_publ_contact_author_name 'Susumu Kitagawa' _publ_contact_author_address ; Department of Synthetic Chemistry and Biological Chemistry Graduate School of Engineering, Kyoto University Katsura, Nishikyo-ku Kyoto 615-8510 JAPAN ; _publ_contact_author_email KITAGAWA@SBCHEM.KYOTO-U.AC.JP _publ_section_title ; title ; loop_ _publ_author_name ; 'Susumu Kitagawa' ; _publ_author_address ; Department of Synthetic Chemistry and Biological Chemistry Graduate School of Engineering, Kyoto University Katsura, Nishikyo-ku Kyoto 615-8510 JAPAN ; data_Zn_SDB_dabco _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8.50 H7 N0.50 O3 S0.50 Zn0.50' _chemical_formula_weight 212.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 22.033(8) _cell_length_b 12.691(5) _cell_length_c 9.603(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.492(5) _cell_angle_gamma 90.00 _cell_volume 2662.3(17) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.062 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 1.023 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8215 _exptl_absorpt_correction_T_max 0.8215 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10735 _diffrn_reflns_av_R_equivalents 0.0754 _diffrn_reflns_av_sigmaI/netI 0.0748 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3165 _reflns_number_gt 2399 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1168P)^2^+3.1185P] 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 3165 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0907 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.2048 _refine_ls_wR_factor_gt 0.1886 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.00090(3) 0.0000 0.15300(6) 0.0222(2) Uani 1 2 d S . . S2 S 0.26519(6) 0.5000 0.07502(16) 0.0269(4) Uani 1 2 d S . . O2 O 0.29891(19) 0.5000 -0.0433(5) 0.0340(10) Uani 1 2 d S . . O3 O 0.29785(19) 0.5000 0.2160(5) 0.0362(10) Uani 1 2 d S . . O1 O 0.06649(15) 0.1110(3) 0.1366(4) 0.0392(8) Uani 1 1 d . . . C8 C 0.21426(18) 0.3913(3) 0.0605(4) 0.0274(9) Uani 1 1 d . . . C1 C 0.08312(19) 0.1435(3) 0.0235(5) 0.0303(9) Uani 1 1 d . . . N1 N -0.0001(2) 0.0000 0.3656(5) 0.0232(10) Uani 1 2 d S . . C9 C 0.13105(19) 0.2301(3) 0.0372(4) 0.0272(9) Uani 1 1 d . . . C10 C 0.1959(2) 0.3486(3) -0.0697(5) 0.0316(10) Uani 1 1 d . . . H1 H 0.2115 0.3743 -0.1496 0.038 Uiso 1 1 calc R . . C11 C 0.1539(2) 0.2670(3) -0.0809(4) 0.0309(9) Uani 1 1 d . . . H2 H 0.1409 0.2367 -0.1690 0.037 Uiso 1 1 calc R . . C12 C 0.1516(3) 0.2699(4) 0.1677(5) 0.0483(14) Uani 1 1 d . . . H3 H 0.1378 0.2414 0.2482 0.058 Uiso 1 1 calc R . . C13 C 0.1935(3) 0.3538(4) 0.1798(5) 0.0488(14) Uani 1 1 d . . . H4 H 0.2071 0.3837 0.2679 0.059 Uiso 1 1 calc R . . C14 C 0.0003(7) 0.1048(11) 0.4171(16) 0.074(4) Uiso 0.50 1 d P . . H5 H -0.0357 0.1426 0.3715 0.089 Uiso 0.50 1 calc PR . . H6 H 0.0369 0.1414 0.3945 0.089 Uiso 0.50 1 calc PR . . C15 C -0.0536(6) -0.0617(10) 0.4008(14) 0.064(3) Uiso 0.50 1 d P . . H7 H -0.0507 -0.1346 0.3688 0.077 Uiso 0.50 1 calc PR . . H8 H -0.0916 -0.0312 0.3528 0.077 Uiso 0.50 1 calc PR . . C16 C 0.0549(6) -0.0598(10) 0.4367(14) 0.059(3) Uiso 0.50 1 d P . . H9 H 0.0926 -0.0258 0.4158 0.071 Uiso 0.50 1 calc PR . . H10 H 0.0544 -0.1321 0.4007 0.071 Uiso 0.50 1 calc PR . . O4 O 0.06295(14) 0.1125(3) -0.0968(3) 0.0365(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0255(4) 0.0269(4) 0.0150(3) 0.000 0.0057(2) 0.000 S2 0.0226(7) 0.0216(7) 0.0363(8) 0.000 0.0032(6) 0.000 O2 0.025(2) 0.029(2) 0.051(3) 0.000 0.0149(19) 0.000 O3 0.023(2) 0.039(3) 0.044(3) 0.000 -0.0035(19) 0.000 O1 0.0405(18) 0.0397(18) 0.0394(18) -0.0049(15) 0.0129(14) -0.0175(15) C8 0.026(2) 0.024(2) 0.032(2) -0.0020(17) 0.0047(16) -0.0061(17) C1 0.030(2) 0.031(2) 0.031(2) -0.0027(18) 0.0100(17) -0.0011(18) N1 0.024(2) 0.026(2) 0.020(2) 0.000 0.0037(18) 0.000 C9 0.032(2) 0.025(2) 0.024(2) -0.0002(16) 0.0049(16) -0.0042(17) C10 0.040(2) 0.029(2) 0.028(2) 0.0012(17) 0.0116(18) -0.0077(19) C11 0.035(2) 0.031(2) 0.027(2) -0.0020(18) 0.0055(17) -0.0048(18) C12 0.070(4) 0.048(3) 0.029(2) -0.006(2) 0.015(2) -0.025(3) C13 0.065(3) 0.055(3) 0.028(2) -0.010(2) 0.010(2) -0.032(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 Zn1 O4 2.028(3) 2 ? Zn1 O4 2.028(3) 5 ? Zn1 O1 2.039(3) . ? Zn1 O1 2.039(3) 6 ? Zn1 N1 2.045(5) . ? Zn1 Zn1 2.9337(16) 5 ? S2 O2 1.437(5) . ? S2 O3 1.448(5) . ? S2 C8 1.773(4) 6_565 ? S2 C8 1.773(4) . ? O1 C1 1.260(5) . ? C8 C13 1.372(6) . ? C8 C10 1.375(6) . ? C1 O4 1.246(5) . ? C1 C9 1.518(6) . ? N1 C14 1.419(14) . ? N1 C14 1.419(14) 6 ? N1 C15 1.490(13) . ? N1 C15 1.490(13) 6 ? N1 C16 1.515(12) 6 ? N1 C16 1.515(12) . ? C9 C12 1.373(6) . ? C9 C11 1.382(6) . ? C10 C11 1.383(6) . ? C10 H1 0.9400 . ? C11 H2 0.9400 . ? C12 C13 1.403(7) . ? C12 H3 0.9400 . ? C13 H4 0.9400 . ? C14 C14 1.59(3) 2_556 ? C14 H5 0.9800 . ? C14 H6 0.9800 . ? C15 C16 1.564(19) 2_556 ? C15 H7 0.9800 . ? C15 H8 0.9800 . ? C16 C15 1.564(19) 2_556 ? C16 H9 0.9800 . ? C16 H10 0.9800 . ? O4 Zn1 2.028(3) 5 ? 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 89.55(18) 2 5 ? O4 Zn1 O1 88.11(14) 2 . ? O4 Zn1 O1 160.07(14) 5 . ? O4 Zn1 O1 160.07(14) 2 6 ? O4 Zn1 O1 88.11(14) 5 6 ? O1 Zn1 O1 87.4(2) . 6 ? O4 Zn1 N1 99.69(13) 2 . ? O4 Zn1 N1 99.69(13) 5 . ? O1 Zn1 N1 100.21(13) . . ? O1 Zn1 N1 100.21(13) 6 . ? O4 Zn1 Zn1 79.35(10) 2 5 ? O4 Zn1 Zn1 79.35(10) 5 5 ? O1 Zn1 Zn1 80.77(10) . 5 ? O1 Zn1 Zn1 80.77(10) 6 5 ? N1 Zn1 Zn1 178.61(13) . 5 ? O2 S2 O3 119.6(3) . . ? O2 S2 C8 108.99(18) . 6_565 ? O3 S2 C8 107.80(18) . 6_565 ? O2 S2 C8 108.99(18) . . ? O3 S2 C8 107.80(18) . . ? C8 S2 C8 102.2(3) 6_565 . ? C1 O1 Zn1 125.6(3) . . ? C13 C8 C10 122.1(4) . . ? C13 C8 S2 118.7(3) . . ? C10 C8 S2 119.1(3) . . ? O4 C1 O1 126.0(4) . . ? O4 C1 C9 117.9(4) . . ? O1 C1 C9 116.1(4) . . ? C14 N1 C14 139.3(13) . 6 ? C14 N1 C15 112.5(9) . . ? C14 N1 C15 53.0(8) 6 . ? C14 N1 C15 53.0(8) . 6 ? C14 N1 C15 112.5(9) 6 6 ? C15 N1 C15 63.4(10) . 6 ? C14 N1 C16 53.5(7) . 6 ? C14 N1 C16 110.1(9) 6 6 ? C15 N1 C16 140.5(8) . 6 ? C15 N1 C16 104.2(7) 6 6 ? C14 N1 C16 110.1(9) . . ? C14 N1 C16 53.5(7) 6 . ? C15 N1 C16 104.2(7) . . ? C15 N1 C16 140.5(8) 6 . ? C16 N1 C16 60.1(10) 6 . ? C14 N1 Zn1 110.3(6) . . ? C14 N1 Zn1 110.3(6) 6 . ? C15 N1 Zn1 109.8(6) . . ? C15 N1 Zn1 109.8(6) 6 . ? C16 N1 Zn1 109.7(5) 6 . ? C16 N1 Zn1 109.7(5) . . ? C12 C9 C11 120.8(4) . . ? C12 C9 C1 119.3(4) . . ? C11 C9 C1 119.9(4) . . ? C8 C10 C11 118.7(4) . . ? C8 C10 H1 120.6 . . ? C11 C10 H1 120.6 . . ? C9 C11 C10 120.1(4) . . ? C9 C11 H2 119.9 . . ? C10 C11 H2 119.9 . . ? C9 C12 C13 119.4(4) . . ? C9 C12 H3 120.3 . . ? C13 C12 H3 120.3 . . ? C8 C13 C12 118.7(4) . . ? C8 C13 H4 120.6 . . ? C12 C13 H4 120.6 . . ? N1 C14 C14 110.3(6) . 2_556 ? N1 C14 H5 109.6 . . ? C14 C14 H5 109.6 2_556 . ? N1 C14 H6 109.6 . . ? C14 C14 H6 109.6 2_556 . ? H5 C14 H6 108.1 . . ? N1 C15 C16 109.6(9) . 2_556 ? N1 C15 H7 109.7 . . ? C16 C15 H7 109.7 2_556 . ? N1 C15 H8 109.7 . . ? C16 C15 H8 109.7 2_556 . ? H7 C15 H8 108.2 . . ? N1 C16 C15 109.8(9) . 2_556 ? N1 C16 H9 109.7 . . ? C15 C16 H9 109.7 2_556 . ? N1 C16 H10 109.7 . . ? C15 C16 H10 109.7 2_556 . ? H9 C16 H10 108.2 . . ? C1 O4 Zn1 128.3(3) . 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 O4 Zn1 O1 C1 -77.8(4) 2 . . . ? O4 Zn1 O1 C1 5.6(6) 5 . . . ? O1 Zn1 O1 C1 82.7(4) 6 . . . ? N1 Zn1 O1 C1 -177.3(4) . . . . ? Zn1 Zn1 O1 C1 1.7(4) 5 . . . ? O2 S2 C8 C13 157.6(4) . . . . ? O3 S2 C8 C13 26.3(5) . . . . ? C8 S2 C8 C13 -87.1(5) 6_565 . . . ? O2 S2 C8 C10 -23.7(4) . . . . ? O3 S2 C8 C10 -154.9(4) . . . . ? C8 S2 C8 C10 91.6(4) 6_565 . . . ? Zn1 O1 C1 O4 -1.0(7) . . . . ? Zn1 O1 C1 C9 177.5(3) . . . . ? O4 Zn1 N1 C14 -45.0(8) 2 . . . ? O4 Zn1 N1 C14 -136.2(7) 5 . . . ? O1 Zn1 N1 C14 44.8(8) . . . . ? O1 Zn1 N1 C14 134.0(7) 6 . . . ? Zn1 Zn1 N1 C14 -90.6(7) 5 . . . ? O4 Zn1 N1 C14 136.2(7) 2 . . 6 ? O4 Zn1 N1 C14 45.0(8) 5 . . 6 ? O1 Zn1 N1 C14 -134.0(7) . . . 6 ? O1 Zn1 N1 C14 -44.8(8) 6 . . 6 ? Zn1 Zn1 N1 C14 90.6(7) 5 . . 6 ? O4 Zn1 N1 C15 79.5(6) 2 . . . ? O4 Zn1 N1 C15 -11.7(6) 5 . . . ? O1 Zn1 N1 C15 169.3(6) . . . . ? O1 Zn1 N1 C15 -101.5(6) 6 . . . ? Zn1 Zn1 N1 C15 33.9(6) 5 . . . ? O4 Zn1 N1 C15 11.7(6) 2 . . 6 ? O4 Zn1 N1 C15 -79.5(6) 5 . . 6 ? O1 Zn1 N1 C15 101.5(6) . . . 6 ? O1 Zn1 N1 C15 -169.3(6) 6 . . 6 ? Zn1 Zn1 N1 C15 -34.0(6) 5 . . 6 ? O4 Zn1 N1 C16 -102.3(5) 2 . . 6 ? O4 Zn1 N1 C16 166.5(5) 5 . . 6 ? O1 Zn1 N1 C16 -12.4(5) . . . 6 ? O1 Zn1 N1 C16 76.7(5) 6 . . 6 ? Zn1 Zn1 N1 C16 -147.9(5) 5 . . 6 ? O4 Zn1 N1 C16 -166.5(5) 2 . . . ? O4 Zn1 N1 C16 102.3(5) 5 . . . ? O1 Zn1 N1 C16 -76.7(5) . . . . ? O1 Zn1 N1 C16 12.4(5) 6 . . . ? Zn1 Zn1 N1 C16 147.8(5) 5 . . . ? O4 C1 C9 C12 176.4(5) . . . . ? O1 C1 C9 C12 -2.2(7) . . . . ? O4 C1 C9 C11 -4.3(6) . . . . ? O1 C1 C9 C11 177.1(4) . . . . ? C13 C8 C10 C11 1.7(7) . . . . ? S2 C8 C10 C11 -177.0(3) . . . . ? C12 C9 C11 C10 -3.1(7) . . . . ? C1 C9 C11 C10 177.6(4) . . . . ? C8 C10 C11 C9 0.2(7) . . . . ? C11 C9 C12 C13 4.0(8) . . . . ? C1 C9 C12 C13 -176.7(4) . . . . ? C10 C8 C13 C12 -0.8(8) . . . . ? S2 C8 C13 C12 177.9(4) . . . . ? C9 C12 C13 C8 -2.1(9) . . . . ? C14 N1 C14 C14 -2(3) 6 . . 2_556 ? C15 N1 C14 C14 57.2(18) . . . 2_556 ? C15 N1 C14 C14 80.3(16) 6 . . 2_556 ? C16 N1 C14 C14 -79.8(16) 6 . . 2_556 ? C16 N1 C14 C14 -58.5(18) . . . 2_556 ? Zn1 N1 C14 C14 -179.8(12) . . . 2_556 ? C14 N1 C15 C16 -55.7(13) . . . 2_556 ? C14 N1 C15 C16 80.0(12) 6 . . 2_556 ? C15 N1 C15 C16 -76.2(10) 6 . . 2_556 ? C16 N1 C15 C16 3.7(19) 6 . . 2_556 ? C16 N1 C15 C16 63.6(9) . . . 2_556 ? Zn1 N1 C15 C16 -179.0(7) . . . 2_556 ? C14 N1 C16 C15 59.4(13) . . . 2_556 ? C14 N1 C16 C15 -77.8(11) 6 . . 2_556 ? C15 N1 C16 C15 -61.5(10) . . . 2_556 ? C15 N1 C16 C15 3.7(19) 6 . . 2_556 ? C16 N1 C16 C15 79.1(10) 6 . . 2_556 ? Zn1 N1 C16 C15 -179.0(7) . . . 2_556 ? O1 C1 O4 Zn1 -1.3(7) . . . 5 ? C9 C1 O4 Zn1 -179.7(3) . . . 5 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.172 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.119 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.426 -0.024 -0.100 1210 257 ' ' _platon_squeeze_details ; ; #===END _publ_contact_author_name 'Susumu Kitagawa' _publ_contact_author_address ; Department of Synthetic Chemistry and Biological Chemistry Graduate School of Engineering, Kyoto University Katsura, Nishikyo-ku Kyoto 615-8510 JAPAN ; _publ_contact_author_email KITAGAWA@SBCHEM.KYOTO-U.AC.JP _publ_section_title ; title ; loop_ _publ_author_name ; 'Susumu Kitagawa' ; _publ_author_address ; Department of Synthetic Chemistry and Biological Chemistry Graduate School of Engineering, Kyoto University Katsura, Nishikyo-ku Kyoto 615-8510 JAPAN ; data_Zn_SDB_bpb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H21 N2 O7 S Zn' _chemical_formula_weight 558.87 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4907(16) _cell_length_b 12.996(3) _cell_length_c 13.151(3) _cell_angle_alpha 84.192(9) _cell_angle_beta 73.567(8) _cell_angle_gamma 72.272(8) _cell_volume 1325.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 574 _exptl_absorpt_coefficient_mu 1.050 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8175 _exptl_absorpt_correction_T_max 0.8175 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10704 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5794 _reflns_number_gt 4768 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'Sir-97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1328P)^2^+2.1176P] 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 5794 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0789 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.2159 _refine_ls_wR_factor_gt 0.2026 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.011 _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 0.67243(6) -0.52336(4) 0.42242(3) 0.02712(19) Uani 1 1 d . . . S2 S 0.19947(17) -0.91031(9) 0.16408(10) 0.0388(3) Uani 1 1 d . . . O7 O 0.2473(5) -1.3506(3) 0.4809(3) 0.0460(9) Uani 1 1 d . . . N10 N 0.8893(4) -0.5160(3) 0.3107(3) 0.0292(7) Uani 1 1 d . . . O8 O 0.3266(5) -0.5831(3) 0.4733(3) 0.0439(8) Uani 1 1 d . . . C6 C 0.4355(6) -0.6311(3) 0.3947(3) 0.0325(9) Uani 1 1 d . . . O9 O 0.5838(4) -0.6232(3) 0.3575(3) 0.0422(8) Uani 1 1 d . . . O10 O 0.5046(4) -1.3973(3) 0.3657(3) 0.0445(8) Uani 1 1 d . . . O11 O 0.3053(6) -0.9225(3) 0.0570(3) 0.0516(10) Uani 1 1 d . . . C10 C 1.3490(6) -0.5045(4) 0.0774(3) 0.0325(9) Uani 1 1 d . . . O12 O 0.0163(5) -0.8662(3) 0.1849(3) 0.0526(10) Uani 1 1 d . . . C12 C 1.0899(6) -0.5706(4) 0.1445(3) 0.0351(10) Uani 1 1 d . . . H1 H 1.1228 -0.6111 0.0827 0.042 Uiso 1 1 calc R . . C13 C 0.9435(6) -0.5719(4) 0.2215(3) 0.0329(9) Uani 1 1 d . . . H2 H 0.8777 -0.6144 0.2110 0.040 Uiso 1 1 calc R . . C14 C 1.1319(6) -0.4493(4) 0.2512(4) 0.0376(10) Uani 1 1 d . . . H3 H 1.1946 -0.4059 0.2640 0.045 Uiso 1 1 calc R . . C15 C 0.1623(7) -0.7815(4) 0.3249(4) 0.0384(10) Uani 1 1 d . . . H4 H 0.0520 -0.7903 0.3510 0.046 Uiso 1 1 calc R . . C16 C 0.3591(6) -1.3349(3) 0.3987(4) 0.0328(9) Uani 1 1 d . . . C17 C 0.1240(6) -1.0556(4) 0.3189(4) 0.0409(11) Uani 1 1 d . . . H5 H 0.0199 -1.0016 0.3433 0.049 Uiso 1 1 calc R . . C18 C 0.2730(6) -0.8320(4) 0.2330(4) 0.0346(9) Uani 1 1 d . . . C19 C 0.3973(6) -1.1152(4) 0.1908(4) 0.0371(10) Uani 1 1 d . . . H6 H 0.4767 -1.1017 0.1288 0.044 Uiso 1 1 calc R . . C20 C 0.1573(6) -1.1535(4) 0.3735(4) 0.0401(10) Uani 1 1 d . . . H7 H 0.0756 -1.1667 0.4344 0.048 Uiso 1 1 calc R . . C21 C 0.2432(6) -1.0377(4) 0.2297(4) 0.0339(9) Uani 1 1 d . . . C22 C 0.4364(7) -0.8211(4) 0.1927(4) 0.0457(12) Uani 1 1 d . . . H8 H 0.5096 -0.8561 0.1302 0.055 Uiso 1 1 calc R . . C23 C 1.4826(6) -0.4802(4) 0.1049(3) 0.0379(10) Uani 1 1 d . . . H9 H 1.4714 -0.4672 0.1760 0.046 Uiso 1 1 calc R . . C24 C 0.3126(6) -1.2317(4) 0.3372(4) 0.0320(9) Uani 1 1 d . . . C25 C 1.6282(6) -0.4755(4) 0.0288(4) 0.0397(11) Uani 1 1 d . . . H10 H 1.7153 -0.4583 0.0485 0.048 Uiso 1 1 calc R . . C26 C 1.1900(5) -0.5081(4) 0.1587(3) 0.0310(9) Uani 1 1 d . . . C27 C 0.9824(6) -0.4548(4) 0.3242(4) 0.0387(11) Uani 1 1 d . . . H11 H 0.9443 -0.4139 0.3861 0.046 Uiso 1 1 calc R . . C28 C 0.2172(6) -0.7176(4) 0.3777(4) 0.0363(10) Uani 1 1 d . . . H12 H 0.1435 -0.6827 0.4402 0.044 Uiso 1 1 calc R . . C29 C 0.4899(7) -0.7574(4) 0.2467(4) 0.0481(13) Uani 1 1 d . . . H13 H 0.6010 -0.7497 0.2210 0.058 Uiso 1 1 calc R . . C31 C 0.4324(6) -1.2119(4) 0.2442(4) 0.0364(10) Uani 1 1 d . . . H14 H 0.5368 -1.2653 0.2188 0.044 Uiso 1 1 calc R . . C32 C 0.3799(6) -0.7047(4) 0.3391(4) 0.0334(9) Uani 1 1 d . . . N9 N 0.9974(7) -0.7917(5) -0.0812(4) 0.0608(13) Uani 1 1 d . . . O6 O 1.1711(6) -0.6876(4) -0.0878(4) 0.0668(12) Uani 1 1 d . . . C36 C 1.0413(8) -0.7153(5) -0.0487(5) 0.0547(14) Uani 1 1 d . . . H21 H 0.9646 -0.6776 0.0115 0.066 Uiso 1 1 calc R . . C37 C 1.1145(13) -0.8565(9) -0.1680(9) 0.118(4) Uani 1 1 d . . . H15 H 1.0931 -0.8232 -0.2341 0.177 Uiso 1 1 calc R . . H16 H 1.0987 -0.9280 -0.1608 0.177 Uiso 1 1 calc R . . H17 H 1.2312 -0.8624 -0.1681 0.177 Uiso 1 1 calc R . . C43 C 0.8375(12) -0.8150(9) -0.0239(8) 0.105(3) Uani 1 1 d . . . H18 H 0.7883 -0.7745 0.0414 0.158 Uiso 1 1 calc R . . H19 H 0.8603 -0.8917 -0.0073 0.158 Uiso 1 1 calc R . . H20 H 0.7576 -0.7941 -0.0675 0.158 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 0.0220(3) 0.0293(3) 0.0264(3) -0.00119(18) 0.00275(19) -0.01042(19) S2 0.0544(7) 0.0300(5) 0.0391(6) 0.0039(4) -0.0214(5) -0.0159(5) O7 0.046(2) 0.0426(19) 0.0376(18) 0.0088(15) -0.0002(15) -0.0087(15) N10 0.0220(16) 0.0351(18) 0.0275(16) -0.0025(14) 0.0035(13) -0.0127(14) O8 0.048(2) 0.048(2) 0.0364(17) -0.0128(15) 0.0058(15) -0.0261(16) C6 0.035(2) 0.031(2) 0.032(2) -0.0016(17) -0.0030(17) -0.0139(17) O9 0.0349(17) 0.0450(19) 0.0481(19) -0.0146(15) -0.0009(15) -0.0185(15) O10 0.0350(18) 0.0414(18) 0.049(2) 0.0105(15) -0.0066(15) -0.0066(14) O11 0.086(3) 0.0415(19) 0.0333(17) 0.0055(15) -0.0213(19) -0.0240(19) C10 0.029(2) 0.046(2) 0.0232(19) -0.0030(17) 0.0014(16) -0.0192(18) O12 0.059(2) 0.0368(19) 0.073(3) 0.0049(18) -0.040(2) -0.0102(17) C12 0.033(2) 0.045(2) 0.028(2) -0.0075(18) -0.0003(17) -0.0169(19) C13 0.030(2) 0.042(2) 0.029(2) -0.0046(17) 0.0007(17) -0.0192(18) C14 0.032(2) 0.052(3) 0.032(2) -0.0097(19) 0.0028(18) -0.024(2) C15 0.040(3) 0.040(2) 0.039(2) -0.0007(19) -0.006(2) -0.021(2) C16 0.033(2) 0.030(2) 0.037(2) -0.0001(17) -0.0098(18) -0.0104(17) C17 0.036(2) 0.032(2) 0.049(3) 0.001(2) -0.008(2) -0.0056(19) C18 0.043(3) 0.029(2) 0.035(2) -0.0008(17) -0.0123(19) -0.0127(18) C19 0.043(3) 0.038(2) 0.033(2) 0.0013(18) -0.0072(19) -0.020(2) C20 0.036(2) 0.038(2) 0.043(3) 0.001(2) -0.005(2) -0.0097(19) C21 0.042(2) 0.030(2) 0.035(2) 0.0014(17) -0.0148(19) -0.0155(18) C22 0.049(3) 0.047(3) 0.039(3) -0.014(2) 0.002(2) -0.020(2) C23 0.031(2) 0.062(3) 0.0240(19) -0.0039(19) -0.0003(17) -0.023(2) C24 0.033(2) 0.031(2) 0.035(2) 0.0006(17) -0.0095(18) -0.0133(17) C25 0.034(2) 0.063(3) 0.026(2) -0.004(2) -0.0022(18) -0.025(2) C26 0.026(2) 0.043(2) 0.0237(18) -0.0020(17) 0.0014(15) -0.0162(18) C27 0.036(2) 0.050(3) 0.029(2) -0.0120(19) 0.0068(18) -0.023(2) C28 0.038(2) 0.039(2) 0.032(2) -0.0034(18) -0.0033(18) -0.0152(19) C29 0.047(3) 0.050(3) 0.049(3) -0.015(2) 0.003(2) -0.026(2) C31 0.037(2) 0.034(2) 0.037(2) -0.0019(18) -0.0060(19) -0.0120(19) C32 0.036(2) 0.032(2) 0.032(2) -0.0024(17) -0.0039(18) -0.0143(18) N9 0.065(3) 0.076(4) 0.054(3) -0.009(3) -0.021(3) -0.031(3) O6 0.060(3) 0.074(3) 0.073(3) -0.007(2) -0.012(2) -0.032(2) C36 0.053(3) 0.060(3) 0.055(3) -0.009(3) -0.017(3) -0.018(3) C37 0.090(6) 0.145(9) 0.128(9) -0.081(8) -0.007(6) -0.043(6) C43 0.090(6) 0.157(10) 0.105(7) 0.004(6) -0.035(6) -0.081(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 N10 2.026(3) . ? Zn1 O7 2.037(3) 2_636 ? Zn1 O9 2.040(3) . ? Zn1 O10 2.050(3) 1_565 ? Zn1 O8 2.048(3) 2_646 ? Zn1 Zn1 2.9822(10) 2_646 ? S2 O11 1.435(4) . ? S2 O12 1.439(4) . ? S2 C21 1.773(5) . ? S2 C18 1.772(5) . ? O7 C16 1.267(6) . ? O7 Zn1 2.037(3) 2_636 ? N10 C27 1.334(6) . ? N10 C13 1.334(5) . ? O8 C6 1.245(5) . ? O8 Zn1 2.048(3) 2_646 ? C6 O9 1.247(5) . ? C6 C32 1.512(6) . ? O10 C16 1.237(6) . ? O10 Zn1 2.050(3) 1_545 ? C10 C25 1.395(6) 2_845 ? C10 C23 1.411(6) . ? C10 C26 1.476(5) . ? C12 C13 1.367(6) . ? C12 C26 1.399(6) . ? C12 H1 0.9400 . ? C13 H2 0.9400 . ? C14 C27 1.375(6) . ? C14 C26 1.388(6) . ? C14 H3 0.9400 . ? C15 C18 1.385(7) . ? C15 C28 1.388(6) . ? C15 H4 0.9400 . ? C16 C24 1.500(6) . ? C17 C21 1.368(7) . ? C17 C20 1.387(7) . ? C17 H5 0.9400 . ? C18 C22 1.383(7) . ? C19 C31 1.368(7) . ? C19 C21 1.382(7) . ? C19 H6 0.9400 . ? C20 C24 1.387(7) . ? C20 H7 0.9400 . ? C22 C29 1.388(7) . ? C22 H8 0.9400 . ? C23 C25 1.367(6) . ? C23 H9 0.9400 . ? C24 C31 1.410(6) . ? C25 C10 1.395(6) 2_845 ? C25 H10 0.9400 . ? C27 H11 0.9400 . ? C28 C32 1.386(6) . ? C28 H12 0.9400 . ? C29 C32 1.399(7) . ? C29 H13 0.9400 . ? C31 H14 0.9400 . ? N9 C36 1.307(8) . ? N9 C37 1.430(10) . ? N9 C43 1.458(10) . ? O6 C36 1.221(7) . ? C36 H21 0.9400 . ? C37 H15 0.9700 . ? C37 H16 0.9700 . ? C37 H17 0.9700 . ? C43 H18 0.9700 . ? C43 H19 0.9700 . ? C43 H20 0.9700 . ? 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 N10 Zn1 O7 104.49(15) . 2_636 ? N10 Zn1 O9 103.30(14) . . ? O7 Zn1 O9 87.61(16) 2_636 . ? N10 Zn1 O10 97.48(15) . 1_565 ? O7 Zn1 O10 158.02(14) 2_636 1_565 ? O9 Zn1 O10 86.83(15) . 1_565 ? N10 Zn1 O8 97.93(14) . 2_646 ? O7 Zn1 O8 90.24(16) 2_636 2_646 ? O9 Zn1 O8 158.52(14) . 2_646 ? O10 Zn1 O8 87.22(16) 1_565 2_646 ? N10 Zn1 Zn1 166.13(11) . 2_646 ? O7 Zn1 Zn1 87.45(10) 2_636 2_646 ? O9 Zn1 Zn1 83.94(10) . 2_646 ? O10 Zn1 Zn1 70.83(10) 1_565 2_646 ? O8 Zn1 Zn1 74.61(10) 2_646 2_646 ? O11 S2 O12 120.2(3) . . ? O11 S2 C21 108.2(2) . . ? O12 S2 C21 108.0(2) . . ? O11 S2 C18 108.5(2) . . ? O12 S2 C18 107.9(2) . . ? C21 S2 C18 102.6(2) . . ? C16 O7 Zn1 116.6(3) . 2_636 ? C27 N10 C13 117.9(3) . . ? C27 N10 Zn1 120.9(3) . . ? C13 N10 Zn1 121.3(3) . . ? C6 O8 Zn1 133.6(3) . 2_646 ? O9 C6 O8 126.4(4) . . ? O9 C6 C32 117.5(4) . . ? O8 C6 C32 116.1(4) . . ? C6 O9 Zn1 121.4(3) . . ? C16 O10 Zn1 138.3(3) . 1_545 ? C25 C10 C23 117.9(4) 2_845 . ? C25 C10 C26 121.2(4) 2_845 . ? C23 C10 C26 120.9(4) . . ? C13 C12 C26 119.2(4) . . ? C13 C12 H1 120.4 . . ? C26 C12 H1 120.4 . . ? N10 C13 C12 123.4(4) . . ? N10 C13 H2 118.3 . . ? C12 C13 H2 118.3 . . ? C27 C14 C26 119.8(4) . . ? C27 C14 H3 120.1 . . ? C26 C14 H3 120.1 . . ? C18 C15 C28 118.7(4) . . ? C18 C15 H4 120.6 . . ? C28 C15 H4 120.6 . . ? O10 C16 O7 125.3(4) . . ? O10 C16 C24 117.2(4) . . ? O7 C16 C24 117.5(4) . . ? C21 C17 C20 119.8(5) . . ? C21 C17 H5 120.1 . . ? C20 C17 H5 120.1 . . ? C15 C18 C22 122.1(4) . . ? C15 C18 S2 118.4(4) . . ? C22 C18 S2 119.5(4) . . ? C31 C19 C21 118.9(4) . . ? C31 C19 H6 120.5 . . ? C21 C19 H6 120.5 . . ? C24 C20 C17 119.3(5) . . ? C24 C20 H7 120.3 . . ? C17 C20 H7 120.3 . . ? C17 C21 C19 121.9(4) . . ? C17 C21 S2 118.7(4) . . ? C19 C21 S2 119.4(4) . . ? C18 C22 C29 118.6(4) . . ? C18 C22 H8 120.7 . . ? C29 C22 H8 120.7 . . ? C25 C23 C10 120.4(4) . . ? C25 C23 H9 119.8 . . ? C10 C23 H9 119.8 . . ? C20 C24 C31 119.8(4) . . ? C20 C24 C16 120.9(4) . . ? C31 C24 C16 119.3(4) . . ? C23 C25 C10 121.7(4) . 2_845 ? C23 C25 H10 119.2 . . ? C10 C25 H10 119.2 2_845 . ? C14 C26 C12 117.1(4) . . ? C14 C26 C10 122.0(4) . . ? C12 C26 C10 120.9(4) . . ? N10 C27 C14 122.6(4) . . ? N10 C27 H11 118.7 . . ? C14 C27 H11 118.7 . . ? C15 C28 C32 120.6(4) . . ? C15 C28 H12 119.7 . . ? C32 C28 H12 119.7 . . ? C22 C29 C32 120.5(5) . . ? C22 C29 H13 119.8 . . ? C32 C29 H13 119.8 . . ? C19 C31 C24 120.2(4) . . ? C19 C31 H14 119.9 . . ? C24 C31 H14 119.9 . . ? C28 C32 C29 119.6(4) . . ? C28 C32 C6 120.1(4) . . ? C29 C32 C6 120.3(4) . . ? C36 N9 C37 118.8(6) . . ? C36 N9 C43 119.9(7) . . ? C37 N9 C43 121.1(7) . . ? O6 C36 N9 127.2(6) . . ? O6 C36 H21 116.4 . . ? N9 C36 H21 116.4 . . ? N9 C37 H15 109.5 . . ? N9 C37 H16 109.5 . . ? H15 C37 H16 109.5 . . ? N9 C37 H17 109.5 . . ? H15 C37 H17 109.5 . . ? H16 C37 H17 109.5 . . ? N9 C43 H18 109.5 . . ? N9 C43 H19 109.5 . . ? H18 C43 H19 109.5 . . ? N9 C43 H20 109.5 . . ? H18 C43 H20 109.5 . . ? H19 C43 H20 109.5 . . ? 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 O7 Zn1 N10 C27 -90.7(4) 2_636 . . . ? O9 Zn1 N10 C27 178.3(4) . . . . ? O10 Zn1 N10 C27 89.8(4) 1_565 . . . ? O8 Zn1 N10 C27 1.6(4) 2_646 . . . ? Zn1 Zn1 N10 C27 58.0(7) 2_646 . . . ? O7 Zn1 N10 C13 89.4(4) 2_636 . . . ? O9 Zn1 N10 C13 -1.6(4) . . . . ? O10 Zn1 N10 C13 -90.1(4) 1_565 . . . ? O8 Zn1 N10 C13 -178.3(4) 2_646 . . . ? Zn1 Zn1 N10 C13 -121.9(4) 2_646 . . . ? Zn1 O8 C6 O9 -1.1(8) 2_646 . . . ? Zn1 O8 C6 C32 179.8(3) 2_646 . . . ? O8 C6 O9 Zn1 -0.9(7) . . . . ? C32 C6 O9 Zn1 178.2(3) . . . . ? N10 Zn1 O9 C6 -166.5(4) . . . . ? O7 Zn1 O9 C6 89.1(4) 2_636 . . . ? O10 Zn1 O9 C6 -69.6(4) 1_565 . . . ? O8 Zn1 O9 C6 4.6(7) 2_646 . . . ? Zn1 Zn1 O9 C6 1.5(4) 2_646 . . . ? C27 N10 C13 C12 0.9(7) . . . . ? Zn1 N10 C13 C12 -179.2(4) . . . . ? C26 C12 C13 N10 0.2(7) . . . . ? Zn1 O10 C16 O7 -19.1(8) 1_545 . . . ? Zn1 O10 C16 C24 159.9(3) 1_545 . . . ? Zn1 O7 C16 O10 10.0(7) 2_636 . . . ? Zn1 O7 C16 C24 -169.0(3) 2_636 . . . ? C28 C15 C18 C22 0.4(7) . . . . ? C28 C15 C18 S2 -178.2(4) . . . . ? O11 S2 C18 C15 160.0(4) . . . . ? O12 S2 C18 C15 28.3(4) . . . . ? C21 S2 C18 C15 -85.6(4) . . . . ? O11 S2 C18 C22 -18.6(5) . . . . ? O12 S2 C18 C22 -150.3(4) . . . . ? C21 S2 C18 C22 95.8(4) . . . . ? C21 C17 C20 C24 0.8(8) . . . . ? C20 C17 C21 C19 0.5(8) . . . . ? C20 C17 C21 S2 -178.1(4) . . . . ? C31 C19 C21 C17 -0.9(7) . . . . ? C31 C19 C21 S2 177.7(4) . . . . ? O11 S2 C21 C17 -159.3(4) . . . . ? O12 S2 C21 C17 -27.7(5) . . . . ? C18 S2 C21 C17 86.1(4) . . . . ? O11 S2 C21 C19 22.0(4) . . . . ? O12 S2 C21 C19 153.7(4) . . . . ? C18 S2 C21 C19 -92.6(4) . . . . ? C15 C18 C22 C29 0.0(8) . . . . ? S2 C18 C22 C29 178.6(4) . . . . ? C25 C10 C23 C25 0.7(9) 2_845 . . . ? C26 C10 C23 C25 -179.0(5) . . . . ? C17 C20 C24 C31 -1.6(7) . . . . ? C17 C20 C24 C16 175.1(4) . . . . ? O10 C16 C24 C20 -174.8(5) . . . . ? O7 C16 C24 C20 4.3(7) . . . . ? O10 C16 C24 C31 1.8(6) . . . . ? O7 C16 C24 C31 -179.0(4) . . . . ? C10 C23 C25 C10 -0.8(9) . . . 2_845 ? C27 C14 C26 C12 0.4(7) . . . . ? C27 C14 C26 C10 179.6(5) . . . . ? C13 C12 C26 C14 -0.8(7) . . . . ? C13 C12 C26 C10 180.0(5) . . . . ? C25 C10 C26 C14 -153.5(5) 2_845 . . . ? C23 C10 C26 C14 26.2(7) . . . . ? C25 C10 C26 C12 25.7(7) 2_845 . . . ? C23 C10 C26 C12 -154.6(5) . . . . ? C13 N10 C27 C14 -1.3(7) . . . . ? Zn1 N10 C27 C14 178.7(4) . . . . ? C26 C14 C27 N10 0.7(8) . . . . ? C18 C15 C28 C32 0.0(7) . . . . ? C18 C22 C29 C32 -0.7(9) . . . . ? C21 C19 C31 C24 0.1(7) . . . . ? C20 C24 C31 C19 1.1(7) . . . . ? C16 C24 C31 C19 -175.6(4) . . . . ? C15 C28 C32 C29 -0.6(8) . . . . ? C15 C28 C32 C6 177.4(4) . . . . ? C22 C29 C32 C28 1.0(8) . . . . ? C22 C29 C32 C6 -177.1(5) . . . . ? O9 C6 C32 C28 179.3(4) . . . . ? O8 C6 C32 C28 -1.5(7) . . . . ? O9 C6 C32 C29 -2.7(7) . . . . ? O8 C6 C32 C29 176.5(5) . . . . ? C37 N9 C36 O6 4.1(12) . . . . ? C43 N9 C36 O6 179.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 4.174 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.150 #===END _publ_contact_author_name 'Susumu Kitagawa' _publ_contact_author_address ; Department of Synthetic Chemistry and Biological Chemistry Graduate School of Engineering, Kyoto University Katsura, Nishikyo-ku Kyoto 615-8510 JAPAN ; _publ_contact_author_email KITAGAWA@SBCHEM.KYOTO-U.AC.JP _publ_section_title ; title ; loop_ _publ_author_name ; 'Susumu Kitagawa' ; _publ_author_address ; Department of Synthetic Chemistry and Biological Chemistry Graduate School of Engineering, Kyoto University Katsura, Nishikyo-ku Kyoto 615-8510 JAPAN ; data_Zn_SDB_bpb_degas _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H14 N O6 S Zn' _chemical_formula_weight 485.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0467(19) _cell_length_b 12.063(4) _cell_length_c 13.016(4) _cell_angle_alpha 86.066(12) _cell_angle_beta 72.390(10) _cell_angle_gamma 79.253(11) _cell_volume 1183.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 494 _exptl_absorpt_coefficient_mu 1.161 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8010 _exptl_absorpt_correction_T_max 0.8010 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9354 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5147 _reflns_number_gt 3708 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'Sir-97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1115P)^2^+1.3542P] 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 5147 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0977 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.2147 _refine_ls_wR_factor_gt 0.1862 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.14623(6) 0.42187(5) 0.02791(4) 0.0426(2) Uani 1 1 d . . . S2 S -0.75732(19) 0.13028(12) 0.42178(11) 0.0536(4) Uani 1 1 d . . . N1 N 0.3587(5) 0.2980(3) 0.0157(3) 0.0416(9) Uani 1 1 d . . . C4 C -0.2113(6) 0.3853(4) 0.1316(4) 0.0418(10) Uani 1 1 d . . . O5 O -0.2704(4) 0.4644(3) 0.0766(3) 0.0509(9) Uani 1 1 d . . . O9 O -1.1264(5) 0.4817(3) 0.8435(3) 0.0541(9) Uani 1 1 d . . . O10 O -0.9085(5) 0.3713(3) 0.8947(3) 0.0555(10) Uani 1 1 d . . . O6 O -0.0516(4) 0.3500(3) 0.1237(3) 0.0532(9) Uani 1 1 d . . . C10 C 0.6678(6) 0.1423(4) 0.0034(4) 0.0412(10) Uani 1 1 d . . . C12 C 0.8380(6) 0.0665(4) 0.0014(4) 0.0457(11) Uani 1 1 d . . . C13 C -0.5281(6) 0.3650(4) 0.2251(4) 0.0470(11) Uani 1 1 d . . . H1 H -0.5649 0.4309 0.1891 0.056 Uiso 1 1 calc R . . C14 C 0.5034(6) 0.1217(4) 0.0683(4) 0.0470(11) Uani 1 1 d . . . H2 H 0.4942 0.0545 0.1092 0.056 Uiso 1 1 calc R . . C15 C -0.5974(7) 0.2089(5) 0.3446(4) 0.0471(11) Uani 1 1 d . . . C16 C 0.6699(6) 0.2407(4) -0.0567(5) 0.0562(14) Uani 1 1 d . . . H3 H 0.7777 0.2564 -0.1032 0.067 Uiso 1 1 calc R . . O7 O -0.6667(6) 0.0194(3) 0.4399(3) 0.0680(12) Uani 1 1 d . . . C18 C -0.9979(6) 0.4000(4) 0.8294(4) 0.0461(11) Uani 1 1 d . . . C19 C -0.3473(6) 0.3267(4) 0.2103(4) 0.0445(11) Uani 1 1 d . . . O8 O -0.8986(5) 0.1437(4) 0.3721(3) 0.0685(12) Uani 1 1 d . . . C21 C -0.8374(7) 0.2038(5) 0.5450(4) 0.0490(12) Uani 1 1 d . . . C22 C 0.5164(7) 0.3162(5) -0.0494(5) 0.0570(14) Uani 1 1 d . . . H4 H 0.5218 0.3828 -0.0914 0.068 Uiso 1 1 calc R . . C23 C -0.9450(6) 0.3314(4) 0.7300(4) 0.0457(11) Uani 1 1 d . . . C24 C -0.4192(7) 0.1733(5) 0.3356(4) 0.0524(12) Uani 1 1 d . . . H5 H -0.3837 0.1096 0.3746 0.063 Uiso 1 1 calc R . . C25 C -0.7925(7) 0.2488(5) 0.7080(4) 0.0525(13) Uani 1 1 d . . . H6 H -0.7261 0.2360 0.7573 0.063 Uiso 1 1 calc R . . C26 C -0.6527(6) 0.3072(5) 0.2918(4) 0.0480(12) Uani 1 1 d . . . H7 H -0.7740 0.3336 0.3017 0.058 Uiso 1 1 calc R . . C27 C -0.2951(7) 0.2316(5) 0.2696(5) 0.0520(12) Uani 1 1 d . . . H8 H -0.1746 0.2078 0.2640 0.062 Uiso 1 1 calc R . . C28 C -0.7370(7) 0.1856(5) 0.6156(4) 0.0543(13) Uani 1 1 d . . . H9 H -0.6328 0.1313 0.6010 0.065 Uiso 1 1 calc R . . C29 C 0.3543(6) 0.2012(4) 0.0717(4) 0.0467(11) Uani 1 1 d . . . H10 H 0.2442 0.1864 0.1157 0.056 Uiso 1 1 calc R . . C30 C -1.0452(7) 0.3469(5) 0.6583(4) 0.0596(15) Uani 1 1 d . . . H11 H -1.1499 0.4007 0.6727 0.072 Uiso 1 1 calc R . . C31 C 0.9816(8) 0.0642(6) -0.0872(7) 0.102(3) Uani 1 1 d . . . H12 H 0.9715 0.1069 -0.1489 0.122 Uiso 1 1 calc R . . C32 C -0.9913(7) 0.2832(6) 0.5654(4) 0.0610(15) Uani 1 1 d . . . H13 H -1.0589 0.2938 0.5168 0.073 Uiso 1 1 calc R . . C35 C 1.1433(9) -0.0011(7) -0.0866(7) 0.102(3) Uani 1 1 d . . . H14 H 1.2423 0.0005 -0.1475 0.123 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 0.0300(3) 0.0443(3) 0.0447(3) 0.0014(2) -0.0115(2) 0.0151(2) S2 0.0547(8) 0.0551(8) 0.0455(7) -0.0059(6) -0.0059(6) -0.0087(6) N1 0.0314(19) 0.042(2) 0.045(2) 0.0021(16) -0.0116(16) 0.0110(16) C4 0.036(2) 0.038(2) 0.044(2) 0.0019(19) -0.0066(18) 0.0031(19) O5 0.0357(18) 0.050(2) 0.058(2) 0.0089(16) -0.0091(15) 0.0049(15) O9 0.048(2) 0.058(2) 0.048(2) -0.0043(16) -0.0107(16) 0.0098(17) O10 0.047(2) 0.066(2) 0.050(2) -0.0090(18) -0.0186(16) 0.0072(18) O6 0.0404(19) 0.059(2) 0.053(2) 0.0093(17) -0.0130(16) 0.0054(16) C10 0.031(2) 0.036(2) 0.049(3) -0.0020(19) -0.0092(19) 0.0093(18) C12 0.031(2) 0.040(3) 0.055(3) 0.001(2) -0.012(2) 0.0177(19) C13 0.041(3) 0.049(3) 0.044(3) 0.003(2) -0.011(2) 0.005(2) C14 0.034(2) 0.041(3) 0.059(3) 0.004(2) -0.012(2) 0.004(2) C15 0.045(3) 0.050(3) 0.039(2) -0.003(2) -0.006(2) -0.001(2) C16 0.028(2) 0.048(3) 0.076(4) 0.016(3) -0.005(2) 0.012(2) O7 0.077(3) 0.048(2) 0.065(3) -0.0052(19) -0.004(2) -0.004(2) C18 0.041(3) 0.047(3) 0.045(3) 0.001(2) -0.009(2) -0.001(2) C19 0.036(2) 0.048(3) 0.042(2) -0.003(2) -0.0080(19) 0.005(2) O8 0.064(3) 0.089(3) 0.058(2) -0.009(2) -0.018(2) -0.024(2) C21 0.045(3) 0.056(3) 0.040(3) 0.001(2) -0.005(2) -0.006(2) C22 0.038(3) 0.048(3) 0.067(3) 0.016(2) -0.008(2) 0.017(2) C23 0.034(2) 0.050(3) 0.043(3) 0.003(2) -0.0047(19) 0.004(2) C24 0.049(3) 0.049(3) 0.052(3) 0.006(2) -0.013(2) 0.000(2) C25 0.044(3) 0.064(3) 0.046(3) -0.003(2) -0.016(2) 0.007(2) C26 0.035(2) 0.058(3) 0.044(3) -0.004(2) -0.0059(19) 0.004(2) C27 0.039(3) 0.050(3) 0.061(3) 0.010(2) -0.013(2) 0.002(2) C28 0.046(3) 0.059(3) 0.050(3) -0.004(2) -0.014(2) 0.009(2) C29 0.030(2) 0.038(2) 0.064(3) 0.003(2) -0.010(2) 0.0069(19) C30 0.047(3) 0.074(4) 0.050(3) -0.006(3) -0.015(2) 0.013(3) C31 0.049(4) 0.089(5) 0.123(6) 0.060(5) 0.002(4) 0.030(3) C32 0.051(3) 0.084(4) 0.041(3) -0.007(3) -0.015(2) 0.009(3) C35 0.045(3) 0.104(6) 0.112(6) 0.047(5) 0.006(4) 0.035(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 O6 2.001(4) . ? Zn1 N1 2.024(3) . ? Zn1 O5 2.040(4) 2_565 ? Zn1 O9 2.053(4) 2_466 ? Zn1 O10 2.069(4) 1_654 ? Zn1 Zn1 2.9685(11) 2_565 ? S2 O7 1.439(4) . ? S2 O8 1.448(4) . ? S2 C15 1.763(6) . ? S2 C21 1.769(5) . ? N1 C29 1.334(6) . ? N1 C22 1.343(6) . ? C4 O6 1.251(5) . ? C4 O5 1.262(6) . ? C4 C19 1.503(7) . ? O5 Zn1 2.040(4) 2_565 ? O9 C18 1.267(6) . ? O9 Zn1 2.053(4) 2_466 ? O10 C18 1.263(6) . ? O10 Zn1 2.069(4) 1_456 ? C10 C16 1.375(7) . ? C10 C14 1.394(7) . ? C10 C12 1.493(6) . ? C12 C35 1.346(9) 2_755 ? C12 C31 1.361(8) . ? C13 C26 1.377(7) . ? C13 C19 1.400(7) . ? C13 H1 0.9400 . ? C14 C29 1.380(6) . ? C14 H2 0.9400 . ? C15 C24 1.389(7) . ? C15 C26 1.397(7) . ? C16 C22 1.374(6) . ? C16 H3 0.9400 . ? C18 C23 1.490(7) . ? C19 C27 1.408(7) . ? C21 C28 1.379(7) . ? C21 C32 1.384(7) . ? C22 H4 0.9400 . ? C23 C30 1.390(7) . ? C23 C25 1.397(7) . ? C24 C27 1.375(8) . ? C24 H5 0.9400 . ? C25 C28 1.378(7) . ? C25 H6 0.9400 . ? C26 H7 0.9400 . ? C27 H8 0.9400 . ? C28 H9 0.9400 . ? C29 H10 0.9400 . ? C30 C32 1.388(7) . ? C30 H11 0.9400 . ? C31 C35 1.392(8) . ? C31 H12 0.9400 . ? C32 H13 0.9400 . ? C35 C12 1.346(9) 2_755 ? C35 H14 0.9400 . ? 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 Zn1 N1 102.17(16) . . ? O6 Zn1 O5 159.07(14) . 2_565 ? N1 Zn1 O5 98.26(15) . 2_565 ? O6 Zn1 O9 87.97(16) . 2_466 ? N1 Zn1 O9 106.39(15) . 2_466 ? O5 Zn1 O9 90.60(16) 2_565 2_466 ? O6 Zn1 O10 89.43(16) . 1_654 ? N1 Zn1 O10 94.51(15) . 1_654 ? O5 Zn1 O10 84.47(16) 2_565 1_654 ? O9 Zn1 O10 159.02(15) 2_466 1_654 ? O6 Zn1 Zn1 83.29(10) . 2_565 ? N1 Zn1 Zn1 160.87(12) . 2_565 ? O5 Zn1 Zn1 75.89(10) 2_565 2_565 ? O9 Zn1 Zn1 92.00(11) 2_466 2_565 ? O10 Zn1 Zn1 67.02(10) 1_654 2_565 ? O7 S2 O8 120.4(3) . . ? O7 S2 C15 107.9(3) . . ? O8 S2 C15 107.8(3) . . ? O7 S2 C21 108.8(3) . . ? O8 S2 C21 108.5(3) . . ? C15 S2 C21 101.8(2) . . ? C29 N1 C22 117.6(4) . . ? C29 N1 Zn1 124.3(3) . . ? C22 N1 Zn1 118.0(3) . . ? O6 C4 O5 126.0(5) . . ? O6 C4 C19 118.1(4) . . ? O5 C4 C19 115.9(4) . . ? C4 O5 Zn1 130.9(3) . 2_565 ? C18 O9 Zn1 111.7(3) . 2_466 ? C18 O10 Zn1 144.2(3) . 1_456 ? C4 O6 Zn1 123.5(3) . . ? C16 C10 C14 117.1(4) . . ? C16 C10 C12 119.8(4) . . ? C14 C10 C12 123.1(5) . . ? C35 C12 C31 118.0(5) 2_755 . ? C35 C12 C10 121.9(5) 2_755 . ? C31 C12 C10 120.1(5) . . ? C26 C13 C19 120.7(5) . . ? C26 C13 H1 119.7 . . ? C19 C13 H1 119.7 . . ? C29 C14 C10 119.1(5) . . ? C29 C14 H2 120.5 . . ? C10 C14 H2 120.5 . . ? C24 C15 C26 120.5(5) . . ? C24 C15 S2 120.6(4) . . ? C26 C15 S2 118.9(4) . . ? C22 C16 C10 120.8(5) . . ? C22 C16 H3 119.6 . . ? C10 C16 H3 119.6 . . ? O10 C18 O9 124.3(5) . . ? O10 C18 C23 116.3(4) . . ? O9 C18 C23 119.4(5) . . ? C13 C19 C27 118.9(5) . . ? C13 C19 C4 120.5(5) . . ? C27 C19 C4 120.6(4) . . ? C28 C21 C32 121.4(5) . . ? C28 C21 S2 118.5(4) . . ? C32 C21 S2 120.0(4) . . ? N1 C22 C16 122.1(5) . . ? N1 C22 H4 119.0 . . ? C16 C22 H4 119.0 . . ? C30 C23 C25 118.7(5) . . ? C30 C23 C18 121.4(4) . . ? C25 C23 C18 119.9(5) . . ? C27 C24 C15 119.9(5) . . ? C27 C24 H5 120.1 . . ? C15 C24 H5 120.1 . . ? C28 C25 C23 121.5(5) . . ? C28 C25 H6 119.2 . . ? C23 C25 H6 119.2 . . ? C13 C26 C15 119.4(5) . . ? C13 C26 H7 120.3 . . ? C15 C26 H7 120.3 . . ? C24 C27 C19 120.4(5) . . ? C24 C27 H8 119.8 . . ? C19 C27 H8 119.8 . . ? C25 C28 C21 118.6(5) . . ? C25 C28 H9 120.7 . . ? C21 C28 H9 120.7 . . ? N1 C29 C14 123.3(5) . . ? N1 C29 H10 118.3 . . ? C14 C29 H10 118.3 . . ? C32 C30 C23 120.2(5) . . ? C32 C30 H11 119.9 . . ? C23 C30 H11 119.9 . . ? C12 C31 C35 120.1(7) . . ? C12 C31 H12 119.9 . . ? C35 C31 H12 119.9 . . ? C21 C32 C30 119.5(5) . . ? C21 C32 H13 120.3 . . ? C30 C32 H13 120.3 . . ? C12 C35 C31 121.8(6) 2_755 . ? C12 C35 H14 119.1 2_755 . ? C31 C35 H14 119.1 . . ? 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 Zn1 N1 C29 -6.8(4) . . . . ? O5 Zn1 N1 C29 177.7(4) 2_565 . . . ? O9 Zn1 N1 C29 84.6(4) 2_466 . . . ? O10 Zn1 N1 C29 -97.2(4) 1_654 . . . ? Zn1 Zn1 N1 C29 -111.7(5) 2_565 . . . ? O6 Zn1 N1 C22 176.3(4) . . . . ? O5 Zn1 N1 C22 0.9(4) 2_565 . . . ? O9 Zn1 N1 C22 -92.2(4) 2_466 . . . ? O10 Zn1 N1 C22 85.9(4) 1_654 . . . ? Zn1 Zn1 N1 C22 71.4(6) 2_565 . . . ? O6 C4 O5 Zn1 -9.3(8) . . . 2_565 ? C19 C4 O5 Zn1 173.1(3) . . . 2_565 ? O5 C4 O6 Zn1 5.2(7) . . . . ? C19 C4 O6 Zn1 -177.3(3) . . . . ? N1 Zn1 O6 C4 -161.9(4) . . . . ? O5 Zn1 O6 C4 5.4(7) 2_565 . . . ? O9 Zn1 O6 C4 91.8(4) 2_466 . . . ? O10 Zn1 O6 C4 -67.4(4) 1_654 . . . ? Zn1 Zn1 O6 C4 -0.5(4) 2_565 . . . ? C16 C10 C12 C35 150.0(7) . . . 2_755 ? C14 C10 C12 C35 -26.5(9) . . . 2_755 ? C16 C10 C12 C31 -28.2(9) . . . . ? C14 C10 C12 C31 155.2(7) . . . . ? C16 C10 C14 C29 -2.0(8) . . . . ? C12 C10 C14 C29 174.6(5) . . . . ? O7 S2 C15 C24 -16.6(5) . . . . ? O8 S2 C15 C24 -148.1(4) . . . . ? C21 S2 C15 C24 97.9(5) . . . . ? O7 S2 C15 C26 162.9(4) . . . . ? O8 S2 C15 C26 31.4(5) . . . . ? C21 S2 C15 C26 -82.7(4) . . . . ? C14 C10 C16 C22 2.1(9) . . . . ? C12 C10 C16 C22 -174.7(5) . . . . ? Zn1 O10 C18 O9 -13.6(10) 1_456 . . . ? Zn1 O10 C18 C23 166.3(4) 1_456 . . . ? Zn1 O9 C18 O10 9.5(7) 2_466 . . . ? Zn1 O9 C18 C23 -170.5(4) 2_466 . . . ? C26 C13 C19 C27 -3.6(8) . . . . ? C26 C13 C19 C4 175.7(4) . . . . ? O6 C4 C19 C13 177.9(5) . . . . ? O5 C4 C19 C13 -4.4(7) . . . . ? O6 C4 C19 C27 -2.8(7) . . . . ? O5 C4 C19 C27 175.0(5) . . . . ? O7 S2 C21 C28 35.4(6) . . . . ? O8 S2 C21 C28 168.1(5) . . . . ? C15 S2 C21 C28 -78.3(5) . . . . ? O7 S2 C21 C32 -148.9(5) . . . . ? O8 S2 C21 C32 -16.3(6) . . . . ? C15 S2 C21 C32 97.3(5) . . . . ? C29 N1 C22 C16 -2.0(9) . . . . ? Zn1 N1 C22 C16 175.0(5) . . . . ? C10 C16 C22 N1 0.0(10) . . . . ? O10 C18 C23 C30 172.8(5) . . . . ? O9 C18 C23 C30 -7.3(8) . . . . ? O10 C18 C23 C25 -6.7(8) . . . . ? O9 C18 C23 C25 173.3(5) . . . . ? C26 C15 C24 C27 -3.6(8) . . . . ? S2 C15 C24 C27 175.8(4) . . . . ? C30 C23 C25 C28 2.1(9) . . . . ? C18 C23 C25 C28 -178.4(5) . . . . ? C19 C13 C26 C15 -0.4(8) . . . . ? C24 C15 C26 C13 4.1(8) . . . . ? S2 C15 C26 C13 -175.4(4) . . . . ? C15 C24 C27 C19 -0.5(8) . . . . ? C13 C19 C27 C24 4.1(8) . . . . ? C4 C19 C27 C24 -175.3(5) . . . . ? C23 C25 C28 C21 -1.2(9) . . . . ? C32 C21 C28 C25 -0.2(9) . . . . ? S2 C21 C28 C25 175.3(5) . . . . ? C22 N1 C29 C14 2.1(8) . . . . ? Zn1 N1 C29 C14 -174.8(4) . . . . ? C10 C14 C29 N1 0.0(8) . . . . ? C25 C23 C30 C32 -1.6(9) . . . . ? C18 C23 C30 C32 178.9(6) . . . . ? C35 C12 C31 C35 -2.3(15) 2_755 . . . ? C10 C12 C31 C35 176.0(7) . . . . ? C28 C21 C32 C30 0.7(10) . . . . ? S2 C21 C32 C30 -174.8(5) . . . . ? C23 C30 C32 C21 0.2(10) . . . . ? C12 C31 C35 C12 2.4(15) . . . 2_755 ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.957 _refine_diff_density_min -1.018 _refine_diff_density_rms 0.107 #===END _publ_contact_author_name 'Susumu Kitagawa' _publ_contact_author_address ; Department of Synthetic Chemistry and Biological Chemistry Graduate School of Engineering, Kyoto University Katsura, Nishikyo-ku Kyoto 615-8510 JAPAN ; _publ_contact_author_email KITAGAWA@SBCHEM.KYOTO-U.AC.JP _publ_section_title ; title ; loop_ _publ_author_name ; 'Susumu Kitagawa' ; _publ_author_address ; Department of Synthetic Chemistry and Biological Chemistry Graduate School of Engineering, Kyoto University Katsura, Nishikyo-ku Kyoto 615-8510 JAPAN ; data_Zn_SDB_bpt _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H19 N4 O7 S Zn' _chemical_formula_weight 560.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3068(12) _cell_length_b 12.984(2) _cell_length_c 14.251(2) _cell_angle_alpha 77.487(6) _cell_angle_beta 77.231(6) _cell_angle_gamma 88.687(7) _cell_volume 1286.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 574 _exptl_absorpt_coefficient_mu 1.084 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8124 _exptl_absorpt_correction_T_max 0.8124 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10345 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5639 _reflns_number_gt 5116 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'Sir-97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1083P)^2^+3.0117P] 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 5639 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1897 _refine_ls_wR_factor_gt 0.1860 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _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 0.81347(5) -0.01522(3) 0.07066(3) 0.02024(16) Uani 1 1 d . . . S2 S 0.6511(2) 0.58436(8) -0.32271(9) 0.0417(3) Uani 1 1 d . . . O3 O 0.7693(4) 0.1235(2) -0.0218(2) 0.0291(6) Uani 1 1 d . . . N1 N 0.5988(4) -0.0235(2) 0.1907(2) 0.0210(6) Uani 1 1 d . . . O11 O 0.7201(4) 0.9013(2) -0.0164(2) 0.0299(6) Uani 1 1 d . . . C35 C 0.9631(7) 0.3474(4) -0.2151(4) 0.0402(10) Uani 1 1 d . . . H1 H 1.0906 0.3302 -0.2250 0.048 Uiso 1 1 calc R . . C36 C 0.5613(6) 0.7112(3) -0.1894(3) 0.0350(9) Uani 1 1 d . . . H2 H 0.4379 0.6846 -0.1777 0.042 Uiso 1 1 calc R . . O12 O 1.0021(4) 0.9295(2) -0.1174(2) 0.0326(6) Uani 1 1 d . . . C9 C 0.9095(8) 0.4410(4) -0.2679(4) 0.0442(11) Uani 1 1 d . . . H3 H 0.9997 0.4875 -0.3139 0.053 Uiso 1 1 calc R . . O10 O 1.0539(4) 0.1488(2) -0.1222(2) 0.0346(7) Uani 1 1 d . . . C12 C 0.8403(5) 0.8885(3) -0.0903(3) 0.0237(7) Uani 1 1 d . . . C13 C 0.6235(5) 0.0124(3) 0.2692(3) 0.0284(8) Uani 1 1 d . . . H4 H 0.7444 0.0349 0.2700 0.034 Uiso 1 1 calc R . . N3 N -0.1671(5) -0.0469(3) 0.5053(3) 0.0353(8) Uani 1 1 d . . . C15 C 0.3001(5) -0.0173(3) 0.3482(3) 0.0242(7) Uani 1 1 d . . . C16 C 0.2758(5) -0.0588(3) 0.2694(3) 0.0260(7) Uani 1 1 d . . . H5 H 0.1582 -0.0861 0.2688 0.031 Uiso 1 1 calc R . . C17 C 0.8294(6) 0.2785(3) -0.1475(3) 0.0281(8) Uani 1 1 d . . . C18 C 0.4275(5) -0.0591(3) 0.1924(3) 0.0234(7) Uani 1 1 d . . . H6 H 0.4099 -0.0856 0.1385 0.028 Uiso 1 1 calc R . . C19 C 0.4776(5) 0.0171(4) 0.3486(3) 0.0299(8) Uani 1 1 d . . . H7 H 0.4987 0.0434 0.4019 0.036 Uiso 1 1 calc R . . C20 C 0.7881(6) 0.8185(3) -0.1528(3) 0.0260(7) Uani 1 1 d . . . C21 C 0.6406(6) 0.3049(3) -0.1328(3) 0.0326(9) Uani 1 1 d . . . H8 H 0.5493 0.2588 -0.0872 0.039 Uiso 1 1 calc R . . N4 N -0.0241(5) -0.0552(3) 0.4323(3) 0.0344(8) Uani 1 1 d . . . O13 O 0.4514(6) 0.5763(3) -0.3124(3) 0.0552(11) Uani 1 1 d . . . C25 C 0.8894(5) 0.1755(3) -0.0922(3) 0.0249(7) Uani 1 1 d . . . C26 C 0.7218(7) 0.4656(3) -0.2523(3) 0.0348(9) Uani 1 1 d . . . C27 C 0.5880(7) 0.3990(3) -0.1856(3) 0.0363(9) Uani 1 1 d . . . H9 H 0.4609 0.4172 -0.1757 0.044 Uiso 1 1 calc R . . C29 C 0.7007(7) 0.6820(3) -0.2609(3) 0.0339(9) Uani 1 1 d . . . C31 C 0.1386(5) -0.0078(3) 0.4302(3) 0.0266(8) Uani 1 1 d . . . C34 C 0.6043(6) 0.7800(3) -0.1350(3) 0.0289(8) Uani 1 1 d . . . H10 H 0.5103 0.8005 -0.0864 0.035 Uiso 1 1 calc R . . O14 O 0.7742(7) 0.6039(3) -0.4184(3) 0.0590(12) Uani 1 1 d . . . O15 O 0.2834(7) 0.8175(3) 0.5709(3) 0.0582(10) Uani 1 1 d . . . C37 C 0.8817(7) 0.7231(4) -0.2823(3) 0.0398(10) Uani 1 1 d . . . H11 H 0.9739 0.7049 -0.3330 0.048 Uiso 1 1 calc R . . C38 C 0.9245(6) 0.7910(4) -0.2282(3) 0.0359(9) Uani 1 1 d . . . H12 H 1.0472 0.8194 -0.2421 0.043 Uiso 1 1 calc R . . N2 N 0.4097(8) 0.7228(4) 0.4570(3) 0.0538(12) Uani 1 1 d . . . C39 C 0.4183(9) 0.7861(4) 0.5186(4) 0.0485(12) Uani 1 1 d . . . H19 H 0.5380 0.8080 0.5218 0.058 Uiso 1 1 calc R . . C40 C 0.2328(12) 0.6813(6) 0.4513(6) 0.082(2) Uani 1 1 d . . . H13 H 0.2140 0.6094 0.4896 0.123 Uiso 1 1 calc R . . H14 H 0.2327 0.6822 0.3831 0.123 Uiso 1 1 calc R . . H15 H 0.1324 0.7244 0.4774 0.123 Uiso 1 1 calc R . . C41 C 0.5768(12) 0.6912(7) 0.3943(5) 0.082(2) Uani 1 1 d . . . H16 H 0.6864 0.7266 0.4020 0.123 Uiso 1 1 calc R . . H17 H 0.5663 0.7104 0.3261 0.123 Uiso 1 1 calc R . . H18 H 0.5894 0.6154 0.4131 0.123 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 0.0173(2) 0.0232(3) 0.0186(2) -0.00666(16) 0.00128(15) 0.00156(15) S2 0.0754(8) 0.0217(5) 0.0394(6) -0.0105(4) -0.0338(6) 0.0082(5) O3 0.0270(13) 0.0254(14) 0.0314(14) -0.0012(11) -0.0044(11) 0.0031(11) N1 0.0180(13) 0.0246(15) 0.0186(13) -0.0057(11) 0.0007(11) 0.0016(11) O11 0.0286(14) 0.0340(15) 0.0296(14) -0.0158(12) -0.0029(11) -0.0002(11) C35 0.035(2) 0.033(2) 0.047(3) -0.0011(19) -0.0048(19) 0.0008(18) C36 0.038(2) 0.029(2) 0.044(2) -0.0116(18) -0.0167(19) -0.0011(17) O12 0.0273(14) 0.0416(17) 0.0315(14) -0.0159(12) -0.0032(11) -0.0069(12) C9 0.051(3) 0.028(2) 0.050(3) 0.0008(19) -0.011(2) -0.002(2) O10 0.0298(14) 0.0305(16) 0.0372(15) -0.0010(12) -0.0012(12) 0.0089(12) C12 0.0253(17) 0.0228(18) 0.0239(16) -0.0064(14) -0.0064(13) 0.0003(13) C13 0.0184(16) 0.045(2) 0.0226(17) -0.0141(16) 0.0008(14) -0.0029(15) N3 0.0236(16) 0.054(2) 0.0282(17) -0.0201(16) 0.0051(13) -0.0038(15) C15 0.0224(16) 0.0284(19) 0.0191(15) -0.0051(14) 0.0011(13) 0.0024(14) C16 0.0197(16) 0.034(2) 0.0240(17) -0.0077(15) -0.0020(13) -0.0017(14) C17 0.0321(19) 0.0242(19) 0.0297(18) -0.0079(15) -0.0088(15) 0.0042(15) C18 0.0189(16) 0.0290(19) 0.0208(16) -0.0071(14) 0.0000(13) 0.0010(13) C19 0.0238(17) 0.045(2) 0.0222(17) -0.0146(16) -0.0002(14) -0.0018(16) C20 0.0319(19) 0.0222(18) 0.0248(17) -0.0080(14) -0.0055(14) 0.0013(14) C21 0.035(2) 0.030(2) 0.032(2) -0.0063(16) -0.0067(16) 0.0071(16) N4 0.0240(16) 0.052(2) 0.0267(16) -0.0176(15) 0.0053(13) -0.0048(15) O13 0.077(3) 0.0323(18) 0.076(3) -0.0169(17) -0.055(2) 0.0125(17) C25 0.0254(17) 0.0241(18) 0.0269(17) -0.0086(14) -0.0067(14) 0.0024(14) C26 0.053(3) 0.0218(19) 0.036(2) -0.0105(16) -0.0214(19) 0.0052(18) C27 0.041(2) 0.031(2) 0.040(2) -0.0102(18) -0.0147(19) 0.0129(18) C29 0.054(3) 0.0193(18) 0.034(2) -0.0087(16) -0.0186(19) 0.0033(17) C31 0.0217(16) 0.035(2) 0.0209(16) -0.0068(14) 0.0015(13) 0.0006(15) C34 0.0308(19) 0.0254(19) 0.0309(19) -0.0073(15) -0.0070(15) 0.0023(15) O14 0.119(4) 0.0328(18) 0.0327(17) -0.0097(14) -0.030(2) 0.010(2) O15 0.074(3) 0.051(2) 0.057(2) -0.0252(19) -0.016(2) 0.005(2) C37 0.054(3) 0.034(2) 0.031(2) -0.0149(18) -0.0009(19) 0.000(2) C38 0.035(2) 0.037(2) 0.036(2) -0.0172(18) 0.0015(17) -0.0036(18) N2 0.082(3) 0.046(3) 0.037(2) -0.0135(19) -0.018(2) 0.008(2) C39 0.069(3) 0.038(3) 0.043(3) -0.010(2) -0.021(2) 0.007(2) C40 0.100(6) 0.074(5) 0.081(5) -0.041(4) -0.013(4) -0.019(4) C41 0.100(6) 0.103(6) 0.055(4) -0.036(4) -0.026(4) 0.040(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.035(3) . ? Zn1 O11 2.042(3) 1_545 ? Zn1 O10 2.043(3) 2_755 ? Zn1 O3 2.054(3) . ? Zn1 O12 2.070(3) 2_765 ? Zn1 Zn1 2.9867(8) 2_755 ? S2 O14 1.432(4) . ? S2 O13 1.438(4) . ? S2 C29 1.778(4) . ? S2 C26 1.781(4) . ? O3 C25 1.255(5) . ? N1 C18 1.338(5) . ? N1 C13 1.348(5) . ? O11 C12 1.252(5) . ? O11 Zn1 2.042(3) 1_565 ? C35 C9 1.381(7) . ? C35 C17 1.391(6) . ? C35 H1 0.9400 . ? C36 C29 1.383(7) . ? C36 C34 1.384(6) . ? C36 H2 0.9400 . ? O12 C12 1.252(5) . ? O12 Zn1 2.070(3) 2_765 ? C9 C26 1.381(7) . ? C9 H3 0.9400 . ? O10 C25 1.251(5) . ? O10 Zn1 2.043(3) 2_755 ? C12 C20 1.512(5) . ? C13 C19 1.384(5) . ? C13 H4 0.9400 . ? N3 N4 1.322(5) . ? N3 C31 1.330(5) 2_556 ? C15 C19 1.383(5) . ? C15 C16 1.391(5) . ? C15 C31 1.490(5) . ? C16 C18 1.377(5) . ? C16 H5 0.9400 . ? C17 C21 1.395(6) . ? C17 C25 1.507(5) . ? C18 H6 0.9400 . ? C19 H7 0.9400 . ? C20 C34 1.394(6) . ? C20 C38 1.397(5) . ? C21 C27 1.384(6) . ? C21 H8 0.9400 . ? N4 C31 1.342(5) . ? C26 C27 1.371(7) . ? C27 H9 0.9400 . ? C29 C37 1.383(7) . ? C31 N3 1.330(5) 2_556 ? C34 H10 0.9400 . ? O15 C39 1.217(7) . ? C37 C38 1.371(6) . ? C37 H11 0.9400 . ? C38 H12 0.9400 . ? N2 C39 1.338(7) . ? N2 C40 1.436(9) . ? N2 C41 1.453(9) . ? C39 H19 0.9400 . ? C40 H13 0.9700 . ? C40 H14 0.9700 . ? C40 H15 0.9700 . ? C41 H16 0.9700 . ? C41 H17 0.9700 . ? C41 H18 0.9700 . ? 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 N1 Zn1 O11 105.31(12) . 1_545 ? N1 Zn1 O10 97.81(12) . 2_755 ? O11 Zn1 O10 86.89(13) 1_545 2_755 ? N1 Zn1 O3 103.45(12) . . ? O11 Zn1 O3 90.07(12) 1_545 . ? O10 Zn1 O3 158.57(12) 2_755 . ? N1 Zn1 O12 96.27(12) . 2_765 ? O11 Zn1 O12 158.33(12) 1_545 2_765 ? O10 Zn1 O12 88.33(13) 2_755 2_765 ? O3 Zn1 O12 86.71(12) . 2_765 ? N1 Zn1 Zn1 164.69(9) . 2_755 ? O11 Zn1 Zn1 89.44(8) 1_545 2_755 ? O10 Zn1 Zn1 78.59(9) 2_755 2_755 ? O3 Zn1 Zn1 80.17(8) . 2_755 ? O12 Zn1 Zn1 68.89(8) 2_765 2_755 ? O14 S2 O13 120.4(3) . . ? O14 S2 C29 108.0(2) . . ? O13 S2 C29 108.9(2) . . ? O14 S2 C26 107.5(2) . . ? O13 S2 C26 107.6(2) . . ? C29 S2 C26 103.12(19) . . ? C25 O3 Zn1 126.1(3) . . ? C18 N1 C13 118.1(3) . . ? C18 N1 Zn1 121.4(2) . . ? C13 N1 Zn1 120.4(2) . . ? C12 O11 Zn1 114.9(2) . 1_565 ? C9 C35 C17 120.3(4) . . ? C9 C35 H1 119.8 . . ? C17 C35 H1 119.8 . . ? C29 C36 C34 119.7(4) . . ? C29 C36 H2 120.1 . . ? C34 C36 H2 120.1 . . ? C12 O12 Zn1 141.1(3) . 2_765 ? C26 C9 C35 119.3(5) . . ? C26 C9 H3 120.4 . . ? C35 C9 H3 120.4 . . ? C25 O10 Zn1 128.9(3) . 2_755 ? O12 C12 O11 125.3(3) . . ? O12 C12 C20 116.6(3) . . ? O11 C12 C20 118.1(3) . . ? N1 C13 C19 122.4(3) . . ? N1 C13 H4 118.8 . . ? C19 C13 H4 118.8 . . ? N4 N3 C31 117.6(3) . 2_556 ? C19 C15 C16 118.8(3) . . ? C19 C15 C31 120.0(3) . . ? C16 C15 C31 121.2(3) . . ? C18 C16 C15 118.7(3) . . ? C18 C16 H5 120.6 . . ? C15 C16 H5 120.6 . . ? C35 C17 C21 119.5(4) . . ? C35 C17 C25 119.8(4) . . ? C21 C17 C25 120.7(4) . . ? N1 C18 C16 122.9(3) . . ? N1 C18 H6 118.5 . . ? C16 C18 H6 118.5 . . ? C15 C19 C13 118.9(3) . . ? C15 C19 H7 120.6 . . ? C13 C19 H7 120.6 . . ? C34 C20 C38 119.6(4) . . ? C34 C20 C12 120.3(3) . . ? C38 C20 C12 120.1(4) . . ? C27 C21 C17 119.9(4) . . ? C27 C21 H8 120.1 . . ? C17 C21 H8 120.1 . . ? N3 N4 C31 116.9(3) . . ? O10 C25 O3 126.1(4) . . ? O10 C25 C17 116.6(3) . . ? O3 C25 C17 117.3(3) . . ? C27 C26 C9 121.3(4) . . ? C27 C26 S2 119.2(4) . . ? C9 C26 S2 119.4(4) . . ? C26 C27 C21 119.7(4) . . ? C26 C27 H9 120.1 . . ? C21 C27 H9 120.1 . . ? C37 C29 C36 121.4(4) . . ? C37 C29 S2 118.7(3) . . ? C36 C29 S2 119.8(4) . . ? N3 C31 N4 125.5(3) 2_556 . ? N3 C31 C15 117.5(4) 2_556 . ? N4 C31 C15 116.9(3) . . ? C36 C34 C20 119.5(4) . . ? C36 C34 H10 120.3 . . ? C20 C34 H10 120.3 . . ? C38 C37 C29 118.9(4) . . ? C38 C37 H11 120.6 . . ? C29 C37 H11 120.6 . . ? C37 C38 C20 120.8(4) . . ? C37 C38 H12 119.6 . . ? C20 C38 H12 119.6 . . ? C39 N2 C40 120.9(6) . . ? C39 N2 C41 122.2(6) . . ? C40 N2 C41 116.9(6) . . ? O15 C39 N2 125.2(6) . . ? O15 C39 H19 117.4 . . ? N2 C39 H19 117.4 . . ? N2 C40 H13 109.5 . . ? N2 C40 H14 109.5 . . ? H13 C40 H14 109.5 . . ? N2 C40 H15 109.5 . . ? H13 C40 H15 109.5 . . ? H14 C40 H15 109.5 . . ? N2 C41 H16 109.5 . . ? N2 C41 H17 109.5 . . ? H16 C41 H17 109.5 . . ? N2 C41 H18 109.5 . . ? H16 C41 H18 109.5 . . ? H17 C41 H18 109.5 . . ? 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 N1 Zn1 O3 C25 160.1(3) . . . . ? O11 Zn1 O3 C25 -94.2(3) 1_545 . . . ? O10 Zn1 O3 C25 -12.5(5) 2_755 . . . ? O12 Zn1 O3 C25 64.4(3) 2_765 . . . ? Zn1 Zn1 O3 C25 -4.7(3) 2_755 . . . ? O11 Zn1 N1 C18 -12.1(3) 1_545 . . . ? O10 Zn1 N1 C18 -101.0(3) 2_755 . . . ? O3 Zn1 N1 C18 81.7(3) . . . . ? O12 Zn1 N1 C18 169.9(3) 2_765 . . . ? Zn1 Zn1 N1 C18 -176.2(2) 2_755 . . . ? O11 Zn1 N1 C13 171.4(3) 1_545 . . . ? O10 Zn1 N1 C13 82.5(3) 2_755 . . . ? O3 Zn1 N1 C13 -94.7(3) . . . . ? O12 Zn1 N1 C13 -6.6(3) 2_765 . . . ? Zn1 Zn1 N1 C13 7.3(6) 2_755 . . . ? C17 C35 C9 C26 0.3(8) . . . . ? Zn1 O12 C12 O11 9.0(7) 2_765 . . . ? Zn1 O12 C12 C20 -171.1(3) 2_765 . . . ? Zn1 O11 C12 O12 -6.2(5) 1_565 . . . ? Zn1 O11 C12 C20 174.0(3) 1_565 . . . ? C18 N1 C13 C19 -2.6(6) . . . . ? Zn1 N1 C13 C19 174.0(3) . . . . ? C19 C15 C16 C18 -3.2(6) . . . . ? C31 C15 C16 C18 175.6(4) . . . . ? C9 C35 C17 C21 -0.3(7) . . . . ? C9 C35 C17 C25 178.5(4) . . . . ? C13 N1 C18 C16 1.3(6) . . . . ? Zn1 N1 C18 C16 -175.2(3) . . . . ? C15 C16 C18 N1 1.6(6) . . . . ? C16 C15 C19 C13 2.1(6) . . . . ? C31 C15 C19 C13 -176.8(4) . . . . ? N1 C13 C19 C15 0.9(7) . . . . ? O12 C12 C20 C34 -172.3(4) . . . . ? O11 C12 C20 C34 7.5(5) . . . . ? O12 C12 C20 C38 8.4(6) . . . . ? O11 C12 C20 C38 -171.8(4) . . . . ? C35 C17 C21 C27 0.0(6) . . . . ? C25 C17 C21 C27 -178.8(4) . . . . ? C31 N3 N4 C31 0.3(7) 2_556 . . . ? Zn1 O10 C25 O3 0.1(6) 2_755 . . . ? Zn1 O10 C25 C17 -178.4(3) 2_755 . . . ? Zn1 O3 C25 O10 4.6(6) . . . . ? Zn1 O3 C25 C17 -176.9(2) . . . . ? C35 C17 C25 O10 -11.8(6) . . . . ? C21 C17 C25 O10 167.1(4) . . . . ? C35 C17 C25 O3 169.6(4) . . . . ? C21 C17 C25 O3 -11.6(5) . . . . ? C35 C9 C26 C27 0.0(7) . . . . ? C35 C9 C26 S2 -178.2(4) . . . . ? O14 S2 C26 C27 -145.0(4) . . . . ? O13 S2 C26 C27 -14.0(4) . . . . ? C29 S2 C26 C27 101.0(4) . . . . ? O14 S2 C26 C9 33.2(4) . . . . ? O13 S2 C26 C9 164.2(4) . . . . ? C29 S2 C26 C9 -80.7(4) . . . . ? C9 C26 C27 C21 -0.3(7) . . . . ? S2 C26 C27 C21 177.9(3) . . . . ? C17 C21 C27 C26 0.3(6) . . . . ? C34 C36 C29 C37 -2.6(7) . . . . ? C34 C36 C29 S2 174.1(3) . . . . ? O14 S2 C29 C37 -30.7(4) . . . . ? O13 S2 C29 C37 -163.0(4) . . . . ? C26 S2 C29 C37 82.9(4) . . . . ? O14 S2 C29 C36 152.6(4) . . . . ? O13 S2 C29 C36 20.2(4) . . . . ? C26 S2 C29 C36 -93.8(4) . . . . ? N3 N4 C31 N3 -0.3(7) . . . 2_556 ? N3 N4 C31 C15 179.9(4) . . . . ? C19 C15 C31 N3 8.8(6) . . . 2_556 ? C16 C15 C31 N3 -170.0(4) . . . 2_556 ? C19 C15 C31 N4 -171.4(4) . . . . ? C16 C15 C31 N4 9.8(6) . . . . ? C29 C36 C34 C20 -0.3(6) . . . . ? C38 C20 C34 C36 2.8(6) . . . . ? C12 C20 C34 C36 -176.5(4) . . . . ? C36 C29 C37 C38 2.7(7) . . . . ? S2 C29 C37 C38 -174.0(4) . . . . ? C29 C37 C38 C20 -0.1(7) . . . . ? C34 C20 C38 C37 -2.7(7) . . . . ? C12 C20 C38 C37 176.6(4) . . . . ? C40 N2 C39 O15 -3.1(9) . . . . ? C41 N2 C39 O15 177.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 5.336 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.150 #===END _publ_contact_author_name 'Susumu Kitagawa' _publ_contact_author_address ; Department of Synthetic Chemistry and Biological Chemistry Graduate School of Engineering, Kyoto University Katsura, Nishikyo-ku Kyoto 615-8510 JAPAN ; _publ_contact_author_email KITAGAWA@SBCHEM.KYOTO-U.AC.JP _publ_section_title ; title ; loop_ _publ_author_name ; 'Susumu Kitagawa' ; _publ_author_address ; Department of Synthetic Chemistry and Biological Chemistry Graduate School of Engineering, Kyoto University Katsura, Nishikyo-ku Kyoto 615-8510 JAPAN ; data_Zn_SDB_bpy _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H24 N2 O12 S2 Zn2' _chemical_formula_weight 895.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.271(6) _cell_length_b 22.155(4) _cell_length_c 12.549(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.764(2) _cell_angle_gamma 90.00 _cell_volume 7600(3) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3632 _exptl_absorpt_coefficient_mu 1.438 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7618 _exptl_absorpt_correction_T_max 0.7618 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30579 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.51 _reflns_number_total 8450 _reflns_number_gt 6639 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR-97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 8450 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.2585 _refine_ls_wR_factor_gt 0.2479 _refine_ls_goodness_of_fit_ref 1.699 _refine_ls_restrained_S_all 1.699 _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 0.18922(2) 0.23946(2) -0.34138(5) 0.0201(2) Uani 1 1 d . . . Zn2 Zn 0.08373(2) 0.26225(3) -0.40350(5) 0.0215(2) Uani 1 1 d . . . S3 S 0.17876(5) 0.51025(6) 0.14910(10) 0.0280(3) Uani 1 1 d . . . S4 S 0.10179(6) -0.01112(6) 0.10945(11) 0.0320(3) Uani 1 1 d . . . O5 O 0.19006(14) 0.30266(17) 0.5435(3) 0.0317(9) Uani 1 1 d . . . O6 O 0.10918(13) 0.31998(17) 0.4958(3) 0.0304(9) Uani 1 1 d . . . N21 N 0.51087(16) 0.2309(2) 0.0217(4) 0.0271(10) Uani 1 1 d . . . O8 O 0.16444(13) 0.18253(18) -0.2406(3) 0.0326(9) Uani 1 1 d . . . O9 O 0.09573(15) 0.19299(18) 0.4978(3) 0.0360(9) Uani 1 1 d . . . O10 O 0.17579(14) 0.17597(18) 0.5385(3) 0.0345(9) Uani 1 1 d . . . N22 N 0.26177(16) 0.23609(19) -0.2642(4) 0.0247(10) Uani 1 1 d . . . O13 O 0.08372(14) 0.19855(18) -0.2855(3) 0.0346(9) Uani 1 1 d . . . C14 C 0.1071(2) 0.0405(2) 0.0042(4) 0.0274(11) Uani 1 1 d . . . O15 O 0.22886(15) 0.53037(19) 0.1706(3) 0.0389(10) Uani 1 1 d . . . O16 O 0.14018(15) 0.55382(17) 0.1329(3) 0.0363(10) Uani 1 1 d . . . C96 C 0.17197(19) 0.4606(2) 0.2558(4) 0.0247(11) Uani 1 1 d . . . C98 C 0.1100(2) 0.0371(2) 0.2252(4) 0.0271(11) Uani 1 1 d . . . C97 C 0.20684(18) 0.3884(2) 0.3948(4) 0.0258(11) Uani 1 1 d . . . H1 H 0.2340 0.3676 0.4379 0.031 Uiso 1 1 calc R . . O17 O 0.14275(17) -0.05116(17) 0.1302(3) 0.0417(11) Uani 1 1 d . . . C22 C 0.1662(2) 0.4623(2) 0.0321(4) 0.0289(12) Uani 1 1 d . . . O18 O 0.05274(15) -0.03432(19) 0.0826(3) 0.0420(10) Uani 1 1 d . . . C24 C 0.12381(19) 0.1183(2) 0.3965(4) 0.0264(11) Uani 1 1 d . . . C25 C 0.15950(18) 0.3771(2) 0.4094(4) 0.0250(11) Uani 1 1 d . . . C26 C 0.1531(2) 0.3299(2) 0.4888(4) 0.0277(11) Uani 1 1 d . . . C27 C 0.21334(18) 0.4296(2) 0.3183(4) 0.0259(11) Uani 1 1 d . . . H2 H 0.2446 0.4369 0.3077 0.031 Uiso 1 1 calc R . . C28 C 0.11661(19) 0.1247(2) -0.1510(4) 0.0263(11) Uani 1 1 d . . . C29 C 0.12055(19) 0.4089(2) 0.3470(4) 0.0298(12) Uani 1 1 d . . . H3 H 0.0890 0.4023 0.3562 0.036 Uiso 1 1 calc R . . C30 C 0.1321(2) 0.1660(2) 0.4855(4) 0.0277(11) Uani 1 1 d . . . C32 C 0.0696(2) 0.0660(3) 0.2476(5) 0.0349(13) Uani 1 1 d . . . H4 H 0.0377 0.0584 0.2046 0.042 Uiso 1 1 calc R . . C33 C 0.1219(2) 0.1720(2) -0.2327(4) 0.0282(12) Uani 1 1 d . . . C34 C 0.35969(18) 0.2334(3) -0.1506(5) 0.0280(12) Uani 1 1 d . . . C35 C 0.14800(19) 0.3827(2) -0.1425(4) 0.0266(11) Uani 1 1 d . . . C36 C 0.1099(2) 0.4068(3) -0.1045(5) 0.0360(14) Uani 1 1 d . . . H5 H 0.0774 0.3962 -0.1383 0.043 Uiso 1 1 calc R . . C37 C 0.0703(2) 0.1058(3) -0.1453(5) 0.0412(15) Uani 1 1 d . . . H6 H 0.0424 0.1219 -0.1945 0.049 Uiso 1 1 calc R . . C38 C 0.2052(2) 0.4399(2) -0.0064(4) 0.0301(12) Uani 1 1 d . . . H7 H 0.2375 0.4517 0.0272 0.036 Uiso 1 1 calc R . . C39 C 0.1274(2) 0.4506(2) 0.2708(4) 0.0302(12) Uani 1 1 d . . . H8 H 0.1005 0.4724 0.2289 0.036 Uiso 1 1 calc R . . C40 C 0.1202(2) 0.4463(3) -0.0170(5) 0.0358(14) Uani 1 1 d . . . H9 H 0.0944 0.4623 0.0088 0.043 Uiso 1 1 calc R . . C41 C 0.1633(2) 0.0885(3) 0.3747(5) 0.0371(14) Uani 1 1 d . . . H10 H 0.1950 0.0958 0.4190 0.045 Uiso 1 1 calc R . . C42 C 0.1565(2) 0.0478(3) 0.2881(5) 0.0395(14) Uani 1 1 d . . . H11 H 0.1834 0.0280 0.2727 0.047 Uiso 1 1 calc R . . C43 C 0.2954(2) 0.2571(3) -0.3084(5) 0.0365(14) Uani 1 1 d . . . H12 H 0.2856 0.2744 -0.3790 0.044 Uiso 1 1 calc R . . C44 C 0.1955(2) 0.4005(3) -0.0937(4) 0.0326(12) Uani 1 1 d . . . H13 H 0.2213 0.3855 -0.1206 0.039 Uiso 1 1 calc R . . C45 C 0.1532(2) 0.0581(3) -0.0025(5) 0.0446(16) Uani 1 1 d . . . H14 H 0.1814 0.0416 0.0451 0.054 Uiso 1 1 calc R . . C46 C 0.0779(2) 0.1059(3) 0.3346(5) 0.0363(13) Uani 1 1 d . . . H15 H 0.0510 0.1251 0.3517 0.044 Uiso 1 1 calc R . . C47 C 0.3247(2) 0.2111(4) -0.1047(6) 0.068(3) Uani 1 1 d . . . H16 H 0.3334 0.1949 -0.0331 0.082 Uiso 1 1 calc R . . C48 C 0.1569(2) 0.1001(3) -0.0800(5) 0.0438(16) Uani 1 1 d . . . H17 H 0.1881 0.1124 -0.0846 0.053 Uiso 1 1 calc R . . C49 C 0.2756(2) 0.2123(4) -0.1642(6) 0.063(3) Uani 1 1 d . . . H18 H 0.2518 0.1957 -0.1325 0.075 Uiso 1 1 calc R . . C50 C 0.41232(19) 0.2322(3) -0.0914(4) 0.0292(12) Uani 1 1 d . . . C51 C 0.0651(2) 0.0633(3) -0.0672(5) 0.0386(14) Uani 1 1 d . . . H19 H 0.0340 0.0503 -0.0631 0.046 Uiso 1 1 calc R . . C52 C 0.4762(3) 0.2417(4) 0.0726(6) 0.057(2) Uani 1 1 d . . . H20 H 0.4855 0.2495 0.1488 0.068 Uiso 1 1 calc R . . C53 C 0.3444(2) 0.2551(3) -0.2568(5) 0.0440(17) Uani 1 1 d . . . H21 H 0.3675 0.2685 -0.2937 0.053 Uiso 1 1 calc R . . C55 C 0.4272(3) 0.2422(4) 0.0203(6) 0.061(2) Uani 1 1 d . . . H22 H 0.4039 0.2493 0.0607 0.073 Uiso 1 1 calc R . . C59 C 0.4959(2) 0.2171(5) -0.0846(7) 0.091(4) Uani 1 1 d . . . H23 H 0.5195 0.2062 -0.1220 0.110 Uiso 1 1 calc R . . C60 C 0.4478(3) 0.2178(5) -0.1424(6) 0.085(3) Uani 1 1 d . . . H24 H 0.4392 0.2083 -0.2179 0.102 Uiso 1 1 calc R . . O19 O 0.09375(15) 0.32648(18) -0.2849(3) 0.0375(10) Uani 1 1 d . . . O20 O 0.17448(17) 0.30837(19) -0.2457(3) 0.0430(11) Uani 1 1 d . . . C99 C 0.1375(2) 0.3359(2) -0.2318(4) 0.0336(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0182(4) 0.0233(3) 0.0176(3) 0.0009(2) 0.0022(2) 0.0013(2) Zn2 0.0182(4) 0.0261(4) 0.0189(3) -0.0001(2) 0.0025(3) 0.0009(2) S3 0.0424(8) 0.0230(6) 0.0197(6) 0.0005(5) 0.0096(6) -0.0016(6) S4 0.0540(9) 0.0232(7) 0.0207(6) -0.0004(5) 0.0133(6) -0.0055(6) O5 0.031(2) 0.031(2) 0.033(2) 0.0094(17) 0.0093(17) 0.0043(17) O6 0.028(2) 0.036(2) 0.027(2) 0.0058(16) 0.0067(16) -0.0027(16) N21 0.017(2) 0.039(3) 0.023(2) -0.0033(19) 0.0019(18) -0.0007(19) O8 0.030(2) 0.039(2) 0.030(2) 0.0079(17) 0.0113(17) -0.0069(17) O9 0.041(2) 0.032(2) 0.036(2) -0.0098(18) 0.0118(18) 0.0051(19) O10 0.042(2) 0.034(2) 0.027(2) -0.0097(16) 0.0084(18) -0.0062(18) N22 0.016(2) 0.031(2) 0.027(2) 0.0054(18) 0.0036(18) 0.0038(17) O13 0.035(2) 0.037(2) 0.030(2) 0.0116(18) 0.0055(17) 0.0012(18) C14 0.041(3) 0.023(2) 0.021(2) 0.000(2) 0.013(2) -0.006(2) O15 0.045(2) 0.041(2) 0.032(2) -0.0012(18) 0.0107(18) -0.015(2) O16 0.053(3) 0.030(2) 0.026(2) 0.0009(16) 0.0083(18) 0.0096(19) C96 0.039(3) 0.020(2) 0.016(2) 0.0026(19) 0.007(2) 0.000(2) C98 0.040(3) 0.021(2) 0.023(3) -0.002(2) 0.012(2) 0.000(2) C97 0.023(3) 0.027(3) 0.024(3) 0.002(2) 0.001(2) 0.002(2) O17 0.070(3) 0.029(2) 0.027(2) 0.0007(17) 0.015(2) 0.010(2) C22 0.047(3) 0.022(2) 0.019(2) 0.000(2) 0.010(2) 0.002(2) O18 0.050(3) 0.044(2) 0.033(2) -0.0052(19) 0.0124(19) -0.024(2) C24 0.033(3) 0.023(2) 0.024(3) 0.001(2) 0.009(2) -0.001(2) C25 0.029(3) 0.023(2) 0.021(2) -0.001(2) 0.004(2) -0.005(2) C26 0.037(3) 0.026(3) 0.020(2) 0.000(2) 0.007(2) -0.003(2) C27 0.022(3) 0.030(3) 0.027(3) -0.001(2) 0.006(2) -0.006(2) C28 0.032(3) 0.028(3) 0.019(2) 0.002(2) 0.006(2) -0.004(2) C29 0.027(3) 0.033(3) 0.031(3) 0.004(2) 0.010(2) 0.003(2) C30 0.038(3) 0.026(3) 0.021(2) 0.002(2) 0.011(2) 0.001(2) C32 0.034(3) 0.039(3) 0.031(3) -0.011(2) 0.007(2) -0.006(3) C33 0.039(3) 0.026(3) 0.019(2) 0.001(2) 0.006(2) -0.002(2) C34 0.015(3) 0.039(3) 0.028(3) 0.002(2) 0.001(2) 0.001(2) C35 0.036(3) 0.025(3) 0.019(2) 0.002(2) 0.007(2) 0.002(2) C36 0.034(3) 0.044(3) 0.028(3) -0.011(3) 0.004(2) 0.008(3) C37 0.032(3) 0.051(4) 0.037(3) 0.017(3) 0.001(3) -0.012(3) C38 0.032(3) 0.030(3) 0.030(3) -0.002(2) 0.011(2) -0.003(2) C39 0.033(3) 0.032(3) 0.023(3) 0.008(2) 0.003(2) 0.012(2) C40 0.033(3) 0.044(3) 0.030(3) -0.009(3) 0.006(2) 0.013(3) C41 0.037(3) 0.038(3) 0.030(3) -0.010(2) -0.003(2) 0.011(3) C42 0.045(4) 0.039(3) 0.033(3) -0.012(3) 0.007(3) 0.013(3) C43 0.027(3) 0.051(4) 0.029(3) 0.016(3) 0.002(3) -0.008(3) C44 0.037(3) 0.035(3) 0.029(3) 0.000(2) 0.015(2) 0.005(2) C45 0.040(3) 0.048(4) 0.046(4) 0.026(3) 0.012(3) 0.009(3) C46 0.035(3) 0.038(3) 0.040(3) -0.014(3) 0.016(3) -0.002(3) C47 0.027(3) 0.119(7) 0.048(4) 0.053(5) -0.011(3) -0.022(4) C48 0.032(3) 0.056(4) 0.045(4) 0.023(3) 0.013(3) -0.001(3) C49 0.023(3) 0.116(7) 0.044(4) 0.048(4) 0.000(3) -0.012(4) C50 0.020(3) 0.041(3) 0.023(3) 0.004(2) 0.001(2) 0.002(2) C51 0.034(3) 0.046(4) 0.034(3) 0.013(3) 0.007(3) -0.007(3) C52 0.030(4) 0.108(7) 0.029(3) -0.008(4) 0.003(3) 0.007(4) C53 0.026(3) 0.070(4) 0.036(4) 0.019(3) 0.007(3) -0.008(3) C55 0.029(4) 0.121(7) 0.032(4) -0.011(4) 0.008(3) 0.009(4) C59 0.024(4) 0.196(11) 0.056(5) -0.055(6) 0.012(3) -0.002(5) C60 0.032(4) 0.186(11) 0.033(4) -0.034(5) 0.000(3) 0.002(5) O19 0.046(2) 0.036(2) 0.031(2) -0.0095(18) 0.0100(19) -0.0075(19) O20 0.062(3) 0.035(2) 0.032(2) -0.0100(18) 0.012(2) 0.011(2) C99 0.056(4) 0.026(3) 0.022(3) 0.002(2) 0.016(3) 0.006(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 Zn1 O5 2.017(4) 1_554 ? Zn1 O10 2.026(4) 1_554 ? Zn1 O8 2.033(4) . ? Zn1 N22 2.034(4) . ? Zn1 O20 2.049(4) . ? Zn1 Zn2 2.9277(10) . ? Zn2 O19 2.027(4) . ? Zn2 N21 2.040(4) 8_455 ? Zn2 O13 2.046(4) . ? Zn2 O6 2.052(4) 1_554 ? Zn2 O9 2.054(4) 1_554 ? S3 O16 1.432(4) . ? S3 O15 1.443(4) . ? S3 C22 1.772(5) . ? S3 C96 1.781(5) . ? S4 O17 1.429(4) . ? S4 O18 1.436(4) . ? S4 C98 1.770(5) . ? S4 C14 1.783(5) . ? O5 C26 1.250(6) . ? O5 Zn1 2.017(4) 1_556 ? O6 C26 1.287(6) . ? O6 Zn2 2.053(4) 1_556 ? N21 C52 1.322(8) . ? N21 C59 1.329(8) . ? N21 Zn2 2.040(4) 8_556 ? O8 C33 1.254(6) . ? O9 C30 1.232(6) . ? O9 Zn2 2.054(4) 1_556 ? O10 C30 1.265(7) . ? O10 Zn1 2.026(4) 1_556 ? N22 C43 1.302(7) . ? N22 C49 1.325(7) . ? O13 C33 1.259(6) . ? C14 C45 1.383(8) . ? C14 C51 1.386(8) . ? C96 C39 1.339(7) . ? C96 C27 1.410(7) . ? C98 C42 1.372(8) . ? C98 C32 1.399(8) . ? C97 C27 1.370(7) . ? C97 C25 1.419(7) . ? C97 H1 0.9400 . ? C22 C40 1.338(8) . ? C22 C38 1.402(7) . ? C24 C46 1.361(8) . ? C24 C41 1.384(8) . ? C24 C30 1.511(7) . ? C25 C29 1.373(7) . ? C25 C26 1.486(7) . ? C27 H2 0.9400 . ? C28 C48 1.368(8) . ? C28 C37 1.393(8) . ? C28 C33 1.499(7) . ? C29 C39 1.378(7) . ? C29 H3 0.9400 . ? C32 C46 1.379(7) . ? C32 H4 0.9400 . ? C34 C47 1.359(8) . ? C34 C53 1.378(8) . ? C34 C50 1.485(8) . ? C35 C44 1.382(8) . ? C35 C36 1.390(7) . ? C35 C99 1.501(7) . ? C36 C40 1.375(7) . ? C36 H5 0.9400 . ? C37 C51 1.394(8) . ? C37 H6 0.9400 . ? C38 C44 1.374(7) . ? C38 H7 0.9400 . ? C39 H8 0.9400 . ? C40 H9 0.9400 . ? C41 C42 1.387(7) . ? C41 H10 0.9400 . ? C42 H11 0.9400 . ? C43 C53 1.373(9) . ? C43 H12 0.9400 . ? C44 H13 0.9400 . ? C45 C48 1.369(8) . ? C45 H14 0.9400 . ? C46 H15 0.9400 . ? C47 C49 1.399(8) . ? C47 H16 0.9400 . ? C48 H17 0.9400 . ? C49 H18 0.9400 . ? C50 C60 1.358(9) . ? C50 C55 1.375(9) . ? C51 H19 0.9400 . ? C52 C55 1.373(10) . ? C52 H20 0.9400 . ? C53 H21 0.9400 . ? C55 H22 0.9400 . ? C59 C60 1.369(10) . ? C59 H23 0.9400 . ? C60 H24 0.9400 . ? O19 C99 1.263(7) . ? O20 C99 1.261(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn1 O10 89.02(17) 1_554 1_554 ? O5 Zn1 O8 160.98(16) 1_554 . ? O10 Zn1 O8 90.19(16) 1_554 . ? O5 Zn1 N22 99.90(16) 1_554 . ? O10 Zn1 N22 107.69(17) 1_554 . ? O8 Zn1 N22 98.43(16) . . ? O5 Zn1 O20 86.77(17) 1_554 . ? O10 Zn1 O20 157.76(18) 1_554 . ? O8 Zn1 O20 86.80(18) . . ? N22 Zn1 O20 94.55(18) . . ? O5 Zn1 Zn2 83.49(11) 1_554 . ? O10 Zn1 Zn2 86.37(11) 1_554 . ? O8 Zn1 Zn2 77.50(11) . . ? N22 Zn1 Zn2 165.50(13) . . ? O20 Zn1 Zn2 71.46(13) . . ? O19 Zn2 N21 102.79(18) . 8_455 ? O19 Zn2 O13 88.76(17) . . ? N21 Zn2 O13 101.41(17) 8_455 . ? O19 Zn2 O6 90.55(17) . 1_554 ? N21 Zn2 O6 98.15(16) 8_455 1_554 ? O13 Zn2 O6 160.09(16) . 1_554 ? O19 Zn2 O9 162.57(17) . 1_554 ? N21 Zn2 O9 94.62(17) 8_455 1_554 ? O13 Zn2 O9 87.23(17) . 1_554 ? O6 Zn2 O9 87.51(17) 1_554 1_554 ? O19 Zn2 Zn1 89.05(12) . . ? N21 Zn2 Zn1 167.40(13) 8_455 . ? O13 Zn2 Zn1 82.89(11) . . ? O6 Zn2 Zn1 77.20(10) 1_554 . ? O9 Zn2 Zn1 73.63(11) 1_554 . ? O16 S3 O15 119.6(3) . . ? O16 S3 C22 107.5(2) . . ? O15 S3 C22 108.6(3) . . ? O16 S3 C96 107.4(2) . . ? O15 S3 C96 109.8(2) . . ? C22 S3 C96 102.5(2) . . ? O17 S4 O18 120.7(3) . . ? O17 S4 C98 107.1(3) . . ? O18 S4 C98 109.0(3) . . ? O17 S4 C14 108.4(3) . . ? O18 S4 C14 108.3(3) . . ? C98 S4 C14 101.7(3) . . ? C26 O5 Zn1 124.6(4) . 1_556 ? C26 O6 Zn2 130.2(3) . 1_556 ? C52 N21 C59 116.2(5) . . ? C52 N21 Zn2 123.4(4) . 8_556 ? C59 N21 Zn2 120.4(4) . 8_556 ? C33 O8 Zn1 130.9(4) . . ? C30 O9 Zn2 135.2(4) . 1_556 ? C30 O10 Zn1 119.0(3) . 1_556 ? C43 N22 C49 118.3(5) . . ? C43 N22 Zn1 122.8(4) . . ? C49 N22 Zn1 118.9(4) . . ? C33 O13 Zn2 123.0(4) . . ? C45 C14 C51 121.5(5) . . ? C45 C14 S4 119.0(4) . . ? C51 C14 S4 119.5(4) . . ? C39 C96 C27 121.2(5) . . ? C39 C96 S3 119.6(4) . . ? C27 C96 S3 119.1(4) . . ? C42 C98 C32 121.2(5) . . ? C42 C98 S4 118.8(4) . . ? C32 C98 S4 119.9(4) . . ? C27 C97 C25 120.5(5) . . ? C27 C97 H1 119.7 . . ? C25 C97 H1 119.7 . . ? C40 C22 C38 120.2(5) . . ? C40 C22 S3 120.5(4) . . ? C38 C22 S3 119.2(4) . . ? C46 C24 C41 119.5(5) . . ? C46 C24 C30 120.5(5) . . ? C41 C24 C30 120.0(5) . . ? C29 C25 C97 118.7(5) . . ? C29 C25 C26 121.8(5) . . ? C97 C25 C26 119.4(5) . . ? O5 C26 O6 124.4(5) . . ? O5 C26 C25 118.7(5) . . ? O6 C26 C25 116.8(5) . . ? C97 C27 C96 118.3(5) . . ? C97 C27 H2 120.9 . . ? C96 C27 H2 120.9 . . ? C48 C28 C37 118.9(5) . . ? C48 C28 C33 120.8(5) . . ? C37 C28 C33 120.3(5) . . ? C25 C29 C39 120.4(5) . . ? C25 C29 H3 119.8 . . ? C39 C29 H3 119.8 . . ? O9 C30 O10 125.7(5) . . ? O9 C30 C24 117.1(5) . . ? O10 C30 C24 117.2(5) . . ? C46 C32 C98 118.1(5) . . ? C46 C32 H4 121.0 . . ? C98 C32 H4 121.0 . . ? O8 C33 O13 125.6(5) . . ? O8 C33 C28 116.7(5) . . ? O13 C33 C28 117.7(5) . . ? C47 C34 C53 117.0(5) . . ? C47 C34 C50 121.8(5) . . ? C53 C34 C50 121.2(5) . . ? C44 C35 C36 119.3(5) . . ? C44 C35 C99 120.8(5) . . ? C36 C35 C99 119.9(5) . . ? C40 C36 C35 119.5(5) . . ? C40 C36 H5 120.2 . . ? C35 C36 H5 120.2 . . ? C28 C37 C51 120.5(5) . . ? C28 C37 H6 119.7 . . ? C51 C37 H6 119.7 . . ? C44 C38 C22 119.0(5) . . ? C44 C38 H7 120.5 . . ? C22 C38 H7 120.5 . . ? C96 C39 C29 120.8(5) . . ? C96 C39 H8 119.6 . . ? C29 C39 H8 119.6 . . ? C22 C40 C36 121.4(5) . . ? C22 C40 H9 119.3 . . ? C36 C40 H9 119.3 . . ? C24 C41 C42 120.5(5) . . ? C24 C41 H10 119.7 . . ? C42 C41 H10 119.7 . . ? C98 C42 C41 118.9(5) . . ? C98 C42 H11 120.5 . . ? C41 C42 H11 120.5 . . ? N22 C43 C53 123.1(5) . . ? N22 C43 H12 118.4 . . ? C53 C43 H12 118.4 . . ? C38 C44 C35 120.5(5) . . ? C38 C44 H13 119.7 . . ? C35 C44 H13 119.7 . . ? C48 C45 C14 118.5(6) . . ? C48 C45 H14 120.7 . . ? C14 C45 H14 120.7 . . ? C24 C46 C32 121.7(5) . . ? C24 C46 H15 119.1 . . ? C32 C46 H15 119.1 . . ? C34 C47 C49 119.8(6) . . ? C34 C47 H16 120.1 . . ? C49 C47 H16 120.1 . . ? C28 C48 C45 122.2(6) . . ? C28 C48 H17 118.9 . . ? C45 C48 H17 118.9 . . ? N22 C49 C47 121.8(6) . . ? N22 C49 H18 119.1 . . ? C47 C49 H18 119.1 . . ? C60 C50 C55 116.6(6) . . ? C60 C50 C34 122.3(5) . . ? C55 C50 C34 121.0(6) . . ? C14 C51 C37 118.3(5) . . ? C14 C51 H19 120.9 . . ? C37 C51 H19 120.9 . . ? N21 C52 C55 123.6(7) . . ? N21 C52 H20 118.2 . . ? C55 C52 H20 118.2 . . ? C43 C53 C34 119.8(6) . . ? C43 C53 H21 120.1 . . ? C34 C53 H21 120.1 . . ? C52 C55 C50 119.7(7) . . ? C52 C55 H22 120.2 . . ? C50 C55 H22 120.2 . . ? N21 C59 C60 123.3(7) . . ? N21 C59 H23 118.3 . . ? C60 C59 H23 118.3 . . ? C50 C60 C59 120.4(7) . . ? C50 C60 H24 119.8 . . ? C59 C60 H24 119.8 . . ? C99 O19 Zn2 116.0(4) . . ? C99 O20 Zn1 137.8(4) . . ? O20 C99 O19 125.6(5) . . ? O20 C99 C35 115.1(5) . . ? O19 C99 C35 119.3(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 O5 Zn1 Zn2 O19 -90.70(17) 1_554 . . . ? O10 Zn1 Zn2 O19 179.87(15) 1_554 . . . ? O8 Zn1 Zn2 O19 88.87(16) . . . . ? N22 Zn1 Zn2 O19 13.8(5) . . . . ? O20 Zn1 Zn2 O19 -1.93(18) . . . . ? O5 Zn1 Zn2 N21 69.6(6) 1_554 . . 8_455 ? O10 Zn1 Zn2 N21 -19.9(6) 1_554 . . 8_455 ? O8 Zn1 Zn2 N21 -110.9(6) . . . 8_455 ? N22 Zn1 Zn2 N21 174.1(7) . . . 8_455 ? O20 Zn1 Zn2 N21 158.3(6) . . . 8_455 ? O5 Zn1 Zn2 O13 -179.56(15) 1_554 . . . ? O10 Zn1 Zn2 O13 91.01(17) 1_554 . . . ? O8 Zn1 Zn2 O13 0.01(16) . . . . ? N22 Zn1 Zn2 O13 -75.1(5) . . . . ? O20 Zn1 Zn2 O13 -90.80(18) . . . . ? O5 Zn1 Zn2 O6 0.08(16) 1_554 . . 1_554 ? O10 Zn1 Zn2 O6 -89.35(16) 1_554 . . 1_554 ? O8 Zn1 Zn2 O6 179.65(15) . . . 1_554 ? N22 Zn1 Zn2 O6 104.6(5) . . . 1_554 ? O20 Zn1 Zn2 O6 88.85(18) . . . 1_554 ? O5 Zn1 Zn2 O9 91.25(17) 1_554 . . 1_554 ? O10 Zn1 Zn2 O9 1.82(17) 1_554 . . 1_554 ? O8 Zn1 Zn2 O9 -89.19(17) . . . 1_554 ? N22 Zn1 Zn2 O9 -164.3(5) . . . 1_554 ? O20 Zn1 Zn2 O9 -179.99(17) . . . 1_554 ? O5 Zn1 O8 C33 3.2(8) 1_554 . . . ? O10 Zn1 O8 C33 -84.4(5) 1_554 . . . ? N22 Zn1 O8 C33 167.7(5) . . . . ? O20 Zn1 O8 C33 73.6(5) . . . . ? Zn2 Zn1 O8 C33 1.9(5) . . . . ? O5 Zn1 N22 C43 -17.7(5) 1_554 . . . ? O10 Zn1 N22 C43 74.5(5) 1_554 . . . ? O8 Zn1 N22 C43 167.4(5) . . . . ? O20 Zn1 N22 C43 -105.2(5) . . . . ? Zn2 Zn1 N22 C43 -120.1(6) . . . . ? O5 Zn1 N22 C49 161.5(6) 1_554 . . . ? O10 Zn1 N22 C49 -106.4(6) 1_554 . . . ? O8 Zn1 N22 C49 -13.5(6) . . . . ? O20 Zn1 N22 C49 74.0(6) . . . . ? Zn2 Zn1 N22 C49 59.0(8) . . . . ? O19 Zn2 O13 C33 -90.9(4) . . . . ? N21 Zn2 O13 C33 166.3(4) 8_455 . . . ? O6 Zn2 O13 C33 -2.7(8) 1_554 . . . ? O9 Zn2 O13 C33 72.2(4) 1_554 . . . ? Zn1 Zn2 O13 C33 -1.7(4) . . . . ? O17 S4 C14 C45 -32.6(6) . . . . ? O18 S4 C14 C45 -165.1(5) . . . . ? C98 S4 C14 C45 80.1(5) . . . . ? O17 S4 C14 C51 149.0(5) . . . . ? O18 S4 C14 C51 16.5(5) . . . . ? C98 S4 C14 C51 -98.3(5) . . . . ? O16 S3 C96 C39 28.9(5) . . . . ? O15 S3 C96 C39 160.5(4) . . . . ? C22 S3 C96 C39 -84.2(5) . . . . ? O16 S3 C96 C27 -155.1(4) . . . . ? O15 S3 C96 C27 -23.6(5) . . . . ? C22 S3 C96 C27 91.8(4) . . . . ? O17 S4 C98 C42 25.8(5) . . . . ? O18 S4 C98 C42 157.9(5) . . . . ? C14 S4 C98 C42 -87.9(5) . . . . ? O17 S4 C98 C32 -157.5(5) . . . . ? O18 S4 C98 C32 -25.4(5) . . . . ? C14 S4 C98 C32 88.8(5) . . . . ? O16 S3 C22 C40 -37.2(5) . . . . ? O15 S3 C22 C40 -168.0(5) . . . . ? C96 S3 C22 C40 75.8(5) . . . . ? O16 S3 C22 C38 144.8(4) . . . . ? O15 S3 C22 C38 14.0(5) . . . . ? C96 S3 C22 C38 -102.2(5) . . . . ? C27 C97 C25 C29 -1.2(8) . . . . ? C27 C97 C25 C26 176.8(5) . . . . ? Zn1 O5 C26 O6 -2.5(8) 1_556 . . . ? Zn1 O5 C26 C25 177.8(3) 1_556 . . . ? Zn2 O6 C26 O5 2.8(8) 1_556 . . . ? Zn2 O6 C26 C25 -177.5(3) 1_556 . . . ? C29 C25 C26 O5 -179.8(5) . . . . ? C97 C25 C26 O5 2.2(7) . . . . ? C29 C25 C26 O6 0.5(8) . . . . ? C97 C25 C26 O6 -177.5(5) . . . . ? C25 C97 C27 C96 0.7(8) . . . . ? C39 C96 C27 C97 0.4(8) . . . . ? S3 C96 C27 C97 -175.5(4) . . . . ? C97 C25 C29 C39 0.7(8) . . . . ? C26 C25 C29 C39 -177.3(5) . . . . ? Zn2 O9 C30 O10 0.7(9) 1_556 . . . ? Zn2 O9 C30 C24 -177.0(3) 1_556 . . . ? Zn1 O10 C30 O9 2.2(7) 1_556 . . . ? Zn1 O10 C30 C24 179.9(3) 1_556 . . . ? C46 C24 C30 O9 -0.9(8) . . . . ? C41 C24 C30 O9 176.8(5) . . . . ? C46 C24 C30 O10 -178.8(5) . . . . ? C41 C24 C30 O10 -1.1(8) . . . . ? C42 C98 C32 C46 0.3(9) . . . . ? S4 C98 C32 C46 -176.2(5) . . . . ? Zn1 O8 C33 O13 -4.0(9) . . . . ? Zn1 O8 C33 C28 177.7(3) . . . . ? Zn2 O13 C33 O8 3.7(8) . . . . ? Zn2 O13 C33 C28 -178.0(3) . . . . ? C48 C28 C33 O8 7.7(8) . . . . ? C37 C28 C33 O8 -173.2(5) . . . . ? C48 C28 C33 O13 -170.8(6) . . . . ? C37 C28 C33 O13 8.3(8) . . . . ? C44 C35 C36 C40 -2.0(9) . . . . ? C99 C35 C36 C40 175.2(5) . . . . ? C48 C28 C37 C51 1.1(10) . . . . ? C33 C28 C37 C51 -178.0(6) . . . . ? C40 C22 C38 C44 -1.1(8) . . . . ? S3 C22 C38 C44 176.9(4) . . . . ? C27 C96 C39 C29 -0.9(8) . . . . ? S3 C96 C39 C29 174.9(4) . . . . ? C25 C29 C39 C96 0.4(9) . . . . ? C38 C22 C40 C36 1.2(9) . . . . ? S3 C22 C40 C36 -176.8(5) . . . . ? C35 C36 C40 C22 0.4(9) . . . . ? C46 C24 C41 C42 2.4(9) . . . . ? C30 C24 C41 C42 -175.3(5) . . . . ? C32 C98 C42 C41 -0.5(9) . . . . ? S4 C98 C42 C41 176.1(5) . . . . ? C24 C41 C42 C98 -0.8(10) . . . . ? C49 N22 C43 C53 0.7(10) . . . . ? Zn1 N22 C43 C53 179.8(5) . . . . ? C22 C38 C44 C35 -0.6(8) . . . . ? C36 C35 C44 C38 2.1(8) . . . . ? C99 C35 C44 C38 -175.0(5) . . . . ? C51 C14 C45 C48 1.7(10) . . . . ? S4 C14 C45 C48 -176.7(5) . . . . ? C41 C24 C46 C32 -2.6(9) . . . . ? C30 C24 C46 C32 175.1(5) . . . . ? C98 C32 C46 C24 1.3(9) . . . . ? C53 C34 C47 C49 -1.5(13) . . . . ? C50 C34 C47 C49 -178.9(7) . . . . ? C37 C28 C48 C45 -0.9(11) . . . . ? C33 C28 C48 C45 178.1(6) . . . . ? C14 C45 C48 C28 -0.4(11) . . . . ? C43 N22 C49 C47 2.1(12) . . . . ? Zn1 N22 C49 C47 -177.0(7) . . . . ? C34 C47 C49 N22 -1.7(15) . . . . ? C47 C34 C50 C60 138.5(10) . . . . ? C53 C34 C50 C60 -38.8(10) . . . . ? C47 C34 C50 C55 -37.5(10) . . . . ? C53 C34 C50 C55 145.1(8) . . . . ? C45 C14 C51 C37 -1.5(9) . . . . ? S4 C14 C51 C37 176.9(5) . . . . ? C28 C37 C51 C14 0.0(10) . . . . ? C59 N21 C52 C55 -3.4(12) . . . . ? Zn2 N21 C52 C55 174.2(6) 8_556 . . . ? N22 C43 C53 C34 -4.0(10) . . . . ? C47 C34 C53 C43 4.2(11) . . . . ? C50 C34 C53 C43 -178.3(6) . . . . ? N21 C52 C55 C50 -1.3(13) . . . . ? C60 C50 C55 C52 4.8(12) . . . . ? C34 C50 C55 C52 -179.0(6) . . . . ? C52 N21 C59 C60 4.6(16) . . . . ? Zn2 N21 C59 C60 -173.1(9) 8_556 . . . ? C55 C50 C60 C59 -3.7(15) . . . . ? C34 C50 C60 C59 -179.8(9) . . . . ? N21 C59 C60 C50 -1.1(19) . . . . ? N21 Zn2 O19 C99 -173.5(4) 8_455 . . . ? O13 Zn2 O19 C99 85.1(4) . . . . ? O6 Zn2 O19 C99 -75.0(4) 1_554 . . . ? O9 Zn2 O19 C99 8.4(8) 1_554 . . . ? Zn1 Zn2 O19 C99 2.2(4) . . . . ? O5 Zn1 O20 C99 87.1(6) 1_554 . . . ? O10 Zn1 O20 C99 7.7(9) 1_554 . . . ? O8 Zn1 O20 C99 -75.0(6) . . . . ? N22 Zn1 O20 C99 -173.2(6) . . . . ? Zn2 Zn1 O20 C99 2.9(5) . . . . ? Zn1 O20 C99 O19 -2.1(10) . . . . ? Zn1 O20 C99 C35 176.7(4) . . . . ? Zn2 O19 C99 O20 -1.2(7) . . . . ? Zn2 O19 C99 C35 -179.9(4) . . . . ? C44 C35 C99 O20 10.5(8) . . . . ? C36 C35 C99 O20 -166.6(5) . . . . ? C44 C35 C99 O19 -170.6(5) . . . . ? C36 C35 C99 O19 12.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 3.274 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.171 #===END