Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Maochun Hong' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter, fuzhou 350002 CHINA ; _publ_contact_author_email HMC@FJIRSM.AC.CN _publ_section_title ; Cd(II)- sulfonyldibenzoilate Coordination Polymers Based on Mono-, Bi-, Tri- and Tetra-Nuclear Cores as Nodes ; loop_ _publ_author_name 'Maochun Hong' 'Jiu-Tong Chen' 'Fei-Long Jiang' 'Fen-Yan Lian' ; Mingyan Wu ; 'Da-Qiang Yuan' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 650347' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H9 Cd0.50 N2 O3.50 S0.50' _chemical_formula_sum 'C17 H9 Cd0.50 N2 O3.50 S0.50' _chemical_formula_weight 369.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 6.0417(10) _cell_length_b 23.070(4) _cell_length_c 24.165(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3368.1(10) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6360 _cell_measurement_theta_min 2.5300 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.762 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8035 _exptl_absorpt_correction_T_max 0.8942 _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 MoK\a _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 24231 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0186 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3942 _reflns_number_gt 3504 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL-97 (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+5.0256P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3942 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1360 _refine_ls_wR_factor_gt 0.1315 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.07981(5) 0.2500 0.5000 0.03732(13) Uani 1 2 d S . . S1 S 0.4977(2) 0.49976(5) 0.2500 0.0381(3) Uani 1 2 d S . . O1 O 0.3584(4) 0.30623(12) 0.45520(12) 0.0566(7) Uani 1 1 d . . . O2 O 0.0170(4) 0.33616(12) 0.44415(11) 0.0553(7) Uani 1 1 d . . . O3 O 0.7327(6) 0.50467(15) 0.2500 0.0486(8) Uani 1 2 d S . . O4 O 0.3640(7) 0.55142(14) 0.2500 0.0514(9) Uani 1 2 d S . . O5 O -0.2938(7) 0.2500 0.5000 0.0604(11) Uani 1 2 d S . . N1 N 0.0892(5) 0.31118(15) 0.57731(14) 0.0536(8) Uani 1 1 d . . . C1 C 0.2174(6) 0.33986(15) 0.43387(13) 0.0420(7) Uani 1 1 d . . . C2 C 0.2956(5) 0.38377(13) 0.39196(13) 0.0379(7) Uani 1 1 d . . . C3 C 0.5072(6) 0.38099(18) 0.37072(16) 0.0548(10) Uani 1 1 d . . . H3 H 0.6080 0.3546 0.3852 0.066 Uiso 1 1 calc R . . C4 C 0.1487(6) 0.42405(16) 0.37105(15) 0.0471(8) Uani 1 1 d . . . H4 H 0.0067 0.4264 0.3858 0.057 Uiso 1 1 calc R . . C5 C 0.5706(6) 0.41726(19) 0.32793(17) 0.0552(10) Uani 1 1 d . . . H5 H 0.7127 0.4150 0.3133 0.066 Uiso 1 1 calc R . . C6 C 0.2091(6) 0.46080(15) 0.32871(14) 0.0456(8) Uani 1 1 d . . . H6 H 0.1094 0.4878 0.3148 0.055 Uiso 1 1 calc R . . C7 C 0.4215(5) 0.45670(13) 0.30723(13) 0.0365(7) Uani 1 1 d . . . C8 C -0.0777(9) 0.3461(2) 0.5869(3) 0.0906(18) Uani 1 1 d . . . H8 H -0.1972 0.3452 0.5626 0.109 Uiso 1 1 calc R . . C9 C 0.2574(10) 0.3142(2) 0.6114(2) 0.0835(15) Uani 1 1 d . . . H9 H 0.3788 0.2903 0.6053 0.100 Uiso 1 1 calc R . . C10 C -0.0854(12) 0.3839(3) 0.6309(3) 0.122(3) Uani 1 1 d . . . H10 H -0.2082 0.4076 0.6362 0.146 Uiso 1 1 calc R . . C11 C 0.2611(13) 0.3520(3) 0.6563(3) 0.109(2) Uani 1 1 d . . . H11 H 0.3841 0.3535 0.6794 0.131 Uiso 1 1 calc R . . C12 C 0.0864(12) 0.3862(3) 0.6661(3) 0.104(2) Uani 1 1 d . . . H12 H 0.0841 0.4109 0.6965 0.125 Uiso 1 1 calc R . . C13 C 0.3215(16) 0.4859(4) 0.5304(4) 0.142(3) Uiso 0.83 1 d P . . N2 N 0.3215(16) 0.4859(4) 0.5304(4) 0.142(3) Uiso 0.17 1 d P . . C14 C 0.3316(18) 0.5374(4) 0.5046(3) 0.135(3) Uiso 0.83 1 d P . . N3 N 0.3316(18) 0.5374(4) 0.5046(3) 0.135(3) Uiso 0.17 1 d P . . C15 C 0.5076(18) 0.5526(4) 0.4749(4) 0.138(3) Uiso 0.83 1 d P . . N4 N 0.5076(18) 0.5526(4) 0.4749(4) 0.138(3) Uiso 0.17 1 d P . . C16 C 0.652(3) 0.2487(6) 0.2500 0.159(6) Uiso 0.83 2 d SP . . N5 N 0.652(3) 0.2487(6) 0.2500 0.159(6) Uiso 0.17 2 d SP . . C17 C 0.7338(19) 0.2601(4) 0.2959(4) 0.147(3) Uiso 0.83 1 d P . . N6 N 0.7338(19) 0.2601(4) 0.2959(4) 0.147(3) Uiso 0.17 1 d P . . C18 C 0.9267(15) 0.2854(4) 0.3000(4) 0.137(3) Uiso 0.83 1 d P . . N7 N 0.9267(15) 0.2854(4) 0.3000(4) 0.137(3) Uiso 0.17 1 d P . . C19 C 1.047(2) 0.2998(6) 0.2500 0.157(5) Uiso 0.83 2 d SP . . N8 N 1.047(2) 0.2998(6) 0.2500 0.157(5) Uiso 0.17 2 d SP . . 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 0.0329(2) 0.0420(2) 0.0370(2) 0.00604(13) 0.000 0.000 S1 0.0493(7) 0.0330(5) 0.0321(5) 0.000 0.000 -0.0081(5) O1 0.0445(14) 0.0568(15) 0.0686(17) 0.0279(13) -0.0026(13) 0.0032(12) O2 0.0367(13) 0.0657(16) 0.0634(16) 0.0249(13) 0.0029(13) -0.0018(12) O3 0.050(2) 0.050(2) 0.0454(18) 0.000 0.000 -0.0171(17) O4 0.076(3) 0.0294(16) 0.0485(18) 0.000 0.000 0.0010(17) O5 0.0346(19) 0.063(2) 0.083(3) 0.034(2) 0.000 0.000 N1 0.057(2) 0.0520(18) 0.0518(17) -0.0028(15) -0.0050(15) 0.0036(15) C1 0.0403(18) 0.0446(17) 0.0410(16) 0.0079(14) -0.0018(14) -0.0025(14) C2 0.0346(16) 0.0399(16) 0.0391(15) 0.0072(13) -0.0005(13) -0.0002(13) C3 0.0370(18) 0.064(2) 0.063(2) 0.0282(19) 0.0032(18) 0.0093(17) C4 0.0371(17) 0.054(2) 0.0499(19) 0.0131(16) 0.0060(15) 0.0093(15) C5 0.0352(18) 0.068(2) 0.062(2) 0.023(2) 0.0080(16) 0.0079(17) C6 0.0423(18) 0.0439(17) 0.0506(18) 0.0113(15) 0.0033(15) 0.0109(15) C7 0.0376(16) 0.0366(15) 0.0354(14) 0.0030(12) -0.0019(12) -0.0043(13) C8 0.088(4) 0.079(3) 0.105(4) -0.035(3) -0.024(3) 0.025(3) C9 0.076(3) 0.096(4) 0.079(3) -0.024(3) -0.020(3) 0.006(3) C10 0.114(6) 0.107(5) 0.144(6) -0.070(5) -0.017(5) 0.023(4) C11 0.124(6) 0.111(5) 0.091(4) -0.037(4) -0.048(4) 0.004(4) C12 0.139(6) 0.086(4) 0.088(4) -0.040(3) -0.009(4) 0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O5 2.257(4) . ? Cd1 N1 2.342(3) 3_556 ? Cd1 N1 2.342(3) . ? Cd1 O1 2.385(3) 3_556 ? Cd1 O1 2.385(3) . ? Cd1 O2 2.432(3) 3_556 ? Cd1 O2 2.432(3) . ? Cd1 C1 2.747(3) 3_556 ? S1 O3 1.424(4) . ? S1 O4 1.440(4) . ? S1 C7 1.764(3) 6_556 ? S1 C7 1.764(3) . ? O1 C1 1.262(4) . ? O2 C1 1.239(4) . ? N1 C9 1.309(6) . ? N1 C8 1.311(6) . ? C1 C2 1.508(4) . ? C2 C3 1.380(5) . ? C2 C4 1.381(5) . ? C3 C5 1.384(5) . ? C3 H3 0.9300 . ? C4 C6 1.378(5) . ? C4 H4 0.9300 . ? C5 C7 1.374(5) . ? C5 H5 0.9300 . ? C6 C7 1.387(5) . ? C6 H6 0.9300 . ? C8 C10 1.376(8) . ? C8 H8 0.9300 . ? C9 C11 1.393(7) . ? C9 H9 0.9300 . ? C10 C12 1.344(9) . ? C10 H10 0.9300 . ? C11 C12 1.339(9) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.343(11) . ? C13 N4 1.368(12) 5_666 ? C13 C15 1.368(12) 5_666 ? C14 C15 1.330(13) . ? C15 N2 1.368(12) 5_666 ? C15 C13 1.368(12) 5_666 ? C16 C17 1.243(11) . ? C16 N6 1.243(11) 6_556 ? C16 C17 1.243(11) 6_556 ? C17 C18 1.306(12) . ? C18 C19 1.451(11) . ? C19 N7 1.451(11) 6_556 ? C19 C18 1.451(11) 6_556 ? 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 O5 Cd1 N1 91.39(8) . 3_556 ? O5 Cd1 N1 91.39(8) . . ? N1 Cd1 N1 177.21(17) 3_556 . ? O5 Cd1 O1 134.89(6) . 3_556 ? N1 Cd1 O1 90.98(11) 3_556 3_556 ? N1 Cd1 O1 87.05(11) . 3_556 ? O5 Cd1 O1 134.89(6) . . ? N1 Cd1 O1 87.05(11) 3_556 . ? N1 Cd1 O1 90.98(12) . . ? O1 Cd1 O1 90.23(12) 3_556 . ? O5 Cd1 O2 81.03(6) . 3_556 ? N1 Cd1 O2 87.36(11) 3_556 3_556 ? N1 Cd1 O2 93.08(11) . 3_556 ? O1 Cd1 O2 54.10(9) 3_556 3_556 ? O1 Cd1 O2 143.75(9) . 3_556 ? O5 Cd1 O2 81.03(6) . . ? N1 Cd1 O2 93.08(11) 3_556 . ? N1 Cd1 O2 87.36(11) . . ? O1 Cd1 O2 143.75(9) 3_556 . ? O1 Cd1 O2 54.10(9) . . ? O2 Cd1 O2 162.06(13) 3_556 . ? O5 Cd1 C1 107.62(7) . 3_556 ? N1 Cd1 C1 90.11(11) 3_556 3_556 ? N1 Cd1 C1 89.05(11) . 3_556 ? O1 Cd1 C1 27.33(9) 3_556 3_556 ? O1 Cd1 C1 117.46(10) . 3_556 ? O2 Cd1 C1 26.81(10) 3_556 3_556 ? O2 Cd1 C1 170.72(10) . 3_556 ? O3 S1 O4 119.6(2) . . ? O3 S1 C7 107.77(14) . 6_556 ? O4 S1 C7 108.64(15) . 6_556 ? O3 S1 C7 107.77(14) . . ? O4 S1 C7 108.64(15) . . ? C7 S1 C7 103.3(2) 6_556 . ? C1 O1 Cd1 92.5(2) . . ? C1 O2 Cd1 90.9(2) . . ? C9 N1 C8 116.9(4) . . ? C9 N1 Cd1 123.6(3) . . ? C8 N1 Cd1 119.5(3) . . ? O2 C1 O1 122.3(3) . . ? O2 C1 C2 119.1(3) . . ? O1 C1 C2 118.4(3) . . ? C3 C2 C4 119.4(3) . . ? C3 C2 C1 120.6(3) . . ? C4 C2 C1 119.8(3) . . ? C2 C3 C5 120.4(3) . . ? C2 C3 H3 119.8 . . ? C5 C3 H3 119.8 . . ? C6 C4 C2 121.0(3) . . ? C6 C4 H4 119.5 . . ? C2 C4 H4 119.5 . . ? C7 C5 C3 119.4(3) . . ? C7 C5 H5 120.3 . . ? C3 C5 H5 120.3 . . ? C4 C6 C7 118.7(3) . . ? C4 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? C5 C7 C6 121.0(3) . . ? C5 C7 S1 119.1(3) . . ? C6 C7 S1 119.8(2) . . ? N1 C8 C10 123.5(6) . . ? N1 C8 H8 118.3 . . ? C10 C8 H8 118.3 . . ? N1 C9 C11 122.5(5) . . ? N1 C9 H9 118.8 . . ? C11 C9 H9 118.8 . . ? C12 C10 C8 119.3(6) . . ? C12 C10 H10 120.4 . . ? C8 C10 H10 120.4 . . ? C12 C11 C9 119.6(6) . . ? C12 C11 H11 120.2 . . ? C9 C11 H11 120.2 . . ? C11 C12 C10 118.2(5) . . ? C11 C12 H12 120.9 . . ? C10 C12 H12 120.9 . . ? C14 C13 N4 119.8(10) . 5_666 ? C14 C13 C15 119.8(10) . 5_666 ? N4 C13 C15 0.0(10) 5_666 5_666 ? C15 C14 C13 121.4(10) . . ? C14 C15 N2 118.8(9) . 5_666 ? C14 C15 C13 118.8(9) . 5_666 ? N2 C15 C13 0.0(10) 5_666 5_666 ? C17 C16 N6 126.3(19) . 6_556 ? C17 C16 C17 126.3(19) . 6_556 ? N6 C16 C17 0.0(9) 6_556 6_556 ? C16 C17 C18 121.2(13) . . ? C17 C18 C19 119.2(10) . . ? N7 C19 C18 0.0(10) 6_556 6_556 ? N7 C19 C18 112.8(13) 6_556 . ? C18 C19 C18 112.8(13) 6_556 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.395 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.076 # Attachment '2.cif' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 650348' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H36 Cd2 N4 O12 S2' _chemical_formula_sum 'C52 H36 Cd2 N4 O12 S2' _chemical_formula_weight 1197.77 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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.478(5) _cell_length_b 22.004(7) _cell_length_c 16.494(6) _cell_angle_alpha 90.00 _cell_angle_beta 114.412(3) _cell_angle_gamma 90.00 _cell_volume 5446(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9062 _cell_measurement_theta_min 2.2806 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 0.919 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9137 _exptl_absorpt_correction_T_max 0.9301 _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 MoK\a _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 42185 _diffrn_reflns_av_R_equivalents 0.0778 _diffrn_reflns_av_sigmaI/netI 0.0833 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12485 _reflns_number_gt 8702 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL-97 (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+7.1259P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12485 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1258 _refine_ls_R_factor_gt 0.0843 _refine_ls_wR_factor_ref 0.1905 _refine_ls_wR_factor_gt 0.1710 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.005 _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 0.23681(3) 0.74042(2) 0.94229(3) 0.03954(15) Uani 1 1 d . . . S1 S -0.1981(2) 0.94120(14) 1.0016(2) 0.1021(11) Uani 1 1 d . . . O1 O 0.1179(3) 0.7983(2) 0.9220(4) 0.0545(13) Uani 1 1 d . . . N1 N 0.1470(4) 0.6569(2) 0.9366(4) 0.0495(15) Uani 1 1 d . . . C1 C 0.1272(4) 0.8203(3) 0.9941(5) 0.0415(15) Uani 1 1 d . . . Cd2 Cd 0.29419(3) 0.77668(2) 1.19867(3) 0.04179(15) Uani 1 1 d . . . S2 S 0.68828(13) 0.54386(9) 1.11837(13) 0.0528(5) Uani 1 1 d . . . O2 O 0.1963(3) 0.8161(3) 1.0628(4) 0.0703(16) Uani 1 1 d . . . N2 N -0.1941(4) 0.3009(3) 0.8165(4) 0.0576(16) Uani 1 1 d . . . C2 C 0.0470(4) 0.8525(3) 0.9965(5) 0.0439(15) Uani 1 1 d . . . O3 O -0.1927(3) 0.8199(2) 1.3758(4) 0.0574(13) Uani 1 1 d . . . N3 N 0.3898(3) 0.8504(2) 1.1904(4) 0.0460(14) Uani 1 1 d . . . C3 C 0.0554(6) 0.8926(4) 1.0606(7) 0.079(3) Uani 1 1 d . . . H3 H 0.1116 0.9010 1.1047 0.095 Uiso 1 1 calc R . . O4 O -0.3073(4) 0.7707(3) 1.2794(4) 0.0730(17) Uani 1 1 d . . . N4 N 0.6701(4) 1.1798(2) 1.0533(4) 0.0524(15) Uani 1 1 d . . . C4 C -0.0200(8) 0.9223(4) 1.0622(8) 0.096(3) Uani 1 1 d . . . H4A H -0.0137 0.9512 1.1055 0.115 Uiso 1 1 calc R . . O5 O -0.2736(5) 0.9277(4) 0.9174(5) 0.137(4) Uani 1 1 d . . . C5 C -0.1017(6) 0.9078(4) 0.9991(6) 0.068(2) Uani 1 1 d . . . O6 O -0.1769(6) 1.0022(3) 1.0288(7) 0.139(4) Uani 1 1 d . . . C6 C -0.1112(6) 0.8661(5) 0.9354(6) 0.094(4) Uani 1 1 d . . . H6 H -0.1677 0.8553 0.8940 0.113 Uiso 1 1 calc R . . O7 O 0.4086(3) 0.7093(2) 1.2269(3) 0.0492(11) Uani 1 1 d . . . C7 C -0.0360(5) 0.8395(4) 0.9322(6) 0.074(3) Uani 1 1 d . . . H7 H -0.0420 0.8128 0.8863 0.088 Uiso 1 1 calc R . . O8 O 0.3325(3) 0.7097(2) 1.0827(3) 0.0575(13) Uani 1 1 d . . . C8 C -0.2129(7) 0.9027(5) 1.0884(7) 0.074(3) Uani 1 1 d . . . O9 O 0.8245(4) 0.7134(3) 0.8585(4) 0.0784(18) Uani 1 1 d . . . C9 C -0.1750(7) 0.9247(4) 1.1728(8) 0.088(3) Uani 1 1 d . . . H9 H -0.1427 0.9608 1.1847 0.105 Uiso 1 1 calc R . . O10 O 0.7274(4) 0.6546(3) 0.7579(5) 0.0849(19) Uani 1 1 d . . . C10 C -0.1849(7) 0.8926(4) 1.2424(6) 0.074(3) Uani 1 1 d . . . H10 H -0.1583 0.9072 1.3005 0.089 Uiso 1 1 calc R . . O11 O 0.6515(4) 0.4856(2) 1.0823(4) 0.0670(15) Uani 1 1 d . . . C11 C -0.2340(5) 0.8399(4) 1.2240(5) 0.0540(18) Uani 1 1 d . . . O12 O 0.7660(3) 0.5471(3) 1.2007(4) 0.0703(16) Uani 1 1 d . . . C12 C -0.2730(6) 0.8192(5) 1.1375(6) 0.079(3) Uani 1 1 d . . . H12 H -0.3076 0.7841 1.1251 0.094 Uiso 1 1 calc R . . C13 C -0.2624(7) 0.8491(6) 1.0680(7) 0.090(3) Uani 1 1 d . . . H13 H -0.2874 0.8339 1.0102 0.108 Uiso 1 1 calc R . . C14 C -0.2457(5) 0.8075(3) 1.2978(5) 0.0494(17) Uani 1 1 d . . . C15 C 0.3993(4) 0.6946(3) 1.1513(5) 0.0402(15) Uani 1 1 d . . . C16 C 0.4706(4) 0.6567(3) 1.1418(5) 0.0420(15) Uani 1 1 d . . . C17 C 0.5533(4) 0.6543(4) 1.2118(5) 0.059(2) Uani 1 1 d . . . H17 H 0.5641 0.6756 1.2640 0.070 Uiso 1 1 calc R . . C18 C 0.6205(5) 0.6199(4) 1.2044(5) 0.065(2) Uani 1 1 d . . . H18 H 0.6769 0.6187 1.2510 0.078 Uiso 1 1 calc R . . C19 C 0.6031(4) 0.5878(3) 1.1276(5) 0.0442(16) Uani 1 1 d . . . C20 C 0.5208(5) 0.5902(3) 1.0568(5) 0.058(2) Uani 1 1 d . . . H20 H 0.5100 0.5684 1.0051 0.070 Uiso 1 1 calc R . . C21 C 0.4555(5) 0.6247(3) 1.0637(5) 0.0557(19) Uani 1 1 d . . . H21 H 0.4001 0.6271 1.0158 0.067 Uiso 1 1 calc R . . C22 C 0.7119(5) 0.5817(3) 1.0367(5) 0.0506(17) Uani 1 1 d . . . C23 C 0.6792(6) 0.5591(4) 0.9512(6) 0.065(2) Uani 1 1 d . . . H23 H 0.6451 0.5239 0.9368 0.078 Uiso 1 1 calc R . . C24 C 0.6970(6) 0.5888(4) 0.8870(6) 0.066(2) Uani 1 1 d . . . H24 H 0.6734 0.5738 0.8291 0.079 Uiso 1 1 calc R . . C25 C 0.7491(5) 0.6402(4) 0.9069(5) 0.0564(19) Uani 1 1 d . . . C26 C 0.7824(5) 0.6619(4) 0.9921(6) 0.069(2) Uani 1 1 d . . . H26 H 0.8180 0.6964 1.0062 0.082 Uiso 1 1 calc R . . C27 C 0.7642(5) 0.6332(4) 1.0587(6) 0.065(2) Uani 1 1 d . . . H27 H 0.7868 0.6486 1.1164 0.078 Uiso 1 1 calc R . . C28 C 0.7692(5) 0.6724(4) 0.8358(6) 0.060(2) Uani 1 1 d . . . C29 C 0.0644(5) 0.6612(3) 0.9284(6) 0.060(2) Uani 1 1 d . . . H29 H 0.0428 0.6996 0.9321 0.072 Uiso 1 1 calc R . . C30 C 0.0072(5) 0.6121(3) 0.9147(6) 0.062(2) Uani 1 1 d . . . H30 H -0.0498 0.6177 0.9120 0.075 Uiso 1 1 calc R . . C31 C 0.0367(5) 0.5543(3) 0.9051(6) 0.056(2) Uani 1 1 d . . . C32 C 0.1229(5) 0.5499(3) 0.9134(7) 0.069(3) Uani 1 1 d . . . H32 H 0.1459 0.5122 0.9080 0.083 Uiso 1 1 calc R . . C33 C 0.1754(5) 0.6008(3) 0.9294(6) 0.064(2) Uani 1 1 d . . . H33 H 0.2338 0.5962 0.9358 0.077 Uiso 1 1 calc R . . C34 C -0.0257(5) 0.5037(3) 0.8851(6) 0.063(2) Uani 1 1 d . . . H34 H -0.0814 0.5123 0.8839 0.076 Uiso 1 1 calc R . . C35 C -0.0114(5) 0.4470(4) 0.8685(7) 0.074(3) Uani 1 1 d . . . H35 H 0.0441 0.4382 0.8691 0.089 Uiso 1 1 calc R . . C36 C -0.0747(5) 0.3968(3) 0.8491(6) 0.066(2) Uani 1 1 d . . . C37 C -0.1632(5) 0.4072(4) 0.8284(6) 0.071(3) Uani 1 1 d . . . H37 H -0.1845 0.4467 0.8250 0.086 Uiso 1 1 calc R . . C38 C -0.2208(5) 0.3582(4) 0.8127(7) 0.075(3) Uani 1 1 d . . . H38 H -0.2806 0.3657 0.7988 0.090 Uiso 1 1 calc R . . C39 C -0.0490(6) 0.3378(4) 0.8506(8) 0.091(4) Uani 1 1 d . . . H39 H 0.0100 0.3287 0.8625 0.110 Uiso 1 1 calc R . . C40 C -0.1105(6) 0.2911(4) 0.8343(8) 0.086(3) Uani 1 1 d . . . H40 H -0.0912 0.2512 0.8362 0.103 Uiso 1 1 calc R . . C41 C 0.4724(4) 0.8407(3) 1.1995(5) 0.0547(19) Uani 1 1 d . . . H41 H 0.4967 0.8021 1.2165 0.066 Uiso 1 1 calc R . . C42 C 0.5240(5) 0.8847(3) 1.1853(6) 0.059(2) Uani 1 1 d . . . H42 H 0.5816 0.8754 1.1922 0.071 Uiso 1 1 calc R . . C43 C 0.4906(4) 0.9432(3) 1.1604(5) 0.0530(19) Uani 1 1 d . . . C44 C 0.4048(4) 0.9530(3) 1.1529(5) 0.0542(19) Uani 1 1 d . . . H44 H 0.3792 0.9914 1.1380 0.065 Uiso 1 1 calc R . . C45 C 0.3579(4) 0.9064(3) 1.1674(6) 0.057(2) Uani 1 1 d . . . H45 H 0.3000 0.9142 1.1608 0.068 Uiso 1 1 calc R . . C46 C 0.5440(5) 0.9892(3) 1.1406(6) 0.063(2) Uani 1 1 d . . . H46 H 0.6024 0.9789 1.1516 0.076 Uiso 1 1 calc R . . C47 C 0.5173(5) 1.0429(4) 1.1092(6) 0.069(2) Uani 1 1 d . . . H47 H 0.4592 1.0532 1.0992 0.083 Uiso 1 1 calc R . . C48 C 0.5694(5) 1.0896(3) 1.0874(6) 0.058(2) Uani 1 1 d . . . C49 C 0.5395(6) 1.1483(4) 1.0713(8) 0.094(4) Uani 1 1 d . . . H49 H 0.4846 1.1586 1.0709 0.112 Uiso 1 1 calc R . . C50 C 0.5911(5) 1.1920(4) 1.0555(8) 0.091(4) Uani 1 1 d . . . H50 H 0.5704 1.2318 1.0459 0.109 Uiso 1 1 calc R . . C51 C 0.6486(5) 1.0767(3) 1.0815(6) 0.066(2) Uani 1 1 d . . . H51 H 0.6697 1.0370 1.0890 0.079 Uiso 1 1 calc R . . C52 C 0.6964(5) 1.1224(3) 1.0646(5) 0.0521(18) Uani 1 1 d . . . H52 H 0.7497 1.1125 1.0609 0.063 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 0.0362(3) 0.0358(3) 0.0489(3) 0.0000(2) 0.0199(2) -0.00206(18) S1 0.122(2) 0.116(2) 0.114(2) 0.0696(19) 0.094(2) 0.0786(19) O1 0.047(3) 0.061(3) 0.059(3) -0.007(3) 0.025(2) 0.008(2) N1 0.046(3) 0.036(3) 0.067(4) -0.004(3) 0.024(3) -0.004(2) C1 0.039(4) 0.039(4) 0.050(4) 0.005(3) 0.022(3) 0.001(3) Cd2 0.0392(3) 0.0417(3) 0.0484(3) -0.0049(2) 0.0221(2) -0.00612(19) S2 0.0575(11) 0.0563(11) 0.0517(12) 0.0157(9) 0.0296(9) 0.0188(9) O2 0.044(3) 0.104(4) 0.055(4) 0.009(3) 0.013(2) 0.012(3) N2 0.049(4) 0.054(4) 0.074(5) -0.014(3) 0.029(3) -0.018(3) C2 0.045(4) 0.048(4) 0.044(4) 0.007(3) 0.024(3) 0.006(3) O3 0.066(3) 0.054(3) 0.060(4) 0.002(3) 0.034(3) -0.003(2) N3 0.035(3) 0.035(3) 0.065(4) 0.001(3) 0.017(3) -0.004(2) C3 0.073(6) 0.084(6) 0.088(7) -0.024(5) 0.041(5) 0.000(5) O4 0.069(4) 0.081(4) 0.067(4) 0.004(3) 0.027(3) -0.026(3) N4 0.050(3) 0.043(3) 0.062(4) 0.006(3) 0.020(3) -0.007(3) C4 0.118(9) 0.073(6) 0.122(10) -0.029(6) 0.075(8) 0.010(6) O5 0.104(5) 0.234(10) 0.087(6) 0.097(6) 0.054(4) 0.110(6) C5 0.077(6) 0.083(6) 0.056(6) 0.023(5) 0.039(5) 0.031(5) O6 0.207(9) 0.084(5) 0.227(11) 0.065(6) 0.191(9) 0.061(5) C6 0.057(5) 0.165(10) 0.060(6) -0.001(6) 0.024(4) 0.050(6) O7 0.050(3) 0.050(3) 0.050(3) -0.002(2) 0.024(2) 0.006(2) C7 0.051(5) 0.117(7) 0.050(5) -0.007(5) 0.017(4) 0.022(5) O8 0.049(3) 0.070(3) 0.051(3) 0.007(3) 0.017(2) 0.015(2) C8 0.086(6) 0.082(6) 0.075(7) 0.035(5) 0.056(5) 0.036(5) O9 0.080(4) 0.079(4) 0.086(5) 0.014(3) 0.044(4) -0.010(3) C9 0.127(9) 0.058(6) 0.103(9) 0.009(6) 0.073(7) 0.010(5) O10 0.097(5) 0.103(5) 0.063(4) 0.013(4) 0.042(4) -0.018(4) C10 0.116(8) 0.062(5) 0.063(6) -0.002(4) 0.054(5) 0.000(5) O11 0.090(4) 0.049(3) 0.077(4) 0.009(3) 0.050(3) 0.008(3) C11 0.057(4) 0.066(5) 0.052(5) -0.001(4) 0.035(4) 0.007(4) O12 0.058(3) 0.102(4) 0.047(3) 0.026(3) 0.018(3) 0.034(3) C12 0.076(6) 0.104(7) 0.056(6) 0.005(5) 0.027(5) -0.010(5) C13 0.078(7) 0.139(10) 0.057(6) 0.014(6) 0.032(5) 0.018(7) C14 0.052(4) 0.055(4) 0.048(5) 0.003(3) 0.027(3) 0.012(3) C15 0.040(3) 0.029(3) 0.052(4) 0.004(3) 0.019(3) 0.000(2) C16 0.048(4) 0.031(3) 0.049(4) -0.002(3) 0.022(3) -0.001(3) C17 0.040(4) 0.082(5) 0.049(5) -0.011(4) 0.014(3) 0.010(4) C18 0.033(4) 0.097(6) 0.051(5) -0.010(4) 0.004(3) 0.012(4) C19 0.050(4) 0.047(4) 0.040(4) 0.008(3) 0.023(3) 0.007(3) C20 0.061(5) 0.072(5) 0.040(4) -0.008(4) 0.020(4) 0.016(4) C21 0.047(4) 0.064(5) 0.046(5) -0.007(4) 0.010(3) 0.012(3) C22 0.056(4) 0.059(5) 0.042(4) 0.003(3) 0.026(3) 0.012(3) C23 0.095(6) 0.060(5) 0.057(5) 0.004(4) 0.047(5) -0.006(4) C24 0.090(6) 0.069(5) 0.050(5) -0.003(4) 0.040(4) -0.007(5) C25 0.050(4) 0.074(5) 0.050(5) 0.009(4) 0.026(4) 0.010(4) C26 0.060(5) 0.070(5) 0.078(7) 0.008(5) 0.031(4) -0.017(4) C27 0.064(5) 0.080(6) 0.046(5) -0.005(4) 0.018(4) -0.009(4) C28 0.055(5) 0.067(5) 0.068(6) 0.027(4) 0.036(4) 0.017(4) C29 0.046(4) 0.050(4) 0.091(7) -0.003(4) 0.035(4) 0.000(3) C30 0.035(4) 0.060(5) 0.094(7) -0.003(4) 0.029(4) -0.009(3) C31 0.048(4) 0.040(4) 0.074(6) 0.006(4) 0.019(4) -0.010(3) C32 0.041(4) 0.038(4) 0.126(8) 0.005(4) 0.032(4) -0.005(3) C33 0.037(4) 0.049(4) 0.106(7) 0.001(4) 0.029(4) -0.006(3) C34 0.051(4) 0.050(4) 0.091(7) -0.004(4) 0.032(4) -0.013(3) C35 0.053(5) 0.062(5) 0.108(8) -0.004(5) 0.034(5) -0.019(4) C36 0.060(5) 0.050(5) 0.090(7) 0.000(4) 0.034(5) -0.015(4) C37 0.049(5) 0.047(4) 0.110(8) 0.012(5) 0.025(5) -0.008(3) C38 0.052(5) 0.056(5) 0.117(8) 0.011(5) 0.035(5) -0.007(4) C39 0.060(5) 0.058(5) 0.173(12) -0.024(6) 0.066(6) -0.018(4) C40 0.069(6) 0.054(5) 0.149(10) -0.020(6) 0.060(6) -0.015(4) C41 0.043(4) 0.045(4) 0.076(6) 0.009(4) 0.024(4) 0.000(3) C42 0.036(4) 0.047(4) 0.094(7) 0.017(4) 0.028(4) 0.006(3) C43 0.040(4) 0.049(4) 0.057(5) 0.011(3) 0.007(3) -0.007(3) C44 0.041(4) 0.043(4) 0.070(5) 0.012(4) 0.014(3) 0.001(3) C45 0.036(4) 0.049(4) 0.079(6) 0.006(4) 0.018(4) 0.002(3) C46 0.052(4) 0.048(4) 0.084(6) 0.013(4) 0.024(4) -0.009(3) C47 0.060(5) 0.055(5) 0.094(7) 0.013(5) 0.033(5) -0.006(4) C48 0.055(5) 0.054(4) 0.065(5) 0.009(4) 0.025(4) -0.013(4) C49 0.060(5) 0.060(5) 0.177(12) 0.026(6) 0.065(7) 0.001(4) C50 0.055(5) 0.050(5) 0.179(11) 0.022(6) 0.060(6) 0.006(4) C51 0.069(5) 0.036(4) 0.102(7) 0.002(4) 0.044(5) -0.003(3) C52 0.057(4) 0.040(4) 0.065(5) -0.001(3) 0.032(4) -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 Cd1 O1 2.244(5) . ? Cd1 O8 2.300(5) . ? Cd1 N4 2.312(5) 3_677 ? Cd1 O3 2.317(5) 4_675 ? Cd1 N1 2.337(5) . ? Cd1 O4 2.488(6) 4_675 ? Cd1 C14 2.727(8) 4_675 ? S1 O6 1.412(9) . ? S1 O5 1.462(9) . ? S1 C5 1.765(8) . ? S1 C8 1.766(9) . ? O1 C1 1.233(8) . ? N1 C29 1.315(8) . ? N1 C33 1.342(9) . ? C1 O2 1.234(8) . ? C1 C2 1.515(9) . ? Cd2 O7 2.289(4) . ? Cd2 N3 2.304(5) . ? Cd2 O10 2.311(6) 4_576 ? Cd2 N2 2.315(6) 3_567 ? Cd2 O2 2.321(5) . ? Cd2 O9 2.481(7) 4_576 ? Cd2 C28 2.703(8) 4_576 ? S2 O12 1.432(5) . ? S2 O11 1.437(6) . ? S2 C22 1.759(8) . ? S2 C19 1.762(7) . ? N2 C40 1.302(10) . ? N2 C38 1.327(10) . ? N2 Cd2 2.315(6) 3_567 ? C2 C3 1.341(11) . ? C2 C7 1.369(10) . ? O3 C14 1.250(9) . ? O3 Cd1 2.317(5) 4_576 ? N3 C41 1.324(8) . ? N3 C45 1.332(8) . ? C3 C4 1.413(12) . ? C3 H3 0.9300 . ? O4 C14 1.234(9) . ? O4 Cd1 2.488(6) 4_576 ? N4 C52 1.324(8) . ? N4 C50 1.343(10) . ? N4 Cd1 2.312(5) 3_677 ? C4 C5 1.356(13) . ? C4 H4A 0.9300 . ? C5 C6 1.354(13) . ? C6 C7 1.392(11) . ? C6 H6 0.9300 . ? O7 C15 1.236(8) . ? C7 H7 0.9300 . ? O8 C15 1.253(8) . ? C8 C9 1.357(14) . ? C8 C13 1.395(14) . ? O9 C28 1.227(10) . ? O9 Cd2 2.481(7) 4_675 ? C9 C10 1.414(12) . ? C9 H9 0.9300 . ? O10 C28 1.243(10) . ? O10 Cd2 2.311(6) 4_675 ? C10 C11 1.374(11) . ? C10 H10 0.9300 . ? C11 C12 1.379(11) . ? C11 C14 1.491(10) . ? C12 C13 1.394(13) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 Cd1 2.727(8) 4_576 ? C15 C16 1.500(9) . ? C16 C17 1.376(9) . ? C16 C21 1.398(10) . ? C17 C18 1.388(10) . ? C17 H17 0.9300 . ? C18 C19 1.373(10) . ? C18 H18 0.9300 . ? C19 C20 1.377(9) . ? C20 C21 1.360(9) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C27 1.378(10) . ? C22 C23 1.378(11) . ? C23 C24 1.373(10) . ? C23 H23 0.9300 . ? C24 C25 1.374(11) . ? C24 H24 0.9300 . ? C25 C26 1.366(11) . ? C25 C28 1.520(11) . ? C26 C27 1.404(11) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 Cd2 2.703(8) 4_675 ? C29 C30 1.388(9) . ? C29 H29 0.9300 . ? C30 C31 1.393(10) . ? C30 H30 0.9300 . ? C31 C32 1.374(10) . ? C31 C34 1.457(9) . ? C32 C33 1.372(9) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.320(11) . ? C34 H34 0.9300 . ? C35 C36 1.462(10) . ? C35 H35 0.9300 . ? C36 C39 1.364(11) . ? C36 C37 1.373(10) . ? C37 C38 1.388(10) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.388(11) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C42 1.372(10) . ? C41 H41 0.9300 . ? C42 C43 1.394(9) . ? C42 H42 0.9300 . ? C43 C44 1.384(9) . ? C43 C46 1.464(10) . ? C44 C45 1.364(9) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C47 1.292(10) . ? C46 H46 0.9300 . ? C47 C48 1.475(10) . ? C47 H47 0.9300 . ? C48 C49 1.368(11) . ? C48 C51 1.377(11) . ? C49 C50 1.379(11) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 C52 1.375(10) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O8 120.68(19) . . ? O1 Cd1 N4 95.8(2) . 3_677 ? O8 Cd1 N4 91.3(2) . 3_677 ? O1 Cd1 O3 146.4(2) . 4_675 ? O8 Cd1 O3 92.26(19) . 4_675 ? N4 Cd1 O3 89.6(2) 3_677 4_675 ? O1 Cd1 N1 86.64(19) . . ? O8 Cd1 N1 88.2(2) . . ? N4 Cd1 N1 177.4(2) 3_677 . ? O3 Cd1 N1 87.88(19) 4_675 . ? O1 Cd1 O4 92.71(18) . 4_675 ? O8 Cd1 O4 146.23(18) . 4_675 ? N4 Cd1 O4 90.1(2) 3_677 4_675 ? O3 Cd1 O4 54.01(18) 4_675 4_675 ? N1 Cd1 O4 88.9(2) . 4_675 ? O1 Cd1 C14 119.3(2) . 4_675 ? O8 Cd1 C14 119.4(2) . 4_675 ? N4 Cd1 C14 90.7(2) 3_677 4_675 ? O3 Cd1 C14 27.16(19) 4_675 4_675 ? N1 Cd1 C14 87.4(2) . 4_675 ? O4 Cd1 C14 26.87(19) 4_675 4_675 ? O6 S1 O5 119.8(6) . . ? O6 S1 C5 107.3(5) . . ? O5 S1 C5 108.3(5) . . ? O6 S1 C8 107.2(5) . . ? O5 S1 C8 108.9(6) . . ? C5 S1 C8 104.3(4) . . ? C1 O1 Cd1 109.0(4) . . ? C29 N1 C33 116.1(6) . . ? C29 N1 Cd1 124.0(5) . . ? C33 N1 Cd1 119.3(5) . . ? O1 C1 O2 123.8(7) . . ? O1 C1 C2 116.5(6) . . ? O2 C1 C2 119.7(7) . . ? O7 Cd2 N3 86.67(18) . . ? O7 Cd2 O10 146.5(2) . 4_576 ? N3 Cd2 O10 91.2(2) . 4_576 ? O7 Cd2 N2 92.0(2) . 3_567 ? N3 Cd2 N2 170.8(2) . 3_567 ? O10 Cd2 N2 94.9(2) 4_576 3_567 ? O7 Cd2 O2 128.55(19) . . ? N3 Cd2 O2 84.2(2) . . ? O10 Cd2 O2 84.4(2) 4_576 . ? N2 Cd2 O2 89.5(2) 3_567 . ? O7 Cd2 O9 93.07(19) . 4_576 ? N3 Cd2 O9 99.1(2) . 4_576 ? O10 Cd2 O9 54.2(2) 4_576 4_576 ? N2 Cd2 O9 90.1(2) 3_567 4_576 ? O2 Cd2 O9 138.4(2) . 4_576 ? O7 Cd2 C28 119.7(2) . 4_576 ? N3 Cd2 C28 95.8(2) . 4_576 ? O10 Cd2 C28 27.3(2) 4_576 4_576 ? N2 Cd2 C28 92.7(2) 3_567 4_576 ? O2 Cd2 C28 111.6(3) . 4_576 ? O9 Cd2 C28 26.9(2) 4_576 4_576 ? O12 S2 O11 119.7(4) . . ? O12 S2 C22 107.9(4) . . ? O11 S2 C22 107.1(4) . . ? O12 S2 C19 108.9(3) . . ? O11 S2 C19 108.1(3) . . ? C22 S2 C19 104.1(3) . . ? C1 O2 Cd2 157.6(5) . . ? C40 N2 C38 117.9(7) . . ? C40 N2 Cd2 122.8(5) . 3_567 ? C38 N2 Cd2 119.2(5) . 3_567 ? C3 C2 C7 119.6(7) . . ? C3 C2 C1 121.5(7) . . ? C7 C2 C1 119.0(7) . . ? C14 O3 Cd1 95.0(5) . 4_576 ? C41 N3 C45 116.7(6) . . ? C41 N3 Cd2 125.2(4) . . ? C45 N3 Cd2 118.0(4) . . ? C2 C3 C4 120.9(9) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C14 O4 Cd1 87.4(5) . 4_576 ? C52 N4 C50 116.9(6) . . ? C52 N4 Cd1 123.1(5) . 3_677 ? C50 N4 Cd1 119.0(5) . 3_677 ? C5 C4 C3 118.6(9) . . ? C5 C4 H4A 120.7 . . ? C3 C4 H4A 120.7 . . ? C6 C5 C4 120.9(8) . . ? C6 C5 S1 118.9(8) . . ? C4 C5 S1 120.1(8) . . ? C5 C6 C7 119.7(9) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C15 O7 Cd2 102.5(4) . . ? C2 C7 C6 120.2(9) . . ? C2 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C15 O8 Cd1 165.2(5) . . ? C9 C8 C13 121.6(9) . . ? C9 C8 S1 120.1(9) . . ? C13 C8 S1 118.2(9) . . ? C28 O9 Cd2 86.7(5) . 4_675 ? C8 C9 C10 119.8(9) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C28 O10 Cd2 94.2(5) . 4_675 ? C11 C10 C9 119.8(9) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 119.3(8) . . ? C10 C11 C14 119.1(7) . . ? C12 C11 C14 121.6(8) . . ? C11 C12 C13 122.1(10) . . ? C11 C12 H12 119.0 . . ? C13 C12 H12 119.0 . . ? C12 C13 C8 117.4(10) . . ? C12 C13 H13 121.3 . . ? C8 C13 H13 121.3 . . ? O4 C14 O3 123.4(7) . . ? O4 C14 C11 119.0(7) . . ? O3 C14 C11 117.6(7) . . ? O4 C14 Cd1 65.7(4) . 4_576 ? O3 C14 Cd1 57.8(4) . 4_576 ? C11 C14 Cd1 173.9(5) . 4_576 ? O7 C15 O8 122.5(6) . . ? O7 C15 C16 118.4(6) . . ? O8 C15 C16 119.2(7) . . ? C17 C16 C21 119.4(6) . . ? C17 C16 C15 118.8(6) . . ? C21 C16 C15 121.8(6) . . ? C16 C17 C18 119.8(7) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C19 C18 C17 119.5(7) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 121.3(7) . . ? C18 C19 S2 119.5(5) . . ? C20 C19 S2 119.2(6) . . ? C21 C20 C19 119.1(7) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 C16 120.8(7) . . ? C20 C21 H21 119.6 . . ? C16 C21 H21 119.6 . . ? C27 C22 C23 120.2(7) . . ? C27 C22 S2 120.0(6) . . ? C23 C22 S2 119.8(6) . . ? C24 C23 C22 120.0(8) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 121.2(8) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C26 C25 C24 118.6(8) . . ? C26 C25 C28 120.5(8) . . ? C24 C25 C28 120.9(8) . . ? C25 C26 C27 121.5(8) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C22 C27 C26 118.4(8) . . ? C22 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? O9 C28 O10 124.9(8) . . ? O9 C28 C25 118.6(9) . . ? O10 C28 C25 116.5(8) . . ? O9 C28 Cd2 66.4(5) . 4_675 ? O10 C28 Cd2 58.5(4) . 4_675 ? C25 C28 Cd2 175.0(7) . 4_675 ? N1 C29 C30 124.4(7) . . ? N1 C29 H29 117.8 . . ? C30 C29 H29 117.8 . . ? C29 C30 C31 118.9(7) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? C32 C31 C30 116.6(6) . . ? C32 C31 C34 124.9(7) . . ? C30 C31 C34 118.5(7) . . ? C33 C32 C31 120.3(7) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? N1 C33 C32 123.6(7) . . ? N1 C33 H33 118.2 . . ? C32 C33 H33 118.2 . . ? C35 C34 C31 126.8(8) . . ? C35 C34 H34 116.6 . . ? C31 C34 H34 116.6 . . ? C34 C35 C36 126.0(8) . . ? C34 C35 H35 117.0 . . ? C36 C35 H35 117.0 . . ? C39 C36 C37 117.0(7) . . ? C39 C36 C35 121.8(8) . . ? C37 C36 C35 121.2(7) . . ? C36 C37 C38 119.3(8) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? N2 C38 C37 122.8(7) . . ? N2 C38 H38 118.6 . . ? C37 C38 H38 118.6 . . ? C36 C39 C40 120.3(8) . . ? C36 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? N2 C40 C39 122.7(8) . . ? N2 C40 H40 118.7 . . ? C39 C40 H40 118.7 . . ? N3 C41 C42 123.2(7) . . ? N3 C41 H41 118.4 . . ? C42 C41 H41 118.4 . . ? C41 C42 C43 120.3(7) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C44 C43 C42 115.8(6) . . ? C44 C43 C46 123.9(7) . . ? C42 C43 C46 120.3(7) . . ? C45 C44 C43 120.0(6) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? N3 C45 C44 124.0(7) . . ? N3 C45 H45 118.0 . . ? C44 C45 H45 118.0 . . ? C47 C46 C43 125.8(8) . . ? C47 C46 H46 117.1 . . ? C43 C46 H46 117.1 . . ? C46 C47 C48 126.7(8) . . ? C46 C47 H47 116.6 . . ? C48 C47 H47 116.6 . . ? C49 C48 C51 117.1(7) . . ? C49 C48 C47 120.4(8) . . ? C51 C48 C47 122.5(7) . . ? C48 C49 C50 119.7(8) . . ? C48 C49 H49 120.2 . . ? C50 C49 H49 120.2 . . ? N4 C50 C49 123.0(8) . . ? N4 C50 H50 118.5 . . ? C49 C50 H50 118.5 . . ? C52 C51 C48 120.2(7) . . ? C52 C51 H51 119.9 . . ? C48 C51 H51 119.9 . . ? N4 C52 C51 123.0(7) . . ? N4 C52 H52 118.5 . . ? C51 C52 H52 118.5 . . ? 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 O8 Cd1 O1 C1 15.8(5) . . . . ? N4 Cd1 O1 C1 -79.2(5) 3_677 . . . ? O3 Cd1 O1 C1 -177.3(4) 4_675 . . . ? N1 Cd1 O1 C1 101.7(5) . . . . ? O4 Cd1 O1 C1 -169.6(5) 4_675 . . . ? C14 Cd1 O1 C1 -173.2(4) 4_675 . . . ? O1 Cd1 N1 C29 -2.7(6) . . . . ? O8 Cd1 N1 C29 118.2(7) . . . . ? N4 Cd1 N1 C29 -164(5) 3_677 . . . ? O3 Cd1 N1 C29 -149.5(7) 4_675 . . . ? O4 Cd1 N1 C29 -95.5(7) 4_675 . . . ? C14 Cd1 N1 C29 -122.3(7) 4_675 . . . ? O1 Cd1 N1 C33 168.2(6) . . . . ? O8 Cd1 N1 C33 -70.9(6) . . . . ? N4 Cd1 N1 C33 7(5) 3_677 . . . ? O3 Cd1 N1 C33 21.4(6) 4_675 . . . ? O4 Cd1 N1 C33 75.5(6) 4_675 . . . ? C14 Cd1 N1 C33 48.6(6) 4_675 . . . ? Cd1 O1 C1 O2 7.8(9) . . . . ? Cd1 O1 C1 C2 -170.4(4) . . . . ? O1 C1 O2 Cd2 -95.5(15) . . . . ? C2 C1 O2 Cd2 82.7(15) . . . . ? O7 Cd2 O2 C1 95.6(14) . . . . ? N3 Cd2 O2 C1 176.6(14) . . . . ? O10 Cd2 O2 C1 -91.6(14) 4_576 . . . ? N2 Cd2 O2 C1 3.4(14) 3_567 . . . ? O9 Cd2 O2 C1 -86.1(15) 4_576 . . . ? C28 Cd2 O2 C1 -89.3(14) 4_576 . . . ? O1 C1 C2 C3 -160.0(8) . . . . ? O2 C1 C2 C3 21.6(11) . . . . ? O1 C1 C2 C7 20.9(10) . . . . ? O2 C1 C2 C7 -157.4(8) . . . . ? O7 Cd2 N3 C41 1.4(6) . . . . ? O10 Cd2 N3 C41 147.9(6) 4_576 . . . ? N2 Cd2 N3 C41 -80.5(15) 3_567 . . . ? O2 Cd2 N3 C41 -127.9(6) . . . . ? O9 Cd2 N3 C41 93.9(6) 4_576 . . . ? C28 Cd2 N3 C41 120.9(6) 4_576 . . . ? O7 Cd2 N3 C45 175.5(6) . . . . ? O10 Cd2 N3 C45 -38.0(6) 4_576 . . . ? N2 Cd2 N3 C45 93.6(14) 3_567 . . . ? O2 Cd2 N3 C45 46.2(6) . . . . ? O9 Cd2 N3 C45 -91.9(6) 4_576 . . . ? C28 Cd2 N3 C45 -64.9(6) 4_576 . . . ? C7 C2 C3 C4 -0.9(14) . . . . ? C1 C2 C3 C4 -179.9(8) . . . . ? C2 C3 C4 C5 2.3(16) . . . . ? C3 C4 C5 C6 -0.5(16) . . . . ? C3 C4 C5 S1 177.1(8) . . . . ? O6 S1 C5 C6 -144.6(9) . . . . ? O5 S1 C5 C6 -14.0(10) . . . . ? C8 S1 C5 C6 101.9(9) . . . . ? O6 S1 C5 C4 37.8(10) . . . . ? O5 S1 C5 C4 168.4(9) . . . . ? C8 S1 C5 C4 -75.7(10) . . . . ? C4 C5 C6 C7 -2.7(16) . . . . ? S1 C5 C6 C7 179.7(8) . . . . ? N3 Cd2 O7 C15 -86.5(4) . . . . ? O10 Cd2 O7 C15 -173.7(4) 4_576 . . . ? N2 Cd2 O7 C15 84.3(4) 3_567 . . . ? O2 Cd2 O7 C15 -6.6(5) . . . . ? O9 Cd2 O7 C15 174.5(4) 4_576 . . . ? C28 Cd2 O7 C15 178.6(4) 4_576 . . . ? C3 C2 C7 C6 -2.3(14) . . . . ? C1 C2 C7 C6 176.8(8) . . . . ? C5 C6 C7 C2 4.1(16) . . . . ? O1 Cd1 O8 C15 -144.8(18) . . . . ? N4 Cd1 O8 C15 -47.3(18) 3_677 . . . ? O3 Cd1 O8 C15 42.4(18) 4_675 . . . ? N1 Cd1 O8 C15 130.2(18) . . . . ? O4 Cd1 O8 C15 45(2) 4_675 . . . ? C14 Cd1 O8 C15 44.2(19) 4_675 . . . ? O6 S1 C8 C9 -22.7(9) . . . . ? O5 S1 C8 C9 -153.7(8) . . . . ? C5 S1 C8 C9 90.8(8) . . . . ? O6 S1 C8 C13 158.6(8) . . . . ? O5 S1 C8 C13 27.6(9) . . . . ? C5 S1 C8 C13 -87.8(8) . . . . ? C13 C8 C9 C10 0.6(15) . . . . ? S1 C8 C9 C10 -178.1(7) . . . . ? C8 C9 C10 C11 -1.0(14) . . . . ? C9 C10 C11 C12 -0.1(13) . . . . ? C9 C10 C11 C14 -178.5(8) . . . . ? C10 C11 C12 C13 1.8(14) . . . . ? C14 C11 C12 C13 -179.9(8) . . . . ? C11 C12 C13 C8 -2.2(14) . . . . ? C9 C8 C13 C12 1.0(14) . . . . ? S1 C8 C13 C12 179.7(7) . . . . ? Cd1 O4 C14 O3 3.2(7) 4_576 . . . ? Cd1 O4 C14 C11 -175.6(6) 4_576 . . . ? Cd1 O3 C14 O4 -3.5(8) 4_576 . . . ? Cd1 O3 C14 C11 175.4(5) 4_576 . . . ? C10 C11 C14 O4 160.6(8) . . . . ? C12 C11 C14 O4 -17.7(11) . . . . ? C10 C11 C14 O3 -18.3(10) . . . . ? C12 C11 C14 O3 163.4(7) . . . . ? C10 C11 C14 Cd1 22(5) . . . 4_576 ? C12 C11 C14 Cd1 -156(4) . . . 4_576 ? Cd2 O7 C15 O8 -8.9(7) . . . . ? Cd2 O7 C15 C16 171.6(4) . . . . ? Cd1 O8 C15 O7 141.2(16) . . . . ? Cd1 O8 C15 C16 -39(2) . . . . ? O7 C15 C16 C17 -18.2(9) . . . . ? O8 C15 C16 C17 162.2(7) . . . . ? O7 C15 C16 C21 162.6(7) . . . . ? O8 C15 C16 C21 -17.0(10) . . . . ? C21 C16 C17 C18 -0.3(12) . . . . ? C15 C16 C17 C18 -179.5(7) . . . . ? C16 C17 C18 C19 -1.2(13) . . . . ? C17 C18 C19 C20 1.6(13) . . . . ? C17 C18 C19 S2 -179.7(6) . . . . ? O12 S2 C19 C18 3.0(8) . . . . ? O11 S2 C19 C18 134.5(7) . . . . ? C22 S2 C19 C18 -111.9(7) . . . . ? O12 S2 C19 C20 -178.3(6) . . . . ? O11 S2 C19 C20 -46.8(7) . . . . ? C22 S2 C19 C20 66.8(7) . . . . ? C18 C19 C20 C21 -0.5(12) . . . . ? S2 C19 C20 C21 -179.2(6) . . . . ? C19 C20 C21 C16 -1.1(12) . . . . ? C17 C16 C21 C20 1.5(12) . . . . ? C15 C16 C21 C20 -179.3(7) . . . . ? O12 S2 C22 C27 -36.7(7) . . . . ? O11 S2 C22 C27 -166.8(6) . . . . ? C19 S2 C22 C27 78.9(7) . . . . ? O12 S2 C22 C23 142.3(6) . . . . ? O11 S2 C22 C23 12.2(7) . . . . ? C19 S2 C22 C23 -102.1(7) . . . . ? C27 C22 C23 C24 -1.5(12) . . . . ? S2 C22 C23 C24 179.5(6) . . . . ? C22 C23 C24 C25 1.7(13) . . . . ? C23 C24 C25 C26 -0.7(13) . . . . ? C23 C24 C25 C28 179.4(7) . . . . ? C24 C25 C26 C27 -0.4(12) . . . . ? C28 C25 C26 C27 179.5(7) . . . . ? C23 C22 C27 C26 0.4(12) . . . . ? S2 C22 C27 C26 179.4(6) . . . . ? C25 C26 C27 C22 0.6(13) . . . . ? Cd2 O9 C28 O10 0.1(9) 4_675 . . . ? Cd2 O9 C28 C25 -179.9(6) 4_675 . . . ? Cd2 O10 C28 O9 -0.1(9) 4_675 . . . ? Cd2 O10 C28 C25 179.9(6) 4_675 . . . ? C26 C25 C28 O9 9.0(11) . . . . ? C24 C25 C28 O9 -171.2(8) . . . . ? C26 C25 C28 O10 -171.0(8) . . . . ? C24 C25 C28 O10 8.9(11) . . . . ? C26 C25 C28 Cd2 -170(6) . . . 4_675 ? C24 C25 C28 Cd2 10(7) . . . 4_675 ? C33 N1 C29 C30 1.0(13) . . . . ? Cd1 N1 C29 C30 172.2(7) . . . . ? N1 C29 C30 C31 -2.7(14) . . . . ? C29 C30 C31 C32 2.4(13) . . . . ? C29 C30 C31 C34 -176.2(8) . . . . ? C30 C31 C32 C33 -0.6(14) . . . . ? C34 C31 C32 C33 177.8(9) . . . . ? C29 N1 C33 C32 0.9(13) . . . . ? Cd1 N1 C33 C32 -170.7(7) . . . . ? C31 C32 C33 N1 -1.1(15) . . . . ? C32 C31 C34 C35 -2.8(15) . . . . ? C30 C31 C34 C35 175.6(10) . . . . ? C31 C34 C35 C36 179.5(9) . . . . ? C34 C35 C36 C39 -166.4(11) . . . . ? C34 C35 C36 C37 13.7(16) . . . . ? C39 C36 C37 C38 1.7(15) . . . . ? C35 C36 C37 C38 -178.4(9) . . . . ? C40 N2 C38 C37 -1.2(15) . . . . ? Cd2 N2 C38 C37 174.5(8) 3_567 . . . ? C36 C37 C38 N2 -0.2(16) . . . . ? C37 C36 C39 C40 -2.0(16) . . . . ? C35 C36 C39 C40 178.2(10) . . . . ? C38 N2 C40 C39 1.0(16) . . . . ? Cd2 N2 C40 C39 -174.5(9) 3_567 . . . ? C36 C39 C40 N2 0.6(18) . . . . ? C45 N3 C41 C42 -1.0(12) . . . . ? Cd2 N3 C41 C42 173.2(6) . . . . ? N3 C41 C42 C43 0.5(13) . . . . ? C41 C42 C43 C44 0.9(12) . . . . ? C41 C42 C43 C46 -176.7(8) . . . . ? C42 C43 C44 C45 -1.6(12) . . . . ? C46 C43 C44 C45 175.9(8) . . . . ? C41 N3 C45 C44 0.2(12) . . . . ? Cd2 N3 C45 C44 -174.4(6) . . . . ? C43 C44 C45 N3 1.1(13) . . . . ? C44 C43 C46 C47 -4.2(15) . . . . ? C42 C43 C46 C47 173.2(9) . . . . ? C43 C46 C47 C48 -179.0(8) . . . . ? C46 C47 C48 C49 -167.1(10) . . . . ? C46 C47 C48 C51 13.5(15) . . . . ? C51 C48 C49 C50 -3.9(16) . . . . ? C47 C48 C49 C50 176.7(10) . . . . ? C52 N4 C50 C49 1.9(16) . . . . ? Cd1 N4 C50 C49 -166.5(9) 3_677 . . . ? C48 C49 C50 N4 1.4(18) . . . . ? C49 C48 C51 C52 3.3(14) . . . . ? C47 C48 C51 C52 -177.3(8) . . . . ? C50 N4 C52 C51 -2.6(13) . . . . ? Cd1 N4 C52 C51 165.3(7) 3_677 . . . ? C48 C51 C52 N4 0.0(14) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.823 _refine_diff_density_min -0.776 _refine_diff_density_rms 0.108 # Attachment '3.cif' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 650349' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H16 Cd N2 O6 S' _chemical_formula_sum 'C24 H16 Cd N2 O6 S' _chemical_formula_weight 572.85 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 12.354(3) _cell_length_b 15.312(3) _cell_length_c 12.315(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.330(3) _cell_angle_gamma 90.00 _cell_volume 2184.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5943 _cell_measurement_theta_min 2.4116 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 1.141 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7259 _exptl_absorpt_correction_T_max 0.9451 _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 'Mercury CCD' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 16904 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4980 _reflns_number_gt 4284 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL-97 (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+0.6765P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4980 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0562 _refine_ls_wR_factor_gt 0.0534 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.007896(11) 0.030146(8) 0.845302(10) 0.02563(5) Uani 1 1 d . . . S1 S -0.51458(4) 0.35599(3) 0.37975(4) 0.02707(10) Uani 1 1 d . . . O1 O -0.14215(12) 0.12390(10) 0.80756(12) 0.0383(3) Uani 1 1 d . . . O2 O -0.02336(12) 0.16515(10) 0.71794(14) 0.0435(4) Uani 1 1 d . . . O3 O -0.95453(11) 0.09131(9) 0.07662(12) 0.0352(3) Uani 1 1 d . . . O4 O -0.83205(12) 0.07937(11) -0.01782(12) 0.0440(4) Uani 1 1 d . . . O5 O -0.56981(12) 0.40560(9) 0.44463(13) 0.0375(3) Uani 1 1 d . . . O6 O -0.47525(12) 0.40004(10) 0.29752(13) 0.0402(3) Uani 1 1 d . . . N1 N -0.11240(15) -0.03286(10) 0.66517(14) 0.0325(4) Uani 1 1 d . . . N2 N 0.12025(14) -0.03585(10) 0.75228(13) 0.0290(3) Uani 1 1 d . . . C1 C -0.11873(16) 0.16787(12) 0.73203(17) 0.0316(4) Uani 1 1 d . . . C2 C -0.21509(15) 0.21964(12) 0.64721(16) 0.0282(4) Uani 1 1 d . . . C3 C -0.32882(16) 0.20148(13) 0.63894(16) 0.0319(4) Uani 1 1 d . . . H3 H -0.3431 0.1625 0.6903 0.038 Uiso 1 1 calc R . . C4 C -0.41964(16) 0.24139(13) 0.55455(17) 0.0315(4) Uani 1 1 d . . . H4 H -0.4954 0.2289 0.5478 0.038 Uiso 1 1 calc R . . C5 C -0.39656(15) 0.30044(12) 0.47988(15) 0.0255(4) Uani 1 1 d . . . C6 C -0.28466(16) 0.32023(12) 0.48737(16) 0.0291(4) Uani 1 1 d . . . H6 H -0.2706 0.3600 0.4367 0.035 Uiso 1 1 calc R . . C7 C -0.19403(15) 0.27926(12) 0.57236(17) 0.0290(4) Uani 1 1 d . . . H7 H -0.1184 0.2920 0.5791 0.035 Uiso 1 1 calc R . . C8 C -0.61135(15) 0.27270(12) 0.30426(14) 0.0251(4) Uani 1 1 d . . . C9 C -0.57550(15) 0.21362(13) 0.23840(16) 0.0319(4) Uani 1 1 d . . . H9 H -0.4983 0.2113 0.2448 0.038 Uiso 1 1 calc R . . C10 C -0.65525(16) 0.15811(13) 0.16304(16) 0.0330(4) Uani 1 1 d . . . H10 H -0.6319 0.1188 0.1179 0.040 Uiso 1 1 calc R . . C11 C -0.77081(15) 0.16119(12) 0.15493(15) 0.0266(4) Uani 1 1 d . . . C12 C -0.80460(15) 0.21764(12) 0.22569(16) 0.0286(4) Uani 1 1 d . . . H12 H -0.8808 0.2175 0.2230 0.034 Uiso 1 1 calc R . . C13 C -0.72551(15) 0.27423(12) 0.30035(16) 0.0281(4) Uani 1 1 d . . . H13 H -0.7483 0.3125 0.3470 0.034 Uiso 1 1 calc R . . C14 C -0.85852(15) 0.10588(12) 0.06567(16) 0.0289(4) Uani 1 1 d . . . C15 C 0.23563(18) -0.03237(12) 0.79674(18) 0.0338(4) Uani 1 1 d . . . H15 H 0.2703 -0.0052 0.8679 0.041 Uiso 1 1 calc R . . C16 C 0.3051(2) -0.06750(14) 0.7413(2) 0.0433(5) Uani 1 1 d . . . H16 H 0.3851 -0.0637 0.7739 0.052 Uiso 1 1 calc R . . C17 C 0.2531(2) -0.10839(16) 0.6365(2) 0.0526(6) Uani 1 1 d . . . H17 H 0.2978 -0.1332 0.5974 0.063 Uiso 1 1 calc R . . C18 C 0.1348(2) -0.11229(15) 0.5901(2) 0.0482(6) Uani 1 1 d . . . H18 H 0.0988 -0.1394 0.5190 0.058 Uiso 1 1 calc R . . C19 C 0.06906(18) -0.07555(12) 0.64967(17) 0.0331(4) Uani 1 1 d . . . C20 C -0.05964(18) -0.07586(12) 0.60345(16) 0.0343(4) Uani 1 1 d . . . C21 C -0.1227(2) -0.11781(17) 0.5008(2) 0.0573(7) Uani 1 1 d . . . H21 H -0.0853 -0.1474 0.4581 0.069 Uiso 1 1 calc R . . C22 C -0.2414(2) -0.11490(18) 0.4634(2) 0.0652(8) Uani 1 1 d . . . H22 H -0.2848 -0.1430 0.3952 0.078 Uiso 1 1 calc R . . C23 C -0.2952(2) -0.07073(16) 0.5266(2) 0.0525(6) Uani 1 1 d . . . H23 H -0.3753 -0.0679 0.5021 0.063 Uiso 1 1 calc R . . C24 C -0.22761(19) -0.03044(13) 0.62766(19) 0.0397(5) Uani 1 1 d . . . H24 H -0.2637 -0.0005 0.6713 0.048 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 0.02335(7) 0.03045(8) 0.02010(7) -0.00265(5) 0.00377(5) -0.00069(5) S1 0.0237(2) 0.0279(2) 0.0254(2) -0.00028(17) 0.00337(17) 0.00059(17) O1 0.0382(8) 0.0485(9) 0.0272(7) 0.0051(6) 0.0101(6) 0.0140(7) O2 0.0251(7) 0.0441(9) 0.0569(10) 0.0103(7) 0.0089(7) 0.0030(6) O3 0.0276(7) 0.0344(7) 0.0389(8) 0.0033(6) 0.0054(6) -0.0053(6) O4 0.0329(7) 0.0625(10) 0.0323(8) -0.0209(7) 0.0060(6) -0.0065(7) O5 0.0333(7) 0.0339(7) 0.0411(8) -0.0090(6) 0.0076(6) 0.0047(6) O6 0.0371(8) 0.0435(8) 0.0376(8) 0.0096(6) 0.0099(6) -0.0029(6) N1 0.0347(9) 0.0331(9) 0.0246(8) -0.0018(6) 0.0038(7) -0.0037(7) N2 0.0335(8) 0.0280(8) 0.0249(8) -0.0022(6) 0.0094(7) -0.0009(7) C1 0.0282(9) 0.0306(10) 0.0298(10) -0.0053(8) 0.0023(8) 0.0029(8) C2 0.0259(9) 0.0303(10) 0.0251(9) -0.0039(7) 0.0045(7) 0.0021(7) C3 0.0298(9) 0.0369(10) 0.0288(10) 0.0051(8) 0.0100(8) 0.0011(8) C4 0.0224(8) 0.0396(11) 0.0324(10) 0.0020(8) 0.0094(8) -0.0013(8) C5 0.0237(8) 0.0279(9) 0.0222(8) -0.0032(7) 0.0045(7) 0.0013(7) C6 0.0271(9) 0.0288(10) 0.0306(10) -0.0006(7) 0.0091(8) -0.0021(7) C7 0.0200(8) 0.0308(10) 0.0339(10) -0.0036(8) 0.0064(7) -0.0022(7) C8 0.0219(8) 0.0310(9) 0.0177(8) -0.0002(7) 0.0011(6) 0.0010(7) C9 0.0196(8) 0.0443(11) 0.0293(10) -0.0061(8) 0.0056(7) 0.0016(8) C10 0.0283(9) 0.0430(11) 0.0265(9) -0.0097(8) 0.0081(8) 0.0016(8) C11 0.0263(8) 0.0307(9) 0.0195(8) -0.0007(7) 0.0038(7) -0.0006(7) C12 0.0223(8) 0.0336(10) 0.0291(9) 0.0005(8) 0.0080(7) 0.0000(7) C13 0.0276(9) 0.0312(10) 0.0267(9) -0.0039(7) 0.0109(7) 0.0014(7) C14 0.0266(9) 0.0287(9) 0.0248(9) 0.0007(7) 0.0006(7) -0.0005(7) C15 0.0349(10) 0.0310(10) 0.0352(11) -0.0037(8) 0.0118(9) -0.0025(8) C16 0.0385(11) 0.0392(12) 0.0555(14) -0.0048(10) 0.0205(11) 0.0014(9) C17 0.0597(15) 0.0499(14) 0.0592(15) -0.0148(12) 0.0347(13) 0.0035(12) C18 0.0582(14) 0.0493(13) 0.0390(12) -0.0162(10) 0.0193(11) 0.0019(11) C19 0.0449(11) 0.0273(10) 0.0262(9) -0.0042(7) 0.0114(8) -0.0015(8) C20 0.0440(11) 0.0301(10) 0.0237(9) -0.0045(8) 0.0050(8) -0.0034(9) C21 0.0591(15) 0.0612(16) 0.0411(13) -0.0260(12) 0.0043(12) -0.0043(13) C22 0.0601(16) 0.0706(18) 0.0447(14) -0.0274(13) -0.0072(12) -0.0092(14) C23 0.0407(12) 0.0509(14) 0.0480(14) -0.0038(11) -0.0071(11) -0.0073(11) C24 0.0361(11) 0.0399(12) 0.0347(11) -0.0015(9) 0.0018(9) -0.0047(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O4 2.2368(14) 1_656 ? Cd1 O1 2.2615(14) . ? Cd1 O3 2.2931(14) 3_456 ? Cd1 N2 2.3163(16) . ? Cd1 N1 2.4020(16) . ? Cd1 O2 2.5420(15) . ? S1 O6 1.4346(15) . ? S1 O5 1.4352(15) . ? S1 C5 1.7666(18) . ? S1 C8 1.7743(18) . ? O1 C1 1.261(2) . ? O2 C1 1.250(2) . ? O3 C14 1.259(2) . ? O3 Cd1 2.2931(14) 3_456 ? O4 C14 1.250(2) . ? O4 Cd1 2.2368(14) 1_454 ? N1 C20 1.334(3) . ? N1 C24 1.336(3) . ? N2 C15 1.339(3) . ? N2 C19 1.346(2) . ? C1 C2 1.508(2) . ? C2 C7 1.385(3) . ? C2 C3 1.401(3) . ? C3 C4 1.379(3) . ? C3 H3 0.9300 . ? C4 C5 1.388(3) . ? C4 H4 0.9300 . ? C5 C6 1.387(2) . ? C6 C7 1.389(3) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.386(3) . ? C8 C13 1.395(2) . ? C9 C10 1.385(3) . ? C9 H9 0.9300 . ? C10 C11 1.397(3) . ? C10 H10 0.9300 . ? C11 C12 1.390(3) . ? C11 C14 1.507(2) . ? C12 C13 1.388(2) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C16 1.379(3) . ? C15 H15 0.9300 . ? C16 C17 1.376(3) . ? C16 H16 0.9300 . ? C17 C18 1.374(4) . ? C17 H17 0.9300 . ? C18 C19 1.389(3) . ? C18 H18 0.9300 . ? C19 C20 1.491(3) . ? C20 C21 1.390(3) . ? C21 C22 1.377(4) . ? C21 H21 0.9300 . ? C22 C23 1.365(4) . ? C22 H22 0.9300 . ? C23 C24 1.380(3) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cd1 O1 112.82(6) 1_656 . ? O4 Cd1 O3 105.36(6) 1_656 3_456 ? O1 Cd1 O3 105.46(5) . 3_456 ? O4 Cd1 N2 89.71(6) 1_656 . ? O1 Cd1 N2 139.87(5) . . ? O3 Cd1 N2 99.36(5) 3_456 . ? O4 Cd1 N1 158.85(6) 1_656 . ? O1 Cd1 N1 82.25(6) . . ? O3 Cd1 N1 83.44(5) 3_456 . ? N2 Cd1 N1 69.69(6) . . ? O4 Cd1 O2 95.51(6) 1_656 . ? O1 Cd1 O2 54.48(5) . . ? O3 Cd1 O2 156.08(5) 3_456 . ? N2 Cd1 O2 92.19(5) . . ? N1 Cd1 O2 81.03(5) . . ? O6 S1 O5 119.16(9) . . ? O6 S1 C5 108.62(9) . . ? O5 S1 C5 107.64(9) . . ? O6 S1 C8 107.45(9) . . ? O5 S1 C8 107.94(9) . . ? C5 S1 C8 105.19(8) . . ? C1 O1 Cd1 96.24(11) . . ? C1 O2 Cd1 83.67(12) . . ? C14 O3 Cd1 127.39(12) . 3_456 ? C14 O4 Cd1 108.30(12) . 1_454 ? C20 N1 C24 119.30(18) . . ? C20 N1 Cd1 117.15(13) . . ? C24 N1 Cd1 123.46(14) . . ? C15 N2 C19 119.23(17) . . ? C15 N2 Cd1 121.08(13) . . ? C19 N2 Cd1 119.64(13) . . ? O2 C1 O1 123.63(18) . . ? O2 C1 C2 118.48(18) . . ? O1 C1 C2 117.62(17) . . ? C7 C2 C3 119.88(17) . . ? C7 C2 C1 121.47(17) . . ? C3 C2 C1 118.47(17) . . ? C4 C3 C2 119.98(18) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 119.16(17) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 121.86(17) . . ? C6 C5 S1 120.21(14) . . ? C4 C5 S1 117.80(14) . . ? C5 C6 C7 118.39(17) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? C2 C7 C6 120.71(17) . . ? C2 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C9 C8 C13 121.04(16) . . ? C9 C8 S1 118.79(14) . . ? C13 C8 S1 119.68(14) . . ? C10 C9 C8 119.67(17) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 119.89(17) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 119.88(17) . . ? C12 C11 C14 120.67(16) . . ? C10 C11 C14 119.41(16) . . ? C13 C12 C11 120.51(17) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C8 118.88(16) . . ? C12 C13 H13 120.6 . . ? C8 C13 H13 120.6 . . ? O4 C14 O3 123.77(17) . . ? O4 C14 C11 117.08(17) . . ? O3 C14 C11 119.12(17) . . ? N2 C15 C16 122.7(2) . . ? N2 C15 H15 118.7 . . ? C16 C15 H15 118.7 . . ? C17 C16 C15 118.3(2) . . ? C17 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? C18 C17 C16 119.5(2) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 119.7(2) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? N2 C19 C18 120.6(2) . . ? N2 C19 C20 116.79(17) . . ? C18 C19 C20 122.59(18) . . ? N1 C20 C21 121.0(2) . . ? N1 C20 C19 116.62(16) . . ? C21 C20 C19 122.3(2) . . ? C22 C21 C20 119.0(2) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C23 C22 C21 119.9(2) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 118.2(2) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 120.9 . . ? N1 C24 C23 122.5(2) . . ? N1 C24 H24 118.7 . . ? C23 C24 H24 118.7 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.621 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.058 # Attachment '4.cif' data_f:\lfy\1\jiegou\0213g\1 _database_code_depnum_ccdc_archive 'CCDC 650350' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H25 Cd1.50 N2 O12 S2' _chemical_formula_sum 'C38 H25 Cd1.50 N2 O12 S2' _chemical_formula_weight 934.32 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 '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 10.940(2) _cell_length_b 13.527(3) _cell_length_c 13.633(3) _cell_angle_alpha 106.1730(10) _cell_angle_beta 106.438(2) _cell_angle_gamma 102.124(2) _cell_volume 1764.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4810 _cell_measurement_theta_min 2.0446 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 934 _exptl_absorpt_coefficient_mu 1.101 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6671 _exptl_absorpt_correction_T_max 0.7703 _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 'Mercury CCD' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 13463 _diffrn_reflns_av_R_equivalents 0.0117 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7904 _reflns_number_gt 7262 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL-97 (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+1.8355P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7904 _refine_ls_number_parameters 502 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0830 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.0000 0.0000 0.0000 0.02719(7) Uani 1 2 d S . . Cd2 Cd -0.151428(17) -0.012621(13) 0.194519(13) 0.02515(6) Uani 1 1 d . . . S1 S 0.47036(7) 0.70053(5) 0.26652(6) 0.03755(16) Uani 1 1 d . . . S2 S 0.69831(6) 0.39117(6) 0.43596(6) 0.03496(14) Uani 1 1 d . . . O1 O 0.1073(2) 0.17314(14) 0.04474(16) 0.0367(4) Uani 1 1 d . . . O2 O 0.2414(2) 0.17517(15) -0.05261(16) 0.0403(4) Uani 1 1 d . . . O3 O 0.1650(2) 0.94582(18) -0.05007(18) 0.0436(5) Uani 1 1 d . . . O4 O 0.3163(2) 0.92195(19) -0.12190(17) 0.0458(5) Uani 1 1 d . . . O5 O 0.4275(3) 0.73536(17) 0.35712(17) 0.0578(7) Uani 1 1 d . . . O6 O 0.6106(2) 0.71562(17) 0.2857(2) 0.0606(7) Uani 1 1 d . . . O7 O 0.08338(18) 0.01820(14) 0.17793(14) 0.0320(4) Uani 1 1 d . . . O8 O 0.0429(2) 0.13937(16) 0.30053(16) 0.0407(4) Uani 1 1 d . . . O9 O 0.9215(3) 0.5587(3) 0.0836(3) 0.0749(9) Uani 1 1 d . . . O10 O 0.9645(3) 0.4018(2) 0.0510(2) 0.0679(7) Uani 1 1 d . . . O11 O 0.7079(2) 0.49571(18) 0.50653(19) 0.0507(5) Uani 1 1 d . . . O12 O 0.7697(2) 0.3275(2) 0.4820(2) 0.0522(6) Uani 1 1 d . . . N1 N -0.2437(2) -0.00253(17) 0.32920(17) 0.0303(4) Uani 1 1 d . . . N2 N -0.0756(2) -0.11717(18) 0.29489(18) 0.0323(4) Uani 1 1 d . . . C1 C -0.3251(3) 0.0566(2) 0.3447(3) 0.0416(6) Uani 1 1 d . . . H1 H -0.3536 0.0889 0.2942 0.050 Uiso 1 1 calc R . . C2 C -0.3693(3) 0.0722(3) 0.4317(3) 0.0471(7) Uani 1 1 d . . . H2 H -0.4258 0.1139 0.4398 0.057 Uiso 1 1 calc R . . C3 C -0.3270(3) 0.0241(3) 0.5056(3) 0.0458(7) Uani 1 1 d . . . H3 H -0.3538 0.0335 0.5656 0.055 Uiso 1 1 calc R . . C4 C -0.2442(3) -0.0383(2) 0.4901(2) 0.0395(6) Uani 1 1 d . . . H4 H -0.2161 -0.0723 0.5390 0.047 Uiso 1 1 calc R . . C5 C -0.2031(2) -0.04997(19) 0.40113(19) 0.0272(5) Uani 1 1 d . . . C6 C -0.1140(2) -0.1166(2) 0.38015(19) 0.0278(5) Uani 1 1 d . . . C7 C -0.0752(3) -0.1769(2) 0.4438(2) 0.0392(6) Uani 1 1 d . . . H7 H -0.1026 -0.1754 0.5027 0.047 Uiso 1 1 calc R . . C8 C 0.0048(3) -0.2391(3) 0.4182(3) 0.0470(7) Uani 1 1 d . . . H8 H 0.0317 -0.2801 0.4597 0.056 Uiso 1 1 calc R . . C9 C 0.0441(3) -0.2397(3) 0.3310(3) 0.0491(7) Uani 1 1 d . . . H9 H 0.0981 -0.2808 0.3127 0.059 Uiso 1 1 calc R . . C10 C 0.0019(3) -0.1780(3) 0.2711(3) 0.0444(7) Uani 1 1 d . . . H10 H 0.0282 -0.1786 0.2118 0.053 Uiso 1 1 calc R . . C11 C 0.2000(2) 0.21866(19) 0.0199(2) 0.0285(5) Uani 1 1 d . . . C12 C 0.2675(2) 0.33875(19) 0.0835(2) 0.0279(5) Uani 1 1 d . . . C13 C 0.2446(3) 0.3910(2) 0.1764(2) 0.0346(6) Uani 1 1 d . . . H13 H 0.1892 0.3511 0.2019 0.042 Uiso 1 1 calc R . . C14 C 0.3032(3) 0.5021(2) 0.2320(2) 0.0378(6) Uani 1 1 d . . . H14 H 0.2870 0.5369 0.2940 0.045 Uiso 1 1 calc R . . C15 C 0.3860(3) 0.56006(19) 0.1936(2) 0.0317(5) Uani 1 1 d . . . C16 C 0.4106(4) 0.5089(2) 0.1012(3) 0.0536(9) Uani 1 1 d . . . H16 H 0.4669 0.5487 0.0763 0.064 Uiso 1 1 calc R . . C17 C 0.3510(4) 0.3987(2) 0.0465(3) 0.0511(8) Uani 1 1 d . . . H17 H 0.3670 0.3642 -0.0157 0.061 Uiso 1 1 calc R . . C18 C 0.4124(3) 0.76439(19) 0.1733(2) 0.0309(5) Uani 1 1 d . . . C19 C 0.2945(3) 0.7893(3) 0.1657(3) 0.0448(7) Uani 1 1 d . . . H19 H 0.2475 0.7735 0.2095 0.054 Uiso 1 1 calc R . . C20 C 0.2473(3) 0.8378(3) 0.0923(3) 0.0438(7) Uani 1 1 d . . . H20 H 0.1676 0.8540 0.0862 0.053 Uiso 1 1 calc R . . C21 C 0.3182(3) 0.86247(19) 0.0277(2) 0.0286(5) Uani 1 1 d . . . C22 C 0.4379(3) 0.8387(2) 0.0376(2) 0.0355(6) Uani 1 1 d . . . H22 H 0.4859 0.8553 -0.0052 0.043 Uiso 1 1 calc R . . C23 C 0.4856(3) 0.7902(2) 0.1114(2) 0.0371(6) Uani 1 1 d . . . H23 H 0.5663 0.7753 0.1190 0.045 Uiso 1 1 calc R . . C24 C 0.2644(3) 0.9132(2) -0.0536(2) 0.0305(5) Uani 1 1 d . . . C25 C 0.9176(3) 0.4699(3) 0.0977(3) 0.0465(7) Uani 1 1 d . . . C26 C 0.8564(3) 0.4473(3) 0.1773(3) 0.0429(6) Uani 1 1 d . . . C27 C 0.7816(3) 0.5099(3) 0.2151(3) 0.0516(8) Uani 1 1 d . . . H27 H 0.7671 0.5648 0.1892 0.062 Uiso 1 1 calc R . . C28 C 0.7292(3) 0.4899(3) 0.2911(3) 0.0482(7) Uani 1 1 d . . . H28 H 0.6786 0.5309 0.3166 0.058 Uiso 1 1 calc R . . C29 C 0.7527(3) 0.4081(2) 0.3293(2) 0.0368(6) Uani 1 1 d . . . C30 C 0.8264(3) 0.3451(2) 0.2913(3) 0.0462(7) Uani 1 1 d . . . H30 H 0.8413 0.2904 0.3174 0.055 Uiso 1 1 calc R . . C31 C 0.8770(3) 0.3646(3) 0.2147(3) 0.0488(7) Uani 1 1 d . . . H31 H 0.9254 0.3222 0.1878 0.059 Uiso 1 1 calc R . . C32 C 0.5257(2) 0.3127(2) 0.3731(2) 0.0298(5) Uani 1 1 d . . . C33 C 0.4435(3) 0.3389(2) 0.4297(2) 0.0339(5) Uani 1 1 d . . . H33 H 0.4761 0.4000 0.4934 0.041 Uiso 1 1 calc R . . C34 C 0.3111(3) 0.2727(2) 0.3901(2) 0.0330(5) Uani 1 1 d . . . H34 H 0.2543 0.2902 0.4269 0.040 Uiso 1 1 calc R . . C35 C 0.2634(2) 0.18073(19) 0.29617(19) 0.0280(5) Uani 1 1 d . . . C36 C 0.3476(3) 0.1560(2) 0.2391(2) 0.0321(5) Uani 1 1 d . . . H36 H 0.3154 0.0946 0.1758 0.039 Uiso 1 1 calc R . . C37 C 0.4788(3) 0.2227(2) 0.2766(2) 0.0333(5) Uani 1 1 d . . . H37 H 0.5345 0.2078 0.2379 0.040 Uiso 1 1 calc R . . C38 C 0.1201(3) 0.1092(2) 0.25534(19) 0.0297(5) Uani 1 1 d . . . H9A H 0.9635 0.5787 0.0431 0.036 Uiso 1 1 d 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 0.03091(13) 0.02361(12) 0.02525(12) 0.00938(9) 0.01172(10) 0.00213(10) Cd2 0.02874(10) 0.02426(10) 0.02522(9) 0.01112(7) 0.01279(7) 0.00671(7) S1 0.0430(4) 0.0188(3) 0.0341(3) 0.0084(2) -0.0043(3) 0.0032(3) S2 0.0252(3) 0.0343(3) 0.0393(3) 0.0109(3) 0.0076(3) 0.0059(3) O1 0.0398(10) 0.0226(8) 0.0435(10) 0.0105(8) 0.0182(9) -0.0006(8) O2 0.0480(11) 0.0251(9) 0.0396(10) 0.0030(8) 0.0210(9) 0.0001(8) O3 0.0469(12) 0.0528(12) 0.0530(12) 0.0350(10) 0.0240(10) 0.0294(10) O4 0.0585(13) 0.0567(13) 0.0443(11) 0.0325(10) 0.0301(10) 0.0264(11) O5 0.103(2) 0.0311(11) 0.0263(10) 0.0070(8) 0.0118(11) 0.0171(12) O6 0.0349(11) 0.0331(11) 0.0843(18) 0.0237(11) -0.0147(11) -0.0009(9) O7 0.0361(9) 0.0260(9) 0.0258(8) 0.0092(7) 0.0062(7) 0.0011(7) O8 0.0348(10) 0.0412(11) 0.0350(10) 0.0049(8) 0.0156(8) -0.0020(8) O9 0.106(2) 0.0772(19) 0.088(2) 0.0526(17) 0.068(2) 0.0450(18) O10 0.083(2) 0.0656(17) 0.0769(18) 0.0308(15) 0.0493(16) 0.0318(15) O11 0.0395(11) 0.0390(11) 0.0539(13) -0.0018(10) 0.0158(10) 0.0000(9) O12 0.0366(11) 0.0683(15) 0.0590(14) 0.0353(12) 0.0113(10) 0.0223(11) N1 0.0341(11) 0.0322(11) 0.0296(10) 0.0135(9) 0.0167(9) 0.0101(9) N2 0.0366(11) 0.0350(11) 0.0338(11) 0.0181(9) 0.0174(9) 0.0142(9) C1 0.0499(17) 0.0440(16) 0.0469(16) 0.0227(13) 0.0286(14) 0.0229(13) C2 0.0521(18) 0.0478(17) 0.0573(19) 0.0208(15) 0.0366(16) 0.0217(15) C3 0.0519(18) 0.0487(17) 0.0426(16) 0.0139(13) 0.0319(14) 0.0104(14) C4 0.0482(16) 0.0417(15) 0.0301(13) 0.0152(11) 0.0192(12) 0.0070(13) C5 0.0262(11) 0.0253(11) 0.0240(11) 0.0075(9) 0.0081(9) -0.0010(9) C6 0.0242(11) 0.0271(11) 0.0260(11) 0.0104(9) 0.0051(9) 0.0002(9) C7 0.0361(14) 0.0481(16) 0.0390(14) 0.0268(13) 0.0119(12) 0.0116(12) C8 0.0407(16) 0.0503(18) 0.0580(19) 0.0352(16) 0.0121(14) 0.0170(14) C9 0.0475(17) 0.0478(17) 0.067(2) 0.0293(16) 0.0254(16) 0.0257(15) C10 0.0539(18) 0.0472(17) 0.0511(17) 0.0260(14) 0.0303(15) 0.0271(15) C11 0.0316(12) 0.0212(11) 0.0268(11) 0.0092(9) 0.0060(9) 0.0024(9) C12 0.0314(12) 0.0204(11) 0.0295(12) 0.0103(9) 0.0094(10) 0.0036(9) C13 0.0458(15) 0.0242(12) 0.0349(13) 0.0127(10) 0.0191(12) 0.0045(11) C14 0.0575(17) 0.0263(12) 0.0303(13) 0.0103(10) 0.0189(12) 0.0103(12) C15 0.0350(13) 0.0185(11) 0.0336(13) 0.0084(9) 0.0053(10) 0.0035(10) C16 0.068(2) 0.0240(13) 0.066(2) 0.0085(14) 0.0432(19) -0.0063(14) C17 0.070(2) 0.0249(13) 0.0582(19) 0.0050(13) 0.0445(18) -0.0015(14) C18 0.0336(13) 0.0208(11) 0.0368(13) 0.0126(10) 0.0081(10) 0.0093(10) C19 0.0538(18) 0.0552(18) 0.0570(18) 0.0398(16) 0.0357(15) 0.0317(15) C20 0.0461(16) 0.0587(18) 0.0611(19) 0.0425(16) 0.0353(15) 0.0346(15) C21 0.0326(12) 0.0249(11) 0.0333(12) 0.0135(10) 0.0148(10) 0.0108(10) C22 0.0346(13) 0.0366(14) 0.0469(15) 0.0218(12) 0.0227(12) 0.0142(11) C23 0.0288(13) 0.0336(13) 0.0525(16) 0.0194(12) 0.0148(12) 0.0116(11) C24 0.0355(13) 0.0245(11) 0.0324(12) 0.0125(10) 0.0121(10) 0.0082(10) C25 0.0376(16) 0.0538(18) 0.0450(17) 0.0182(14) 0.0143(13) 0.0086(13) C26 0.0337(14) 0.0435(16) 0.0481(16) 0.0167(13) 0.0135(13) 0.0069(12) C27 0.0521(19) 0.0547(19) 0.067(2) 0.0362(17) 0.0280(17) 0.0252(16) C28 0.0443(17) 0.0514(18) 0.065(2) 0.0289(16) 0.0271(15) 0.0258(15) C29 0.0284(12) 0.0344(14) 0.0446(15) 0.0136(12) 0.0122(11) 0.0059(11) C30 0.0474(17) 0.0366(15) 0.063(2) 0.0200(14) 0.0272(15) 0.0163(13) C31 0.0487(18) 0.0442(17) 0.060(2) 0.0201(15) 0.0256(15) 0.0166(14) C32 0.0265(11) 0.0273(12) 0.0346(12) 0.0137(10) 0.0082(10) 0.0071(9) C33 0.0325(13) 0.0284(12) 0.0322(13) 0.0053(10) 0.0106(10) 0.0015(10) C34 0.0332(13) 0.0306(12) 0.0303(12) 0.0059(10) 0.0147(10) 0.0026(10) C35 0.0292(12) 0.0269(12) 0.0251(11) 0.0123(9) 0.0072(9) 0.0032(9) C36 0.0328(13) 0.0290(12) 0.0288(12) 0.0066(10) 0.0079(10) 0.0080(10) C37 0.0293(12) 0.0338(13) 0.0359(13) 0.0101(11) 0.0118(10) 0.0115(10) C38 0.0315(12) 0.0310(12) 0.0235(11) 0.0134(10) 0.0077(9) 0.0018(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.2090(18) . ? Cd1 O1 2.2090(18) 2 ? Cd1 O7 2.2578(18) . ? Cd1 O7 2.2578(18) 2 ? Cd1 O3 2.288(2) 1_545 ? Cd1 O3 2.288(2) 2_565 ? Cd2 O2 2.2781(19) 2 ? Cd2 N1 2.318(2) . ? Cd2 N2 2.343(2) . ? Cd2 O3 2.366(2) 2_565 ? Cd2 O8 2.3674(19) . ? Cd2 O4 2.517(2) 2_565 ? Cd2 O7 2.5991(19) . ? S1 O5 1.437(3) . ? S1 O6 1.440(3) . ? S1 C15 1.773(2) . ? S1 C18 1.775(2) . ? S2 O12 1.433(2) . ? S2 O11 1.435(2) . ? S2 C29 1.772(3) . ? S2 C32 1.779(3) . ? O1 C11 1.253(3) . ? O2 C11 1.253(3) . ? O2 Cd2 2.2781(19) 2 ? O3 C24 1.265(3) . ? O3 Cd1 2.288(2) 1_565 ? O3 Cd2 2.366(2) 2_565 ? O4 C24 1.239(3) . ? O4 Cd2 2.517(2) 2_565 ? O7 C38 1.272(3) . ? O8 C38 1.249(3) . ? O9 C25 1.263(4) . ? O9 H9A 0.8739 . ? O10 C25 1.255(4) . ? N1 C1 1.337(3) . ? N1 C5 1.339(3) . ? N2 C10 1.342(4) . ? N2 C6 1.342(3) . ? C1 C2 1.383(4) . ? C1 H1 0.9300 . ? C2 C3 1.371(5) . ? C2 H2 0.9300 . ? C3 C4 1.382(4) . ? C3 H3 0.9300 . ? C4 C5 1.389(3) . ? C4 H4 0.9300 . ? C5 C6 1.492(4) . ? C6 C7 1.389(3) . ? C7 C8 1.384(4) . ? C7 H7 0.9300 . ? C8 C9 1.372(5) . ? C8 H8 0.9300 . ? C9 C10 1.381(4) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.512(3) . ? C12 C13 1.386(4) . ? C12 C17 1.387(4) . ? C13 C14 1.390(4) . ? C13 H13 0.9300 . ? C14 C15 1.381(4) . ? C14 H14 0.9300 . ? C15 C16 1.386(4) . ? C16 C17 1.379(4) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.380(4) . ? C18 C19 1.383(4) . ? C19 C20 1.384(4) . ? C19 H19 0.9300 . ? C20 C21 1.389(4) . ? C20 H20 0.9300 . ? C21 C22 1.392(4) . ? C21 C24 1.507(3) . ? C22 C23 1.389(4) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C25 C26 1.493(4) . ? C26 C31 1.386(4) . ? C26 C27 1.392(5) . ? C27 C28 1.380(5) . ? C27 H27 0.9300 . ? C28 C29 1.387(4) . ? C28 H28 0.9300 . ? C29 C30 1.387(4) . ? C30 C31 1.374(5) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.380(4) . ? C32 C37 1.393(4) . ? C33 C34 1.391(4) . ? C33 H33 0.9300 . ? C34 C35 1.386(3) . ? C34 H34 0.9300 . ? C35 C36 1.398(4) . ? C35 C38 1.508(3) . ? C36 C37 1.386(4) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O1 180.00(5) . 2 ? O1 Cd1 O7 89.66(7) . . ? O1 Cd1 O7 90.34(7) 2 . ? O1 Cd1 O7 90.34(7) . 2 ? O1 Cd1 O7 89.66(7) 2 2 ? O7 Cd1 O7 180.00(8) . 2 ? O1 Cd1 O3 92.68(8) . 1_545 ? O1 Cd1 O3 87.32(8) 2 1_545 ? O7 Cd1 O3 97.38(7) . 1_545 ? O7 Cd1 O3 82.62(7) 2 1_545 ? O1 Cd1 O3 87.32(8) . 2_565 ? O1 Cd1 O3 92.68(8) 2 2_565 ? O7 Cd1 O3 82.62(7) . 2_565 ? O7 Cd1 O3 97.38(7) 2 2_565 ? O3 Cd1 O3 180.00(11) 1_545 2_565 ? O2 Cd2 N1 113.90(7) 2 . ? O2 Cd2 N2 83.03(8) 2 . ? N1 Cd2 N2 70.76(8) . . ? O2 Cd2 O3 82.13(8) 2 2_565 ? N1 Cd2 O3 137.12(7) . 2_565 ? N2 Cd2 O3 152.05(7) . 2_565 ? O2 Cd2 O8 145.47(7) 2 . ? N1 Cd2 O8 96.63(7) . . ? N2 Cd2 O8 92.79(8) . . ? O3 Cd2 O8 86.25(8) 2_565 . ? O2 Cd2 O4 97.97(8) 2 2_565 ? N1 Cd2 O4 84.62(7) . 2_565 ? N2 Cd2 O4 153.17(7) . 2_565 ? O3 Cd2 O4 53.04(7) 2_565 2_565 ? O8 Cd2 O4 100.70(8) . 2_565 ? O2 Cd2 O7 92.95(6) 2 . ? N1 Cd2 O7 138.88(7) . . ? N2 Cd2 O7 83.09(7) . . ? O3 Cd2 O7 74.20(6) 2_565 . ? O8 Cd2 O7 52.54(6) . . ? O4 Cd2 O7 123.46(6) 2_565 . ? O5 S1 O6 120.12(17) . . ? O5 S1 C15 108.58(14) . . ? O6 S1 C15 106.30(13) . . ? O5 S1 C18 108.18(13) . . ? O6 S1 C18 107.54(14) . . ? C15 S1 C18 105.16(12) . . ? O12 S2 O11 118.87(15) . . ? O12 S2 C29 107.20(14) . . ? O11 S2 C29 108.38(14) . . ? O12 S2 C32 107.34(13) . . ? O11 S2 C32 107.74(13) . . ? C29 S2 C32 106.72(13) . . ? C11 O1 Cd1 131.37(17) . . ? C11 O2 Cd2 131.68(17) . 2 ? C24 O3 Cd1 165.01(18) . 1_565 ? C24 O3 Cd2 95.95(16) . 2_565 ? Cd1 O3 Cd2 98.46(7) 1_565 2_565 ? C24 O4 Cd2 89.52(16) . 2_565 ? C38 O7 Cd1 121.98(15) . . ? C38 O7 Cd2 86.90(15) . . ? Cd1 O7 Cd2 92.80(6) . . ? C38 O8 Cd2 98.27(16) . . ? C25 O9 H9A 120.7 . . ? C1 N1 C5 118.5(2) . . ? C1 N1 Cd2 123.16(18) . . ? C5 N1 Cd2 117.98(16) . . ? C10 N2 C6 118.7(2) . . ? C10 N2 Cd2 123.87(18) . . ? C6 N2 Cd2 117.44(17) . . ? N1 C1 C2 123.5(3) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 117.9(3) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C2 C3 C4 119.4(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.6(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N1 C5 C4 121.1(2) . . ? N1 C5 C6 116.9(2) . . ? C4 C5 C6 122.0(2) . . ? N2 C6 C7 121.6(2) . . ? N2 C6 C5 116.5(2) . . ? C7 C6 C5 121.9(2) . . ? C8 C7 C6 119.0(3) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C9 C8 C7 119.4(3) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 118.7(3) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? N2 C10 C9 122.7(3) . . ? N2 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? O1 C11 O2 126.8(2) . . ? O1 C11 C12 116.4(2) . . ? O2 C11 C12 116.9(2) . . ? C13 C12 C17 119.2(2) . . ? C13 C12 C11 121.3(2) . . ? C17 C12 C11 119.5(2) . . ? C12 C13 C14 120.9(2) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C14 C13 118.8(2) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C14 C15 C16 120.9(2) . . ? C14 C15 S1 120.3(2) . . ? C16 C15 S1 118.7(2) . . ? C17 C16 C15 119.6(3) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C12 120.5(3) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? C23 C18 C19 121.1(2) . . ? C23 C18 S1 120.2(2) . . ? C19 C18 S1 118.7(2) . . ? C18 C19 C20 119.3(3) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C19 C20 C21 120.4(3) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C22 119.6(2) . . ? C20 C21 C24 120.0(2) . . ? C22 C21 C24 120.4(2) . . ? C23 C22 C21 120.0(2) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C18 C23 C22 119.5(2) . . ? C18 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? O4 C24 O3 121.5(2) . . ? O4 C24 C21 120.5(2) . . ? O3 C24 C21 118.0(2) . . ? O10 C25 O9 123.9(3) . . ? O10 C25 C26 118.9(3) . . ? O9 C25 C26 117.2(3) . . ? C31 C26 C27 120.4(3) . . ? C31 C26 C25 119.2(3) . . ? C27 C26 C25 120.3(3) . . ? C28 C27 C26 119.5(3) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 119.4(3) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C30 C29 C28 121.3(3) . . ? C30 C29 S2 119.5(2) . . ? C28 C29 S2 119.1(2) . . ? C31 C30 C29 119.0(3) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C30 C31 C26 120.4(3) . . ? C30 C31 H31 119.8 . . ? C26 C31 H31 119.8 . . ? C33 C32 C37 121.7(2) . . ? C33 C32 S2 116.8(2) . . ? C37 C32 S2 121.2(2) . . ? C32 C33 C34 119.0(2) . . ? C32 C33 H33 120.5 . . ? C34 C33 H33 120.5 . . ? C35 C34 C33 120.3(2) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 119.9(2) . . ? C34 C35 C38 119.6(2) . . ? C36 C35 C38 120.5(2) . . ? C37 C36 C35 120.2(2) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C32 118.8(2) . . ? C36 C37 H37 120.6 . . ? C32 C37 H37 120.6 . . ? O8 C38 O7 122.3(2) . . ? O8 C38 C35 119.2(2) . . ? O7 C38 C35 118.5(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 O9 H9A O10 0.87 1.73 2.602(4) 171.3 2_765 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.056 _refine_diff_density_min -1.259 _refine_diff_density_rms 0.080 # Attachment '5.cif' data_compound5 _database_code_depnum_ccdc_archive 'CCDC 650351' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C69 H46 Cd4 N2 O24 S4' _chemical_formula_sum 'C69 H46 Cd4 N2 O24 S4' _chemical_formula_weight 1864.92 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.887(4) _cell_length_b 12.971(4) _cell_length_c 23.254(9) _cell_angle_alpha 74.358(15) _cell_angle_beta 75.948(14) _cell_angle_gamma 60.853(12) _cell_volume 3240.4(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5677 _cell_measurement_theta_min 2.1482 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.911 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1844 _exptl_absorpt_coefficient_mu 1.512 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7520 _exptl_absorpt_correction_T_max 0.9283 _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 'Mercury CCD' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 24780 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.1563 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.48 _reflns_number_total 14469 _reflns_number_gt 6332 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL-97 (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1220P)^2^+26.7801P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14469 _refine_ls_number_parameters 919 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1653 _refine_ls_R_factor_gt 0.0928 _refine_ls_wR_factor_ref 0.3124 _refine_ls_wR_factor_gt 0.2740 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.20819(10) 0.84418(9) 0.43518(4) 0.0255(3) Uani 1 1 d . . . S1 S 0.4655(3) 0.1110(3) 0.37099(18) 0.0286(8) Uani 1 1 d . . . O1 O 0.2752(11) 0.6767(9) 0.3945(5) 0.035(3) Uani 1 1 d . . . N1 N 0.2363(11) 0.7597(11) 0.5315(5) 0.033(3) Uani 1 1 d . . . C1 C 0.2817(12) 0.6495(11) 0.3465(7) 0.025(3) Uani 1 1 d . . . Cd2 Cd 0.24830(9) 0.90304(9) 0.28840(5) 0.0246(3) Uani 1 1 d . . . S2 S 0.9628(3) 0.5336(3) 0.11777(18) 0.0303(8) Uani 1 1 d . . . O2 O 0.2638(10) 0.7154(9) 0.2955(4) 0.028(2) Uani 1 1 d . . . N2 N 0.2458(12) 0.7933(12) 0.9656(6) 0.035(3) Uani 1 1 d . . . C2 C 0.3272(13) 0.5127(12) 0.3513(6) 0.026(3) Uani 1 1 d . . . Cd3 Cd 0.17193(10) 0.74345(9) 0.21462(5) 0.0250(3) Uani 1 1 d . . . S3 S -0.5733(3) 1.0201(3) 0.13390(18) 0.0297(8) Uani 1 1 d . . . O3 O 1.0211(11) -0.1142(11) 0.4418(6) 0.046(3) Uani 1 1 d . . . C3 C 0.3788(15) 0.4597(13) 0.3020(6) 0.032(4) Uani 1 1 d . . . H3 H 0.3822 0.5066 0.2642 0.039 Uiso 1 1 calc R . . Cd4 Cd 0.20924(10) 0.80179(9) 0.06485(5) 0.0253(3) Uani 1 1 d . . . S4 S -0.0091(3) 0.6307(3) 0.36457(17) 0.0256(8) Uani 1 1 d . . . O4 O 1.0600(11) -0.0691(12) 0.3415(6) 0.052(3) Uani 1 1 d . . . C4 C 0.4275(16) 0.3338(14) 0.3076(7) 0.039(4) Uani 1 1 d . . . H4 H 0.4700 0.2959 0.2747 0.046 Uiso 1 1 calc R . . O5 O 0.4056(9) 0.0733(8) 0.4274(5) 0.040(3) Uani 1 1 d . . . C5 C 0.4097(13) 0.2687(11) 0.3639(7) 0.027(3) Uani 1 1 d . . . O6 O 0.4565(10) 0.0882(9) 0.3151(6) 0.041(3) Uani 1 1 d . . . C6 C 0.3541(13) 0.3209(14) 0.4141(7) 0.030(3) Uani 1 1 d . . . H6 H 0.3439 0.2755 0.4516 0.036 Uiso 1 1 calc R . . O7 O 0.3680(9) 0.7153(10) 0.1682(5) 0.039(3) Uani 1 1 d . . . C7 C 0.3127(14) 0.4463(12) 0.4070(7) 0.031(3) Uani 1 1 d . . . H7 H 0.2754 0.4840 0.4403 0.038 Uiso 1 1 calc R . . O8 O 0.3962(9) 0.7516(9) 0.0683(5) 0.036(3) Uani 1 1 d . . . C8 C 0.6173(12) 0.0546(11) 0.3766(6) 0.023(3) Uani 1 1 d . . . O9 O 1.1546(9) -0.0686(8) 0.2100(4) 0.027(2) Uani 1 1 d . . . C9 C 0.7025(14) 0.0286(14) 0.3263(7) 0.030(3) Uani 1 1 d . . . H9 H 0.6786 0.0402 0.2894 0.036 Uiso 1 1 calc R . . O10 O 1.1552(11) -0.0422(9) 0.1110(5) 0.035(3) Uani 1 1 d . . . C10 C 0.8248(12) -0.0152(11) 0.3300(7) 0.028(3) Uani 1 1 d . . . H10 H 0.8813 -0.0310 0.2959 0.034 Uiso 1 1 calc R . . O11 O 1.0137(9) 0.5669(10) 0.0592(5) 0.040(3) Uani 1 1 d . . . C11 C 0.8595(14) -0.0346(11) 0.3853(7) 0.028(3) Uani 1 1 d . . . O12 O 0.9779(12) 0.5642(11) 0.1690(5) 0.044(3) Uani 1 1 d . . . C12 C 0.7736(12) -0.0138(13) 0.4368(7) 0.027(3) Uani 1 1 d . . . H12 H 0.7986 -0.0324 0.4742 0.032 Uiso 1 1 calc R . . O13 O 0.0136(10) 0.8595(11) 0.0765(5) 0.042(3) Uani 1 1 d . . . C13 C 0.6514(14) 0.0340(14) 0.4333(7) 0.033(4) Uani 1 1 d . . . H13 H 0.5946 0.0516 0.4673 0.040 Uiso 1 1 calc R . . O14 O -0.0057(10) 0.8310(10) 0.1773(5) 0.040(3) Uani 1 1 d . . . C14 C 0.9897(16) -0.0755(18) 0.3890(8) 0.047(5) Uani 1 1 d . . . O15 O -0.7542(13) 1.6108(10) 0.0931(5) 0.046(3) Uani 1 1 d . . . C15 C 0.4286(14) 0.7200(12) 0.1196(7) 0.029(3) Uani 1 1 d . . . O16 O -0.7771(10) 1.5688(10) 0.1939(5) 0.039(3) Uani 1 1 d . . . C16 C 0.5623(14) 0.6756(14) 0.1203(7) 0.032(3) Uani 1 1 d . . . O17 O -0.5920(12) 1.0087(10) 0.0789(5) 0.045(3) Uani 1 1 d . . . C17 C 0.6436(14) 0.6233(14) 0.0717(6) 0.031(3) Uani 1 1 d . . . H17 H 0.6155 0.6165 0.0403 0.037 Uiso 1 1 calc R . . O18 O -0.6171(10) 0.9630(9) 0.1902(5) 0.039(3) Uani 1 1 d . . . C18 C 0.7654(14) 0.5821(15) 0.0706(6) 0.037(4) Uani 1 1 d . . . H18 H 0.8194 0.5473 0.0387 0.044 Uiso 1 1 calc R . . O19 O 0.1965(10) 0.0726(8) 0.3184(5) 0.032(2) Uani 1 1 d . . . C19 C 0.8059(14) 0.5930(12) 0.1172(7) 0.028(3) Uani 1 1 d . . . O20 O 0.1554(10) 0.0384(9) 0.4193(5) 0.035(3) Uani 1 1 d . . . C20 C 0.7248(14) 0.6451(14) 0.1648(8) 0.036(4) Uani 1 1 d . . . H20 H 0.7526 0.6534 0.1958 0.043 Uiso 1 1 calc R . . O21 O -0.5669(10) 0.8131(10) 0.3131(5) 0.036(3) Uani 1 1 d . . . C21 C 0.6047(16) 0.6845(14) 0.1668(7) 0.036(4) Uani 1 1 d . . . H21 H 0.5517 0.7172 0.1995 0.043 Uiso 1 1 calc R . . O22 O -0.5993(11) 0.8131(11) 0.4119(5) 0.043(3) Uani 1 1 d . . . C22 C 1.0175(13) 0.3727(12) 0.1304(6) 0.025(3) Uiso 1 1 d . . . O23 O 0.0408(11) 0.6790(9) 0.3076(5) 0.039(3) Uani 1 1 d . . . C23 C 1.0622(14) 0.3163(11) 0.0807(7) 0.030(4) Uani 1 1 d . . . H23 H 1.0606 0.3603 0.0418 0.037 Uiso 1 1 calc R . . O24 O 0.0067(8) 0.6485(8) 0.4194(5) 0.030(2) Uani 1 1 d . . . C24 C 1.1091(16) 0.1929(13) 0.0908(7) 0.036(4) Uani 1 1 d . . . H24 H 1.1443 0.1522 0.0584 0.043 Uiso 1 1 calc R . . C25 C 1.1037(11) 0.1292(11) 0.1493(6) 0.021(3) Uani 1 1 d U . . C26 C 1.0619(14) 0.1855(13) 0.1980(7) 0.029(3) Uani 1 1 d . . . H26 H 1.0628 0.1414 0.2369 0.035 Uiso 1 1 calc R . . C27 C 1.0167(13) 0.3127(13) 0.1886(7) 0.029(3) Uani 1 1 d . . . H27 H 0.9879 0.3532 0.2208 0.035 Uiso 1 1 calc R . . C28 C 1.1407(14) -0.0017(15) 0.1561(7) 0.033(4) Uani 1 1 d . . . C29 C -0.0412(14) 0.8545(13) 0.1276(6) 0.031(3) Uani 1 1 d . . . C30 C -0.1745(12) 0.8928(13) 0.1299(7) 0.026(3) Uani 1 1 d . . . C31 C -0.2237(15) 0.9138(16) 0.0779(7) 0.040(4) Uani 1 1 d . . . H31 H -0.1737 0.9042 0.0413 0.048 Uiso 1 1 calc R . . C32 C -0.3429(14) 0.9479(14) 0.0791(7) 0.037(4) Uani 1 1 d . . . H32 H -0.3738 0.9593 0.0444 0.044 Uiso 1 1 calc R . . C33 C -0.4148(13) 0.9646(13) 0.1332(7) 0.031(3) Uani 1 1 d . . . C34 C -0.3746(13) 0.9501(15) 0.1848(7) 0.037(4) Uani 1 1 d . . . H34 H -0.4267 0.9642 0.2205 0.044 Uiso 1 1 calc R . . C35 C -0.2490(16) 0.9121(14) 0.1830(8) 0.041(4) Uani 1 1 d . . . H35 H -0.2186 0.9007 0.2178 0.049 Uiso 1 1 calc R . . C36 C -0.6336(12) 1.1748(12) 0.1366(6) 0.024(3) Uani 1 1 d . . . C37 C -0.6475(15) 1.2560(12) 0.0830(7) 0.032(4) Uani 1 1 d . . . H37 H -0.6313 1.2315 0.0464 0.039 Uiso 1 1 calc R . . C38 C -0.6865(17) 1.3755(14) 0.0856(6) 0.036(4) Uani 1 1 d . . . H38 H -0.6969 1.4317 0.0501 0.043 Uiso 1 1 calc R . . C39 C -0.7100(13) 1.4123(12) 0.1394(6) 0.022(3) Uiso 1 1 d . . . C40 C -0.6902(15) 1.3254(12) 0.1924(6) 0.028(3) Uani 1 1 d . . . H40 H -0.7044 1.3485 0.2292 0.034 Uiso 1 1 calc R . . C41 C -0.6512(15) 1.2094(13) 0.1905(7) 0.034(4) Uani 1 1 d . . . H41 H -0.6359 1.1525 0.2257 0.041 Uiso 1 1 calc R . . C42 C -0.7508(13) 1.5414(13) 0.1422(7) 0.026(3) Uani 1 1 d . . . C43 C 0.1658(12) 0.1019(12) 0.3699(6) 0.022(3) Uani 1 1 d . . . C44 C 0.1231(14) 0.2351(14) 0.3688(6) 0.029(3) Uani 1 1 d . . . C45 C 0.0841(15) 0.2802(12) 0.4231(7) 0.033(4) Uani 1 1 d . . . H45 H 0.0853 0.2290 0.4599 0.040 Uiso 1 1 calc R . . C46 C 0.0450(17) 0.3987(13) 0.4210(7) 0.037(4) Uani 1 1 d . . . H46 H 0.0159 0.4289 0.4567 0.045 Uiso 1 1 calc R . . C47 C 0.0473(12) 0.4749(12) 0.3674(6) 0.022(3) Uani 1 1 d . . . C48 C 0.0845(18) 0.4321(16) 0.3134(7) 0.043(4) Uani 1 1 d . . . H48 H 0.0830 0.4835 0.2766 0.051 Uiso 1 1 calc R . . C49 C 0.1237(12) 0.3107(13) 0.3159(6) 0.025(3) Uani 1 1 d . . . H49 H 0.1512 0.2806 0.2802 0.029 Uiso 1 1 calc R . . C50 C -0.1632(12) 0.6842(11) 0.3634(6) 0.022(3) Uani 1 1 d . . . C51 C -0.2465(15) 0.7179(14) 0.4150(7) 0.037(4) Uani 1 1 d . . . H51 H -0.2200 0.7148 0.4495 0.045 Uiso 1 1 calc R . . C52 C -0.3659(14) 0.7553(16) 0.4150(8) 0.040(4) Uani 1 1 d . . . H52 H -0.4190 0.7775 0.4497 0.048 Uiso 1 1 calc R . . C53 C -0.4109(14) 0.7612(12) 0.3635(6) 0.030(3) Uani 1 1 d . . . C54 C -0.3217(14) 0.7289(18) 0.3122(7) 0.044(5) Uani 1 1 d . . . H54 H -0.3469 0.7393 0.2759 0.052 Uiso 1 1 calc R . . C55 C -0.1996(15) 0.6830(17) 0.3137(8) 0.042(4) Uani 1 1 d . . . H55 H -0.1440 0.6521 0.2813 0.050 Uiso 1 1 calc R . . C56 C -0.5361(11) 0.7992(12) 0.3621(6) 0.022(3) Uani 1 1 d . . . C57 C 0.3418(17) 0.6760(18) 0.5457(8) 0.056(6) Uani 1 1 d . . . H57 H 0.4037 0.6501 0.5145 0.067 Uiso 1 1 calc R . . C58 C 0.3670(17) 0.6238(18) 0.6042(8) 0.065(7) Uani 1 1 d . . . H58 H 0.4442 0.5669 0.6118 0.078 Uiso 1 1 calc R . . C59 C 0.2760(15) 0.6577(13) 0.6508(7) 0.033(4) Uani 1 1 d . . . C60 C 0.1661(15) 0.7428(13) 0.6363(7) 0.038(4) Uani 1 1 d . . . H60 H 0.1013 0.7683 0.6663 0.046 Uiso 1 1 calc R . . C61 C 0.1524(13) 0.7903(13) 0.5769(6) 0.027(3) Uani 1 1 d . . . H61 H 0.0767 0.8496 0.5682 0.033 Uiso 1 1 calc R . . C62 C 0.2981(18) 0.6028(15) 0.7165(7) 0.044(4) Uani 1 1 d . . . H62A H 0.2453 0.5660 0.7353 0.052 Uiso 1 1 calc R . . H62B H 0.3799 0.5399 0.7172 0.052 Uiso 1 1 calc R . . C63 C 0.2779(16) 0.6932(13) 0.7540(7) 0.036(4) Uani 1 1 d . . . H63A H 0.1929 0.7446 0.7628 0.043 Uiso 1 1 calc R . . H63B H 0.3166 0.7431 0.7319 0.043 Uiso 1 1 calc R . . C64 C 0.3323(16) 0.6211(15) 0.8130(7) 0.040(4) Uani 1 1 d . . . H64A H 0.3053 0.5598 0.8295 0.048 Uiso 1 1 calc R . . H64B H 0.4188 0.5805 0.8032 0.048 Uiso 1 1 calc R . . C65 C 0.3027(13) 0.6926(15) 0.8612(7) 0.034(4) Uani 1 1 d . . . C66 C 0.388(2) 0.672(3) 0.8945(10) 0.088(9) Uani 1 1 d . . . H66 H 0.4687 0.6259 0.8816 0.106 Uiso 1 1 calc R . . C67 C 0.3569(19) 0.717(2) 0.9462(9) 0.070(6) Uani 1 1 d U . . H67 H 0.4170 0.6929 0.9693 0.084 Uiso 1 1 calc R . . C68 C 0.168(2) 0.820(2) 0.9312(10) 0.068(7) Uani 1 1 d . . . H68 H 0.0891 0.8727 0.9423 0.082 Uiso 1 1 calc R . . C69 C 0.193(2) 0.776(2) 0.8801(10) 0.074(8) Uani 1 1 d . . . H69 H 0.1320 0.8043 0.8570 0.089 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 0.0220(6) 0.0249(5) 0.0284(5) -0.0039(4) -0.0069(4) -0.0085(4) S1 0.0157(18) 0.0169(16) 0.051(2) -0.0030(15) -0.0114(16) -0.0037(13) O1 0.045(7) 0.021(5) 0.039(6) -0.012(4) -0.005(5) -0.010(5) N1 0.015(6) 0.035(7) 0.035(7) -0.007(5) -0.014(5) 0.005(5) C1 0.015(7) 0.011(6) 0.044(9) -0.009(6) -0.004(6) -0.001(5) Cd2 0.0210(6) 0.0210(5) 0.0320(6) -0.0062(4) -0.0095(4) -0.0063(4) S2 0.023(2) 0.0206(17) 0.046(2) -0.0024(15) -0.0114(16) -0.0082(14) O2 0.033(6) 0.035(6) 0.026(5) -0.003(4) -0.010(4) -0.021(5) N2 0.028(8) 0.035(7) 0.048(8) -0.013(6) -0.001(6) -0.018(6) C2 0.018(7) 0.021(7) 0.031(8) -0.011(6) 0.004(6) -0.003(6) Cd3 0.0236(6) 0.0196(5) 0.0324(6) -0.0063(4) -0.0087(4) -0.0072(4) S3 0.023(2) 0.0201(17) 0.048(2) -0.0091(15) -0.0091(16) -0.0081(14) O3 0.029(7) 0.043(7) 0.063(8) -0.012(6) -0.013(6) -0.008(5) C3 0.041(10) 0.028(8) 0.021(7) -0.001(6) -0.006(6) -0.012(7) Cd4 0.0230(6) 0.0229(5) 0.0297(6) -0.0070(4) -0.0059(4) -0.0079(4) S4 0.0128(17) 0.0200(17) 0.044(2) -0.0089(14) -0.0053(14) -0.0048(13) O4 0.026(7) 0.072(9) 0.064(8) -0.020(7) 0.006(6) -0.028(6) C4 0.047(11) 0.037(9) 0.024(8) -0.005(6) -0.006(7) -0.012(8) O5 0.015(6) 0.014(5) 0.071(8) 0.007(5) -0.004(5) 0.002(4) C5 0.020(8) 0.011(6) 0.049(9) -0.002(6) -0.021(6) 0.000(5) O6 0.017(6) 0.023(5) 0.075(8) -0.011(5) -0.023(5) 0.004(4) C6 0.014(7) 0.042(9) 0.030(8) -0.007(6) 0.006(6) -0.014(6) O7 0.007(5) 0.043(7) 0.061(8) -0.017(5) 0.003(5) -0.006(5) C7 0.032(9) 0.019(7) 0.036(8) -0.005(6) -0.003(7) -0.006(6) O8 0.020(6) 0.033(6) 0.052(7) -0.007(5) -0.023(5) -0.002(4) C8 0.005(6) 0.015(6) 0.043(8) -0.006(6) -0.006(6) 0.002(5) O9 0.025(6) 0.015(5) 0.037(6) 0.000(4) -0.012(4) -0.004(4) C9 0.022(8) 0.042(9) 0.032(8) -0.012(6) -0.001(6) -0.016(7) O10 0.044(7) 0.024(5) 0.041(6) -0.007(4) -0.011(5) -0.016(5) C10 0.008(7) 0.012(6) 0.043(8) 0.000(6) 0.005(6) 0.005(5) O11 0.014(6) 0.039(6) 0.052(7) 0.003(5) -0.001(5) -0.008(5) C11 0.029(8) 0.006(6) 0.047(9) -0.007(6) -0.012(7) -0.002(5) O12 0.047(8) 0.041(7) 0.059(7) -0.017(6) -0.010(6) -0.025(6) C12 0.007(7) 0.029(8) 0.038(8) -0.002(6) 0.003(6) -0.008(5) O13 0.019(6) 0.052(7) 0.058(8) -0.011(6) -0.008(5) -0.016(5) C13 0.020(8) 0.037(9) 0.030(8) -0.006(6) 0.001(6) -0.006(6) O14 0.018(6) 0.037(6) 0.055(7) -0.012(5) -0.005(5) -0.001(5) C14 0.024(9) 0.070(13) 0.052(11) -0.027(9) -0.010(8) -0.016(9) O15 0.070(10) 0.027(6) 0.041(6) 0.006(5) -0.011(6) -0.027(6) C15 0.031(9) 0.020(7) 0.042(9) -0.016(6) 0.010(7) -0.018(6) O16 0.033(7) 0.038(6) 0.045(7) -0.019(5) -0.002(5) -0.011(5) C16 0.023(8) 0.043(9) 0.031(8) -0.007(6) -0.004(6) -0.015(7) O17 0.047(8) 0.040(7) 0.058(7) -0.024(6) -0.012(6) -0.017(6) C17 0.022(8) 0.053(10) 0.020(7) -0.008(6) -0.005(6) -0.016(7) O18 0.024(6) 0.030(6) 0.056(7) -0.004(5) -0.003(5) -0.011(5) C18 0.024(9) 0.059(11) 0.017(7) 0.004(7) 0.003(6) -0.019(8) O19 0.029(6) 0.017(5) 0.046(6) -0.017(4) 0.001(5) -0.005(4) C19 0.037(9) 0.015(7) 0.037(8) -0.003(6) -0.003(7) -0.018(6) O20 0.039(7) 0.022(5) 0.039(6) 0.002(4) -0.011(5) -0.012(5) C20 0.020(8) 0.038(9) 0.053(10) -0.018(7) -0.012(7) -0.009(7) O21 0.034(7) 0.039(6) 0.032(6) -0.004(5) -0.009(5) -0.013(5) C21 0.049(11) 0.033(8) 0.025(8) -0.005(6) -0.010(7) -0.015(7) O22 0.039(8) 0.053(8) 0.041(7) -0.013(5) -0.007(6) -0.020(6) O23 0.041(7) 0.026(6) 0.061(7) 0.000(5) -0.014(6) -0.025(5) C23 0.037(9) 0.008(6) 0.032(8) 0.000(5) -0.007(7) 0.000(6) O24 0.010(5) 0.023(5) 0.055(7) -0.019(4) -0.008(4) 0.002(4) C24 0.044(11) 0.022(8) 0.037(9) -0.009(6) -0.004(7) -0.010(7) C25 0.005(6) 0.019(6) 0.035(7) -0.004(5) -0.010(5) 0.000(5) C26 0.026(8) 0.024(7) 0.031(8) 0.003(6) -0.014(6) -0.006(6) C27 0.018(8) 0.036(8) 0.037(8) -0.020(6) 0.001(6) -0.010(6) C28 0.026(9) 0.048(10) 0.029(8) -0.011(7) -0.005(6) -0.017(7) C29 0.027(9) 0.031(8) 0.024(8) -0.007(6) -0.004(6) -0.004(6) C30 0.005(6) 0.033(8) 0.039(8) -0.007(6) -0.008(6) -0.004(5) C31 0.028(9) 0.053(11) 0.038(9) -0.015(7) 0.011(7) -0.021(8) C32 0.023(9) 0.039(9) 0.048(9) -0.004(7) -0.029(7) -0.005(7) C33 0.016(8) 0.031(8) 0.042(9) -0.018(7) -0.003(6) -0.002(6) C34 0.012(8) 0.059(11) 0.035(8) -0.020(7) 0.005(6) -0.011(7) C35 0.041(11) 0.033(9) 0.052(10) -0.009(7) -0.025(8) -0.010(7) C36 0.012(7) 0.029(7) 0.029(7) -0.009(6) 0.001(5) -0.009(6) C37 0.037(10) 0.018(7) 0.043(9) -0.008(6) -0.010(7) -0.010(6) C38 0.059(12) 0.031(8) 0.021(7) -0.001(6) -0.008(7) -0.024(8) C40 0.044(10) 0.020(7) 0.025(7) -0.008(5) -0.002(6) -0.017(7) C41 0.033(9) 0.026(8) 0.032(8) -0.004(6) -0.001(7) -0.006(7) C42 0.017(7) 0.024(7) 0.043(9) -0.011(6) -0.007(6) -0.010(6) C43 0.011(7) 0.029(7) 0.027(7) -0.006(6) 0.002(5) -0.010(5) C44 0.029(9) 0.034(8) 0.030(8) -0.005(6) -0.004(6) -0.018(7) C45 0.037(10) 0.016(7) 0.039(8) -0.001(6) -0.005(7) -0.008(6) C46 0.056(12) 0.027(8) 0.031(8) -0.008(6) -0.020(8) -0.012(7) C47 0.018(7) 0.023(7) 0.028(7) -0.006(5) -0.003(6) -0.011(6) C48 0.071(14) 0.047(10) 0.029(8) -0.006(7) -0.004(8) -0.043(10) C49 0.014(7) 0.033(8) 0.025(7) -0.012(6) 0.004(5) -0.008(6) C50 0.005(6) 0.015(6) 0.037(8) 0.002(5) -0.005(5) 0.000(5) C51 0.032(10) 0.037(9) 0.038(9) -0.018(7) -0.001(7) -0.007(7) C52 0.015(8) 0.057(11) 0.049(10) -0.018(8) -0.003(7) -0.014(7) C53 0.026(9) 0.021(7) 0.034(8) -0.008(6) -0.009(6) -0.001(6) C54 0.015(8) 0.090(14) 0.029(8) -0.031(8) 0.004(6) -0.019(8) C55 0.023(9) 0.063(12) 0.044(10) -0.029(8) 0.007(7) -0.018(8) C56 0.002(6) 0.026(7) 0.037(8) -0.010(6) 0.001(5) -0.004(5) C57 0.025(10) 0.063(13) 0.044(10) -0.009(9) 0.001(8) 0.003(8) C58 0.029(11) 0.064(13) 0.041(10) -0.009(9) -0.006(8) 0.025(9) C59 0.040(10) 0.028(8) 0.031(8) -0.006(6) -0.013(7) -0.010(7) C60 0.032(9) 0.022(8) 0.039(9) 0.000(6) -0.007(7) 0.003(6) C61 0.016(7) 0.029(8) 0.027(7) -0.005(6) 0.011(6) -0.010(6) C62 0.058(13) 0.040(10) 0.034(9) -0.008(7) -0.008(8) -0.020(9) C63 0.043(10) 0.028(8) 0.035(8) 0.000(6) -0.004(7) -0.017(7) C64 0.039(10) 0.039(9) 0.027(8) -0.006(7) -0.001(7) -0.009(7) C65 0.013(8) 0.048(10) 0.042(9) -0.012(7) -0.001(6) -0.014(7) C66 0.035(13) 0.16(3) 0.074(15) -0.074(17) 0.000(11) -0.027(15) C67 0.037(11) 0.107(15) 0.064(11) -0.033(10) -0.025(9) -0.014(10) C68 0.051(14) 0.070(14) 0.077(14) -0.033(11) -0.044(11) 0.004(10) C69 0.048(14) 0.092(17) 0.064(13) -0.046(12) -0.024(11) 0.005(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O3 2.174(13) 1_465 ? Cd1 O20 2.213(10) 1_565 ? Cd1 N1 2.242(12) . ? Cd1 O22 2.258(13) 1_655 ? Cd1 O1 2.290(10) . ? S1 O5 1.445(12) . ? S1 O6 1.451(12) . ? S1 C8 1.748(14) . ? S1 C5 1.781(13) . ? O1 C1 1.231(17) . ? N1 C61 1.302(17) . ? N1 C57 1.31(2) . ? C1 O2 1.258(17) . ? C1 C2 1.555(18) . ? Cd2 O19 2.223(9) 1_565 ? Cd2 O21 2.227(11) 1_655 ? Cd2 O9 2.279(10) 1_465 ? Cd2 O2 2.306(10) . ? Cd2 O4 2.340(12) 1_465 ? S2 O11 1.412(12) . ? S2 O12 1.435(12) . ? S2 C19 1.781(17) . ? S2 C22 1.810(14) . ? O2 Cd3 2.316(9) . ? N2 C68 1.29(2) . ? N2 C67 1.33(2) . ? N2 Cd4 2.263(13) 1_556 ? C2 C3 1.355(19) . ? C2 C7 1.38(2) . ? Cd3 O16 2.187(11) 1_645 ? Cd3 O14 2.276(11) . ? Cd3 O9 2.312(9) 1_465 ? Cd3 O7 2.381(10) . ? Cd3 O23 2.619(11) . ? S3 O17 1.415(12) . ? S3 O18 1.451(12) . ? S3 C36 1.777(14) . ? S3 C33 1.802(16) . ? O3 C14 1.28(2) . ? O3 Cd1 2.174(13) 1_645 ? C3 C4 1.42(2) . ? C3 H3 0.9300 . ? Cd4 O8 2.185(11) . ? Cd4 O15 2.219(11) 1_645 ? Cd4 O13 2.220(11) . ? Cd4 N2 2.263(13) 1_554 ? Cd4 O10 2.273(10) 1_465 ? S4 O24 1.433(11) . ? S4 O23 1.445(12) . ? S4 C50 1.761(14) . ? S4 C47 1.772(14) . ? O4 C14 1.26(2) . ? O4 Cd2 2.340(12) 1_645 ? C4 C5 1.39(2) . ? C4 H4 0.9300 . ? C5 C6 1.37(2) . ? C6 C7 1.42(2) . ? C6 H6 0.9300 . ? O7 C15 1.213(17) . ? C7 H7 0.9300 . ? O8 C15 1.255(18) . ? C8 C9 1.38(2) . ? C8 C13 1.41(2) . ? O9 C28 1.313(17) . ? O9 Cd2 2.279(10) 1_645 ? O9 Cd3 2.312(9) 1_645 ? C9 C10 1.41(2) . ? C9 H9 0.9300 . ? O10 C28 1.232(17) . ? O10 Cd4 2.273(10) 1_645 ? C10 C11 1.38(2) . ? C10 H10 0.9300 . ? C11 C12 1.41(2) . ? C11 C14 1.51(2) . ? C12 C13 1.40(2) . ? C12 H12 0.9300 . ? O13 C29 1.229(18) . ? C13 H13 0.9300 . ? O14 C29 1.253(18) . ? O15 C42 1.244(18) . ? O15 Cd4 2.219(11) 1_465 ? C15 C16 1.53(2) . ? O16 C42 1.265(17) . ? O16 Cd3 2.187(11) 1_465 ? C16 C21 1.38(2) . ? C16 C17 1.41(2) . ? C17 C18 1.39(2) . ? C17 H17 0.9300 . ? C18 C19 1.38(2) . ? C18 H18 0.9300 . ? O19 C43 1.266(16) . ? O19 Cd2 2.223(9) 1_545 ? C19 C20 1.39(2) . ? O20 C43 1.240(16) . ? O20 Cd1 2.213(10) 1_545 ? C20 C21 1.37(2) . ? C20 H20 0.9300 . ? O21 C56 1.236(17) . ? O21 Cd2 2.227(11) 1_455 ? C21 H21 0.9300 . ? O22 C56 1.244(17) . ? O22 Cd1 2.258(13) 1_455 ? C22 C27 1.37(2) . ? C22 C23 1.388(19) . ? C23 C24 1.380(19) . ? C23 H23 0.9300 . ? C24 C25 1.39(2) . ? C24 H24 0.9300 . ? C25 C26 1.37(2) . ? C25 C28 1.50(2) . ? C26 C27 1.43(2) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C29 C30 1.53(2) . ? C30 C35 1.37(2) . ? C30 C31 1.40(2) . ? C31 C32 1.37(2) . ? C31 H31 0.9300 . ? C32 C33 1.37(2) . ? C32 H32 0.9300 . ? C33 C34 1.35(2) . ? C34 C35 1.44(2) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C41 1.38(2) . ? C36 C37 1.38(2) . ? C37 C38 1.39(2) . ? C37 H37 0.9300 . ? C38 C39 1.371(19) . ? C38 H38 0.9300 . ? C39 C40 1.408(19) . ? C39 C42 1.507(19) . ? C40 C41 1.34(2) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C43 C44 1.53(2) . ? C44 C49 1.35(2) . ? C44 C45 1.41(2) . ? C45 C46 1.36(2) . ? C45 H45 0.9300 . ? C46 C47 1.37(2) . ? C46 H46 0.9300 . ? C47 C48 1.39(2) . ? C48 C49 1.39(2) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C50 C55 1.35(2) . ? C50 C51 1.41(2) . ? C51 C52 1.37(2) . ? C51 H51 0.9300 . ? C52 C53 1.42(2) . ? C52 H52 0.9300 . ? C53 C54 1.43(2) . ? C53 C56 1.45(2) . ? C54 C55 1.39(2) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C57 C58 1.38(2) . ? C57 H57 0.9300 . ? C58 C59 1.37(2) . ? C58 H58 0.9300 . ? C59 C60 1.36(2) . ? C59 C62 1.53(2) . ? C60 C61 1.37(2) . ? C60 H60 0.9300 . ? C61 H61 0.9300 . ? C62 C63 1.53(2) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.54(2) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 C65 1.51(2) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 C69 1.35(2) . ? C65 C66 1.38(3) . ? C66 C67 1.36(3) . ? C66 H66 0.9300 . ? C67 H67 0.9300 . ? C68 C69 1.36(3) . ? C68 H68 0.9300 . ? C69 H69 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cd1 O20 89.5(4) 1_465 1_565 ? O3 Cd1 N1 98.9(5) 1_465 . ? O20 Cd1 N1 111.2(4) 1_565 . ? O3 Cd1 O22 170.5(4) 1_465 1_655 ? O20 Cd1 O22 87.5(4) 1_565 1_655 ? N1 Cd1 O22 90.6(4) . 1_655 ? O3 Cd1 O1 93.0(4) 1_465 . ? O20 Cd1 O1 147.6(4) 1_565 . ? N1 Cd1 O1 100.3(4) . . ? O22 Cd1 O1 84.7(4) 1_655 . ? O5 S1 O6 120.4(8) . . ? O5 S1 C8 109.7(7) . . ? O6 S1 C8 108.3(7) . . ? O5 S1 C5 106.1(7) . . ? O6 S1 C5 107.9(7) . . ? C8 S1 C5 103.3(7) . . ? C1 O1 Cd1 139.6(9) . . ? C61 N1 C57 115.2(14) . . ? C61 N1 Cd1 123.7(10) . . ? C57 N1 Cd1 121.1(11) . . ? O1 C1 O2 128.8(13) . . ? O1 C1 C2 112.8(12) . . ? O2 C1 C2 118.1(12) . . ? O19 Cd2 O21 94.6(4) 1_565 1_655 ? O19 Cd2 O9 113.2(4) 1_565 1_465 ? O21 Cd2 O9 139.0(4) 1_655 1_465 ? O19 Cd2 O2 157.0(4) 1_565 . ? O21 Cd2 O2 88.1(4) 1_655 . ? O9 Cd2 O2 77.9(3) 1_465 . ? O19 Cd2 O4 81.8(4) 1_565 1_465 ? O21 Cd2 O4 134.5(4) 1_655 1_465 ? O9 Cd2 O4 81.1(4) 1_465 1_465 ? O2 Cd2 O4 80.2(4) . 1_465 ? O11 S2 O12 120.8(8) . . ? O11 S2 C19 107.9(7) . . ? O12 S2 C19 107.3(7) . . ? O11 S2 C22 106.9(7) . . ? O12 S2 C22 108.5(7) . . ? C19 S2 C22 104.3(7) . . ? C1 O2 Cd2 114.8(8) . . ? C1 O2 Cd3 138.3(9) . . ? Cd2 O2 Cd3 102.1(4) . . ? C68 N2 C67 113.4(16) . . ? C68 N2 Cd4 126.8(14) . 1_556 ? C67 N2 Cd4 115.5(12) . 1_556 ? C3 C2 C7 120.5(14) . . ? C3 C2 C1 121.2(13) . . ? C7 C2 C1 118.3(12) . . ? O16 Cd3 O14 93.0(4) 1_645 . ? O16 Cd3 O9 163.0(4) 1_645 1_465 ? O14 Cd3 O9 89.6(4) . 1_465 ? O16 Cd3 O2 109.2(4) 1_645 . ? O14 Cd3 O2 145.2(4) . . ? O9 Cd3 O2 77.0(3) 1_465 . ? O16 Cd3 O7 86.2(4) 1_645 . ? O14 Cd3 O7 132.1(4) . . ? O9 Cd3 O7 79.6(4) 1_465 . ? O2 Cd3 O7 77.4(4) . . ? O16 Cd3 O23 83.3(4) 1_645 . ? O14 Cd3 O23 79.8(4) . . ? O9 Cd3 O23 113.7(3) 1_465 . ? O2 Cd3 O23 76.6(4) . . ? O7 Cd3 O23 146.9(4) . . ? O17 S3 O18 119.2(8) . . ? O17 S3 C36 109.1(7) . . ? O18 S3 C36 108.0(7) . . ? O17 S3 C33 108.6(7) . . ? O18 S3 C33 107.3(7) . . ? C36 S3 C33 103.6(7) . . ? C14 O3 Cd1 109.1(11) . 1_645 ? C2 C3 C4 120.7(13) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? O8 Cd4 O15 90.4(5) . 1_645 ? O8 Cd4 O13 170.5(4) . . ? O15 Cd4 O13 90.8(5) 1_645 . ? O8 Cd4 N2 92.3(5) . 1_554 ? O15 Cd4 N2 93.2(4) 1_645 1_554 ? O13 Cd4 N2 97.1(5) . 1_554 ? O8 Cd4 O10 88.2(4) . 1_465 ? O15 Cd4 O10 136.8(4) 1_645 1_465 ? O13 Cd4 O10 84.5(4) . 1_465 ? N2 Cd4 O10 130.0(4) 1_554 1_465 ? O24 S4 O23 119.2(7) . . ? O24 S4 C50 108.8(6) . . ? O23 S4 C50 108.6(7) . . ? O24 S4 C47 108.8(6) . . ? O23 S4 C47 107.9(6) . . ? C50 S4 C47 102.1(7) . . ? C14 O4 Cd2 153.1(12) . 1_645 ? C5 C4 C3 117.7(14) . . ? C5 C4 H4 121.1 . . ? C3 C4 H4 121.1 . . ? C6 C5 C4 122.5(14) . . ? C6 C5 S1 119.3(12) . . ? C4 C5 S1 118.2(12) . . ? C5 C6 C7 117.7(13) . . ? C5 C6 H6 121.1 . . ? C7 C6 H6 121.1 . . ? C15 O7 Cd3 142.9(11) . . ? C2 C7 C6 120.6(13) . . ? C2 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C15 O8 Cd4 116.9(10) . . ? C9 C8 C13 120.7(13) . . ? C9 C8 S1 120.5(11) . . ? C13 C8 S1 118.8(11) . . ? C28 O9 Cd2 136.5(10) . 1_645 ? C28 O9 Cd3 113.4(9) . 1_645 ? Cd2 O9 Cd3 103.0(3) 1_645 1_645 ? C8 C9 C10 121.0(14) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C28 O10 Cd4 151.3(11) . 1_645 ? C11 C10 C9 119.0(13) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 C12 119.9(14) . . ? C10 C11 C14 119.1(14) . . ? C12 C11 C14 121.0(14) . . ? C13 C12 C11 121.6(14) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C29 O13 Cd4 119.4(11) . . ? C12 C13 C8 117.7(13) . . ? C12 C13 H13 121.2 . . ? C8 C13 H13 121.2 . . ? C29 O14 Cd3 138.0(10) . . ? O4 C14 O3 123.9(17) . . ? O4 C14 C11 119.8(15) . . ? O3 C14 C11 116.3(16) . . ? C42 O15 Cd4 135.1(10) . 1_465 ? O7 C15 O8 127.9(16) . . ? O7 C15 C16 116.5(14) . . ? O8 C15 C16 115.5(13) . . ? C42 O16 Cd3 127.1(10) . 1_465 ? C21 C16 C17 119.7(15) . . ? C21 C16 C15 122.2(14) . . ? C17 C16 C15 118.1(13) . . ? C18 C17 C16 119.9(14) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C19 C18 C17 119.6(14) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C43 O19 Cd2 132.7(9) . 1_545 ? C18 C19 C20 119.9(15) . . ? C18 C19 S2 119.6(12) . . ? C20 C19 S2 120.4(12) . . ? C43 O20 Cd1 126.0(9) . 1_545 ? C21 C20 C19 121.1(15) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C56 O21 Cd2 128.2(9) . 1_455 ? C20 C21 C16 119.8(15) . . ? C20 C21 H21 120.1 . . ? C16 C21 H21 120.1 . . ? C56 O22 Cd1 127.1(10) . 1_455 ? C27 C22 C23 123.5(13) . . ? C27 C22 S2 118.2(11) . . ? C23 C22 S2 118.3(10) . . ? S4 O23 Cd3 168.2(7) . . ? C24 C23 C22 118.0(13) . . ? C24 C23 H23 121.0 . . ? C22 C23 H23 121.0 . . ? C23 C24 C25 120.1(14) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 121.1(13) . . ? C26 C25 C28 121.8(13) . . ? C24 C25 C28 117.0(12) . . ? C25 C26 C27 119.4(13) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C22 C27 C26 117.7(13) . . ? C22 C27 H27 121.2 . . ? C26 C27 H27 121.2 . . ? O10 C28 O9 122.5(15) . . ? O10 C28 C25 118.6(13) . . ? O9 C28 C25 118.8(12) . . ? O13 C29 O14 129.3(16) . . ? O13 C29 C30 114.6(13) . . ? O14 C29 C30 115.9(13) . . ? C35 C30 C31 118.7(14) . . ? C35 C30 C29 119.8(13) . . ? C31 C30 C29 121.4(13) . . ? C32 C31 C30 122.2(14) . . ? C32 C31 H31 118.9 . . ? C30 C31 H31 118.9 . . ? C33 C32 C31 117.6(14) . . ? C33 C32 H32 121.2 . . ? C31 C32 H32 121.2 . . ? C34 C33 C32 123.5(14) . . ? C34 C33 S3 118.6(11) . . ? C32 C33 S3 117.7(11) . . ? C33 C34 C35 118.1(14) . . ? C33 C34 H34 120.9 . . ? C35 C34 H34 120.9 . . ? C30 C35 C34 119.8(14) . . ? C30 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C41 C36 C37 121.2(14) . . ? C41 C36 S3 119.6(11) . . ? C37 C36 S3 118.7(11) . . ? C36 C37 C38 117.9(14) . . ? C36 C37 H37 121.0 . . ? C38 C37 H37 121.0 . . ? C39 C38 C37 121.4(13) . . ? C39 C38 H38 119.3 . . ? C37 C38 H38 119.3 . . ? C38 C39 C40 118.4(13) . . ? C38 C39 C42 121.5(12) . . ? C40 C39 C42 120.0(12) . . ? C41 C40 C39 120.8(13) . . ? C41 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? C40 C41 C36 120.1(14) . . ? C40 C41 H41 120.0 . . ? C36 C41 H41 120.0 . . ? O15 C42 O16 126.3(14) . . ? O15 C42 C39 116.4(13) . . ? O16 C42 C39 117.3(13) . . ? O20 C43 O19 127.4(13) . . ? O20 C43 C44 117.6(12) . . ? O19 C43 C44 114.5(12) . . ? C49 C44 C45 119.1(14) . . ? C49 C44 C43 120.5(13) . . ? C45 C44 C43 120.4(13) . . ? C46 C45 C44 119.4(14) . . ? C46 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C45 C46 C47 121.4(14) . . ? C45 C46 H46 119.3 . . ? C47 C46 H46 119.3 . . ? C46 C47 C48 119.9(14) . . ? C46 C47 S4 121.3(11) . . ? C48 C47 S4 118.6(11) . . ? C49 C48 C47 118.3(14) . . ? C49 C48 H48 120.9 . . ? C47 C48 H48 120.9 . . ? C44 C49 C48 121.8(13) . . ? C44 C49 H49 119.1 . . ? C48 C49 H49 119.1 . . ? C55 C50 C51 120.2(14) . . ? C55 C50 S4 118.9(11) . . ? C51 C50 S4 120.7(12) . . ? C52 C51 C50 121.0(15) . . ? C52 C51 H51 119.5 . . ? C50 C51 H51 119.5 . . ? C51 C52 C53 121.7(15) . . ? C51 C52 H52 119.1 . . ? C53 C52 H52 119.1 . . ? C52 C53 C54 114.2(14) . . ? C52 C53 C56 123.3(14) . . ? C54 C53 C56 122.5(13) . . ? C55 C54 C53 123.6(14) . . ? C55 C54 H54 118.2 . . ? C53 C54 H54 118.2 . . ? C50 C55 C54 118.7(14) . . ? C50 C55 H55 120.6 . . ? C54 C55 H55 120.6 . . ? O21 C56 O22 128.3(13) . . ? O21 C56 C53 117.6(12) . . ? O22 C56 C53 114.1(13) . . ? N1 C57 C58 124.3(16) . . ? N1 C57 H57 117.9 . . ? C58 C57 H57 117.9 . . ? C59 C58 C57 118.7(16) . . ? C59 C58 H58 120.7 . . ? C57 C58 H58 120.7 . . ? C60 C59 C58 117.4(14) . . ? C60 C59 C62 121.5(15) . . ? C58 C59 C62 121.2(15) . . ? C59 C60 C61 118.8(15) . . ? C59 C60 H60 120.6 . . ? C61 C60 H60 120.6 . . ? N1 C61 C60 125.6(14) . . ? N1 C61 H61 117.2 . . ? C60 C61 H61 117.2 . . ? C63 C62 C59 114.0(13) . . ? C63 C62 H62A 108.8 . . ? C59 C62 H62A 108.8 . . ? C63 C62 H62B 108.8 . . ? C59 C62 H62B 108.8 . . ? H62A C62 H62B 107.6 . . ? C62 C63 C64 107.5(13) . . ? C62 C63 H63A 110.2 . . ? C64 C63 H63A 110.2 . . ? C62 C63 H63B 110.2 . . ? C64 C63 H63B 110.2 . . ? H63A C63 H63B 108.5 . . ? C65 C64 C63 116.0(14) . . ? C65 C64 H64A 108.3 . . ? C63 C64 H64A 108.3 . . ? C65 C64 H64B 108.3 . . ? C63 C64 H64B 108.3 . . ? H64A C64 H64B 107.4 . . ? C69 C65 C66 112.0(18) . . ? C69 C65 C64 126.4(16) . . ? C66 C65 C64 121.5(16) . . ? C67 C66 C65 121(2) . . ? C67 C66 H66 119.4 . . ? C65 C66 H66 119.4 . . ? N2 C67 C66 124.4(19) . . ? N2 C67 H67 117.8 . . ? C66 C67 H67 117.8 . . ? N2 C68 C69 125(2) . . ? N2 C68 H68 117.5 . . ? C69 C68 H68 117.5 . . ? C65 C69 C68 123(2) . . ? C65 C69 H69 118.4 . . ? C68 C69 H69 118.4 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 2.270 _refine_diff_density_min -1.865 _refine_diff_density_rms 0.243