# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global ## Crystallographic Data for compound 1 data_Zn #TrackingRef 'web_deposit_cif_file_0_Qing-YanLiu_1361176667.Zn Cd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H17 N2 O6 S Zn' _chemical_formula_weight 442.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.440(5) _cell_length_b 8.974(3) _cell_length_c 18.728(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.099(5) _cell_angle_gamma 90.00 _cell_volume 3421.7(17) _cell_formula_units_Z 8 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 2492 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 27.38 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.719 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 1.597 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6373 _exptl_absorpt_correction_T_max 0.8439 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10406 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 28.70 _reflns_number_total 4140 _reflns_number_gt 3025 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1034P)^2^+35.5777P] 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 4140 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.2076 _refine_ls_wR_factor_gt 0.1898 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 Zn1 Zn 0.0000 0.67396(9) 0.2500 0.0259(2) Uani 1 2 d S . . Zn2 Zn 0.0000 0.5000 0.0000 0.0246(2) Uani 1 2 d S . . S1 S -0.11150(14) 0.7613(3) -0.02740(12) 0.0699(6) Uani 1 1 d . . . O2 O -0.0026(2) 0.8197(4) 0.17129(19) 0.0371(10) Uani 1 1 d . . . O3 O -0.0816(2) 0.6230(4) -0.0407(2) 0.0348(9) Uani 1 1 d . . . O1 O 0.0049(2) 0.6347(4) 0.09448(19) 0.0293(8) Uani 1 1 d . . . O5 O -0.1440(3) 0.7568(10) 0.0356(4) 0.103(3) Uani 1 1 d . . . O4 O -0.1551(3) 0.8152(7) -0.0780(5) 0.090(2) Uani 1 1 d . . . N1 N 0.0897(2) 0.5733(5) 0.2601(2) 0.0285(9) Uani 1 1 d . . . N2 N 0.4379(2) 0.8555(5) 0.0565(2) 0.0292(10) Uani 1 1 d . . . C13 C 0.3790(3) 0.8116(7) 0.0287(3) 0.0379(13) Uani 1 1 d . . . H13A H 0.3632 0.8490 -0.0158 0.045 Uiso 1 1 calc R . . C2 C -0.0460(3) 0.8848(6) -0.0108(3) 0.0260(10) Uani 1 1 d . . . C4 C -0.0003(3) 0.7700(6) 0.1088(3) 0.0254(10) Uani 1 1 d . . . C5 C 0.1141(3) 0.5007(6) 0.2051(3) 0.0323(12) Uani 1 1 d . . . H5B H 0.0875 0.4897 0.1625 0.039 Uiso 1 1 calc R . . C15 C 0.3622(3) 0.6537(6) 0.1286(3) 0.0330(12) Uani 1 1 d . . . C11 C 0.3361(3) 0.5179(7) 0.2442(3) 0.0391(14) Uani 1 1 d . . . H11A H 0.3344 0.6122 0.2693 0.047 Uiso 1 1 calc R . . H11B H 0.3806 0.4797 0.2523 0.047 Uiso 1 1 calc R . . C1 C -0.0025(3) 0.8863(6) 0.0507(2) 0.0246(10) Uani 1 1 d . . . C7 C 0.2188(3) 0.4617(6) 0.2704(3) 0.0288(11) Uani 1 1 d . . . C9 C 0.1294(3) 0.5882(7) 0.3197(3) 0.0340(12) Uani 1 1 d . . . H9A H 0.1134 0.6363 0.3586 0.041 Uiso 1 1 calc R . . C3 C -0.0431(3) 0.9977(6) -0.0602(3) 0.0278(11) Uani 1 1 d . . . H3 H -0.0724 0.9968 -0.1012 0.033 Uiso 1 1 calc R . . C16 C 0.4235(3) 0.7005(7) 0.1577(3) 0.0370(13) Uani 1 1 d . . . H16A H 0.4405 0.6649 0.2022 0.044 Uiso 1 1 calc R . . C17 C 0.4591(3) 0.7997(7) 0.1207(3) 0.0354(13) Uani 1 1 d . . . H17A H 0.5001 0.8295 0.1414 0.042 Uiso 1 1 calc R . . C6 C 0.1764(3) 0.4424(7) 0.2093(3) 0.0341(12) Uani 1 1 d . . . H6A H 0.1903 0.3895 0.1707 0.041 Uiso 1 1 calc R . . C12 C 0.3200(3) 0.5441(8) 0.1645(3) 0.0453(16) Uani 1 1 d . . . H12A H 0.3224 0.4491 0.1402 0.054 Uiso 1 1 calc R . . H12B H 0.2748 0.5779 0.1571 0.054 Uiso 1 1 calc R . . C10 C 0.2888(3) 0.4078(7) 0.2754(3) 0.0370(13) Uani 1 1 d . . . H10A H 0.2905 0.3137 0.2501 0.044 Uiso 1 1 calc R . . H10B H 0.3034 0.3897 0.3254 0.044 Uiso 1 1 calc R . . C8 C 0.1937(3) 0.5357(7) 0.3273(3) 0.0367(13) Uani 1 1 d . . . H8A H 0.2197 0.5500 0.3700 0.044 Uiso 1 1 calc R . . C14 C 0.3406(3) 0.7138(8) 0.0624(3) 0.0414(14) Uani 1 1 d . . . H14A H 0.2995 0.6874 0.0408 0.050 Uiso 1 1 calc R . . O1W O 0.2378(4) 0.4514(9) 0.0099(5) 0.119(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 Zn1 0.0337(5) 0.0244(4) 0.0203(4) 0.000 0.0063(3) 0.000 Zn2 0.0339(5) 0.0187(4) 0.0220(4) -0.0007(3) 0.0078(3) -0.0040(3) S1 0.1010(18) 0.0524(12) 0.0557(12) -0.0008(10) 0.0036(12) -0.0105(12) O2 0.067(3) 0.028(2) 0.0165(17) 0.0013(15) 0.0096(18) -0.0005(19) O3 0.037(2) 0.0204(18) 0.047(2) 0.0006(16) 0.0022(18) -0.0022(15) O1 0.046(2) 0.0196(17) 0.0229(18) 0.0003(14) 0.0037(16) -0.0018(15) O5 0.072(4) 0.133(7) 0.109(6) -0.027(5) 0.036(4) -0.003(5) O4 0.050(3) 0.058(4) 0.154(7) -0.011(4) -0.026(4) 0.009(3) N1 0.032(2) 0.028(2) 0.026(2) 0.0024(18) 0.0074(18) 0.0013(18) N2 0.037(3) 0.023(2) 0.028(2) 0.0009(17) 0.0115(19) -0.0029(18) C13 0.039(3) 0.038(3) 0.036(3) 0.007(3) 0.005(2) -0.005(2) C2 0.033(3) 0.024(2) 0.021(2) -0.0010(19) 0.007(2) -0.004(2) C4 0.034(3) 0.022(2) 0.021(2) -0.0012(19) 0.006(2) -0.0037(19) C5 0.035(3) 0.033(3) 0.030(3) -0.005(2) 0.005(2) -0.006(2) C15 0.040(3) 0.029(3) 0.032(3) 0.004(2) 0.014(2) -0.001(2) C11 0.034(3) 0.039(3) 0.045(3) 0.005(3) 0.008(3) -0.004(2) C1 0.036(3) 0.021(2) 0.017(2) 0.0009(18) 0.0065(19) 0.000(2) C7 0.030(3) 0.024(2) 0.034(3) 0.006(2) 0.010(2) -0.002(2) C9 0.035(3) 0.041(3) 0.027(3) -0.004(2) 0.008(2) 0.000(2) C3 0.040(3) 0.024(3) 0.019(2) -0.0010(19) 0.000(2) -0.002(2) C16 0.042(3) 0.042(3) 0.027(3) 0.008(2) 0.006(2) -0.009(3) C17 0.038(3) 0.036(3) 0.033(3) 0.001(2) 0.006(2) -0.012(2) C6 0.040(3) 0.031(3) 0.033(3) -0.002(2) 0.010(2) -0.003(2) C12 0.047(4) 0.052(4) 0.037(3) 0.009(3) 0.009(3) -0.021(3) C10 0.036(3) 0.038(3) 0.038(3) 0.013(3) 0.011(2) 0.002(2) C8 0.037(3) 0.047(3) 0.026(3) 0.003(2) 0.002(2) -0.002(3) C14 0.038(3) 0.048(4) 0.038(3) 0.008(3) 0.002(3) -0.012(3) O1W 0.118(7) 0.090(6) 0.143(8) -0.020(6) -0.017(6) 0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2 1.968(4) 2 ? Zn1 O2 1.968(4) . ? Zn1 N1 2.038(5) 2 ? Zn1 N1 2.038(5) . ? Zn2 O3 2.087(4) 5_565 ? Zn2 O3 2.087(4) . ? Zn2 O1 2.138(4) . ? Zn2 O1 2.138(4) 5_565 ? Zn2 N2 2.156(4) 7_565 ? Zn2 N2 2.156(4) 3_445 ? S1 O4 1.332(7) . ? S1 O5 1.406(7) . ? S1 O3 1.415(5) . ? S1 C2 1.744(6) . ? O2 C4 1.258(6) . ? O1 C4 1.250(6) . ? N1 C9 1.328(7) . ? N1 C5 1.350(7) . ? N2 C13 1.329(8) . ? N2 C17 1.338(7) . ? N2 Zn2 2.156(4) 3 ? C13 C14 1.370(8) . ? C13 H13A 0.9300 . ? C2 C3 1.377(7) . ? C2 C1 1.393(7) . ? C4 C1 1.505(7) . ? C5 C6 1.373(8) . ? C5 H5B 0.9300 . ? C15 C16 1.386(9) . ? C15 C14 1.387(8) . ? C15 C12 1.507(7) . ? C11 C12 1.519(9) . ? C11 C10 1.535(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C1 C3 1.398(7) 5_575 ? C7 C6 1.382(8) . ? C7 C8 1.392(8) . ? C7 C10 1.505(8) . ? C9 C8 1.391(8) . ? C9 H9A 0.9300 . ? C3 C1 1.398(7) 5_575 ? C3 H3 0.9300 . ? C16 C17 1.376(7) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C6 H6A 0.9300 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C8 H8A 0.9300 . ? C14 H14A 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 O2 Zn1 O2 96.7(2) 2 . ? O2 Zn1 N1 109.14(18) 2 2 ? O2 Zn1 N1 105.13(18) . 2 ? O2 Zn1 N1 105.13(18) 2 . ? O2 Zn1 N1 109.14(18) . . ? N1 Zn1 N1 127.4(3) 2 . ? O3 Zn2 O3 180.0(3) 5_565 . ? O3 Zn2 O1 91.13(15) 5_565 . ? O3 Zn2 O1 88.87(15) . . ? O3 Zn2 O1 88.87(15) 5_565 5_565 ? O3 Zn2 O1 91.13(15) . 5_565 ? O1 Zn2 O1 180.00(11) . 5_565 ? O3 Zn2 N2 90.67(17) 5_565 7_565 ? O3 Zn2 N2 89.33(17) . 7_565 ? O1 Zn2 N2 94.61(15) . 7_565 ? O1 Zn2 N2 85.39(15) 5_565 7_565 ? O3 Zn2 N2 89.33(17) 5_565 3_445 ? O3 Zn2 N2 90.67(17) . 3_445 ? O1 Zn2 N2 85.39(15) . 3_445 ? O1 Zn2 N2 94.61(15) 5_565 3_445 ? N2 Zn2 N2 180.0(2) 7_565 3_445 ? O4 S1 O5 105.7(5) . . ? O4 S1 O3 117.7(4) . . ? O5 S1 O3 111.5(4) . . ? O4 S1 C2 110.5(4) . . ? O5 S1 C2 106.3(4) . . ? O3 S1 C2 104.6(3) . . ? C4 O2 Zn1 117.4(3) . . ? S1 O3 Zn2 138.0(3) . . ? C4 O1 Zn2 136.7(3) . . ? C9 N1 C5 116.8(5) . . ? C9 N1 Zn1 120.7(4) . . ? C5 N1 Zn1 122.2(4) . . ? C13 N2 C17 116.8(5) . . ? C13 N2 Zn2 122.5(4) . 3 ? C17 N2 Zn2 120.6(4) . 3 ? N2 C13 C14 123.1(6) . . ? N2 C13 H13A 118.5 . . ? C14 C13 H13A 118.5 . . ? C3 C2 C1 119.1(5) . . ? C3 C2 S1 115.2(4) . . ? C1 C2 S1 125.3(4) . . ? O1 C4 O2 123.7(5) . . ? O1 C4 C1 121.1(4) . . ? O2 C4 C1 115.2(4) . . ? N1 C5 C6 122.9(5) . . ? N1 C5 H5B 118.5 . . ? C6 C5 H5B 118.5 . . ? C16 C15 C14 116.1(5) . . ? C16 C15 C12 123.8(5) . . ? C14 C15 C12 120.2(6) . . ? C12 C11 C10 112.6(5) . . ? C12 C11 H11A 109.1 . . ? C10 C11 H11A 109.1 . . ? C12 C11 H11B 109.1 . . ? C10 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? C2 C1 C3 118.8(5) . 5_575 ? C2 C1 C4 124.6(5) . . ? C3 C1 C4 116.6(5) 5_575 . ? C6 C7 C8 116.5(5) . . ? C6 C7 C10 122.2(5) . . ? C8 C7 C10 121.2(5) . . ? N1 C9 C8 123.5(5) . . ? N1 C9 H9A 118.2 . . ? C8 C9 H9A 118.2 . . ? C2 C3 C1 122.0(5) . 5_575 ? C2 C3 H3 119.0 . . ? C1 C3 H3 119.0 5_575 . ? C17 C16 C15 119.8(5) . . ? C17 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? N2 C17 C16 123.5(6) . . ? N2 C17 H17A 118.3 . . ? C16 C17 H17A 118.3 . . ? C5 C6 C7 120.6(5) . . ? C5 C6 H6A 119.7 . . ? C7 C6 H6A 119.7 . . ? C15 C12 C11 117.2(5) . . ? C15 C12 H12A 108.0 . . ? C11 C12 H12A 108.0 . . ? C15 C12 H12B 108.0 . . ? C11 C12 H12B 108.0 . . ? H12A C12 H12B 107.2 . . ? C7 C10 C11 113.4(5) . . ? C7 C10 H10A 108.9 . . ? C11 C10 H10A 108.9 . . ? C7 C10 H10B 108.9 . . ? C11 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C9 C8 C7 119.5(5) . . ? C9 C8 H8A 120.2 . . ? C7 C8 H8A 120.2 . . ? C13 C14 C15 120.7(6) . . ? C13 C14 H14A 119.6 . . ? C15 C14 H14A 119.6 . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.699 _refine_diff_density_min -1.838 _refine_diff_density_rms 0.156 _database_code_depnum_ccdc_archive 'CCDC 924894' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global #===END OF 1 ## Crystallographic Data for compound 2 data_Cd #TrackingRef 'web_deposit_cif_file_0_Qing-YanLiu_1361176667.Zn Cd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H45 Cd4 N6 O18 S2' _chemical_formula_weight 1615.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.3069(17) _cell_length_b 9.3535(6) _cell_length_c 25.2396(18) _cell_angle_alpha 90.00 _cell_angle_beta 101.6200(10) _cell_angle_gamma 90.00 _cell_volume 5620.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3968 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 25.23 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.909 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3188 _exptl_absorpt_coefficient_mu 1.649 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6463 _exptl_absorpt_correction_T_max 0.7669 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17216 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 29.08 _reflns_number_total 6924 _reflns_number_gt 5078 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+3.8492P] 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 6924 _refine_ls_number_parameters 393 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0874 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 0.227770(11) 0.82287(3) 0.082449(12) 0.02793(9) Uani 1 1 d . . . Cd2 Cd 0.071909(11) 0.93098(3) -0.003669(12) 0.02736(9) Uani 1 1 d . . . S1 S 0.04848(4) 1.16990(10) 0.09358(4) 0.0285(2) Uani 1 1 d . . . N1 N 0.30472(13) 0.7518(4) 0.14970(14) 0.0327(8) Uani 1 1 d . . . N2 N 0.17280(13) 0.6959(3) 0.13230(13) 0.0299(7) Uani 1 1 d . . . N3 N 0.09191(13) 0.8995(3) 0.44032(13) 0.0284(7) Uani 1 1 d . . . O1 O 0.05389(11) 1.7059(3) 0.02656(12) 0.0336(7) Uani 1 1 d . . . O2 O 0.12701(12) 1.7325(3) -0.01097(12) 0.0373(7) Uani 1 1 d . . . O3 O 0.21451(11) 1.5356(3) -0.04584(12) 0.0320(6) Uani 1 1 d . . . O4 O 0.24379(10) 1.6203(3) 0.03770(12) 0.0324(6) Uani 1 1 d . . . O5 O 0.15414(10) 0.9794(3) 0.05785(12) 0.0317(6) Uani 1 1 d . . . O6 O 0.21481(12) 1.0841(3) 0.12308(13) 0.0410(7) Uani 1 1 d . . . O7 O 0.02489(10) 1.0692(3) 0.04847(11) 0.0291(6) Uani 1 1 d . . . O8 O 0.08162(12) 1.0949(3) 0.13874(12) 0.0411(7) Uani 1 1 d . . . O9 O 0.00495(11) 1.2604(3) 0.10510(13) 0.0396(7) Uani 1 1 d . . . C1 C 0.11424(14) 1.5050(4) 0.02602(15) 0.0228(8) Uani 1 1 d . . . C2 C 0.16788(14) 1.4572(4) 0.02241(15) 0.0223(8) Uani 1 1 d . . . C3 C 0.18466(15) 1.3216(4) 0.04229(15) 0.0239(8) Uani 1 1 d . . . H3A H 0.2205 1.2898 0.0404 0.029 Uiso 1 1 calc R . . C4 C 0.14995(14) 1.2330(4) 0.06465(15) 0.0220(8) Uani 1 1 d . . . C5 C 0.09529(15) 1.2791(4) 0.06578(15) 0.0229(8) Uani 1 1 d . . . C6 C 0.07808(14) 1.4145(4) 0.04702(15) 0.0243(8) Uani 1 1 d . . . H6A H 0.0420 1.4455 0.0484 0.029 Uiso 1 1 calc R . . C7 C 0.09667(15) 1.6563(4) 0.01211(16) 0.0267(8) Uani 1 1 d . . . C8 C 0.21125(15) 1.5483(4) 0.00275(17) 0.0269(8) Uani 1 1 d . . . C9 C 0.17373(15) 1.0896(4) 0.08659(18) 0.0295(9) Uani 1 1 d . . . C10 C 0.30489(17) 0.6901(5) 0.19767(17) 0.0366(10) Uani 1 1 d . . . H10A H 0.2732 0.7005 0.2127 0.044 Uiso 1 1 calc R . . C11 C 0.34934(17) 0.6123(5) 0.22601(18) 0.0400(10) Uani 1 1 d . . . H11A H 0.3470 0.5702 0.2589 0.048 Uiso 1 1 calc R . . C12 C 0.39763(16) 0.5972(4) 0.20521(18) 0.0344(10) Uani 1 1 d . . . C13 C 0.39861(17) 0.6657(4) 0.15688(17) 0.0356(10) Uani 1 1 d . . . H13A H 0.4307 0.6620 0.1422 0.043 Uiso 1 1 calc R . . C14 C 0.35234(17) 0.7392(5) 0.13069(18) 0.0368(10) Uani 1 1 d . . . H14A H 0.3539 0.7828 0.0979 0.044 Uiso 1 1 calc R . . C15 C 0.44795(17) 0.5118(5) 0.2329(2) 0.0446(12) Uani 1 1 d . . . H15A H 0.4391 0.4656 0.2646 0.053 Uiso 1 1 calc R . . H15B H 0.4555 0.4375 0.2086 0.053 Uiso 1 1 calc R . . C16 C 0.5000 0.6015(6) 0.2500 0.0385(15) Uani 1 2 d S . . H16A H 0.4953 0.6627 0.2798 0.046 Uiso 0.50 1 d PR . . C17 C 0.13020(17) 0.7542(4) 0.14993(18) 0.0371(10) Uani 1 1 d . . . H17A H 0.1199 0.8477 0.1399 0.045 Uiso 1 1 calc R . . C18 C 0.10056(18) 0.6816(4) 0.18248(18) 0.0384(10) Uani 1 1 d . . . H18A H 0.0705 0.7260 0.1935 0.046 Uiso 1 1 calc R . . C19 C 0.11510(17) 0.5434(4) 0.19901(16) 0.0330(9) Uani 1 1 d . . . C20 C 0.15896(17) 0.4825(4) 0.18021(17) 0.0340(9) Uani 1 1 d . . . H20A H 0.1700 0.3891 0.1896 0.041 Uiso 1 1 calc R . . C21 C 0.18637(16) 0.5606(4) 0.14742(16) 0.0312(9) Uani 1 1 d . . . H21A H 0.2159 0.5177 0.1350 0.037 Uiso 1 1 calc R . . C22 C 0.0850(2) 0.4593(4) 0.23621(18) 0.0416(11) Uani 1 1 d . . . H22A H 0.1074 0.3761 0.2495 0.050 Uiso 1 1 calc R . . H22B H 0.0494 0.4254 0.2154 0.050 Uiso 1 1 calc R . . C23 C 0.07373(19) 0.5448(5) 0.28460(18) 0.0411(11) Uani 1 1 d . . . H23A H 0.0500 0.6258 0.2712 0.049 Uiso 1 1 calc R . . H23B H 0.0530 0.4849 0.3051 0.049 Uiso 1 1 calc R . . C24 C 0.12617(18) 0.5995(5) 0.32234(18) 0.0408(11) Uani 1 1 d . . . H24A H 0.1473 0.5184 0.3397 0.049 Uiso 1 1 calc R . . H24B H 0.1495 0.6483 0.3010 0.049 Uiso 1 1 calc R . . C25 C 0.14160(17) 0.8979(4) 0.42473(18) 0.0369(10) Uani 1 1 d . . . H25A H 0.1689 0.9640 0.4398 0.044 Uiso 1 1 calc R . . C26 C 0.15364(17) 0.8023(4) 0.38734(18) 0.0375(10) Uani 1 1 d . . . H26A H 0.1881 0.8065 0.3767 0.045 Uiso 1 1 calc R . . C27 C 0.11476(17) 0.7002(4) 0.36553(16) 0.0310(9) Uani 1 1 d . . . C28 C 0.06538(19) 0.6979(5) 0.3843(2) 0.0443(11) Uani 1 1 d . . . H28A H 0.0387 0.6275 0.3724 0.053 Uiso 1 1 calc R . . C29 C 0.05526(18) 0.7990(4) 0.42058(19) 0.0393(11) Uani 1 1 d . . . H29A H 0.0211 0.7968 0.4317 0.047 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 0.02446(14) 0.02392(15) 0.03672(18) 0.00927(12) 0.00933(12) 0.00386(11) Cd2 0.02484(14) 0.02033(14) 0.03762(18) 0.00553(12) 0.00798(12) 0.00304(11) S1 0.0278(5) 0.0256(5) 0.0345(6) 0.0024(4) 0.0118(4) -0.0021(4) N1 0.0258(17) 0.042(2) 0.030(2) 0.0002(16) 0.0043(15) -0.0015(15) N2 0.0300(17) 0.0291(17) 0.0304(19) 0.0043(15) 0.0057(15) 0.0001(14) N3 0.0298(17) 0.0295(17) 0.0276(19) -0.0051(14) 0.0104(14) -0.0011(14) O1 0.0285(14) 0.0218(13) 0.055(2) 0.0070(13) 0.0182(14) 0.0066(11) O2 0.0448(17) 0.0218(14) 0.052(2) 0.0081(13) 0.0262(15) 0.0065(12) O3 0.0358(15) 0.0273(14) 0.0362(18) 0.0012(12) 0.0151(13) -0.0031(12) O4 0.0261(14) 0.0262(14) 0.0443(18) -0.0010(13) 0.0053(13) -0.0049(11) O5 0.0302(14) 0.0162(12) 0.0485(19) 0.0032(12) 0.0074(13) 0.0011(11) O6 0.0349(16) 0.0390(17) 0.044(2) 0.0067(14) -0.0028(14) 0.0063(13) O7 0.0229(13) 0.0278(14) 0.0372(17) -0.0032(12) 0.0075(12) -0.0034(11) O8 0.0457(17) 0.0433(17) 0.0339(18) 0.0118(14) 0.0067(14) -0.0004(14) O9 0.0367(16) 0.0330(16) 0.057(2) -0.0004(14) 0.0291(15) 0.0009(13) C1 0.0231(17) 0.0194(17) 0.027(2) -0.0012(15) 0.0065(15) -0.0008(14) C2 0.0229(17) 0.0216(18) 0.023(2) -0.0012(15) 0.0063(15) -0.0013(14) C3 0.0205(17) 0.0205(18) 0.032(2) 0.0003(16) 0.0079(16) 0.0022(14) C4 0.0230(17) 0.0206(17) 0.022(2) -0.0003(15) 0.0043(15) -0.0026(14) C5 0.0264(18) 0.0192(17) 0.023(2) 0.0011(15) 0.0062(15) -0.0039(14) C6 0.0193(17) 0.0229(18) 0.031(2) -0.0005(16) 0.0058(16) 0.0015(14) C7 0.0253(19) 0.0233(19) 0.032(2) 0.0031(16) 0.0058(17) 0.0029(16) C8 0.0253(19) 0.0189(18) 0.038(2) 0.0090(17) 0.0111(18) 0.0026(15) C9 0.0208(18) 0.0187(18) 0.046(3) 0.0084(17) -0.0004(17) -0.0017(15) C10 0.026(2) 0.051(3) 0.032(2) 0.005(2) 0.0074(18) -0.0020(19) C11 0.037(2) 0.047(3) 0.034(3) 0.008(2) 0.004(2) -0.008(2) C12 0.030(2) 0.030(2) 0.040(3) -0.0052(19) -0.0017(19) -0.0076(17) C13 0.027(2) 0.046(3) 0.033(2) 0.000(2) 0.0071(18) 0.0032(18) C14 0.035(2) 0.043(2) 0.032(2) 0.005(2) 0.0048(19) -0.0013(19) C15 0.038(2) 0.034(2) 0.057(3) 0.006(2) -0.004(2) -0.0010(19) C16 0.029(3) 0.037(3) 0.044(4) 0.000 -0.005(3) 0.000 C17 0.041(2) 0.029(2) 0.043(3) 0.0062(19) 0.013(2) 0.0038(19) C18 0.042(2) 0.038(2) 0.039(3) 0.001(2) 0.018(2) 0.011(2) C19 0.044(2) 0.031(2) 0.025(2) -0.0042(17) 0.0090(19) -0.0042(18) C20 0.043(2) 0.028(2) 0.032(2) 0.0016(18) 0.0082(19) 0.0006(18) C21 0.032(2) 0.031(2) 0.031(2) 0.0025(18) 0.0061(18) 0.0032(17) C22 0.059(3) 0.031(2) 0.039(3) -0.0023(19) 0.021(2) -0.011(2) C23 0.051(3) 0.042(3) 0.035(3) -0.005(2) 0.020(2) -0.006(2) C24 0.045(3) 0.042(3) 0.038(3) -0.007(2) 0.014(2) 0.007(2) C25 0.031(2) 0.035(2) 0.044(3) -0.002(2) 0.006(2) -0.0034(18) C26 0.028(2) 0.042(2) 0.044(3) 0.002(2) 0.0112(19) 0.0041(18) C27 0.036(2) 0.029(2) 0.029(2) 0.0005(17) 0.0096(18) 0.0055(17) C28 0.045(3) 0.040(3) 0.052(3) -0.014(2) 0.021(2) -0.015(2) C29 0.036(2) 0.037(2) 0.051(3) -0.015(2) 0.024(2) -0.0106(19) _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 2.258(3) 7_575 ? Cd1 O4 2.279(3) 1_545 ? Cd1 O5 2.299(2) . ? Cd1 N2 2.336(3) . ? Cd1 N1 2.354(3) . ? Cd2 N3 2.242(3) 6_575 ? Cd2 O7 2.306(3) . ? Cd2 O1 2.311(2) 1_545 ? Cd2 O5 2.315(3) . ? Cd2 O2 2.318(3) 1_545 ? Cd2 O7 2.397(2) 5_575 ? Cd2 C7 2.650(4) 1_545 ? S1 O9 1.430(3) . ? S1 O8 1.439(3) . ? S1 O7 1.500(3) . ? S1 C5 1.775(4) . ? N1 C10 1.340(5) . ? N1 C14 1.345(5) . ? N2 C17 1.324(5) . ? N2 C21 1.343(5) . ? N3 C29 1.321(5) . ? N3 C25 1.344(5) . ? N3 Cd2 2.242(3) 6_576 ? O1 C7 1.258(4) . ? O1 Cd2 2.311(2) 1_565 ? O2 C7 1.251(4) . ? O2 Cd2 2.318(3) 1_565 ? O3 C8 1.250(5) . ? O3 Cd1 2.258(3) 7_575 ? O4 C8 1.255(5) . ? O4 Cd1 2.279(3) 1_565 ? O5 C9 1.295(4) . ? O6 C9 1.216(5) . ? O7 Cd2 2.397(2) 5_575 ? C1 C2 1.399(5) . ? C1 C6 1.400(5) . ? C1 C7 1.499(5) . ? C2 C3 1.394(5) . ? C2 C8 1.515(5) . ? C3 C4 1.382(5) . ? C3 H3A 0.9300 . ? C4 C5 1.403(5) . ? C4 C9 1.520(5) . ? C5 C6 1.386(5) . ? C6 H6A 0.9300 . ? C7 Cd2 2.650(4) 1_565 ? C10 C11 1.377(6) . ? C10 H10A 0.9300 . ? C11 C12 1.386(6) . ? C11 H11A 0.9300 . ? C12 C13 1.383(6) . ? C12 C15 1.509(6) . ? C13 C14 1.369(6) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C16 1.507(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C15 1.507(5) 2_655 ? C16 H16A 0.9700 . ? C17 C18 1.376(6) . ? C17 H17A 0.9300 . ? C18 C19 1.382(5) . ? C18 H18A 0.9300 . ? C19 C20 1.375(5) . ? C19 C22 1.521(5) . ? C20 C21 1.373(5) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.530(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.518(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C27 1.508(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.373(6) . ? C25 H25A 0.9300 . ? C26 C27 1.378(6) . ? C26 H26A 0.9300 . ? C27 C28 1.377(6) . ? C28 C29 1.372(6) . ? C28 H28A 0.9300 . ? C29 H29A 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 O4 95.88(9) 7_575 1_545 ? O3 Cd1 O5 91.72(9) 7_575 . ? O4 Cd1 O5 126.66(10) 1_545 . ? O3 Cd1 N2 171.36(11) 7_575 . ? O4 Cd1 N2 91.02(10) 1_545 . ? O5 Cd1 N2 88.31(10) . . ? O3 Cd1 N1 89.53(11) 7_575 . ? O4 Cd1 N1 86.11(11) 1_545 . ? O5 Cd1 N1 146.81(11) . . ? N2 Cd1 N1 85.74(11) . . ? N3 Cd2 O7 99.12(10) 6_575 . ? N3 Cd2 O1 158.77(11) 6_575 1_545 ? O7 Cd2 O1 100.01(9) . 1_545 ? N3 Cd2 O5 90.97(10) 6_575 . ? O7 Cd2 O5 88.15(9) . . ? O1 Cd2 O5 98.76(9) 1_545 . ? N3 Cd2 O2 108.32(10) 6_575 1_545 ? O7 Cd2 O2 148.79(10) . 1_545 ? O1 Cd2 O2 56.47(9) 1_545 1_545 ? O5 Cd2 O2 77.02(10) . 1_545 ? N3 Cd2 O7 91.14(10) 6_575 5_575 ? O7 Cd2 O7 73.58(10) . 5_575 ? O1 Cd2 O7 85.51(9) 1_545 5_575 ? O5 Cd2 O7 161.71(9) . 5_575 ? O2 Cd2 O7 119.34(10) 1_545 5_575 ? N3 Cd2 C7 135.15(12) 6_575 1_545 ? O7 Cd2 C7 125.55(11) . 1_545 ? O1 Cd2 C7 28.32(10) 1_545 1_545 ? O5 Cd2 C7 87.11(10) . 1_545 ? O2 Cd2 C7 28.15(10) 1_545 1_545 ? O7 Cd2 C7 104.00(10) 5_575 1_545 ? O9 S1 O8 116.52(19) . . ? O9 S1 O7 109.92(17) . . ? O8 S1 O7 111.26(16) . . ? O9 S1 C5 107.41(17) . . ? O8 S1 C5 107.01(17) . . ? O7 S1 C5 103.82(16) . . ? C10 N1 C14 116.0(3) . . ? C10 N1 Cd1 129.1(3) . . ? C14 N1 Cd1 112.6(3) . . ? C17 N2 C21 117.1(3) . . ? C17 N2 Cd1 122.9(3) . . ? C21 N2 Cd1 119.8(3) . . ? C29 N3 C25 117.3(3) . . ? C29 N3 Cd2 121.7(3) . 6_576 ? C25 N3 Cd2 121.0(3) . 6_576 ? C7 O1 Cd2 91.0(2) . 1_565 ? C7 O2 Cd2 90.8(2) . 1_565 ? C8 O3 Cd1 120.8(2) . 7_575 ? C8 O4 Cd1 130.4(2) . 1_565 ? C9 O5 Cd1 100.2(2) . . ? C9 O5 Cd2 134.6(2) . . ? Cd1 O5 Cd2 125.21(11) . . ? S1 O7 Cd2 128.89(14) . . ? S1 O7 Cd2 123.20(14) . 5_575 ? Cd2 O7 Cd2 106.42(10) . 5_575 ? C2 C1 C6 119.7(3) . . ? C2 C1 C7 120.8(3) . . ? C6 C1 C7 119.3(3) . . ? C3 C2 C1 118.5(3) . . ? C3 C2 C8 117.2(3) . . ? C1 C2 C8 124.1(3) . . ? C4 C3 C2 122.3(3) . . ? C4 C3 H3A 118.8 . . ? C2 C3 H3A 118.8 . . ? C3 C4 C5 118.8(3) . . ? C3 C4 C9 117.4(3) . . ? C5 C4 C9 123.8(3) . . ? C6 C5 C4 119.7(3) . . ? C6 C5 S1 119.2(3) . . ? C4 C5 S1 121.1(3) . . ? C5 C6 C1 120.8(3) . . ? C5 C6 H6A 119.6 . . ? C1 C6 H6A 119.6 . . ? O2 C7 O1 121.7(3) . . ? O2 C7 C1 118.7(3) . . ? O1 C7 C1 119.5(3) . . ? O2 C7 Cd2 61.00(19) . 1_565 ? O1 C7 Cd2 60.69(18) . 1_565 ? C1 C7 Cd2 174.5(3) . 1_565 ? O3 C8 O4 125.8(3) . . ? O3 C8 C2 117.0(3) . . ? O4 C8 C2 116.9(3) . . ? O6 C9 O5 123.0(3) . . ? O6 C9 C4 120.5(3) . . ? O5 C9 C4 115.4(3) . . ? N1 C10 C11 123.8(4) . . ? N1 C10 H10A 118.1 . . ? C11 C10 H10A 118.1 . . ? C10 C11 C12 119.5(4) . . ? C10 C11 H11A 120.2 . . ? C12 C11 H11A 120.2 . . ? C13 C12 C11 116.9(4) . . ? C13 C12 C15 119.9(4) . . ? C11 C12 C15 123.2(4) . . ? C14 C13 C12 120.0(4) . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? N1 C14 C13 123.7(4) . . ? N1 C14 H14A 118.2 . . ? C13 C14 H14A 118.2 . . ? C16 C15 C12 113.2(4) . . ? C16 C15 H15A 108.9 . . ? C12 C15 H15A 108.9 . . ? C16 C15 H15B 108.9 . . ? C12 C15 H15B 108.9 . . ? H15A C15 H15B 107.8 . . ? C15 C16 C15 112.3(5) . 2_655 ? C15 C16 H16A 109.1 . . ? C15 C16 H16A 109.3 2_655 . ? N2 C17 C18 122.5(4) . . ? N2 C17 H17A 118.8 . . ? C18 C17 H17A 118.8 . . ? C17 C18 C19 120.6(4) . . ? C17 C18 H18A 119.7 . . ? C19 C18 H18A 119.7 . . ? C20 C19 C18 116.9(4) . . ? C20 C19 C22 120.1(4) . . ? C18 C19 C22 123.0(4) . . ? C21 C20 C19 119.4(4) . . ? C21 C20 H20A 120.3 . . ? C19 C20 H20A 120.3 . . ? N2 C21 C20 123.5(4) . . ? N2 C21 H21A 118.3 . . ? C20 C21 H21A 118.3 . . ? C19 C22 C23 114.1(3) . . ? C19 C22 H22A 108.7 . . ? C23 C22 H22A 108.7 . . ? C19 C22 H22B 108.7 . . ? C23 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? C24 C23 C22 114.5(4) . . ? C24 C23 H23A 108.6 . . ? C22 C23 H23A 108.6 . . ? C24 C23 H23B 108.6 . . ? C22 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? C27 C24 C23 114.2(3) . . ? C27 C24 H24A 108.7 . . ? C23 C24 H24A 108.7 . . ? C27 C24 H24B 108.7 . . ? C23 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? N3 C25 C26 122.5(4) . . ? N3 C25 H25A 118.8 . . ? C26 C25 H25A 118.8 . . ? C25 C26 C27 120.1(4) . . ? C25 C26 H26A 119.9 . . ? C27 C26 H26A 119.9 . . ? C28 C27 C26 116.6(4) . . ? C28 C27 C24 122.7(4) . . ? C26 C27 C24 120.7(4) . . ? C29 C28 C27 120.3(4) . . ? C29 C28 H28A 119.8 . . ? C27 C28 H28A 119.8 . . ? N3 C29 C28 122.9(4) . . ? N3 C29 H29A 118.5 . . ? C28 C29 H29A 118.5 . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 29.08 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.912 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.115 #===END OF 2 _database_code_depnum_ccdc_archive 'CCDC 924895'