# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email spaceljb@163.com _publ_contact_author_name 'Jia-bin Li' loop_ _publ_author_name 'Shuang-Quan Zang' 'Jia-Bin Li' data_20110520C _database_code_depnum_ccdc_archive 'CCDC 857054' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C16 H12 Cd2 O11 S, H2 O' _chemical_formula_sum 'C16 H14 Cd2 O12 S' _chemical_formula_weight 655.13 _chemical_melting_point ? _chemical_name_common ? _chemical_name_systematic ? 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' 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' _space_group_IT_number 14 _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_angle_alpha 90.00 _cell_angle_beta 94.2943(19) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 11.6973(2) _cell_length_b 10.2680(2) _cell_length_c 15.3761(3) _cell_measurement_reflns_used 3478 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 29.1104 _cell_measurement_theta_min 2.8929 _cell_volume 1841.61(7) _exptl_absorpt_coefficient_mu 2.492 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.77705 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS(2009) _exptl_crystal_F_000 1272 _exptl_crystal_colour ? _exptl_crystal_density_diffrn 2.363 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 7409 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.90 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 2724 _reflns_number_total 3227 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _computing_publication_material ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.271 _refine_diff_density_min -0.948 _refine_diff_density_rms 0.122 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0377 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.456 _refine_ls_hydrogen_treatment CONSTR _refine_ls_matrix_type full _refine_ls_number_parameters 280 _refine_ls_number_reflns 3227 _refine_ls_number_restraints 15 _refine_ls_restrained_S_all 1.511 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_wR_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.0556 _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 O5 O 1.1340(3) 0.8081(4) 1.0556(3) 0.0465(10) Uani 1 1 d U . . Cd1 Cd 1.03745(3) 0.86512(4) 0.90732(3) 0.02832(13) Uani 1 1 d U . . Cd2 Cd 0.96276(3) 0.74447(4) 0.65546(3) 0.02686(12) Uani 1 1 d U . . O1 O 0.8971(3) 0.7161(4) 0.8990(3) 0.0410(11) Uani 1 1 d . . . O2 O 0.8955(3) 0.6350(4) 0.7649(2) 0.0430(11) Uani 1 1 d . . . O3 O 0.7761(3) 0.4189(3) 0.6548(2) 0.0329(10) Uani 1 1 d . . . O4 O 0.9245(3) 0.3542(3) 0.7387(2) 0.0285(9) Uani 1 1 d . . . O6 O 0.9073(3) 0.0538(4) 0.8415(3) 0.0441(11) Uani 1 1 d U . . O7 O 0.9053(3) -0.0639(3) 1.0190(2) 0.0260(9) Uani 1 1 d . . . O8 O 0.7874(3) -0.2008(3) 1.0789(2) 0.0262(9) Uani 1 1 d . . . O1W O 1.1465(4) 0.6560(4) 0.9140(3) 0.0839(17) Uani 1 1 d U . . H1WB H 1.1288 0.6127 0.8678 0.126 Uiso 1 1 d R . . H1WC H 1.1288 0.6124 0.9580 0.126 Uiso 1 1 d R . . O2W O 0.8312(4) 0.9252(4) 0.6975(3) 0.0917(19) Uani 1 1 d U . . H2WA H 0.8549 0.9664 0.7433 0.138 Uiso 1 1 d R . . H2WB H 0.7963 0.8937 0.6604 0.138 Uiso 1 1 d R . . O3W O 0.9743(4) 0.9107(4) 0.5602(3) 0.0715(15) Uani 1 1 d . . . H3WB H 0.9974 0.9789 0.5874 0.107 Uiso 1 1 d R . . H3WC H 0.9515 0.8736 0.5126 0.107 Uiso 1 1 d R . . S1 S 0.65080(12) 0.19148(13) 0.76331(9) 0.0295(4) Uani 1 1 d . . . C1 C 0.7794(4) 0.5330(5) 0.8623(3) 0.0216(12) Uani 1 1 d . . . C2 C 0.7583(4) 0.4239(5) 0.8084(3) 0.0205(12) Uani 1 1 d . . . C3 C 0.6767(4) 0.3312(5) 0.8310(3) 0.0227(13) Uani 1 1 d . . . C4 C 0.6171(4) 0.3494(5) 0.9054(4) 0.0322(15) Uani 1 1 d . . . H4 H 0.5619 0.2895 0.9196 0.039 Uiso 1 1 calc R . . C5 C 0.6406(5) 0.4566(5) 0.9579(4) 0.0351(15) Uani 1 1 d . . . H5 H 0.6020 0.4680 1.0081 0.042 Uiso 1 1 calc R . . C6 C 0.7209(4) 0.5468(5) 0.9362(4) 0.0290(14) Uani 1 1 d . . . H6 H 0.7360 0.6184 0.9723 0.035 Uiso 1 1 calc R . . C7 C 0.8635(4) 0.6373(5) 0.8395(4) 0.0242(13) Uani 1 1 d . . . C8 C 0.8225(4) 0.3996(5) 0.7286(3) 0.0211(12) Uani 1 1 d . . . C9 C 0.6350(4) 0.0672(5) 0.8433(3) 0.0228(13) Uani 1 1 d . . . C10 C 0.7282(4) 0.0297(5) 0.9018(3) 0.0196(12) Uani 1 1 d . . . C11 C 0.7108(4) -0.0704(5) 0.9613(3) 0.0180(12) Uani 1 1 d . . . C12 C 0.6050(4) -0.1310(5) 0.9617(3) 0.0262(13) Uani 1 1 d . . . H12 H 0.5941 -0.1965 1.0020 0.031 Uiso 1 1 calc R . . C13 C 0.5145(4) -0.0946(5) 0.9023(4) 0.0302(14) Uani 1 1 d . . . H13 H 0.4442 -0.1368 0.9025 0.036 Uiso 1 1 calc R . . C14 C 0.5297(4) 0.0040(5) 0.8434(4) 0.0289(14) Uani 1 1 d . . . H14 H 0.4696 0.0284 0.8037 0.035 Uiso 1 1 calc R . . C15 C 0.8436(4) 0.0965(6) 0.8960(4) 0.0295(14) Uani 1 1 d . . . C16 C 0.8062(4) -0.1148(5) 1.0248(3) 0.0214(12) Uani 1 1 d . . . O4W O 0.6402(5) 0.7119(7) 0.2020(5) 0.165(3) Uani 1 1 d . . . H4WA H 0.6929 0.7692 0.1858 0.248 Uiso 1 1 d R . . H4WB H 0.5717 0.7335 0.2101 0.248 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 O5 0.0416(17) 0.0398(18) 0.0559(17) -0.0018(16) -0.0121(14) 0.0029(16) Cd1 0.0333(2) 0.0289(3) 0.0235(2) -0.0059(2) 0.00744(18) -0.0097(2) Cd2 0.0265(2) 0.0313(3) 0.0225(2) 0.0029(2) -0.00015(18) -0.0024(2) O1 0.052(3) 0.035(3) 0.038(3) -0.016(2) 0.016(2) -0.022(2) O2 0.065(3) 0.036(3) 0.031(3) -0.004(2) 0.020(2) -0.026(2) O3 0.040(2) 0.036(2) 0.021(2) 0.0088(19) -0.0017(19) 0.000(2) O4 0.026(2) 0.035(2) 0.026(2) -0.0001(19) 0.0082(17) 0.0052(19) O6 0.0374(17) 0.0575(19) 0.0380(18) 0.0048(16) 0.0056(15) -0.0036(16) O7 0.0155(18) 0.033(2) 0.029(2) -0.0019(18) -0.0010(17) -0.0028(18) O8 0.032(2) 0.023(2) 0.023(2) 0.0058(18) -0.0004(17) -0.0016(18) O1W 0.089(4) 0.067(3) 0.095(4) 0.037(3) 0.004(3) 0.026(3) O2W 0.103(4) 0.078(4) 0.090(4) -0.054(3) -0.021(3) 0.033(3) O3W 0.102(4) 0.050(3) 0.059(4) 0.003(3) -0.017(3) -0.014(3) S1 0.0353(8) 0.0239(8) 0.0281(8) 0.0043(7) -0.0064(7) -0.0065(7) C1 0.019(3) 0.014(3) 0.032(3) 0.003(3) 0.005(2) 0.002(3) C2 0.018(3) 0.020(3) 0.024(3) 0.005(2) 0.001(2) 0.002(3) C3 0.020(3) 0.019(3) 0.029(3) 0.005(3) 0.001(2) -0.001(3) C4 0.021(3) 0.028(4) 0.049(4) 0.005(3) 0.015(3) -0.006(3) C5 0.037(3) 0.032(4) 0.040(4) 0.002(3) 0.024(3) 0.004(3) C6 0.028(3) 0.023(3) 0.037(4) -0.004(3) 0.009(3) 0.004(3) C7 0.024(3) 0.020(3) 0.029(3) 0.003(3) 0.004(3) 0.005(3) C8 0.028(3) 0.009(3) 0.026(3) 0.004(2) 0.003(3) -0.004(3) C9 0.026(3) 0.017(3) 0.025(3) 0.001(3) 0.000(3) -0.006(3) C10 0.020(3) 0.018(3) 0.021(3) -0.006(2) 0.004(2) -0.003(2) C11 0.017(3) 0.015(3) 0.021(3) -0.004(2) 0.001(2) 0.000(2) C12 0.032(3) 0.021(3) 0.027(3) 0.000(3) 0.006(3) -0.003(3) C13 0.022(3) 0.029(3) 0.040(4) 0.000(3) -0.002(3) -0.007(3) C14 0.027(3) 0.026(3) 0.033(3) 0.002(3) -0.007(3) 0.000(3) C15 0.027(3) 0.036(4) 0.023(3) 0.001(3) -0.011(3) 0.012(3) C16 0.025(3) 0.020(3) 0.019(3) -0.009(3) 0.005(2) 0.001(3) O4W 0.066(4) 0.240(8) 0.191(8) 0.118(7) 0.016(4) -0.005(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 O5 Cd1 2.536(4) . ? O5 C15 1.246(6) 3_767 ? Cd1 O1 2.241(4) . ? Cd1 O3 2.507(3) 2_756 ? Cd1 O4 2.324(3) 2_756 ? Cd1 O6 2.620(4) 1_565 ? Cd1 O7 2.503(3) 1_565 ? Cd1 O7 2.405(3) 3_767 ? Cd1 O1W 2.496(4) . ? Cd2 O2 2.216(4) . ? Cd2 O4 2.310(4) 2_756 ? Cd2 O6 2.477(4) 2_756 ? Cd2 O8 2.331(3) 4_565 ? Cd2 O2W 2.526(4) . ? Cd2 O3W 2.260(4) . ? O1 C7 1.262(6) . ? O2 C7 1.234(6) . ? O3 Cd1 2.507(3) 2_746 ? O3 C8 1.237(6) . ? O4 Cd1 2.324(3) 2_746 ? O4 Cd2 2.310(3) 2_746 ? O4 C8 1.280(5) . ? O6 Cd1 2.620(4) 1_545 ? O6 Cd2 2.477(4) 2_746 ? O6 C15 1.242(6) . ? O7 Cd1 2.503(3) 1_545 ? O7 Cd1 2.405(3) 3_767 ? O7 C16 1.281(5) . ? O8 Cd2 2.331(3) 4_566 ? O8 C16 1.245(6) . ? O1W H1WB 0.8499 . ? O1W H1WC 0.8500 . ? O2W H2WA 0.8503 . ? O2W H2WB 0.7500 . ? O3W H3WB 0.8500 . ? O3W H3WC 0.8494 . ? S1 C3 1.785(5) . ? S1 C9 1.791(5) . ? C1 C2 1.404(7) . ? C1 C6 1.378(6) . ? C1 C7 1.512(7) . ? C2 C3 1.410(6) . ? C2 C8 1.507(7) . ? C3 C4 1.396(7) . ? C4 H4 0.9300 . ? C4 C5 1.380(7) . ? C5 H5 0.9300 . ? C5 C6 1.378(7) . ? C6 H6 0.9300 . ? C9 C10 1.415(7) . ? C9 C14 1.392(6) . ? C10 C11 1.401(7) . ? C10 C15 1.523(7) . ? C11 C12 1.385(6) . ? C11 C16 1.498(7) . ? C12 H12 0.9300 . ? C12 C13 1.396(7) . ? C13 H13 0.9300 . ? C13 C14 1.379(7) . ? C14 H14 0.9300 . ? C15 O5 1.246(6) 3_767 ? O4W H4WA 0.9001 . ? O4W H4WB 0.8500 . ? 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 O6 136.46(12) . 1_565 ? O5 C15 C10 117.8(5) 3_767 . ? Cd1 O7 Cd1 113.97(13) 3_767 1_545 ? Cd1 O1W H1WB 108.9 . . ? Cd1 O1W H1WC 109.4 . . ? Cd2 O4 Cd1 124.32(14) 2_746 2_746 ? Cd2 O6 Cd1 103.83(13) 2_746 1_545 ? Cd2 O2W H2WA 114.3 . . ? Cd2 O2W H2WB 78.2 . . ? Cd2 O3W H3WB 109.6 . . ? Cd2 O3W H3WC 100.9 . . ? O1 Cd1 O5 99.71(14) . . ? O1 Cd1 O3 141.55(12) . 2_756 ? O1 Cd1 O4 95.98(13) . 2_756 ? O1 Cd1 O6 94.64(13) . 1_565 ? O1 Cd1 O7 141.56(12) . 3_767 ? O1 Cd1 O7 75.58(12) . 1_565 ? O1 Cd1 O1W 77.55(15) . . ? O1 C7 C1 117.3(5) . . ? O2 Cd2 O4 85.93(13) . 2_756 ? O2 Cd2 O6 80.61(14) . 2_756 ? O2 Cd2 O8 86.37(13) . 4_565 ? O2 Cd2 O2W 85.44(16) . . ? O2 Cd2 O3W 156.50(15) . . ? O2 C7 O1 125.9(5) . . ? O2 C7 C1 116.7(5) . . ? O3 Cd1 O5 92.95(13) 2_756 . ? O3 Cd1 O6 100.78(12) 2_756 1_565 ? O3 C8 O4 120.7(5) . . ? O3 C8 C2 120.6(5) . . ? O4 Cd1 O5 138.84(13) 2_756 . ? O4 Cd1 O3 53.70(11) 2_756 2_756 ? O4 Cd1 O6 79.06(12) 2_756 1_565 ? O4 Cd1 O7 115.45(12) 2_756 3_767 ? O4 Cd1 O7 148.14(11) 2_756 1_565 ? O4 Cd1 O1W 82.19(14) 2_756 . ? O4 Cd2 O6 93.17(12) 2_756 2_756 ? O4 Cd2 O8 152.11(12) 2_756 4_565 ? O4 Cd2 O2W 77.74(14) 2_756 . ? O4 C8 C2 118.6(5) . . ? O6 Cd2 O2W 163.88(15) 2_756 . ? O6 C15 O5 124.8(6) . 3_767 ? O6 C15 C10 117.3(5) . . ? O7 Cd1 O5 71.50(12) 3_767 . ? O7 Cd1 O5 72.96(12) 1_565 . ? O7 Cd1 O3 142.78(11) 1_565 2_756 ? O7 Cd1 O3 76.89(11) 3_767 2_756 ? O7 Cd1 O6 71.81(12) 3_767 1_565 ? O7 Cd1 O6 71.26(11) 1_565 1_565 ? O7 Cd1 O7 66.03(13) 3_767 1_565 ? O7 Cd1 O1W 125.98(14) 3_767 . ? O7 C16 C11 117.7(4) . . ? O8 Cd2 O6 111.92(12) 4_565 2_756 ? O8 Cd2 O2W 74.95(14) 4_565 . ? O8 C16 O7 122.9(5) . . ? O8 C16 C11 119.4(5) . . ? O1W Cd1 O5 64.69(15) . . ? O1W Cd1 O3 75.46(13) . 2_756 ? O1W Cd1 O6 158.82(15) . 1_565 ? O1W Cd1 O7 124.22(13) . 1_565 ? H1WB O1W H1WC 109.5 . . ? H2WA O2W H2WB 166.1 . . ? O3W Cd2 O4 91.69(14) . 2_756 ? O3W Cd2 O6 122.89(15) . 2_756 ? O3W Cd2 O8 84.89(14) . 4_565 ? O3W Cd2 O2W 71.23(17) . . ? H3WB O3W H3WC 149.5 . . ? C1 C2 C3 119.1(5) . . ? C1 C2 C8 122.4(4) . . ? C1 C6 C5 121.4(5) . . ? C1 C6 H6 119.3 . . ? C2 C1 C7 121.1(5) . . ? C2 C3 S1 119.2(4) . . ? C3 S1 C9 101.2(2) . . ? C3 C2 C8 118.5(4) . . ? C3 C4 H4 120.1 . . ? C4 C3 S1 120.8(4) . . ? C4 C3 C2 120.0(5) . . ? C4 C5 H5 119.9 . . ? C5 C4 C3 119.8(5) . . ? C5 C4 H4 120.1 . . ? C5 C6 H6 119.3 . . ? C6 C1 C2 119.5(5) . . ? C6 C1 C7 119.3(5) . . ? C6 C5 C4 120.2(5) . . ? C6 C5 H5 119.9 . . ? C7 O1 Cd1 131.8(3) . . ? C7 O2 Cd2 147.8(4) . . ? C8 O3 Cd1 88.8(3) . 2_746 ? C8 O4 Cd1 96.3(3) . 2_746 ? C8 O4 Cd2 137.8(3) . 2_746 ? C9 C10 C15 119.0(4) . . ? C9 C14 H14 120.0 . . ? C10 C9 S1 121.1(4) . . ? C10 C11 C16 120.7(4) . . ? C11 C10 C9 118.2(4) . . ? C11 C10 C15 122.8(5) . . ? C11 C12 H12 119.6 . . ? C11 C12 C13 120.7(5) . . ? C12 C11 C10 120.4(5) . . ? C12 C11 C16 118.9(5) . . ? C12 C13 H13 120.1 . . ? C13 C12 H12 119.6 . . ? C13 C14 C9 120.0(5) . . ? C13 C14 H14 120.0 . . ? C14 C9 S1 118.0(4) . . ? C14 C9 C10 120.8(5) . . ? C14 C13 C12 119.8(5) . . ? C14 C13 H13 120.1 . . ? C15 O5 Cd1 114.5(3) 3_767 . ? C15 O6 Cd1 111.1(3) . 1_545 ? C15 O6 Cd2 96.1(4) . 2_746 ? C16 O7 Cd1 122.3(3) . 3_767 ? C16 O7 Cd1 122.5(3) . 1_545 ? C16 O8 Cd2 106.3(3) . 4_566 ? H4WA O4W H4WB 122.9 . . ? 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 O5 Cd1 O1 C7 -131.3(5) . . . . ? Cd1 O1 C7 O2 -8.5(9) . . . . ? Cd1 O1 C7 C1 169.2(3) . . . . ? Cd1 O3 C8 O4 -6.7(5) 2_746 . . . ? Cd1 O3 C8 C2 175.7(4) 2_746 . . . ? Cd1 O4 C8 O3 7.3(5) 2_746 . . . ? Cd1 O4 C8 C2 -175.1(4) 2_746 . . . ? Cd1 O6 C15 O5 94.1(6) 1_545 . . 3_767 ? Cd1 O6 C15 C10 -88.0(5) 1_545 . . . ? Cd1 O7 C16 O8 -94.4(5) 3_767 . . . ? Cd1 O7 C16 O8 98.9(5) 1_545 . . . ? Cd1 O7 C16 C11 -79.2(5) 1_545 . . . ? Cd1 O7 C16 C11 87.6(5) 3_767 . . . ? Cd2 O2 C7 O1 -28.2(11) . . . . ? Cd2 O2 C7 C1 154.1(5) . . . . ? Cd2 O4 C8 O3 -157.8(3) 2_746 . . . ? Cd2 O4 C8 C2 19.8(7) 2_746 . . . ? Cd2 O6 C15 O5 -13.2(6) 2_746 . . 3_767 ? Cd2 O6 C15 C10 164.6(4) 2_746 . . . ? Cd2 O8 C16 O7 -1.6(6) 4_566 . . . ? Cd2 O8 C16 C11 176.4(3) 4_566 . . . ? O3 Cd1 O1 C7 -23.9(6) 2_756 . . . ? O4 Cd1 O1 C7 10.5(5) 2_756 . . . ? O4 Cd2 O2 C7 40.0(7) 2_756 . . . ? O6 Cd1 O1 C7 90.0(5) 1_565 . . . ? O6 Cd2 O2 C7 133.9(7) 2_756 . . . ? O7 Cd1 O1 C7 159.2(5) 1_565 . . . ? O7 Cd1 O1 C7 156.3(4) 3_767 . . . ? O8 Cd2 O2 C7 -113.2(7) 4_565 . . . ? O1W Cd1 O1 C7 -70.1(5) . . . . ? O2W Cd2 O2 C7 -38.0(7) . . . . ? O3W Cd2 O2 C7 -44.9(9) . . . . ? S1 C3 C4 C5 178.5(4) . . . . ? S1 C9 C10 C11 -178.5(4) . . . . ? S1 C9 C10 C15 -0.2(7) . . . . ? S1 C9 C14 C13 178.3(4) . . . . ? C1 C2 C3 S1 -179.3(4) . . . . ? C1 C2 C3 C4 0.8(7) . . . . ? C1 C2 C8 O3 -104.8(6) . . . . ? C1 C2 C8 O4 77.6(6) . . . . ? C2 C1 C6 C5 -1.0(8) . . . . ? C2 C1 C7 O1 -164.7(5) . . . . ? C2 C1 C7 O2 13.3(7) . . . . ? C2 C3 C4 C5 -1.6(8) . . . . ? C3 S1 C9 C10 -66.0(5) . . . . ? C3 S1 C9 C14 117.1(4) . . . . ? C3 C2 C8 O3 77.2(6) . . . . ? C3 C2 C8 O4 -100.4(6) . . . . ? C3 C4 C5 C6 1.2(9) . . . . ? C4 C5 C6 C1 0.2(8) . . . . ? C6 C1 C2 C3 0.6(8) . . . . ? C6 C1 C2 C8 -177.4(5) . . . . ? C6 C1 C7 O1 16.6(7) . . . . ? C6 C1 C7 O2 -165.4(5) . . . . ? C7 C1 C2 C3 -178.2(4) . . . . ? C7 C1 C2 C8 3.9(8) . . . . ? C7 C1 C6 C5 177.7(5) . . . . ? C8 C2 C3 S1 -1.3(6) . . . . ? C8 C2 C3 C4 178.8(5) . . . . ? C9 S1 C3 C2 140.6(4) . . . . ? C9 S1 C3 C4 -39.5(5) . . . . ? C9 C10 C11 C12 0.5(7) . . . . ? C9 C10 C11 C16 179.8(4) . . . . ? C9 C10 C15 O5 94.2(6) . . . 3_767 ? C9 C10 C15 O6 -83.8(6) . . . . ? C10 C9 C14 C13 1.4(8) . . . . ? C10 C11 C12 C13 0.8(8) . . . . ? C10 C11 C16 O7 -4.3(7) . . . . ? C10 C11 C16 O8 177.6(4) . . . . ? C11 C10 C15 O5 -87.6(6) . . . 3_767 ? C11 C10 C15 O6 94.4(6) . . . . ? C11 C12 C13 C14 -1.0(8) . . . . ? C12 C11 C16 O7 175.0(4) . . . . ? C12 C11 C16 O8 -3.1(7) . . . . ? C12 C13 C14 C9 -0.1(8) . . . . ? C14 C9 C10 C11 -1.6(8) . . . . ? C14 C9 C10 C15 176.7(5) . . . . ? C15 O5 Cd1 O1 -133.9(4) 3_767 . . . ? C15 O5 Cd1 O3 82.6(4) 3_767 . . 2_756 ? C15 O5 Cd1 O4 115.3(4) 3_767 . . 2_756 ? C15 O5 Cd1 O6 -26.4(5) 3_767 . . 1_565 ? C15 O5 Cd1 O7 7.5(4) 3_767 . . 3_767 ? C15 O5 Cd1 O7 -62.3(4) 3_767 . . 1_565 ? C15 O5 Cd1 O1W 155.0(4) 3_767 . . . ? C15 C10 C11 C12 -177.7(5) . . . . ? C15 C10 C11 C16 1.6(7) . . . . ? C16 C11 C12 C13 -178.5(5) . . . . ? # Attachment '2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 857055' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H32 Cd4 N2 O21 S2' _chemical_formula_weight 1438.44 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' 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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'C 2/c' 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 24.577(5) _cell_length_b 9.858(2) _cell_length_c 19.961(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.71(3) _cell_angle_gamma 90.00 _cell_volume 4552.8(18) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6704 _cell_measurement_theta_min 2.1674 _cell_measurement_theta_max 29.1994 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.099 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2808 _exptl_absorpt_coefficient_mu 2.024 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6877 _exptl_absorpt_correction_T_max 0.7378 _exptl_absorpt_process_details SADABS(2009) _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 ? _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 21976 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4012 _reflns_number_gt 3690 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+22.3790P] 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 4012 _refine_ls_number_parameters 330 _refine_ls_number_restraints 225 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0874 _refine_ls_wR_factor_gt 0.0846 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.127 _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 1.044729(16) 0.86263(4) 1.16629(2) 0.03176(12) Uani 1 1 d U . . Cd2 Cd 0.999014(15) 0.50932(4) 1.100590(18) 0.02740(11) Uani 1 1 d U . . O1 O 0.84136(15) 0.3396(4) 0.7351(2) 0.0438(10) Uani 1 1 d U . . O2 O 0.92744(14) 0.3818(3) 0.81544(17) 0.0302(8) Uani 1 1 d U . . O3 O 0.97834(14) 0.7447(3) 1.07152(19) 0.0324(8) Uani 1 1 d U . . O4 O 0.93912(15) 0.9038(4) 1.11746(19) 0.0391(9) Uani 1 1 d U . . O5 O 0.94220(15) 0.6590(4) 0.91114(19) 0.0351(8) Uani 1 1 d U . . O6 O 0.93536(15) 0.5010(3) 0.98638(19) 0.0374(9) Uani 1 1 d U . . O7 O 0.93388(17) 0.4531(4) 0.6693(2) 0.0413(9) Uani 1 1 d U . . O8 O 0.95725(18) 0.6589(4) 0.6472(2) 0.0506(11) Uani 1 1 d U . . O1W O 1.03376(19) 1.0991(4) 1.1544(3) 0.0649(13) Uani 1 1 d U . . H1WA H 1.0499 1.1272 1.1255 0.097 Uiso 1 1 d R . . H1WB H 0.9980 1.1185 1.1385 0.097 Uiso 1 1 d R . . O2W O 1.0000 0.7564(5) 1.2500 0.0317(11) Uani 1 2 d SU . . H2WA H 0.9722 0.7086 1.2215 0.038 Uiso 1 1 d R . . O3W O 1.11113(15) 0.8925(4) 1.27584(19) 0.0386(9) Uani 1 1 d U . . H3WA H 1.1285 0.8186 1.2738 0.046 Uiso 1 1 d R . . H3WB H 1.0978 0.8926 1.3099 0.046 Uiso 1 1 d R . . N1 N 1.11162(19) 0.8613(4) 1.1078(2) 0.0352(10) Uani 1 1 d U . . C1 C 0.8771(2) 0.7900(5) 1.0142(3) 0.0270(11) Uani 1 1 d U . . C2 C 0.8704(2) 0.6919(5) 0.9623(3) 0.0282(11) Uani 1 1 d U . . C3 C 0.8155(2) 0.6720(5) 0.9101(3) 0.0292(11) Uani 1 1 d U . . C4 C 0.7698(2) 0.7526(6) 0.9109(3) 0.0380(13) Uani 1 1 d U . . H4 H 0.7336 0.7398 0.8765 0.046 Uiso 1 1 calc R . . C5 C 0.7770(2) 0.8526(6) 0.9623(3) 0.0389(13) Uani 1 1 d U . . H5 H 0.7461 0.9076 0.9618 0.047 Uiso 1 1 calc R . . C6 C 0.8300(2) 0.8696(5) 1.0138(3) 0.0340(12) Uani 1 1 d U . . H6 H 0.8347 0.9350 1.0488 0.041 Uiso 1 1 calc R . . C7 C 0.9344(2) 0.8147(5) 1.0714(2) 0.0294(11) Uani 1 1 d U . . C8 C 0.9203(2) 0.6117(5) 0.9542(3) 0.0301(11) Uani 1 1 d U . . C9 C 0.8299(2) 0.6315(5) 0.7822(3) 0.0290(11) Uani 1 1 d U . . C10 C 0.8675(2) 0.5667(5) 0.7536(2) 0.0262(10) Uani 1 1 d U . . C11 C 0.8888(2) 0.6402(5) 0.7073(3) 0.0286(11) Uani 1 1 d U . . C12 C 0.8717(2) 0.7736(5) 0.6906(3) 0.0337(12) Uani 1 1 d U . . H12 H 0.8875 0.8233 0.6621 0.040 Uiso 1 1 calc R . . C13 C 0.8316(2) 0.8339(5) 0.7158(3) 0.0379(13) Uani 1 1 d U . . H13 H 0.8187 0.9216 0.7019 0.046 Uiso 1 1 calc R . . C14 C 0.8109(2) 0.7627(5) 0.7618(3) 0.0338(12) Uani 1 1 d U . . H14 H 0.7840 0.8028 0.7792 0.041 Uiso 1 1 calc R . . C15 C 0.9297(2) 0.5786(6) 0.6732(3) 0.0358(13) Uani 1 1 d U . . C16 C 0.8800(2) 0.4187(5) 0.7686(3) 0.0302(11) Uani 1 1 d U . . C17 C 1.1674(2) 0.8890(7) 1.1420(3) 0.0491(16) Uani 1 1 d U . . H17 H 1.1775 0.9274 1.1871 0.059 Uiso 1 1 calc R . . C18 C 1.2105(3) 0.8644(7) 1.1147(4) 0.0586(18) Uani 1 1 d U . . H18 H 1.2484 0.8893 1.1402 0.070 Uiso 1 1 calc R . . C19 C 1.1979(3) 0.8029(7) 1.0495(4) 0.0592(19) Uani 1 1 d U . . C20 C 1.1408(4) 0.7724(7) 1.0136(4) 0.063(2) Uani 1 1 d U . . H20 H 1.1302 0.7309 0.9692 0.076 Uiso 1 1 calc R . . C21 C 1.0993(3) 0.8036(7) 1.0437(3) 0.0533(17) Uani 1 1 d U . . H21 H 1.0609 0.7834 1.0182 0.064 Uiso 1 1 calc R . . C22 C 1.2485(5) 0.7788(9) 1.0243(5) 0.091(3) Uani 1 1 d U . . H22 H 1.2832 0.8170 1.0530 0.109 Uiso 1 1 calc R . . S1 S 0.80528(6) 0.54257(14) 0.84445(7) 0.0351(3) Uani 1 1 d U . . 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 0.0291(2) 0.0349(2) 0.0306(2) -0.00137(16) 0.00924(16) -0.00404(16) Cd2 0.0249(2) 0.0297(2) 0.0271(2) 0.00015(15) 0.00830(15) -0.00012(15) O1 0.030(2) 0.038(2) 0.050(2) -0.0078(18) -0.0038(18) -0.0042(17) O2 0.0228(18) 0.034(2) 0.0285(18) 0.0001(15) 0.0012(15) -0.0013(14) O3 0.0262(19) 0.0295(19) 0.041(2) 0.0043(15) 0.0102(16) -0.0009(15) O4 0.0354(15) 0.044(2) 0.036(2) -0.0061(17) 0.0101(16) -0.0024(16) O5 0.030(2) 0.041(2) 0.037(2) 0.0005(17) 0.0150(17) 0.0035(16) O6 0.031(2) 0.033(2) 0.0376(17) -0.0002(16) -0.0027(14) 0.0001(16) O7 0.051(2) 0.040(2) 0.039(2) 0.0054(17) 0.0229(19) 0.0192(18) O8 0.056(3) 0.047(2) 0.068(3) -0.001(2) 0.046(2) 0.002(2) O1W 0.049(3) 0.046(3) 0.106(4) 0.018(3) 0.035(3) 0.007(2) O2W 0.031(3) 0.031(3) 0.031(3) 0.000 0.008(2) 0.000 O3W 0.038(2) 0.039(2) 0.036(2) 0.0005(16) 0.0080(17) -0.0036(17) N1 0.039(3) 0.034(2) 0.036(2) -0.0025(19) 0.018(2) -0.004(2) C1 0.021(2) 0.032(3) 0.028(3) 0.007(2) 0.009(2) 0.001(2) C2 0.023(3) 0.034(3) 0.028(3) 0.006(2) 0.009(2) 0.003(2) C3 0.020(2) 0.042(3) 0.026(3) 0.005(2) 0.008(2) -0.001(2) C4 0.022(3) 0.055(4) 0.036(3) 0.006(3) 0.008(2) 0.002(2) C5 0.032(3) 0.048(3) 0.040(3) 0.002(3) 0.016(3) 0.008(2) C6 0.035(3) 0.037(3) 0.032(3) 0.000(2) 0.014(2) 0.000(2) C7 0.038(3) 0.031(3) 0.020(2) 0.005(2) 0.011(2) -0.001(2) C8 0.025(3) 0.035(3) 0.025(3) -0.004(2) 0.001(2) -0.003(2) C9 0.024(3) 0.034(3) 0.029(3) 0.001(2) 0.009(2) -0.001(2) C10 0.020(2) 0.028(3) 0.028(3) -0.002(2) 0.004(2) 0.001(2) C11 0.026(3) 0.031(3) 0.028(3) -0.002(2) 0.008(2) 0.004(2) C12 0.032(3) 0.036(3) 0.036(3) 0.001(2) 0.017(2) -0.001(2) C13 0.037(3) 0.033(3) 0.046(3) 0.004(2) 0.016(3) 0.005(2) C14 0.030(3) 0.038(3) 0.033(3) -0.007(2) 0.010(2) 0.002(2) C15 0.028(3) 0.055(4) 0.023(3) 0.000(2) 0.007(2) 0.010(3) C16 0.027(3) 0.035(3) 0.029(3) 0.002(2) 0.010(2) 0.003(2) C17 0.037(3) 0.071(4) 0.037(3) 0.007(3) 0.009(3) -0.006(3) C18 0.038(4) 0.084(5) 0.056(4) 0.027(4) 0.018(3) 0.013(3) C19 0.066(5) 0.044(4) 0.086(5) 0.023(4) 0.050(4) 0.014(3) C20 0.101(6) 0.052(4) 0.058(4) -0.020(3) 0.054(4) -0.021(4) C21 0.055(4) 0.064(4) 0.046(4) -0.015(3) 0.023(3) -0.022(3) C22 0.123(7) 0.077(6) 0.098(7) 0.028(5) 0.073(6) 0.029(5) S1 0.0290(7) 0.0450(8) 0.0307(7) -0.0017(6) 0.0093(6) -0.0079(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 Cd1 O3W 2.264(4) . ? Cd1 N1 2.316(4) . ? Cd1 O3 2.347(4) . ? Cd1 O1W 2.349(4) . ? Cd1 O4 2.479(4) . ? Cd1 O2 2.497(3) 5_767 ? Cd1 O2W 2.517(2) . ? Cd2 O5 2.264(3) 5_767 ? Cd2 O2 2.277(3) 5_767 ? Cd2 O6 2.290(4) . ? Cd2 O8 2.306(4) 6_566 ? Cd2 O3 2.404(3) . ? Cd2 O7 2.462(4) 6_566 ? Cd2 C15 2.724(5) 6_566 ? O1 C16 1.237(6) . ? O2 C16 1.276(6) . ? O2 Cd2 2.277(3) 5_767 ? O2 Cd1 2.497(3) 5_767 ? O3 C7 1.282(6) . ? O4 C7 1.249(6) . ? O5 C8 1.249(6) . ? O5 Cd2 2.264(3) 5_767 ? O6 C8 1.256(6) . ? O7 C15 1.246(7) . ? O7 Cd2 2.462(4) 6_565 ? O8 C15 1.261(7) . ? O8 Cd2 2.306(4) 6_565 ? O1W H1WA 0.8500 . ? O1W H1WB 0.8499 . ? O2W Cd1 2.517(2) 2_757 ? O2W H2WA 0.8668 . ? O3W H3WA 0.8526 . ? O3W H3WB 0.8490 . ? N1 C21 1.337(7) . ? N1 C17 1.338(7) . ? C1 C2 1.387(7) . ? C1 C6 1.395(7) . ? C1 C7 1.503(7) . ? C2 C3 1.412(7) . ? C2 C8 1.512(7) . ? C3 C4 1.381(7) . ? C3 S1 1.785(5) . ? C4 C5 1.391(8) . ? C4 H4 0.9300 . ? C5 C6 1.371(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C9 C14 1.389(7) . ? C9 C10 1.394(7) . ? C9 S1 1.784(5) . ? C10 C11 1.408(7) . ? C10 C16 1.501(7) . ? C11 C12 1.385(7) . ? C11 C15 1.518(7) . ? C12 C13 1.383(7) . ? C12 H12 0.9300 . ? C13 C14 1.383(7) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 Cd2 2.724(5) 6_565 ? C17 C18 1.367(8) . ? C17 H17 0.9300 . ? C18 C19 1.372(10) . ? C18 H18 0.9300 . ? C19 C20 1.378(10) . ? C19 C22 1.510(10) . ? C20 C21 1.382(9) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C22 1.147(16) 7_767 ? C22 H22 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 O3W Cd1 N1 94.87(15) . . ? O3W Cd1 O3 157.16(12) . . ? N1 Cd1 O3 90.55(14) . . ? O3W Cd1 O1W 89.37(16) . . ? N1 Cd1 O1W 91.81(15) . . ? O3 Cd1 O1W 112.66(15) . . ? O3W Cd1 O4 132.58(13) . . ? N1 Cd1 O4 129.04(14) . . ? O3 Cd1 O4 54.07(12) . . ? O1W Cd1 O4 74.25(14) . . ? O3W Cd1 O2 84.93(12) . 5_767 ? N1 Cd1 O2 82.09(13) . 5_767 ? O3 Cd1 O2 73.84(11) . 5_767 ? O1W Cd1 O2 171.25(13) . 5_767 ? O4 Cd1 O2 114.48(12) . 5_767 ? O3W Cd1 O2W 75.33(10) . . ? N1 Cd1 O2W 151.15(14) . . ? O3 Cd1 O2W 89.34(10) . . ? O1W Cd1 O2W 114.75(15) . . ? O4 Cd1 O2W 72.26(10) . . ? O2 Cd1 O2W 70.20(12) 5_767 . ? O5 Cd2 O2 92.63(13) 5_767 5_767 ? O5 Cd2 O6 96.69(13) 5_767 . ? O2 Cd2 O6 148.82(13) 5_767 . ? O5 Cd2 O8 84.32(14) 5_767 6_566 ? O2 Cd2 O8 113.13(14) 5_767 6_566 ? O6 Cd2 O8 97.39(15) . 6_566 ? O5 Cd2 O3 140.62(12) 5_767 . ? O2 Cd2 O3 76.90(12) 5_767 . ? O6 Cd2 O3 77.08(12) . . ? O8 Cd2 O3 134.83(13) 6_566 . ? O5 Cd2 O7 136.51(13) 5_767 6_566 ? O2 Cd2 O7 91.31(12) 5_767 6_566 ? O6 Cd2 O7 101.86(14) . 6_566 ? O8 Cd2 O7 54.66(13) 6_566 6_566 ? O3 Cd2 O7 82.24(12) . 6_566 ? O5 Cd2 C15 110.94(16) 5_767 6_566 ? O2 Cd2 C15 104.00(14) 5_767 6_566 ? O6 Cd2 C15 100.28(15) . 6_566 ? O8 Cd2 C15 27.47(15) 6_566 6_566 ? O3 Cd2 C15 108.43(15) . 6_566 ? O7 Cd2 C15 27.20(15) 6_566 6_566 ? C16 O2 Cd2 135.0(3) . 5_767 ? C16 O2 Cd1 121.3(3) . 5_767 ? Cd2 O2 Cd1 103.71(12) 5_767 5_767 ? C7 O3 Cd1 95.3(3) . . ? C7 O3 Cd2 129.0(3) . . ? Cd1 O3 Cd2 104.51(13) . . ? C7 O4 Cd1 90.0(3) . . ? C8 O5 Cd2 103.6(3) . 5_767 ? C8 O6 Cd2 117.5(3) . . ? C15 O7 Cd2 88.2(3) . 6_565 ? C15 O8 Cd2 95.0(3) . 6_565 ? Cd1 O1W H1WA 109.1 . . ? Cd1 O1W H1WB 109.3 . . ? H1WA O1W H1WB 109.5 . . ? Cd1 O2W Cd1 130.83(19) 2_757 . ? Cd1 O2W H2WA 103.7 2_757 . ? Cd1 O2W H2WA 102.5 . . ? Cd1 O3W H3WA 93.0 . . ? Cd1 O3W H3WB 115.2 . . ? H3WA O3W H3WB 112.0 . . ? C21 N1 C17 116.0(5) . . ? C21 N1 Cd1 120.9(4) . . ? C17 N1 Cd1 121.4(4) . . ? C2 C1 C6 119.9(5) . . ? C2 C1 C7 121.7(4) . . ? C6 C1 C7 118.4(5) . . ? C1 C2 C3 119.4(4) . . ? C1 C2 C8 123.2(4) . . ? C3 C2 C8 117.2(4) . . ? C4 C3 C2 119.4(5) . . ? C4 C3 S1 120.3(4) . . ? C2 C3 S1 120.2(4) . . ? C3 C4 C5 120.9(5) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 119.4(5) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C1 120.9(5) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? O4 C7 O3 120.5(5) . . ? O4 C7 C1 120.3(5) . . ? O3 C7 C1 119.2(4) . . ? O5 C8 O6 123.7(5) . . ? O5 C8 C2 115.5(4) . . ? O6 C8 C2 120.6(5) . . ? C14 C9 C10 120.7(5) . . ? C14 C9 S1 120.1(4) . . ? C10 C9 S1 119.2(4) . . ? C9 C10 C11 118.6(5) . . ? C9 C10 C16 118.9(4) . . ? C11 C10 C16 122.3(4) . . ? C12 C11 C10 119.8(5) . . ? C12 C11 C15 117.7(5) . . ? C10 C11 C15 122.5(5) . . ? C13 C12 C11 121.1(5) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C14 C13 C12 119.4(5) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C9 120.3(5) . . ? C13 C14 H14 119.9 . . ? C9 C14 H14 119.9 . . ? O7 C15 O8 122.1(5) . . ? O7 C15 C11 120.4(5) . . ? O8 C15 C11 117.4(5) . . ? O7 C15 Cd2 64.6(3) . 6_565 ? O8 C15 Cd2 57.5(3) . 6_565 ? C11 C15 Cd2 173.4(4) . 6_565 ? O1 C16 O2 124.2(5) . . ? O1 C16 C10 115.8(4) . . ? O2 C16 C10 119.9(4) . . ? N1 C17 C18 124.0(6) . . ? N1 C17 H17 118.0 . . ? C18 C17 H17 118.0 . . ? C17 C18 C19 119.9(6) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 C20 117.0(6) . . ? C18 C19 C22 115.9(8) . . ? C20 C19 C22 127.0(8) . . ? C19 C20 C21 119.8(6) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? N1 C21 C20 123.2(6) . . ? N1 C21 H21 118.4 . . ? C20 C21 H21 118.4 . . ? C22 C22 C19 130.8(15) 7_767 . ? C22 C22 H22 114.6 7_767 . ? C19 C22 H22 114.6 . . ? C9 S1 C3 99.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3W Cd1 O3 C7 117.8(4) . . . . ? N1 Cd1 O3 C7 -138.2(3) . . . . ? O1W Cd1 O3 C7 -46.1(3) . . . . ? O4 Cd1 O3 C7 2.2(3) . . . . ? O2 Cd1 O3 C7 140.2(3) 5_767 . . . ? O2W Cd1 O3 C7 70.6(3) . . . . ? O3W Cd1 O3 Cd2 -14.8(4) . . . . ? N1 Cd1 O3 Cd2 89.16(15) . . . . ? O1W Cd1 O3 Cd2 -178.65(14) . . . . ? O4 Cd1 O3 Cd2 -130.40(18) . . . . ? O2 Cd1 O3 Cd2 7.57(11) 5_767 . . . ? O2W Cd1 O3 Cd2 -61.98(13) . . . . ? O5 Cd2 O3 C7 164.5(4) 5_767 . . . ? O2 Cd2 O3 C7 -117.5(4) 5_767 . . . ? O6 Cd2 O3 C7 79.8(4) . . . . ? O8 Cd2 O3 C7 -7.8(5) 6_566 . . . ? O7 Cd2 O3 C7 -24.4(4) 6_566 . . . ? C15 Cd2 O3 C7 -16.9(4) 6_566 . . . ? O5 Cd2 O3 Cd1 -86.1(2) 5_767 . . . ? O2 Cd2 O3 Cd1 -8.19(12) 5_767 . . . ? O6 Cd2 O3 Cd1 -170.88(16) . . . . ? O8 Cd2 O3 Cd1 101.5(2) 6_566 . . . ? O7 Cd2 O3 Cd1 84.99(14) 6_566 . . . ? C15 Cd2 O3 Cd1 92.43(15) 6_566 . . . ? O3W Cd1 O4 C7 -153.9(3) . . . . ? N1 Cd1 O4 C7 52.8(3) . . . . ? O3 Cd1 O4 C7 -2.2(3) . . . . ? O1W Cd1 O4 C7 132.1(3) . . . . ? O2 Cd1 O4 C7 -47.2(3) 5_767 . . . ? O2W Cd1 O4 C7 -104.8(3) . . . . ? O5 Cd2 O6 C8 -134.6(4) 5_767 . . . ? O2 Cd2 O6 C8 -28.1(5) 5_767 . . . ? O8 Cd2 O6 C8 140.3(4) 6_566 . . . ? O3 Cd2 O6 C8 5.9(4) . . . . ? O7 Cd2 O6 C8 85.0(4) 6_566 . . . ? C15 Cd2 O6 C8 112.7(4) 6_566 . . . ? O3W Cd1 O2W Cd1 74.48(10) . . . 2_757 ? N1 Cd1 O2W Cd1 147.4(2) . . . 2_757 ? O3 Cd1 O2W Cd1 -122.64(8) . . . 2_757 ? O1W Cd1 O2W Cd1 -7.87(13) . . . 2_757 ? O4 Cd1 O2W Cd1 -70.40(9) . . . 2_757 ? O2 Cd1 O2W Cd1 164.32(8) 5_767 . . 2_757 ? O3W Cd1 N1 C21 157.9(5) . . . . ? O3 Cd1 N1 C21 0.1(5) . . . . ? O1W Cd1 N1 C21 -112.6(5) . . . . ? O4 Cd1 N1 C21 -41.5(5) . . . . ? O2 Cd1 N1 C21 73.7(5) 5_767 . . . ? O2W Cd1 N1 C21 89.7(5) . . . . ? O3W Cd1 N1 C17 -6.6(4) . . . . ? O3 Cd1 N1 C17 -164.3(4) . . . . ? O1W Cd1 N1 C17 83.0(4) . . . . ? O4 Cd1 N1 C17 154.1(4) . . . . ? O2 Cd1 N1 C17 -90.7(4) 5_767 . . . ? O2W Cd1 N1 C17 -74.7(5) . . . . ? C6 C1 C2 C3 -1.2(7) . . . . ? C7 C1 C2 C3 179.5(4) . . . . ? C6 C1 C2 C8 173.3(5) . . . . ? C7 C1 C2 C8 -6.0(7) . . . . ? C1 C2 C3 C4 1.4(7) . . . . ? C8 C2 C3 C4 -173.4(5) . . . . ? C1 C2 C3 S1 -177.9(4) . . . . ? C8 C2 C3 S1 7.2(6) . . . . ? C2 C3 C4 C5 -0.2(8) . . . . ? S1 C3 C4 C5 179.2(4) . . . . ? C3 C4 C5 C6 -1.3(8) . . . . ? C4 C5 C6 C1 1.5(8) . . . . ? C2 C1 C6 C5 -0.2(8) . . . . ? C7 C1 C6 C5 179.1(5) . . . . ? Cd1 O4 C7 O3 3.9(5) . . . . ? Cd1 O4 C7 C1 -175.0(4) . . . . ? Cd1 O3 C7 O4 -4.1(5) . . . . ? Cd2 O3 C7 O4 109.4(5) . . . . ? Cd1 O3 C7 C1 174.8(4) . . . . ? Cd2 O3 C7 C1 -71.7(5) . . . . ? C2 C1 C7 O4 179.9(5) . . . . ? C6 C1 C7 O4 0.6(7) . . . . ? C2 C1 C7 O3 1.0(7) . . . . ? C6 C1 C7 O3 -178.3(4) . . . . ? Cd2 O5 C8 O6 6.7(5) 5_767 . . . ? Cd2 O5 C8 C2 -169.1(3) 5_767 . . . ? Cd2 O6 C8 O5 98.4(5) . . . . ? Cd2 O6 C8 C2 -86.0(5) . . . . ? C1 C2 C8 O5 -93.7(6) . . . . ? C3 C2 C8 O5 80.9(6) . . . . ? C1 C2 C8 O6 90.4(6) . . . . ? C3 C2 C8 O6 -95.0(6) . . . . ? C14 C9 C10 C11 4.3(7) . . . . ? S1 C9 C10 C11 -176.9(4) . . . . ? C14 C9 C10 C16 -171.0(4) . . . . ? S1 C9 C10 C16 7.8(6) . . . . ? C9 C10 C11 C12 -0.7(7) . . . . ? C16 C10 C11 C12 174.4(4) . . . . ? C9 C10 C11 C15 -179.8(4) . . . . ? C16 C10 C11 C15 -4.6(7) . . . . ? C10 C11 C12 C13 -3.4(8) . . . . ? C15 C11 C12 C13 175.7(5) . . . . ? C11 C12 C13 C14 4.0(8) . . . . ? C12 C13 C14 C9 -0.3(8) . . . . ? C10 C9 C14 C13 -3.8(8) . . . . ? S1 C9 C14 C13 177.4(4) . . . . ? Cd2 O7 C15 O8 -2.2(5) 6_565 . . . ? Cd2 O7 C15 C11 175.3(4) 6_565 . . . ? Cd2 O8 C15 O7 2.4(6) 6_565 . . . ? Cd2 O8 C15 C11 -175.2(4) 6_565 . . . ? C12 C11 C15 O7 -159.7(5) . . . . ? C10 C11 C15 O7 19.4(7) . . . . ? C12 C11 C15 O8 17.9(7) . . . . ? C10 C11 C15 O8 -163.0(5) . . . . ? Cd2 O2 C16 O1 -168.1(4) 5_767 . . . ? Cd1 O2 C16 O1 9.1(7) 5_767 . . . ? Cd2 O2 C16 C10 9.2(7) 5_767 . . . ? Cd1 O2 C16 C10 -173.5(3) 5_767 . . . ? C9 C10 C16 O1 75.7(6) . . . . ? C11 C10 C16 O1 -99.4(6) . . . . ? C9 C10 C16 O2 -101.9(5) . . . . ? C11 C10 C16 O2 83.0(6) . . . . ? C21 N1 C17 C18 1.4(9) . . . . ? Cd1 N1 C17 C18 166.6(5) . . . . ? N1 C17 C18 C19 -2.6(10) . . . . ? C17 C18 C19 C20 1.9(10) . . . . ? C17 C18 C19 C22 -179.4(6) . . . . ? C18 C19 C20 C21 -0.2(10) . . . . ? C22 C19 C20 C21 -178.7(7) . . . . ? C17 N1 C21 C20 0.4(9) . . . . ? Cd1 N1 C21 C20 -164.9(5) . . . . ? C19 C20 C21 N1 -1.0(11) . . . . ? C18 C19 C22 C22 173.2(13) . . . 7_767 ? C20 C19 C22 C22 -8.2(18) . . . 7_767 ? C14 C9 S1 C3 -47.0(4) . . . . ? C10 C9 S1 C3 134.2(4) . . . . ? C4 C3 S1 C9 97.5(4) . . . . ? C2 C3 S1 C9 -83.2(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.147 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.107 # Attachment '3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 857056' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H20 Cd2 N4 O8 S' _chemical_formula_weight 821.36 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' 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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'P 21/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 11.418(2) _cell_length_b 14.628(3) _cell_length_c 20.288(6) _cell_angle_alpha 90.00 _cell_angle_beta 120.49(2) _cell_angle_gamma 90.00 _cell_volume 2920.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7120 _cell_measurement_theta_min 2.0698 _cell_measurement_theta_max 29.1862 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.868 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 1.587 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5266 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS(2009) _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 ? _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 28641 _diffrn_reflns_av_R_equivalents 0.0814 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5137 _reflns_number_gt 4489 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0886P)^2^+8.1160P] 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 5137 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0929 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.2045 _refine_ls_wR_factor_gt 0.1870 _refine_ls_goodness_of_fit_ref 1.226 _refine_ls_restrained_S_all 1.226 _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 0.05001(7) 0.84624(5) 0.56879(4) 0.0439(2) Uani 1 1 d . . . Cd2 Cd 0.33324(6) 0.96150(5) 0.48217(4) 0.0437(3) Uani 1 1 d . . . O1 O 0.5460(6) 0.9900(5) 0.5812(4) 0.0485(16) Uani 1 1 d . . . O2 O 0.5012(7) 0.8411(5) 0.5726(4) 0.061(2) Uani 1 1 d . . . O3 O 0.7669(7) 0.9024(5) 0.5643(4) 0.0564(18) Uani 1 1 d . . . O4 O 0.9664(7) 0.8378(5) 0.6452(4) 0.061(2) Uani 1 1 d . . . O5 O 0.1857(7) 1.2464(5) 0.5341(4) 0.063(2) Uani 1 1 d . . . O6 O 0.1026(6) 1.1128(5) 0.5450(4) 0.0521(17) Uani 1 1 d . . . O7 O 0.1975(7) 0.9507(4) 0.6497(4) 0.0491(16) Uani 1 1 d . . . O8 O 0.2368(6) 0.9385(4) 0.5550(4) 0.0459(16) Uani 1 1 d . . . N1 N 0.1501(8) 0.7159(6) 0.5708(5) 0.054(2) Uani 1 1 d . . . N2 N 0.2720(8) 0.6163(6) 0.5509(4) 0.049(2) Uani 1 1 d . . . N3 N 0.0332(7) 0.3718(6) 0.2163(4) 0.0472(19) Uani 1 1 d . . . N4 N -0.1721(8) 0.3904(6) 0.1197(4) 0.050(2) Uani 1 1 d . . . C1 C 0.6997(9) 0.8946(6) 0.6852(5) 0.040(2) Uani 1 1 d . . . C2 C 0.8272(9) 0.8787(6) 0.6947(5) 0.042(2) Uani 1 1 d . . . C3 C 0.9377(10) 0.8663(7) 0.7682(5) 0.052(3) Uani 1 1 d . . . H3 H 1.0241 0.8592 0.7751 0.062 Uiso 1 1 calc R . . C4 C 0.9214(10) 0.8643(8) 0.8306(6) 0.060(3) Uani 1 1 d . . . H4 H 0.9954 0.8528 0.8791 0.072 Uiso 1 1 calc R . . C5 C 0.7948(10) 0.8794(7) 0.8212(5) 0.053(3) Uani 1 1 d . . . H5 H 0.7833 0.8789 0.8634 0.063 Uiso 1 1 calc R . . C6 C 0.6858(9) 0.8952(7) 0.7497(5) 0.044(2) Uani 1 1 d . . . C7 C 0.4891(9) 1.0268(6) 0.7136(5) 0.044(2) Uani 1 1 d . . . C8 C 0.5866(9) 1.0940(7) 0.7502(5) 0.043(2) Uani 1 1 d . . . H8 H 0.6713 1.0781 0.7912 0.052 Uiso 1 1 calc R . . C9 C 0.5603(10) 1.1849(7) 0.7270(6) 0.054(3) Uani 1 1 d . . . H9 H 0.6266 1.2295 0.7523 0.065 Uiso 1 1 calc R . . C10 C 0.4354(10) 1.2080(7) 0.6663(6) 0.051(2) Uani 1 1 d . . . H10 H 0.4183 1.2680 0.6489 0.061 Uiso 1 1 calc R . . C11 C 0.3331(9) 1.1416(6) 0.6301(5) 0.038(2) Uani 1 1 d . . . C12 C 0.3622(8) 1.0517(6) 0.6533(5) 0.039(2) Uani 1 1 d . . . C13 C 0.5751(9) 0.9080(8) 0.6070(5) 0.045(2) Uani 1 1 d . . . C14 C 0.8530(9) 0.8734(6) 0.6291(5) 0.044(2) Uani 1 1 d . . . C15 C 0.1983(9) 1.1714(7) 0.5648(5) 0.042(2) Uani 1 1 d . . . C16 C 0.2583(9) 0.9769(6) 0.6154(5) 0.043(2) Uani 1 1 d . . . C17 C 0.2604(10) 0.7039(7) 0.5658(5) 0.049(2) Uani 1 1 d . . . H17 H 0.3213 0.7499 0.5719 0.059 Uiso 1 1 calc R . . C18 C 0.0890(10) 0.6321(7) 0.5576(6) 0.052(2) Uani 1 1 d . . . H18 H 0.0081 0.6203 0.5565 0.063 Uiso 1 1 calc R . . C19 C 0.1627(10) 0.5697(7) 0.5464(6) 0.053(2) Uani 1 1 d . . . H19 H 0.1442 0.5075 0.5374 0.063 Uiso 1 1 calc R . . C20 C 0.3841(10) 0.5764(9) 0.5446(6) 0.067(3) Uani 1 1 d . . . H20A H 0.4372 0.5366 0.5880 0.080 Uiso 1 1 calc R . . H20B H 0.4431 0.6250 0.5460 0.080 Uiso 1 1 calc R . . C21 C 0.3325(10) 0.5224(7) 0.4714(6) 0.053(3) Uani 1 1 d . . . C22 C 0.3085(11) 0.5652(8) 0.4056(7) 0.064(3) Uani 1 1 d . . . H22 H 0.3255 0.6274 0.4063 0.076 Uiso 1 1 calc R . . C23 C 0.2593(10) 0.5167(8) 0.3383(6) 0.058(3) Uani 1 1 d . . . H23 H 0.2428 0.5466 0.2939 0.070 Uiso 1 1 calc R . . C24 C 0.2345(10) 0.4242(8) 0.3364(6) 0.052(3) Uani 1 1 d . . . C25 C 0.2619(10) 0.3809(8) 0.4029(6) 0.055(3) Uani 1 1 d . . . H25 H 0.2469 0.3184 0.4027 0.066 Uiso 1 1 calc R . . C26 C 0.3119(11) 0.4302(9) 0.4707(6) 0.067(3) Uani 1 1 d . . . H26 H 0.3313 0.4004 0.5156 0.080 Uiso 1 1 calc R . . C27 C 0.1810(10) 0.3701(8) 0.2630(6) 0.060(3) Uani 1 1 d . . . H27A H 0.2190 0.3951 0.2335 0.072 Uiso 1 1 calc R . . H27B H 0.2112 0.3072 0.2754 0.072 Uiso 1 1 calc R . . C28 C -0.0435(9) 0.3993(7) 0.1448(5) 0.049(2) Uani 1 1 d . . . H28 H -0.0086 0.4225 0.1156 0.059 Uiso 1 1 calc R . . C29 C -0.1818(10) 0.3563(8) 0.1788(6) 0.061(3) Uani 1 1 d . . . H29 H -0.2623 0.3433 0.1779 0.073 Uiso 1 1 calc R . . C30 C -0.0567(11) 0.3445(9) 0.2384(6) 0.068(3) Uani 1 1 d . . . H30 H -0.0346 0.3219 0.2862 0.082 Uiso 1 1 calc R . . S1 S 0.5225(3) 0.91049(18) 0.74140(15) 0.0508(6) 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 Cd1 0.0370(4) 0.0483(4) 0.0431(4) 0.0018(3) 0.0179(3) 0.0032(3) Cd2 0.0312(4) 0.0593(5) 0.0359(4) 0.0031(3) 0.0135(3) -0.0023(3) O1 0.037(4) 0.062(4) 0.048(4) 0.013(3) 0.022(3) 0.008(3) O2 0.045(4) 0.080(5) 0.056(4) -0.007(4) 0.024(4) -0.011(4) O3 0.060(4) 0.064(5) 0.043(4) 0.007(3) 0.025(4) 0.014(4) O4 0.044(4) 0.079(5) 0.061(5) 0.013(4) 0.029(4) 0.009(4) O5 0.059(5) 0.053(4) 0.058(4) 0.008(4) 0.018(4) 0.000(3) O6 0.029(3) 0.075(5) 0.044(4) 0.010(3) 0.012(3) -0.002(3) O7 0.044(4) 0.052(4) 0.050(4) 0.000(3) 0.023(3) -0.007(3) O8 0.040(4) 0.049(4) 0.045(4) -0.012(3) 0.018(3) -0.009(3) N1 0.047(5) 0.045(5) 0.061(5) 0.002(4) 0.022(4) -0.001(4) N2 0.038(4) 0.065(5) 0.046(4) -0.005(4) 0.023(4) 0.006(4) N3 0.029(4) 0.070(5) 0.042(4) 0.008(4) 0.017(3) 0.006(4) N4 0.035(4) 0.067(5) 0.046(4) 0.007(4) 0.018(4) 0.004(4) C1 0.034(5) 0.045(5) 0.040(5) 0.001(4) 0.019(4) -0.004(4) C2 0.030(5) 0.046(5) 0.047(5) 0.002(4) 0.017(4) 0.006(4) C3 0.034(5) 0.079(7) 0.047(6) -0.009(5) 0.024(5) -0.007(5) C4 0.033(5) 0.081(8) 0.048(6) -0.010(5) 0.008(5) 0.003(5) C5 0.057(6) 0.059(6) 0.037(5) -0.005(4) 0.020(5) 0.010(5) C6 0.040(5) 0.050(5) 0.045(5) 0.006(4) 0.023(4) 0.009(4) C7 0.041(5) 0.050(5) 0.035(5) -0.008(4) 0.016(4) 0.004(4) C8 0.033(5) 0.056(6) 0.038(5) -0.004(4) 0.015(4) 0.003(4) C9 0.038(5) 0.051(6) 0.055(6) -0.019(5) 0.010(5) -0.011(5) C10 0.048(6) 0.055(6) 0.048(5) -0.006(5) 0.023(5) -0.001(5) C11 0.032(5) 0.045(5) 0.042(5) 0.000(4) 0.021(4) -0.001(4) C12 0.030(5) 0.056(6) 0.031(4) -0.011(4) 0.015(4) -0.009(4) C13 0.024(4) 0.075(7) 0.039(5) -0.006(5) 0.018(4) -0.013(5) C14 0.038(5) 0.044(5) 0.043(5) 0.003(4) 0.017(4) -0.010(4) C15 0.042(5) 0.050(6) 0.049(5) 0.003(4) 0.032(5) 0.009(4) C16 0.041(5) 0.049(5) 0.039(5) 0.000(4) 0.021(4) 0.000(4) C17 0.040(6) 0.054(6) 0.051(6) -0.005(5) 0.021(5) -0.002(4) C18 0.047(6) 0.058(6) 0.059(6) 0.010(5) 0.033(5) 0.009(5) C19 0.047(6) 0.053(6) 0.054(6) -0.005(5) 0.023(5) -0.006(5) C20 0.036(6) 0.094(9) 0.067(7) -0.020(6) 0.024(5) 0.010(6) C21 0.042(6) 0.049(6) 0.055(6) -0.010(5) 0.015(5) 0.006(4) C22 0.056(7) 0.047(6) 0.079(8) 0.005(6) 0.027(6) 0.007(5) C23 0.044(6) 0.070(7) 0.053(6) 0.007(5) 0.019(5) 0.012(5) C24 0.042(6) 0.068(7) 0.054(6) 0.010(5) 0.029(5) 0.012(5) C25 0.049(6) 0.056(6) 0.054(6) 0.005(5) 0.021(5) 0.009(5) C26 0.057(7) 0.079(8) 0.053(6) 0.000(6) 0.020(6) 0.017(6) C27 0.043(6) 0.075(7) 0.046(6) -0.001(5) 0.012(5) 0.009(5) C28 0.041(6) 0.069(7) 0.038(5) 0.008(5) 0.021(4) 0.004(5) C29 0.042(6) 0.083(8) 0.057(6) 0.023(6) 0.025(5) 0.006(5) C30 0.049(7) 0.094(9) 0.049(6) 0.030(6) 0.016(5) 0.011(6) S1 0.0453(14) 0.0572(15) 0.0546(15) 0.0139(12) 0.0287(12) 0.0063(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O6 2.154(6) 3_576 ? Cd1 O4 2.198(7) 1_455 ? Cd1 N1 2.212(8) . ? Cd1 O7 2.250(6) . ? Cd2 N4 2.208(8) 2 ? Cd2 O3 2.250(7) 3_676 ? Cd2 O8 2.271(7) . ? Cd2 O1 2.271(6) . ? Cd2 O1 2.421(6) 3_676 ? Cd2 O2 2.564(8) . ? O1 C13 1.282(12) . ? O1 Cd2 2.421(6) 3_676 ? O2 C13 1.249(12) . ? O3 C14 1.250(11) . ? O3 Cd2 2.250(7) 3_676 ? O4 C14 1.275(11) . ? O4 Cd1 2.198(7) 1_655 ? O5 C15 1.232(11) . ? O6 C15 1.283(11) . ? O6 Cd1 2.154(6) 3_576 ? O7 C16 1.267(11) . ? O8 C16 1.254(11) . ? N1 C17 1.326(13) . ? N1 C18 1.368(13) . ? N2 C17 1.337(13) . ? N2 C19 1.384(13) . ? N2 C20 1.471(12) . ? N3 C28 1.321(11) . ? N3 C30 1.371(14) . ? N3 C27 1.458(12) . ? N4 C28 1.294(12) . ? N4 C29 1.354(13) . ? N4 Cd2 2.208(8) 2_545 ? C1 C2 1.388(12) . ? C1 C6 1.397(13) . ? C1 C13 1.512(12) . ? C2 C3 1.393(13) . ? C2 C14 1.504(13) . ? C3 C4 1.370(14) . ? C3 H3 0.9300 . ? C4 C5 1.376(14) . ? C4 H4 0.9300 . ? C5 C6 1.369(13) . ? C5 H5 0.9300 . ? C6 S1 1.799(9) . ? C7 C8 1.385(13) . ? C7 C12 1.388(12) . ? C7 S1 1.773(10) . ? C8 C9 1.392(14) . ? C8 H8 0.9300 . ? C9 C10 1.372(13) . ? C9 H9 0.9300 . ? C10 C11 1.405(13) . ? C10 H10 0.9300 . ? C11 C12 1.380(12) . ? C11 C15 1.499(12) . ? C12 C16 1.507(12) . ? C17 H17 0.9300 . ? C18 C19 1.337(14) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.512(14) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C26 1.367(16) . ? C21 C22 1.370(16) . ? C22 C23 1.381(15) . ? C22 H22 0.9300 . ? C23 C24 1.378(16) . ? C23 H23 0.9300 . ? C24 C25 1.375(14) . ? C24 C27 1.516(14) . ? C25 C26 1.392(15) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28 0.9300 . ? C29 C30 1.334(14) . ? C29 H29 0.9300 . ? C30 H30 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 O6 Cd1 O4 111.5(3) 3_576 1_455 ? O6 Cd1 N1 112.9(3) 3_576 . ? O4 Cd1 N1 110.1(3) 1_455 . ? O6 Cd1 O7 119.5(3) 3_576 . ? O4 Cd1 O7 87.5(3) 1_455 . ? N1 Cd1 O7 112.5(3) . . ? N4 Cd2 O3 91.1(3) 2 3_676 ? N4 Cd2 O8 95.1(3) 2 . ? O3 Cd2 O8 95.3(2) 3_676 . ? N4 Cd2 O1 157.4(3) 2 . ? O3 Cd2 O1 107.2(3) 3_676 . ? O8 Cd2 O1 96.1(2) . . ? N4 Cd2 O1 94.0(3) 2 3_676 ? O3 Cd2 O1 79.8(2) 3_676 3_676 ? O8 Cd2 O1 169.7(2) . 3_676 ? O1 Cd2 O1 77.0(2) . 3_676 ? N4 Cd2 O2 108.2(3) 2 . ? O3 Cd2 O2 160.7(2) 3_676 . ? O8 Cd2 O2 82.3(2) . . ? O1 Cd2 O2 54.3(2) . . ? O1 Cd2 O2 99.3(2) 3_676 . ? C13 O1 Cd2 97.4(6) . . ? C13 O1 Cd2 113.0(6) . 3_676 ? Cd2 O1 Cd2 103.0(2) . 3_676 ? C13 O2 Cd2 84.8(6) . . ? C14 O3 Cd2 134.6(7) . 3_676 ? C14 O4 Cd1 122.9(6) . 1_655 ? C15 O6 Cd1 104.3(6) . 3_576 ? C16 O7 Cd1 102.7(6) . . ? C16 O8 Cd2 130.6(6) . . ? C17 N1 C18 106.0(9) . . ? C17 N1 Cd1 128.0(7) . . ? C18 N1 Cd1 124.2(7) . . ? C17 N2 C19 107.4(8) . . ? C17 N2 C20 126.1(9) . . ? C19 N2 C20 126.4(10) . . ? C28 N3 C30 105.0(8) . . ? C28 N3 C27 128.4(9) . . ? C30 N3 C27 126.6(9) . . ? C28 N4 C29 105.9(8) . . ? C28 N4 Cd2 124.2(7) . 2_545 ? C29 N4 Cd2 126.7(7) . 2_545 ? C2 C1 C6 118.8(8) . . ? C2 C1 C13 122.0(8) . . ? C6 C1 C13 119.2(8) . . ? C1 C2 C3 119.1(9) . . ? C1 C2 C14 123.2(8) . . ? C3 C2 C14 117.7(8) . . ? C4 C3 C2 121.3(9) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 119.5(9) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 120.1(10) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 121.1(9) . . ? C5 C6 S1 117.5(8) . . ? C1 C6 S1 121.3(7) . . ? C8 C7 C12 118.8(9) . . ? C8 C7 S1 121.7(7) . . ? C12 C7 S1 119.4(7) . . ? C7 C8 C9 121.3(9) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C10 C9 C8 119.1(9) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C9 C10 C11 120.6(10) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 119.2(8) . . ? C12 C11 C15 122.7(8) . . ? C10 C11 C15 118.0(8) . . ? C11 C12 C7 120.9(8) . . ? C11 C12 C16 121.8(8) . . ? C7 C12 C16 117.3(8) . . ? O2 C13 O1 122.9(9) . . ? O2 C13 C1 119.6(9) . . ? O1 C13 C1 117.4(8) . . ? O3 C14 O4 124.3(9) . . ? O3 C14 C2 120.8(9) . . ? O4 C14 C2 115.0(8) . . ? O5 C15 O6 125.0(9) . . ? O5 C15 C11 120.6(9) . . ? O6 C15 C11 114.3(8) . . ? O8 C16 O7 120.8(9) . . ? O8 C16 C12 122.5(8) . . ? O7 C16 C12 116.6(8) . . ? N1 C17 N2 110.6(9) . . ? N1 C17 H17 124.7 . . ? N2 C17 H17 124.7 . . ? C19 C18 N1 110.1(9) . . ? C19 C18 H18 124.9 . . ? N1 C18 H18 124.9 . . ? C18 C19 N2 106.0(9) . . ? C18 C19 H19 127.0 . . ? N2 C19 H19 127.0 . . ? N2 C20 C21 111.7(8) . . ? N2 C20 H20A 109.3 . . ? C21 C20 H20A 109.3 . . ? N2 C20 H20B 109.3 . . ? C21 C20 H20B 109.3 . . ? H20A C20 H20B 107.9 . . ? C26 C21 C22 119.4(10) . . ? C26 C21 C20 120.3(11) . . ? C22 C21 C20 120.2(11) . . ? C21 C22 C23 120.6(11) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 120.4(11) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 118.9(10) . . ? C25 C24 C27 120.1(10) . . ? C23 C24 C27 120.9(10) . . ? C24 C25 C26 120.3(11) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C21 C26 C25 120.2(11) . . ? C21 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? N3 C27 C24 112.7(9) . . ? N3 C27 H27A 109.1 . . ? C24 C27 H27A 109.1 . . ? N3 C27 H27B 109.1 . . ? C24 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? N4 C28 N3 112.9(9) . . ? N4 C28 H28 123.5 . . ? N3 C28 H28 123.5 . . ? C30 C29 N4 108.7(9) . . ? C30 C29 H29 125.7 . . ? N4 C29 H29 125.7 . . ? C29 C30 N3 107.5(9) . . ? C29 C30 H30 126.3 . . ? N3 C30 H30 126.3 . . ? C7 S1 C6 101.2(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 N4 Cd2 O1 C13 -47.5(10) 2 . . . ? O3 Cd2 O1 C13 169.4(5) 3_676 . . . ? O8 Cd2 O1 C13 71.9(6) . . . . ? O1 Cd2 O1 C13 -115.8(6) 3_676 . . . ? O2 Cd2 O1 C13 -4.1(5) . . . . ? N4 Cd2 O1 Cd2 68.3(8) 2 . . 3_676 ? O3 Cd2 O1 Cd2 -74.8(3) 3_676 . . 3_676 ? O8 Cd2 O1 Cd2 -172.3(3) . . . 3_676 ? O1 Cd2 O1 Cd2 0.0 3_676 . . 3_676 ? O2 Cd2 O1 Cd2 111.7(4) . . . 3_676 ? N4 Cd2 O2 C13 168.1(5) 2 . . . ? O3 Cd2 O2 C13 -14.9(11) 3_676 . . . ? O8 Cd2 O2 C13 -98.9(5) . . . . ? O1 Cd2 O2 C13 4.2(5) . . . . ? O1 Cd2 O2 C13 70.8(6) 3_676 . . . ? O6 Cd1 O7 C16 -61.1(6) 3_576 . . . ? O4 Cd1 O7 C16 -174.5(6) 1_455 . . . ? N1 Cd1 O7 C16 74.8(6) . . . . ? N4 Cd2 O8 C16 -163.0(8) 2 . . . ? O3 Cd2 O8 C16 -71.4(8) 3_676 . . . ? O1 Cd2 O8 C16 36.6(8) . . . . ? O1 Cd2 O8 C16 -10.1(17) 3_676 . . . ? O2 Cd2 O8 C16 89.3(8) . . . . ? O6 Cd1 N1 C17 90.0(8) 3_576 . . . ? O4 Cd1 N1 C17 -144.7(8) 1_455 . . . ? O7 Cd1 N1 C17 -48.9(9) . . . . ? O6 Cd1 N1 C18 -72.1(9) 3_576 . . . ? O4 Cd1 N1 C18 53.2(9) 1_455 . . . ? O7 Cd1 N1 C18 149.0(8) . . . . ? C6 C1 C2 C3 -1.7(14) . . . . ? C13 C1 C2 C3 -179.5(9) . . . . ? C6 C1 C2 C14 177.9(9) . . . . ? C13 C1 C2 C14 0.0(15) . . . . ? C1 C2 C3 C4 3.8(16) . . . . ? C14 C2 C3 C4 -175.8(10) . . . . ? C2 C3 C4 C5 -3.3(17) . . . . ? C3 C4 C5 C6 0.8(17) . . . . ? C4 C5 C6 C1 1.2(16) . . . . ? C4 C5 C6 S1 177.9(8) . . . . ? C2 C1 C6 C5 -0.8(15) . . . . ? C13 C1 C6 C5 177.2(9) . . . . ? C2 C1 C6 S1 -177.3(7) . . . . ? C13 C1 C6 S1 0.6(13) . . . . ? C12 C7 C8 C9 -1.2(14) . . . . ? S1 C7 C8 C9 178.7(8) . . . . ? C7 C8 C9 C10 -0.3(15) . . . . ? C8 C9 C10 C11 2.8(16) . . . . ? C9 C10 C11 C12 -3.9(14) . . . . ? C9 C10 C11 C15 179.2(9) . . . . ? C10 C11 C12 C7 2.4(14) . . . . ? C15 C11 C12 C7 179.2(8) . . . . ? C10 C11 C12 C16 -178.2(8) . . . . ? C15 C11 C12 C16 -1.4(14) . . . . ? C8 C7 C12 C11 0.1(14) . . . . ? S1 C7 C12 C11 -179.8(7) . . . . ? C8 C7 C12 C16 -179.4(8) . . . . ? S1 C7 C12 C16 0.8(11) . . . . ? Cd2 O2 C13 O1 -7.3(9) . . . . ? Cd2 O2 C13 C1 168.3(8) . . . . ? Cd2 O1 C13 O2 8.2(10) . . . . ? Cd2 O1 C13 O2 -99.4(9) 3_676 . . . ? Cd2 O1 C13 C1 -167.4(7) . . . . ? Cd2 O1 C13 C1 85.0(8) 3_676 . . . ? C2 C1 C13 O2 93.7(11) . . . . ? C6 C1 C13 O2 -84.1(12) . . . . ? C2 C1 C13 O1 -90.5(12) . . . . ? C6 C1 C13 O1 91.7(11) . . . . ? Cd2 O3 C14 O4 -121.6(10) 3_676 . . . ? Cd2 O3 C14 C2 58.6(12) 3_676 . . . ? Cd1 O4 C14 O3 13.0(13) 1_655 . . . ? Cd1 O4 C14 C2 -167.1(6) 1_655 . . . ? C1 C2 C14 O3 15.6(14) . . . . ? C3 C2 C14 O3 -164.9(9) . . . . ? C1 C2 C14 O4 -164.3(9) . . . . ? C3 C2 C14 O4 15.3(13) . . . . ? Cd1 O6 C15 O5 18.2(11) 3_576 . . . ? Cd1 O6 C15 C11 -161.3(6) 3_576 . . . ? C12 C11 C15 O5 -162.8(9) . . . . ? C10 C11 C15 O5 14.1(13) . . . . ? C12 C11 C15 O6 16.7(13) . . . . ? C10 C11 C15 O6 -166.5(8) . . . . ? Cd2 O8 C16 O7 -176.5(6) . . . . ? Cd2 O8 C16 C12 -0.2(13) . . . . ? Cd1 O7 C16 O8 -6.2(10) . . . . ? Cd1 O7 C16 C12 177.3(6) . . . . ? C11 C12 C16 O8 83.3(12) . . . . ? C7 C12 C16 O8 -97.3(11) . . . . ? C11 C12 C16 O7 -100.3(11) . . . . ? C7 C12 C16 O7 79.1(11) . . . . ? C18 N1 C17 N2 -0.6(11) . . . . ? Cd1 N1 C17 N2 -165.3(6) . . . . ? C19 N2 C17 N1 -0.2(11) . . . . ? C20 N2 C17 N1 -177.3(9) . . . . ? C17 N1 C18 C19 1.3(12) . . . . ? Cd1 N1 C18 C19 166.7(7) . . . . ? N1 C18 C19 N2 -1.5(12) . . . . ? C17 N2 C19 C18 1.0(11) . . . . ? C20 N2 C19 C18 178.1(10) . . . . ? C17 N2 C20 C21 -128.8(11) . . . . ? C19 N2 C20 C21 54.7(15) . . . . ? N2 C20 C21 C26 -93.8(13) . . . . ? N2 C20 C21 C22 87.5(14) . . . . ? C26 C21 C22 C23 2.3(17) . . . . ? C20 C21 C22 C23 -178.9(10) . . . . ? C21 C22 C23 C24 -0.5(17) . . . . ? C22 C23 C24 C25 -1.1(15) . . . . ? C22 C23 C24 C27 -179.8(10) . . . . ? C23 C24 C25 C26 0.9(15) . . . . ? C27 C24 C25 C26 179.6(10) . . . . ? C22 C21 C26 C25 -2.5(17) . . . . ? C20 C21 C26 C25 178.8(10) . . . . ? C24 C25 C26 C21 0.9(17) . . . . ? C28 N3 C27 C24 123.0(12) . . . . ? C30 N3 C27 C24 -57.0(15) . . . . ? C25 C24 C27 N3 94.5(12) . . . . ? C23 C24 C27 N3 -86.9(13) . . . . ? C29 N4 C28 N3 1.1(13) . . . . ? Cd2 N4 C28 N3 162.2(7) 2_545 . . . ? C30 N3 C28 N4 -1.1(13) . . . . ? C27 N3 C28 N4 179.0(10) . . . . ? C28 N4 C29 C30 -0.7(13) . . . . ? Cd2 N4 C29 C30 -161.1(8) 2_545 . . . ? N4 C29 C30 N3 0.1(14) . . . . ? C28 N3 C30 C29 0.6(13) . . . . ? C27 N3 C30 C29 -179.5(11) . . . . ? C8 C7 S1 C6 -46.3(9) . . . . ? C12 C7 S1 C6 133.5(8) . . . . ? C5 C6 S1 C7 113.2(8) . . . . ? C1 C6 S1 C7 -70.1(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.622 _refine_diff_density_min -1.795 _refine_diff_density_rms 0.271 # Attachment '4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 857057' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H32 Cd2 N2 O17 S' _chemical_formula_weight 925.42 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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 19.695(4) _cell_length_b 9.2506(19) _cell_length_c 18.770(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3419.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 10885 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 29.12 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 1.383 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7599 _exptl_absorpt_correction_T_max 0.7988 _exptl_absorpt_process_details 'SADABS (Bruker, 2009)' _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 'Bruker Smart APEX II CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32536 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6001 _reflns_number_gt 5896 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 (Bruker, 2009)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2009)' _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^)+(0.0301P)^2^+2.3560P] 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 0.00(10) _refine_ls_number_reflns 5142 _refine_ls_number_parameters 454 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0663 _refine_ls_wR_factor_gt 0.0659 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.093 _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 0.663020(15) 0.83652(4) 0.270368(18) 0.03151(8) Uani 1 1 d . . . Cd2 Cd 0.107179(15) 0.70834(4) -0.282651(18) 0.03243(9) Uani 1 1 d . . . S1 S 0.36748(6) 0.98302(13) -0.00003(7) 0.0364(3) Uani 1 1 d . . . N1 N 0.1955(2) 0.7072(5) 0.6366(2) 0.0369(10) Uani 1 1 d . . . N2 N 0.5723(2) 0.7848(5) 0.3453(2) 0.0381(10) Uani 1 1 d . . . O1 O 0.41914(16) 0.9565(3) 0.18401(16) 0.0350(7) Uani 1 1 d . . . O2 O 0.46136(16) 1.1338(3) 0.11985(17) 0.0333(7) Uani 1 1 d . . . O3 O 0.57962(17) 0.9477(4) 0.18628(17) 0.0416(8) Uani 1 1 d . . . O4 O 0.61846(17) 0.7273(4) 0.17006(19) 0.0428(9) Uani 1 1 d . . . O5 O 0.33372(17) 0.9074(4) -0.18569(17) 0.0393(8) Uani 1 1 d . . . O6 O 0.27513(16) 1.0773(3) -0.13260(16) 0.0342(7) Uani 1 1 d . . . O7 O 0.1788(2) 0.8413(4) -0.20051(19) 0.0507(10) Uani 1 1 d . . . O8 O 0.1578(2) 0.6141(5) -0.1806(2) 0.0638(12) Uani 1 1 d . . . O9 O 0.3335(2) 0.7167(5) 0.4093(2) 0.0636(12) Uani 1 1 d . . . H9 H 0.2994 0.6716 0.3975 0.095 Uiso 1 1 calc R . . O10 O 0.43384(19) 0.7221(5) 0.5666(2) 0.0523(10) Uani 1 1 d . . . H10A H 0.4662 0.7705 0.5802 0.079 Uiso 1 1 calc R . . C1 C 0.5384(2) 0.8146(5) 0.0867(2) 0.0304(10) Uani 1 1 d . . . C2 C 0.4788(2) 0.8947(5) 0.0772(2) 0.0269(10) Uani 1 1 d . . . C3 C 0.4406(2) 0.8749(5) 0.0149(2) 0.0323(11) Uani 1 1 d . . . C4 C 0.4624(3) 0.7787(6) -0.0369(3) 0.0428(14) Uani 1 1 d . . . H4 H 0.4375 0.7675 -0.0786 0.051 Uiso 1 1 calc R . . C5 C 0.5207(3) 0.6996(6) -0.0268(3) 0.0502(16) Uani 1 1 d . . . H5 H 0.5346 0.6341 -0.0614 0.060 Uiso 1 1 calc R . . C6 C 0.5587(3) 0.7172(6) 0.0345(3) 0.0426(14) Uani 1 1 d . . . H6 H 0.5982 0.6635 0.0409 0.051 Uiso 1 1 calc R . . C7 C 0.4520(2) 1.0003(5) 0.1313(2) 0.0261(10) Uani 1 1 d . . . C8 C 0.5808(2) 0.8327(6) 0.1520(3) 0.0342(11) Uani 1 1 d . . . C9 C 0.3049(2) 0.8487(5) -0.0160(2) 0.0300(10) Uani 1 1 d . . . C10 C 0.2857(3) 0.7525(6) 0.0386(3) 0.0403(12) Uani 1 1 d . . . H10 H 0.3069 0.7576 0.0828 0.048 Uiso 1 1 calc R . . C11 C 0.2365(3) 0.6522(5) 0.0271(3) 0.0418(13) Uani 1 1 d . . . H11 H 0.2239 0.5890 0.0633 0.050 Uiso 1 1 calc R . . C12 C 0.2052(3) 0.6447(6) -0.0390(3) 0.0407(12) Uani 1 1 d . . . H12 H 0.1725 0.5740 -0.0470 0.049 Uiso 1 1 calc R . . C13 C 0.2214(2) 0.7393(5) -0.0931(2) 0.0319(11) Uani 1 1 d . . . C14 C 0.2718(2) 0.8432(5) -0.0812(2) 0.0258(9) Uani 1 1 d . . . C15 C 0.2940(2) 0.9487(5) -0.1380(2) 0.0280(10) Uani 1 1 d . . . C16 C 0.1841(2) 0.7317(6) -0.1624(3) 0.0350(11) Uani 1 1 d . . . C17 C 0.5180(3) 0.8703(6) 0.3406(3) 0.0470(14) Uani 1 1 d . . . H17 H 0.5154 0.9347 0.3026 0.056 Uiso 1 1 calc R . . C18 C 0.4662(3) 0.8680(6) 0.3886(3) 0.0432(13) Uani 1 1 d . . . H18 H 0.4292 0.9292 0.3825 0.052 Uiso 1 1 calc R . . C19 C 0.4682(2) 0.7754(6) 0.4461(3) 0.0335(11) Uani 1 1 d . . . C20 C 0.5251(3) 0.6864(7) 0.4515(3) 0.0486(15) Uani 1 1 d . . . H20 H 0.5291 0.6211 0.4889 0.058 Uiso 1 1 calc R . . C21 C 0.5750(3) 0.6965(6) 0.4009(3) 0.0463(14) Uani 1 1 d . . . H21 H 0.6131 0.6379 0.4059 0.056 Uiso 1 1 calc R . . C22 C 0.4120(2) 0.7729(6) 0.5011(3) 0.0405(12) Uani 1 1 d . . . H22 H 0.3947 0.8715 0.5072 0.049 Uiso 1 1 calc R . . C23 C 0.3531(2) 0.6750(7) 0.4762(3) 0.0446(14) Uani 1 1 d . . . H23 H 0.3696 0.5751 0.4738 0.054 Uiso 1 1 calc R . . C24 C 0.2960(2) 0.6824(6) 0.5307(3) 0.0381(12) Uani 1 1 d . . . C25 C 0.2457(3) 0.7860(6) 0.5282(3) 0.0416(13) Uani 1 1 d . . . H25 H 0.2444 0.8504 0.4902 0.050 Uiso 1 1 calc R . . C26 C 0.1980(3) 0.7955(6) 0.5806(3) 0.0421(13) Uani 1 1 d . . . H26 H 0.1653 0.8677 0.5770 0.051 Uiso 1 1 calc R . . C27 C 0.2422(2) 0.6024(6) 0.6381(3) 0.0418(12) Uani 1 1 d . . . H27 H 0.2408 0.5369 0.6756 0.050 Uiso 1 1 calc R . . C28 C 0.2922(2) 0.5855(6) 0.5873(3) 0.0422(12) Uani 1 1 d . . . H28 H 0.3231 0.5099 0.5909 0.051 Uiso 1 1 calc R . . O1W O 0.7206(2) 0.6201(4) 0.2976(2) 0.0659(12) Uani 1 1 d . . . H1WA H 0.6917 0.5534 0.3048 0.099 Uiso 1 1 d R . . H1WB H 0.7520 0.5604 0.3036 0.099 Uiso 1 1 d R . . O2W O 0.75606(16) 0.9276(4) 0.20740(18) 0.0467(8) Uani 1 1 d . . . H2WB H 0.7690 1.0146 0.2128 0.070 Uiso 1 1 d R . . H2WA H 0.7964 0.9005 0.2162 0.070 Uiso 1 1 d R . . O3W O 0.0754(2) 0.9436(4) -0.3146(2) 0.0694(13) Uani 1 1 d . . . H3WA H 0.0374 0.9476 -0.3158 0.104 Uiso 1 1 d R . . H3WB H 0.1042 0.9149 -0.2831 0.104 Uiso 1 1 d R . . O4W O -0.0029(2) 0.7000(5) -0.2310(3) 0.0798(14) Uani 1 1 d . . . H4WC H -0.0228 0.6350 -0.2553 0.120 Uiso 1 1 d R . . H4WA H -0.0305 0.7542 -0.2241 0.120 Uiso 1 1 d R . . O5W O 0.06253(19) 0.0389(4) 0.1814(2) 0.0579(10) Uani 1 1 d . . . H5WA H 0.0804 -0.0442 0.1784 0.087 Uiso 1 1 d R . . H5WB H 0.0638 0.0898 0.1504 0.087 Uiso 1 1 d R . . O6W O 0.3756(2) 0.7054(4) 0.2515(2) 0.0682(13) Uani 1 1 d . . . H6WA H 0.4041 0.6407 0.2632 0.102 Uiso 1 1 d R . . H6WB H 0.3870 0.7734 0.2235 0.102 Uiso 1 1 d R . . O7W O 0.1387(3) 0.1145(5) 0.3024(3) 0.0951(17) Uani 1 1 d . . . H7WA H 0.1484 0.2051 0.3063 0.143 Uiso 1 1 d R . . H7WB H 0.1226 0.1258 0.2666 0.143 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 0.02617(16) 0.03950(17) 0.02886(15) -0.00471(17) -0.00157(15) -0.00362(13) Cd2 0.02941(16) 0.03794(17) 0.02995(16) -0.00031(16) -0.00430(16) -0.00452(13) S1 0.0366(6) 0.0328(6) 0.0397(6) -0.0040(5) -0.0159(5) 0.0017(5) N1 0.029(2) 0.048(3) 0.034(2) 0.004(2) -0.0005(19) -0.0059(19) N2 0.029(2) 0.048(3) 0.038(2) 0.001(2) 0.0065(18) -0.0020(19) O1 0.0359(17) 0.0365(18) 0.0324(17) -0.0016(14) 0.0067(15) 0.0003(14) O2 0.0305(18) 0.0318(18) 0.0376(18) -0.0037(14) 0.0055(14) -0.0048(14) O3 0.044(2) 0.044(2) 0.0370(18) -0.0066(16) -0.0151(16) 0.0003(16) O4 0.039(2) 0.050(2) 0.039(2) -0.0057(18) -0.0111(17) 0.0048(17) O5 0.048(2) 0.0353(19) 0.0343(18) 0.0016(15) 0.0135(16) 0.0008(16) O6 0.0389(19) 0.0299(18) 0.0337(18) 0.0056(14) -0.0007(15) 0.0035(14) O7 0.066(3) 0.045(2) 0.041(2) 0.0063(17) -0.0259(18) -0.0060(19) O8 0.083(3) 0.058(3) 0.050(2) 0.014(2) -0.031(2) -0.034(2) O9 0.049(3) 0.086(3) 0.056(3) 0.003(2) 0.000(2) -0.021(2) O10 0.042(2) 0.069(3) 0.046(2) 0.009(2) -0.0092(18) -0.0234(19) C1 0.026(2) 0.039(3) 0.026(2) -0.003(2) -0.004(2) -0.001(2) C2 0.029(2) 0.028(2) 0.024(2) -0.0050(18) -0.0019(19) -0.0034(19) C3 0.031(2) 0.037(3) 0.029(2) 0.000(2) -0.001(2) -0.005(2) C4 0.045(3) 0.056(4) 0.027(3) -0.016(2) -0.013(2) 0.008(3) C5 0.056(4) 0.057(4) 0.037(3) -0.026(3) -0.009(3) 0.015(3) C6 0.038(3) 0.053(4) 0.037(3) -0.009(2) -0.003(2) 0.014(2) C7 0.018(2) 0.037(3) 0.024(2) -0.0018(19) -0.0055(18) -0.0003(18) C8 0.025(2) 0.044(3) 0.033(3) -0.001(2) -0.002(2) 0.003(2) C9 0.031(2) 0.031(2) 0.027(2) 0.0026(19) -0.004(2) 0.0030(18) C10 0.052(3) 0.041(3) 0.028(2) 0.005(2) -0.008(2) -0.001(3) C11 0.063(4) 0.032(3) 0.031(3) 0.012(2) 0.000(2) -0.003(2) C12 0.046(3) 0.039(3) 0.037(3) 0.010(2) -0.005(2) -0.013(2) C13 0.033(3) 0.035(3) 0.028(2) 0.003(2) -0.002(2) 0.001(2) C14 0.025(2) 0.029(2) 0.023(2) -0.0003(18) -0.0037(18) -0.0005(18) C15 0.031(2) 0.028(2) 0.025(2) -0.0003(19) -0.004(2) -0.0017(19) C16 0.027(2) 0.045(3) 0.033(3) 0.010(2) -0.005(2) -0.012(2) C17 0.039(3) 0.054(4) 0.048(3) 0.018(3) 0.007(3) 0.003(3) C18 0.031(3) 0.048(3) 0.051(3) 0.010(3) 0.008(2) 0.006(2) C19 0.023(2) 0.040(3) 0.038(3) -0.002(2) -0.004(2) -0.006(2) C20 0.034(3) 0.057(4) 0.055(4) 0.018(3) 0.005(3) 0.002(3) C21 0.037(3) 0.052(4) 0.050(3) 0.015(3) 0.009(3) 0.004(2) C22 0.029(2) 0.056(3) 0.036(3) 0.008(2) -0.003(2) -0.010(2) C23 0.025(3) 0.075(4) 0.033(3) 0.008(3) -0.003(2) -0.018(2) C24 0.026(3) 0.048(3) 0.040(3) -0.006(2) 0.005(2) -0.016(2) C25 0.044(3) 0.047(3) 0.034(3) 0.015(2) 0.003(2) -0.006(2) C26 0.035(3) 0.041(3) 0.051(3) 0.006(2) 0.004(3) 0.000(2) C27 0.035(3) 0.048(3) 0.042(3) 0.012(2) 0.000(2) 0.000(2) C28 0.025(2) 0.056(3) 0.046(3) 0.009(3) -0.001(2) -0.004(2) O1W 0.061(3) 0.043(2) 0.094(3) -0.005(2) -0.017(2) 0.0112(19) O2W 0.0378(18) 0.058(2) 0.044(2) -0.0014(19) 0.0102(17) -0.0066(16) O3W 0.046(2) 0.048(2) 0.114(4) 0.004(2) -0.021(2) 0.0054(19) O4W 0.073(3) 0.085(3) 0.081(3) 0.017(3) 0.039(3) 0.026(2) O5W 0.057(2) 0.054(2) 0.062(2) 0.009(2) 0.006(2) 0.0080(19) O6W 0.063(3) 0.049(2) 0.092(3) 0.006(2) -0.002(2) -0.0080(19) O7W 0.132(5) 0.048(3) 0.106(4) -0.010(3) -0.030(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O4 2.310(3) . ? Cd1 N2 2.324(4) . ? Cd1 O6 2.331(3) 2_675 ? Cd1 O2W 2.338(3) . ? Cd1 O1W 2.357(4) . ? Cd1 O3 2.499(3) . ? Cd1 O5 2.509(3) 2_675 ? Cd1 C15 2.760(4) 2_675 ? Cd2 N1 2.308(4) 1_554 ? Cd2 O8 2.330(4) . ? Cd2 O3W 2.343(4) . ? Cd2 O2 2.376(3) 3_544 ? Cd2 O4W 2.377(4) . ? Cd2 O7 2.424(4) . ? Cd2 O1 2.467(3) 3_544 ? Cd2 H3WB 1.9119 . ? S1 C9 1.776(5) . ? S1 C3 1.775(5) . ? N1 C26 1.332(6) . ? N1 C27 1.335(7) . ? N1 Cd2 2.308(4) 1_556 ? N2 C21 1.327(7) . ? N2 C17 1.332(7) . ? O1 C7 1.250(5) . ? O1 Cd2 2.467(3) 3 ? O2 C7 1.267(5) . ? O2 Cd2 2.376(3) 3 ? O3 C8 1.243(6) . ? O4 C8 1.272(6) . ? O5 C15 1.248(5) . ? O5 Cd1 2.509(3) 2_674 ? O6 C15 1.251(5) . ? O6 Cd1 2.331(3) 2_674 ? O7 C16 1.245(6) . ? O8 C16 1.252(6) . ? O9 C23 1.370(6) . ? O9 H9 0.8200 . ? O10 C22 1.384(6) . ? O10 H10A 0.8200 . ? C1 C6 1.390(7) . ? C1 C2 1.399(6) . ? C1 C8 1.493(7) . ? C2 C3 1.402(6) . ? C2 C7 1.505(6) . ? C3 C4 1.386(7) . ? C4 C5 1.374(8) . ? C4 H4 0.9300 . ? C5 C6 1.384(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C9 C14 1.388(6) . ? C9 C10 1.409(7) . ? C10 C11 1.359(7) . ? C10 H10 0.9300 . ? C11 C12 1.387(7) . ? C11 H11 0.9300 . ? C12 C13 1.379(7) . ? C12 H12 0.9300 . ? C13 C14 1.399(6) . ? C13 C16 1.495(7) . ? C14 C15 1.510(6) . ? C15 Cd1 2.760(4) 2_674 ? C17 C18 1.361(7) . ? C17 H17 0.9300 . ? C18 C19 1.379(7) . ? C18 H18 0.9300 . ? C19 C20 1.393(8) . ? C19 C22 1.514(7) . ? C20 C21 1.369(8) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.545(7) . ? C22 H22 0.9800 . ? C23 C24 1.522(7) . ? C23 H23 0.9800 . ? C24 C25 1.380(8) . ? C24 C28 1.392(7) . ? C25 C26 1.364(8) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.379(7) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? O1W H1WA 0.8499 . ? O1W H1WB 0.8364 . ? O2W H2WB 0.8501 . ? O2W H2WA 0.8500 . ? O3W H3WA 0.7503 . ? O3W H3WB 0.8624 . ? O4W H4WC 0.8500 . ? O4W H4WA 0.7500 . ? O5W H5WA 0.8464 . ? O5W H5WB 0.7499 . ? O6W H6WA 0.8501 . ? O6W H6WB 0.8500 . ? O7W H7WA 0.8625 . ? O7W H7WB 0.7500 . ? 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 N2 96.36(14) . . ? O4 Cd1 O6 169.96(12) . 2_675 ? N2 Cd1 O6 89.98(13) . 2_675 ? O4 Cd1 O2W 92.48(13) . . ? N2 Cd1 O2W 169.43(14) . . ? O6 Cd1 O2W 82.09(12) 2_675 . ? O4 Cd1 O1W 89.31(14) . . ? N2 Cd1 O1W 93.66(15) . . ? O6 Cd1 O1W 82.49(13) 2_675 . ? O2W Cd1 O1W 92.21(14) . . ? O4 Cd1 O3 54.24(12) . . ? N2 Cd1 O3 87.78(13) . . ? O6 Cd1 O3 134.11(11) 2_675 . ? O2W Cd1 O3 92.73(12) . . ? O1W Cd1 O3 143.39(12) . . ? O4 Cd1 O5 133.69(12) . 2_675 ? N2 Cd1 O5 90.88(13) . 2_675 ? O6 Cd1 O5 53.64(10) 2_675 2_675 ? O2W Cd1 O5 78.81(12) . 2_675 ? O1W Cd1 O5 135.91(12) . 2_675 ? O3 Cd1 O5 80.56(11) . 2_675 ? O4 Cd1 C15 159.89(13) . 2_675 ? N2 Cd1 C15 90.41(14) . 2_675 ? O6 Cd1 C15 26.78(12) 2_675 2_675 ? O2W Cd1 C15 79.35(12) . 2_675 ? O1W Cd1 C15 109.19(13) . 2_675 ? O3 Cd1 C15 107.38(12) . 2_675 ? O5 Cd1 C15 26.86(12) 2_675 2_675 ? N1 Cd2 O8 102.45(16) 1_554 . ? N1 Cd2 O3W 92.14(15) 1_554 . ? O8 Cd2 O3W 132.30(15) . . ? N1 Cd2 O2 85.49(13) 1_554 3_544 ? O8 Cd2 O2 140.19(12) . 3_544 ? O3W Cd2 O2 85.42(13) . 3_544 ? N1 Cd2 O4W 162.90(16) 1_554 . ? O8 Cd2 O4W 92.47(17) . . ? O3W Cd2 O4W 83.74(14) . . ? O2 Cd2 O4W 77.66(15) 3_544 . ? N1 Cd2 O7 88.94(14) 1_554 . ? O8 Cd2 O7 54.40(13) . . ? O3W Cd2 O7 81.21(14) . . ? O2 Cd2 O7 165.31(11) 3_544 . ? O4W Cd2 O7 106.73(17) . . ? N1 Cd2 O1 89.29(13) 1_554 3_544 ? O8 Cd2 O1 86.85(12) . 3_544 ? O3W Cd2 O1 139.11(13) . 3_544 ? O2 Cd2 O1 53.94(10) 3_544 3_544 ? O4W Cd2 O1 83.16(13) . 3_544 ? O7 Cd2 O1 139.69(11) . 3_544 ? N1 Cd2 H3WB 91.4 1_554 . ? O8 Cd2 H3WB 113.0 . . ? O3W Cd2 H3WB 20.3 . . ? O2 Cd2 H3WB 105.6 3_544 . ? O4W Cd2 H3WB 90.4 . . ? O7 Cd2 H3WB 60.9 . . ? O1 Cd2 H3WB 159.4 3_544 . ? C9 S1 C3 101.3(2) . . ? C26 N1 C27 115.9(5) . . ? C26 N1 Cd2 122.8(4) . 1_556 ? C27 N1 Cd2 120.6(3) . 1_556 ? C21 N2 C17 116.7(5) . . ? C21 N2 Cd1 124.9(4) . . ? C17 N2 Cd1 117.0(3) . . ? C7 O1 Cd2 90.2(3) . 3 ? C7 O2 Cd2 94.0(3) . 3 ? C8 O3 Cd1 87.9(3) . . ? C8 O4 Cd1 95.9(3) . . ? C15 O5 Cd1 87.8(3) . 2_674 ? C15 O6 Cd1 96.1(3) . 2_674 ? C16 O7 Cd2 90.1(3) . . ? C16 O8 Cd2 94.3(3) . . ? C23 O9 H9 109.5 . . ? C22 O10 H10A 109.5 . . ? C6 C1 C2 119.7(4) . . ? C6 C1 C8 119.3(4) . . ? C2 C1 C8 121.0(4) . . ? C1 C2 C3 119.2(4) . . ? C1 C2 C7 123.5(4) . . ? C3 C2 C7 117.4(4) . . ? C4 C3 C2 120.1(4) . . ? C4 C3 S1 120.2(4) . . ? C2 C3 S1 119.5(4) . . ? C5 C4 C3 120.3(5) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.3(5) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.4(5) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? O1 C7 O2 121.7(4) . . ? O1 C7 C2 120.4(4) . . ? O2 C7 C2 117.9(4) . . ? O3 C8 O4 121.9(4) . . ? O3 C8 C1 120.7(4) . . ? O4 C8 C1 117.4(4) . . ? C14 C9 C10 119.6(4) . . ? C14 C9 S1 120.0(3) . . ? C10 C9 S1 120.3(4) . . ? C11 C10 C9 120.4(4) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 119.5(5) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 C11 121.7(5) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C14 118.8(4) . . ? C12 C13 C16 119.8(4) . . ? C14 C13 C16 121.3(4) . . ? C9 C14 C13 119.9(4) . . ? C9 C14 C15 117.6(4) . . ? C13 C14 C15 122.5(4) . . ? O5 C15 O6 122.4(4) . . ? O5 C15 C14 119.3(4) . . ? O6 C15 C14 118.1(4) . . ? O5 C15 Cd1 65.3(2) . 2_674 ? O6 C15 Cd1 57.1(2) . 2_674 ? C14 C15 Cd1 173.6(3) . 2_674 ? O7 C16 O8 121.1(5) . . ? O7 C16 C13 120.2(5) . . ? O8 C16 C13 118.7(4) . . ? N2 C17 C18 123.2(5) . . ? N2 C17 H17 118.4 . . ? C18 C17 H17 118.4 . . ? C17 C18 C19 120.4(5) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C18 C19 C20 116.5(5) . . ? C18 C19 C22 121.5(5) . . ? C20 C19 C22 121.9(5) . . ? C21 C20 C19 119.1(5) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? N2 C21 C20 123.9(5) . . ? N2 C21 H21 118.0 . . ? C20 C21 H21 118.0 . . ? O10 C22 C19 112.6(4) . . ? O10 C22 C23 107.6(4) . . ? C19 C22 C23 110.6(4) . . ? O10 C22 H22 108.6 . . ? C19 C22 H22 108.6 . . ? C23 C22 H22 108.6 . . ? O9 C23 C24 113.4(5) . . ? O9 C23 C22 108.9(4) . . ? C24 C23 C22 109.0(4) . . ? O9 C23 H23 108.5 . . ? C24 C23 H23 108.5 . . ? C22 C23 H23 108.5 . . ? C25 C24 C28 115.8(5) . . ? C25 C24 C23 122.6(5) . . ? C28 C24 C23 121.7(5) . . ? C26 C25 C24 121.0(5) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? N1 C26 C25 123.6(5) . . ? N1 C26 H26 118.2 . . ? C25 C26 H26 118.2 . . ? N1 C27 C28 124.0(5) . . ? N1 C27 H27 118.0 . . ? C28 C27 H27 118.0 . . ? C27 C28 C24 119.5(5) . . ? C27 C28 H28 120.2 . . ? C24 C28 H28 120.2 . . ? Cd1 O1W H1WA 109.2 . . ? Cd1 O1W H1WB 160.9 . . ? H1WA O1W H1WB 89.7 . . ? Cd1 O2W H2WB 121.1 . . ? Cd1 O2W H2WA 121.9 . . ? H2WB O2W H2WA 88.6 . . ? Cd2 O3W H3WA 108.7 . . ? Cd2 O3W H3WB 50.4 . . ? H3WA O3W H3WB 133.9 . . ? Cd2 O4W H4WC 102.9 . . ? Cd2 O4W H4WA 135.1 . . ? H4WC O4W H4WA 103.5 . . ? H5WA O5W H5WB 120.3 . . ? H6WA O6W H6WB 120.5 . . ? H7WA O7W H7WB 91.9 . . ? 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 O4 Cd1 N2 C21 113.4(5) . . . . ? O6 Cd1 N2 C21 -58.8(5) 2_675 . . . ? O2W Cd1 N2 C21 -99.9(8) . . . . ? O1W Cd1 N2 C21 23.7(5) . . . . ? O3 Cd1 N2 C21 167.1(5) . . . . ? O5 Cd1 N2 C21 -112.4(5) 2_675 . . . ? C15 Cd1 N2 C21 -85.5(5) 2_675 . . . ? O4 Cd1 N2 C17 -80.3(4) . . . . ? O6 Cd1 N2 C17 107.5(4) 2_675 . . . ? O2W Cd1 N2 C17 66.4(9) . . . . ? O1W Cd1 N2 C17 -170.0(4) . . . . ? O3 Cd1 N2 C17 -26.6(4) . . . . ? O5 Cd1 N2 C17 53.9(4) 2_675 . . . ? C15 Cd1 N2 C17 80.7(4) 2_675 . . . ? O4 Cd1 O3 C8 0.8(3) . . . . ? N2 Cd1 O3 C8 -98.7(3) . . . . ? O6 Cd1 O3 C8 173.5(3) 2_675 . . . ? O2W Cd1 O3 C8 91.9(3) . . . . ? O1W Cd1 O3 C8 -5.5(4) . . . . ? O5 Cd1 O3 C8 170.1(3) 2_675 . . . ? C15 Cd1 O3 C8 171.6(3) 2_675 . . . ? N2 Cd1 O4 C8 81.9(3) . . . . ? O6 Cd1 O4 C8 -149.3(7) 2_675 . . . ? O2W Cd1 O4 C8 -92.4(3) . . . . ? O1W Cd1 O4 C8 175.5(3) . . . . ? O3 Cd1 O4 C8 -0.8(3) . . . . ? O5 Cd1 O4 C8 -15.5(4) 2_675 . . . ? C15 Cd1 O4 C8 -27.1(5) 2_675 . . . ? N1 Cd2 O7 C16 -108.1(3) 1_554 . . . ? O8 Cd2 O7 C16 -1.9(3) . . . . ? O3W Cd2 O7 C16 159.6(3) . . . . ? O2 Cd2 O7 C16 -175.7(4) 3_544 . . . ? O4W Cd2 O7 C16 78.9(3) . . . . ? O1 Cd2 O7 C16 -20.4(4) 3_544 . . . ? N1 Cd2 O8 C16 81.5(4) 1_554 . . . ? O3W Cd2 O8 C16 -23.2(4) . . . . ? O2 Cd2 O8 C16 179.4(3) 3_544 . . . ? O4W Cd2 O8 C16 -107.0(4) . . . . ? O7 Cd2 O8 C16 1.9(3) . . . . ? O1 Cd2 O8 C16 170.0(4) 3_544 . . . ? C6 C1 C2 C3 0.0(7) . . . . ? C8 C1 C2 C3 179.6(4) . . . . ? C6 C1 C2 C7 178.7(5) . . . . ? C8 C1 C2 C7 -1.7(7) . . . . ? C1 C2 C3 C4 -0.9(7) . . . . ? C7 C2 C3 C4 -179.7(5) . . . . ? C1 C2 C3 S1 -176.6(4) . . . . ? C7 C2 C3 S1 4.7(6) . . . . ? C9 S1 C3 C4 57.8(5) . . . . ? C9 S1 C3 C2 -126.5(4) . . . . ? C2 C3 C4 C5 1.5(8) . . . . ? S1 C3 C4 C5 177.1(5) . . . . ? C3 C4 C5 C6 -1.1(9) . . . . ? C4 C5 C6 C1 0.1(9) . . . . ? C2 C1 C6 C5 0.4(8) . . . . ? C8 C1 C6 C5 -179.2(5) . . . . ? Cd2 O1 C7 O2 4.1(4) 3 . . . ? Cd2 O1 C7 C2 -172.8(3) 3 . . . ? Cd2 O2 C7 O1 -4.3(4) 3 . . . ? Cd2 O2 C7 C2 172.7(3) 3 . . . ? C1 C2 C7 O1 -80.6(6) . . . . ? C3 C2 C7 O1 98.1(5) . . . . ? C1 C2 C7 O2 102.4(5) . . . . ? C3 C2 C7 O2 -78.9(5) . . . . ? Cd1 O3 C8 O4 -1.4(5) . . . . ? Cd1 O3 C8 C1 179.5(4) . . . . ? Cd1 O4 C8 O3 1.5(5) . . . . ? Cd1 O4 C8 C1 -179.4(4) . . . . ? C6 C1 C8 O3 154.2(5) . . . . ? C2 C1 C8 O3 -25.4(7) . . . . ? C6 C1 C8 O4 -24.9(7) . . . . ? C2 C1 C8 O4 155.5(5) . . . . ? C3 S1 C9 C14 -118.2(4) . . . . ? C3 S1 C9 C10 65.4(4) . . . . ? C14 C9 C10 C11 1.8(8) . . . . ? S1 C9 C10 C11 178.2(4) . . . . ? C9 C10 C11 C12 0.2(8) . . . . ? C10 C11 C12 C13 -1.8(9) . . . . ? C11 C12 C13 C14 1.4(8) . . . . ? C11 C12 C13 C16 -177.1(5) . . . . ? C10 C9 C14 C13 -2.2(7) . . . . ? S1 C9 C14 C13 -178.6(4) . . . . ? C10 C9 C14 C15 179.9(4) . . . . ? S1 C9 C14 C15 3.5(6) . . . . ? C12 C13 C14 C9 0.6(7) . . . . ? C16 C13 C14 C9 179.1(4) . . . . ? C12 C13 C14 C15 178.4(5) . . . . ? C16 C13 C14 C15 -3.0(7) . . . . ? Cd1 O5 C15 O6 0.3(4) 2_674 . . . ? Cd1 O5 C15 C14 -175.0(4) 2_674 . . . ? Cd1 O6 C15 O5 -0.3(5) 2_674 . . . ? Cd1 O6 C15 C14 175.0(3) 2_674 . . . ? C9 C14 C15 O5 99.1(5) . . . . ? C13 C14 C15 O5 -78.8(6) . . . . ? C9 C14 C15 O6 -76.3(5) . . . . ? C13 C14 C15 O6 105.8(5) . . . . ? Cd2 O7 C16 O8 3.4(6) . . . . ? Cd2 O7 C16 C13 -175.8(4) . . . . ? Cd2 O8 C16 O7 -3.5(6) . . . . ? Cd2 O8 C16 C13 175.6(4) . . . . ? C12 C13 C16 O7 153.5(5) . . . . ? C14 C13 C16 O7 -25.0(8) . . . . ? C12 C13 C16 O8 -25.7(8) . . . . ? C14 C13 C16 O8 155.8(5) . . . . ? C21 N2 C17 C18 -1.4(9) . . . . ? Cd1 N2 C17 C18 -168.8(4) . . . . ? N2 C17 C18 C19 0.7(9) . . . . ? C17 C18 C19 C20 -0.3(8) . . . . ? C17 C18 C19 C22 178.7(5) . . . . ? C18 C19 C20 C21 0.6(8) . . . . ? C22 C19 C20 C21 -178.3(5) . . . . ? C17 N2 C21 C20 1.8(9) . . . . ? Cd1 N2 C21 C20 168.1(5) . . . . ? C19 C20 C21 N2 -1.5(10) . . . . ? C18 C19 C22 O10 -155.2(5) . . . . ? C20 C19 C22 O10 23.7(7) . . . . ? C18 C19 C22 C23 84.4(6) . . . . ? C20 C19 C22 C23 -96.8(6) . . . . ? O10 C22 C23 O9 -175.9(5) . . . . ? C19 C22 C23 O9 -52.6(6) . . . . ? O10 C22 C23 C24 59.9(6) . . . . ? C19 C22 C23 C24 -176.7(4) . . . . ? O9 C23 C24 C25 -33.8(7) . . . . ? C22 C23 C24 C25 87.6(6) . . . . ? O9 C23 C24 C28 147.4(5) . . . . ? C22 C23 C24 C28 -91.2(6) . . . . ? C28 C24 C25 C26 3.4(8) . . . . ? C23 C24 C25 C26 -175.5(5) . . . . ? C27 N1 C26 C25 -2.2(8) . . . . ? Cd2 N1 C26 C25 -172.6(4) 1_556 . . . ? C24 C25 C26 N1 -0.7(9) . . . . ? C26 N1 C27 C28 2.3(8) . . . . ? Cd2 N1 C27 C28 172.9(4) 1_556 . . . ? N1 C27 C28 C24 0.5(8) . . . . ? C25 C24 C28 C27 -3.2(7) . . . . ? C23 C24 C28 C27 175.7(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O10 H10A O2 0.82 1.84 2.652(5) 173.5 2_675 O9 H9 O6 0.82 1.80 2.619(5) 177.0 3_545 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.855 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.065 # Attachment '5.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 857058' #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H110 N8 O61 S4 Zn8' _chemical_formula_weight 3099.20 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 ? _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2969(5) _cell_length_b 15.1541(7) _cell_length_c 21.5699(10) _cell_angle_alpha 77.950(4) _cell_angle_beta 89.748(4) _cell_angle_gamma 86.294(4) _cell_volume 2965.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7529 _cell_measurement_theta_min 2.8912 _cell_measurement_theta_max 29.2219 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1582 _exptl_absorpt_coefficient_mu 1.767 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.87128 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details SADABS(2009) _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 ? _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 22353 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10401 _reflns_number_gt 7672 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+3.6982P] 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 10401 _refine_ls_number_parameters 836 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1170 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.954 _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 Zn1 Zn 0.30404(5) 0.38064(3) -0.51679(2) 0.02389(13) Uani 1 1 d . . . Zn2 Zn 0.29743(6) 0.21812(4) -0.06600(2) 0.03447(15) Uani 1 1 d . . . Zn3 Zn 0.75410(6) 0.22049(5) 0.05506(3) 0.0513(2) Uani 1 1 d U . . Zn4 Zn 1.30785(5) -0.12092(3) 0.49231(2) 0.02369(13) Uani 1 1 d . . . N1 N 0.8992(4) 0.1907(3) 0.12737(17) 0.0386(10) Uani 1 1 d . . . N2 N 1.2625(4) -0.0164(2) 0.41052(15) 0.0280(9) Uani 1 1 d . . . N3 N 0.1560(4) 0.2796(3) -0.13599(16) 0.0315(9) Uani 1 1 d . . . N4 N -0.2511(4) 0.5148(2) -0.40255(15) 0.0280(9) Uani 1 1 d . . . O1 O 0.3386(4) 0.3435(2) -0.35953(13) 0.0403(9) Uani 1 1 d . . . O2 O 0.3462(3) 0.27045(18) -0.43907(12) 0.0237(6) Uani 1 1 d . . . O3 O 0.1166(3) 0.0951(2) -0.43334(14) 0.0361(8) Uani 1 1 d . . . O4 O 0.0441(3) 0.2151(2) -0.39515(13) 0.0313(7) Uani 1 1 d . . . O5 O 0.5190(4) 0.3023(2) -0.12774(15) 0.0435(7) Uani 1 1 d . . . O6 O 0.4642(3) 0.1596(2) -0.10354(14) 0.0429(8) Uani 1 1 d U . . O7 O 0.7099(4) 0.1908(2) -0.02529(15) 0.0493(10) Uani 1 1 d . . . O8 O 0.9290(4) 0.1262(3) -0.01740(15) 0.0588(11) Uani 1 1 d . . . O9 O 1.1182(3) -0.4097(2) 0.57360(14) 0.0360(8) Uani 1 1 d . . . O10 O 1.0428(3) -0.2880(2) 0.60964(14) 0.0328(7) Uani 1 1 d . . . O11 O 1.3466(3) -0.22974(18) 0.57033(12) 0.0229(6) Uani 1 1 d . . . O12 O 1.3094(4) -0.15351(19) 0.64802(13) 0.0384(8) Uani 1 1 d . . . O13 O 1.5177(4) -0.1423(3) 0.86726(17) 0.0603(12) Uani 1 1 d . . . O14 O 1.4175(4) -0.2720(3) 0.90759(16) 0.0543(10) Uani 1 1 d . . . O15 O 1.6777(4) -0.2522(3) 0.98559(15) 0.0520(10) Uani 1 1 d . . . O16 O 1.8853(6) -0.3347(4) 0.9980(3) 0.0634(15) Uani 0.658(6) 1 d PDU A 1 O16' O 1.7601(13) -0.3828(6) 1.0174(4) 0.0634(15) Uani 0.342(6) 1 d PD A 2 O1W O 0.0918(3) 0.36749(19) -0.49039(13) 0.0287(7) Uani 1 1 d . . . H1WA H 0.0845 0.3187 -0.4660 0.043 Uiso 1 1 d R . . H1WB H 0.0326 0.3805 -0.5222 0.043 Uiso 1 1 d R . . O2W O 0.3274(3) 0.47608(18) -0.45642(12) 0.0261(7) Uani 1 1 d . . . H2WB H 0.3328 0.4371 -0.4199 0.039 Uiso 1 1 d R . . H2WA H 0.2510 0.5060 -0.4556 0.039 Uiso 1 1 d R . . O3W O 0.5191(3) 0.3738(2) -0.53464(15) 0.0420(8) Uani 1 1 d . . . H3WA H 0.5661 0.3406 -0.5475 0.063 Uiso 1 1 d R . . H3WB H 0.5502 0.4237 -0.5367 0.063 Uiso 1 1 d R . . O4W O 0.2679(4) 0.2826(2) -0.57775(15) 0.0461(9) Uani 1 1 d . . . H4WA H 0.2953 0.2298 -0.5577 0.069 Uiso 1 1 d R . . H4WB H 0.1893 0.2833 -0.5873 0.069 Uiso 1 1 d R . . O5W O 0.2111(4) 0.0954(2) -0.03446(16) 0.0537(10) Uani 1 1 d . . . H5WB H 0.2470 0.0721 -0.0038 0.081 Uiso 1 1 d R . . H5WA H 0.1316 0.1025 -0.0296 0.081 Uiso 1 1 d R . . O6W O 0.7292(7) 0.0641(4) 0.0985(3) 0.0441(17) Uani 0.50 1 d P . . H6WB H 0.6528 0.0555 0.0997 0.066 Uiso 0.50 1 d PR . . H6WA H 0.7704 0.0362 0.0784 0.066 Uiso 0.50 1 d PR . . O7W O 0.8272(4) 0.3457(3) 0.01607(17) 0.0610(9) Uani 1 1 d U . . H7WB H 0.9117 0.3577 0.0056 0.092 Uiso 1 1 d R . . H7WA H 0.7942 0.3634 -0.0199 0.092 Uiso 1 1 d R . . O8W O 1.0940(3) -0.1365(2) 0.51613(13) 0.0309(7) Uani 1 1 d . . . H8WB H 1.0311 -0.1174 0.4860 0.046 Uiso 1 1 d R . . H8WA H 1.0870 -0.1842 0.5418 0.046 Uiso 1 1 d R . . O9W O 1.3267(3) -0.02448(18) 0.55013(12) 0.0262(7) Uani 1 1 d . . . H9WA H 1.2570 0.0068 0.5516 0.039 Uiso 1 1 d R . . H9WB H 1.3361 -0.0507 0.5873 0.039 Uiso 1 1 d R . . O10W O 1.2726(4) -0.2214(2) 0.43102(15) 0.0478(9) Uani 1 1 d . . . O11W O 1.5260(3) -0.1282(2) 0.47824(14) 0.0371(8) Uani 1 1 d . . . H11A H 1.5587 -0.0833 0.4714 0.056 Uiso 1 1 d R . . H11B H 1.5470 -0.1691 0.4650 0.056 Uiso 1 1 d R . . O12W O 0.3759(5) 0.0226(3) 0.0651(2) 0.0866(15) Uani 1 1 d . . . H12A H 0.4375 0.0311 0.0835 0.130 Uiso 1 1 d R . . H12B H 0.3958 -0.0243 0.0501 0.130 Uiso 1 1 d R . . O13W O 0.5441(5) 0.4643(3) 0.0609(2) 0.0877(15) Uani 1 1 d . . . H13A H 0.5406 0.4197 0.0921 0.132 Uiso 1 1 d R . . H13B H 0.6188 0.4892 0.0694 0.132 Uiso 1 1 d R . . O14W O 0.8222(11) 0.4888(7) 0.0780(5) 0.272(5) Uani 1 1 d . . . H14A H 0.8311 0.5441 0.0788 0.407 Uiso 1 1 d R . . H14B H 0.8689 0.4758 0.0525 0.407 Uiso 1 1 d R . . O15W O 0.6848(4) 0.4261(3) 0.90765(18) 0.0667(12) Uani 1 1 d . . . H15A H 0.6534 0.3896 0.8943 0.100 Uiso 1 1 d R . . H15B H 0.6178 0.4466 0.9199 0.100 Uiso 1 1 d R . . S1 S 0.54693(14) 0.25045(8) -0.27029(5) 0.0377(3) Uani 1 1 d . . . S2 S 1.51568(14) -0.23827(8) 0.74204(5) 0.0354(3) Uani 1 1 d . . . C1 C 0.3383(4) 0.1851(3) -0.33466(17) 0.0223(9) Uani 1 1 d . . . C2 C 0.2423(4) 0.1221(3) -0.34417(18) 0.0224(9) Uani 1 1 d . . . C3 C 0.2478(5) 0.0368(3) -0.30409(19) 0.0280(10) Uani 1 1 d . . . H3 H 0.1869 -0.0065 -0.3111 0.034 Uiso 1 1 calc R . . C4 C 0.3451(5) 0.0172(3) -0.25345(19) 0.0306(11) Uani 1 1 d . . . H4 H 0.3485 -0.0396 -0.2267 0.037 Uiso 1 1 calc R . . C5 C 0.4359(5) 0.0798(3) -0.24233(18) 0.0272(10) Uani 1 1 d . . . H5 H 0.4984 0.0658 -0.2076 0.033 Uiso 1 1 calc R . . C6 C 0.4351(4) 0.1644(3) -0.28274(18) 0.0249(10) Uani 1 1 d . . . C7 C 0.6875(5) 0.1894(3) -0.2195(2) 0.0318(11) Uani 1 1 d . . . C8 C 0.8055(5) 0.1528(3) -0.2463(2) 0.0406(12) Uani 1 1 d . . . H8 H 0.8065 0.1552 -0.2898 0.049 Uiso 1 1 calc R . . C9 C 0.9228(5) 0.1124(4) -0.2093(2) 0.0467(14) Uani 1 1 d . . . H9 H 1.0008 0.0856 -0.2273 0.056 Uiso 1 1 calc R . . C10 C 0.9221(5) 0.1127(3) -0.1459(2) 0.0408(12) Uani 1 1 d . . . H10 H 1.0019 0.0870 -0.1212 0.049 Uiso 1 1 calc R . . C11 C 0.8063(5) 0.1499(3) -0.1175(2) 0.0305(10) Uani 1 1 d . . . C12 C 0.6855(5) 0.1877(3) -0.15452(19) 0.0278(9) Uani 1 1 d U . . C13 C 0.3414(4) 0.2740(3) -0.38095(18) 0.0220(9) Uani 1 1 d . . . C14 C 0.1259(4) 0.1462(3) -0.39465(18) 0.0238(9) Uani 1 1 d . . . C15 C 0.5483(6) 0.2212(4) -0.1256(2) 0.0435(7) Uani 1 1 d U . . C16 C 0.8175(5) 0.1546(3) -0.0487(2) 0.0360(11) Uani 1 1 d . . . C17 C 0.8628(5) 0.2149(3) 0.1820(2) 0.0404(13) Uani 1 1 d . . . H17 H 0.7800 0.2525 0.1827 0.049 Uiso 1 1 calc R . . C18 C 1.0221(6) 0.1422(4) 0.1270(2) 0.0501(15) Uani 1 1 d . . . H18 H 1.0516 0.1268 0.0891 0.060 Uiso 1 1 calc R . . C19 C 0.9426(5) 0.1865(3) 0.2371(2) 0.0395(13) Uani 1 1 d . . . H19 H 0.9123 0.2043 0.2740 0.047 Uiso 1 1 calc R . . C20 C 1.1092(5) 0.1129(3) 0.1800(2) 0.0431(14) Uani 1 1 d . . . H20 H 1.1964 0.0805 0.1767 0.052 Uiso 1 1 calc R . . C21 C 1.0677(5) 0.1314(3) 0.23752(19) 0.0284(10) Uani 1 1 d . . . C22 C 1.1438(5) 0.0891(3) 0.29744(19) 0.0260(10) Uani 1 1 d . . . C23 C 1.2760(5) 0.0416(3) 0.2993(2) 0.0366(12) Uani 1 1 d . . . H23 H 1.3283 0.0443 0.2621 0.044 Uiso 1 1 calc R . . C24 C 1.0787(5) 0.0878(3) 0.35554(19) 0.0313(11) Uani 1 1 d . . . H24 H 0.9937 0.1227 0.3579 0.038 Uiso 1 1 calc R . . C25 C 1.1402(5) 0.0346(3) 0.4098(2) 0.0336(11) Uani 1 1 d . . . H25 H 1.0937 0.0345 0.4481 0.040 Uiso 1 1 calc R . . C26 C 1.3311(5) -0.0097(3) 0.3551(2) 0.0364(12) Uani 1 1 d . . . H26 H 1.4201 -0.0412 0.3545 0.044 Uiso 1 1 calc R . . C27 C 1.3252(4) -0.3125(3) 0.67496(17) 0.0217(9) Uani 1 1 d . . . C28 C 1.2395(4) -0.3797(3) 0.66392(18) 0.0257(10) Uani 1 1 d . . . C29 C 1.2493(5) -0.4649(3) 0.7038(2) 0.0361(11) Uani 1 1 d . . . H29 H 1.1940 -0.5103 0.6958 0.043 Uiso 1 1 calc R . . C30 C 1.3422(5) -0.4814(3) 0.7555(2) 0.0421(13) Uani 1 1 d . . . H30 H 1.3497 -0.5385 0.7819 0.051 Uiso 1 1 calc R . . C31 C 1.4230(5) -0.4153(3) 0.7682(2) 0.0351(11) Uani 1 1 d . . . H31 H 1.4829 -0.4274 0.8037 0.042 Uiso 1 1 calc R . . C32 C 1.4169(4) -0.3296(3) 0.72848(18) 0.0239(9) Uani 1 1 d . . . C33 C 1.6498(5) -0.2932(3) 0.7977(2) 0.0300(10) Uani 1 1 d . . . C34 C 1.7660(5) -0.3419(4) 0.7774(3) 0.0461(11) Uani 1 1 d U . . H34 H 1.7714 -0.3470 0.7352 0.055 Uiso 1 1 calc R . . C35 C 1.8736(6) -0.3826(4) 0.8197(3) 0.0490(11) Uani 1 1 d U . . H35 H 1.9505 -0.4162 0.8064 0.059 Uiso 1 1 calc R . . C36 C 1.8663(6) -0.3732(4) 0.8815(3) 0.0527(15) Uani 1 1 d U . . H36 H 1.9376 -0.4019 0.9102 0.063 Uiso 1 1 calc R . . C37 C 1.7555(5) -0.3219(3) 0.9022(2) 0.0420(13) Uani 1 1 d . A . C38 C 1.6438(5) -0.2811(3) 0.8600(2) 0.0302(10) Uani 1 1 d . . . C39 C 1.1249(4) -0.3574(3) 0.61165(19) 0.0258(10) Uani 1 1 d . . . C40 C 1.3265(4) -0.2249(3) 0.62819(18) 0.0224(9) Uani 1 1 d . . . C41 C 1.5171(5) -0.2257(4) 0.8805(2) 0.0383(12) Uani 1 1 d . . . C42 C 1.7559(6) -0.3093(4) 0.9693(3) 0.067(2) Uani 1 1 d D . . C43 C 0.1833(5) 0.2674(4) -0.1942(2) 0.0456(14) Uani 1 1 d . . . H43 H 0.2657 0.2323 -0.2006 0.055 Uiso 1 1 calc R . . C44 C 0.0369(5) 0.3294(4) -0.1292(2) 0.0447(14) Uani 1 1 d . . . H44 H 0.0140 0.3378 -0.0887 0.054 Uiso 1 1 calc R . . C45 C 0.0959(5) 0.3041(4) -0.2453(2) 0.0452(14) Uani 1 1 d . . . H45 H 0.1187 0.2919 -0.2848 0.054 Uiso 1 1 calc R . . C46 C -0.0551(5) 0.3693(3) -0.1782(2) 0.0425(14) Uani 1 1 d . . . H46 H -0.1373 0.4034 -0.1704 0.051 Uiso 1 1 calc R . . C47 C -0.0254(5) 0.3589(3) -0.23900(18) 0.0256(10) Uani 1 1 d . . . C48 C -0.1129(5) 0.4063(3) -0.29473(18) 0.0258(10) Uani 1 1 d . . . C49 C -0.0660(5) 0.4053(3) -0.35574(19) 0.0350(12) Uani 1 1 d . . . H49 H 0.0138 0.3679 -0.3619 0.042 Uiso 1 1 calc R . . C50 C -0.2390(5) 0.4604(3) -0.2907(2) 0.0414(13) Uani 1 1 d . . . H50 H -0.2800 0.4610 -0.2513 0.050 Uiso 1 1 calc R . . C51 C -0.3026(5) 0.5124(3) -0.3445(2) 0.0389(13) Uani 1 1 d . . . H51 H -0.3860 0.5479 -0.3403 0.047 Uiso 1 1 calc R . . C52 C -0.1366(5) 0.4589(3) -0.4070(2) 0.0358(12) Uani 1 1 d . . . H52 H -0.1026 0.4561 -0.4473 0.043 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 Zn1 0.0240(3) 0.0248(3) 0.0219(3) -0.00394(19) -0.00144(19) 0.0027(2) Zn2 0.0319(3) 0.0486(4) 0.0226(3) -0.0078(2) -0.0082(2) 0.0017(3) Zn3 0.0363(4) 0.0945(5) 0.0279(3) -0.0243(3) -0.0092(2) -0.0021(3) Zn4 0.0235(3) 0.0259(3) 0.0211(3) -0.00453(19) -0.00026(19) 0.0015(2) N1 0.040(2) 0.047(3) 0.029(2) -0.0107(18) -0.0033(18) 0.007(2) N2 0.028(2) 0.031(2) 0.0240(19) -0.0043(15) -0.0006(15) 0.0049(17) N3 0.031(2) 0.041(2) 0.0227(19) -0.0075(16) -0.0049(16) -0.0016(18) N4 0.030(2) 0.030(2) 0.0229(19) -0.0057(15) -0.0027(15) 0.0075(17) O1 0.078(3) 0.0230(17) 0.0209(16) -0.0059(13) -0.0068(16) -0.0038(17) O2 0.0288(16) 0.0238(16) 0.0172(15) -0.0027(11) -0.0019(12) 0.0024(13) O3 0.0388(19) 0.0373(19) 0.0361(18) -0.0204(15) -0.0179(14) 0.0114(15) O4 0.0310(18) 0.0292(17) 0.0346(17) -0.0106(13) -0.0051(13) 0.0056(15) O5 0.0408(16) 0.0453(16) 0.0447(16) -0.0129(14) -0.0129(12) 0.0072(13) O6 0.0331(19) 0.063(2) 0.0337(18) -0.0118(16) -0.0019(14) -0.0013(15) O7 0.048(2) 0.069(3) 0.0348(19) -0.0252(17) -0.0168(16) 0.020(2) O8 0.038(2) 0.104(3) 0.0312(19) -0.0114(19) -0.0156(16) 0.013(2) O9 0.0345(19) 0.0367(19) 0.0404(19) -0.0194(15) -0.0166(14) 0.0093(15) O10 0.0260(17) 0.0331(18) 0.0399(18) -0.0110(14) -0.0043(13) 0.0045(15) O11 0.0282(16) 0.0235(15) 0.0168(14) -0.0039(11) 0.0011(12) -0.0010(13) O12 0.071(2) 0.0215(17) 0.0224(16) -0.0053(13) -0.0022(15) 0.0021(16) O13 0.074(3) 0.055(3) 0.053(2) -0.0228(19) -0.014(2) 0.027(2) O14 0.028(2) 0.097(3) 0.043(2) -0.029(2) -0.0006(16) -0.002(2) O15 0.046(2) 0.084(3) 0.0292(18) -0.0254(18) -0.0107(15) 0.016(2) O16 0.061(2) 0.072(2) 0.057(2) -0.0139(17) -0.0060(17) 0.0001(17) O16' 0.061(2) 0.072(2) 0.057(2) -0.0139(17) -0.0060(17) 0.0001(17) O1W 0.0245(16) 0.0325(17) 0.0264(16) -0.0009(12) -0.0047(12) 0.0011(13) O2W 0.0291(16) 0.0219(15) 0.0255(15) -0.0019(12) -0.0014(12) 0.0018(13) O3W 0.0308(19) 0.0283(18) 0.070(2) -0.0170(16) 0.0158(16) -0.0034(15) O4W 0.055(2) 0.040(2) 0.046(2) -0.0172(16) -0.0045(17) -0.0017(18) O5W 0.039(2) 0.068(3) 0.050(2) -0.0002(18) -0.0026(17) -0.0103(19) O6W 0.051(4) 0.045(4) 0.039(4) -0.013(3) 0.004(3) -0.007(3) O7W 0.038(2) 0.083(2) 0.063(2) -0.020(2) -0.0082(18) 0.0023(18) O8W 0.0225(16) 0.0379(18) 0.0286(16) 0.0011(13) -0.0073(12) 0.0004(14) O9W 0.0303(17) 0.0240(16) 0.0240(15) -0.0062(12) -0.0010(12) 0.0036(13) O10W 0.064(2) 0.045(2) 0.0389(19) -0.0194(16) 0.0028(17) -0.0056(18) O11W 0.0296(18) 0.0264(17) 0.058(2) -0.0129(15) 0.0137(15) -0.0050(14) O12W 0.097(4) 0.049(3) 0.107(4) -0.002(2) -0.050(3) -0.003(3) O13W 0.087(4) 0.091(4) 0.079(3) -0.011(3) 0.009(3) 0.012(3) O14W 0.247(12) 0.236(11) 0.326(14) -0.054(10) -0.025(11) 0.005(10) O15W 0.061(3) 0.070(3) 0.072(3) -0.023(2) 0.003(2) -0.005(2) S1 0.0469(8) 0.0332(7) 0.0312(6) 0.0007(5) -0.0164(5) -0.0129(6) S2 0.0473(8) 0.0332(7) 0.0267(6) -0.0059(5) -0.0130(5) -0.0094(6) C1 0.025(2) 0.024(2) 0.017(2) -0.0032(16) -0.0011(17) 0.0023(19) C2 0.024(2) 0.024(2) 0.019(2) -0.0059(17) 0.0033(17) -0.0029(19) C3 0.031(3) 0.025(2) 0.030(2) -0.0090(18) -0.0003(19) -0.003(2) C4 0.034(3) 0.028(2) 0.026(2) 0.0027(18) 0.0011(19) 0.000(2) C5 0.029(2) 0.033(3) 0.018(2) -0.0033(18) -0.0012(17) 0.002(2) C6 0.027(2) 0.032(2) 0.017(2) -0.0075(17) 0.0017(17) -0.003(2) C7 0.034(3) 0.034(3) 0.029(2) -0.0065(19) -0.004(2) -0.012(2) C8 0.042(3) 0.060(3) 0.024(2) -0.016(2) 0.001(2) -0.015(3) C9 0.033(3) 0.064(4) 0.048(3) -0.025(3) 0.004(2) -0.001(3) C10 0.034(3) 0.050(3) 0.040(3) -0.013(2) -0.009(2) 0.000(2) C11 0.030(3) 0.036(3) 0.028(2) -0.0094(19) -0.0072(19) -0.003(2) C12 0.033(2) 0.027(2) 0.023(2) -0.0029(17) -0.0074(17) -0.0071(19) C13 0.020(2) 0.022(2) 0.022(2) -0.0011(17) -0.0049(17) -0.0025(18) C14 0.021(2) 0.026(2) 0.024(2) -0.0042(18) 0.0022(17) 0.0003(19) C15 0.0408(16) 0.0453(16) 0.0447(16) -0.0129(14) -0.0129(12) 0.0072(13) C16 0.034(3) 0.043(3) 0.032(3) -0.008(2) -0.008(2) -0.006(2) C17 0.036(3) 0.053(3) 0.031(3) -0.012(2) -0.004(2) 0.016(2) C18 0.058(4) 0.068(4) 0.023(3) -0.013(2) 0.002(2) 0.021(3) C19 0.040(3) 0.054(3) 0.024(2) -0.011(2) 0.000(2) 0.010(3) C20 0.039(3) 0.061(3) 0.027(3) -0.009(2) 0.002(2) 0.022(3) C21 0.028(2) 0.031(3) 0.023(2) 0.0003(18) -0.0002(18) 0.002(2) C22 0.027(2) 0.027(2) 0.024(2) -0.0050(18) 0.0016(18) -0.0017(19) C23 0.032(3) 0.053(3) 0.023(2) -0.005(2) 0.0059(19) 0.008(2) C24 0.031(3) 0.036(3) 0.025(2) -0.0071(19) 0.0014(19) 0.009(2) C25 0.042(3) 0.037(3) 0.021(2) -0.0055(19) 0.0007(19) 0.006(2) C26 0.027(3) 0.049(3) 0.031(3) -0.009(2) 0.001(2) 0.013(2) C27 0.028(2) 0.022(2) 0.016(2) -0.0070(16) 0.0015(17) -0.0005(19) C28 0.027(2) 0.028(2) 0.022(2) -0.0057(18) 0.0004(17) -0.001(2) C29 0.041(3) 0.029(3) 0.037(3) 0.001(2) -0.010(2) -0.012(2) C30 0.051(3) 0.031(3) 0.038(3) 0.011(2) -0.010(2) -0.011(2) C31 0.038(3) 0.041(3) 0.023(2) 0.002(2) -0.0087(19) -0.006(2) C32 0.028(2) 0.027(2) 0.017(2) -0.0062(17) 0.0001(17) -0.0028(19) C33 0.031(3) 0.031(3) 0.031(2) -0.0118(19) -0.0067(19) -0.005(2) C34 0.037(2) 0.052(3) 0.058(2) -0.033(2) -0.0006(19) -0.001(2) C35 0.038(2) 0.052(3) 0.065(2) -0.032(2) -0.0001(19) 0.002(2) C36 0.045(3) 0.053(3) 0.065(3) -0.028(3) -0.027(3) 0.013(3) C37 0.042(3) 0.050(3) 0.038(3) -0.021(2) -0.017(2) 0.010(3) C38 0.030(3) 0.034(3) 0.030(2) -0.0118(19) -0.0062(19) -0.004(2) C39 0.025(2) 0.029(2) 0.023(2) -0.0016(18) 0.0014(18) -0.004(2) C40 0.019(2) 0.022(2) 0.025(2) -0.0031(17) -0.0068(17) 0.0004(18) C41 0.034(3) 0.062(4) 0.021(2) -0.018(2) -0.011(2) 0.007(3) C42 0.088(5) 0.072(4) 0.043(3) -0.029(3) -0.042(3) 0.036(4) C43 0.036(3) 0.071(4) 0.028(3) -0.012(2) -0.003(2) 0.021(3) C44 0.051(3) 0.064(4) 0.018(2) -0.012(2) -0.004(2) 0.017(3) C45 0.043(3) 0.071(4) 0.019(2) -0.013(2) -0.002(2) 0.021(3) C46 0.044(3) 0.055(3) 0.026(3) -0.010(2) -0.001(2) 0.023(3) C47 0.028(2) 0.027(2) 0.021(2) -0.0013(17) 0.0005(17) -0.0003(19) C48 0.031(2) 0.025(2) 0.022(2) -0.0048(17) -0.0002(18) -0.0025(19) C49 0.042(3) 0.035(3) 0.024(2) -0.0034(19) 0.002(2) 0.017(2) C50 0.039(3) 0.060(3) 0.022(2) -0.006(2) 0.002(2) 0.014(3) C51 0.035(3) 0.051(3) 0.027(2) -0.005(2) 0.004(2) 0.018(2) C52 0.046(3) 0.039(3) 0.021(2) -0.0060(19) 0.003(2) 0.011(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3W 2.035(3) . ? Zn1 O1W 2.062(3) . ? Zn1 O2 2.122(3) . ? Zn1 N4 2.129(3) 2_564 ? Zn1 O2W 2.160(3) . ? Zn1 O4W 2.221(3) . ? Zn2 O15 1.929(3) 2_756 ? Zn2 O6 1.989(3) . ? Zn2 N3 2.037(3) . ? Zn2 O5W 2.055(4) . ? Zn3 O7 1.932(3) . ? Zn3 O14 1.973(3) 2_756 ? Zn3 N1 2.025(4) . ? Zn3 O7W 2.066(4) . ? Zn3 O6W 2.386(6) . ? Zn4 O11W 2.049(3) . ? Zn4 O8W 2.067(3) . ? Zn4 O11 2.110(2) . ? Zn4 O9W 2.126(3) . ? Zn4 N2 2.133(3) . ? Zn4 O10W 2.255(3) . ? N1 C18 1.320(6) . ? N1 C17 1.340(6) . ? N2 C25 1.332(5) . ? N2 C26 1.341(5) . ? N3 C44 1.324(5) . ? N3 C43 1.328(5) . ? N4 C51 1.332(5) . ? N4 C52 1.334(5) . ? N4 Zn1 2.129(3) 2_564 ? O1 C13 1.234(5) . ? O2 C13 1.267(4) . ? O3 C14 1.259(5) . ? O4 C14 1.249(4) . ? O5 C15 1.233(6) . ? O6 C15 1.270(6) . ? O7 C16 1.264(5) . ? O8 C16 1.242(5) . ? O9 C39 1.260(5) . ? O10 C39 1.252(5) . ? O11 C40 1.278(5) . ? O12 C40 1.244(5) . ? O13 C41 1.238(6) . ? O14 C41 1.264(6) . ? O14 Zn3 1.973(3) 2_756 ? O15 C42 1.202(6) . ? O15 Zn2 1.929(3) 2_756 ? O16 C42 1.352(6) . ? O16' C42 1.354(6) . ? S1 C6 1.783(5) . ? S1 C7 1.788(4) . ? S2 C33 1.775(4) . ? S2 C32 1.783(5) . ? C1 C2 1.395(6) . ? C1 C6 1.410(5) . ? C1 C13 1.503(5) . ? C2 C3 1.394(6) . ? C2 C14 1.511(5) . ? C3 C4 1.393(6) . ? C4 C5 1.368(6) . ? C5 C6 1.391(6) . ? C7 C8 1.378(6) . ? C7 C12 1.397(6) . ? C8 C9 1.385(6) . ? C9 C10 1.369(6) . ? C10 C11 1.384(6) . ? C11 C12 1.401(6) . ? C11 C16 1.504(6) . ? C12 C15 1.521(7) . ? C17 C19 1.379(6) . ? C18 C20 1.382(6) . ? C19 C21 1.385(6) . ? C20 C21 1.377(6) . ? C21 C22 1.478(5) . ? C22 C23 1.380(6) . ? C22 C24 1.386(6) . ? C23 C26 1.371(6) . ? C24 C25 1.378(6) . ? C27 C28 1.391(6) . ? C27 C32 1.408(5) . ? C27 C40 1.492(5) . ? C28 C29 1.392(6) . ? C28 C39 1.525(6) . ? C29 C30 1.383(6) . ? C30 C31 1.362(7) . ? C31 C32 1.396(6) . ? C33 C34 1.389(6) . ? C33 C38 1.394(6) . ? C34 C35 1.381(7) . ? C35 C36 1.372(7) . ? C36 C37 1.378(7) . ? C37 C38 1.407(6) . ? C37 C42 1.499(7) . ? C38 C41 1.520(6) . ? C43 C45 1.370(6) . ? C44 C46 1.375(6) . ? C45 C47 1.380(6) . ? C46 C47 1.377(6) . ? C47 C48 1.481(5) . ? C48 C49 1.387(6) . ? C48 C50 1.400(6) . ? C49 C52 1.370(6) . ? C50 C51 1.372(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3W Zn1 O1W 171.09(12) . . ? O3W Zn1 O2 87.28(12) . . ? O1W Zn1 O2 84.24(10) . . ? O3W Zn1 N4 94.94(13) . 2_564 ? O1W Zn1 N4 93.36(12) . 2_564 ? O2 Zn1 N4 175.76(13) . 2_564 ? O3W Zn1 O2W 92.15(12) . . ? O1W Zn1 O2W 90.70(11) . . ? O2 Zn1 O2W 90.97(10) . . ? N4 Zn1 O2W 92.55(12) 2_564 . ? O3W Zn1 O4W 90.83(13) . . ? O1W Zn1 O4W 86.33(12) . . ? O2 Zn1 O4W 89.07(11) . . ? N4 Zn1 O4W 87.30(13) 2_564 . ? O2W Zn1 O4W 177.01(12) . . ? O15 Zn2 O6 119.04(14) 2_756 . ? O15 Zn2 N3 125.98(14) 2_756 . ? O6 Zn2 N3 109.57(13) . . ? O15 Zn2 O5W 99.08(16) 2_756 . ? O6 Zn2 O5W 91.28(15) . . ? N3 Zn2 O5W 102.07(15) . . ? O7 Zn3 O14 111.78(14) . 2_756 ? O7 Zn3 N1 141.89(14) . . ? O14 Zn3 N1 103.90(14) 2_756 . ? O7 Zn3 O7W 95.15(16) . . ? O14 Zn3 O7W 93.54(16) 2_756 . ? N1 Zn3 O7W 95.60(16) . . ? O7 Zn3 O6W 85.31(19) . . ? O14 Zn3 O6W 99.1(2) 2_756 . ? N1 Zn3 O6W 76.1(2) . . ? O7W Zn3 O6W 166.19(19) . . ? O11W Zn4 O8W 169.84(11) . . ? O11W Zn4 O11 86.50(11) . . ? O8W Zn4 O11 83.82(11) . . ? O11W Zn4 O9W 91.37(12) . . ? O8W Zn4 O9W 92.05(11) . . ? O11 Zn4 O9W 91.86(10) . . ? O11W Zn4 N2 94.71(13) . . ? O8W Zn4 N2 94.77(12) . . ? O11 Zn4 N2 176.48(13) . . ? O9W Zn4 N2 91.42(12) . . ? O11W Zn4 O10W 92.21(13) . . ? O8W Zn4 O10W 84.52(13) . . ? O11 Zn4 O10W 89.00(11) . . ? O9W Zn4 O10W 176.36(12) . . ? N2 Zn4 O10W 87.66(13) . . ? C18 N1 C17 116.8(4) . . ? C18 N1 Zn3 124.9(3) . . ? C17 N1 Zn3 117.9(3) . . ? C25 N2 C26 116.3(3) . . ? C25 N2 Zn4 117.5(3) . . ? C26 N2 Zn4 124.7(3) . . ? C44 N3 C43 116.2(4) . . ? C44 N3 Zn2 126.5(3) . . ? C43 N3 Zn2 117.3(3) . . ? C51 N4 C52 116.4(3) . . ? C51 N4 Zn1 124.8(3) . 2_564 ? C52 N4 Zn1 117.1(3) . 2_564 ? C13 O2 Zn1 126.1(2) . . ? C15 O6 Zn2 107.1(3) . . ? C16 O7 Zn3 112.5(3) . . ? C40 O11 Zn4 124.6(2) . . ? C41 O14 Zn3 124.0(4) . 2_756 ? C42 O15 Zn2 121.9(3) . 2_756 ? C6 S1 C7 103.5(2) . . ? C33 S2 C32 102.9(2) . . ? C2 C1 C6 120.1(4) . . ? C2 C1 C13 119.8(3) . . ? C6 C1 C13 120.1(4) . . ? C3 C2 C1 119.6(4) . . ? C3 C2 C14 119.0(4) . . ? C1 C2 C14 121.2(3) . . ? C4 C3 C2 119.4(4) . . ? C5 C4 C3 121.3(4) . . ? C4 C5 C6 120.2(4) . . ? C5 C6 C1 119.2(4) . . ? C5 C6 S1 122.9(3) . . ? C1 C6 S1 117.9(3) . . ? C8 C7 C12 120.3(4) . . ? C8 C7 S1 118.8(3) . . ? C12 C7 S1 120.4(3) . . ? C7 C8 C9 120.7(4) . . ? C10 C9 C8 118.9(5) . . ? C9 C10 C11 122.0(4) . . ? C10 C11 C12 119.1(4) . . ? C10 C11 C16 119.2(4) . . ? C12 C11 C16 121.7(4) . . ? C7 C12 C11 119.0(4) . . ? C7 C12 C15 118.8(4) . . ? C11 C12 C15 122.1(4) . . ? O1 C13 O2 125.9(4) . . ? O1 C13 C1 117.9(4) . . ? O2 C13 C1 116.3(4) . . ? O4 C14 O3 124.0(4) . . ? O4 C14 C2 118.2(4) . . ? O3 C14 C2 117.8(3) . . ? O5 C15 O6 123.7(5) . . ? O5 C15 C12 121.7(5) . . ? O6 C15 C12 114.4(4) . . ? O8 C16 O7 122.2(4) . . ? O8 C16 C11 121.1(4) . . ? O7 C16 C11 116.7(4) . . ? N1 C17 C19 123.0(4) . . ? N1 C18 C20 123.3(4) . . ? C17 C19 C21 120.1(4) . . ? C21 C20 C18 120.4(4) . . ? C20 C21 C19 116.1(4) . . ? C20 C21 C22 122.4(4) . . ? C19 C21 C22 121.3(4) . . ? C23 C22 C24 115.9(4) . . ? C23 C22 C21 122.8(4) . . ? C24 C22 C21 121.0(4) . . ? C26 C23 C22 120.8(4) . . ? C25 C24 C22 120.0(4) . . ? N2 C25 C24 123.6(4) . . ? N2 C26 C23 123.0(4) . . ? C28 C27 C32 119.7(4) . . ? C28 C27 C40 120.0(3) . . ? C32 C27 C40 120.1(4) . . ? C27 C28 C29 120.2(4) . . ? C27 C28 C39 119.8(4) . . ? C29 C28 C39 119.8(4) . . ? C30 C29 C28 119.4(4) . . ? C31 C30 C29 121.0(4) . . ? C30 C31 C32 120.9(4) . . ? C31 C32 C27 118.7(4) . . ? C31 C32 S2 124.1(3) . . ? C27 C32 S2 117.2(3) . . ? C34 C33 C38 120.6(4) . . ? C34 C33 S2 119.5(4) . . ? C38 C33 S2 119.8(3) . . ? C35 C34 C33 120.2(5) . . ? C36 C35 C34 119.5(5) . . ? C35 C36 C37 121.4(5) . . ? C36 C37 C38 119.8(4) . . ? C36 C37 C42 119.6(4) . . ? C38 C37 C42 120.5(4) . . ? C33 C38 C37 118.4(4) . . ? C33 C38 C41 119.5(4) . . ? C37 C38 C41 122.1(4) . . ? O10 C39 O9 124.2(4) . . ? O10 C39 C28 117.5(4) . . ? O9 C39 C28 118.2(3) . . ? O12 C40 O11 125.2(4) . . ? O12 C40 C27 118.4(4) . . ? O11 C40 C27 116.4(3) . . ? O13 C41 O14 126.8(5) . . ? O13 C41 C38 118.6(5) . . ? O14 C41 C38 114.5(5) . . ? O15 C42 O16 120.3(5) . . ? O15 C42 O16' 106.8(7) . . ? O16 C42 O16' 63.8(6) . . ? O15 C42 C37 121.2(4) . . ? O16 C42 C37 112.0(5) . . ? O16' C42 C37 119.4(7) . . ? N3 C43 C45 123.0(4) . . ? N3 C44 C46 124.0(4) . . ? C43 C45 C47 121.1(4) . . ? C44 C46 C47 120.1(4) . . ? C46 C47 C45 115.5(4) . . ? C46 C47 C48 122.8(4) . . ? C45 C47 C48 121.7(4) . . ? C49 C48 C50 115.4(4) . . ? C49 C48 C47 120.6(4) . . ? C50 C48 C47 123.8(4) . . ? C52 C49 C48 120.5(4) . . ? C51 C50 C48 120.2(4) . . ? N4 C51 C50 123.5(4) . . ? N4 C52 C49 123.7(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.771 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.082