15 Zn O1D 91.03(15) . 2 ? N1' Zn O1D 88.18(17) . . yes N1' Zn O1D 91.82(17) 2 . ? O15 Zn O1D 91.03(15) 2 . ? O15 Zn O1D 88.97(15) . . yes O1D Zn O1D 180.0 2 . ? O1D S1D C1D 104.5(3) . . ? O1D S1D C2D 105.3(3) . . ? C1D S1D C2D 98.3(3) . . ? C14 O15 Zn 129.4(3) . . yes C2' N1' C5' 109.6(5) . . yes C2' N1' Zn 124.2(4) . . yes C5' N1' Zn 125.3(4) . . ? C14 N16 C2' 126.1(5) . . yes S1D O1D Zn 126.2(2) . . yes O15 C14 N16 123.6(5) . . yes O15 C14 C3 123.0(5) . . yes N16 C14 C3 113.5(4) . . yes C4 C3 N2 121.1(5) . . yes C4 C3 C14 124.3(5) . . yes N2 C3 C14 114.6(5) . . yes C4' S3' C2' 89.5(3) . . yes O2 S1 O1 118.5(3) . . yes O2 S1 N2 108.9(3) . . yes O1 S1 N2 108.2(3) . . yes O2 S1 C9 110.6(3) . . ? O1 S1 C9 107.6(3) . . ? N2 S1 C9 101.7(3) . . yes C3 N2 C13 115.9(5) . . yes C3 N2 S1 114.0(4) . . yes C13 N2 S1 116.3(4) . . yes C4' C5' N1' 117.4(5) . . ? N1' C2' N16 126.9(5) . . yes N1' C2' S3' 114.7(4) . . yes N16 C2' S3' 118.3(4) . . yes C5' C4' C6' 129.8(6) . . ? C5' C4' S3' 108.8(4) . . yes C6' C4' S3' 121.3(5) . . yes O17 C4 C3 124.1(5) . . yes O17 C4 C10 117.1(5) . . ? C3 C4 C10 118.8(5) . . ? C5 C10 C9 117.6(5) . . ? C5 C10 C4 120.1(5) . . ? C9 C10 C4 122.3(5) . . yes C7 C8 C9 118.2(6) . . ? C8 C9 C10 121.8(6) . . ? C8 C9 S1 121.7(5) . . ? C10 C9 S1 116.4(4) . . ? C6 C5 C10 120.9(6) . . ? C5 C6 C7 120.5(6) . . ? C6 C7 C8 121.0(6) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.605 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.096 #===END data_v32cbcen _database_code_CSD 169595 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-bis(O15,N1'-(4-Hydroxy-2-methyl-N-(5-methyl-1,3-thiazol-2-yl)- 2H-1,2-benzothiazine-3-carbox-amide 1,1-Dioxide)-trans- bis(O-dimethylsolfoxide)cadmiun(II) ; _chemical_name_common ? _chemical_formula_moiety 'C32 H36 Cd N6 O10 S6' _chemical_formula_sum 'C32 H36 Cd N6 O10 S6' _chemical_formula_weight 969.43 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 triclin _symmetry_space_group_name_H-M P-1 #nø 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.978(1) _cell_length_b 9.413(4) _cell_length_c 13.766(1) _cell_angle_alpha 78.72(1) _cell_angle_beta 86.35(1) _cell_angle_gamma 82.56(2) _cell_volume 1004.5(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 11 _cell_measurement_theta_max 35 _exptl_crystal_description parallelepiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 494 _exptl_absorpt_coefficient_mu 0.916 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 Siemens P4 _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3802 _diffrn_reflns_av_R_equivalents 0.0088 _diffrn_reflns_av_sigmaI/netI 0.0155 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3528 _reflns_number_gt 3237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Scans,Siemens' _computing_cell_refinement 'Scans,Siemens' _computing_data_reduction 'Scans,Siemens' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Johnson&Burnett; L.J. Ferrugia, Glasgow, 1998)' _computing_publication_material 'CIFTAB(sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+0.2699P] 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 3528 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0763 _refine_ls_wR_factor_gt 0.0735 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd 0.0000 0.0000 0.0000 0.03027(10) Uani 1 d S . . S1D S 0.33676(9) 0.17536(8) -0.10933(6) 0.05213(19) Uani 1 d . . . O15 O 0.0896(2) -0.18904(18) 0.12185(12) 0.0367(4) Uani 1 d . . . N1' N 0.0812(3) -0.1693(2) -0.09437(14) 0.0346(4) Uani 1 d . . . N16 N 0.1364(3) -0.3787(2) 0.03474(14) 0.0361(4) Uani 1 d . . . H16 H 0.1425 -0.4722 0.0431 0.043 Uiso 1 calc R . . O1D O 0.2731(2) 0.0609(2) -0.02657(17) 0.0538(5) Uani 1 d . . . C14 C 0.1286(3) -0.3209(2) 0.12010(16) 0.0301(5) Uani 1 d . . . C3 C 0.1712(3) -0.4269(3) 0.20733(17) 0.0329(5) Uani 1 d . . . S3' S 0.21843(9) -0.39872(7) -0.15372(5) 0.04496(17) Uani 1 d . . . S1 S 0.31853(9) -0.43395(8) 0.36991(5) 0.04461(17) Uani 1 d . . . O1 O 0.4739(3) -0.4067(2) 0.31577(15) 0.0563(5) Uani 1 d . . . O17 O 0.2333(3) -0.6334(2) 0.13244(13) 0.0471(4) Uani 1 d . . . N2 N 0.1628(3) -0.3681(2) 0.29740(14) 0.0390(5) Uani 1 d . . . C5' C 0.1034(3) -0.1344(3) -0.19672(18) 0.0396(6) Uani 1 d . . . H5' H 0.0710 -0.0410 -0.2319 0.048 Uiso 1 calc R . . O2 O 0.2835(3) -0.3836(3) 0.46152(15) 0.0699(7) Uani 1 d . . . C2' C 0.1354(3) -0.3052(3) -0.06161(17) 0.0322(5) Uani 1 d . . . C4' C 0.1739(4) -0.2419(3) -0.24211(19) 0.0430(6) Uani 1 d . . . C4 C 0.2219(3) -0.5753(3) 0.20903(17) 0.0355(5) Uani 1 d . . . C10 C 0.2638(3) -0.6742(3) 0.30582(19) 0.0389(5) Uani 1 d . . . C8 C 0.3350(4) -0.7123(4) 0.4796(2) 0.0516(7) Uani 1 d . . . H8 H 0.3599 -0.6745 0.5339 0.062 Uiso 1 calc R . . C13 C -0.0064(4) -0.3445(4) 0.3445(2) 0.0604(8) Uani 1 d . . . H13A H 0.0019 -0.3063 0.4035 0.072 Uiso 1 calc R . . H13B H -0.0534 -0.4354 0.3613 0.072 Uiso 1 calc R . . H13C H -0.0784 -0.2762 0.2994 0.072 Uiso 1 calc R . . C1D C 0.4774(3) 0.2612(3) -0.0521(2) 0.0526(7) Uani 1 d . . . H1D1 H 0.4140 0.3217 -0.0107 0.063 Uiso 1 calc R . . H1D2 H 0.5414 0.3201 -0.1021 0.063 Uiso 1 calc R . . H1D3 H 0.5531 0.1883 -0.0124 0.063 Uiso 1 calc R . . C9 C 0.3045(3) -0.6214(3) 0.38857(18) 0.0402(6) Uani 1 d . . . C5 C 0.2609(4) -0.8234(3) 0.3163(2) 0.0501(7) Uani 1 d . . . H5 H 0.2383 -0.8623 0.2621 0.060 Uiso 1 calc R . . C6' C 0.2104(5) -0.2410(4) -0.3504(2) 0.0629(9) Uani 1 d . . . H6'1 H 0.2613 -0.3360 -0.3593 0.075 Uiso 1 calc R . . H6'2 H 0.2866 -0.1704 -0.3762 0.075 Uiso 1 calc R . . H6'3 H 0.1068 -0.2160 -0.3850 0.075 Uiso 1 calc R . . C6 C 0.2912(4) -0.9150(4) 0.4069(3) 0.0634(9) Uani 1 d . . . H6 H 0.2873 -1.0147 0.4133 0.076 Uiso 1 calc R . . C2D C 0.4883(5) 0.0756(4) -0.1789(3) 0.0743(10) Uani 1 d . . . H2D1 H 0.4312 0.0207 -0.2156 0.089 Uiso 1 calc R . . H2D2 H 0.5642 0.0101 -0.1346 0.089 Uiso 1 calc R . . H2D3 H 0.5513 0.1422 -0.2241 0.089 Uiso 1 calc R . . C7 C 0.3274(4) -0.8586(4) 0.4878(2) 0.0621(9) Uani 1 d . . . H7 H 0.3468 -0.9208 0.5484 0.074 Uiso 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 Cd 0.02718(14) 0.02714(14) 0.03647(15) -0.00814(9) -0.00004(9) -0.00057(9) S1D 0.0361(4) 0.0459(4) 0.0700(5) 0.0036(3) -0.0078(3) -0.0080(3) O15 0.0452(10) 0.0331(9) 0.0314(8) -0.0085(7) -0.0028(7) 0.0014(7) N1' 0.0421(11) 0.0319(10) 0.0302(10) -0.0078(8) -0.0021(8) -0.0031(8) N16 0.0486(12) 0.0307(10) 0.0297(10) -0.0072(8) -0.0039(9) -0.0043(9) O1D 0.0310(9) 0.0483(11) 0.0773(14) 0.0025(10) 0.0010(9) -0.0102(8) C14 0.0267(11) 0.0345(13) 0.0292(11) -0.0074(9) -0.0003(9) -0.0028(9) C3 0.0348(12) 0.0365(12) 0.0278(11) -0.0086(9) -0.0005(9) -0.0019(10) S3' 0.0594(4) 0.0404(4) 0.0340(3) -0.0133(3) -0.0003(3) 0.0069(3) S1 0.0546(4) 0.0509(4) 0.0295(3) -0.0079(3) -0.0068(3) -0.0078(3) O1 0.0519(12) 0.0665(13) 0.0507(12) -0.0001(10) -0.0098(9) -0.0213(10) O17 0.0655(12) 0.0376(10) 0.0380(10) -0.0126(8) -0.0043(9) 0.0035(9) N2 0.0476(12) 0.0420(12) 0.0268(10) -0.0097(8) 0.0004(9) 0.0007(9) C5' 0.0490(14) 0.0366(13) 0.0325(13) -0.0026(10) -0.0039(11) -0.0074(11) O2 0.1039(18) 0.0756(16) 0.0334(11) -0.0203(10) -0.0137(11) -0.0019(14) C2' 0.0348(12) 0.0340(12) 0.0299(12) -0.0107(9) -0.0041(9) -0.0033(9) C4' 0.0514(15) 0.0464(15) 0.0314(13) -0.0076(11) 0.0007(11) -0.0073(12) C4 0.0345(12) 0.0388(13) 0.0326(12) -0.0068(10) -0.0001(10) -0.0026(10) C10 0.0320(12) 0.0421(14) 0.0395(13) -0.0041(11) -0.0005(10) 0.0009(10) C8 0.0421(15) 0.068(2) 0.0377(14) 0.0022(13) -0.0008(11) 0.0020(13) C13 0.0564(18) 0.075(2) 0.0462(16) -0.0178(15) 0.0096(14) 0.0103(16) C1D 0.0377(14) 0.0425(15) 0.077(2) -0.0097(14) 0.0077(14) -0.0086(12) C9 0.0331(12) 0.0478(15) 0.0353(13) -0.0010(11) -0.0004(10) 0.0003(11) C5 0.0486(16) 0.0425(15) 0.0553(17) -0.0039(13) -0.0054(13) 0.0023(12) C6' 0.083(2) 0.072(2) 0.0316(14) -0.0099(14) 0.0085(15) -0.0062(18) C6 0.0587(19) 0.0448(17) 0.075(2) 0.0125(15) -0.0038(16) 0.0021(14) C2D 0.087(3) 0.075(2) 0.065(2) -0.0207(18) 0.0124(19) -0.023(2) C7 0.0537(18) 0.066(2) 0.0519(18) 0.0174(16) -0.0049(14) 0.0039(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd N1' 2.254(2) . yes Cd N1' 2.254(2) 2 ? Cd O15 2.2686(17) 2 ? Cd O15 2.2686(17) . yes Cd O1D 2.3133(18) 2 ? Cd O1D 2.3133(18) . yes S1D O1D 1.518(2) . yes S1D C1D 1.769(3) . ? S1D C2D 1.781(4) . ? O15 C14 1.244(3) . yes N1' C2' 1.297(3) . yes N1' C5' 1.388(3) . ? N16 C2' 1.371(3) . yes N16 C14 1.383(3) . yes C14 C3 1.431(3) . yes C3 C4 1.399(3) . yes C3 N2 1.448(3) . yes S3' C2' 1.732(2) . yes S3' C4' 1.733(3) . ? S1 O2 1.431(2) . yes S1 O1 1.431(2) . yes S1 N2 1.625(2) . yes S1 C9 1.750(3) . ? O17 C4 1.272(3) . yes N2 C13 1.470(3) . yes C5' C4' 1.336(4) . ? C4' C6' 1.499(4) . ? C4 C10 1.498(3) . ? C10 C5 1.386(4) . ? C10 C9 1.400(4) . ? C8 C7 1.369(5) . ? C8 C9 1.388(4) . ? C5 C6 1.385(4) . ? C6 C7 1.385(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 N1' Cd N1' 180.0 . 2 ? N1' Cd O15 98.57(7) . 2 ? N1' Cd O15 81.43(7) 2 2 ? N1' Cd O15 81.43(7) . . yes N1' Cd O15 98.57(7) 2 . ? O15 Cd O15 180.0 2 . ? N1' Cd O1D 93.79(8) . 2 ? N1' Cd O1D 86.21(8) 2 2 ? O15 Cd O1D 89.93(7) 2 2 ? O15 Cd O1D 90.07(7) . 2 ? N1' Cd O1D 86.21(8) . . yes N1' Cd O1D 93.79(8) 2 . ? O15 Cd O1D 90.07(7) 2 . ? O15 Cd O1D 89.93(7) . . yes O1D Cd O1D 180.0 2 . ? O1D S1D C1D 104.70(14) . . ? O1D S1D C2D 104.77(16) . . ? C1D S1D C2D 98.59(17) . . ? C14 O15 Cd 130.60(15) . . yes C2' N1' C5' 110.9(2) . . yes C2' N1' Cd 125.64(16) . . yes C5' N1' Cd 122.81(16) . . ? C2' N16 C14 127.9(2) . . yes S1D O1D Cd 126.88(12) . . yes O15 C14 N16 123.7(2) . . yes O15 C14 C3 122.5(2) . . yes N16 C14 C3 113.8(2) . . yes C4 C3 C14 124.9(2) . . yes C4 C3 N2 120.7(2) . . yes C14 C3 N2 114.4(2) . . yes C2' S3' C4' 89.92(12) . . yes O2 S1 O1 118.95(15) . . yes O2 S1 N2 108.52(13) . . yes O1 S1 N2 108.53(11) . . yes O2 S1 C9 109.81(14) . . ? O1 S1 C9 107.99(13) . . ? N2 S1 C9 101.64(12) . . yes C3 N2 C13 116.0(2) . . yes C3 N2 S1 114.03(16) . . yes C13 N2 S1 117.26(18) . . yes C4' C5' N1' 116.6(2) . . ? N1' C2' N16 127.8(2) . . yes N1' C2' S3' 113.77(18) . . yes N16 C2' S3' 118.41(18) . . yes C5' C4' C6' 129.6(3) . . ? C5' C4' S3' 108.86(19) . . yes C6' C4' S3' 121.5(2) . . yes O17 C4 C3 123.7(2) . . yes O17 C4 C10 117.0(2) . . ? C3 C4 C10 119.2(2) . . ? C5 C10 C9 117.6(2) . . ? C5 C10 C4 120.2(2) . . ? C9 C10 C4 122.3(2) . . yes C7 C8 C9 118.6(3) . . ? C8 C9 C10 122.2(3) . . ? C8 C9 S1 121.8(2) . . ? C10 C9 S1 115.98(19) . . ? C6 C5 C10 120.6(3) . . ? C5 C6 C7 120.2(3) . . ? C8 C7 C6 120.8(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.362 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.060