# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Qingjin Meng' _publ_contact_author_address ; Coordination Chemistry Institute, State Key Laboratory of Coordination Chemistry Nanjing 210093 CHINA ; _publ_contact_author_email MENGQJ@NJU.EDU.CN _publ_section_title ; Ligand-to-Metal Ratio Controlled Assembly of Nanoporous Metal-Organic Frameworks ; loop_ _publ_author_name 'Qingjin Meng' 'Song Gao' 'Yi-Zhi Li' 'Jian-Guo Lin' 'Chang-Sheng Lu' ; Ling Qiu ; 'Yan-Yan Xu' 'Shuang-Quan Zang' data_70308a _database_code_depnum_ccdc_archive 'CCDC 675548' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H20 Cd N4 O4 S, H4 O2, 4(H2 O)' _chemical_formula_sum 'C32 H32 Cd N4 O10 S' _chemical_formula_weight 777.08 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M FDD2 _symmetry_space_group_name_Hall F2-2d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 28.6911(19) _cell_length_b 50.103(3) _cell_length_c 10.0620(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14464.3(17) _cell_formula_units_Z 16 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6336 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8131 _exptl_absorpt_correction_T_max 0.8463 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19434 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 61 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6355 _reflns_number_gt 5628 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+85.3446P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(3) _refine_ls_number_reflns 6355 _refine_ls_number_parameters 421 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.1146 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1878(2) 0.27404(15) 1.0078(8) 0.0402(17) Uani 1 1 d . . . C2 C 0.1897(2) 0.24728(16) 1.0164(7) 0.0416(18) Uani 1 1 d . . . H2 H 0.1906 0.2369 0.9399 0.050 Uiso 1 1 calc R . . C3 C 0.1905(3) 0.23507(11) 1.1443(10) 0.0465(15) Uani 1 1 d . . . H3 H 0.1932 0.2166 1.1527 0.056 Uiso 1 1 calc R . . C4 C 0.1871(3) 0.25083(18) 1.2539(9) 0.054(2) Uani 1 1 d . . . H4 H 0.1869 0.2429 1.3376 0.064 Uiso 1 1 calc R . . C5 C 0.1840(2) 0.27858(13) 1.2440(7) 0.0367(16) Uani 1 1 d . . . C6 C 0.1843(2) 0.28934(13) 1.1252(8) 0.0433(14) Uani 1 1 d . . . H6 H 0.1820 0.3078 1.1179 0.052 Uiso 1 1 calc R . . C7 C 0.1897(2) 0.28633(14) 0.8732(8) 0.0440(16) Uani 1 1 d . . . C8 C 0.1804(2) 0.29438(14) 1.3713(7) 0.0398(15) Uani 1 1 d . . . C9 C 0.1536(2) 0.45991(11) 0.7092(7) 0.0394(15) Uani 1 1 d . . . C10 C 0.1892(2) 0.44369(11) 0.6565(8) 0.0403(17) Uani 1 1 d . . . C11 C 0.2276(2) 0.45892(13) 0.6104(6) 0.0401(15) Uani 1 1 d . . . C12 C 0.22151(19) 0.48650(11) 0.6269(8) 0.0381(14) Uani 1 1 d . . . C13 C 0.1080(2) 0.45277(12) 0.7583(7) 0.0372(15) Uani 1 1 d . . . C14 C 0.0844(2) 0.46893(12) 0.8457(6) 0.0366(15) Uani 1 1 d . . . H14 H 0.0987 0.4842 0.8784 0.044 Uiso 1 1 calc R . . C15 C 0.03882(19) 0.46254(11) 0.8864(8) 0.0361(13) Uani 1 1 d . . . H15 H 0.0239 0.4741 0.9451 0.043 Uiso 1 1 calc R . . C16 C 0.0395(2) 0.42509(12) 0.7644(7) 0.0358(15) Uani 1 1 d . . . H16 H 0.0244 0.4098 0.7350 0.043 Uiso 1 1 calc R . . C17 C 0.0846(2) 0.42952(13) 0.7203(7) 0.0422(16) Uani 1 1 d . . . H17 H 0.0992 0.4171 0.6657 0.051 Uiso 1 1 calc R . . C18 C 0.1893(2) 0.41463(11) 0.6528(8) 0.0355(14) Uani 1 1 d . . . C19 C 0.1886(2) 0.39946(15) 0.7633(8) 0.048(2) Uani 1 1 d . . . H19 H 0.1875 0.4079 0.8456 0.057 Uiso 1 1 calc R . . C20 C 0.1896(3) 0.37180(15) 0.7593(8) 0.0401(17) Uani 1 1 d . . . H20 H 0.1896 0.3621 0.8380 0.048 Uiso 1 1 calc R . . C21 C 0.1904(3) 0.37446(16) 0.5352(9) 0.049(2) Uani 1 1 d . . . H21 H 0.1899 0.3659 0.4532 0.058 Uiso 1 1 calc R . . C22 C 0.1911(3) 0.40115(16) 0.5342(8) 0.0487(19) Uani 1 1 d . . . H22 H 0.1928 0.4104 0.4544 0.058 Uiso 1 1 calc R . . C23 C 0.2713(2) 0.44863(13) 0.5551(8) 0.0427(17) Uani 1 1 d . . . C24 C 0.2993(2) 0.43208(13) 0.6156(9) 0.051 Uani 1 1 d . . . H24 H 0.2897 0.4246 0.6957 0.061 Uiso 1 1 calc R . . C25 C 0.3426(2) 0.42512(15) 0.5662(8) 0.0475(17) Uani 1 1 d . . . H25 H 0.3629 0.4152 0.6187 0.057 Uiso 1 1 calc R . . C26 C 0.32580(19) 0.44668(13) 0.3793(8) 0.0400(14) Uani 1 1 d . . . H26 H 0.3345 0.4518 0.2940 0.048 Uiso 1 1 calc R . . C27 C 0.2828(2) 0.45511(13) 0.4222(7) 0.0413(16) Uani 1 1 d . . . H27 H 0.2625 0.4645 0.3673 0.050 Uiso 1 1 calc R . . C28 C 0.2499(2) 0.51002(12) 0.5987(7) 0.0422(17) Uani 1 1 d . . . C29 C 0.2970(2) 0.50957(14) 0.6268(9) 0.0523(18) Uani 1 1 d . . . H29 H 0.3109 0.4943 0.6615 0.063 Uiso 1 1 calc R . . C30 C 0.3237(2) 0.53276(15) 0.6018(8) 0.052(2) Uani 1 1 d . . . H30 H 0.3558 0.5320 0.6141 0.062 Uiso 1 1 calc R . . C31 C 0.2617(3) 0.55437(14) 0.5344(9) 0.062(2) Uani 1 1 d . . . H31 H 0.2484 0.5700 0.5023 0.074 Uiso 1 1 calc R . . C32 C 0.2340(3) 0.53355(14) 0.5467(8) 0.0508(18) Uani 1 1 d . . . H32 H 0.2031 0.5349 0.5195 0.061 Uiso 1 1 calc R . . Cd1 Cd 0.186834(16) 0.312860(8) 0.63658(5) 0.03689(12) Uani 1 1 d . . . N1 N 0.01610(18) 0.44131(10) 0.8464(5) 0.0371(13) Uani 1 1 d . . . N2 N 0.19040(19) 0.35910(9) 0.6424(7) 0.0413(11) Uani 1 1 d . . . N3 N 0.3556(2) 0.43236(10) 0.4449(6) 0.0418(13) Uani 1 1 d . . . N4 N 0.3054(2) 0.55501(12) 0.5626(6) 0.0444(14) Uani 1 1 d . . . O1 O 0.19976(18) 0.31143(8) 0.8678(5) 0.0449(12) Uani 1 1 d . . . O2 O 0.18410(18) 0.27262(11) 0.7751(5) 0.050 Uani 1 1 d . . . O3 O 0.18320(17) 0.31969(10) 1.3605(6) 0.0530(15) Uani 1 1 d . . . O4 O 0.17421(16) 0.28351(10) 1.4792(5) 0.0444(12) Uani 1 1 d . . . O5 O 0.27576(19) 0.33704(11) 0.9749(6) 0.0632(15) Uani 1 1 d . . . H5D H 0.2524 0.3289 0.9425 0.076 Uiso 1 1 d R . . H5C H 0.2737 0.3536 0.9571 0.076 Uiso 1 1 d R . . O6 O 0.32428(18) 0.38069(11) 0.8613(6) 0.0652(15) Uani 1 1 d . . . H6D H 0.3521 0.3749 0.8639 0.078 Uiso 1 1 d R . . H6A H 0.3221 0.3948 0.9077 0.078 Uiso 1 1 d R . . O7 O 0.40692(17) 0.35672(10) 0.8845(6) 0.0590(13) Uani 1 1 d . . . H7A H 0.4270 0.3675 0.8529 0.071 Uiso 1 1 d R . . H7C H 0.4077 0.3422 0.8412 0.071 Uiso 1 1 d R . . O8 O 0.47642(19) 0.39195(11) 0.9494(6) 0.0651(15) Uani 1 1 d . . . H8D H 0.5048 0.3874 0.9393 0.078 Uiso 1 1 d R . . H8B H 0.4703 0.4058 0.9039 0.078 Uiso 1 1 d R . . O9 O 0.57507(19) 0.38732(12) 0.9355(6) 0.0706(18) Uani 1 1 d . . . H9D H 0.5810 0.3726 0.8973 0.085 Uiso 1 1 d R . . H9B H 0.5867 0.4002 0.8913 0.085 Uiso 1 1 d R . . O10 O 0.3431(2) 0.41115(11) 1.0567(6) 0.0643(16) Uani 1 1 d . . . H10A H 0.3706 0.4163 1.0742 0.077 Uiso 1 1 d R . . H10C H 0.3427 0.4037 0.9807 0.077 Uiso 1 1 d R . . S1 S 0.16732(5) 0.49280(3) 0.69897(17) 0.0338(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.042(4) 0.036(4) 0.043(4) -0.019(3) 0.007(3) 0.001(3) C2 0.040(4) 0.047(4) 0.037(4) -0.013(3) 0.013(3) -0.007(3) C3 0.060(4) 0.030(3) 0.049(4) -0.004(4) 0.001(4) -0.006(3) C4 0.063(5) 0.053(5) 0.045(5) 0.029(4) -0.004(4) 0.006(4) C5 0.048(4) 0.032(3) 0.030(4) -0.017(3) 0.000(3) 0.003(3) C6 0.048(3) 0.048(3) 0.034(4) -0.006(3) -0.009(3) -0.001(3) C7 0.045(4) 0.055(4) 0.033(4) 0.005(3) -0.001(4) -0.004(3) C8 0.037(3) 0.053(4) 0.030(4) 0.006(3) 0.003(3) -0.009(3) C9 0.036(3) 0.029(3) 0.053(4) -0.005(3) 0.001(3) 0.002(2) C10 0.042(3) 0.033(3) 0.046(5) -0.012(3) -0.001(3) -0.014(3) C11 0.048(4) 0.052(4) 0.021(4) 0.007(3) 0.008(3) 0.001(3) C12 0.027(3) 0.034(3) 0.053(4) 0.003(3) 0.015(3) 0.004(2) C13 0.045(4) 0.032(3) 0.035(4) 0.000(3) 0.004(3) 0.000(3) C14 0.040(3) 0.037(3) 0.033(4) 0.007(2) 0.009(3) -0.001(3) C15 0.027(3) 0.038(3) 0.043(4) -0.002(3) -0.006(3) 0.010(2) C16 0.034(3) 0.030(3) 0.043(4) -0.020(3) 0.016(3) -0.004(2) C17 0.035(3) 0.049(4) 0.042(4) -0.021(3) 0.011(3) 0.010(3) C18 0.033(3) 0.036(3) 0.038(4) -0.006(3) 0.009(3) -0.006(3) C19 0.046(4) 0.046(4) 0.052(5) -0.016(3) 0.032(4) -0.010(3) C20 0.051(4) 0.034(4) 0.035(4) 0.008(3) 0.010(3) -0.007(3) C21 0.052(5) 0.043(4) 0.051(5) -0.002(3) -0.009(4) 0.009(3) C22 0.062(5) 0.042(4) 0.042(5) -0.004(3) 0.006(4) 0.003(3) C23 0.026(3) 0.044(4) 0.059(5) 0.007(3) 0.021(3) 0.007(3) C24 0.045 0.042 0.066 0.006 0.011 0.003 C25 0.038(4) 0.061(4) 0.044(4) 0.013(3) 0.010(3) 0.016(3) C26 0.023(3) 0.060(4) 0.036(4) 0.011(4) 0.010(3) 0.003(2) C27 0.030(3) 0.053(4) 0.041(4) 0.011(3) 0.007(3) 0.023(3) C28 0.032(3) 0.038(3) 0.056(5) -0.010(3) 0.020(3) -0.005(3) C29 0.052(4) 0.051(4) 0.054(5) 0.002(4) 0.024(4) -0.016(3) C30 0.038(4) 0.051(4) 0.065(6) -0.005(4) 0.012(3) -0.010(3) C31 0.080(6) 0.035(4) 0.072(6) 0.003(4) 0.039(5) -0.007(4) C32 0.048(4) 0.043(4) 0.062(5) 0.006(3) 0.021(4) 0.005(3) Cd1 0.0421(2) 0.02821(18) 0.0403(2) -0.0017(2) 0.0067(2) -0.00085(19) N1 0.035(3) 0.038(3) 0.038(4) 0.002(2) 0.005(2) -0.001(2) N2 0.048(3) 0.036(2) 0.039(3) 0.014(3) 0.011(3) 0.007(2) N3 0.043(3) 0.037(3) 0.045(3) 0.007(2) 0.012(3) 0.004(2) N4 0.036(3) 0.049(3) 0.048(4) -0.011(3) 0.010(3) -0.015(3) O1 0.056(3) 0.036(3) 0.043(3) 0.010(2) 0.006(3) -0.0103(19) O2 0.057 0.048 0.044 0.008 0.006 -0.009 O3 0.063(3) 0.044(3) 0.052(4) -0.010(2) 0.005(3) 0.001(2) O4 0.046(3) 0.064(3) 0.024(3) -0.005(2) 0.007(2) 0.000(2) O5 0.062(3) 0.062(3) 0.065(4) 0.009(3) -0.012(3) -0.024(3) O6 0.068(3) 0.061(3) 0.067(4) -0.015(3) -0.020(3) -0.010(3) O7 0.059(3) 0.059(3) 0.059(3) -0.015(3) -0.006(3) 0.013(2) O8 0.065(3) 0.066(3) 0.064(4) 0.006(3) 0.015(3) 0.022(3) O9 0.071(4) 0.065(4) 0.075(5) -0.011(3) -0.025(3) 0.019(3) O10 0.064(3) 0.065(3) 0.064(4) 0.018(3) -0.007(3) 0.013(3) S1 0.0285(7) 0.0257(7) 0.0472(9) -0.0078(6) 0.0127(7) -0.0029(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.345(10) . ? C1 C6 1.411(10) . ? C1 C7 1.489(11) . ? C2 C3 1.425(12) . ? C2 H2 0.9300 . ? C3 C4 1.360(12) . ? C3 H3 0.9300 . ? C4 C5 1.397(11) . ? C4 H4 0.9300 . ? C5 C6 1.312(11) . ? C5 C8 1.509(10) . ? C6 H6 0.9300 . ? C7 O2 1.213(9) . ? C7 O1 1.292(8) . ? C7 Cd1 2.728(8) . ? C8 O4 1.228(9) . ? C8 O3 1.275(8) . ? C9 C10 1.409(9) . ? C9 C13 1.443(9) . ? C9 S1 1.697(6) . ? C10 C11 1.418(9) . ? C10 C18 1.456(8) . ? C11 C12 1.403(9) . ? C11 C23 1.465(9) . ? C12 C28 1.461(8) . ? C12 S1 1.744(6) . ? C13 C14 1.374(9) . ? C13 C17 1.398(9) . ? C14 C15 1.407(8) . ? C14 H14 0.9300 . ? C15 N1 1.311(8) . ? C15 H15 0.9300 . ? C16 N1 1.338(7) . ? C16 C17 1.387(9) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.347(11) . ? C18 C22 1.372(11) . ? C19 C20 1.387(10) . ? C19 H19 0.9300 . ? C20 N2 1.338(10) . ? C20 H20 0.9300 . ? C21 N2 1.325(10) . ? C21 C22 1.338(11) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.305(10) . ? C23 C27 1.415(10) . ? C24 C25 1.384(9) . ? C24 H24 0.9300 . ? C25 N3 1.327(9) . ? C25 H25 0.9300 . ? C26 N3 1.297(8) . ? C26 C27 1.374(8) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C32 1.368(10) . ? C28 C29 1.381(10) . ? C29 C30 1.414(9) . ? C29 H29 0.9300 . ? C30 N4 1.294(10) . ? C30 H30 0.9300 . ? C31 N4 1.286(11) . ? C31 C32 1.316(10) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? Cd1 O4 2.191(5) 1_554 ? Cd1 N1 2.319(5) 7_554 ? Cd1 N2 2.320(4) . ? Cd1 O1 2.357(5) . ? Cd1 N3 2.414(6) 15_455 ? Cd1 O2 2.452(5) . ? Cd1 O6 5.676(5) . ? N1 Cd1 2.319(5) 15_455 ? N3 Cd1 2.414(6) 7_554 ? O4 Cd1 2.191(5) 1_556 ? O5 H5D 0.8497 . ? O5 H5C 0.8499 . ? O6 O10 2.547(8) . ? O6 H6D 0.8501 . ? O6 H6A 0.8500 . ? O7 H7A 0.8501 . ? O7 H7C 0.8499 . ? O8 H8D 0.8499 . ? O8 H8B 0.8502 . ? O9 H9D 0.8499 . ? O9 H9B 0.8500 . ? O10 H10A 0.8501 . ? O10 H10C 0.8499 . ? 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 C2 C1 C6 119.4(8) . . ? C2 C1 C7 118.0(6) . . ? C6 C1 C7 122.6(7) . . ? C1 C2 C3 119.1(7) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C4 C3 C2 118.8(6) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 121.6(7) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 118.3(7) . . ? C6 C5 C8 123.9(6) . . ? C4 C5 C8 117.8(7) . . ? C5 C6 C1 122.7(6) . . ? C5 C6 H6 118.7 . . ? C1 C6 H6 118.7 . . ? O2 C7 O1 123.1(7) . . ? O2 C7 C1 120.1(6) . . ? O1 C7 C1 116.7(7) . . ? O2 C7 Cd1 64.0(4) . . ? O1 C7 Cd1 59.7(4) . . ? C1 C7 Cd1 174.0(5) . . ? O4 C8 O3 121.7(7) . . ? O4 C8 C5 121.8(6) . . ? O3 C8 C5 116.5(6) . . ? C10 C9 C13 130.0(5) . . ? C10 C9 S1 111.7(5) . . ? C13 C9 S1 118.1(4) . . ? C9 C10 C11 112.1(5) . . ? C9 C10 C18 126.0(6) . . ? C11 C10 C18 121.9(6) . . ? C12 C11 C10 113.2(6) . . ? C12 C11 C23 119.9(6) . . ? C10 C11 C23 126.8(6) . . ? C11 C12 C28 134.6(5) . . ? C11 C12 S1 109.8(4) . . ? C28 C12 S1 115.6(4) . . ? C14 C13 C17 115.4(6) . . ? C14 C13 C9 121.3(6) . . ? C17 C13 C9 123.3(6) . . ? C13 C14 C15 120.7(6) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? N1 C15 C14 123.9(6) . . ? N1 C15 H15 118.1 . . ? C14 C15 H15 118.1 . . ? N1 C16 C17 124.6(6) . . ? N1 C16 H16 117.7 . . ? C17 C16 H16 117.7 . . ? C16 C17 C13 119.6(6) . . ? C16 C17 H17 120.2 . . ? C13 C17 H17 120.2 . . ? C19 C18 C22 116.1(6) . . ? C19 C18 C10 122.9(7) . . ? C22 C18 C10 120.9(8) . . ? C18 C19 C20 122.7(7) . . ? C18 C19 H19 118.7 . . ? C20 C19 H19 118.7 . . ? N2 C20 C19 120.1(7) . . ? N2 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? N2 C21 C22 125.9(8) . . ? N2 C21 H21 117.0 . . ? C22 C21 H21 117.0 . . ? C21 C22 C18 119.0(8) . . ? C21 C22 H22 120.5 . . ? C18 C22 H22 120.5 . . ? C24 C23 C27 116.4(6) . . ? C24 C23 C11 124.9(7) . . ? C27 C23 C11 118.5(6) . . ? C23 C24 C25 123.0(7) . . ? C23 C24 H24 118.5 . . ? C25 C24 H24 118.5 . . ? N3 C25 C24 121.0(7) . . ? N3 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? N3 C26 C27 127.1(7) . . ? N3 C26 H26 116.4 . . ? C27 C26 H26 116.4 . . ? C26 C27 C23 115.8(6) . . ? C26 C27 H27 122.1 . . ? C23 C27 H27 122.1 . . ? C32 C28 C29 114.7(6) . . ? C32 C28 C12 125.7(6) . . ? C29 C28 C12 119.6(6) . . ? C28 C29 C30 118.7(7) . . ? C28 C29 H29 120.6 . . ? C30 C29 H29 120.6 . . ? N4 C30 C29 122.8(7) . . ? N4 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? N4 C31 C32 125.9(8) . . ? N4 C31 H31 117.0 . . ? C32 C31 H31 117.0 . . ? C31 C32 C28 121.2(8) . . ? C31 C32 H32 119.4 . . ? C28 C32 H32 119.4 . . ? O4 Cd1 N1 88.60(18) 1_554 7_554 ? O4 Cd1 N2 134.1(2) 1_554 . ? N1 Cd1 N2 92.93(19) 7_554 . ? O4 Cd1 O1 135.98(17) 1_554 . ? N1 Cd1 O1 90.88(18) 7_554 . ? N2 Cd1 O1 89.9(2) . . ? O4 Cd1 N3 94.74(18) 1_554 15_455 ? N1 Cd1 N3 175.9(2) 7_554 15_455 ? N2 Cd1 N3 86.41(18) . 15_455 ? O1 Cd1 N3 85.1(2) . 15_455 ? O4 Cd1 O2 81.6(2) 1_554 . ? N1 Cd1 O2 93.24(18) 7_554 . ? N2 Cd1 O2 143.9(2) . . ? O1 Cd1 O2 54.49(16) . . ? N3 Cd1 O2 84.99(19) 15_455 . ? O4 Cd1 C7 108.0(2) 1_554 . ? N1 Cd1 C7 94.55(19) 7_554 . ? N2 Cd1 C7 117.6(2) . . ? O1 Cd1 C7 28.24(18) . . ? N3 Cd1 C7 82.2(2) 15_455 . ? O2 Cd1 C7 26.41(19) . . ? O4 Cd1 O6 143.57(14) 1_554 . ? N1 Cd1 O6 56.09(14) 7_554 . ? N2 Cd1 O6 50.31(16) . . ? O1 Cd1 O6 61.03(12) . . ? N3 Cd1 O6 120.95(15) 15_455 . ? O2 Cd1 O6 106.75(14) . . ? C7 Cd1 O6 85.60(16) . . ? C15 N1 C16 115.6(5) . . ? C15 N1 Cd1 120.5(4) . 15_455 ? C16 N1 Cd1 123.0(4) . 15_455 ? C21 N2 C20 116.1(5) . . ? C21 N2 Cd1 124.0(6) . . ? C20 N2 Cd1 119.7(5) . . ? C26 N3 C25 115.6(6) . . ? C26 N3 Cd1 117.3(4) . 7_554 ? C25 N3 Cd1 121.5(5) . 7_554 ? C31 N4 C30 116.3(6) . . ? C7 O1 Cd1 92.0(4) . . ? C7 O2 Cd1 89.6(4) . . ? C8 O4 Cd1 108.5(5) . 1_556 ? H5D O5 H5C 109.5 . . ? O10 O6 Cd1 144.5(2) . . ? O10 O6 H6D 88.9 . . ? Cd1 O6 H6D 117.5 . . ? Cd1 O6 H6A 131.8 . . ? H6D O6 H6A 109.6 . . ? H7A O7 H7C 109.5 . . ? H8D O8 H8B 110.6 . . ? H9D O9 H9B 110.0 . . ? O6 O10 H10A 122.7 . . ? H10A O10 H10C 109.5 . . ? C9 S1 C12 93.2(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.611 _refine_diff_density_min -0.837 _refine_diff_density_rms 0.082 # Attachment 'A2.cif' data_11 _database_code_depnum_ccdc_archive 'CCDC 675549' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H20 Cd N4 O4 S, C8 H6 O4' _chemical_formula_sum 'C40 H26 Cd N4 O8 S' _chemical_formula_weight 835.11 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 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.0936(18) _cell_length_b 15.105(3) _cell_length_c 24.167(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.780(3) _cell_angle_gamma 90.00 _cell_volume 3650.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.435 _cell_measurement_theta_max 24.215 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 0.715 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20849 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7924 _reflns_number_gt 5827 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7924 _refine_ls_number_parameters 489 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0628 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 C1 C 0.2068(3) 0.38084(19) 0.42163(13) 0.0390(7) Uani 1 1 d . . . C2 C 0.0839(2) 0.37950(19) 0.45110(11) 0.0349(6) Uani 1 1 d . . . C3 C 0.0954(3) 0.3877(2) 0.50837(12) 0.0462(8) Uani 1 1 d . . . H3 H 0.1794 0.3921 0.5294 0.055 Uiso 1 1 calc R . . C4 C -0.0186(3) 0.3894(2) 0.53439(12) 0.0501(9) Uani 1 1 d . . . H4 H -0.0112 0.3959 0.5729 0.060 Uiso 1 1 calc R . . C5 C -0.1419(3) 0.3814(2) 0.50368(11) 0.0421(7) Uani 1 1 d . . . H5 H -0.2179 0.3834 0.5215 0.051 Uiso 1 1 calc R . . C6 C -0.1551(2) 0.37055(18) 0.44642(11) 0.0327(6) Uani 1 1 d . . . C7 C -0.0407(2) 0.37059(18) 0.42051(11) 0.0345(7) Uani 1 1 d . . . H7 H -0.0482 0.3645 0.3819 0.041 Uiso 1 1 calc R . . C8 C -0.2903(3) 0.36189(18) 0.41305(13) 0.0376(7) Uani 1 1 d . . . C9 C 0.3664(3) 0.5865(2) 0.34088(12) 0.0493(8) Uani 1 1 d . . . H9 H 0.3279 0.5616 0.3073 0.059 Uiso 1 1 calc R . . C10 C 0.3459(3) 0.6744(2) 0.34929(12) 0.0481(8) Uani 1 1 d . . . H10 H 0.2951 0.7080 0.3219 0.058 Uiso 1 1 calc R . . C11 C 0.4014(3) 0.71312(18) 0.39903(11) 0.0324(7) Uani 1 1 d . . . C12 C 0.4754(3) 0.65934(18) 0.43757(11) 0.0354(7) Uani 1 1 d . . . H12 H 0.5140 0.6821 0.4718 0.042 Uiso 1 1 calc R . . C13 C 0.4917(3) 0.57166(18) 0.42483(11) 0.0360(7) Uani 1 1 d . . . H13 H 0.5435 0.5366 0.4510 0.043 Uiso 1 1 calc R . . C14 C 0.3778(3) 0.80626(18) 0.41141(10) 0.0348(7) Uani 1 1 d . . . C15 C 0.3914(2) 0.88137(18) 0.38066(10) 0.0313(6) Uani 1 1 d . . . C16 C 0.3537(3) 0.95955(18) 0.40812(11) 0.0318(7) Uani 1 1 d . . . C17 C 0.3108(3) 0.94187(18) 0.45875(11) 0.0349(7) Uani 1 1 d . . . C18 C 0.2658(3) 1.00391(19) 0.49954(11) 0.0379(7) Uani 1 1 d . . . C19 C 0.1734(3) 0.9765(2) 0.53357(12) 0.0509(9) Uani 1 1 d . . . H19 H 0.1393 0.9192 0.5310 0.061 Uiso 1 1 calc R . . C20 C 0.1333(3) 1.0355(3) 0.57120(13) 0.0621(10) Uani 1 1 d . . . H20 H 0.0721 1.0160 0.5940 0.074 Uiso 1 1 calc R . . C21 C 0.2645(3) 1.1433(2) 0.54506(13) 0.0552(9) Uani 1 1 d . . . H21 H 0.2957 1.2012 0.5484 0.066 Uiso 1 1 calc R . . C22 C 0.3135(3) 1.0885(2) 0.50697(11) 0.0458(8) Uani 1 1 d . . . H22 H 0.3786 1.1090 0.4864 0.055 Uiso 1 1 calc R . . C23 C 0.3650(3) 1.05021(17) 0.38640(10) 0.0307(6) Uani 1 1 d . . . C24 C 0.4889(3) 1.08527(19) 0.38055(11) 0.0378(7) Uani 1 1 d . . . H24 H 0.5648 1.0497 0.3859 0.045 Uiso 1 1 calc R . . C25 C 0.4989(3) 1.17256(19) 0.36685(11) 0.0414(7) Uani 1 1 d . . . H25 H 0.5833 1.1952 0.3638 0.050 Uiso 1 1 calc R . . C26 C 0.2737(3) 1.19111(19) 0.35986(11) 0.0414(7) Uani 1 1 d . . . H26 H 0.1987 1.2269 0.3516 0.050 Uiso 1 1 calc R . . C27 C 0.2555(3) 1.10455(18) 0.37372(11) 0.0398(7) Uani 1 1 d . . . H27 H 0.1698 1.0825 0.3746 0.048 Uiso 1 1 calc R . . C28 C 0.4416(3) 0.88391(18) 0.32594(10) 0.0317(6) Uani 1 1 d . . . C29 C 0.3827(3) 0.93808(18) 0.28339(11) 0.0362(7) Uani 1 1 d . . . H29 H 0.3083 0.9719 0.2884 0.043 Uiso 1 1 calc R . . C30 C 0.4346(3) 0.94158(19) 0.23391(11) 0.0392(7) Uani 1 1 d . . . H30 H 0.3942 0.9793 0.2062 0.047 Uiso 1 1 calc R . . C31 C 0.5947(3) 0.8412(2) 0.26397(11) 0.0409(7) Uani 1 1 d . . . H31 H 0.6676 0.8069 0.2574 0.049 Uiso 1 1 calc R . . C32 C 0.5507(3) 0.83412(18) 0.31502(11) 0.0389(7) Uani 1 1 d . . . H32 H 0.5936 0.7963 0.3421 0.047 Uiso 1 1 calc R . . C33 C -0.1435(3) 0.1727(3) 0.31073(15) 0.0596(10) Uani 1 1 d . . . C34 C -0.0632(3) 0.1299(2) 0.27009(12) 0.0484(8) Uani 1 1 d . . . C35 C -0.0506(3) 0.0396(2) 0.26817(14) 0.0623(10) Uani 1 1 d . . . H35 H -0.0926 0.0043 0.2921 0.075 Uiso 1 1 calc R . . C36 C 0.0241(4) 0.0009(3) 0.23104(15) 0.0668(10) Uani 1 1 d . . . H36 H 0.0312 -0.0605 0.2294 0.080 Uiso 1 1 calc R . . C37 C 0.0884(3) 0.0533(2) 0.19628(13) 0.0595(10) Uani 1 1 d . . . H37 H 0.1404 0.0273 0.1717 0.071 Uiso 1 1 calc R . . C38 C 0.0757(3) 0.1437(2) 0.19780(12) 0.0476(8) Uani 1 1 d . . . C39 C -0.0007(3) 0.1826(2) 0.23435(12) 0.0461(8) Uani 1 1 d . . . H39 H -0.0102 0.2438 0.2350 0.055 Uiso 1 1 calc R . . C40 C 0.1421(3) 0.2006(3) 0.15895(13) 0.0560(10) Uani 1 1 d . . . Cd1 Cd 0.429236(19) 0.379931(13) 0.371404(8) 0.03008(6) Uani 1 1 d . . . N1 N 0.4380(2) 0.53421(14) 0.37765(9) 0.0361(6) Uani 1 1 d . . . N2 N 0.1753(3) 1.1174(2) 0.57722(10) 0.0574(7) Uani 1 1 d . . . N3 N 0.3944(2) 1.22689(15) 0.35758(9) 0.0386(6) Uani 1 1 d . . . N4 N 0.5392(2) 0.89433(15) 0.22296(9) 0.0361(6) Uani 1 1 d . . . O1 O 0.19344(17) 0.38893(13) 0.37006(8) 0.0395(5) Uani 1 1 d . . . O2 O 0.31806(18) 0.37286(15) 0.45098(8) 0.0567(6) Uani 1 1 d . . . O3 O -0.30165(18) 0.34317(15) 0.36238(8) 0.0516(6) Uani 1 1 d . . . O4 O -0.39050(17) 0.37457(13) 0.43777(8) 0.0463(5) Uani 1 1 d . . . O5 O -0.1680(2) 0.25539(17) 0.29992(9) 0.0702(7) Uani 1 1 d . . . H5A H -0.2105 0.2762 0.3234 0.105 Uiso 1 1 calc R . . O6 O -0.1825(3) 0.1331(2) 0.34820(12) 0.1138(12) Uani 1 1 d . . . O7 O 0.0911(3) 0.27982(18) 0.15375(10) 0.0767(8) Uani 1 1 d . . . H7A H 0.1227 0.3065 0.1290 0.115 Uiso 1 1 calc R . . O8 O 0.2332(2) 0.17493(17) 0.13533(9) 0.0724(8) Uani 1 1 d . . . S1 S 0.31803(8) 0.83079(5) 0.47296(3) 0.0439(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0298(16) 0.0380(18) 0.0504(19) 0.0015(16) 0.0098(14) 0.0013(15) C2 0.0274(14) 0.0408(18) 0.0374(17) 0.0033(14) 0.0080(13) 0.0011(14) C3 0.0308(16) 0.067(2) 0.0392(18) -0.0002(16) 0.0004(14) 0.0001(16) C4 0.0416(18) 0.080(3) 0.0294(17) -0.0015(16) 0.0092(14) 0.0035(18) C5 0.0305(16) 0.058(2) 0.0408(18) 0.0004(16) 0.0149(13) -0.0007(16) C6 0.0248(14) 0.0349(17) 0.0397(17) 0.0009(13) 0.0086(12) 0.0007(13) C7 0.0323(15) 0.0396(18) 0.0325(16) 0.0003(13) 0.0077(12) 0.0034(14) C8 0.0311(16) 0.0308(18) 0.052(2) 0.0070(14) 0.0076(15) -0.0015(13) C9 0.065(2) 0.039(2) 0.0395(19) -0.0094(15) -0.0086(16) 0.0004(17) C10 0.066(2) 0.0343(19) 0.0405(19) 0.0040(14) -0.0065(16) 0.0095(16) C11 0.0415(17) 0.0277(16) 0.0294(16) -0.0016(12) 0.0096(13) -0.0028(13) C12 0.0466(18) 0.0316(17) 0.0278(16) -0.0009(13) 0.0047(13) -0.0013(14) C13 0.0426(18) 0.0321(18) 0.0330(17) 0.0028(13) 0.0042(14) 0.0015(14) C14 0.0458(18) 0.0324(17) 0.0272(16) -0.0027(12) 0.0088(13) 0.0009(14) C15 0.0382(16) 0.0283(15) 0.0282(15) 0.0021(13) 0.0074(12) -0.0002(14) C16 0.0379(16) 0.0286(16) 0.0302(16) 0.0002(12) 0.0094(13) 0.0013(13) C17 0.0442(17) 0.0283(17) 0.0341(17) -0.0007(13) 0.0118(14) -0.0016(13) C18 0.0477(19) 0.0368(18) 0.0304(17) 0.0020(13) 0.0097(14) 0.0059(15) C19 0.067(2) 0.042(2) 0.048(2) -0.0006(15) 0.0262(18) 0.0001(17) C20 0.075(3) 0.071(3) 0.047(2) 0.0006(19) 0.0336(19) 0.006(2) C21 0.071(2) 0.045(2) 0.050(2) -0.0125(16) 0.0105(18) -0.0018(18) C22 0.054(2) 0.045(2) 0.0420(19) -0.0121(15) 0.0194(16) -0.0053(16) C23 0.0410(17) 0.0271(16) 0.0259(15) -0.0026(12) 0.0109(13) 0.0009(13) C24 0.0383(17) 0.0344(18) 0.0431(18) -0.0015(13) 0.0140(14) 0.0057(14) C25 0.0442(19) 0.0347(19) 0.050(2) 0.0006(14) 0.0218(15) -0.0021(15) C26 0.0423(18) 0.0334(18) 0.0471(19) 0.0009(14) 0.0014(15) 0.0030(15) C27 0.0381(17) 0.0330(19) 0.0492(19) -0.0022(14) 0.0094(14) -0.0069(14) C28 0.0401(16) 0.0264(15) 0.0300(15) -0.0030(13) 0.0093(12) -0.0017(14) C29 0.0411(17) 0.0356(18) 0.0337(17) -0.0012(13) 0.0109(14) 0.0121(14) C30 0.0518(19) 0.0355(18) 0.0308(17) 0.0034(13) 0.0069(15) 0.0086(15) C31 0.0448(18) 0.0446(19) 0.0344(18) -0.0030(14) 0.0090(14) 0.0138(15) C32 0.0514(19) 0.0350(18) 0.0306(17) 0.0045(13) 0.0069(14) 0.0108(15) C33 0.058(2) 0.068(3) 0.057(2) 0.018(2) 0.0193(19) 0.005(2) C34 0.0435(18) 0.064(3) 0.0378(19) 0.0087(17) 0.0061(14) -0.0065(18) C35 0.066(2) 0.063(3) 0.058(2) 0.0190(19) 0.0068(19) -0.007(2) C36 0.083(3) 0.050(2) 0.068(3) 0.005(2) 0.010(2) 0.002(2) C37 0.062(2) 0.068(3) 0.049(2) -0.0066(18) 0.0083(18) -0.002(2) C38 0.0463(19) 0.060(3) 0.0368(19) -0.0013(15) 0.0069(15) -0.0073(17) C39 0.045(2) 0.050(2) 0.042(2) 0.0031(15) 0.0052(15) -0.0073(16) C40 0.056(2) 0.074(3) 0.039(2) -0.0103(19) 0.0075(18) -0.017(2) Cd1 0.03299(11) 0.02744(11) 0.03134(12) -0.00020(10) 0.00988(8) -0.00189(10) N1 0.0460(15) 0.0286(14) 0.0333(14) -0.0012(11) 0.0040(12) -0.0019(12) N2 0.073(2) 0.061(2) 0.0418(16) -0.0088(15) 0.0227(14) 0.0110(17) N3 0.0436(15) 0.0315(15) 0.0423(15) 0.0018(11) 0.0115(12) -0.0024(12) N4 0.0422(14) 0.0362(15) 0.0317(13) 0.0007(11) 0.0115(11) 0.0066(12) O1 0.0343(11) 0.0492(14) 0.0364(12) 0.0047(10) 0.0100(9) 0.0032(10) O2 0.0258(11) 0.100(2) 0.0448(13) 0.0052(12) 0.0072(10) 0.0034(12) O3 0.0352(12) 0.0788(17) 0.0401(13) -0.0039(11) 0.0020(10) -0.0068(11) O4 0.0248(10) 0.0624(15) 0.0534(13) -0.0016(11) 0.0111(9) 0.0041(10) O5 0.0879(19) 0.0669(19) 0.0640(17) -0.0006(13) 0.0396(14) -0.0049(15) O6 0.145(3) 0.108(3) 0.109(2) 0.0533(19) 0.090(2) 0.033(2) O7 0.099(2) 0.073(2) 0.0670(19) 0.0196(14) 0.0466(15) -0.0028(17) O8 0.0662(16) 0.091(2) 0.0668(17) -0.0189(14) 0.0338(14) -0.0225(14) S1 0.0671(6) 0.0312(4) 0.0377(5) 0.0022(3) 0.0222(4) -0.0005(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 C1 O1 1.241(3) . ? C1 O2 1.250(3) . ? C1 C2 1.512(3) . ? C2 C7 1.377(3) . ? C2 C3 1.379(3) . ? C3 C4 1.385(3) . ? C3 H3 0.9300 . ? C4 C5 1.365(4) . ? C4 H4 0.9300 . ? C5 C6 1.382(3) . ? C5 H5 0.9300 . ? C6 C7 1.386(3) . ? C6 C8 1.494(4) . ? C7 H7 0.9300 . ? C8 O3 1.247(3) . ? C8 O4 1.256(3) . ? C9 N1 1.328(3) . ? C9 C10 1.364(4) . ? C9 H9 0.9300 . ? C10 C11 1.385(4) . ? C10 H10 0.9300 . ? C11 C12 1.377(3) . ? C11 C14 1.464(4) . ? C12 C13 1.374(4) . ? C12 H12 0.9300 . ? C13 N1 1.321(3) . ? C13 H13 0.9300 . ? C14 C15 1.373(3) . ? C14 S1 1.720(3) . ? C15 C16 1.431(3) . ? C15 C28 1.480(3) . ? C16 C17 1.378(3) . ? C16 C23 1.477(3) . ? C17 C18 1.476(4) . ? C17 S1 1.712(3) . ? C18 C22 1.369(4) . ? C18 C19 1.388(3) . ? C19 C20 1.374(4) . ? C19 H19 0.9300 . ? C20 N2 1.309(4) . ? C20 H20 0.9300 . ? C21 N2 1.325(4) . ? C21 C22 1.377(4) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C27 1.378(3) . ? C23 C24 1.382(3) . ? C24 C25 1.367(4) . ? C24 H24 0.9300 . ? C25 N3 1.331(3) . ? C25 H25 0.9300 . ? C26 N3 1.341(3) . ? C26 C27 1.368(4) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.384(3) . ? C28 C32 1.388(3) . ? C29 C30 1.370(3) . ? C29 H29 0.9300 . ? C30 N4 1.330(3) . ? C30 H30 0.9300 . ? C31 N4 1.338(3) . ? C31 C32 1.371(3) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O6 1.195(3) . ? C33 O5 1.293(4) . ? C33 C34 1.502(4) . ? C34 C35 1.371(4) . ? C34 C39 1.388(4) . ? C35 C36 1.378(4) . ? C35 H35 0.9300 . ? C36 C37 1.378(4) . ? C36 H36 0.9300 . ? C37 C38 1.373(4) . ? C37 H37 0.9300 . ? C38 C39 1.380(4) . ? C38 C40 1.497(4) . ? C39 H39 0.9300 . ? C40 O8 1.210(3) . ? C40 O7 1.302(4) . ? Cd1 O4 2.2582(18) 1_655 ? Cd1 N1 2.336(2) . ? Cd1 N4 2.355(2) 2_645 ? Cd1 N3 2.355(2) 1_545 ? Cd1 O2 2.3565(18) . ? Cd1 O1 2.3797(17) . ? N3 Cd1 2.355(2) 1_565 ? N4 Cd1 2.355(2) 2_655 ? O4 Cd1 2.2582(18) 1_455 ? O5 H5A 0.8200 . ? O7 H7A 0.8200 . ? 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 C1 O2 123.1(2) . . ? O1 C1 C2 119.3(3) . . ? O2 C1 C2 117.6(3) . . ? C7 C2 C3 119.7(2) . . ? C7 C2 C1 119.8(2) . . ? C3 C2 C1 120.6(2) . . ? C2 C3 C4 119.7(3) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 120.3(3) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.8(2) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C7 118.6(2) . . ? C5 C6 C8 120.5(2) . . ? C7 C6 C8 120.8(2) . . ? C2 C7 C6 120.9(2) . . ? C2 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? O3 C8 O4 121.9(3) . . ? O3 C8 C6 120.4(2) . . ? O4 C8 C6 117.7(3) . . ? N1 C9 C10 124.0(3) . . ? N1 C9 H9 118.0 . . ? C10 C9 H9 118.0 . . ? C9 C10 C11 119.2(3) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 117.2(3) . . ? C12 C11 C14 121.1(2) . . ? C10 C11 C14 121.7(3) . . ? C13 C12 C11 119.2(3) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? N1 C13 C12 123.9(3) . . ? N1 C13 H13 118.0 . . ? C12 C13 H13 118.0 . . ? C15 C14 C11 130.7(2) . . ? C15 C14 S1 111.2(2) . . ? C11 C14 S1 118.0(2) . . ? C14 C15 C16 112.3(2) . . ? C14 C15 C28 125.2(2) . . ? C16 C15 C28 122.5(2) . . ? C17 C16 C15 112.8(2) . . ? C17 C16 C23 123.0(2) . . ? C15 C16 C23 124.2(2) . . ? C16 C17 C18 129.2(3) . . ? C16 C17 S1 111.0(2) . . ? C18 C17 S1 119.8(2) . . ? C22 C18 C19 117.0(3) . . ? C22 C18 C17 123.1(3) . . ? C19 C18 C17 119.9(3) . . ? C20 C19 C18 118.7(3) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? N2 C20 C19 124.6(3) . . ? N2 C20 H20 117.7 . . ? C19 C20 H20 117.7 . . ? N2 C21 C22 123.3(3) . . ? N2 C21 H21 118.4 . . ? C22 C21 H21 118.4 . . ? C18 C22 C21 119.8(3) . . ? C18 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C27 C23 C24 117.3(3) . . ? C27 C23 C16 122.2(2) . . ? C24 C23 C16 120.4(3) . . ? C25 C24 C23 119.5(3) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? N3 C25 C24 123.5(3) . . ? N3 C25 H25 118.2 . . ? C24 C25 H25 118.2 . . ? N3 C26 C27 123.2(3) . . ? N3 C26 H26 118.4 . . ? C27 C26 H26 118.4 . . ? C26 C27 C23 119.6(3) . . ? C26 C27 H27 120.2 . . ? C23 C27 H27 120.2 . . ? C29 C28 C32 116.8(2) . . ? C29 C28 C15 121.0(2) . . ? C32 C28 C15 122.2(2) . . ? C30 C29 C28 119.7(2) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? N4 C30 C29 124.1(3) . . ? N4 C30 H30 118.0 . . ? C29 C30 H30 118.0 . . ? N4 C31 C32 124.0(3) . . ? N4 C31 H31 118.0 . . ? C32 C31 H31 118.0 . . ? C31 C32 C28 119.4(3) . . ? C31 C32 H32 120.3 . . ? C28 C32 H32 120.3 . . ? O6 C33 O5 124.3(4) . . ? O6 C33 C34 122.8(4) . . ? O5 C33 C34 112.9(3) . . ? C35 C34 C39 119.8(3) . . ? C35 C34 C33 120.8(3) . . ? C39 C34 C33 119.4(3) . . ? C34 C35 C36 120.4(3) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C37 119.8(4) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C38 C37 C36 120.1(3) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C39 120.2(3) . . ? C37 C38 C40 120.3(3) . . ? C39 C38 C40 119.5(3) . . ? C38 C39 C34 119.6(3) . . ? C38 C39 H39 120.2 . . ? C34 C39 H39 120.2 . . ? O8 C40 O7 124.4(3) . . ? O8 C40 C38 123.0(4) . . ? O7 C40 C38 112.6(3) . . ? O4 Cd1 N1 88.28(8) 1_655 . ? O4 Cd1 N4 119.30(7) 1_655 2_645 ? N1 Cd1 N4 87.80(8) . 2_645 ? O4 Cd1 N3 98.97(8) 1_655 1_545 ? N1 Cd1 N3 172.70(8) . 1_545 ? N4 Cd1 N3 89.45(7) 2_645 1_545 ? O4 Cd1 O2 81.12(6) 1_655 . ? N1 Cd1 O2 90.61(8) . . ? N4 Cd1 O2 159.43(7) 2_645 . ? N3 Cd1 O2 89.60(8) 1_545 . ? O4 Cd1 O1 136.05(6) 1_655 . ? N1 Cd1 O1 88.46(7) . . ? N4 Cd1 O1 104.34(7) 2_645 . ? N3 Cd1 O1 85.67(7) 1_545 . ? O2 Cd1 O1 55.10(6) . . ? C13 N1 C9 116.4(2) . . ? C13 N1 Cd1 119.37(18) . . ? C9 N1 Cd1 122.52(19) . . ? C20 N2 C21 116.6(3) . . ? C25 N3 C26 116.6(3) . . ? C25 N3 Cd1 118.80(19) . 1_565 ? C26 N3 Cd1 120.57(19) . 1_565 ? C30 N4 C31 116.0(2) . . ? C30 N4 Cd1 117.21(18) . 2_655 ? C31 N4 Cd1 124.30(18) . 2_655 ? C1 O1 Cd1 90.48(16) . . ? C1 O2 Cd1 91.34(16) . . ? C8 O4 Cd1 106.90(18) . 1_455 ? C33 O5 H5A 109.5 . . ? C40 O7 H7A 109.5 . . ? C17 S1 C14 92.75(13) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.878 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.066