# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef '- revised cif.cif' _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Shan Gao' _publ_contact_author_address ; Key Laboratory of Functional Inorganic Material Chemistry, Ministry of Education, Heilongjiang University, Harbin 150080 CHINA ; _publ_contact_author_email shangao67@yahoo.com _publ_section_title ; Syntheses, crystal structures and luminescent properties of Zn(II)/Cd(II) supramolecular complexes incorporating rare 4-sulfinobenzoate and its in situ oxidized ligand ; loop_ _publ_author_name 'Huang Wang' 'Li-Hua Huo' 'Zhao-Peng Deng' 'Hui Zhao' 'Shan Gao' data_complex1 #TrackingRef '- revised cif.cif' _database_code_depnum_ccdc_archive 'CCDC 855412' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H14 O10 S2 Zn, 2(H2 O)' _chemical_formula_sum 'C14 H18 O12 S2 Zn' _chemical_formula_weight 507.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.4378(11) _cell_length_b 7.0974(14) _cell_length_c 12.031(2) _cell_angle_alpha 90.52(3) _cell_angle_beta 95.20(3) _cell_angle_gamma 102.28(3) _cell_volume 451.65(16) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3770 _cell_measurement_theta_min 3.35 _cell_measurement_theta_max 27.44 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.867 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 260 _exptl_absorpt_coefficient_mu 1.658 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7546 _exptl_absorpt_correction_T_max 0.8387 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4412 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2034 _reflns_number_gt 1718 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0361P)^2^+0.8507P] 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 2034 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0862 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 1.0000 0.5000 0.01878(13) Uani 1 2 d S . . S1 S 0.50781(11) 0.94564(9) 0.64083(5) 0.01789(15) Uani 1 1 d . . . O1W O 0.0916(4) 1.2521(3) 0.60390(16) 0.0323(5) Uani 1 1 d . . . H1W1 H 0.1627 1.2487 0.6695 0.048 Uiso 1 1 d R . . H1W2 H -0.0273 1.3121 0.6071 0.048 Uiso 1 1 d R . . O4 O 0.2458(4) 0.8553(3) 0.58765(16) 0.0248(4) Uani 1 1 d . . . O2 O 0.2880(4) 0.6082(3) 1.15364(17) 0.0346(5) Uani 1 1 d . . . H2B H 0.3051 0.5915 1.2210 0.052 Uiso 1 1 calc R . . O1 O 0.6969(4) 0.7473(3) 1.18232(17) 0.0340(5) Uani 1 1 d . . . O3 O 0.7004(4) 0.8483(3) 0.59169(16) 0.0259(4) Uani 1 1 d . . . O2W O 0.3032(5) 0.5392(3) 1.37296(18) 0.0363(5) Uani 1 1 d . . . H2W1 H 0.3040 0.4216 1.3854 0.055 Uiso 1 1 d R . . H2W2 H 0.3964 0.6086 1.4250 0.055 Uiso 1 1 d R . . C1 C 0.5008(5) 0.8477(4) 0.7785(2) 0.0186(5) Uani 1 1 d . . . C4 C 0.4966(5) 0.7393(4) 0.9989(2) 0.0205(5) Uani 1 1 d . . . C5 C 0.2778(5) 0.6899(4) 0.9264(2) 0.0247(6) Uani 1 1 d . . . H5A H 0.1298 0.6203 0.9520 0.030 Uiso 1 1 calc R . . C6 C 0.2791(5) 0.7443(4) 0.8155(2) 0.0244(6) Uani 1 1 d . . . H6A H 0.1328 0.7116 0.7669 0.029 Uiso 1 1 calc R . . C7 C 0.5048(5) 0.6980(4) 1.1206(2) 0.0237(6) Uani 1 1 d . . . C3 C 0.7177(5) 0.8378(4) 0.9597(2) 0.0264(6) Uani 1 1 d . . . H3A H 0.8655 0.8662 1.0078 0.032 Uiso 1 1 calc R . . C2 C 0.7225(5) 0.8947(4) 0.8501(2) 0.0250(6) Uani 1 1 d . . . H2A H 0.8712 0.9633 0.8246 0.030 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 0.0164(2) 0.0251(2) 0.0153(2) 0.00366(15) 0.00064(15) 0.00566(17) S1 0.0173(3) 0.0214(3) 0.0162(3) 0.0059(2) 0.0024(2) 0.0063(2) O1W 0.0421(12) 0.0360(11) 0.0198(10) -0.0058(8) -0.0049(9) 0.0142(10) O4 0.0204(9) 0.0309(10) 0.0228(10) 0.0080(8) -0.0028(7) 0.0065(8) O2 0.0368(12) 0.0440(13) 0.0202(10) 0.0091(9) 0.0057(8) 0.0005(10) O1 0.0368(12) 0.0432(12) 0.0194(10) 0.0028(9) -0.0035(9) 0.0051(10) O3 0.0260(10) 0.0301(10) 0.0266(10) 0.0107(8) 0.0114(8) 0.0134(8) O2W 0.0513(14) 0.0286(11) 0.0283(11) 0.0060(8) 0.0005(10) 0.0077(10) C1 0.0197(12) 0.0213(12) 0.0160(11) 0.0027(9) 0.0031(9) 0.0066(10) C4 0.0237(13) 0.0215(12) 0.0164(12) 0.0017(9) 0.0022(10) 0.0047(10) C5 0.0217(13) 0.0287(14) 0.0220(13) 0.0059(10) 0.0033(10) 0.0009(11) C6 0.0187(12) 0.0311(14) 0.0214(13) 0.0048(10) -0.0010(10) 0.0020(11) C7 0.0309(14) 0.0218(12) 0.0187(13) 0.0000(10) 0.0032(11) 0.0059(11) C3 0.0237(13) 0.0327(14) 0.0199(13) 0.0030(11) -0.0026(10) 0.0014(12) C2 0.0157(12) 0.0328(14) 0.0232(13) 0.0037(11) 0.0019(10) -0.0019(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 Zn1 O4 2.0740(19) 2_576 ? Zn1 O4 2.0740(19) . ? Zn1 O1W 2.116(2) . ? Zn1 O1W 2.116(2) 2_576 ? Zn1 O3 2.152(2) 1_455 ? Zn1 O3 2.152(2) 2_676 ? S1 O4 1.513(2) . ? S1 O3 1.528(2) . ? S1 C1 1.803(3) . ? O1W H1W1 0.8500 . ? O1W H1W2 0.8500 . ? O2 C7 1.313(4) . ? O2 H2B 0.8200 . ? O1 C7 1.210(3) . ? O3 Zn1 2.152(2) 1_655 ? O2W H2W1 0.8500 . ? O2W H2W2 0.8500 . ? C1 C6 1.385(4) . ? C1 C2 1.393(4) . ? C4 C3 1.381(4) . ? C4 C5 1.389(4) . ? C4 C7 1.495(4) . ? C5 C6 1.392(4) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C3 C2 1.385(4) . ? C3 H3A 0.9300 . ? C2 H2A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O4 180.000(1) 2_576 . ? O4 Zn1 O1W 84.02(8) 2_576 . ? O4 Zn1 O1W 95.98(8) . . ? O4 Zn1 O1W 95.98(8) 2_576 2_576 ? O4 Zn1 O1W 84.02(8) . 2_576 ? O1W Zn1 O1W 180.00(7) . 2_576 ? O4 Zn1 O3 91.08(8) 2_576 1_455 ? O4 Zn1 O3 88.92(8) . 1_455 ? O1W Zn1 O3 96.25(9) . 1_455 ? O1W Zn1 O3 83.75(9) 2_576 1_455 ? O4 Zn1 O3 88.92(8) 2_576 2_676 ? O4 Zn1 O3 91.08(8) . 2_676 ? O1W Zn1 O3 83.75(9) . 2_676 ? O1W Zn1 O3 96.25(9) 2_576 2_676 ? O3 Zn1 O3 180.00(10) 1_455 2_676 ? O4 S1 O3 109.21(12) . . ? O4 S1 C1 101.81(12) . . ? O3 S1 C1 101.36(11) . . ? Zn1 O1W H1W1 120.0 . . ? Zn1 O1W H1W2 114.8 . . ? H1W1 O1W H1W2 108.3 . . ? S1 O4 Zn1 125.80(12) . . ? C7 O2 H2B 109.5 . . ? S1 O3 Zn1 123.29(11) . 1_655 ? H2W1 O2W H2W2 108.4 . . ? C6 C1 C2 120.9(2) . . ? C6 C1 S1 121.5(2) . . ? C2 C1 S1 117.3(2) . . ? C3 C4 C5 119.7(2) . . ? C3 C4 C7 117.1(2) . . ? C5 C4 C7 123.1(2) . . ? C4 C5 C6 120.2(3) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C1 C6 C5 119.3(2) . . ? C1 C6 H6A 120.4 . . ? C5 C6 H6A 120.4 . . ? O1 C7 O2 123.9(3) . . ? O1 C7 C4 121.6(3) . . ? O2 C7 C4 114.5(2) . . ? C4 C3 C2 120.9(3) . . ? C4 C3 H3A 119.5 . . ? C2 C3 H3A 119.5 . . ? C3 C2 C1 118.9(3) . . ? C3 C2 H2A 120.6 . . ? C1 C2 H2A 120.6 . . ? 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 O3 S1 O4 Zn1 -121.63(14) . . . . ? C1 S1 O4 Zn1 131.75(14) . . . . ? O1W Zn1 O4 S1 -38.05(15) . . . . ? O1W Zn1 O4 S1 141.95(15) 2_576 . . . ? O3 Zn1 O4 S1 -134.23(15) 1_455 . . . ? O3 Zn1 O4 S1 45.77(15) 2_676 . . . ? O4 S1 O3 Zn1 118.28(14) . . . 1_655 ? C1 S1 O3 Zn1 -134.80(13) . . . 1_655 ? O4 S1 C1 C6 -8.8(2) . . . . ? O3 S1 C1 C6 -121.5(2) . . . . ? O4 S1 C1 C2 176.8(2) . . . . ? O3 S1 C1 C2 64.2(2) . . . . ? C3 C4 C5 C6 -1.9(4) . . . . ? C7 C4 C5 C6 175.5(3) . . . . ? C2 C1 C6 C5 1.1(4) . . . . ? S1 C1 C6 C5 -173.0(2) . . . . ? C4 C5 C6 C1 0.1(4) . . . . ? C3 C4 C7 O1 -0.6(4) . . . . ? C5 C4 C7 O1 -178.0(3) . . . . ? C3 C4 C7 O2 178.4(2) . . . . ? C5 C4 C7 O2 1.0(4) . . . . ? C5 C4 C3 C2 2.5(4) . . . . ? C7 C4 C3 C2 -175.1(3) . . . . ? C4 C3 C2 C1 -1.3(4) . . . . ? C6 C1 C2 C3 -0.6(4) . . . . ? S1 C1 C2 C3 173.9(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W1 O1 0.85 1.87 2.720(3) 175.7 2_677 O1W H1W2 O2W 0.85 2.04 2.887(3) 175.7 2_577 O2 H2B O2W 0.82 1.87 2.685(3) 173.1 . O2W H2W1 O3 0.85 1.93 2.783(3) 177.9 2_667 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.597 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.098 #===END data_complex2 #TrackingRef '- revised cif.cif' _database_code_depnum_ccdc_archive 'CCDC 855413' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H14 Cd O10 S2, 2(H2 O)' _chemical_formula_sum 'C14 H18 Cd O12 S2' _chemical_formula_weight 554.80 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.6965(11) _cell_length_b 7.1619(14) _cell_length_c 11.935(2) _cell_angle_alpha 93.51(3) _cell_angle_beta 92.42(3) _cell_angle_gamma 105.53(3) _cell_volume 467.41(16) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3214 _cell_measurement_theta_min 3.33 _cell_measurement_theta_max 25.01 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.971 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 278 _exptl_absorpt_coefficient_mu 1.456 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7400 _exptl_absorpt_correction_T_max 0.8221 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3689 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 25.01 _reflns_number_total 1646 _reflns_number_gt 1539 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.1260P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1646 _refine_ls_number_parameters 145 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1537 _refine_ls_wR_factor_gt 0.1518 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.089 _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 0.0000 0.5000 0.0000 0.0259(3) Uani 1 2 d S . . S1 S 0.4867(2) 0.43320(17) 0.14250(10) 0.0245(4) Uani 1 1 d . . . O1 O 0.7053(8) 0.2455(6) 0.6765(3) 0.0445(11) Uani 1 1 d . . . O1W O -0.0898(9) 0.2223(7) -0.1165(4) 0.0473(11) Uani 1 1 d D . . H1W1 H 0.013(12) 0.156(10) -0.114(6) 0.071 Uiso 1 1 d D . . H1W2 H -0.128(13) 0.238(11) -0.184(2) 0.071 Uiso 1 1 d D . . O2W O 0.3067(9) 0.0443(6) 0.8780(3) 0.0409(10) Uani 1 1 d D . . H2W1 H 0.314(14) -0.069(4) 0.891(6) 0.061 Uiso 1 1 d D . . H2W2 H 0.400(12) 0.129(7) 0.925(5) 0.061 Uiso 1 1 d D . . O2 O 0.3025(9) 0.1164(7) 0.6604(4) 0.0450(11) Uani 1 1 d . . . H2A H 0.3227 0.1005 0.7273 0.067 Uiso 1 1 calc R . . O3 O 0.2258(7) 0.3421(6) 0.0979(3) 0.0346(9) Uani 1 1 d . . . O4 O 0.6528(7) 0.3287(5) 0.0815(3) 0.0343(9) Uani 1 1 d . . . C1 C 0.5148(10) 0.2014(7) 0.6208(5) 0.0299(12) Uani 1 1 d . . . C2 C 0.4968(10) 0.2417(7) 0.5005(4) 0.0278(11) Uani 1 1 d . . . C3 C 0.7115(10) 0.3345(8) 0.4527(5) 0.0342(12) Uani 1 1 d . . . H3 H 0.8593 0.3610 0.4948 0.041 Uiso 1 1 calc R . . C4 C 0.7087(10) 0.3880(9) 0.3430(5) 0.0339(12) Uani 1 1 d . . . H4 H 0.8522 0.4534 0.3121 0.041 Uiso 1 1 calc R . . C5 C 0.4865(9) 0.3418(7) 0.2802(4) 0.0252(10) Uani 1 1 d . . . C6 C 0.2738(10) 0.2474(8) 0.3252(4) 0.0312(12) Uani 1 1 d . . . H6 H 0.1271 0.2177 0.2820 0.037 Uiso 1 1 calc R . . C7 C 0.2776(10) 0.1960(8) 0.4360(5) 0.0326(12) Uani 1 1 d . . . H7 H 0.1335 0.1312 0.4666 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0249(4) 0.0330(4) 0.0226(4) 0.0071(2) 0.0014(2) 0.0114(2) S1 0.0264(7) 0.0259(7) 0.0241(7) 0.0074(5) 0.0030(5) 0.0107(5) O1 0.051(3) 0.054(3) 0.029(2) 0.0064(18) -0.0104(19) 0.014(2) O1W 0.058(3) 0.054(3) 0.035(2) -0.0091(19) -0.010(2) 0.029(2) O2W 0.055(3) 0.035(2) 0.034(2) 0.0088(17) -0.0037(19) 0.0148(19) O2 0.052(3) 0.051(2) 0.029(2) 0.0132(18) 0.0033(19) 0.008(2) O3 0.030(2) 0.042(2) 0.033(2) 0.0116(17) -0.0042(16) 0.0111(16) O4 0.043(2) 0.0343(19) 0.032(2) 0.0083(16) 0.0121(17) 0.0201(17) C1 0.042(3) 0.023(2) 0.027(3) 0.006(2) 0.004(2) 0.012(2) C2 0.040(3) 0.022(2) 0.023(3) 0.0016(19) -0.001(2) 0.010(2) C3 0.028(3) 0.041(3) 0.033(3) 0.008(2) -0.004(2) 0.009(2) C4 0.029(3) 0.043(3) 0.029(3) 0.006(2) 0.000(2) 0.009(2) C5 0.031(3) 0.026(2) 0.021(2) 0.0034(19) 0.002(2) 0.012(2) C6 0.023(3) 0.041(3) 0.027(3) 0.007(2) -0.002(2) 0.004(2) C7 0.027(3) 0.036(3) 0.034(3) 0.011(2) 0.005(2) 0.004(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 Cd1 O3 2.261(4) 2_565 ? Cd1 O3 2.261(4) . ? Cd1 O1W 2.282(5) 2_565 ? Cd1 O1W 2.282(5) . ? Cd1 O4 2.318(4) 2_665 ? Cd1 O4 2.318(4) 1_455 ? S1 O3 1.513(4) . ? S1 O4 1.535(4) . ? S1 C5 1.806(5) . ? O1 C1 1.204(7) . ? O1W H1W1 0.85(2) . ? O1W H1W2 0.85(2) . ? O2W H2W1 0.85(2) . ? O2W H2W2 0.85(2) . ? O2 C1 1.321(7) . ? O2 H2A 0.8200 . ? O4 Cd1 2.318(4) 1_655 ? C1 C2 1.486(7) . ? C2 C7 1.389(8) . ? C2 C3 1.391(8) . ? C3 C4 1.386(8) . ? C3 H3 0.9300 . ? C4 C5 1.393(8) . ? C4 H4 0.9300 . ? C5 C6 1.369(7) . ? C6 C7 1.395(8) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cd1 O3 180.00(15) 2_565 . ? O3 Cd1 O1W 82.84(16) 2_565 2_565 ? O3 Cd1 O1W 97.16(16) . 2_565 ? O3 Cd1 O1W 97.16(16) 2_565 . ? O3 Cd1 O1W 82.84(16) . . ? O1W Cd1 O1W 180.00(19) 2_565 . ? O3 Cd1 O4 89.96(14) 2_565 2_665 ? O3 Cd1 O4 90.04(14) . 2_665 ? O1W Cd1 O4 81.34(16) 2_565 2_665 ? O1W Cd1 O4 98.66(16) . 2_665 ? O3 Cd1 O4 90.04(14) 2_565 1_455 ? O3 Cd1 O4 89.96(14) . 1_455 ? O1W Cd1 O4 98.66(16) 2_565 1_455 ? O1W Cd1 O4 81.34(16) . 1_455 ? O4 Cd1 O4 180.00(17) 2_665 1_455 ? O3 S1 O4 108.6(2) . . ? O3 S1 C5 101.8(2) . . ? O4 S1 C5 101.7(2) . . ? Cd1 O1W H1W1 116(6) . . ? Cd1 O1W H1W2 114(5) . . ? H1W1 O1W H1W2 111(7) . . ? H2W1 O2W H2W2 111(6) . . ? C1 O2 H2A 109.5 . . ? S1 O3 Cd1 123.9(2) . . ? S1 O4 Cd1 121.5(2) . 1_655 ? O1 C1 O2 123.7(5) . . ? O1 C1 C2 122.7(5) . . ? O2 C1 C2 113.6(5) . . ? C7 C2 C3 119.4(5) . . ? C7 C2 C1 123.3(5) . . ? C3 C2 C1 117.4(5) . . ? C4 C3 C2 121.0(5) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 118.6(5) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C6 C5 C4 121.2(5) . . ? C6 C5 S1 121.4(4) . . ? C4 C5 S1 117.1(4) . . ? C5 C6 C7 119.9(5) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C2 C7 C6 119.9(5) . . ? C2 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? 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 S1 O3 Cd1 -114.6(3) . . . . ? C5 S1 O3 Cd1 138.6(3) . . . . ? O1W Cd1 O3 S1 -47.0(3) 2_565 . . . ? O1W Cd1 O3 S1 133.0(3) . . . . ? O4 Cd1 O3 S1 34.3(3) 2_665 . . . ? O4 Cd1 O3 S1 -145.7(3) 1_455 . . . ? O3 S1 O4 Cd1 129.9(2) . . . 1_655 ? C5 S1 O4 Cd1 -123.2(2) . . . 1_655 ? O1 C1 C2 C7 -178.4(5) . . . . ? O2 C1 C2 C7 0.5(8) . . . . ? O1 C1 C2 C3 -0.1(8) . . . . ? O2 C1 C2 C3 178.8(5) . . . . ? C7 C2 C3 C4 2.3(8) . . . . ? C1 C2 C3 C4 -176.0(5) . . . . ? C2 C3 C4 C5 -1.9(9) . . . . ? C3 C4 C5 C6 0.7(9) . . . . ? C3 C4 C5 S1 174.6(5) . . . . ? O3 S1 C5 C6 -10.5(5) . . . . ? O4 S1 C5 C6 -122.6(5) . . . . ? O3 S1 C5 C4 175.7(4) . . . . ? O4 S1 C5 C4 63.6(5) . . . . ? C4 C5 C6 C7 0.0(9) . . . . ? S1 C5 C6 C7 -173.6(4) . . . . ? C3 C2 C7 C6 -1.5(8) . . . . ? C1 C2 C7 C6 176.7(5) . . . . ? C5 C6 C7 C2 0.4(9) . . . . ? 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 O1W H1W1 O2W 0.85(2) 2.04(2) 2.877(7) 169(8) 1_554 O1W H1W2 O1 0.85(2) 1.89(2) 2.721(6) 165(8) 1_454 O2W H2W1 O4 0.85(2) 1.97(2) 2.811(6) 177(8) 2_656 O2W H2W2 O4 0.85(2) 2.45(2) 3.283(6) 170(7) 1_556 O2 H2A O2W 0.82 1.87 2.678(6) 169.5 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.458 _refine_diff_density_min -0.731 _refine_diff_density_rms 0.245 #===END data_complex3 #TrackingRef '- revised cif.cif' _database_code_depnum_ccdc_archive 'CCDC 855414' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H32 Cd2 N4 O12 S2' _chemical_formula_sum 'C34 H32 Cd2 N4 O12 S2' _chemical_formula_weight 977.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7849(16) _cell_length_b 9.839(2) _cell_length_c 12.367(3) _cell_angle_alpha 76.16(3) _cell_angle_beta 84.00(3) _cell_angle_gamma 71.71(3) _cell_volume 872.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 7703 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 27.45 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.860 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 1.410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7562 _exptl_absorpt_correction_T_max 0.8380 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8612 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3939 _reflns_number_gt 3532 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0447P)^2^+0.7591P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3939 _refine_ls_number_parameters 256 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0807 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.061 _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 0.40725(3) 0.35753(2) 0.222024(16) 0.02869(8) Uani 1 1 d . . . S1 S 0.00493(10) 0.26329(8) 0.20145(6) 0.03069(16) Uani 1 1 d . . . O1W O 0.5719(3) 0.5380(3) 0.1757(2) 0.0405(5) Uani 1 1 d D . . H1W1 H 0.6834(19) 0.497(4) 0.164(3) 0.061 Uiso 1 1 d D . . H1W2 H 0.525(4) 0.601(4) 0.119(2) 0.061 Uiso 1 1 d D . . O2W O 0.2153(3) 0.5371(3) 0.09357(19) 0.0399(5) Uani 1 1 d D . . H2W1 H 0.255(5) 0.577(4) 0.0316(17) 0.060 Uiso 1 1 d D . . H2W2 H 0.128(4) 0.508(5) 0.084(3) 0.060 Uiso 1 1 d D . . O1 O 0.4260(4) -0.1194(3) -0.1921(2) 0.0503(6) Uani 1 1 d . . . O2 O 0.4338(3) -0.2983(3) -0.0473(2) 0.0469(6) Uani 1 1 d . . . O3 O 0.1642(3) 0.2595(2) 0.26327(17) 0.0347(5) Uani 1 1 d . . . O4 O -0.0653(3) 0.4122(2) 0.12560(19) 0.0381(5) Uani 1 1 d . . . N1 N 0.5192(4) 0.2568(3) 0.4037(2) 0.0359(6) Uani 1 1 d . . . N2 N 0.2424(3) 0.5075(3) 0.3498(2) 0.0315(5) Uani 1 1 d . . . C1 C 0.3890(4) -0.1643(4) -0.0920(3) 0.0351(7) Uani 1 1 d . . . C2 C 0.2901(4) -0.0545(3) -0.0232(2) 0.0295(6) Uani 1 1 d . . . C3 C 0.2125(5) -0.1005(3) 0.0797(3) 0.0369(7) Uani 1 1 d . . . H3 H 0.2217 -0.1993 0.1059 0.044 Uiso 1 1 calc R . . C4 C 0.1215(4) -0.0003(3) 0.1436(3) 0.0353(7) Uani 1 1 d . . . H4 H 0.0667 -0.0313 0.2115 0.042 Uiso 1 1 calc R . . C5 C 0.1124(4) 0.1451(3) 0.1065(2) 0.0278(6) Uani 1 1 d . . . C6 C 0.1867(4) 0.1943(3) 0.0031(3) 0.0322(6) Uani 1 1 d . . . H6 H 0.1773 0.2932 -0.0222 0.039 Uiso 1 1 calc R . . C7 C 0.2752(4) 0.0941(3) -0.0622(3) 0.0336(6) Uani 1 1 d . . . H7 H 0.3246 0.1261 -0.1318 0.040 Uiso 1 1 calc R . . C8 C 0.6455(5) 0.1266(4) 0.4286(3) 0.0484(8) Uani 1 1 d . . . H8 H 0.7072 0.0839 0.3708 0.058 Uiso 1 1 calc R . . C9 C 0.6883(6) 0.0527(5) 0.5373(3) 0.0568(10) Uani 1 1 d . . . H9 H 0.7778 -0.0373 0.5517 0.068 Uiso 1 1 calc R . . C10 C 0.5984(6) 0.1129(5) 0.6222(3) 0.0590(11) Uani 1 1 d . . . H10 H 0.6216 0.0631 0.6958 0.071 Uiso 1 1 calc R . . C11 C 0.4721(5) 0.2491(5) 0.5982(3) 0.0505(9) Uani 1 1 d . . . H11 H 0.4130 0.2940 0.6555 0.061 Uiso 1 1 calc R . . C12 C 0.4328(4) 0.3196(4) 0.4875(3) 0.0346(6) Uani 1 1 d . . . C13 C 0.2920(4) 0.4636(3) 0.4563(3) 0.0328(6) Uani 1 1 d . . . C14 C 0.2092(5) 0.5483(4) 0.5344(3) 0.0457(8) Uani 1 1 d . . . H14 H 0.2467 0.5183 0.6076 0.055 Uiso 1 1 calc R . . C15 C 0.0721(6) 0.6759(4) 0.5019(3) 0.0537(10) Uani 1 1 d . . . H15 H 0.0152 0.7328 0.5531 0.064 Uiso 1 1 calc R . . C16 C 0.0197(5) 0.7188(4) 0.3932(3) 0.0488(9) Uani 1 1 d . . . H16 H -0.0734 0.8046 0.3698 0.059 Uiso 1 1 calc R . . C17 C 0.1080(4) 0.6320(3) 0.3195(3) 0.0384(7) Uani 1 1 d . . . H17 H 0.0727 0.6611 0.2459 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03304(13) 0.02676(12) 0.02306(12) -0.00867(8) -0.00095(8) -0.00202(8) S1 0.0315(3) 0.0312(4) 0.0300(4) -0.0128(3) 0.0030(3) -0.0069(3) O1W 0.0342(11) 0.0395(13) 0.0454(13) -0.0136(10) 0.0040(10) -0.0059(10) O2W 0.0446(13) 0.0370(12) 0.0356(12) -0.0070(10) -0.0097(10) -0.0066(10) O1 0.0588(15) 0.0518(15) 0.0354(13) -0.0212(11) 0.0096(11) -0.0047(12) O2 0.0515(14) 0.0318(12) 0.0576(15) -0.0237(11) 0.0096(12) -0.0060(11) O3 0.0408(11) 0.0375(12) 0.0288(10) -0.0084(9) -0.0051(9) -0.0137(10) O4 0.0351(11) 0.0309(11) 0.0426(12) -0.0121(10) -0.0055(9) 0.0024(9) N1 0.0430(14) 0.0371(14) 0.0276(12) -0.0063(11) -0.0052(11) -0.0113(12) N2 0.0355(13) 0.0296(12) 0.0303(12) -0.0122(10) 0.0044(10) -0.0086(10) C1 0.0301(14) 0.0409(17) 0.0368(16) -0.0171(14) 0.0012(12) -0.0084(13) C2 0.0280(13) 0.0325(15) 0.0294(14) -0.0114(12) -0.0028(11) -0.0069(12) C3 0.0466(17) 0.0256(14) 0.0381(16) -0.0095(12) 0.0061(14) -0.0109(13) C4 0.0451(17) 0.0325(15) 0.0282(14) -0.0095(12) 0.0083(13) -0.0122(13) C5 0.0257(13) 0.0307(14) 0.0299(14) -0.0120(12) -0.0022(11) -0.0080(11) C6 0.0363(15) 0.0257(14) 0.0338(15) -0.0085(12) 0.0027(12) -0.0080(12) C7 0.0353(15) 0.0336(15) 0.0298(14) -0.0088(12) 0.0056(12) -0.0083(12) C8 0.053(2) 0.0421(19) 0.0441(19) -0.0054(16) -0.0149(16) -0.0045(16) C9 0.059(2) 0.053(2) 0.050(2) 0.0081(18) -0.0225(19) -0.0123(19) C10 0.058(2) 0.077(3) 0.0354(19) 0.0130(19) -0.0164(17) -0.024(2) C11 0.054(2) 0.070(3) 0.0275(16) -0.0063(17) -0.0014(15) -0.023(2) C12 0.0376(15) 0.0443(17) 0.0278(14) -0.0083(13) -0.0008(12) -0.0201(14) C13 0.0394(16) 0.0388(16) 0.0291(14) -0.0163(12) 0.0086(12) -0.0207(14) C14 0.060(2) 0.053(2) 0.0336(16) -0.0237(15) 0.0135(15) -0.0251(18) C15 0.066(2) 0.053(2) 0.050(2) -0.0312(18) 0.0278(19) -0.0231(19) C16 0.050(2) 0.0347(18) 0.059(2) -0.0157(16) 0.0197(18) -0.0121(15) C17 0.0423(17) 0.0348(16) 0.0372(16) -0.0102(13) 0.0093(14) -0.0116(14) _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 O2W 2.318(3) . ? Cd1 O3 2.341(2) . ? Cd1 N1 2.365(3) . ? Cd1 O1 2.390(3) 2_655 ? Cd1 N2 2.414(3) . ? Cd1 O1W 2.432(3) . ? Cd1 O2 2.476(3) 2_655 ? S1 O4 1.507(2) . ? S1 O3 1.509(2) . ? S1 C5 1.808(3) . ? O1W H1W1 0.85(3) . ? O1W H1W2 0.85(3) . ? O2W H2W1 0.85(3) . ? O2W H2W2 0.85(3) . ? O1 C1 1.247(4) . ? O1 Cd1 2.390(3) 2_655 ? O2 C1 1.252(4) . ? O2 Cd1 2.476(3) 2_655 ? N1 C8 1.337(5) . ? N1 C12 1.345(4) . ? N2 C17 1.340(4) . ? N2 C13 1.341(4) . ? C1 C2 1.505(4) . ? C2 C3 1.388(4) . ? C2 C7 1.397(4) . ? C3 C4 1.385(4) . ? C3 H3 0.9300 . ? C4 C5 1.375(4) . ? C4 H4 0.9300 . ? C5 C6 1.388(4) . ? C6 C7 1.392(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.386(5) . ? C8 H8 0.9300 . ? C9 C10 1.352(6) . ? C9 H9 0.9300 . ? C10 C11 1.376(6) . ? C10 H10 0.9300 . ? C11 C12 1.396(5) . ? C11 H11 0.9300 . ? C12 C13 1.486(5) . ? C13 C14 1.400(4) . ? C14 C15 1.372(6) . ? C14 H14 0.9300 . ? C15 C16 1.374(6) . ? C15 H15 0.9300 . ? C16 C17 1.380(5) . ? C16 H16 0.9300 . ? C17 H17 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 O2W Cd1 O3 84.37(9) . . ? O2W Cd1 N1 152.08(9) . . ? O3 Cd1 N1 92.68(9) . . ? O2W Cd1 O1 123.98(9) . 2_655 ? O3 Cd1 O1 84.31(9) . 2_655 ? N1 Cd1 O1 83.11(10) . 2_655 ? O2W Cd1 N2 82.98(9) . . ? O3 Cd1 N2 82.30(8) . . ? N1 Cd1 N2 69.12(10) . . ? O1 Cd1 N2 148.40(9) 2_655 . ? O2W Cd1 O1W 80.08(9) . . ? O3 Cd1 O1W 159.81(8) . . ? N1 Cd1 O1W 95.04(9) . . ? O1 Cd1 O1W 115.11(9) 2_655 . ? N2 Cd1 O1W 83.08(8) . . ? O2W Cd1 O2 80.45(9) . 2_655 ? O3 Cd1 O2 110.08(8) . 2_655 ? N1 Cd1 O2 126.10(9) . 2_655 ? O1 Cd1 O2 53.21(9) 2_655 2_655 ? N2 Cd1 O2 158.08(9) . 2_655 ? O1W Cd1 O2 80.02(8) . 2_655 ? O4 S1 O3 109.58(13) . . ? O4 S1 C5 103.61(13) . . ? O3 S1 C5 101.98(13) . . ? Cd1 O1W H1W1 111(3) . . ? Cd1 O1W H1W2 108(3) . . ? H1W1 O1W H1W2 110.8(17) . . ? Cd1 O2W H2W1 121(3) . . ? Cd1 O2W H2W2 109(3) . . ? H2W1 O2W H2W2 110.7(17) . . ? C1 O1 Cd1 94.6(2) . 2_655 ? C1 O2 Cd1 90.5(2) . 2_655 ? S1 O3 Cd1 135.94(13) . . ? C8 N1 C12 118.6(3) . . ? C8 N1 Cd1 121.7(2) . . ? C12 N1 Cd1 118.8(2) . . ? C17 N2 C13 119.0(3) . . ? C17 N2 Cd1 123.6(2) . . ? C13 N2 Cd1 117.4(2) . . ? O1 C1 O2 121.6(3) . . ? O1 C1 C2 119.1(3) . . ? O2 C1 C2 119.3(3) . . ? C3 C2 C7 119.5(3) . . ? C3 C2 C1 120.0(3) . . ? C7 C2 C1 120.5(3) . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 119.9(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.8(3) . . ? C4 C5 S1 116.0(2) . . ? C6 C5 S1 123.2(2) . . ? C5 C6 C7 119.4(3) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C6 C7 C2 120.0(3) . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? N1 C8 C9 122.6(4) . . ? N1 C8 H8 118.7 . . ? C9 C8 H8 118.7 . . ? C10 C9 C8 119.3(4) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 118.9(3) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C10 C11 C12 119.9(4) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? N1 C12 C11 120.6(3) . . ? N1 C12 C13 116.9(3) . . ? C11 C12 C13 122.5(3) . . ? N2 C13 C14 120.9(3) . . ? N2 C13 C12 116.9(3) . . ? C14 C13 C12 122.1(3) . . ? C15 C14 C13 119.4(4) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 119.4(3) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 C17 118.7(4) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? N2 C17 C16 122.6(3) . . ? N2 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? 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 S1 O3 Cd1 -36.5(2) . . . . ? C5 S1 O3 Cd1 72.8(2) . . . . ? O2W Cd1 O3 S1 26.40(19) . . . . ? N1 Cd1 O3 S1 178.56(19) . . . . ? O1 Cd1 O3 S1 -98.64(19) 2_655 . . . ? N2 Cd1 O3 S1 110.1(2) . . . . ? O1W Cd1 O3 S1 66.1(3) . . . . ? O2 Cd1 O3 S1 -51.3(2) 2_655 . . . ? O2W Cd1 N1 C8 176.6(2) . . . . ? O3 Cd1 N1 C8 93.5(3) . . . . ? O1 Cd1 N1 C8 9.6(3) 2_655 . . . ? N2 Cd1 N1 C8 174.2(3) . . . . ? O1W Cd1 N1 C8 -105.1(3) . . . . ? O2 Cd1 N1 C8 -23.8(3) 2_655 . . . ? O2W Cd1 N1 C12 7.9(4) . . . . ? O3 Cd1 N1 C12 -75.1(2) . . . . ? O1 Cd1 N1 C12 -159.0(2) 2_655 . . . ? N2 Cd1 N1 C12 5.6(2) . . . . ? O1W Cd1 N1 C12 86.2(2) . . . . ? O2 Cd1 N1 C12 167.5(2) 2_655 . . . ? O2W Cd1 N2 C17 0.1(2) . . . . ? O3 Cd1 N2 C17 -85.1(2) . . . . ? N1 Cd1 N2 C17 179.0(3) . . . . ? O1 Cd1 N2 C17 -150.9(2) 2_655 . . . ? O1W Cd1 N2 C17 80.9(2) . . . . ? O2 Cd1 N2 C17 41.2(4) 2_655 . . . ? O2W Cd1 N2 C13 -178.7(2) . . . . ? O3 Cd1 N2 C13 96.1(2) . . . . ? N1 Cd1 N2 C13 0.2(2) . . . . ? O1 Cd1 N2 C13 30.3(3) 2_655 . . . ? O1W Cd1 N2 C13 -97.9(2) . . . . ? O2 Cd1 N2 C13 -137.6(2) 2_655 . . . ? Cd1 O1 C1 O2 -3.7(3) 2_655 . . . ? Cd1 O1 C1 C2 175.6(2) 2_655 . . . ? Cd1 O2 C1 O1 3.5(3) 2_655 . . . ? Cd1 O2 C1 C2 -175.7(2) 2_655 . . . ? O1 C1 C2 C3 165.8(3) . . . . ? O2 C1 C2 C3 -15.0(4) . . . . ? O1 C1 C2 C7 -14.1(4) . . . . ? O2 C1 C2 C7 165.2(3) . . . . ? C7 C2 C3 C4 -0.2(5) . . . . ? C1 C2 C3 C4 179.9(3) . . . . ? C2 C3 C4 C5 -1.9(5) . . . . ? C3 C4 C5 C6 2.8(5) . . . . ? C3 C4 C5 S1 -175.6(3) . . . . ? O4 S1 C5 C4 -153.8(2) . . . . ? O3 S1 C5 C4 92.4(2) . . . . ? O4 S1 C5 C6 27.9(3) . . . . ? O3 S1 C5 C6 -85.9(3) . . . . ? C4 C5 C6 C7 -1.6(5) . . . . ? S1 C5 C6 C7 176.6(2) . . . . ? C5 C6 C7 C2 -0.5(5) . . . . ? C3 C2 C7 C6 1.4(5) . . . . ? C1 C2 C7 C6 -178.7(3) . . . . ? C12 N1 C8 C9 1.3(5) . . . . ? Cd1 N1 C8 C9 -167.4(3) . . . . ? N1 C8 C9 C10 0.7(6) . . . . ? C8 C9 C10 C11 -2.7(6) . . . . ? C9 C10 C11 C12 2.9(6) . . . . ? C8 N1 C12 C11 -1.1(5) . . . . ? Cd1 N1 C12 C11 167.9(3) . . . . ? C8 N1 C12 C13 -179.4(3) . . . . ? Cd1 N1 C12 C13 -10.4(4) . . . . ? C10 C11 C12 N1 -1.0(5) . . . . ? C10 C11 C12 C13 177.2(3) . . . . ? C17 N2 C13 C14 -2.0(4) . . . . ? Cd1 N2 C13 C14 176.8(2) . . . . ? C17 N2 C13 C12 175.8(3) . . . . ? Cd1 N2 C13 C12 -5.4(3) . . . . ? N1 C12 C13 N2 10.4(4) . . . . ? C11 C12 C13 N2 -167.8(3) . . . . ? N1 C12 C13 C14 -171.8(3) . . . . ? C11 C12 C13 C14 9.9(5) . . . . ? N2 C13 C14 C15 1.8(5) . . . . ? C12 C13 C14 C15 -175.9(3) . . . . ? C13 C14 C15 C16 -0.5(5) . . . . ? C14 C15 C16 C17 -0.4(6) . . . . ? C13 N2 C17 C16 1.1(5) . . . . ? Cd1 N2 C17 C16 -177.7(2) . . . . ? C15 C16 C17 N2 0.1(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 O1W H1W1 O4 0.85(3) 1.93(3) 2.775(3) 176(4) 1_655 O1W H1W2 O2 0.85(3) 2.14(3) 2.960(4) 163(4) 1_565 O2W H2W1 O2 0.85(3) 2.15(2) 2.882(4) 145(3) 1_565 O2W H2W1 O4 0.85(3) 2.52(3) 2.934(3) 111(3) 2_565 O2W H2W2 O4 0.85(3) 1.98(3) 2.777(3) 158(3) . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.855 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.110 #===END data_complex4 #TrackingRef '- revised cif.cif' _database_code_depnum_ccdc_archive 'CCDC 855415' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H18 N2 O7 S Zn' _chemical_formula_sum 'C17 H18 N2 O7 S Zn' _chemical_formula_weight 459.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6682(17) _cell_length_b 10.7302(19) _cell_length_c 11.371(2) _cell_angle_alpha 89.097(5) _cell_angle_beta 72.836(6) _cell_angle_gamma 89.849(6) _cell_volume 893.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4401 _cell_measurement_theta_min 3.37 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 1.536 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7287 _exptl_absorpt_correction_T_max 0.8137 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7808 _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_av_sigmaI/netI 0.0964 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3985 _reflns_number_gt 2308 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.1326P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3985 _refine_ls_number_parameters 254 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1229 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.2249 _refine_ls_wR_factor_gt 0.1744 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.76708(13) 0.25835(11) 0.18879(8) 0.0352(3) Uani 1 1 d . . . S1 S 0.3163(3) 0.2060(2) 0.2978(2) 0.0400(6) Uani 1 1 d D . . O1 O 0.5114(8) 0.1639(6) 0.2465(5) 0.0353(14) Uani 1 1 d . . . O2 O 0.2861(9) 0.3353(7) 0.2565(6) 0.0455(17) Uani 1 1 d . . . O3 O 0.1792(10) 0.1387(6) 0.9112(6) 0.0437(17) Uani 1 1 d . . . O4 O 0.2126(10) 0.3464(7) 0.8978(6) 0.0455(18) Uani 1 1 d . . . O1W O 0.6307(9) 0.4374(6) 0.2126(5) 0.0388(15) Uani 1 1 d . . . H1W1 H 0.5199 0.4268 0.2358 0.058 Uiso 1 1 d R . . H1W2 H 0.6595 0.4758 0.1468 0.058 Uiso 1 1 d R . . O2W O 1.0184(8) 0.3551(6) 0.1333(5) 0.0392(15) Uani 1 1 d . . . H2W1 H 1.0668 0.3452 0.0595 0.059 Uiso 1 1 d R . . H2W2 H 1.0863 0.3290 0.1720 0.059 Uiso 1 1 d R . . O3W O 0.9283(9) 0.0910(6) 0.1493(5) 0.0383(15) Uani 1 1 d . . . H3W1 H 0.8645 0.0330 0.1398 0.057 Uiso 1 1 d R . . H3W2 H 1.0122 0.1024 0.0859 0.057 Uiso 1 1 d R . . N2 N 0.7404(7) 0.2553(9) 1.0065(5) 0.0323(15) Uani 1 1 d D . . N1 N 0.7738(8) 0.2578(8) 0.3773(5) 0.0325(15) Uani 1 1 d D . . C1 C 0.2866(7) 0.2232(8) 0.4614(7) 0.033(2) Uani 1 1 d D . . C2 C 0.3406(9) 0.1243(8) 0.5232(7) 0.036(2) Uani 1 1 d D . . H2 H 0.3917 0.0536 0.4802 0.044 Uiso 1 1 calc R . . C3 C 0.3187(9) 0.1302(8) 0.6479(7) 0.0352(19) Uani 1 1 d D . . H3 H 0.3552 0.0638 0.6885 0.042 Uiso 1 1 calc R . . C4 C 0.2418(8) 0.2361(8) 0.7131(7) 0.0326(18) Uani 1 1 d D . . C5 C 0.1893(10) 0.3346(9) 0.6505(8) 0.039(2) Uani 1 1 d D . . H5 H 0.1392 0.4057 0.6931 0.046 Uiso 1 1 calc R . . C6 C 0.2108(10) 0.3281(9) 0.5245(7) 0.037(2) Uani 1 1 d D . . H6 H 0.1742 0.3942 0.4835 0.045 Uiso 1 1 calc R . . C7 C 0.2157(9) 0.2418(10) 0.8504(7) 0.038(2) Uani 1 1 d D . . C8 C 0.8398(9) 0.1622(7) 0.4257(7) 0.0294(18) Uani 1 1 d D . . H8 H 0.8960 0.0975 0.3750 0.035 Uiso 1 1 calc R . . C9 C 0.8273(10) 0.1555(8) 0.5525(8) 0.037(2) Uani 1 1 d D . . H9 H 0.8750 0.0870 0.5834 0.044 Uiso 1 1 calc R . . C10 C 0.7468(9) 0.2478(10) 0.6285(6) 0.0323(18) Uani 1 1 d D . . C11 C 0.6765(10) 0.3493(9) 0.5775(7) 0.036(2) Uani 1 1 d D . . H11 H 0.6200 0.4148 0.6270 0.044 Uiso 1 1 calc R . . C12 C 0.6925(10) 0.3510(7) 0.4516(7) 0.0327(19) Uani 1 1 d D . . H12 H 0.6456 0.4184 0.4183 0.039 Uiso 1 1 calc R . . C13 C 0.7101(9) 0.1498(9) 0.9552(8) 0.039(2) Uani 1 1 d D . . H13 H 0.6919 0.0772 1.0031 0.047 Uiso 1 1 calc R . . C14 C 0.7039(11) 0.1413(9) 0.8337(8) 0.040(2) Uani 1 1 d D . . H14 H 0.6813 0.0658 0.8018 0.048 Uiso 1 1 calc R . . C15 C 0.7334(9) 0.2525(10) 0.7612(6) 0.0338(18) Uani 1 1 d D . . C16 C 0.7615(11) 0.3610(8) 0.8168(8) 0.0308(19) Uani 1 1 d D . . H16 H 0.7776 0.4361 0.7729 0.037 Uiso 1 1 calc R . . C17 C 0.7658(10) 0.3586(9) 0.9365(7) 0.038(2) Uani 1 1 d D . . H17 H 0.7875 0.4330 0.9708 0.045 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 0.0361(6) 0.0530(6) 0.0172(4) -0.0011(6) -0.0091(4) 0.0056(6) S1 0.0340(12) 0.0608(16) 0.0250(10) -0.0012(10) -0.0084(9) -0.0003(11) O1 0.031(3) 0.049(4) 0.019(3) -0.001(3) 0.004(2) 0.002(3) O2 0.047(4) 0.049(4) 0.040(4) 0.008(3) -0.014(3) 0.005(3) O3 0.048(4) 0.052(4) 0.026(3) 0.002(3) -0.003(3) 0.004(3) O4 0.056(5) 0.050(4) 0.023(3) -0.003(3) -0.001(3) -0.013(3) O1W 0.038(4) 0.054(4) 0.020(3) 0.000(3) -0.004(3) 0.005(3) O2W 0.041(4) 0.054(4) 0.024(3) 0.002(3) -0.012(3) 0.001(3) O3W 0.041(4) 0.045(4) 0.029(3) -0.013(3) -0.010(3) 0.010(3) N2 0.032(3) 0.052(4) 0.012(3) 0.003(4) -0.006(2) 0.005(4) N1 0.035(3) 0.048(4) 0.017(3) 0.003(3) -0.012(3) 0.005(4) C1 0.021(4) 0.049(6) 0.025(4) -0.004(4) -0.003(3) 0.005(4) C2 0.049(6) 0.039(5) 0.025(4) -0.005(3) -0.017(4) 0.012(4) C3 0.044(5) 0.034(5) 0.024(4) 0.001(3) -0.004(4) -0.002(4) C4 0.029(4) 0.040(5) 0.028(4) -0.009(4) -0.008(3) 0.000(4) C5 0.028(5) 0.051(6) 0.036(5) -0.001(4) -0.009(4) -0.005(4) C6 0.038(5) 0.051(6) 0.020(4) -0.005(4) -0.005(4) 0.008(4) C7 0.034(4) 0.052(6) 0.026(4) 0.003(4) -0.004(3) 0.012(5) C8 0.036(5) 0.026(4) 0.028(4) -0.006(3) -0.013(4) 0.007(3) C9 0.036(5) 0.046(5) 0.026(4) -0.005(4) -0.006(4) 0.016(4) C10 0.020(4) 0.053(5) 0.023(3) -0.004(4) -0.004(3) 0.012(5) C11 0.028(5) 0.059(6) 0.020(4) -0.007(4) -0.004(3) 0.002(4) C12 0.051(5) 0.022(4) 0.028(4) -0.016(3) -0.015(4) 0.008(4) C13 0.056(6) 0.034(5) 0.025(4) 0.003(4) -0.010(4) 0.003(4) C14 0.054(6) 0.039(5) 0.036(5) 0.002(4) -0.026(5) -0.004(4) C15 0.027(4) 0.053(5) 0.022(3) -0.004(4) -0.009(3) 0.003(4) C16 0.045(5) 0.027(4) 0.024(4) 0.000(3) -0.017(4) 0.002(4) C17 0.051(6) 0.046(5) 0.017(4) -0.007(4) -0.011(4) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2W 2.112(6) . ? Zn1 O1 2.129(6) . ? Zn1 N2 2.143(5) 1_554 ? Zn1 O3W 2.155(6) . ? Zn1 N1 2.160(6) . ? Zn1 O1W 2.167(6) . ? S1 O2 1.498(7) . ? S1 O1 1.507(6) . ? S1 C1 1.818(8) . ? O3 C7 1.282(11) . ? O4 C7 1.251(11) . ? O1W H1W1 0.8200 . ? O1W H1W2 0.8200 . ? O2W H2W1 0.8200 . ? O2W H2W2 0.8200 . ? O3W H3W1 0.8200 . ? O3W H3W2 0.8200 . ? N2 C13 1.334(12) . ? N2 C17 1.335(12) . ? N2 Zn1 2.143(5) 1_556 ? N1 C8 1.325(11) . ? N1 C12 1.347(10) . ? C1 C6 1.377(12) . ? C1 C2 1.393(12) . ? C2 C3 1.380(11) . ? C2 H2 0.9300 . ? C3 C4 1.398(12) . ? C3 H3 0.9300 . ? C4 C5 1.388(12) . ? C4 C7 1.516(10) . ? C5 C6 1.396(11) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.416(11) . ? C8 H8 0.9300 . ? C9 C10 1.348(12) . ? C9 H9 0.9300 . ? C10 C11 1.405(13) . ? C10 C15 1.484(10) . ? C11 C12 1.401(11) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.401(12) . ? C13 H13 0.9300 . ? C14 C15 1.419(13) . ? C14 H14 0.9300 . ? C15 C16 1.381(12) . ? C16 C17 1.371(11) . ? C16 H16 0.9300 . ? C17 H17 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 O2W Zn1 O1 178.9(2) . . ? O2W Zn1 N2 93.8(2) . 1_554 ? O1 Zn1 N2 86.6(2) . 1_554 ? O2W Zn1 O3W 86.0(3) . . ? O1 Zn1 O3W 95.1(3) . . ? N2 Zn1 O3W 89.2(3) 1_554 . ? O2W Zn1 N1 90.2(2) . . ? O1 Zn1 N1 89.4(2) . . ? N2 Zn1 N1 175.9(2) 1_554 . ? O3W Zn1 N1 92.2(3) . . ? O2W Zn1 O1W 88.1(3) . . ? O1 Zn1 O1W 90.9(2) . . ? N2 Zn1 O1W 88.2(3) 1_554 . ? O3W Zn1 O1W 173.3(2) . . ? N1 Zn1 O1W 90.9(3) . . ? O2 S1 O1 112.7(4) . . ? O2 S1 C1 103.2(4) . . ? O1 S1 C1 104.0(3) . . ? S1 O1 Zn1 134.0(4) . . ? Zn1 O1W H1W1 109.7 . . ? Zn1 O1W H1W2 109.3 . . ? H1W1 O1W H1W2 109.5 . . ? Zn1 O2W H2W1 109.4 . . ? Zn1 O2W H2W2 110.2 . . ? H2W1 O2W H2W2 109.5 . . ? Zn1 O3W H3W1 109.6 . . ? Zn1 O3W H3W2 108.8 . . ? H3W1 O3W H3W2 109.5 . . ? C13 N2 C17 117.2(6) . . ? C13 N2 Zn1 121.8(6) . 1_556 ? C17 N2 Zn1 120.8(6) . 1_556 ? C8 N1 C12 118.6(6) . . ? C8 N1 Zn1 121.7(6) . . ? C12 N1 Zn1 119.3(6) . . ? C6 C1 C2 120.0(7) . . ? C6 C1 S1 122.5(7) . . ? C2 C1 S1 117.5(6) . . ? C3 C2 C1 120.5(8) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 120.0(8) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 119.1(7) . . ? C5 C4 C7 121.0(8) . . ? C3 C4 C7 119.9(8) . . ? C4 C5 C6 120.8(9) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C1 C6 C5 119.5(9) . . ? C1 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? O4 C7 O3 124.6(7) . . ? O4 C7 C4 118.4(8) . . ? O3 C7 C4 116.7(8) . . ? N1 C8 C9 122.0(7) . . ? N1 C8 H8 119.0 . . ? C9 C8 H8 119.0 . . ? C10 C9 C8 120.5(8) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 117.8(7) . . ? C9 C10 C15 124.8(9) . . ? C11 C10 C15 117.4(9) . . ? C12 C11 C10 119.4(8) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? N1 C12 C11 121.8(8) . . ? N1 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? N2 C13 C14 124.1(8) . . ? N2 C13 H13 117.9 . . ? C14 C13 H13 117.9 . . ? C13 C14 C15 117.4(8) . . ? C13 C14 H14 121.3 . . ? C15 C14 H14 121.3 . . ? C16 C15 C14 117.4(7) . . ? C16 C15 C10 122.3(9) . . ? C14 C15 C10 120.1(9) . . ? C17 C16 C15 120.3(8) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? N2 C17 C16 123.5(8) . . ? N2 C17 H17 118.2 . . ? C16 C17 H17 118.2 . . ? 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 O2 S1 O1 Zn1 27.8(6) . . . . ? C1 S1 O1 Zn1 -83.2(5) . . . . ? N2 Zn1 O1 S1 -94.5(5) 1_554 . . . ? O3W Zn1 O1 S1 176.6(4) . . . . ? N1 Zn1 O1 S1 84.5(5) . . . . ? O1W Zn1 O1 S1 -6.4(5) . . . . ? O2W Zn1 N1 C8 -94.8(4) . . . . ? O1 Zn1 N1 C8 86.2(4) . . . . ? O3W Zn1 N1 C8 -8.8(4) . . . . ? O1W Zn1 N1 C8 177.1(4) . . . . ? O2W Zn1 N1 C12 92.0(4) . . . . ? O1 Zn1 N1 C12 -86.9(4) . . . . ? O3W Zn1 N1 C12 178.0(4) . . . . ? O1W Zn1 N1 C12 3.9(4) . . . . ? O2 S1 C1 C6 13.4(5) . . . . ? O1 S1 C1 C6 131.2(4) . . . . ? O2 S1 C1 C2 -167.8(4) . . . . ? O1 S1 C1 C2 -50.0(4) . . . . ? C6 C1 C2 C3 0.0(3) . . . . ? S1 C1 C2 C3 -178.79(19) . . . . ? C1 C2 C3 C4 0.0(3) . . . . ? C2 C3 C4 C5 -0.4(5) . . . . ? C2 C3 C4 C7 179.2(3) . . . . ? C3 C4 C5 C6 0.7(7) . . . . ? C7 C4 C5 C6 -178.9(5) . . . . ? C2 C1 C6 C5 0.3(6) . . . . ? S1 C1 C6 C5 179.0(4) . . . . ? C4 C5 C6 C1 -0.6(7) . . . . ? C5 C4 C7 O4 -26.5(9) . . . . ? C3 C4 C7 O4 153.9(7) . . . . ? C5 C4 C7 O3 146.4(7) . . . . ? C3 C4 C7 O3 -33.2(8) . . . . ? C12 N1 C8 C9 -0.1(3) . . . . ? Zn1 N1 C8 C9 -173.3(4) . . . . ? N1 C8 C9 C10 0.0(3) . . . . ? C8 C9 C10 C11 0.1(6) . . . . ? C8 C9 C10 C15 -177.3(7) . . . . ? C9 C10 C11 C12 0.0(7) . . . . ? C15 C10 C11 C12 177.6(7) . . . . ? C8 N1 C12 C11 0.1(6) . . . . ? Zn1 N1 C12 C11 173.5(5) . . . . ? C10 C11 C12 N1 -0.1(8) . . . . ? C17 N2 C13 C14 0.1(3) . . . . ? Zn1 N2 C13 C14 -175.5(4) 1_556 . . . ? N2 C13 C14 C15 0.6(3) . . . . ? C13 C14 C15 C16 -1.6(6) . . . . ? C13 C14 C15 C10 174.0(5) . . . . ? C9 C10 C15 C16 138.2(7) . . . . ? C11 C10 C15 C16 -39.3(8) . . . . ? C9 C10 C15 C14 -37.1(8) . . . . ? C11 C10 C15 C14 145.4(6) . . . . ? C14 C15 C16 C17 2.0(8) . . . . ? C10 C15 C16 C17 -173.5(6) . . . . ? C13 N2 C17 C16 0.3(6) . . . . ? Zn1 N2 C17 C16 175.9(5) 1_556 . . . ? C15 C16 C17 N2 -1.3(8) . . . . ? 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 O1W H1W1 O2 0.82 2.00 2.766(9) 156.1 . O1W H1W2 O4 0.82 2.13 2.727(10) 129.4 2_666 O2W H2W1 O4 0.82 1.85 2.655(9) 167.8 1_654 O2W H2W2 O2 0.82 2.04 2.812(9) 157.4 1_655 O3W H3W1 O3 0.82 2.00 2.761(9) 154.4 2_656 O3W H3W2 O3 0.82 2.05 2.860(9) 168.0 1_654 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.843 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.131 #===END data_complex5 #TrackingRef '- revised cif.cif' _database_code_depnum_ccdc_archive 'CCDC 855416' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 N4 O4 Zn, C7 H4 O5 S, 4(H2 O)' _chemical_formula_sum 'C27 H36 N4 O13 S Zn' _chemical_formula_weight 722.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.1106(14) _cell_length_b 18.310(4) _cell_length_c 12.360(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.11(3) _cell_angle_gamma 90.00 _cell_volume 1584.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 8654 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 27.36 _exptl_crystal_description prim _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 0.912 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7348 _exptl_absorpt_correction_T_max 0.8458 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15429 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0924 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.38 _reflns_number_total 6971 _reflns_number_gt 4161 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0732P)^2^+2.2316P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.29(2) _refine_ls_number_reflns 6971 _refine_ls_number_parameters 452 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.1156 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1900 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.52595(11) 0.53938(4) 0.19321(6) 0.0463(2) Uani 1 1 d . . . S1 S 1.0126(3) 0.81411(10) 0.69740(18) 0.0591(5) Uani 1 1 d . . . O1W O 0.2679(8) 0.5835(4) 0.2283(5) 0.0631(15) Uani 1 1 d D . . H1W1 H 0.176(8) 0.605(5) 0.188(6) 0.095 Uiso 1 1 d D . . H1W2 H 0.232(10) 0.567(5) 0.286(4) 0.095 Uiso 1 1 d D . . O1 O 1.1974(7) 0.8099(3) 0.6646(5) 0.0731(17) Uani 1 1 d . . . O2W O 0.6438(8) 0.6441(3) 0.1811(5) 0.0558(13) Uani 1 1 d D . . H2W1 H 0.578(8) 0.683(2) 0.173(7) 0.084 Uiso 1 1 d D . . H2W2 H 0.761(3) 0.654(4) 0.182(7) 0.084 Uiso 1 1 d D . . O2 O 0.9816(10) 0.7556(3) 0.7703(6) 0.0837(19) Uani 1 1 d . . . O3W O 0.7809(8) 0.4932(3) 0.1578(5) 0.0620(15) Uani 1 1 d D . . H3W1 H 0.823(13) 0.459(3) 0.202(5) 0.093 Uiso 1 1 d D . . H3W2 H 0.798(13) 0.483(4) 0.093(2) 0.093 Uiso 1 1 d D . . O3 O 0.9730(8) 0.8854(3) 0.7399(5) 0.0677(16) Uani 1 1 d . . . O4W O 0.3942(9) 0.4337(3) 0.2005(5) 0.0616(14) Uani 1 1 d D . . H4W1 H 0.341(13) 0.429(4) 0.256(5) 0.092 Uiso 1 1 d D . . H4W2 H 0.417(14) 0.392(2) 0.175(7) 0.092 Uiso 1 1 d D . . O4 O 0.2293(8) 0.7836(4) 0.3096(6) 0.0759(17) Uani 1 1 d . . . O5 O 0.4495(9) 0.7677(4) 0.2027(6) 0.0789(18) Uani 1 1 d . . . O5W O 0.0031(8) 0.6947(3) 0.1585(6) 0.0666(15) Uani 1 1 d D . . H5W1 H 0.068(12) 0.723(4) 0.206(5) 0.100 Uiso 1 1 d D . . H5W2 H -0.036(14) 0.719(4) 0.100(4) 0.100 Uiso 1 1 d D . . N1 N 0.4160(6) 0.5417(4) 0.0206(4) 0.0420(11) Uani 1 1 d . . . N2 N 0.1923(10) 0.5676(4) -0.5609(5) 0.0556(17) Uani 1 1 d . . . N3 N 0.6371(7) 0.5326(3) 0.3660(4) 0.0399(11) Uani 1 1 d . . . N4 N 0.8787(9) 0.5201(4) 0.9506(5) 0.0605(18) Uani 1 1 d . . . C1 C 0.8406(10) 0.8019(4) 0.5767(7) 0.0539(19) Uani 1 1 d . . . C2 C 0.6473(11) 0.7971(4) 0.5893(8) 0.061(2) Uani 1 1 d . . . H2A H 0.6151 0.7977 0.6590 0.073 Uiso 1 1 calc R . . C3 C 0.5101(13) 0.7917(5) 0.4996(9) 0.0585(17) Uani 1 1 d . . . H3A H 0.3829 0.7904 0.5083 0.070 Uiso 1 1 calc R . . C4 C 0.5525(10) 0.7881(4) 0.3954(7) 0.058(2) Uani 1 1 d . . . C5 C 0.7470(11) 0.7926(4) 0.3812(7) 0.0577(19) Uani 1 1 d . . . H5A H 0.7789 0.7903 0.3115 0.069 Uiso 1 1 calc R . . C6 C 0.8888(10) 0.8007(4) 0.4745(7) 0.056(2) Uani 1 1 d . . . H6A H 1.0161 0.8052 0.4669 0.068 Uiso 1 1 calc R . . C7 C 0.4001(12) 0.7801(4) 0.2962(8) 0.061(2) Uani 1 1 d . . . C8 C 0.3415(11) 0.6032(4) -0.0299(6) 0.0513(18) Uani 1 1 d . . . H8A H 0.3265 0.6435 0.0135 0.062 Uiso 1 1 calc R . . C9 C 0.2870(11) 0.6094(4) -0.1410(6) 0.0490(17) Uani 1 1 d . . . H9A H 0.2348 0.6530 -0.1709 0.059 Uiso 1 1 calc R . . C10 C 0.3085(8) 0.5515(4) -0.2095(5) 0.0400(15) Uani 1 1 d . . . C11 C 0.3817(10) 0.4873(4) -0.1573(6) 0.0482(17) Uani 1 1 d . . . H11A H 0.3971 0.4461 -0.1989 0.058 Uiso 1 1 calc R . . C12 C 0.4314(12) 0.4847(4) -0.0438(6) 0.0520(18) Uani 1 1 d . . . H12A H 0.4777 0.4409 -0.0112 0.062 Uiso 1 1 calc R . . C13 C 0.2623(9) 0.5570(4) -0.3309(6) 0.0434(16) Uani 1 1 d . . . C14 C 0.2451(12) 0.6239(4) -0.3843(6) 0.0538(18) Uani 1 1 d . . . H14A H 0.2558 0.6669 -0.3437 0.065 Uiso 1 1 calc R . . C15 C 0.2124(12) 0.6265(4) -0.4972(6) 0.058(2) Uani 1 1 d . . . H15A H 0.2038 0.6721 -0.5308 0.070 Uiso 1 1 calc R . . C16 C 0.2044(12) 0.5037(5) -0.5113(7) 0.0559(19) Uani 1 1 d . . . H16A H 0.1886 0.4617 -0.5543 0.067 Uiso 1 1 calc R . . C17 C 0.2398(12) 0.4962(4) -0.3976(6) 0.056(2) Uani 1 1 d . . . H17A H 0.2483 0.4499 -0.3663 0.068 Uiso 1 1 calc R . . C18 C 0.6758(13) 0.5930(4) 0.4264(7) 0.055(2) Uani 1 1 d . . . H18A H 0.6682 0.6375 0.3899 0.066 Uiso 1 1 calc R . . C19 C 0.7259(13) 0.5937(4) 0.5386(7) 0.055(2) Uani 1 1 d . . . H19A H 0.7428 0.6380 0.5760 0.066 Uiso 1 1 calc R . . C20 C 0.7514(8) 0.5288(4) 0.5960(5) 0.0413(15) Uani 1 1 d . . . C21 C 0.7189(12) 0.4655(4) 0.5328(7) 0.055(2) Uani 1 1 d . . . H21A H 0.7345 0.4200 0.5665 0.066 Uiso 1 1 calc R . . C22 C 0.6642(12) 0.4702(4) 0.4214(7) 0.052(2) Uani 1 1 d . . . H22A H 0.6445 0.4269 0.3817 0.062 Uiso 1 1 calc R . . C23 C 0.7990(9) 0.5263(4) 0.7194(5) 0.0453(17) Uani 1 1 d . . . C24 C 0.7819(11) 0.5875(5) 0.7834(6) 0.0545(19) Uani 1 1 d . . . H24A H 0.7455 0.6323 0.7507 0.065 Uiso 1 1 calc R . . C25 C 0.8197(12) 0.5810(5) 0.8957(6) 0.060(2) Uani 1 1 d . . . H25A H 0.8028 0.6223 0.9368 0.072 Uiso 1 1 calc R . . C26 C 0.9028(11) 0.4634(5) 0.8880(7) 0.063(2) Uani 1 1 d . . . H26A H 0.9473 0.4204 0.9235 0.076 Uiso 1 1 calc R . . C27 C 0.8678(11) 0.4625(5) 0.7744(7) 0.0556(18) Uani 1 1 d . . . H27A H 0.8894 0.4207 0.7357 0.067 Uiso 1 1 calc R . . O6W O 0.5198(10) 0.3034(4) 0.1423(8) 0.111(3) Uani 1 1 d D . . H6W1 H 0.6002 0.3051 0.2019 0.167 Uiso 1 1 d RD . . H6W2 H 0.5806 0.3056 0.0890 0.167 Uiso 1 1 d RD . . O8W O 0.8633(12) 0.7736(6) 0.9681(7) 0.120(3) Uani 1 1 d D . . H8W1 H 0.889(18) 0.768(10) 0.904(5) 0.180 Uiso 1 1 d D . . H8W2 H 0.744(5) 0.781(10) 0.964(11) 0.180 Uiso 1 1 d D . . O7W O 0.2805(14) 0.8109(6) 0.0117(8) 0.146(4) Uani 1 1 d D . . H7W1 H 0.1629 0.7994 0.0019 0.219 Uiso 1 1 d RD . . H7W2 H 0.3334 0.7959 0.0748 0.219 Uiso 1 1 d RD . . 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 0.0487(4) 0.0514(4) 0.0379(4) 0.0025(4) 0.0045(3) 0.0029(4) S1 0.0577(11) 0.0447(10) 0.0723(14) 0.0017(9) 0.0041(10) -0.0005(9) O1W 0.052(3) 0.089(4) 0.052(3) 0.011(3) 0.018(3) 0.017(3) O1 0.041(3) 0.084(4) 0.096(5) -0.003(3) 0.015(3) 0.012(3) O2W 0.053(3) 0.056(3) 0.057(3) 0.002(3) 0.007(3) -0.001(2) O2 0.093(4) 0.065(4) 0.093(5) 0.027(3) 0.015(4) 0.001(3) O3W 0.062(3) 0.084(4) 0.044(3) 0.019(3) 0.023(3) 0.030(3) O3 0.062(3) 0.050(3) 0.086(4) -0.018(3) -0.001(3) -0.005(3) O4W 0.080(4) 0.049(3) 0.057(4) 0.005(3) 0.015(3) -0.005(3) O4 0.045(3) 0.080(4) 0.100(5) -0.013(4) 0.004(3) 0.000(3) O5 0.069(4) 0.093(5) 0.074(5) -0.003(4) 0.008(3) 0.011(4) O5W 0.050(3) 0.068(4) 0.078(4) 0.002(3) 0.001(3) -0.007(3) N1 0.039(2) 0.051(3) 0.034(3) 0.003(3) 0.0011(19) 0.002(3) N2 0.055(4) 0.066(4) 0.045(4) 0.000(3) 0.011(3) -0.007(3) N3 0.039(2) 0.044(3) 0.035(3) 0.004(3) 0.0016(19) -0.004(3) N4 0.060(4) 0.078(5) 0.042(4) 0.010(3) 0.004(3) -0.008(3) C1 0.052(4) 0.038(4) 0.073(5) -0.011(3) 0.017(4) -0.005(3) C2 0.059(4) 0.052(4) 0.074(6) -0.015(4) 0.016(4) -0.002(4) C3 0.049(4) 0.055(4) 0.074(5) -0.016(3) 0.018(3) 0.002(3) C4 0.053(4) 0.034(3) 0.082(6) -0.007(4) 0.002(4) 0.000(3) C5 0.049(4) 0.048(4) 0.078(6) -0.002(4) 0.018(4) 0.006(3) C6 0.042(4) 0.047(4) 0.082(6) -0.010(4) 0.015(4) 0.005(3) C7 0.066(5) 0.043(4) 0.074(6) -0.004(4) 0.008(4) -0.002(4) C8 0.050(4) 0.059(4) 0.041(4) -0.003(3) 0.000(3) 0.004(3) C9 0.061(5) 0.042(4) 0.042(4) 0.000(3) 0.002(3) 0.006(3) C10 0.038(3) 0.047(4) 0.034(3) -0.003(3) 0.005(2) -0.001(3) C11 0.055(4) 0.047(4) 0.040(4) -0.005(3) -0.001(3) -0.002(3) C12 0.073(5) 0.041(4) 0.041(4) -0.003(3) 0.007(4) 0.003(3) C13 0.036(3) 0.050(4) 0.044(4) -0.002(3) 0.009(3) 0.005(3) C14 0.076(5) 0.046(4) 0.041(4) 0.002(3) 0.011(4) 0.005(4) C15 0.073(5) 0.054(4) 0.047(5) 0.008(3) 0.009(4) -0.009(4) C16 0.062(5) 0.055(4) 0.052(5) -0.009(4) 0.013(4) -0.006(4) C17 0.078(5) 0.045(4) 0.048(5) 0.001(3) 0.015(4) 0.001(4) C18 0.077(6) 0.044(4) 0.042(5) 0.007(3) 0.004(4) -0.007(4) C19 0.078(6) 0.034(4) 0.053(5) 0.000(3) 0.011(4) -0.003(4) C20 0.036(3) 0.049(4) 0.040(3) 0.005(3) 0.010(2) 0.003(3) C21 0.080(5) 0.039(4) 0.042(5) 0.008(3) -0.002(4) -0.002(4) C22 0.065(5) 0.041(4) 0.050(5) 0.000(3) 0.009(4) 0.007(3) C23 0.036(3) 0.058(5) 0.042(4) 0.000(3) 0.007(3) -0.008(3) C24 0.058(5) 0.055(4) 0.049(5) -0.004(4) 0.007(4) -0.004(4) C25 0.059(5) 0.082(6) 0.042(5) -0.018(4) 0.014(4) -0.028(4) C26 0.060(5) 0.072(5) 0.057(5) 0.016(4) 0.009(4) 0.012(4) C27 0.063(5) 0.058(4) 0.046(5) 0.003(4) 0.011(4) 0.000(4) O6W 0.082(5) 0.095(5) 0.153(8) -0.017(5) 0.008(4) 0.006(4) O8W 0.096(5) 0.147(8) 0.106(7) 0.045(7) -0.012(5) 0.007(6) O7W 0.127(7) 0.176(10) 0.126(8) 0.014(7) -0.005(6) -0.020(7) _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 O2W 2.109(5) . ? Zn1 O3W 2.115(5) . ? Zn1 O1W 2.119(5) . ? Zn1 N1 2.140(5) . ? Zn1 N3 2.147(5) . ? Zn1 O4W 2.159(5) . ? S1 O2 1.441(6) . ? S1 O1 1.444(5) . ? S1 O3 1.452(5) . ? S1 C1 1.770(8) . ? O1W H1W1 0.85(8) . ? O1W H1W2 0.85(8) . ? O2W H2W1 0.85(8) . ? O2W H2W2 0.85(8) . ? O3W H3W1 0.85(8) . ? O3W H3W2 0.85(8) . ? O4W H4W1 0.85(8) . ? O4W H4W2 0.85(8) . ? O4 C7 1.256(10) . ? O5 C7 1.286(10) . ? O5W H5W1 0.85(8) . ? O5W H5W2 0.85(8) . ? N1 C12 1.330(10) . ? N1 C8 1.349(10) . ? N2 C16 1.318(10) . ? N2 C15 1.328(10) . ? N3 C22 1.329(9) . ? N3 C18 1.335(10) . ? N4 C26 1.324(11) . ? N4 C25 1.334(11) . ? C1 C6 1.366(11) . ? C1 C2 1.412(10) . ? C2 C3 1.346(13) . ? C2 H2A 0.9300 . ? C3 C4 1.374(12) . ? C3 H3A 0.9300 . ? C4 C5 1.427(10) . ? C4 C7 1.494(11) . ? C5 C6 1.400(11) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C8 C9 1.365(10) . ? C8 H8A 0.9300 . ? C9 C10 1.382(9) . ? C9 H9A 0.9300 . ? C10 C11 1.397(9) . ? C10 C13 1.482(9) . ? C11 C12 1.386(10) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C17 1.378(10) . ? C13 C14 1.386(9) . ? C14 C15 1.375(10) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.391(11) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C19 1.369(11) . ? C18 H18A 0.9300 . ? C19 C20 1.380(10) . ? C19 H19A 0.9300 . ? C20 C21 1.394(10) . ? C20 C23 1.505(9) . ? C21 C22 1.366(11) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.389(10) . ? C23 C27 1.396(10) . ? C24 C25 1.371(11) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 C27 1.382(12) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? O6W H6W1 0.8500 . ? O6W H6W2 0.8499 . ? O8W H8W1 0.85(8) . ? O8W H8W2 0.85(8) . ? O7W H7W1 0.8501 . ? O7W H7W2 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 O2W Zn1 O3W 89.0(2) . . ? O2W Zn1 O1W 92.1(2) . . ? O3W Zn1 O1W 178.8(3) . . ? O2W Zn1 N1 89.5(2) . . ? O3W Zn1 N1 88.7(2) . . ? O1W Zn1 N1 91.1(2) . . ? O2W Zn1 N3 92.4(2) . . ? O3W Zn1 N3 90.2(2) . . ? O1W Zn1 N3 90.0(2) . . ? N1 Zn1 N3 177.8(3) . . ? O2W Zn1 O4W 177.4(2) . . ? O3W Zn1 O4W 92.5(2) . . ? O1W Zn1 O4W 86.3(2) . . ? N1 Zn1 O4W 88.5(2) . . ? N3 Zn1 O4W 89.6(2) . . ? O2 S1 O1 112.5(4) . . ? O2 S1 O3 112.4(4) . . ? O1 S1 O3 113.2(4) . . ? O2 S1 C1 106.0(4) . . ? O1 S1 C1 106.5(4) . . ? O3 S1 C1 105.6(3) . . ? Zn1 O1W H1W1 131(5) . . ? Zn1 O1W H1W2 116(5) . . ? H1W1 O1W H1W2 110(7) . . ? Zn1 O2W H2W1 124(5) . . ? Zn1 O2W H2W2 127(5) . . ? H2W1 O2W H2W2 110(6) . . ? Zn1 O3W H3W1 112(6) . . ? Zn1 O3W H3W2 124(6) . . ? H3W1 O3W H3W2 111(7) . . ? Zn1 O4W H4W1 113(5) . . ? Zn1 O4W H4W2 132(6) . . ? H4W1 O4W H4W2 111(8) . . ? H5W1 O5W H5W2 109(7) . . ? C12 N1 C8 116.5(6) . . ? C12 N1 Zn1 121.8(5) . . ? C8 N1 Zn1 121.5(5) . . ? C16 N2 C15 117.0(7) . . ? C22 N3 C18 115.3(6) . . ? C22 N3 Zn1 123.8(5) . . ? C18 N3 Zn1 120.8(5) . . ? C26 N4 C25 114.8(7) . . ? C6 C1 C2 120.5(8) . . ? C6 C1 S1 122.2(6) . . ? C2 C1 S1 117.2(6) . . ? C3 C2 C1 119.5(9) . . ? C3 C2 H2A 120.2 . . ? C1 C2 H2A 120.2 . . ? C2 C3 C4 121.9(8) . . ? C2 C3 H3A 119.0 . . ? C4 C3 H3A 119.0 . . ? C3 C4 C5 119.3(8) . . ? C3 C4 C7 121.8(7) . . ? C5 C4 C7 118.9(8) . . ? C6 C5 C4 118.6(8) . . ? C6 C5 H5A 120.7 . . ? C4 C5 H5A 120.7 . . ? C1 C6 C5 120.1(7) . . ? C1 C6 H6A 119.9 . . ? C5 C6 H6A 119.9 . . ? O4 C7 O5 123.4(8) . . ? O4 C7 C4 117.7(8) . . ? O5 C7 C4 118.8(8) . . ? N1 C8 C9 123.6(7) . . ? N1 C8 H8A 118.2 . . ? C9 C8 H8A 118.2 . . ? C8 C9 C10 120.7(7) . . ? C8 C9 H9A 119.7 . . ? C10 C9 H9A 119.7 . . ? C9 C10 C11 115.7(6) . . ? C9 C10 C13 122.6(6) . . ? C11 C10 C13 121.6(6) . . ? C12 C11 C10 120.3(7) . . ? C12 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? N1 C12 C11 123.1(7) . . ? N1 C12 H12A 118.5 . . ? C11 C12 H12A 118.5 . . ? C17 C13 C14 116.0(6) . . ? C17 C13 C10 122.1(6) . . ? C14 C13 C10 121.9(6) . . ? C15 C14 C13 120.0(7) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? N2 C15 C14 123.7(7) . . ? N2 C15 H15A 118.2 . . ? C14 C15 H15A 118.2 . . ? N2 C16 C17 122.9(7) . . ? N2 C16 H16A 118.6 . . ? C17 C16 H16A 118.6 . . ? C13 C17 C16 120.4(7) . . ? C13 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? N3 C18 C19 124.5(7) . . ? N3 C18 H18A 117.8 . . ? C19 C18 H18A 117.8 . . ? C18 C19 C20 119.9(7) . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C19 C20 C21 115.7(6) . . ? C19 C20 C23 122.2(6) . . ? C21 C20 C23 122.0(6) . . ? C22 C21 C20 120.1(7) . . ? C22 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? N3 C22 C21 124.3(7) . . ? N3 C22 H22A 117.9 . . ? C21 C22 H22A 117.9 . . ? C24 C23 C27 117.1(7) . . ? C24 C23 C20 121.8(6) . . ? C27 C23 C20 121.0(7) . . ? C25 C24 C23 119.0(8) . . ? C25 C24 H24A 120.5 . . ? C23 C24 H24A 120.5 . . ? N4 C25 C24 125.2(8) . . ? N4 C25 H25A 117.4 . . ? C24 C25 H25A 117.4 . . ? N4 C26 C27 125.7(8) . . ? N4 C26 H26A 117.1 . . ? C27 C26 H26A 117.1 . . ? C26 C27 C23 118.0(8) . . ? C26 C27 H27A 121.0 . . ? C23 C27 H27A 121.0 . . ? H6W1 O6W H6W2 108.3 . . ? H8W1 O8W H8W2 110(12) . . ? H7W1 O7W H7W2 108.5 . . ? 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 O2W Zn1 N1 C12 135.0(6) . . . . ? O3W Zn1 N1 C12 46.0(6) . . . . ? O1W Zn1 N1 C12 -132.9(6) . . . . ? O4W Zn1 N1 C12 -46.6(6) . . . . ? O2W Zn1 N1 C8 -39.4(5) . . . . ? O3W Zn1 N1 C8 -128.5(5) . . . . ? O1W Zn1 N1 C8 52.7(5) . . . . ? O4W Zn1 N1 C8 139.0(5) . . . . ? O2W Zn1 N3 C22 -158.5(6) . . . . ? O3W Zn1 N3 C22 -69.5(6) . . . . ? O1W Zn1 N3 C22 109.4(6) . . . . ? O4W Zn1 N3 C22 23.0(6) . . . . ? O2W Zn1 N3 C18 24.6(6) . . . . ? O3W Zn1 N3 C18 113.7(6) . . . . ? O1W Zn1 N3 C18 -67.5(6) . . . . ? O4W Zn1 N3 C18 -153.8(6) . . . . ? O2 S1 C1 C6 -128.8(6) . . . . ? O1 S1 C1 C6 -8.9(7) . . . . ? O3 S1 C1 C6 111.8(7) . . . . ? O2 S1 C1 C2 54.3(7) . . . . ? O1 S1 C1 C2 174.3(6) . . . . ? O3 S1 C1 C2 -65.1(7) . . . . ? C6 C1 C2 C3 -0.4(11) . . . . ? S1 C1 C2 C3 176.5(6) . . . . ? C1 C2 C3 C4 2.3(13) . . . . ? C2 C3 C4 C5 -2.1(12) . . . . ? C2 C3 C4 C7 178.3(8) . . . . ? C3 C4 C5 C6 0.0(11) . . . . ? C7 C4 C5 C6 179.6(7) . . . . ? C2 C1 C6 C5 -1.7(11) . . . . ? S1 C1 C6 C5 -178.5(6) . . . . ? C4 C5 C6 C1 1.9(11) . . . . ? C3 C4 C7 O4 6.6(11) . . . . ? C5 C4 C7 O4 -173.0(7) . . . . ? C3 C4 C7 O5 -171.3(7) . . . . ? C5 C4 C7 O5 9.2(11) . . . . ? C12 N1 C8 C9 -1.4(11) . . . . ? Zn1 N1 C8 C9 173.3(6) . . . . ? N1 C8 C9 C10 -0.9(12) . . . . ? C8 C9 C10 C11 2.2(10) . . . . ? C8 C9 C10 C13 -176.2(7) . . . . ? C9 C10 C11 C12 -1.2(10) . . . . ? C13 C10 C11 C12 177.2(7) . . . . ? C8 N1 C12 C11 2.4(11) . . . . ? Zn1 N1 C12 C11 -172.3(6) . . . . ? C10 C11 C12 N1 -1.1(12) . . . . ? C9 C10 C13 C17 -164.1(7) . . . . ? C11 C10 C13 C17 17.6(10) . . . . ? C9 C10 C13 C14 18.0(10) . . . . ? C11 C10 C13 C14 -160.3(7) . . . . ? C17 C13 C14 C15 -1.5(10) . . . . ? C10 C13 C14 C15 176.5(7) . . . . ? C16 N2 C15 C14 0.2(12) . . . . ? C13 C14 C15 N2 1.1(12) . . . . ? C15 N2 C16 C17 -1.1(12) . . . . ? C14 C13 C17 C16 0.7(11) . . . . ? C10 C13 C17 C16 -177.3(7) . . . . ? N2 C16 C17 C13 0.6(13) . . . . ? C22 N3 C18 C19 -4.9(11) . . . . ? Zn1 N3 C18 C19 172.2(7) . . . . ? N3 C18 C19 C20 4.2(14) . . . . ? C18 C19 C20 C21 -1.3(10) . . . . ? C18 C19 C20 C23 -177.6(7) . . . . ? C19 C20 C21 C22 -0.4(11) . . . . ? C23 C20 C21 C22 175.8(7) . . . . ? C18 N3 C22 C21 3.0(10) . . . . ? Zn1 N3 C22 C21 -174.0(6) . . . . ? C20 C21 C22 N3 -0.4(13) . . . . ? C19 C20 C23 C24 13.4(10) . . . . ? C21 C20 C23 C24 -162.7(7) . . . . ? C19 C20 C23 C27 -164.7(7) . . . . ? C21 C20 C23 C27 19.3(10) . . . . ? C27 C23 C24 C25 -4.6(11) . . . . ? C20 C23 C24 C25 177.2(6) . . . . ? C26 N4 C25 C24 0.9(12) . . . . ? C23 C24 C25 N4 2.3(12) . . . . ? C25 N4 C26 C27 -1.7(12) . . . . ? N4 C26 C27 C23 -0.7(12) . . . . ? C24 C23 C27 C26 3.9(10) . . . . ? C20 C23 C27 C26 -178.0(6) . . . . ? 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 O1W H1W1 O5W 0.85(8) 2.04(5) 2.804(8) 149(10) . O1W H1W2 N2 0.85(8) 1.96(4) 2.766(8) 157(10) 1_556 O2W H2W1 O5 0.85(8) 1.87(3) 2.689(8) 162(9) . O2W H2W2 O5W 0.85(8) 1.94(2) 2.777(8) 166(8) 1_655 O3W H3W1 O3 0.85(8) 2.02(5) 2.790(7) 151(8) 2_746 O3W H3W2 N4 0.85(8) 2.07(5) 2.812(8) 147(8) 1_554 O4W H4W1 O3 0.85(8) 2.38(8) 2.970(8) 127(8) 2_646 O4W H4W2 O6W 0.85(8) 1.86(3) 2.688(9) 167(11) . O5W H5W1 O4 0.85(8) 1.920(15) 2.769(9) 176(10) . O5W H5W2 O8W 0.85(8) 1.939(15) 2.792(10) 177(11) 1_454 O6W H6W1 O1 0.85 1.99 2.841(10) 176.1 2_746 O6W H6W2 O7W 0.85 1.72 2.570(13) 175.6 2_645 O8W H8W1 O2 0.85(8) 1.90(2) 2.742(12) 172(13) . O8W H8W2 O6W 0.85(8) 2.13(8) 2.877(11) 146(12) 2_656 O7W H7W1 O8W 0.85 2.15 3.000(14) 176.7 1_454 O7W H7W2 O5 0.85 1.73 2.579(11) 177.5 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.38 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.645 _refine_diff_density_min -0.966 _refine_diff_density_rms 0.106 #===END data_complex6 #TrackingRef '- revised cif.cif' _database_code_depnum_ccdc_archive 'CCDC 855417' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H46 Cd2 N8 O13 S2, 3(H2 O)' _chemical_formula_sum 'C54 H52 Cd2 N8 O16 S2' _chemical_formula_weight 1357.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 18.490(4) _cell_length_b 12.400(3) _cell_length_c 25.000(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.99(3) _cell_angle_gamma 90.00 _cell_volume 5451.5(19) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 19179 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 27.45 _exptl_crystal_description prim _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 0.936 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8496 _exptl_absorpt_correction_T_max 0.8960 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 26385 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12107 _reflns_number_gt 10391 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0640P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(17) _refine_ls_number_reflns 12107 _refine_ls_number_parameters 739 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0971 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.022 _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 0.445909(11) 0.13764(2) 0.265459(9) 0.02936(8) Uani 1 1 d . . . Cd2 Cd 0.569239(14) 0.37133(2) 0.738411(11) 0.03601(9) Uani 1 1 d . . . S1 S 0.34845(10) -0.37981(12) 0.47217(7) 0.0603(4) Uani 1 1 d . . . S2 S 0.14657(8) 0.63896(10) 0.06289(6) 0.0492(3) Uani 1 1 d . . . O1W O 0.6848(2) 0.3883(4) 0.72265(17) 0.0712(12) Uani 1 1 d . . . H1W1 H 0.7199 0.4016 0.7082 0.107 Uiso 1 1 d R . . H1W2 H 0.7001 0.3359 0.7458 0.107 Uiso 1 1 d R . . O1 O 0.33332(17) 0.2501(3) 0.24142(13) 0.0460(7) Uani 1 1 d . . . O2W O 0.5878(2) 0.1927(3) 0.76614(15) 0.0591(9) Uani 1 1 d . . . H2W1 H 0.5839 0.1275 0.7750 0.089 Uiso 1 1 d R . . H2W2 H 0.6121 0.2421 0.7553 0.089 Uiso 1 1 d R . . O2 O 0.42840(17) 0.3140(3) 0.21675(14) 0.0472(8) Uani 1 1 d . . . O3W O 0.53557(19) 0.5466(3) 0.70605(14) 0.0464(7) Uani 1 1 d . . . H3W1 H 0.5767 0.5136 0.7085 0.070 Uiso 1 1 d R . . H3W2 H 0.5074 0.5047 0.7178 0.070 Uiso 1 1 d R . . O3 O 0.0740(3) 0.6009(8) 0.0532(4) 0.179(5) Uani 1 1 d . . . O4 O 0.1692(3) 0.6579(5) 0.0141(2) 0.0887(16) Uani 1 1 d . . . O4W O 0.5300(3) -0.3399(4) 0.61296(18) 0.0705(11) Uani 1 1 d . . . H4W1 H 0.5444 -0.2798 0.6029 0.106 Uiso 1 1 d R . . H4W2 H 0.4994 -0.3679 0.5827 0.106 Uiso 1 1 d R . . O5 O 0.1595(6) 0.7326(5) 0.0962(3) 0.169(4) Uani 1 1 d . . . O5W O 0.2435(3) -0.3093(5) -0.1884(2) 0.0925(16) Uani 1 1 d . . . H5W1 H 0.2704 -0.2904 -0.2100 0.139 Uiso 1 1 d R . . H5W2 H 0.2546 -0.2800 -0.1563 0.139 Uiso 1 1 d R . . O6 O 0.3717(3) 0.0151(3) 0.29448(16) 0.0639(10) Uani 1 1 d . . . O6W O 0.1674(3) 0.5413(5) -0.0808(2) 0.1027(18) Uani 1 1 d . . . H6W1 H 0.1659 0.5802 -0.0532 0.154 Uiso 1 1 d R . . H6W2 H 0.1965 0.4880 -0.0682 0.154 Uiso 1 1 d R . . O7 O 0.4840(2) -0.0593(4) 0.30604(18) 0.0685(11) Uani 1 1 d . . . O8 O 0.2714(4) -0.3585(4) 0.4713(3) 0.106(2) Uani 1 1 d . . . O9 O 0.3504(4) -0.4787(4) 0.4436(3) 0.1000(17) Uani 1 1 d . . . O10 O 0.4065(5) -0.3774(6) 0.5244(2) 0.150(4) Uani 1 1 d . . . N1 N 0.4083(2) 0.0645(3) 0.17478(15) 0.0411(9) Uani 1 1 d . . . N2 N 0.3030(2) -0.2013(4) -0.08815(16) 0.0483(10) Uani 1 1 d . . . N3 N 0.4840(2) 0.1995(3) 0.35921(15) 0.0394(8) Uani 1 1 d . . . N4 N 0.5243(2) 0.3122(3) 0.64463(16) 0.0397(8) Uani 1 1 d . . . N5 N 0.5738(2) 0.1408(3) 0.26907(18) 0.0343(9) Uani 1 1 d . . . N6 N 0.9491(2) 0.1343(3) 0.25279(17) 0.0368(10) Uani 1 1 d . . . N7 N 0.6176(2) 0.4347(3) 0.83098(16) 0.0396(9) Uani 1 1 d . . . N8 N 0.6920(2) 0.6103(4) 1.11275(18) 0.0550(11) Uani 1 1 d . . . C1 C 0.3595(2) 0.3151(3) 0.21394(16) 0.0341(8) Uani 1 1 d . . . C2 C 0.3062(2) 0.3924(3) 0.17476(16) 0.0318(8) Uani 1 1 d . . . C3 C 0.3251(2) 0.4389(4) 0.13132(19) 0.0433(10) Uani 1 1 d . . . H3A H 0.3713 0.4215 0.1259 0.052 Uiso 1 1 calc R . . C4 C 0.2764(2) 0.5123(4) 0.09487(19) 0.0448(10) Uani 1 1 d . . . H4A H 0.2892 0.5422 0.0649 0.054 Uiso 1 1 calc R . . C5 C 0.2087(2) 0.5394(3) 0.10452(17) 0.0374(9) Uani 1 1 d . . . C6 C 0.1888(2) 0.4918(3) 0.14786(18) 0.0378(9) Uani 1 1 d . . . H6A H 0.1427 0.5089 0.1534 0.045 Uiso 1 1 calc R . . C7 C 0.2373(2) 0.4189(4) 0.18297(18) 0.0374(9) Uani 1 1 d . . . H7A H 0.2238 0.3874 0.2123 0.045 Uiso 1 1 calc R . . C8 C 0.4218(3) -0.0560(4) 0.31532(19) 0.0503(12) Uani 1 1 d . . . C9 C 0.4041(3) -0.1351(4) 0.3550(2) 0.0451(11) Uani 1 1 d . . . C10 C 0.3288(3) -0.1550(4) 0.3530(2) 0.0456(10) Uani 1 1 d . . . H10A H 0.2892 -0.1192 0.3268 0.055 Uiso 1 1 calc R . . C11 C 0.3130(3) -0.2284(4) 0.3900(2) 0.0445(10) Uani 1 1 d . . . H11A H 0.2629 -0.2433 0.3878 0.053 Uiso 1 1 calc R . . C12 C 0.3709(3) -0.2781(4) 0.4292(2) 0.0459(10) Uani 1 1 d . . . C13 C 0.4468(3) -0.2570(5) 0.4335(2) 0.0643(15) Uani 1 1 d . . . H13A H 0.4862 -0.2895 0.4613 0.077 Uiso 1 1 calc R . . C14 C 0.4617(3) -0.1869(5) 0.3954(2) 0.0591(14) Uani 1 1 d . . . H14A H 0.5119 -0.1743 0.3970 0.071 Uiso 1 1 calc R . . C15 C 0.3621(3) -0.0199(4) 0.16400(18) 0.0448(11) Uani 1 1 d . . . H15A H 0.3444 -0.0454 0.1926 0.054 Uiso 1 1 calc R . . C16 C 0.3389(3) -0.0719(4) 0.11315(19) 0.0441(10) Uani 1 1 d . . . H16A H 0.3048 -0.1292 0.1075 0.053 Uiso 1 1 calc R . . C17 C 0.3666(3) -0.0384(4) 0.07010(18) 0.0388(10) Uani 1 1 d . . . C18 C 0.4150(3) 0.0472(5) 0.0815(2) 0.0556(13) Uani 1 1 d . . . H18A H 0.4356 0.0722 0.0543 0.067 Uiso 1 1 calc R . . C19 C 0.4339(3) 0.0973(5) 0.1337(2) 0.0607(15) Uani 1 1 d . . . H19A H 0.4661 0.1568 0.1400 0.073 Uiso 1 1 calc R . . C20 C 0.3002(3) -0.2507(4) -0.0413(2) 0.0514(11) Uani 1 1 d . . . H20A H 0.2842 -0.3222 -0.0437 0.062 Uiso 1 1 calc R . . C21 C 0.3198(3) -0.2004(4) 0.01012(19) 0.0439(10) Uani 1 1 d . . . H21A H 0.3162 -0.2370 0.0417 0.053 Uiso 1 1 calc R . . C22 C 0.3450(2) -0.0948(4) 0.01445(19) 0.0381(9) Uani 1 1 d . . . C23 C 0.3490(3) -0.0457(4) -0.0333(2) 0.0461(10) Uani 1 1 d . . . H23A H 0.3662 0.0250 -0.0320 0.055 Uiso 1 1 calc R . . C24 C 0.3272(3) -0.1015(5) -0.0839(2) 0.0517(12) Uani 1 1 d . . . H24A H 0.3299 -0.0665 -0.1161 0.062 Uiso 1 1 calc R . . C25 C 0.5230(4) 0.1355(4) 0.3995(3) 0.0527(16) Uani 1 1 d . . . H25A H 0.5441 0.0732 0.3898 0.063 Uiso 1 1 calc R . . C26 C 0.5344(3) 0.1566(5) 0.4566(2) 0.0519(14) Uani 1 1 d . . . H26A H 0.5627 0.1089 0.4838 0.062 Uiso 1 1 calc R . . C27 C 0.5038(2) 0.2476(4) 0.47249(17) 0.0351(9) Uani 1 1 d . . . C28 C 0.4641(3) 0.3158(4) 0.42921(19) 0.0418(10) Uani 1 1 d . . . H28A H 0.4435 0.3797 0.4375 0.050 Uiso 1 1 calc R . . C29 C 0.4554(3) 0.2893(4) 0.3742(2) 0.0456(11) Uani 1 1 d . . . H29A H 0.4282 0.3360 0.3460 0.055 Uiso 1 1 calc R . . C30 C 0.5495(3) 0.2213(4) 0.6292(2) 0.0453(12) Uani 1 1 d . . . H30A H 0.5729 0.1716 0.6570 0.054 Uiso 1 1 calc R . . C31 C 0.5433(3) 0.1961(4) 0.5745(2) 0.0491(12) Uani 1 1 d . . . H31A H 0.5615 0.1305 0.5660 0.059 Uiso 1 1 calc R . . C32 C 0.5097(2) 0.2693(4) 0.53194(17) 0.0338(9) Uani 1 1 d . . . C33 C 0.4810(3) 0.3631(4) 0.5483(2) 0.0426(12) Uani 1 1 d . . . H33A H 0.4565 0.4138 0.5214 0.051 Uiso 1 1 calc R . . C34 C 0.4885(3) 0.3808(4) 0.6027(2) 0.0418(12) Uani 1 1 d . . . H34A H 0.4679 0.4438 0.6121 0.050 Uiso 1 1 calc R . . C35 C 0.6268(2) 0.0748(4) 0.30134(19) 0.0437(10) Uani 1 1 d . . . H35A H 0.6130 0.0278 0.3255 0.052 Uiso 1 1 calc R . . C36 C 0.7012(2) 0.0736(4) 0.3004(2) 0.0473(11) Uani 1 1 d . . . H36A H 0.7359 0.0254 0.3230 0.057 Uiso 1 1 calc R . . C37 C 0.7239(2) 0.1434(3) 0.26608(18) 0.0349(9) Uani 1 1 d . . . C38 C 0.6693(3) 0.2131(4) 0.2334(2) 0.0481(11) Uani 1 1 d . . . H38A H 0.6823 0.2628 0.2100 0.058 Uiso 1 1 calc R . . C39 C 0.5968(2) 0.2084(4) 0.2355(2) 0.0462(11) Uani 1 1 d . . . H39A H 0.5610 0.2547 0.2124 0.055 Uiso 1 1 calc R . . C40 C 0.9313(3) 0.0848(4) 0.2937(2) 0.0465(11) Uani 1 1 d . . . H40A H 0.9694 0.0465 0.3199 0.056 Uiso 1 1 calc R . . C41 C 0.8605(2) 0.0862(4) 0.3003(2) 0.0427(10) Uani 1 1 d . . . H41A H 0.8514 0.0501 0.3302 0.051 Uiso 1 1 calc R . . C42 C 0.8026(2) 0.1419(3) 0.26191(19) 0.0321(9) Uani 1 1 d . . . C43 C 0.8209(3) 0.1945(4) 0.2189(2) 0.0480(11) Uani 1 1 d . . . H43A H 0.7839 0.2332 0.1920 0.058 Uiso 1 1 calc R . . C44 C 0.8935(3) 0.1894(4) 0.2161(2) 0.0454(10) Uani 1 1 d . . . H44A H 0.9047 0.2261 0.1871 0.055 Uiso 1 1 calc R . . C45 C 0.6246(3) 0.3657(4) 0.8737(2) 0.0424(11) Uani 1 1 d . . . H45A H 0.6195 0.2923 0.8658 0.051 Uiso 1 1 calc R . . C46 C 0.6390(3) 0.3985(4) 0.92854(19) 0.0427(10) Uani 1 1 d . . . H46A H 0.6433 0.3476 0.9567 0.051 Uiso 1 1 calc R . . C47 C 0.6471(2) 0.5069(4) 0.94195(17) 0.0370(10) Uani 1 1 d . . . C48 C 0.6407(3) 0.5782(4) 0.89812(19) 0.0436(10) Uani 1 1 d . . . H48A H 0.6465 0.6519 0.9050 0.052 Uiso 1 1 calc R . . C49 C 0.6256(3) 0.5389(4) 0.84372(19) 0.0454(11) Uani 1 1 d . . . H49A H 0.6208 0.5881 0.8147 0.055 Uiso 1 1 calc R . . C50 C 0.6574(3) 0.5170(5) 1.0938(2) 0.0560(12) Uani 1 1 d . . . H50A H 0.6427 0.4739 1.1191 0.067 Uiso 1 1 calc R . . C51 C 0.6421(3) 0.4808(5) 1.0401(2) 0.0508(11) Uani 1 1 d . . . H51A H 0.6182 0.4147 1.0295 0.061 Uiso 1 1 calc R . . C52 C 0.6630(2) 0.5440(4) 1.00131(19) 0.0401(9) Uani 1 1 d . . . C53 C 0.7001(3) 0.6396(4) 1.0211(2) 0.0506(12) Uani 1 1 d . . . H53A H 0.7174 0.6832 0.9973 0.061 Uiso 1 1 calc R . . C54 C 0.7114(3) 0.6700(5) 1.0756(2) 0.0607(14) Uani 1 1 d . . . H54A H 0.7341 0.7365 1.0872 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03271(16) 0.03068(15) 0.02598(15) 0.00030(12) 0.01096(11) -0.00027(12) Cd2 0.03951(18) 0.0445(2) 0.02695(16) -0.00246(13) 0.01456(13) 0.00231(13) S1 0.0816(10) 0.0498(8) 0.0565(9) 0.0187(6) 0.0314(8) 0.0022(6) S2 0.0506(7) 0.0523(8) 0.0461(7) 0.0155(5) 0.0169(5) 0.0161(5) O1W 0.045(2) 0.123(4) 0.050(2) 0.019(2) 0.0213(17) 0.016(2) O1 0.0449(17) 0.0467(19) 0.0468(17) 0.0103(14) 0.0147(13) 0.0060(13) O2W 0.078(2) 0.047(2) 0.052(2) 0.0050(16) 0.0197(17) 0.0096(17) O2 0.0377(17) 0.0393(18) 0.062(2) 0.0098(15) 0.0110(15) 0.0069(12) O3W 0.0537(19) 0.0412(19) 0.0497(19) 0.0019(14) 0.0238(14) 0.0050(14) O3 0.044(3) 0.235(8) 0.243(9) 0.180(8) 0.021(4) 0.026(4) O4 0.108(4) 0.094(4) 0.072(3) 0.038(3) 0.041(3) 0.044(3) O4W 0.091(3) 0.061(2) 0.065(3) 0.008(2) 0.033(2) -0.009(2) O5 0.284(10) 0.087(4) 0.093(4) 0.004(3) -0.004(5) 0.113(6) O5W 0.080(3) 0.128(5) 0.067(3) -0.043(3) 0.018(2) -0.012(3) O6 0.100(3) 0.049(2) 0.051(2) 0.0039(17) 0.0359(19) -0.014(2) O6W 0.088(3) 0.117(5) 0.093(4) -0.048(3) 0.013(3) -0.021(3) O7 0.078(3) 0.075(3) 0.062(3) -0.007(2) 0.036(2) -0.029(2) O8 0.120(5) 0.083(4) 0.156(6) 0.050(3) 0.102(4) 0.026(3) O9 0.150(5) 0.043(3) 0.131(5) 0.018(3) 0.079(4) 0.001(3) O10 0.178(7) 0.176(7) 0.064(3) 0.059(4) -0.008(4) -0.083(5) N1 0.052(2) 0.041(2) 0.0277(19) -0.0016(15) 0.0089(15) -0.0038(16) N2 0.049(2) 0.057(3) 0.039(2) -0.0140(18) 0.0144(17) -0.0076(18) N3 0.040(2) 0.051(2) 0.0258(18) 0.0010(16) 0.0091(15) 0.0042(16) N4 0.048(2) 0.040(2) 0.033(2) -0.0053(16) 0.0151(15) 0.0035(16) N5 0.033(2) 0.041(2) 0.030(2) 0.0012(14) 0.0113(15) -0.0011(13) N6 0.037(2) 0.045(2) 0.033(2) 0.0017(14) 0.0160(16) 0.0002(14) N7 0.0344(19) 0.053(3) 0.034(2) -0.0035(16) 0.0129(14) -0.0002(15) N8 0.051(2) 0.076(3) 0.037(2) -0.015(2) 0.0128(19) -0.005(2) C1 0.036(2) 0.030(2) 0.0334(19) -0.0010(15) 0.0058(15) 0.0062(15) C2 0.0302(19) 0.033(2) 0.0291(18) -0.0007(15) 0.0039(15) -0.0006(14) C3 0.039(2) 0.052(3) 0.044(2) 0.0009(19) 0.0198(17) 0.0024(18) C4 0.048(3) 0.050(3) 0.039(2) 0.0043(19) 0.017(2) 0.0048(19) C5 0.039(2) 0.033(2) 0.036(2) 0.0005(16) 0.0057(17) 0.0049(16) C6 0.034(2) 0.036(2) 0.044(2) -0.0002(17) 0.0133(16) 0.0031(15) C7 0.038(2) 0.036(2) 0.039(2) 0.0004(17) 0.0134(17) 0.0006(16) C8 0.079(3) 0.040(3) 0.034(2) -0.0059(19) 0.022(2) -0.020(2) C9 0.062(3) 0.039(3) 0.041(2) -0.0024(17) 0.025(2) -0.0153(18) C10 0.064(3) 0.036(2) 0.038(2) 0.0029(18) 0.018(2) -0.001(2) C11 0.052(3) 0.038(3) 0.050(3) 0.0001(19) 0.026(2) 0.0000(19) C12 0.063(3) 0.035(3) 0.047(3) 0.0029(19) 0.028(2) 0.0010(19) C13 0.062(3) 0.069(4) 0.057(3) 0.019(3) 0.010(2) -0.002(2) C14 0.042(3) 0.073(4) 0.062(3) 0.009(3) 0.015(2) -0.006(2) C15 0.056(3) 0.046(3) 0.032(2) 0.0033(18) 0.0136(19) -0.013(2) C16 0.055(3) 0.040(3) 0.036(2) -0.0014(18) 0.0132(19) -0.0098(19) C17 0.045(2) 0.041(3) 0.032(2) -0.0024(17) 0.0129(17) 0.0011(17) C18 0.072(3) 0.063(3) 0.039(2) -0.011(2) 0.029(2) -0.029(3) C19 0.078(4) 0.065(3) 0.042(3) -0.015(2) 0.023(3) -0.036(3) C20 0.059(3) 0.049(3) 0.049(3) -0.008(2) 0.021(2) -0.008(2) C21 0.052(3) 0.042(3) 0.038(2) -0.0048(18) 0.0151(18) -0.0078(19) C22 0.036(2) 0.040(2) 0.041(2) -0.0050(19) 0.0144(17) 0.0024(17) C23 0.062(3) 0.042(3) 0.039(2) -0.0052(19) 0.023(2) -0.005(2) C24 0.063(3) 0.064(3) 0.030(2) -0.004(2) 0.017(2) 0.000(2) C25 0.060(4) 0.056(4) 0.037(3) -0.013(2) 0.008(3) 0.022(2) C26 0.059(3) 0.060(3) 0.029(2) -0.008(2) 0.002(2) 0.025(2) C27 0.034(2) 0.040(2) 0.029(2) -0.0056(16) 0.0072(17) 0.0015(16) C28 0.056(3) 0.037(3) 0.033(2) -0.0022(18) 0.015(2) 0.0077(19) C29 0.054(3) 0.046(3) 0.037(3) 0.000(2) 0.014(2) 0.007(2) C30 0.062(3) 0.047(3) 0.026(2) 0.0037(19) 0.014(2) 0.011(2) C31 0.061(3) 0.044(3) 0.042(3) -0.004(2) 0.016(2) 0.013(2) C32 0.038(2) 0.037(2) 0.028(2) -0.0082(16) 0.0117(17) -0.0003(16) C33 0.055(3) 0.035(3) 0.036(3) -0.0033(17) 0.011(2) 0.0088(17) C34 0.055(3) 0.036(3) 0.035(3) -0.0035(17) 0.016(2) 0.0102(19) C35 0.040(2) 0.049(3) 0.044(2) 0.0115(19) 0.0170(18) -0.0021(18) C36 0.040(2) 0.054(3) 0.050(3) 0.015(2) 0.0173(19) 0.0026(19) C37 0.040(2) 0.039(2) 0.030(2) -0.0020(16) 0.0180(19) -0.0034(15) C38 0.047(2) 0.046(3) 0.059(3) 0.015(2) 0.027(2) 0.0027(19) C39 0.039(2) 0.039(3) 0.061(3) 0.016(2) 0.018(2) 0.0056(17) C40 0.035(2) 0.058(3) 0.047(3) 0.007(2) 0.0148(18) 0.0021(19) C41 0.035(2) 0.050(3) 0.048(2) 0.016(2) 0.0201(18) 0.0059(18) C42 0.032(2) 0.038(2) 0.029(2) -0.0040(16) 0.0141(17) -0.0044(15) C43 0.042(2) 0.061(3) 0.046(3) 0.012(2) 0.0200(19) 0.011(2) C44 0.045(2) 0.054(3) 0.043(2) 0.014(2) 0.0229(18) 0.0084(19) C45 0.041(3) 0.049(3) 0.034(2) -0.0050(17) 0.0066(19) 0.0028(17) C46 0.045(2) 0.050(3) 0.033(2) 0.0035(19) 0.0129(18) 0.0041(19) C47 0.029(2) 0.053(3) 0.028(2) -0.0029(18) 0.0095(15) -0.0020(17) C48 0.048(2) 0.041(3) 0.042(2) -0.0061(19) 0.0153(19) -0.0066(18) C49 0.045(3) 0.056(3) 0.037(2) 0.007(2) 0.0157(19) -0.004(2) C50 0.066(3) 0.067(4) 0.042(3) 0.000(2) 0.027(2) -0.003(2) C51 0.049(3) 0.065(3) 0.040(2) -0.007(2) 0.0159(19) -0.011(2) C52 0.037(2) 0.048(3) 0.038(2) -0.0055(19) 0.0144(17) -0.0038(18) C53 0.060(3) 0.054(3) 0.038(3) -0.009(2) 0.015(2) -0.014(2) C54 0.068(3) 0.069(4) 0.048(3) -0.020(3) 0.022(3) -0.018(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 O6 2.310(4) . ? Cd1 N1 2.339(4) . ? Cd1 N5 2.339(4) . ? Cd1 N3 2.358(4) . ? Cd1 O1 2.422(3) . ? Cd1 O2 2.475(3) . ? Cd2 O1W 2.300(4) . ? Cd2 O2W 2.314(4) . ? Cd2 O3W 2.336(3) . ? Cd2 N7 2.344(4) . ? Cd2 N4 2.350(4) . ? Cd2 N6 2.359(4) 4_455 ? Cd2 H2W2 1.7797 . ? Cd2 H3W1 1.9376 . ? Cd2 H3W2 1.9855 . ? S1 O10 1.412(6) . ? S1 O9 1.424(5) . ? S1 O8 1.443(6) . ? S1 C12 1.786(5) . ? S2 O3 1.371(6) . ? S2 O5 1.406(7) . ? S2 O4 1.426(5) . ? S2 C5 1.785(4) . ? O1W H1W1 0.8507 . ? O1W H1W2 0.8579 . ? O1 C1 1.249(5) . ? O2W H2W1 0.8472 . ? O2W H2W2 0.8514 . ? O2 C1 1.255(5) . ? O3W H3W1 0.8500 . ? O3W H3W2 0.8499 . ? O4W H4W1 0.8547 . ? O4W H4W2 0.8658 . ? O5W H5W1 0.8705 . ? O5W H5W2 0.8479 . ? O6 C8 1.268(7) . ? O6W H6W1 0.8500 . ? O6W H6W2 0.8500 . ? O7 C8 1.242(6) . ? N1 C19 1.322(6) . ? N1 C15 1.325(6) . ? N2 C24 1.309(7) . ? N2 C20 1.336(7) . ? N3 C25 1.311(7) . ? N3 C29 1.335(6) . ? N4 C30 1.323(6) . ? N4 C34 1.353(6) . ? N5 C35 1.339(6) . ? N5 C39 1.344(6) . ? N6 C40 1.319(6) . ? N6 C44 1.335(6) . ? N6 Cd2 2.359(4) 4_554 ? N7 C49 1.328(7) . ? N7 C45 1.343(6) . ? N8 C54 1.322(8) . ? N8 C50 1.336(7) . ? C1 C2 1.500(5) . ? C2 C3 1.367(6) . ? C2 C7 1.391(6) . ? C3 C4 1.401(6) . ? C3 H3A 0.9300 . ? C4 C5 1.388(6) . ? C4 H4A 0.9300 . ? C5 C6 1.380(6) . ? C6 C7 1.380(6) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.502(6) . ? C9 C14 1.379(8) . ? C9 C10 1.400(7) . ? C10 C11 1.392(7) . ? C10 H10A 0.9300 . ? C11 C12 1.357(7) . ? C11 H11A 0.9300 . ? C12 C13 1.398(7) . ? C13 C14 1.379(8) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C16 1.371(6) . ? C15 H15A 0.9300 . ? C16 C17 1.391(6) . ? C16 H16A 0.9300 . ? C17 C18 1.361(7) . ? C17 C22 1.497(6) . ? C18 C19 1.387(7) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.374(7) . ? C20 H20A 0.9300 . ? C21 C22 1.383(7) . ? C21 H21A 0.9300 . ? C22 C23 1.361(7) . ? C23 C24 1.388(7) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C26 1.401(8) . ? C25 H25A 0.9300 . ? C26 C27 1.375(7) . ? C26 H26A 0.9300 . ? C27 C28 1.391(6) . ? C27 C32 1.481(5) . ? C28 C29 1.375(7) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C30 C31 1.371(7) . ? C30 H30A 0.9300 . ? C31 C32 1.391(7) . ? C31 H31A 0.9300 . ? C32 C33 1.391(6) . ? C33 C34 1.341(8) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C35 C36 1.383(6) . ? C35 H35A 0.9300 . ? C36 C37 1.371(6) . ? C36 H36A 0.9300 . ? C37 C38 1.387(6) . ? C37 C42 1.492(5) . ? C38 C39 1.359(6) . ? C38 H38A 0.9300 . ? C39 H39A 0.9300 . ? C40 C41 1.369(6) . ? C40 H40A 0.9300 . ? C41 C42 1.381(6) . ? C41 H41A 0.9300 . ? C42 C43 1.386(6) . ? C43 C44 1.367(6) . ? C43 H43A 0.9300 . ? C44 H44A 0.9300 . ? C45 C46 1.375(7) . ? C45 H45A 0.9300 . ? C46 C47 1.383(7) . ? C46 H46A 0.9300 . ? C47 C48 1.384(6) . ? C47 C52 1.494(6) . ? C48 C49 1.389(7) . ? C48 H48A 0.9300 . ? C49 H49A 0.9300 . ? C50 C51 1.360(7) . ? C50 H50A 0.9300 . ? C51 C52 1.391(7) . ? C51 H51A 0.9300 . ? C52 C53 1.383(7) . ? C53 C54 1.365(7) . ? C53 H53A 0.9300 . ? C54 H54A 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 N1 91.24(14) . . ? O6 Cd1 N5 133.69(14) . . ? N1 Cd1 N5 92.20(14) . . ? O6 Cd1 N3 85.76(14) . . ? N1 Cd1 N3 176.17(13) . . ? N5 Cd1 N3 88.16(14) . . ? O6 Cd1 O1 84.73(14) . . ? N1 Cd1 O1 90.42(13) . . ? N5 Cd1 O1 141.37(12) . . ? N3 Cd1 O1 91.68(12) . . ? O6 Cd1 O2 137.37(13) . . ? N1 Cd1 O2 84.91(13) . . ? N5 Cd1 O2 88.92(11) . . ? N3 Cd1 O2 98.91(13) . . ? O1 Cd1 O2 52.95(10) . . ? O1W Cd2 O2W 94.55(16) . . ? O1W Cd2 O3W 91.01(14) . . ? O2W Cd2 O3W 173.36(13) . . ? O1W Cd2 N7 92.70(14) . . ? O2W Cd2 N7 92.81(14) . . ? O3W Cd2 N7 90.55(14) . . ? O1W Cd2 N4 85.35(15) . . ? O2W Cd2 N4 88.54(13) . . ? O3W Cd2 N4 88.29(13) . . ? N7 Cd2 N4 177.71(14) . . ? O1W Cd2 N6 176.28(16) . 4_455 ? O2W Cd2 N6 89.17(14) . 4_455 ? O3W Cd2 N6 85.27(13) . 4_455 ? N7 Cd2 N6 87.12(13) . 4_455 ? N4 Cd2 N6 94.75(14) . 4_455 ? O1W Cd2 H2W2 75.8 . . ? O2W Cd2 H2W2 18.8 . . ? O3W Cd2 H2W2 166.3 . . ? N7 Cd2 H2W2 93.5 . . ? N4 Cd2 H2W2 87.2 . . ? N6 Cd2 H2W2 108.0 4_455 . ? O1W Cd2 H3W1 70.7 . . ? O2W Cd2 H3W1 164.8 . . ? O3W Cd2 H3W1 20.3 . . ? N7 Cd2 H3W1 91.4 . . ? N4 Cd2 H3W1 86.8 . . ? N6 Cd2 H3W1 105.6 4_455 . ? H2W2 Cd2 H3W1 146.3 . . ? O1W Cd2 H3W2 111.7 . . ? O2W Cd2 H3W2 153.5 . . ? O3W Cd2 H3W2 20.7 . . ? N7 Cd2 H3W2 89.5 . . ? N4 Cd2 H3W2 90.1 . . ? N6 Cd2 H3W2 64.6 4_455 . ? H2W2 Cd2 H3W2 171.8 . . ? H3W1 Cd2 H3W2 41.0 . . ? O10 S1 O9 110.7(5) . . ? O10 S1 O8 118.3(5) . . ? O9 S1 O8 109.1(4) . . ? O10 S1 C12 106.9(3) . . ? O9 S1 C12 105.1(3) . . ? O8 S1 C12 105.9(3) . . ? O3 S2 O5 111.6(7) . . ? O3 S2 O4 115.8(5) . . ? O5 S2 O4 109.2(5) . . ? O3 S2 C5 106.5(3) . . ? O5 S2 C5 105.3(3) . . ? O4 S2 C5 107.9(2) . . ? Cd2 O1W H1W1 164.1 . . ? Cd2 O1W H1W2 86.9 . . ? H1W1 O1W H1W2 107.2 . . ? C1 O1 Cd1 93.4(2) . . ? Cd2 O2W H2W1 167.1 . . ? H2W1 O2W H2W2 149.9 . . ? C1 O2 Cd1 90.8(2) . . ? Cd2 O3W H3W1 52.4 . . ? Cd2 O3W H3W2 55.7 . . ? H3W1 O3W H3W2 108.1 . . ? H4W1 O4W H4W2 105.9 . . ? H5W1 O5W H5W2 117.0 . . ? C8 O6 Cd1 99.0(3) . . ? H6W1 O6W H6W2 108.3 . . ? C19 N1 C15 116.6(4) . . ? C19 N1 Cd1 124.3(3) . . ? C15 N1 Cd1 118.9(3) . . ? C24 N2 C20 117.8(4) . . ? C25 N3 C29 117.5(4) . . ? C25 N3 Cd1 119.5(3) . . ? C29 N3 Cd1 121.8(3) . . ? C30 N4 C34 116.2(4) . . ? C30 N4 Cd2 120.6(3) . . ? C34 N4 Cd2 121.0(3) . . ? C35 N5 C39 116.4(4) . . ? C35 N5 Cd1 123.8(3) . . ? C39 N5 Cd1 119.8(3) . . ? C40 N6 C44 116.7(4) . . ? C40 N6 Cd2 125.2(3) . 4_554 ? C44 N6 Cd2 118.1(3) . 4_554 ? C49 N7 C45 116.9(4) . . ? C49 N7 Cd2 122.9(3) . . ? C45 N7 Cd2 119.0(3) . . ? C54 N8 C50 116.1(5) . . ? O1 C1 O2 121.4(4) . . ? O1 C1 C2 118.9(4) . . ? O2 C1 C2 119.6(4) . . ? C3 C2 C7 119.2(4) . . ? C3 C2 C1 120.7(4) . . ? C7 C2 C1 120.1(4) . . ? C2 C3 C4 121.3(4) . . ? C2 C3 H3A 119.3 . . ? C4 C3 H3A 119.3 . . ? C5 C4 C3 118.5(4) . . ? C5 C4 H4A 120.7 . . ? C3 C4 H4A 120.7 . . ? C6 C5 C4 120.4(4) . . ? C6 C5 S2 118.3(3) . . ? C4 C5 S2 121.2(3) . . ? C5 C6 C7 120.1(4) . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C6 C7 C2 120.4(4) . . ? C6 C7 H7A 119.8 . . ? C2 C7 H7A 119.8 . . ? O7 C8 O6 123.2(5) . . ? O7 C8 C9 120.3(5) . . ? O6 C8 C9 116.4(5) . . ? C14 C9 C10 118.6(4) . . ? C14 C9 C8 120.8(5) . . ? C10 C9 C8 120.6(5) . . ? C11 C10 C9 120.1(4) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C12 C11 C10 119.8(5) . . ? C12 C11 H11A 120.1 . . ? C10 C11 H11A 120.1 . . ? C11 C12 C13 121.3(5) . . ? C11 C12 S1 118.5(4) . . ? C13 C12 S1 120.0(4) . . ? C14 C13 C12 118.4(5) . . ? C14 C13 H13A 120.8 . . ? C12 C13 H13A 120.8 . . ? C13 C14 C9 121.7(5) . . ? C13 C14 H14A 119.2 . . ? C9 C14 H14A 119.2 . . ? N1 C15 C16 123.9(4) . . ? N1 C15 H15A 118.1 . . ? C16 C15 H15A 118.1 . . ? C15 C16 C17 119.5(4) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C18 C17 C16 116.5(4) . . ? C18 C17 C22 121.9(4) . . ? C16 C17 C22 121.5(4) . . ? C17 C18 C19 120.3(5) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? N1 C19 C18 123.1(4) . . ? N1 C19 H19A 118.4 . . ? C18 C19 H19A 118.4 . . ? N2 C20 C21 122.8(5) . . ? N2 C20 H20A 118.6 . . ? C21 C20 H20A 118.6 . . ? C20 C21 C22 119.2(5) . . ? C20 C21 H21A 120.4 . . ? C22 C21 H21A 120.4 . . ? C23 C22 C21 117.6(4) . . ? C23 C22 C17 122.3(4) . . ? C21 C22 C17 120.1(4) . . ? C22 C23 C24 119.8(5) . . ? C22 C23 H23A 120.1 . . ? C24 C23 H23A 120.1 . . ? N2 C24 C23 122.7(5) . . ? N2 C24 H24A 118.6 . . ? C23 C24 H24A 118.6 . . ? N3 C25 C26 122.9(5) . . ? N3 C25 H25A 118.5 . . ? C26 C25 H25A 118.5 . . ? C27 C26 C25 120.1(5) . . ? C27 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C26 C27 C28 116.1(4) . . ? C26 C27 C32 122.0(4) . . ? C28 C27 C32 121.9(4) . . ? C29 C28 C27 120.2(4) . . ? C29 C28 H28A 119.9 . . ? C27 C28 H28A 119.9 . . ? N3 C29 C28 123.1(5) . . ? N3 C29 H29A 118.5 . . ? C28 C29 H29A 118.5 . . ? N4 C30 C31 123.8(5) . . ? N4 C30 H30A 118.1 . . ? C31 C30 H30A 118.1 . . ? C30 C31 C32 119.6(5) . . ? C30 C31 H31A 120.2 . . ? C32 C31 H31A 120.2 . . ? C33 C32 C31 116.2(4) . . ? C33 C32 C27 122.1(4) . . ? C31 C32 C27 121.8(4) . . ? C34 C33 C32 120.4(5) . . ? C34 C33 H33A 119.8 . . ? C32 C33 H33A 119.8 . . ? C33 C34 N4 123.8(4) . . ? C33 C34 H34A 118.1 . . ? N4 C34 H34A 118.1 . . ? N5 C35 C36 122.9(4) . . ? N5 C35 H35A 118.6 . . ? C36 C35 H35A 118.6 . . ? C37 C36 C35 120.1(4) . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C36 C37 C38 117.0(4) . . ? C36 C37 C42 121.9(4) . . ? C38 C37 C42 121.0(4) . . ? C39 C38 C37 119.8(4) . . ? C39 C38 H38A 120.1 . . ? C37 C38 H38A 120.1 . . ? N5 C39 C38 123.8(4) . . ? N5 C39 H39A 118.1 . . ? C38 C39 H39A 118.1 . . ? N6 C40 C41 124.3(4) . . ? N6 C40 H40A 117.9 . . ? C41 C40 H40A 117.9 . . ? C40 C41 C42 119.2(4) . . ? C40 C41 H41A 120.4 . . ? C42 C41 H41A 120.4 . . ? C41 C42 C43 116.9(4) . . ? C41 C42 C37 121.4(4) . . ? C43 C42 C37 121.7(4) . . ? C44 C43 C42 119.8(4) . . ? C44 C43 H43A 120.1 . . ? C42 C43 H43A 120.1 . . ? N6 C44 C43 123.2(4) . . ? N6 C44 H44A 118.4 . . ? C43 C44 H44A 118.4 . . ? N7 C45 C46 123.1(4) . . ? N7 C45 H45A 118.5 . . ? C46 C45 H45A 118.5 . . ? C45 C46 C47 120.2(4) . . ? C45 C46 H46A 119.9 . . ? C47 C46 H46A 119.9 . . ? C46 C47 C48 116.9(4) . . ? C46 C47 C52 120.9(4) . . ? C48 C47 C52 122.2(4) . . ? C47 C48 C49 119.6(4) . . ? C47 C48 H48A 120.2 . . ? C49 C48 H48A 120.2 . . ? N7 C49 C48 123.3(4) . . ? N7 C49 H49A 118.3 . . ? C48 C49 H49A 118.3 . . ? N8 C50 C51 124.5(5) . . ? N8 C50 H50A 117.8 . . ? C51 C50 H50A 117.8 . . ? C50 C51 C52 119.0(5) . . ? C50 C51 H51A 120.5 . . ? C52 C51 H51A 120.5 . . ? C53 C52 C51 116.6(4) . . ? C53 C52 C47 122.9(4) . . ? C51 C52 C47 120.5(4) . . ? C54 C53 C52 119.9(5) . . ? C54 C53 H53A 120.0 . . ? C52 C53 H53A 120.0 . . ? N8 C54 C53 123.8(5) . . ? N8 C54 H54A 118.1 . . ? C53 C54 H54A 118.1 . . ? 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 O6 Cd1 O1 C1 -167.7(3) . . . . ? N1 Cd1 O1 C1 -76.5(3) . . . . ? N5 Cd1 O1 C1 17.6(4) . . . . ? N3 Cd1 O1 C1 106.7(3) . . . . ? O2 Cd1 O1 C1 6.8(2) . . . . ? O6 Cd1 O2 C1 1.3(3) . . . . ? N1 Cd1 O2 C1 87.6(2) . . . . ? N5 Cd1 O2 C1 179.9(3) . . . . ? N3 Cd1 O2 C1 -92.1(2) . . . . ? O1 Cd1 O2 C1 -6.8(2) . . . . ? N1 Cd1 O6 C8 95.0(3) . . . . ? N5 Cd1 O6 C8 0.8(4) . . . . ? N3 Cd1 O6 C8 -82.6(3) . . . . ? O1 Cd1 O6 C8 -174.7(3) . . . . ? O2 Cd1 O6 C8 178.8(3) . . . . ? O6 Cd1 N1 C19 -177.4(5) . . . . ? O1 Cd1 N1 C19 97.8(5) . . . . ? O2 Cd1 N1 C19 45.1(5) . . . . ? O6 Cd1 N1 C15 -2.0(4) . . . . ? N5 Cd1 N1 C15 131.8(4) . . . . ? O1 Cd1 N1 C15 -86.7(4) . . . . ? O2 Cd1 N1 C15 -139.5(4) . . . . ? O6 Cd1 N3 C25 65.2(5) . . . . ? N5 Cd1 N3 C25 -68.9(5) . . . . ? O1 Cd1 N3 C25 149.7(5) . . . . ? O2 Cd1 N3 C25 -157.5(4) . . . . ? O6 Cd1 N3 C29 -101.8(4) . . . . ? N5 Cd1 N3 C29 124.1(4) . . . . ? O1 Cd1 N3 C29 -17.2(4) . . . . ? O2 Cd1 N3 C29 35.5(4) . . . . ? O1W Cd2 N4 C30 65.1(4) . . . . ? O2W Cd2 N4 C30 -29.6(4) . . . . ? O3W Cd2 N4 C30 156.2(4) . . . . ? N6 Cd2 N4 C30 -118.7(4) 4_455 . . . ? O1W Cd2 N4 C34 -97.3(4) . . . . ? O2W Cd2 N4 C34 168.0(4) . . . . ? O3W Cd2 N4 C34 -6.2(4) . . . . ? N6 Cd2 N4 C34 79.0(4) 4_455 . . . ? O6 Cd1 N5 C35 -15.1(5) . . . . ? N1 Cd1 N5 C35 -108.9(4) . . . . ? N3 Cd1 N5 C35 67.3(4) . . . . ? O1 Cd1 N5 C35 157.7(3) . . . . ? O2 Cd1 N5 C35 166.2(4) . . . . ? O6 Cd1 N5 C39 161.8(3) . . . . ? N1 Cd1 N5 C39 68.0(4) . . . . ? N3 Cd1 N5 C39 -115.9(4) . . . . ? O1 Cd1 N5 C39 -25.5(5) . . . . ? O2 Cd1 N5 C39 -16.9(4) . . . . ? O1W Cd2 N7 C49 82.2(4) . . . . ? O2W Cd2 N7 C49 176.9(4) . . . . ? O3W Cd2 N7 C49 -8.8(3) . . . . ? N6 Cd2 N7 C49 -94.1(4) 4_455 . . . ? O1W Cd2 N7 C45 -110.4(4) . . . . ? O2W Cd2 N7 C45 -15.7(4) . . . . ? O3W Cd2 N7 C45 158.5(3) . . . . ? N6 Cd2 N7 C45 73.3(3) 4_455 . . . ? Cd1 O1 C1 O2 -12.7(4) . . . . ? Cd1 O1 C1 C2 164.4(3) . . . . ? Cd1 O2 C1 O1 12.4(4) . . . . ? Cd1 O2 C1 C2 -164.7(3) . . . . ? O1 C1 C2 C3 -158.4(4) . . . . ? O2 C1 C2 C3 18.7(6) . . . . ? O1 C1 C2 C7 22.8(6) . . . . ? O2 C1 C2 C7 -160.1(4) . . . . ? C7 C2 C3 C4 -0.3(7) . . . . ? C1 C2 C3 C4 -179.1(4) . . . . ? C2 C3 C4 C5 1.6(7) . . . . ? C3 C4 C5 C6 -2.3(7) . . . . ? C3 C4 C5 S2 175.8(4) . . . . ? O3 S2 C5 C6 -42.2(6) . . . . ? O5 S2 C5 C6 76.4(6) . . . . ? O4 S2 C5 C6 -167.0(4) . . . . ? O3 S2 C5 C4 139.7(6) . . . . ? O5 S2 C5 C4 -101.8(6) . . . . ? O4 S2 C5 C4 14.8(5) . . . . ? C4 C5 C6 C7 1.8(6) . . . . ? S2 C5 C6 C7 -176.4(3) . . . . ? C5 C6 C7 C2 -0.4(6) . . . . ? C3 C2 C7 C6 -0.3(6) . . . . ? C1 C2 C7 C6 178.5(4) . . . . ? Cd1 O6 C8 O7 -15.4(5) . . . . ? Cd1 O6 C8 C9 161.6(3) . . . . ? O7 C8 C9 C14 22.0(7) . . . . ? O6 C8 C9 C14 -155.1(5) . . . . ? O7 C8 C9 C10 -160.0(5) . . . . ? O6 C8 C9 C10 22.8(6) . . . . ? C14 C9 C10 C11 -2.0(7) . . . . ? C8 C9 C10 C11 -180.0(4) . . . . ? C9 C10 C11 C12 2.0(7) . . . . ? C10 C11 C12 C13 0.1(8) . . . . ? C10 C11 C12 S1 -175.0(4) . . . . ? O10 S1 C12 C11 -149.6(6) . . . . ? O9 S1 C12 C11 92.8(5) . . . . ? O8 S1 C12 C11 -22.7(5) . . . . ? O10 S1 C12 C13 35.2(6) . . . . ? O9 S1 C12 C13 -82.4(5) . . . . ? O8 S1 C12 C13 162.2(5) . . . . ? C11 C12 C13 C14 -2.3(9) . . . . ? S1 C12 C13 C14 172.8(5) . . . . ? C12 C13 C14 C9 2.3(10) . . . . ? C10 C9 C14 C13 -0.2(9) . . . . ? C8 C9 C14 C13 177.8(6) . . . . ? C19 N1 C15 C16 -1.5(8) . . . . ? Cd1 N1 C15 C16 -177.3(4) . . . . ? N1 C15 C16 C17 2.4(8) . . . . ? C15 C16 C17 C18 -1.2(7) . . . . ? C15 C16 C17 C22 178.0(5) . . . . ? C16 C17 C18 C19 -0.7(9) . . . . ? C22 C17 C18 C19 -179.8(5) . . . . ? C15 N1 C19 C18 -0.6(9) . . . . ? Cd1 N1 C19 C18 175.0(5) . . . . ? C17 C18 C19 N1 1.7(10) . . . . ? C24 N2 C20 C21 1.5(8) . . . . ? N2 C20 C21 C22 -1.2(8) . . . . ? C20 C21 C22 C23 0.0(7) . . . . ? C20 C21 C22 C17 179.9(4) . . . . ? C18 C17 C22 C23 -23.5(7) . . . . ? C16 C17 C22 C23 157.3(5) . . . . ? C18 C17 C22 C21 156.5(5) . . . . ? C16 C17 C22 C21 -22.6(7) . . . . ? C21 C22 C23 C24 0.8(7) . . . . ? C17 C22 C23 C24 -179.1(4) . . . . ? C20 N2 C24 C23 -0.6(8) . . . . ? C22 C23 C24 N2 -0.6(8) . . . . ? C29 N3 C25 C26 1.1(9) . . . . ? Cd1 N3 C25 C26 -166.5(5) . . . . ? N3 C25 C26 C27 0.3(11) . . . . ? C25 C26 C27 C28 -1.8(9) . . . . ? C25 C26 C27 C32 175.7(5) . . . . ? C26 C27 C28 C29 1.9(7) . . . . ? C32 C27 C28 C29 -175.5(4) . . . . ? C25 N3 C29 C28 -0.9(8) . . . . ? Cd1 N3 C29 C28 166.3(4) . . . . ? C27 C28 C29 N3 -0.6(8) . . . . ? C34 N4 C30 C31 2.0(8) . . . . ? Cd2 N4 C30 C31 -161.2(4) . . . . ? N4 C30 C31 C32 0.9(9) . . . . ? C30 C31 C32 C33 -2.9(8) . . . . ? C30 C31 C32 C27 178.0(4) . . . . ? C26 C27 C32 C33 177.8(6) . . . . ? C28 C27 C32 C33 -5.0(6) . . . . ? C26 C27 C32 C31 -3.2(7) . . . . ? C28 C27 C32 C31 174.0(5) . . . . ? C31 C32 C33 C34 2.0(8) . . . . ? C27 C32 C33 C34 -179.0(5) . . . . ? C32 C33 C34 N4 1.0(9) . . . . ? C30 N4 C34 C33 -3.0(8) . . . . ? Cd2 N4 C34 C33 160.1(4) . . . . ? C39 N5 C35 C36 -0.9(7) . . . . ? Cd1 N5 C35 C36 176.0(4) . . . . ? N5 C35 C36 C37 1.2(8) . . . . ? C35 C36 C37 C38 0.0(7) . . . . ? C35 C36 C37 C42 -177.4(5) . . . . ? C36 C37 C38 C39 -1.3(7) . . . . ? C42 C37 C38 C39 176.1(5) . . . . ? C35 N5 C39 C38 -0.5(7) . . . . ? Cd1 N5 C39 C38 -177.6(4) . . . . ? C37 C38 C39 N5 1.7(8) . . . . ? C44 N6 C40 C41 0.5(7) . . . . ? Cd2 N6 C40 C41 -177.7(4) 4_554 . . . ? N6 C40 C41 C42 0.4(8) . . . . ? C40 C41 C42 C43 -0.7(7) . . . . ? C40 C41 C42 C37 178.2(5) . . . . ? C36 C37 C42 C41 -13.4(7) . . . . ? C38 C37 C42 C41 169.3(4) . . . . ? C36 C37 C42 C43 165.5(5) . . . . ? C38 C37 C42 C43 -11.8(7) . . . . ? C41 C42 C43 C44 0.1(7) . . . . ? C37 C42 C43 C44 -178.8(5) . . . . ? C40 N6 C44 C43 -1.1(7) . . . . ? Cd2 N6 C44 C43 177.2(4) 4_554 . . . ? C42 C43 C44 N6 0.8(8) . . . . ? C49 N7 C45 C46 0.3(7) . . . . ? Cd2 N7 C45 C46 -167.8(4) . . . . ? N7 C45 C46 C47 -0.1(8) . . . . ? C45 C46 C47 C48 -0.5(7) . . . . ? C45 C46 C47 C52 -179.8(4) . . . . ? C46 C47 C48 C49 1.0(6) . . . . ? C52 C47 C48 C49 -179.7(4) . . . . ? C45 N7 C49 C48 0.2(7) . . . . ? Cd2 N7 C49 C48 167.8(3) . . . . ? C47 C48 C49 N7 -0.8(7) . . . . ? C54 N8 C50 C51 0.6(8) . . . . ? N8 C50 C51 C52 -0.5(8) . . . . ? C50 C51 C52 C53 1.7(7) . . . . ? C50 C51 C52 C47 -179.9(4) . . . . ? C46 C47 C52 C53 153.7(5) . . . . ? C48 C47 C52 C53 -25.5(7) . . . . ? C46 C47 C52 C51 -24.6(6) . . . . ? C48 C47 C52 C51 156.2(5) . . . . ? C51 C52 C53 C54 -3.0(8) . . . . ? C47 C52 C53 C54 178.6(5) . . . . ? C50 N8 C54 C53 -2.1(9) . . . . ? C52 C53 C54 N8 3.4(9) . . . . ? 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 O1W H1W1 N8 0.85 2.29 2.791(6) 118.3 2_564 O1W H1W2 O5W 0.86 2.40 3.261(7) 179.2 3_556 O2W H2W1 O7 0.85 2.37 2.932(6) 124.4 2 O2W H2W2 O1W 0.85 2.54 3.389(6) 179.6 . O3W H3W1 O1W 0.85 2.47 3.307(5) 168.8 . O3W H3W2 N6 0.85 2.34 3.180(5) 169.0 4_455 O4W H4W1 O5 0.85 2.26 2.880(9) 129.2 4 O4W H4W2 O10 0.87 1.88 2.685(8) 153.7 . O5W H5W1 O1 0.87 1.99 2.858(6) 178.7 2_554 O5W H5W2 N2 0.85 1.93 2.754(6) 164.9 . O6W H6W1 O4 0.85 1.92 2.770(8) 174.4 . O6W H6W2 O8 0.85 2.15 2.998(9) 174.8 2_554 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.071 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.106