data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H14 Cd F6 N O4 S' _chemical_formula_sum 'C26 H14 Cd F6 N O4 S' _chemical_formula_weight 662.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 2/c' _symmetry_space_group_name_Hall '-P 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 15.9717(15) _cell_length_b 7.6328(7) _cell_length_c 23.774(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.924(2) _cell_angle_gamma 90.00 _cell_volume 2877.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6536 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.39 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1308 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7739 _exptl_absorpt_correction_T_max 0.9153 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15595 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5050 _reflns_number_gt 4456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+0.3694P] 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 5050 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0970 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4002(2) -0.2956(5) 0.42380(14) 0.0487(8) Uani 1 1 d U . . C2 C 0.3457(2) -0.1995(4) 0.37832(13) 0.0418(7) Uani 1 1 d U . . C3 C 0.2740(2) -0.2757(5) 0.35122(15) 0.0543(8) Uani 1 1 d U . . H3 H 0.2579 -0.3856 0.3629 0.065 Uiso 1 1 calc R . . C4 C 0.2254(2) -0.1933(5) 0.30709(16) 0.0544(8) Uani 1 1 d U . . H4 H 0.1772 -0.2480 0.2895 0.065 Uiso 1 1 calc R . . C5 C 0.24796(19) -0.0303(4) 0.28883(13) 0.0443(7) Uani 1 1 d U . . C6 C 0.3187(2) 0.0497(4) 0.31722(13) 0.0439(7) Uani 1 1 d U . . H6 H 0.3338 0.1613 0.3064 0.053 Uiso 1 1 calc R . . C7 C 0.3673(2) -0.0333(5) 0.36133(14) 0.0540(5) Uani 1 1 d U . . H7 H 0.4146 0.0224 0.3797 0.065 Uiso 1 1 calc R . . C8 C 0.1978(2) 0.0710(5) 0.23953(14) 0.0540(5) Uani 1 1 d U . . C9 C 0.1407(2) -0.0524(5) 0.19920(14) 0.0540(5) Uani 1 1 d U . . C10 C 0.1416(2) 0.2032(6) 0.26620(17) 0.0615(9) Uani 1 1 d U . . C11 C 0.2580(2) 0.1583(4) 0.20168(14) 0.0455(7) Uani 1 1 d U . . C12 C 0.2448(2) 0.3252(5) 0.17823(15) 0.0522(8) Uani 1 1 d U . . H12 H 0.1992 0.3920 0.1867 0.063 Uiso 1 1 calc R . . C13 C 0.2987(2) 0.3910(5) 0.14275(14) 0.0515(8) Uani 1 1 d U . . H13 H 0.2896 0.5029 0.1278 0.062 Uiso 1 1 calc R . . C14 C 0.3662(2) 0.2948(5) 0.12887(13) 0.0442(7) Uani 1 1 d U . . C15 C 0.3802(2) 0.1293(5) 0.15249(14) 0.0487(8) Uani 1 1 d U . . H15 H 0.4258 0.0627 0.1440 0.058 Uiso 1 1 calc R . . C16 C 0.3263(2) 0.0644(5) 0.18840(13) 0.0491(7) Uani 1 1 d U . . H16 H 0.3365 -0.0462 0.2042 0.059 Uiso 1 1 calc R . . C17 C 0.4214(2) 0.3631(4) 0.08651(14) 0.0453(8) Uani 1 1 d U . . C18 C 0.6694(2) -0.0132(4) 0.48976(15) 0.0504(8) Uani 1 1 d U . . H18 H 0.6186 0.0199 0.4693 0.060 Uiso 1 1 calc R . . C19 C 0.7366(2) 0.0988(5) 0.49197(17) 0.0611(9) Uani 1 1 d U . . H19 H 0.7304 0.2064 0.4736 0.073 Uiso 1 1 calc R . . C20 C 0.8128(2) 0.0542(5) 0.52090(16) 0.0583(9) Uani 1 1 d U . . C21 C 0.8175(2) -0.1059(6) 0.5489(2) 0.0714(11) Uani 1 1 d U . . H21 H 0.8676 -0.1422 0.5697 0.086 Uiso 1 1 calc R . . C22 C 0.7466(2) -0.2099(5) 0.54538(18) 0.0625(10) Uani 1 1 d U . . H22 H 0.7500 -0.3156 0.5650 0.075 Uiso 1 1 calc R . . C23 C 0.8857(3) 0.1728(5) 0.5242(2) 0.0736(11) Uani 1 1 d U . . C24 C 0.9616(3) 0.1571(7) 0.5544(3) 0.1066(16) Uani 1 1 d U . . H24 H 0.9771 0.0635 0.5785 0.128 Uiso 1 1 calc R . . C25 C 1.0163(3) 0.2998(8) 0.5457(3) 0.1159(18) Uani 1 1 d U . . H25 H 1.0713 0.3079 0.5635 0.139 Uiso 1 1 calc R . . C26 C 0.9817(3) 0.4197(7) 0.5098(2) 0.0934(15) Uani 1 1 d U . . Cd1 Cd 0.560844(12) -0.34200(2) 0.509462(8) 0.03139(11) Uani 1 1 d . . . F1 F 0.18294(18) -0.1880(3) 0.18284(11) 0.0801(7) Uani 1 1 d U . . F2 F 0.10867(18) 0.0328(4) 0.15264(10) 0.1030(10) Uani 1 1 d . . . F3 F 0.07484(15) -0.1159(4) 0.22289(12) 0.0923(9) Uani 1 1 d . . . F4 F 0.08455(15) 0.2802(4) 0.22886(11) 0.0918(9) Uani 1 1 d . . . F5 F 0.09918(16) 0.1271(4) 0.30460(12) 0.0863(8) Uani 1 1 d . . . F6 F 0.18740(17) 0.3307(3) 0.29294(11) 0.0758(7) Uani 1 1 d . . . N1 N 0.67409(16) -0.1684(3) 0.51589(11) 0.0375(6) Uani 1 1 d . . . O1 O 0.37827(17) -0.4467(3) 0.43580(11) 0.0663(7) Uani 1 1 d . . . O2 O 0.46546(16) -0.2172(4) 0.44660(10) 0.0589(6) Uani 1 1 d . . . O3 O 0.48263(16) 0.2706(3) 0.07695(10) 0.0550(6) Uani 1 1 d . . . O4 O 0.40034(18) 0.5064(3) 0.06406(11) 0.0667(7) Uani 1 1 d . . . S1 S 0.88197(7) 0.35915(15) 0.48379(6) 0.0856(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0462(18) 0.0577(19) 0.0431(16) 0.0055(15) 0.0089(15) 0.0087(16) C2 0.0418(16) 0.0454(16) 0.0387(15) 0.0047(13) 0.0073(13) 0.0010(14) C3 0.0532(19) 0.0508(18) 0.0577(19) 0.0146(16) 0.0021(16) -0.0140(16) C4 0.0457(17) 0.0616(18) 0.0538(18) 0.0122(15) -0.0029(15) -0.0176(15) C5 0.0372(15) 0.0557(17) 0.0399(14) 0.0121(13) 0.0043(12) -0.0046(13) C6 0.0406(15) 0.0482(16) 0.0423(14) 0.0103(13) 0.0027(13) -0.0080(13) C7 0.0420(10) 0.0741(12) 0.0440(9) 0.0151(9) -0.0021(8) -0.0141(9) C8 0.0420(10) 0.0741(12) 0.0440(9) 0.0151(9) -0.0021(8) -0.0141(9) C9 0.0420(10) 0.0741(12) 0.0440(9) 0.0151(9) -0.0021(8) -0.0141(9) C10 0.0450(18) 0.083(2) 0.0574(19) 0.0193(18) 0.0115(16) 0.0049(18) C11 0.0371(16) 0.0623(18) 0.0367(14) 0.0122(13) 0.0031(13) 0.0012(13) C12 0.0439(17) 0.0648(19) 0.0488(16) 0.0155(14) 0.0099(14) 0.0127(14) C13 0.0500(18) 0.0563(18) 0.0489(17) 0.0176(15) 0.0096(15) 0.0079(16) C14 0.0437(17) 0.0550(17) 0.0344(14) 0.0097(13) 0.0067(13) -0.0002(15) C15 0.0460(18) 0.0578(18) 0.0434(16) 0.0096(14) 0.0095(14) 0.0086(15) C16 0.0485(17) 0.0565(18) 0.0429(15) 0.0145(14) 0.0076(14) 0.0030(15) C17 0.0449(18) 0.0540(19) 0.0373(15) 0.0065(14) 0.0062(14) -0.0062(15) C18 0.0342(16) 0.0486(18) 0.0653(19) 0.0174(15) -0.0065(15) -0.0130(14) C19 0.0461(18) 0.0524(18) 0.080(2) 0.0281(18) -0.0110(17) -0.0220(16) C20 0.0404(17) 0.059(2) 0.072(2) 0.0218(17) -0.0063(16) -0.0260(15) C21 0.0414(18) 0.067(2) 0.099(3) 0.039(2) -0.0162(19) -0.0220(17) C22 0.0414(18) 0.0533(19) 0.089(2) 0.0314(18) -0.0081(18) -0.0139(16) C23 0.0478(19) 0.072(2) 0.094(2) 0.0405(18) -0.0187(18) -0.0357(17) C24 0.069(3) 0.102(3) 0.136(3) 0.064(2) -0.036(2) -0.047(2) C25 0.065(3) 0.117(3) 0.152(4) 0.066(3) -0.043(3) -0.055(3) C26 0.054(2) 0.098(3) 0.120(3) 0.048(3) -0.026(2) -0.052(2) Cd1 0.02912(15) 0.03095(15) 0.03446(15) -0.00048(8) 0.00532(10) -0.00991(8) F1 0.0824(18) 0.0866(16) 0.0694(15) -0.0159(12) 0.0017(13) -0.0178(12) F2 0.0808(17) 0.150(3) 0.0681(15) 0.0326(16) -0.0346(14) -0.0301(18) F3 0.0485(14) 0.134(2) 0.0901(18) 0.0265(17) -0.0089(13) -0.0354(15) F4 0.0454(13) 0.137(2) 0.0944(18) 0.0439(18) 0.0156(13) 0.0318(15) F5 0.0593(15) 0.125(2) 0.0821(17) 0.0347(15) 0.0375(13) 0.0130(14) F6 0.0720(16) 0.0809(18) 0.0779(16) 0.0010(12) 0.0230(13) 0.0178(13) N1 0.0342(14) 0.0330(13) 0.0453(14) 0.0030(10) 0.0054(12) -0.0116(10) O1 0.0640(17) 0.0587(16) 0.0753(17) 0.0329(14) 0.0046(14) 0.0045(13) O2 0.0568(16) 0.0665(15) 0.0501(13) 0.0083(12) -0.0073(12) 0.0087(13) O3 0.0570(15) 0.0638(15) 0.0481(13) 0.0086(12) 0.0215(12) 0.0029(13) O4 0.0743(18) 0.0700(17) 0.0597(15) 0.0286(13) 0.0236(13) 0.0050(14) S1 0.0547(6) 0.0800(8) 0.1130(10) 0.0481(7) -0.0272(6) -0.0444(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.248(4) . ? C1 O2 1.265(4) . ? C1 C2 1.496(5) . ? C2 C3 1.373(5) . ? C2 C7 1.387(5) . ? C3 C4 1.379(5) . ? C3 H3 0.9300 . ? C4 C5 1.380(5) . ? C4 H4 0.9300 . ? C5 C6 1.387(4) . ? C5 C8 1.545(5) . ? C6 C7 1.381(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C10 1.537(6) . ? C8 C11 1.545(5) . ? C8 C9 1.558(5) . ? C9 F1 1.319(5) . ? C9 F2 1.331(4) . ? C9 F3 1.342(4) . ? C10 F4 1.330(4) . ? C10 F6 1.332(5) . ? C10 F5 1.333(4) . ? C11 C16 1.374(5) . ? C11 C12 1.397(4) . ? C12 C13 1.372(5) . ? C12 H12 0.9300 . ? C13 C14 1.377(5) . ? C13 H13 0.9300 . ? C14 C15 1.389(5) . ? C14 C17 1.509(4) . ? C15 C16 1.375(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O4 1.245(4) . ? C17 O3 1.249(4) . ? C18 N1 1.335(4) . ? C18 C19 1.369(4) . ? C18 H18 0.9300 . ? C19 C20 1.367(5) . ? C19 H19 0.9300 . ? C20 C21 1.390(5) . ? C20 C23 1.469(5) . ? C21 C22 1.378(5) . ? C21 H21 0.9300 . ? C22 N1 1.318(4) . ? C22 H22 0.9300 . ? C23 C24 1.338(6) . ? C23 S1 1.714(4) . ? C24 C25 1.427(6) . ? C24 H24 0.9300 . ? C25 C26 1.326(7) . ? C25 H25 0.9300 . ? C26 C26 1.457(8) 3_766 ? C26 S1 1.702(4) . ? Cd1 O2 2.216(2) . ? Cd1 O3 2.217(2) 4_556 ? Cd1 O1 2.222(2) 3_646 ? Cd1 N1 2.233(2) . ? Cd1 O4 2.245(2) 2_645 ? Cd1 Cd1 3.0962(4) 3_646 ? O1 Cd1 2.222(2) 3_646 ? O3 Cd1 2.217(2) 4 ? O4 Cd1 2.245(2) 2_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 125.3(3) . . ? O1 C1 C2 117.6(3) . . ? O2 C1 C2 117.1(3) . . ? C3 C2 C7 118.2(3) . . ? C3 C2 C1 120.7(3) . . ? C7 C2 C1 121.0(3) . . ? C2 C3 C4 121.7(3) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C3 C4 C5 120.4(3) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C6 118.2(3) . . ? C4 C5 C8 124.0(3) . . ? C6 C5 C8 117.8(3) . . ? C7 C6 C5 121.2(3) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C2 120.3(3) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? C10 C8 C11 113.1(3) . . ? C10 C8 C5 106.9(3) . . ? C11 C8 C5 110.8(3) . . ? C10 C8 C9 108.8(3) . . ? C11 C8 C9 105.2(3) . . ? C5 C8 C9 112.1(3) . . ? F1 C9 F2 107.3(3) . . ? F1 C9 F3 107.1(3) . . ? F2 C9 F3 106.5(3) . . ? F1 C9 C8 111.9(3) . . ? F2 C9 C8 110.7(3) . . ? F3 C9 C8 113.0(3) . . ? F4 C10 F6 106.7(4) . . ? F4 C10 F5 106.6(3) . . ? F6 C10 F5 106.7(4) . . ? F4 C10 C8 113.7(3) . . ? F6 C10 C8 111.2(3) . . ? F5 C10 C8 111.5(3) . . ? C16 C11 C12 118.1(3) . . ? C16 C11 C8 118.5(3) . . ? C12 C11 C8 123.4(3) . . ? C13 C12 C11 120.2(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 121.4(3) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C13 C14 C15 118.7(3) . . ? C13 C14 C17 120.8(3) . . ? C15 C14 C17 120.4(3) . . ? C16 C15 C14 119.8(3) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C11 C16 C15 121.9(3) . . ? C11 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? O4 C17 O3 126.5(3) . . ? O4 C17 C14 116.1(3) . . ? O3 C17 C14 117.3(3) . . ? N1 C18 C19 122.4(3) . . ? N1 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? C20 C19 C18 120.7(3) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 117.0(3) . . ? C19 C20 C23 121.7(3) . . ? C21 C20 C23 121.3(3) . . ? C22 C21 C20 118.7(3) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? N1 C22 C21 123.9(3) . . ? N1 C22 H22 118.1 . . ? C21 C22 H22 118.1 . . ? C24 C23 C20 129.4(4) . . ? C24 C23 S1 110.0(3) . . ? C20 C23 S1 120.5(3) . . ? C23 C24 C25 112.6(4) . . ? C23 C24 H24 123.7 . . ? C25 C24 H24 123.7 . . ? C26 C25 C24 113.9(4) . . ? C26 C25 H25 123.0 . . ? C24 C25 H25 123.0 . . ? C25 C26 C26 129.3(5) . 3_766 ? C25 C26 S1 110.2(3) . . ? C26 C26 S1 120.4(4) 3_766 . ? O2 Cd1 O3 88.91(9) . 4_556 ? O2 Cd1 O1 157.47(10) . 3_646 ? O3 Cd1 O1 89.98(10) 4_556 3_646 ? O2 Cd1 N1 106.04(10) . . ? O3 Cd1 N1 109.09(9) 4_556 . ? O1 Cd1 N1 95.57(10) 3_646 . ? O2 Cd1 O4 85.89(10) . 2_645 ? O3 Cd1 O4 157.33(10) 4_556 2_645 ? O1 Cd1 O4 86.52(10) 3_646 2_645 ? N1 Cd1 O4 93.54(10) . 2_645 ? O2 Cd1 Cd1 82.44(7) . 3_646 ? O3 Cd1 Cd1 84.14(7) 4_556 3_646 ? O1 Cd1 Cd1 75.06(7) 3_646 3_646 ? N1 Cd1 Cd1 164.06(7) . 3_646 ? O4 Cd1 Cd1 73.31(7) 2_645 3_646 ? C22 N1 C18 117.2(3) . . ? C22 N1 Cd1 123.1(2) . . ? C18 N1 Cd1 119.7(2) . . ? C1 O1 Cd1 133.6(2) . 3_646 ? C1 O2 Cd1 123.3(2) . . ? C17 O3 Cd1 121.0(2) . 4 ? C17 O4 Cd1 134.5(2) . 2_665 ? C26 S1 C23 93.1(2) . . ? 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 0.500 -0.397 0.250 153 36 ' ' 2 0.500 0.397 0.750 153 36 ' ' 3 0.220 0.222 0.575 9 0 ' ' 4 0.780 0.222 0.925 9 0 ' ' 5 0.000 0.493 0.250 101 1 ' ' 6 0.000 0.506 0.750 101 1 ' ' 7 0.220 0.778 0.075 9 0 ' ' 8 0.780 0.778 0.425 9 0 ' ' _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.802 _refine_diff_density_min -0.850 _refine_diff_density_rms 0.061 # === END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H14 F6 N O4 S Zn' _chemical_formula_sum 'C26 H14 F6 N O4 S Zn' _chemical_formula_weight 615.81 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 2/c' _symmetry_space_group_name_Hall '-P 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 15.4994(14) _cell_length_b 7.5708(7) _cell_length_c 23.427(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.993(2) _cell_angle_gamma 90.00 _cell_volume 2728.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3249 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 26.57 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 1.049 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7437 _exptl_absorpt_correction_T_max 0.8176 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12967 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4762 _reflns_number_gt 3781 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.0100P] 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 4762 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.57015(17) 0.3714(4) 0.41472(12) 0.0177(6) Uani 1 1 d U . . C2 C 0.62427(17) 0.3035(4) 0.37010(11) 0.0171(6) Uani 1 1 d U . . C3 C 0.69341(17) 0.4029(4) 0.35530(12) 0.0205(6) Uani 1 1 d U . . H3 H 0.7025 0.5163 0.3701 0.025 Uiso 1 1 calc R . . C4 C 0.74922(18) 0.3345(4) 0.31858(12) 0.0206(6) Uani 1 1 d U . . H4 H 0.7953 0.4024 0.3088 0.025 Uiso 1 1 calc R . . C5 C 0.73622(17) 0.1649(4) 0.29646(11) 0.0188(6) Uani 1 1 d U . . C6 C 0.66457(17) 0.0681(4) 0.30993(12) 0.0201(6) Uani 1 1 d U . . H6 H 0.6539 -0.0435 0.2940 0.024 Uiso 1 1 calc R . . C7 C 0.60957(18) 0.1360(4) 0.34648(12) 0.0208(6) Uani 1 1 d U . . H7 H 0.5625 0.0696 0.3554 0.025 Uiso 1 1 calc R . . C8 C 0.79966(17) 0.0727(4) 0.25981(12) 0.0202(6) Uani 1 1 d U . . C9 C 0.85795(19) -0.0471(4) 0.30198(13) 0.0266(7) Uani 1 1 d U . . C10 C 0.85893(18) 0.2040(4) 0.23263(13) 0.0242(7) Uani 1 1 d U . . C11 C 0.74911(17) -0.0306(4) 0.20975(12) 0.0197(6) Uani 1 1 d U . . C12 C 0.77180(18) -0.1999(4) 0.19362(12) 0.0232(6) Uani 1 1 d U . . H12 H 0.8204 -0.2551 0.2130 0.028 Uiso 1 1 calc R . . C13 C 0.72216(18) -0.2868(4) 0.14874(13) 0.0235(6) Uani 1 1 d U . . H13 H 0.7376 -0.4002 0.1386 0.028 Uiso 1 1 calc R . . C14 C 0.64955(17) -0.2059(4) 0.11887(12) 0.0159(6) Uani 1 1 d U . . C15 C 0.62837(17) -0.0354(3) 0.13400(12) 0.0172(6) Uani 1 1 d U . . H15 H 0.5809 0.0212 0.1138 0.021 Uiso 1 1 calc R . . C16 C 0.67715(17) 0.0510(4) 0.17886(11) 0.0176(6) Uani 1 1 d U . . H16 H 0.6619 0.1650 0.1886 0.021 Uiso 1 1 calc R . . C17 C 0.59474(17) -0.3033(4) 0.07211(12) 0.0178(6) Uani 1 1 d U . . C18 C 0.25792(18) 0.2261(4) 0.45664(13) 0.0258(7) Uani 1 1 d U . . H18 H 0.2528 0.3353 0.4383 0.031 Uiso 1 1 calc R . . C19 C 0.18585(19) 0.1180(4) 0.45258(14) 0.0309(7) Uani 1 1 d U . . H19 H 0.1338 0.1537 0.4318 0.037 Uiso 1 1 calc R . . C20 C 0.19198(18) -0.0462(4) 0.48016(13) 0.0226(6) Uani 1 1 d U . . C21 C 0.27223(18) -0.0913(4) 0.50961(13) 0.0228(6) Uani 1 1 d U . . H21 H 0.2795 -0.1999 0.5282 0.027 Uiso 1 1 calc R . . C22 C 0.34102(17) 0.0247(4) 0.51133(12) 0.0181(6) Uani 1 1 d U . . H22 H 0.3941 -0.0083 0.5314 0.022 Uiso 1 1 calc R . . C23 C 0.11740(19) -0.1662(4) 0.47703(14) 0.0285(7) Uani 1 1 d U . . C24 C 0.0368(2) -0.1487(5) 0.44784(18) 0.0557(10) Uani 1 1 d U . . H24 H 0.0200 -0.0522 0.4246 0.067 Uiso 1 1 calc R . . C25 C -0.0189(2) -0.2900(5) 0.45608(19) 0.0585(11) Uani 1 1 d U . . H25 H -0.0762 -0.2954 0.4390 0.070 Uiso 1 1 calc R . . C26 C 0.0187(2) -0.4178(4) 0.49119(15) 0.0361(8) Uani 1 1 d U . . F1 F 0.81325(11) -0.1848(2) 0.31924(7) 0.0311(4) Uani 1 1 d . . . F2 F 0.88960(11) 0.0408(2) 0.34965(7) 0.0359(5) Uani 1 1 d . . . F3 F 0.92659(10) -0.1128(2) 0.27945(7) 0.0328(4) Uani 1 1 d . . . F4 F 0.91681(10) 0.2847(2) 0.27093(7) 0.0319(4) Uani 1 1 d . . . F5 F 0.90384(10) 0.1255(2) 0.19441(7) 0.0309(4) Uani 1 1 d . . . F6 F 0.81181(10) 0.3330(2) 0.20368(7) 0.0281(4) Uani 1 1 d . . . N1 N 0.33500(13) 0.1825(3) 0.48555(9) 0.0149(5) Uani 1 1 d . . . O1 O 0.59522(12) 0.5138(3) 0.43905(8) 0.0254(5) Uani 1 1 d . . . O2 O 0.50746(12) 0.2783(3) 0.42632(8) 0.0209(4) Uani 1 1 d . . . O3 O 0.52849(12) -0.2250(2) 0.04788(8) 0.0215(4) Uani 1 1 d . . . O4 O 0.61897(12) -0.4562(2) 0.06034(9) 0.0240(5) Uani 1 1 d . . . S1 S 0.12352(5) -0.36064(11) 0.51572(4) 0.0341(2) Uani 1 1 d . . . Zn1 Zn 0.437994(19) 0.34906(4) 0.491309(13) 0.01283(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0190(14) 0.0187(15) 0.0156(14) 0.0006(11) 0.0025(12) 0.0020(12) C2 0.0177(13) 0.0190(14) 0.0140(13) -0.0010(11) -0.0003(11) 0.0007(11) C3 0.0235(14) 0.0186(14) 0.0197(14) -0.0038(11) 0.0040(12) -0.0033(12) C4 0.0181(13) 0.0235(14) 0.0205(14) -0.0042(11) 0.0037(11) -0.0042(12) C5 0.0165(13) 0.0243(14) 0.0153(13) -0.0025(11) 0.0009(11) 0.0029(12) C6 0.0208(13) 0.0200(14) 0.0192(14) -0.0060(11) 0.0008(12) -0.0023(12) C7 0.0172(14) 0.0226(15) 0.0230(15) -0.0043(12) 0.0043(12) -0.0052(12) C8 0.0161(13) 0.0250(14) 0.0197(14) -0.0059(12) 0.0026(12) 0.0016(12) C9 0.0214(15) 0.0321(17) 0.0260(16) -0.0053(13) 0.0015(13) 0.0049(13) C10 0.0166(14) 0.0329(16) 0.0236(15) -0.0065(13) 0.0038(12) 0.0006(13) C11 0.0175(13) 0.0225(14) 0.0199(14) -0.0051(11) 0.0058(11) 0.0008(11) C12 0.0198(14) 0.0247(15) 0.0242(15) -0.0023(12) -0.0005(12) 0.0078(12) C13 0.0246(15) 0.0176(14) 0.0284(16) -0.0059(12) 0.0029(13) 0.0073(12) C14 0.0150(13) 0.0168(14) 0.0167(13) -0.0007(11) 0.0044(11) 0.0014(11) C15 0.0136(13) 0.0169(14) 0.0218(15) 0.0007(11) 0.0046(11) 0.0025(11) C16 0.0185(13) 0.0157(13) 0.0194(14) -0.0019(11) 0.0051(11) 0.0054(11) C17 0.0181(14) 0.0170(14) 0.0195(14) 0.0000(11) 0.0070(12) 0.0004(12) C18 0.0188(15) 0.0190(15) 0.0383(17) 0.0109(13) -0.0026(13) -0.0034(12) C19 0.0197(15) 0.0252(16) 0.0456(18) 0.0162(14) -0.0049(14) -0.0058(13) C20 0.0163(14) 0.0237(15) 0.0266(15) 0.0059(12) -0.0017(12) -0.0096(12) C21 0.0212(14) 0.0160(14) 0.0304(16) 0.0077(12) -0.0003(13) -0.0047(12) C22 0.0158(13) 0.0165(14) 0.0215(15) 0.0006(11) -0.0001(12) -0.0015(12) C23 0.0189(14) 0.0249(15) 0.0396(17) 0.0140(13) -0.0051(13) -0.0114(13) C24 0.0370(19) 0.045(2) 0.077(2) 0.0370(18) -0.0243(18) -0.0221(17) C25 0.0301(18) 0.054(2) 0.084(3) 0.037(2) -0.0257(19) -0.0256(17) C26 0.0247(17) 0.0320(18) 0.048(2) 0.0170(15) -0.0104(16) -0.0174(14) F1 0.0320(10) 0.0331(11) 0.0277(10) 0.0050(8) 0.0011(8) 0.0080(8) F2 0.0336(10) 0.0449(12) 0.0257(10) -0.0111(8) -0.0107(8) 0.0088(9) F3 0.0203(9) 0.0426(12) 0.0341(11) -0.0059(8) -0.0020(8) 0.0121(8) F4 0.0169(8) 0.0442(12) 0.0353(11) -0.0138(8) 0.0054(8) -0.0098(8) F5 0.0222(9) 0.0418(11) 0.0310(10) -0.0103(8) 0.0122(8) -0.0006(8) F6 0.0272(9) 0.0279(10) 0.0305(10) 0.0008(8) 0.0083(8) -0.0043(8) N1 0.0133(12) 0.0142(12) 0.0174(12) -0.0009(9) 0.0031(10) -0.0023(9) O1 0.0273(11) 0.0213(11) 0.0302(12) -0.0121(9) 0.0135(10) -0.0080(9) O2 0.0207(10) 0.0218(11) 0.0218(11) -0.0042(8) 0.0091(9) -0.0075(9) O3 0.0223(11) 0.0164(10) 0.0237(11) -0.0021(8) -0.0057(9) 0.0020(9) O4 0.0188(10) 0.0188(11) 0.0339(12) -0.0112(9) 0.0009(9) 0.0040(9) S1 0.0216(4) 0.0278(5) 0.0493(5) 0.0195(4) -0.0100(4) -0.0151(4) Zn1 0.01233(17) 0.01040(16) 0.01607(18) -0.00064(13) 0.00301(12) -0.00361(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.257(3) . ? C1 O1 1.259(3) . ? C1 C2 1.508(4) . ? C2 C3 1.388(4) . ? C2 C7 1.391(4) . ? C3 C4 1.392(4) . ? C3 H3 0.9300 . ? C4 C5 1.390(4) . ? C4 H4 0.9300 . ? C5 C6 1.398(4) . ? C5 C8 1.548(4) . ? C6 C7 1.379(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C11 1.542(4) . ? C8 C10 1.543(4) . ? C8 C9 1.548(4) . ? C9 F3 1.340(3) . ? C9 F2 1.341(3) . ? C9 F1 1.341(3) . ? C10 F4 1.337(3) . ? C10 F5 1.338(3) . ? C10 F6 1.352(3) . ? C11 C12 1.393(4) . ? C11 C16 1.398(4) . ? C12 C13 1.390(4) . ? C12 H12 0.9300 . ? C13 C14 1.393(4) . ? C13 H13 0.9300 . ? C14 C15 1.388(4) . ? C14 C17 1.497(4) . ? C15 C16 1.382(4) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O4 1.258(3) . ? C17 O3 1.260(3) . ? C18 N1 1.341(3) . ? C18 C19 1.379(4) . ? C18 H18 0.9300 . ? C19 C20 1.399(4) . ? C19 H19 0.9300 . ? C20 C21 1.390(4) . ? C20 C23 1.465(4) . ? C21 C22 1.378(4) . ? C21 H21 0.9300 . ? C22 N1 1.337(3) . ? C22 H22 0.9300 . ? C23 C24 1.355(4) . ? C23 S1 1.725(3) . ? C24 C25 1.402(5) . ? C24 H24 0.9300 . ? C25 C26 1.355(5) . ? C25 H25 0.9300 . ? C26 C26 1.453(6) 3_546 ? C26 S1 1.712(3) . ? N1 Zn1 2.026(2) . ? O1 Zn1 2.0517(18) 3_666 ? O2 Zn1 2.0405(18) . ? O3 Zn1 2.0379(18) 4 ? O4 Zn1 2.0389(19) 2_645 ? Zn1 O3 2.0379(18) 4_556 ? Zn1 O4 2.0389(19) 2_665 ? Zn1 O1 2.0518(18) 3_666 ? Zn1 Zn1 2.9822(6) 3_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 125.9(2) . . ? O2 C1 C2 117.9(2) . . ? O1 C1 C2 116.0(2) . . ? C3 C2 C7 119.3(2) . . ? C3 C2 C1 120.0(2) . . ? C7 C2 C1 120.6(2) . . ? C2 C3 C4 120.7(3) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 118.9(2) . . ? C4 C5 C8 123.4(2) . . ? C6 C5 C8 117.7(2) . . ? C7 C6 C5 120.9(3) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C2 120.2(3) . . ? C6 C7 H7 119.9 . . ? C2 C7 H7 119.9 . . ? C11 C8 C10 106.6(2) . . ? C11 C8 C5 110.6(2) . . ? C10 C8 C5 112.9(2) . . ? C11 C8 C9 113.0(2) . . ? C10 C8 C9 108.1(2) . . ? C5 C8 C9 105.7(2) . . ? F3 C9 F2 106.6(2) . . ? F3 C9 F1 107.1(2) . . ? F2 C9 F1 106.5(2) . . ? F3 C9 C8 113.3(2) . . ? F2 C9 C8 111.5(2) . . ? F1 C9 C8 111.4(2) . . ? F4 C10 F5 106.9(2) . . ? F4 C10 F6 106.5(2) . . ? F5 C10 F6 106.2(2) . . ? F4 C10 C8 113.7(2) . . ? F5 C10 C8 112.0(2) . . ? F6 C10 C8 111.1(2) . . ? C12 C11 C16 118.6(3) . . ? C12 C11 C8 123.5(2) . . ? C16 C11 C8 118.0(2) . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 120.7(3) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C15 C14 C13 118.8(3) . . ? C15 C14 C17 121.0(2) . . ? C13 C14 C17 120.2(2) . . ? C16 C15 C14 120.7(3) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C11 120.8(3) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? O4 C17 O3 125.7(3) . . ? O4 C17 C14 117.1(2) . . ? O3 C17 C14 117.2(2) . . ? N1 C18 C19 123.6(3) . . ? N1 C18 H18 118.2 . . ? C19 C18 H18 118.2 . . ? C18 C19 C20 119.1(3) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C21 C20 C19 117.0(3) . . ? C21 C20 C23 121.7(3) . . ? C19 C20 C23 121.3(3) . . ? C22 C21 C20 120.0(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? N1 C22 C21 123.0(3) . . ? N1 C22 H22 118.5 . . ? C21 C22 H22 118.5 . . ? C24 C23 C20 129.6(3) . . ? C24 C23 S1 109.7(2) . . ? C20 C23 S1 120.7(2) . . ? C23 C24 C25 113.6(3) . . ? C23 C24 H24 123.2 . . ? C25 C24 H24 123.2 . . ? C26 C25 C24 113.7(3) . . ? C26 C25 H25 123.1 . . ? C24 C25 H25 123.1 . . ? C25 C26 C26 128.9(4) . 3_546 ? C25 C26 S1 110.1(2) . . ? C26 C26 S1 121.1(3) 3_546 . ? C22 N1 C18 117.2(2) . . ? C22 N1 Zn1 121.00(18) . . ? C18 N1 Zn1 121.78(18) . . ? C1 O1 Zn1 134.43(18) . 3_666 ? C1 O2 Zn1 120.41(17) . . ? C17 O3 Zn1 122.33(18) . 4 ? C17 O4 Zn1 132.55(18) . 2_645 ? C26 S1 C23 92.88(15) . . ? N1 Zn1 O3 103.34(8) . 4_556 ? N1 Zn1 O4 97.46(8) . 2_665 ? O3 Zn1 O4 158.94(8) 4_556 2_665 ? N1 Zn1 O2 105.66(8) . . ? O3 Zn1 O2 88.87(8) 4_556 . ? O4 Zn1 O2 88.67(8) 2_665 . ? N1 Zn1 O1 95.51(8) . 3_666 ? O3 Zn1 O1 86.31(8) 4_556 3_666 ? O4 Zn1 O1 88.48(8) 2_665 3_666 ? O2 Zn1 O1 158.83(7) . 3_666 ? N1 Zn1 Zn1 167.34(6) . 3_666 ? O3 Zn1 Zn1 83.30(5) 4_556 3_666 ? O4 Zn1 Zn1 75.65(5) 2_665 3_666 ? O2 Zn1 Zn1 85.03(5) . 3_666 ? O1 Zn1 Zn1 73.95(5) 3_666 3_666 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 179.1(2) . . . . ? O1 C1 C2 C3 -4.3(4) . . . . ? O2 C1 C2 C7 -5.5(4) . . . . ? O1 C1 C2 C7 171.0(3) . . . . ? C7 C2 C3 C4 -1.9(4) . . . . ? C1 C2 C3 C4 173.5(3) . . . . ? C2 C3 C4 C5 -0.2(4) . . . . ? C3 C4 C5 C6 2.5(4) . . . . ? C3 C4 C5 C8 -174.4(3) . . . . ? C4 C5 C6 C7 -2.8(4) . . . . ? C8 C5 C6 C7 174.3(3) . . . . ? C5 C6 C7 C2 0.7(4) . . . . ? C3 C2 C7 C6 1.6(4) . . . . ? C1 C2 C7 C6 -173.7(3) . . . . ? C4 C5 C8 C11 -139.6(3) . . . . ? C6 C5 C8 C11 43.4(3) . . . . ? C4 C5 C8 C10 -20.3(4) . . . . ? C6 C5 C8 C10 162.8(2) . . . . ? C4 C5 C8 C9 97.7(3) . . . . ? C6 C5 C8 C9 -79.3(3) . . . . ? C11 C8 C9 F3 70.0(3) . . . . ? C10 C8 C9 F3 -47.7(3) . . . . ? C5 C8 C9 F3 -168.8(2) . . . . ? C11 C8 C9 F2 -169.7(2) . . . . ? C10 C8 C9 F2 72.5(3) . . . . ? C5 C8 C9 F2 -48.6(3) . . . . ? C11 C8 C9 F1 -50.8(3) . . . . ? C10 C8 C9 F1 -168.6(2) . . . . ? C5 C8 C9 F1 70.3(3) . . . . ? C11 C8 C10 F4 -170.3(2) . . . . ? C5 C8 C10 F4 68.1(3) . . . . ? C9 C8 C10 F4 -48.5(3) . . . . ? C11 C8 C10 F5 -48.9(3) . . . . ? C5 C8 C10 F5 -170.6(2) . . . . ? C9 C8 C10 F5 72.8(3) . . . . ? C11 C8 C10 F6 69.6(3) . . . . ? C5 C8 C10 F6 -52.1(3) . . . . ? C9 C8 C10 F6 -168.6(2) . . . . ? C10 C8 C11 C12 100.1(3) . . . . ? C5 C8 C11 C12 -136.8(3) . . . . ? C9 C8 C11 C12 -18.5(4) . . . . ? C10 C8 C11 C16 -79.5(3) . . . . ? C5 C8 C11 C16 43.6(3) . . . . ? C9 C8 C11 C16 162.0(2) . . . . ? C16 C11 C12 C13 -1.8(4) . . . . ? C8 C11 C12 C13 178.7(3) . . . . ? C11 C12 C13 C14 0.6(4) . . . . ? C12 C13 C14 C15 1.1(4) . . . . ? C12 C13 C14 C17 -177.7(3) . . . . ? C13 C14 C15 C16 -1.6(4) . . . . ? C17 C14 C15 C16 177.2(2) . . . . ? C14 C15 C16 C11 0.4(4) . . . . ? C12 C11 C16 C15 1.3(4) . . . . ? C8 C11 C16 C15 -179.1(2) . . . . ? C15 C14 C17 O4 178.9(2) . . . . ? C13 C14 C17 O4 -2.3(4) . . . . ? C15 C14 C17 O3 -0.9(4) . . . . ? C13 C14 C17 O3 177.9(2) . . . . ? N1 C18 C19 C20 0.5(5) . . . . ? C18 C19 C20 C21 -1.0(5) . . . . ? C18 C19 C20 C23 -179.8(3) . . . . ? C19 C20 C21 C22 0.8(4) . . . . ? C23 C20 C21 C22 179.6(3) . . . . ? C20 C21 C22 N1 -0.1(4) . . . . ? C21 C20 C23 C24 -175.8(4) . . . . ? C19 C20 C23 C24 3.0(6) . . . . ? C21 C20 C23 S1 6.2(4) . . . . ? C19 C20 C23 S1 -175.0(3) . . . . ? C20 C23 C24 C25 -178.7(4) . . . . ? S1 C23 C24 C25 -0.5(5) . . . . ? C23 C24 C25 C26 -0.6(6) . . . . ? C24 C25 C26 C26 -179.4(5) . . . 3_546 ? C24 C25 C26 S1 1.4(5) . . . . ? C21 C22 N1 C18 -0.5(4) . . . . ? C21 C22 N1 Zn1 178.6(2) . . . . ? C19 C18 N1 C22 0.3(4) . . . . ? C19 C18 N1 Zn1 -178.8(2) . . . . ? O2 C1 O1 Zn1 6.7(5) . . . 3_666 ? C2 C1 O1 Zn1 -169.61(18) . . . 3_666 ? O1 C1 O2 Zn1 -1.9(4) . . . . ? C2 C1 O2 Zn1 174.29(18) . . . . ? O4 C17 O3 Zn1 8.7(4) . . . 4 ? C14 C17 O3 Zn1 -171.49(16) . . . 4 ? O3 C17 O4 Zn1 -8.5(4) . . . 2_645 ? C14 C17 O4 Zn1 171.68(17) . . . 2_645 ? C25 C26 S1 C23 -1.4(3) . . . . ? C26 C26 S1 C23 179.4(4) 3_546 . . . ? C24 C23 S1 C26 1.1(3) . . . . ? C20 C23 S1 C26 179.5(3) . . . . ? C22 N1 Zn1 O3 -6.1(2) . . . 4_556 ? C18 N1 Zn1 O3 172.9(2) . . . 4_556 ? C22 N1 Zn1 O4 177.2(2) . . . 2_665 ? C18 N1 Zn1 O4 -3.8(2) . . . 2_665 ? C22 N1 Zn1 O2 86.5(2) . . . . ? C18 N1 Zn1 O2 -94.5(2) . . . . ? C22 N1 Zn1 O1 -93.6(2) . . . 3_666 ? C18 N1 Zn1 O1 85.4(2) . . . 3_666 ? C22 N1 Zn1 Zn1 -126.7(3) . . . 3_666 ? C18 N1 Zn1 Zn1 52.3(4) . . . 3_666 ? C1 O2 Zn1 N1 171.77(19) . . . . ? C1 O2 Zn1 O3 -84.7(2) . . . 4_556 ? C1 O2 Zn1 O4 74.4(2) . . . 2_665 ? C1 O2 Zn1 O1 -7.9(3) . . . 3_666 ? C1 O2 Zn1 Zn1 -1.31(19) . . . 3_666 ? 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 0.500 0.403 0.750 127 10 ' ' 2 0.500 0.597 0.250 127 10 ' ' 3 0.000 0.497 0.250 91 5 ' ' 4 0.000 0.502 0.750 91 5 ' ' _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.520 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.076 # === END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H14 Co F6 N O4 S' _chemical_formula_sum 'C26 H14 Co F6 N O4 S' _chemical_formula_weight 609.37 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' 'F' 'F' 0.0171 0.0103 '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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 2/c' _symmetry_space_group_name_Hall '-P 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 15.4985(11) _cell_length_b 7.5058(5) _cell_length_c 23.5458(17) _cell_angle_alpha 90.00 _cell_angle_beta 96.2720(10) _cell_angle_gamma 90.00 _cell_volume 2722.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7807 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.22 _exptl_crystal_description block _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.780 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7997 _exptl_absorpt_correction_T_max 0.8920 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19205 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4769 _reflns_number_gt 4281 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+1.0887P] 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 SHELXL _refine_ls_extinction_coef 0.0016(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4769 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1358 _refine_ls_wR_factor_gt 0.1323 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 C1 C 0.42517(17) 0.6314(3) 0.58333(11) 0.0337(6) Uani 1 1 d . . . C2 C 0.37154(17) 0.7006(4) 0.62794(11) 0.0357(6) Uani 1 1 d . . . C3 C 0.30112(18) 0.6042(4) 0.64256(12) 0.0429(7) Uani 1 1 d . . . H3 H 0.2903 0.4912 0.6272 0.051 Uiso 1 1 calc R . . C4 C 0.24680(19) 0.6734(4) 0.67971(13) 0.0445(7) Uani 1 1 d . . . H4 H 0.1996 0.6070 0.6890 0.053 Uiso 1 1 calc R . . C5 C 0.26210(17) 0.8417(4) 0.70336(12) 0.0379(6) Uani 1 1 d . . . C6 C 0.33388(18) 0.9362(4) 0.68917(12) 0.0430(7) Uani 1 1 d . . . H6 H 0.3455 1.0482 0.7051 0.052 Uiso 1 1 calc R . . C7 C 0.38794(19) 0.8676(4) 0.65221(12) 0.0422(7) Uani 1 1 d . . . H7 H 0.4357 0.9330 0.6434 0.051 Uiso 1 1 calc R . . C8 C 0.20005(17) 0.9357(4) 0.74110(11) 0.0399(6) Uani 1 1 d . . . C9 C 0.1440(2) 1.0598(5) 0.70037(14) 0.0570(9) Uani 1 1 d . . . C10 C 0.14115(19) 0.8028(5) 0.76809(14) 0.0525(8) Uani 1 1 d . . . C11 C 0.25198(16) 1.0371(4) 0.79116(11) 0.0357(6) Uani 1 1 d . . . C12 C 0.22896(19) 1.2043(4) 0.80882(13) 0.0466(7) Uani 1 1 d . . . H12 H 0.1802 1.2607 0.7905 0.056 Uiso 1 1 calc R . . C13 C 0.27760(19) 1.2877(4) 0.85327(13) 0.0466(7) Uani 1 1 d . . . H13 H 0.2617 1.4009 0.8644 0.056 Uiso 1 1 calc R . . C14 C 0.35013(16) 1.2061(4) 0.88189(11) 0.0336(6) Uani 1 1 d . . . C15 C 0.37115(16) 1.0361(3) 0.86563(11) 0.0333(5) Uani 1 1 d . . . H15 H 0.4184 0.9774 0.8850 0.040 Uiso 1 1 calc R . . C16 C 0.32227(17) 0.9528(4) 0.82070(11) 0.0366(6) Uani 1 1 d . . . H16 H 0.3369 0.8382 0.8102 0.044 Uiso 1 1 calc R . . C17 C 0.40560(16) 1.3035(4) 0.92745(11) 0.0330(6) Uani 1 1 d . . . C18 C 0.74052(19) 0.7701(4) 0.54238(16) 0.0541(9) Uani 1 1 d . . . H18 H 0.7451 0.6612 0.5613 0.065 Uiso 1 1 calc R . . C19 C 0.8124(2) 0.8789(5) 0.54606(18) 0.0640(11) Uani 1 1 d . . . H19 H 0.8640 0.8424 0.5667 0.077 Uiso 1 1 calc R . . C20 C 0.80779(17) 1.0428(4) 0.51897(12) 0.0411(7) Uani 1 1 d . . . C21 C 0.72893(18) 1.0868(4) 0.49063(14) 0.0469(7) Uani 1 1 d . . . H21 H 0.7217 1.1970 0.4727 0.056 Uiso 1 1 calc R . . C22 C 0.66007(16) 0.9702(4) 0.48828(12) 0.0408(7) Uani 1 1 d . . . H22 H 0.6076 1.0039 0.4682 0.049 Uiso 1 1 calc R . . C23 C 0.8820(2) 1.1644(4) 0.52288(16) 0.0533(8) Uani 1 1 d . . . C24 C 0.9576(3) 1.1539(7) 0.5549(3) 0.114(2) Uani 1 1 d . . . H24 H 0.9718 1.0613 0.5805 0.137 Uiso 1 1 calc R . . C25 C 1.0152(3) 1.2961(7) 0.5466(3) 0.118(2) Uani 1 1 d . . . H25 H 1.0711 1.3038 0.5652 0.141 Uiso 1 1 calc R . . C26 C 0.9810(2) 1.4177(5) 0.50943(16) 0.0628(10) Uani 1 1 d . . . Co1 Co 0.557951(19) 0.64631(4) 0.507868(12) 0.02477(15) Uani 1 1 d . . . F1 F 0.18860(15) 1.1968(3) 0.68335(9) 0.0690(6) Uani 1 1 d . . . F2 F 0.11040(15) 0.9736(4) 0.65333(9) 0.0834(7) Uani 1 1 d . . . F3 F 0.07573(12) 1.1273(3) 0.72381(10) 0.0747(7) Uani 1 1 d . . . F4 F 0.18728(14) 0.6731(3) 0.79577(9) 0.0631(5) Uani 1 1 d . . . F5 F 0.09675(13) 0.8825(3) 0.80662(10) 0.0721(6) Uani 1 1 d . . . F6 F 0.08277(12) 0.7242(3) 0.73061(9) 0.0725(6) Uani 1 1 d . . . N1 N 0.66525(13) 0.8120(3) 0.51340(9) 0.0282(4) Uani 1 1 d . . . O1 O 0.48919(12) 0.7219(3) 0.57203(8) 0.0407(4) Uani 1 1 d . . . O2 O 0.39953(13) 0.4889(3) 0.55937(8) 0.0455(5) Uani 1 1 d . . . O3 O 0.47348(12) 1.2263(3) 0.94994(8) 0.0402(4) Uani 1 1 d . . . O4 O 0.38178(12) 1.4557(3) 0.94031(9) 0.0437(5) Uani 1 1 d . . . S1 S 0.87909(6) 1.35400(12) 0.48204(5) 0.0668(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0364(14) 0.0360(15) 0.0294(12) -0.0036(10) 0.0076(11) 0.0018(11) C2 0.0371(13) 0.0380(14) 0.0327(12) -0.0083(11) 0.0075(11) -0.0009(11) C3 0.0457(15) 0.0409(15) 0.0434(15) -0.0144(13) 0.0110(12) -0.0096(13) C4 0.0402(15) 0.0504(18) 0.0452(15) -0.0163(13) 0.0147(12) -0.0125(13) C5 0.0350(14) 0.0446(17) 0.0350(13) -0.0113(11) 0.0078(11) -0.0014(11) C6 0.0469(15) 0.0395(16) 0.0439(15) -0.0162(12) 0.0101(12) -0.0060(13) C7 0.0420(15) 0.0428(16) 0.0442(15) -0.0118(12) 0.0153(12) -0.0114(12) C8 0.0315(12) 0.0498(17) 0.0385(14) -0.0141(12) 0.0038(11) 0.0034(12) C9 0.0463(17) 0.076(3) 0.0465(17) -0.0182(17) -0.0071(14) 0.0143(17) C10 0.0395(15) 0.069(2) 0.0509(17) -0.0228(17) 0.0153(14) -0.0049(16) C11 0.0303(12) 0.0436(15) 0.0331(12) -0.0103(11) 0.0041(10) 0.0032(11) C12 0.0400(15) 0.0500(17) 0.0470(16) -0.0141(14) -0.0085(12) 0.0203(14) C13 0.0483(16) 0.0368(15) 0.0530(16) -0.0150(13) -0.0025(13) 0.0170(13) C14 0.0340(13) 0.0324(13) 0.0344(12) -0.0052(11) 0.0035(10) 0.0046(11) C15 0.0311(12) 0.0350(14) 0.0335(12) -0.0019(10) 0.0021(10) 0.0074(11) C16 0.0386(13) 0.0319(14) 0.0399(13) -0.0082(11) 0.0069(11) 0.0064(11) C17 0.0333(13) 0.0338(14) 0.0330(12) -0.0037(11) 0.0080(10) 0.0017(11) C18 0.0379(15) 0.0388(17) 0.082(2) 0.0272(16) -0.0094(15) -0.0129(13) C19 0.0353(16) 0.0526(19) 0.098(3) 0.0328(19) -0.0187(17) -0.0184(14) C20 0.0328(13) 0.0372(15) 0.0520(16) 0.0109(12) -0.0010(12) -0.0159(12) C21 0.0399(15) 0.0309(14) 0.0670(19) 0.0177(14) -0.0070(13) -0.0141(12) C22 0.0306(13) 0.0355(15) 0.0543(16) 0.0129(12) -0.0041(12) -0.0104(11) C23 0.0410(16) 0.0464(18) 0.070(2) 0.0217(15) -0.0055(15) -0.0228(13) C24 0.070(3) 0.098(4) 0.159(5) 0.088(3) -0.059(3) -0.057(3) C25 0.068(3) 0.101(3) 0.167(5) 0.080(4) -0.064(3) -0.064(3) C26 0.0471(18) 0.060(2) 0.076(2) 0.0255(19) -0.0160(16) -0.0356(17) Co1 0.0250(2) 0.0215(2) 0.0281(2) -0.00089(11) 0.00469(14) -0.00755(11) F1 0.0733(13) 0.0740(14) 0.0579(11) 0.0109(11) -0.0005(10) 0.0140(12) F2 0.0777(14) 0.1093(19) 0.0557(12) -0.0279(12) -0.0273(11) 0.0211(13) F3 0.0439(11) 0.1021(18) 0.0755(14) -0.0200(12) -0.0051(10) 0.0269(11) F4 0.0633(12) 0.0627(12) 0.0664(12) 0.0000(10) 0.0208(10) -0.0092(10) F5 0.0575(12) 0.0959(16) 0.0691(13) -0.0282(12) 0.0348(10) -0.0072(11) F6 0.0404(9) 0.1036(17) 0.0749(13) -0.0348(13) 0.0127(9) -0.0214(11) N1 0.0286(10) 0.0224(10) 0.0339(10) 0.0000(8) 0.0054(8) -0.0071(8) O1 0.0435(10) 0.0404(11) 0.0408(10) -0.0085(8) 0.0166(8) -0.0068(9) O2 0.0509(11) 0.0450(11) 0.0433(10) -0.0181(9) 0.0169(9) -0.0074(9) O3 0.0390(10) 0.0377(11) 0.0420(10) -0.0058(8) -0.0048(8) 0.0033(8) O4 0.0409(10) 0.0355(11) 0.0540(11) -0.0192(9) 0.0014(9) 0.0034(8) S1 0.0464(5) 0.0549(6) 0.0927(7) 0.0352(5) -0.0213(5) -0.0342(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.253(3) . ? C1 O1 1.255(3) . ? C1 C2 1.502(3) . ? C2 C3 1.384(4) . ? C2 C7 1.389(4) . ? C3 C4 1.380(4) . ? C3 H3 0.9300 . ? C4 C5 1.391(4) . ? C4 H4 0.9300 . ? C5 C6 1.390(4) . ? C5 C8 1.549(3) . ? C6 C7 1.372(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C10 1.536(5) . ? C8 C9 1.537(5) . ? C8 C11 1.552(4) . ? C9 F1 1.325(5) . ? C9 F2 1.338(4) . ? C9 F3 1.344(4) . ? C10 F6 1.331(4) . ? C10 F4 1.335(4) . ? C10 F5 1.338(3) . ? C11 C16 1.380(4) . ? C11 C12 1.381(4) . ? C12 C13 1.372(4) . ? C12 H12 0.9300 . ? C13 C14 1.389(4) . ? C13 H13 0.9300 . ? C14 C15 1.381(4) . ? C14 C17 1.491(4) . ? C15 C16 1.382(4) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O4 1.248(3) . ? C17 O3 1.265(3) . ? C18 N1 1.323(4) . ? C18 C19 1.377(4) . ? C18 H18 0.9300 . ? C19 C20 1.384(4) . ? C19 H19 0.9300 . ? C20 C21 1.368(4) . ? C20 C23 1.463(4) . ? C21 C22 1.377(4) . ? C21 H21 0.9300 . ? C22 N1 1.325(3) . ? C22 H22 0.9300 . ? C23 C24 1.325(5) . ? C23 S1 1.716(3) . ? C24 C25 1.418(5) . ? C24 H24 0.9300 . ? C25 C26 1.333(5) . ? C25 H25 0.9300 . ? C26 C26 1.458(6) 3_786 ? C26 S1 1.708(3) . ? Co1 O1 2.0229(18) . ? Co1 O3 2.0243(18) 4_575 ? Co1 O4 2.0392(18) 2_646 ? Co1 O2 2.0492(18) 3_666 ? Co1 N1 2.0693(19) . ? Co1 Co1 2.8359(6) 3_666 ? O2 Co1 2.0492(18) 3_666 ? O3 Co1 2.0243(18) 4_576 ? O4 Co1 2.0392(18) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 125.9(2) . . ? O2 C1 C2 115.9(2) . . ? O1 C1 C2 118.2(2) . . ? C3 C2 C7 118.9(2) . . ? C3 C2 C1 120.3(2) . . ? C7 C2 C1 120.6(2) . . ? C4 C3 C2 120.9(3) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 120.4(3) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 118.2(2) . . ? C6 C5 C8 118.0(2) . . ? C4 C5 C8 123.7(3) . . ? C7 C6 C5 121.4(3) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C2 120.1(3) . . ? C6 C7 H7 119.9 . . ? C2 C7 H7 119.9 . . ? C10 C8 C9 109.3(3) . . ? C10 C8 C5 112.1(2) . . ? C9 C8 C5 105.2(2) . . ? C10 C8 C11 106.6(2) . . ? C9 C8 C11 112.8(3) . . ? C5 C8 C11 110.9(2) . . ? F1 C9 F2 107.1(3) . . ? F1 C9 F3 107.0(3) . . ? F2 C9 F3 105.7(3) . . ? F1 C9 C8 112.4(3) . . ? F2 C9 C8 111.4(3) . . ? F3 C9 C8 112.9(3) . . ? F6 C10 F4 106.8(3) . . ? F6 C10 F5 106.6(2) . . ? F4 C10 F5 106.4(3) . . ? F6 C10 C8 113.9(3) . . ? F4 C10 C8 111.4(2) . . ? F5 C10 C8 111.3(3) . . ? C16 C11 C12 118.7(2) . . ? C16 C11 C8 118.2(2) . . ? C12 C11 C8 123.0(2) . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 121.1(3) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C15 C14 C13 118.4(2) . . ? C15 C14 C17 121.2(2) . . ? C13 C14 C17 120.3(2) . . ? C14 C15 C16 120.3(2) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C11 C16 C15 121.0(2) . . ? C11 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? O4 C17 O3 124.9(2) . . ? O4 C17 C14 117.5(2) . . ? O3 C17 C14 117.7(2) . . ? N1 C18 C19 123.6(3) . . ? N1 C18 H18 118.2 . . ? C19 C18 H18 118.2 . . ? C18 C19 C20 119.8(3) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C21 C20 C19 116.0(2) . . ? C21 C20 C23 122.3(3) . . ? C19 C20 C23 121.6(3) . . ? C20 C21 C22 120.9(3) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? N1 C22 C21 122.9(2) . . ? N1 C22 H22 118.6 . . ? C21 C22 H22 118.6 . . ? C24 C23 C20 129.7(3) . . ? C24 C23 S1 109.6(2) . . ? C20 C23 S1 120.7(2) . . ? C23 C24 C25 114.1(3) . . ? C23 C24 H24 123.0 . . ? C25 C24 H24 123.0 . . ? C26 C25 C24 113.3(3) . . ? C26 C25 H25 123.4 . . ? C24 C25 H25 123.4 . . ? C25 C26 C26 129.5(4) . 3_786 ? C25 C26 S1 109.9(2) . . ? C26 C26 S1 120.6(3) 3_786 . ? O1 Co1 O3 90.92(8) . 4_575 ? O1 Co1 O4 89.66(8) . 2_646 ? O3 Co1 O4 162.68(8) 4_575 2_646 ? O1 Co1 O2 162.96(8) . 3_666 ? O3 Co1 O2 87.26(8) 4_575 3_666 ? O4 Co1 O2 87.13(9) 2_646 3_666 ? O1 Co1 N1 105.65(8) . . ? O3 Co1 N1 102.40(8) 4_575 . ? O4 Co1 N1 94.10(8) 2_646 . ? O2 Co1 N1 91.27(8) 3_666 . ? O1 Co1 Co1 86.38(6) . 3_666 ? O3 Co1 Co1 85.63(6) 4_575 3_666 ? O4 Co1 Co1 77.12(6) 2_646 3_666 ? O2 Co1 Co1 76.59(6) 3_666 3_666 ? N1 Co1 Co1 165.22(6) . 3_666 ? C18 N1 C22 116.7(2) . . ? C18 N1 Co1 123.15(18) . . ? C22 N1 Co1 120.09(16) . . ? C1 O1 Co1 119.99(17) . . ? C1 O2 Co1 131.10(17) . 3_666 ? C17 O3 Co1 120.85(17) . 4_576 ? C17 O4 Co1 131.22(17) . 2_666 ? C26 S1 C23 93.12(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 3.2(4) . . . . ? O1 C1 C2 C3 -178.9(3) . . . . ? O2 C1 C2 C7 -172.3(3) . . . . ? O1 C1 C2 C7 5.6(4) . . . . ? C7 C2 C3 C4 1.3(5) . . . . ? C1 C2 C3 C4 -174.2(3) . . . . ? C2 C3 C4 C5 -0.2(5) . . . . ? C3 C4 C5 C6 -0.9(5) . . . . ? C3 C4 C5 C8 174.5(3) . . . . ? C4 C5 C6 C7 1.0(5) . . . . ? C8 C5 C6 C7 -174.7(3) . . . . ? C5 C6 C7 C2 0.1(5) . . . . ? C3 C2 C7 C6 -1.3(4) . . . . ? C1 C2 C7 C6 174.3(3) . . . . ? C6 C5 C8 C10 -162.7(3) . . . . ? C4 C5 C8 C10 21.9(4) . . . . ? C6 C5 C8 C9 78.6(3) . . . . ? C4 C5 C8 C9 -96.8(3) . . . . ? C6 C5 C8 C11 -43.7(4) . . . . ? C4 C5 C8 C11 140.9(3) . . . . ? C10 C8 C9 F1 168.9(2) . . . . ? C5 C8 C9 F1 -70.5(3) . . . . ? C11 C8 C9 F1 50.5(3) . . . . ? C10 C8 C9 F2 -70.9(3) . . . . ? C5 C8 C9 F2 49.6(3) . . . . ? C11 C8 C9 F2 170.6(3) . . . . ? C10 C8 C9 F3 47.8(4) . . . . ? C5 C8 C9 F3 168.4(3) . . . . ? C11 C8 C9 F3 -70.6(4) . . . . ? C9 C8 C10 F6 48.1(3) . . . . ? C5 C8 C10 F6 -68.2(3) . . . . ? C11 C8 C10 F6 170.3(2) . . . . ? C9 C8 C10 F4 169.0(2) . . . . ? C5 C8 C10 F4 52.7(3) . . . . ? C11 C8 C10 F4 -68.8(3) . . . . ? C9 C8 C10 F5 -72.4(3) . . . . ? C5 C8 C10 F5 171.3(2) . . . . ? C11 C8 C10 F5 49.8(3) . . . . ? C10 C8 C11 C16 78.4(3) . . . . ? C9 C8 C11 C16 -161.6(3) . . . . ? C5 C8 C11 C16 -43.9(4) . . . . ? C10 C8 C11 C12 -98.9(3) . . . . ? C9 C8 C11 C12 21.1(4) . . . . ? C5 C8 C11 C12 138.8(3) . . . . ? C16 C11 C12 C13 2.9(5) . . . . ? C8 C11 C12 C13 -179.8(3) . . . . ? C11 C12 C13 C14 -0.7(5) . . . . ? C12 C13 C14 C15 -1.7(5) . . . . ? C12 C13 C14 C17 175.9(3) . . . . ? C13 C14 C15 C16 2.0(4) . . . . ? C17 C14 C15 C16 -175.6(2) . . . . ? C12 C11 C16 C15 -2.6(4) . . . . ? C8 C11 C16 C15 179.9(2) . . . . ? C14 C15 C16 C11 0.2(4) . . . . ? C15 C14 C17 O4 -179.1(2) . . . . ? C13 C14 C17 O4 3.4(4) . . . . ? C15 C14 C17 O3 1.3(4) . . . . ? C13 C14 C17 O3 -176.2(3) . . . . ? N1 C18 C19 C20 0.7(7) . . . . ? C18 C19 C20 C21 1.3(6) . . . . ? C18 C19 C20 C23 178.5(4) . . . . ? C19 C20 C21 C22 -2.0(5) . . . . ? C23 C20 C21 C22 -179.2(3) . . . . ? C20 C21 C22 N1 0.9(5) . . . . ? C21 C20 C23 C24 169.2(5) . . . . ? C19 C20 C23 C24 -7.8(7) . . . . ? C21 C20 C23 S1 -11.0(5) . . . . ? C19 C20 C23 S1 172.0(3) . . . . ? C20 C23 C24 C25 178.9(5) . . . . ? S1 C23 C24 C25 -0.9(7) . . . . ? C23 C24 C25 C26 2.2(9) . . . . ? C24 C25 C26 C26 179.0(6) . . . 3_786 ? C24 C25 C26 S1 -2.4(8) . . . . ? C19 C18 N1 C22 -1.9(5) . . . . ? C19 C18 N1 Co1 179.6(3) . . . . ? C21 C22 N1 C18 1.1(4) . . . . ? C21 C22 N1 Co1 179.7(2) . . . . ? O1 Co1 N1 C18 92.9(3) . . . . ? O3 Co1 N1 C18 -172.6(2) 4_575 . . . ? O4 Co1 N1 C18 2.1(3) 2_646 . . . ? O2 Co1 N1 C18 -85.1(3) 3_666 . . . ? Co1 Co1 N1 C18 -50.7(4) 3_666 . . . ? O1 Co1 N1 C22 -85.6(2) . . . . ? O3 Co1 N1 C22 8.9(2) 4_575 . . . ? O4 Co1 N1 C22 -176.4(2) 2_646 . . . ? O2 Co1 N1 C22 96.4(2) 3_666 . . . ? Co1 Co1 N1 C22 130.8(2) 3_666 . . . ? O2 C1 O1 Co1 2.7(4) . . . . ? C2 C1 O1 Co1 -174.93(17) . . . . ? O3 Co1 O1 C1 84.8(2) 4_575 . . . ? O4 Co1 O1 C1 -77.8(2) 2_646 . . . ? O2 Co1 O1 C1 1.2(4) 3_666 . . . ? N1 Co1 O1 C1 -172.00(19) . . . . ? Co1 Co1 O1 C1 -0.72(19) 3_666 . . . ? O1 C1 O2 Co1 -4.0(4) . . . 3_666 ? C2 C1 O2 Co1 173.72(18) . . . 3_666 ? O4 C17 O3 Co1 -4.2(4) . . . 4_576 ? C14 C17 O3 Co1 175.38(17) . . . 4_576 ? O3 C17 O4 Co1 7.4(4) . . . 2_666 ? C14 C17 O4 Co1 -172.14(17) . . . 2_666 ? C25 C26 S1 C23 1.6(5) . . . . ? C26 C26 S1 C23 -179.6(5) 3_786 . . . ? C24 C23 S1 C26 -0.4(4) . . . . ? C20 C23 S1 C26 179.8(3) . . . . ? 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 1 0.500 0.409 0.750 131.1 39.9 2 0.500 0.591 0.250 131.1 40.1 3 -0.039 0.490 0.147 44.0 1.6 4 0.040 0.488 0.355 43.9 2.1 5 0.039 0.510 0.853 44.9 2.0 6 0.960 0.512 0.645 43.1 1.7 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.391 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.081 # === END data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H22 N2 O4 S2 Zn' _chemical_formula_sum 'C26 H22 N2 O4 S2 Zn' _chemical_formula_weight 555.95 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' 'Zn' 'Zn' 0.2839 1.4301 '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' 'O' 'O' 0.0106 0.0060 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 2/c' _symmetry_space_group_name_Hall '-P 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 12.9879(16) _cell_length_b 6.2776(8) _cell_length_c 19.1040(17) _cell_angle_alpha 90.00 _cell_angle_beta 114.325(6) _cell_angle_gamma 90.00 _cell_volume 1419.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3439 _cell_measurement_theta_min 3.25 _cell_measurement_theta_max 28.18 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_absorpt_coefficient_mu 1.044 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7448 _exptl_absorpt_correction_T_max 0.8344 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7143 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2496 _reflns_number_gt 2205 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+1.9900P] 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 2496 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.1147 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 O2 O 0.8772(3) 0.5687(5) 0.84283(18) 0.0657(10) Uani 1 1 d . . . Zn1 Zn 1.0000 0.61594(7) 0.7500 0.01830(17) Uani 1 2 d S . . C6 C 0.7821(3) 0.0726(5) 0.67506(18) 0.0303(7) Uani 1 1 d . . . H6 H 0.7671 -0.0415 0.7005 0.036 Uiso 1 1 calc R . . C8 C 0.7575(2) 0.2595(5) 0.56105(16) 0.0213(6) Uani 1 1 d . . . H8 H 0.7258 0.2742 0.5079 0.026 Uiso 1 1 calc R . . S1 S 0.60216(6) -0.27646(12) 0.58944(4) 0.0241(2) Uani 1 1 d . . . N1 N 0.8788(2) 0.4020(4) 0.68368(14) 0.0212(5) Uani 1 1 d . . . O1 O 0.9931(2) 0.8033(4) 0.82955(12) 0.0299(5) Uani 1 1 d . . . C13 C 0.5327(2) -0.4046(5) 0.50219(18) 0.0237(7) Uani 1 1 d . . . C10 C 0.6562(2) -0.0848(5) 0.54802(17) 0.0232(6) Uani 1 1 d . . . C2 C 0.9445(3) 0.8450(5) 0.93640(16) 0.0213(6) Uani 1 1 d . . . H2 H 0.8874 0.7865 0.9523 0.026 Uiso 1 1 calc R . . C9 C 0.8303(2) 0.4122(5) 0.60655(17) 0.0220(6) Uani 1 1 d . . . H9 H 0.8467 0.5285 0.5828 0.026 Uiso 1 1 calc R . . C3 C 1.0619(3) 0.8031(5) 1.00118(17) 0.0238(6) Uani 1 1 d . . . H3A H 1.0725 0.6510 1.0103 0.029 Uiso 1 1 calc R . . H3B H 1.1197 0.8539 0.9855 0.029 Uiso 1 1 calc R . . C4 C 1.0751(3) 0.9145(5) 1.07532(17) 0.0247(7) Uani 1 1 d . . . H4A H 1.1506 0.8888 1.1144 0.030 Uiso 1 1 calc R . . H4B H 1.0215 0.8550 1.0933 0.030 Uiso 1 1 calc R . . C11 C 0.6200(3) -0.1207(5) 0.47114(18) 0.0277(7) Uani 1 1 d . . . H11 H 0.6392 -0.0342 0.4388 0.033 Uiso 1 1 calc R . . C7 C 0.7314(2) 0.0824(5) 0.59477(17) 0.0221(6) Uani 1 1 d . . . C1 C 0.9336(3) 0.7318(5) 0.86334(17) 0.0237(7) Uani 1 1 d . . . C12 C 0.5505(3) -0.3021(5) 0.44553(18) 0.0298(7) Uani 1 1 d . . . H12 H 0.5198 -0.3473 0.3947 0.036 Uiso 1 1 calc R . . C5 C 0.8541(3) 0.2314(5) 0.71614(19) 0.0320(8) Uani 1 1 d . . . H5 H 0.8876 0.2202 0.7694 0.038 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 O2 0.091(2) 0.070(2) 0.0593(19) -0.0390(17) 0.0543(18) -0.0486(19) Zn1 0.0238(3) 0.0173(3) 0.0135(3) 0.000 0.00731(19) 0.000 C6 0.0386(18) 0.0286(17) 0.0203(15) 0.0024(13) 0.0088(14) -0.0097(15) C8 0.0196(14) 0.0311(16) 0.0120(13) -0.0015(12) 0.0055(11) 0.0018(12) S1 0.0265(4) 0.0230(4) 0.0212(4) -0.0052(3) 0.0082(3) -0.0031(3) N1 0.0239(13) 0.0218(13) 0.0164(12) -0.0006(10) 0.0067(10) -0.0003(10) O1 0.0441(13) 0.0298(12) 0.0237(11) -0.0068(9) 0.0219(10) -0.0064(10) C13 0.0207(14) 0.0237(16) 0.0223(15) -0.0062(12) 0.0044(12) 0.0024(12) C10 0.0211(14) 0.0240(16) 0.0239(15) -0.0028(12) 0.0088(12) 0.0012(12) C2 0.0256(15) 0.0238(15) 0.0177(14) -0.0009(12) 0.0121(12) -0.0012(12) C9 0.0212(14) 0.0245(16) 0.0211(15) 0.0017(12) 0.0095(12) 0.0012(12) C3 0.0324(16) 0.0216(15) 0.0216(15) -0.0009(12) 0.0151(13) 0.0049(13) C4 0.0312(16) 0.0249(16) 0.0183(14) 0.0016(12) 0.0104(13) 0.0049(13) C11 0.0295(16) 0.0307(17) 0.0205(15) -0.0024(13) 0.0079(13) -0.0043(13) C7 0.0190(14) 0.0232(15) 0.0234(15) -0.0037(12) 0.0080(12) 0.0015(12) C1 0.0295(16) 0.0244(16) 0.0194(15) -0.0018(12) 0.0125(13) -0.0004(13) C12 0.0298(17) 0.0326(18) 0.0223(16) -0.0073(14) 0.0059(13) -0.0034(14) C5 0.042(2) 0.0327(18) 0.0172(15) 0.0004(13) 0.0077(14) -0.0095(15) _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 O2 C1 1.225(4) . ? Zn1 O1 1.953(2) . ? Zn1 O1 1.953(2) 2_756 ? Zn1 N1 2.060(2) . ? Zn1 N1 2.060(2) 2_756 ? C6 C5 1.371(5) . ? C6 C7 1.399(4) . ? C6 H6 0.9300 . ? C8 C9 1.375(4) . ? C8 C7 1.395(4) . ? C8 H8 0.9300 . ? S1 C13 1.732(3) . ? S1 C10 1.739(3) . ? N1 C5 1.341(4) . ? N1 C9 1.344(4) . ? O1 C1 1.275(4) . ? C13 C12 1.359(5) . ? C13 C13 1.450(6) 3_646 ? C10 C11 1.364(4) . ? C10 C7 1.461(4) . ? C2 C1 1.520(4) . ? C2 C4 1.533(4) 3_777 ? C2 C3 1.540(4) . ? C2 H2 0.9800 . ? C9 H9 0.9300 . ? C3 C4 1.524(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C2 1.533(4) 3_777 ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C11 C12 1.409(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C5 H5 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O1 105.93(14) . 2_756 ? O1 Zn1 N1 127.09(10) . . ? O1 Zn1 N1 100.51(10) 2_756 . ? O1 Zn1 N1 100.51(10) . 2_756 ? O1 Zn1 N1 127.08(10) 2_756 2_756 ? N1 Zn1 N1 98.62(14) . 2_756 ? C5 C6 C7 119.8(3) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C9 C8 C7 119.9(3) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C13 S1 C10 91.81(15) . . ? C5 N1 C9 116.8(3) . . ? C5 N1 Zn1 120.3(2) . . ? C9 N1 Zn1 122.5(2) . . ? C1 O1 Zn1 114.4(2) . . ? C12 C13 C13 129.3(4) . 3_646 ? C12 C13 S1 110.7(2) . . ? C13 C13 S1 120.0(3) 3_646 . ? C11 C10 C7 128.7(3) . . ? C11 C10 S1 110.5(2) . . ? C7 C10 S1 120.8(2) . . ? C1 C2 C4 112.3(2) . 3_777 ? C1 C2 C3 110.2(2) . . ? C4 C2 C3 109.6(3) 3_777 . ? C1 C2 H2 108.2 . . ? C4 C2 H2 108.2 3_777 . ? C3 C2 H2 108.2 . . ? N1 C9 C8 123.3(3) . . ? N1 C9 H9 118.3 . . ? C8 C9 H9 118.3 . . ? C4 C3 C2 111.3(2) . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C3 C4 C2 111.6(2) . 3_777 ? C3 C4 H4A 109.3 . . ? C2 C4 H4A 109.3 3_777 . ? C3 C4 H4B 109.3 . . ? C2 C4 H4B 109.3 3_777 . ? H4A C4 H4B 108.0 . . ? C10 C11 C12 113.3(3) . . ? C10 C11 H11 123.4 . . ? C12 C11 H11 123.4 . . ? C8 C7 C6 116.5(3) . . ? C8 C7 C10 121.3(3) . . ? C6 C7 C10 122.2(3) . . ? O2 C1 O1 122.6(3) . . ? O2 C1 C2 120.1(3) . . ? O1 C1 C2 117.0(3) . . ? C13 C12 C11 113.6(3) . . ? C13 C12 H12 123.2 . . ? C11 C12 H12 123.2 . . ? N1 C5 C6 123.6(3) . . ? N1 C5 H5 118.2 . . ? C6 C5 H5 118.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Zn1 N1 C5 -66.1(3) . . . . ? O1 Zn1 N1 C5 174.6(2) 2_756 . . . ? N1 Zn1 N1 C5 44.1(2) 2_756 . . . ? O1 Zn1 N1 C9 121.2(2) . . . . ? O1 Zn1 N1 C9 1.9(2) 2_756 . . . ? N1 Zn1 N1 C9 -128.5(3) 2_756 . . . ? O1 Zn1 O1 C1 145.8(3) 2_756 . . . ? N1 Zn1 O1 C1 28.8(3) . . . . ? N1 Zn1 O1 C1 -80.5(2) 2_756 . . . ? C10 S1 C13 C12 -0.5(3) . . . . ? C10 S1 C13 C13 179.2(3) . . . 3_646 ? C13 S1 C10 C11 0.7(2) . . . . ? C13 S1 C10 C7 -178.1(2) . . . . ? C5 N1 C9 C8 0.6(4) . . . . ? Zn1 N1 C9 C8 173.5(2) . . . . ? C7 C8 C9 N1 -0.3(4) . . . . ? C1 C2 C3 C4 -179.9(3) . . . . ? C4 C2 C3 C4 56.1(3) 3_777 . . . ? C2 C3 C4 C2 -57.2(4) . . . 3_777 ? C7 C10 C11 C12 178.0(3) . . . . ? S1 C10 C11 C12 -0.8(4) . . . . ? C9 C8 C7 C6 0.3(4) . . . . ? C9 C8 C7 C10 -178.7(3) . . . . ? C5 C6 C7 C8 -0.5(5) . . . . ? C5 C6 C7 C10 178.5(3) . . . . ? C11 C10 C7 C8 14.1(5) . . . . ? S1 C10 C7 C8 -167.3(2) . . . . ? C11 C10 C7 C6 -164.9(3) . . . . ? S1 C10 C7 C6 13.7(4) . . . . ? Zn1 O1 C1 O2 -6.3(4) . . . . ? Zn1 O1 C1 C2 167.4(2) . . . . ? C4 C2 C1 O2 -132.9(4) 3_777 . . . ? C3 C2 C1 O2 104.6(4) . . . . ? C4 C2 C1 O1 53.2(4) 3_777 . . . ? C3 C2 C1 O1 -69.3(4) . . . . ? C13 C13 C12 C11 -179.5(4) 3_646 . . . ? S1 C13 C12 C11 0.1(4) . . . . ? C10 C11 C12 C13 0.4(4) . . . . ? C9 N1 C5 C6 -0.9(5) . . . . ? Zn1 N1 C5 C6 -173.9(3) . . . . ? C7 C6 C5 N1 0.9(6) . . . . ? 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 0.500 -0.028 0.250 188 31 ' ' 2 0.500 -0.061 0.750 188 31 ' ' _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.955 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.091 # === END data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H28 N2 O12 S4 Zn2' _chemical_formula_sum 'C46 H28 N2 O12 S4 Zn2' _chemical_formula_weight 1059.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.7472(12) _cell_length_b 21.8339(19) _cell_length_c 15.9121(14) _cell_angle_alpha 90.00 _cell_angle_beta 115.59 _cell_angle_gamma 90.00 _cell_volume 4307.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5210 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 28.35 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 1.377 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6829 _exptl_absorpt_correction_T_max 0.7897 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24017 _diffrn_reflns_av_R_equivalents 0.1136 _diffrn_reflns_av_sigmaI/netI 0.0953 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7574 _reflns_number_gt 5177 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+0.1000P] 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 7574 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0952 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.2193 _refine_ls_wR_factor_gt 0.1789 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3045(5) -0.1354(3) 0.6179(5) 0.0178(15) Uani 1 1 d . . . C2 C 0.3673(5) -0.1330(3) 0.5594(5) 0.0159(15) Uani 1 1 d . . . C3 C 0.3683(5) -0.1833(3) 0.5048(5) 0.0166(15) Uani 1 1 d . . . H3 H 0.3293 -0.2184 0.5034 0.020 Uiso 1 1 calc R . . C4 C 0.4278(5) -0.1805(3) 0.4528(5) 0.0192(15) Uani 1 1 d . . . H4 H 0.4276 -0.2131 0.4151 0.023 Uiso 1 1 calc R . . C5 C 0.4878(5) -0.1277(3) 0.4585(5) 0.0169(15) Uani 1 1 d . . . C6 C 0.4919(6) -0.0789(3) 0.5166(5) 0.0213(16) Uani 1 1 d . . . H6 H 0.5357 -0.0451 0.5224 0.026 Uiso 1 1 calc R . . C7 C 0.4292(6) -0.0818(3) 0.5652(5) 0.0205(16) Uani 1 1 d . . . H7 H 0.4288 -0.0489 0.6023 0.025 Uiso 1 1 calc R . . C8 C 0.6910(5) -0.1147(3) 0.4567(5) 0.0183(15) Uani 1 1 d . . . C9 C 0.7417(5) -0.1670(3) 0.5085(5) 0.0161(15) Uani 1 1 d . . . H9 H 0.7011 -0.2007 0.5099 0.019 Uiso 1 1 calc R . . C10 C 0.8518(6) -0.1676(3) 0.5570(5) 0.0207(16) Uani 1 1 d . . . H10 H 0.8863 -0.2028 0.5889 0.025 Uiso 1 1 calc R . . C11 C 0.9140(5) -0.1152(3) 0.5592(5) 0.0155(14) Uani 1 1 d . . . C12 C 0.8609(5) -0.0629(3) 0.5111(5) 0.0198(16) Uani 1 1 d . . . H12 H 0.9005 -0.0276 0.5153 0.024 Uiso 1 1 calc R . . C13 C 0.7495(5) -0.0624(3) 0.4567(5) 0.0168(15) Uani 1 1 d . . . H13 H 0.7152 -0.0282 0.4215 0.020 Uiso 1 1 calc R . . C14 C 1.0349(5) -0.1153(3) 0.6229(5) 0.0196(16) Uani 1 1 d . . . C15 C 0.1579(5) -0.1328(3) 0.8664(4) 0.0153(14) Uani 1 1 d . . . C16 C 0.0997(5) -0.1346(3) 0.9262(5) 0.0164(15) Uani 1 1 d . . . C17 C 0.0851(5) -0.1887(3) 0.9657(5) 0.0173(15) Uani 1 1 d . . . H17 H 0.1151 -0.2250 0.9572 0.021 Uiso 1 1 calc R . . C18 C 0.0256(5) -0.1887(3) 1.0180(5) 0.0193(15) Uani 1 1 d . . . H18 H 0.0157 -0.2248 1.0444 0.023 Uiso 1 1 calc R . . C19 C -0.0182(5) -0.1347(3) 1.0302(5) 0.0139(14) Uani 1 1 d . . . C20 C -0.0046(6) -0.0802(3) 0.9904(6) 0.0257(18) Uani 1 1 d . . . H20 H -0.0372 -0.0443 0.9969 0.031 Uiso 1 1 calc R . . C21 C 0.0564(6) -0.0798(3) 0.9420(5) 0.0228(17) Uani 1 1 d . . . H21 H 0.0695 -0.0431 0.9192 0.027 Uiso 1 1 calc R . . C22 C -0.2306(5) -0.1262(3) 1.0206(5) 0.0160(15) Uani 1 1 d . . . C23 C -0.2798(6) -0.1775(3) 0.9664(5) 0.0193(16) Uani 1 1 d . . . H23 H -0.2388 -0.2104 0.9630 0.023 Uiso 1 1 calc R . . C24 C -0.3894(5) -0.1781(3) 0.9185(5) 0.0180(15) Uani 1 1 d . . . H24 H -0.4242 -0.2134 0.8872 0.022 Uiso 1 1 calc R . . C25 C -0.4497(5) -0.1259(3) 0.9162(4) 0.0144(14) Uani 1 1 d . . . C26 C -0.3981(5) -0.0749(3) 0.9642(5) 0.0239(17) Uani 1 1 d . . . H26 H -0.4380 -0.0398 0.9605 0.029 Uiso 1 1 calc R . . C27 C -0.2874(5) -0.0741(3) 1.0186(5) 0.0173(15) Uani 1 1 d . . . H27 H -0.2529 -0.0395 1.0525 0.021 Uiso 1 1 calc R . . C28 C -0.5706(6) -0.1266(3) 0.8584(6) 0.0228(17) Uani 1 1 d . . . C29 C 0.3455(6) 0.0593(3) 0.7912(5) 0.0177(15) Uani 1 1 d . . . H29 H 0.4051 0.0336 0.8159 0.021 Uiso 1 1 calc R . . C30 C 0.3636(6) 0.1214(3) 0.7991(5) 0.0189(15) Uani 1 1 d . . . H30 H 0.4332 0.1367 0.8310 0.023 Uiso 1 1 calc R . . C31 C 0.2762(6) 0.1609(3) 0.7587(5) 0.0207(16) Uani 1 1 d . . . C32 C 0.1731(6) 0.1345(3) 0.7124(5) 0.0214(16) Uani 1 1 d . . . H32 H 0.1124 0.1592 0.6834 0.026 Uiso 1 1 calc R . . C33 C 0.1633(6) 0.0711(3) 0.7108(5) 0.0177(15) Uani 1 1 d . . . H33 H 0.0948 0.0540 0.6810 0.021 Uiso 1 1 calc R . . C34 C 0.2921(6) 0.2278(3) 0.7624(5) 0.0181(15) Uani 1 1 d . . . C35 C 0.3862(6) 0.2586(3) 0.7840(5) 0.0240(17) Uani 1 1 d . . . H35 H 0.4520 0.2394 0.7987 0.029 Uiso 1 1 calc R . . C36 C 0.3726(6) 0.3226(3) 0.7814(5) 0.0239(17) Uani 1 1 d . . . H36 H 0.4294 0.3499 0.7954 0.029 Uiso 1 1 calc R . . C37 C 0.2711(6) 0.3408(3) 0.7571(5) 0.0177(15) Uani 1 1 d . . . C38 C 0.2293(6) 0.4029(3) 0.7547(4) 0.0184(15) Uani 1 1 d . . . C39 C 0.1362(6) 0.4203(3) 0.7596(5) 0.0222(16) Uani 1 1 d . . . H39 H 0.0858 0.3928 0.7619 0.027 Uiso 1 1 calc R . . C40 C 0.1253(6) 0.4838(3) 0.7609(5) 0.0241(17) Uani 1 1 d . . . H40 H 0.0680 0.5029 0.7667 0.029 Uiso 1 1 calc R . . C41 C 0.2060(6) 0.5154(3) 0.7528(5) 0.0190(15) Uani 1 1 d . . . C42 C 0.2153(5) 0.5816(3) 0.7495(4) 0.0168(15) Uani 1 1 d . . . C43 C 0.1650(6) 0.6200(3) 0.7879(5) 0.0216(16) Uani 1 1 d . . . H43 H 0.1280 0.6032 0.8194 0.026 Uiso 1 1 calc R . . C44 C 0.1687(6) 0.6827(3) 0.7802(5) 0.0189(15) Uani 1 1 d . . . H44 H 0.1303 0.7066 0.8038 0.023 Uiso 1 1 calc R . . C45 C 0.2748(5) 0.6751(3) 0.7027(6) 0.0251(17) Uani 1 1 d . . . H45 H 0.3120 0.6936 0.6727 0.030 Uiso 1 1 calc R . . C46 C 0.2725(6) 0.6110(3) 0.7074(6) 0.0245(18) Uani 1 1 d . . . H46 H 0.3099 0.5877 0.6820 0.029 Uiso 1 1 calc R . . N1 N 0.2479(4) 0.0334(3) 0.7502(4) 0.0149(12) Uani 1 1 d . . . N2 N 0.2232(4) 0.7106(3) 0.7415(4) 0.0148(12) Uani 1 1 d . . . O1 O 0.2978(4) -0.0860(2) 0.6564(4) 0.0250(12) Uani 1 1 d . . . O2 O 0.2667(4) -0.1867(2) 0.6260(4) 0.0229(11) Uani 1 1 d . . . O3 O 1.0814(4) -0.0646(2) 0.6370(4) 0.0248(12) Uani 1 1 d . . . O4 O 1.0758(4) -0.1663(2) 0.6555(3) 0.0169(10) Uani 1 1 d . . . O5 O 0.5191(4) -0.0608(2) 0.3382(3) 0.0214(11) Uani 1 1 d . . . O6 O 0.5315(4) -0.1742(2) 0.3285(4) 0.0235(11) Uani 1 1 d . . . O7 O 0.1635(4) -0.0820(2) 0.8310(4) 0.0273(13) Uani 1 1 d . . . O8 O 0.1936(4) -0.1834(2) 0.8511(4) 0.0214(11) Uani 1 1 d . . . O9 O -0.6197(4) -0.0763(2) 0.8507(4) 0.0264(12) Uani 1 1 d . . . O10 O -0.6138(4) -0.1764(2) 0.8180(3) 0.0201(11) Uani 1 1 d . . . O11 O -0.0636(4) -0.0743(2) 1.1503(3) 0.0184(11) Uani 1 1 d . . . O12 O -0.0756(4) -0.1891(2) 1.1471(3) 0.0202(11) Uani 1 1 d . . . S1 S 0.18635(15) 0.27835(8) 0.73819(14) 0.0232(4) Uani 1 1 d . . . S2 S 0.29957(15) 0.46588(8) 0.74498(14) 0.0229(4) Uani 1 1 d . . . S3 S 0.55199(13) -0.11917(7) 0.38416(12) 0.0146(4) Uani 1 1 d . . . S4 S -0.09152(13) -0.13139(7) 1.09814(12) 0.0147(4) Uani 1 1 d . . . Zn1 Zn 0.23145(6) -0.05883(3) 0.74344(5) 0.0133(2) Uani 1 1 d . . . Zn2 Zn 0.22870(6) -0.19645(3) 0.73725(5) 0.0134(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.011(4) 0.020(4) 0.021(4) 0.000(3) 0.006(3) 0.005(3) C2 0.010(3) 0.021(4) 0.017(4) 0.000(3) 0.005(3) 0.004(3) C3 0.016(4) 0.018(4) 0.018(4) -0.001(3) 0.010(3) -0.005(3) C4 0.011(4) 0.018(4) 0.027(4) 0.000(3) 0.007(3) -0.003(3) C5 0.009(3) 0.017(3) 0.025(4) 0.006(3) 0.008(3) 0.003(3) C6 0.018(4) 0.013(3) 0.032(4) -0.003(3) 0.010(3) -0.003(3) C7 0.023(4) 0.015(4) 0.027(4) 0.003(3) 0.014(3) 0.003(3) C8 0.007(3) 0.019(4) 0.026(4) 0.005(3) 0.005(3) 0.003(3) C9 0.017(4) 0.014(3) 0.015(4) 0.006(3) 0.005(3) 0.002(3) C10 0.019(4) 0.014(4) 0.026(4) 0.008(3) 0.006(3) 0.003(3) C11 0.011(4) 0.016(3) 0.015(4) 0.001(3) 0.001(3) 0.002(3) C12 0.011(4) 0.016(4) 0.030(4) -0.001(3) 0.007(3) -0.006(3) C13 0.016(4) 0.016(3) 0.018(4) 0.003(3) 0.006(3) 0.003(3) C14 0.011(4) 0.018(4) 0.030(4) 0.007(3) 0.009(3) 0.002(3) C15 0.012(4) 0.022(4) 0.009(3) -0.001(3) 0.001(3) 0.002(3) C16 0.014(4) 0.010(3) 0.026(4) 0.000(3) 0.010(3) 0.002(3) C17 0.014(4) 0.018(4) 0.016(4) -0.002(3) 0.002(3) 0.003(3) C18 0.014(4) 0.019(4) 0.022(4) 0.008(3) 0.005(3) 0.002(3) C19 0.009(3) 0.017(3) 0.014(3) 0.000(3) 0.004(3) 0.000(3) C20 0.034(5) 0.012(4) 0.044(5) -0.005(3) 0.029(4) 0.003(3) C21 0.027(4) 0.014(4) 0.036(5) 0.001(3) 0.022(4) 0.001(3) C22 0.018(4) 0.016(3) 0.016(4) 0.008(3) 0.010(3) 0.003(3) C23 0.019(4) 0.014(3) 0.026(4) 0.006(3) 0.011(3) 0.002(3) C24 0.016(4) 0.020(4) 0.017(4) 0.000(3) 0.007(3) 0.000(3) C25 0.014(4) 0.022(4) 0.005(3) 0.003(3) 0.002(3) 0.003(3) C26 0.012(4) 0.016(4) 0.042(5) 0.001(3) 0.010(3) 0.006(3) C27 0.015(4) 0.019(4) 0.012(3) -0.005(3) 0.000(3) -0.003(3) C28 0.020(4) 0.011(4) 0.044(5) 0.003(3) 0.020(4) 0.000(3) C29 0.019(4) 0.017(4) 0.015(4) 0.002(3) 0.006(3) 0.002(3) C30 0.023(4) 0.023(4) 0.009(3) 0.001(3) 0.006(3) -0.004(3) C31 0.029(4) 0.014(4) 0.031(4) -0.005(3) 0.024(4) -0.002(3) C32 0.022(4) 0.018(4) 0.028(4) -0.002(3) 0.014(3) 0.001(3) C33 0.018(4) 0.020(4) 0.014(3) -0.001(3) 0.006(3) 0.002(3) C34 0.023(4) 0.017(4) 0.020(4) -0.003(3) 0.015(3) -0.002(3) C35 0.016(4) 0.019(4) 0.033(5) -0.001(3) 0.007(3) 0.003(3) C36 0.021(4) 0.022(4) 0.022(4) -0.006(3) 0.002(3) -0.002(3) C37 0.024(4) 0.011(3) 0.019(4) -0.002(3) 0.010(3) -0.005(3) C38 0.022(4) 0.020(4) 0.005(3) 0.000(3) -0.002(3) -0.002(3) C39 0.023(4) 0.023(4) 0.020(4) -0.003(3) 0.008(3) -0.004(3) C40 0.027(4) 0.018(4) 0.030(4) 0.005(3) 0.015(3) 0.007(3) C41 0.024(4) 0.015(4) 0.015(4) 0.003(3) 0.005(3) 0.003(3) C42 0.021(4) 0.012(3) 0.010(3) 0.001(3) 0.000(3) 0.002(3) C43 0.018(4) 0.016(4) 0.028(4) -0.001(3) 0.007(3) -0.007(3) C44 0.021(4) 0.015(4) 0.024(4) 0.004(3) 0.013(3) 0.005(3) C45 0.009(4) 0.014(4) 0.045(5) 0.001(3) 0.004(3) -0.001(3) C46 0.011(4) 0.012(3) 0.045(5) -0.001(3) 0.007(3) 0.006(3) N1 0.016(3) 0.017(3) 0.014(3) -0.001(2) 0.008(2) 0.003(2) N2 0.011(3) 0.014(3) 0.018(3) -0.004(2) 0.004(2) 0.001(2) O1 0.021(3) 0.019(3) 0.040(3) -0.002(2) 0.018(2) 0.002(2) O2 0.021(3) 0.023(3) 0.030(3) -0.001(2) 0.016(2) -0.005(2) O3 0.010(3) 0.014(3) 0.042(3) 0.001(2) 0.004(2) -0.0025(19) O4 0.015(3) 0.016(3) 0.014(2) 0.004(2) 0.002(2) 0.0024(19) O5 0.011(3) 0.017(2) 0.032(3) 0.004(2) 0.005(2) -0.0009(19) O6 0.016(3) 0.020(3) 0.034(3) -0.006(2) 0.010(2) -0.007(2) O7 0.019(3) 0.012(3) 0.058(4) 0.000(2) 0.024(3) 0.002(2) O8 0.019(3) 0.015(2) 0.032(3) 0.004(2) 0.013(2) 0.005(2) O9 0.015(3) 0.015(3) 0.045(3) -0.002(2) 0.009(2) 0.003(2) O10 0.016(3) 0.015(3) 0.023(3) 0.004(2) 0.003(2) 0.0019(19) O11 0.015(3) 0.022(3) 0.019(3) -0.008(2) 0.009(2) -0.001(2) O12 0.017(3) 0.020(3) 0.024(3) 0.000(2) 0.008(2) 0.0014(19) S1 0.0220(10) 0.0137(9) 0.0344(11) 0.0011(8) 0.0126(8) 0.0002(7) S2 0.0228(10) 0.0126(9) 0.0328(11) -0.0001(8) 0.0118(8) 0.0000(7) S3 0.0114(9) 0.0180(9) 0.0135(9) -0.0006(7) 0.0047(7) -0.0004(6) S4 0.0112(9) 0.0166(9) 0.0149(9) -0.0012(7) 0.0042(7) -0.0002(6) Zn1 0.0107(4) 0.0092(4) 0.0192(4) 0.0013(3) 0.0058(3) 0.0013(3) Zn2 0.0109(4) 0.0091(4) 0.0191(5) 0.0007(3) 0.0056(3) 0.0009(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 C1 O2 1.263(8) . ? C1 O1 1.263(8) . ? C1 C2 1.520(9) . ? C2 C7 1.385(9) . ? C2 C3 1.403(9) . ? C3 C4 1.395(9) . ? C3 H3 0.9300 . ? C4 C5 1.397(9) . ? C4 H4 0.9300 . ? C5 C6 1.396(9) . ? C5 S3 1.765(7) . ? C6 C7 1.387(9) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C13 1.395(9) . ? C8 C9 1.405(9) . ? C8 S3 1.757(7) . ? C9 C10 1.370(10) . ? C9 H9 0.9300 . ? C10 C11 1.419(9) . ? C10 H10 0.9300 . ? C11 C12 1.393(9) . ? C11 C14 1.528(9) . ? C12 C13 1.397(9) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O3 1.249(8) . ? C14 O4 1.253(8) . ? C15 O7 1.261(8) . ? C15 O8 1.275(8) . ? C15 C16 1.483(9) . ? C16 C17 1.393(9) . ? C16 C21 1.406(9) . ? C17 C18 1.397(9) . ? C17 H17 0.9300 . ? C18 C19 1.374(9) . ? C18 H18 0.9300 . ? C19 C20 1.398(9) . ? C19 S4 1.770(6) . ? C20 C21 1.362(9) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C27 1.373(9) . ? C22 C23 1.396(9) . ? C22 S4 1.775(7) . ? C23 C24 1.363(10) . ? C23 H23 0.9300 . ? C24 C25 1.402(9) . ? C24 H24 0.9300 . ? C25 C26 1.363(10) . ? C25 C28 1.512(10) . ? C26 C27 1.388(10) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 O9 1.268(8) . ? C28 O10 1.272(8) . ? C29 N1 1.337(9) . ? C29 C30 1.374(9) . ? C29 H29 0.9300 . ? C30 C31 1.391(10) . ? C30 H30 0.9300 . ? C31 C32 1.408(10) . ? C31 C34 1.474(10) . ? C32 C33 1.392(10) . ? C32 H32 0.9300 . ? C33 N1 1.339(9) . ? C33 H33 0.9300 . ? C34 C35 1.364(10) . ? C34 S1 1.731(7) . ? C35 C36 1.408(10) . ? C35 H35 0.9300 . ? C36 C37 1.337(10) . ? C36 H36 0.9300 . ? C37 C38 1.467(10) . ? C37 S1 1.733(7) . ? C38 C39 1.368(10) . ? C38 S2 1.727(7) . ? C39 C40 1.397(10) . ? C39 H39 0.9300 . ? C40 C41 1.358(10) . ? C40 H40 0.9300 . ? C41 C42 1.455(10) . ? C41 S2 1.725(7) . ? C42 C43 1.386(10) . ? C42 C46 1.391(10) . ? C43 C44 1.378(9) . ? C43 H43 0.9300 . ? C44 N2 1.306(8) . ? C44 H44 0.9300 . ? C45 N2 1.366(9) . ? C45 C46 1.403(9) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? N1 Zn1 2.024(6) . ? N2 Zn2 2.034(6) 1_565 ? O1 Zn1 2.048(5) . ? O2 Zn2 2.062(5) . ? O3 Zn1 2.030(5) 1_655 ? O4 Zn2 2.046(4) 1_655 ? O5 S3 1.441(5) . ? O6 S3 1.447(5) . ? O7 Zn1 2.047(5) . ? O8 Zn2 2.086(5) . ? O9 Zn1 2.056(5) 1_455 ? O10 Zn2 2.031(5) 1_455 ? O11 S4 1.455(5) . ? O12 S4 1.448(5) . ? Zn1 O3 2.030(5) 1_455 ? Zn1 O9 2.056(5) 1_655 ? Zn2 O10 2.031(5) 1_655 ? Zn2 N2 2.034(6) 1_545 ? Zn2 O4 2.045(4) 1_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 126.0(6) . . ? O2 C1 C2 117.4(6) . . ? O1 C1 C2 116.6(6) . . ? C7 C2 C3 120.2(6) . . ? C7 C2 C1 118.9(6) . . ? C3 C2 C1 120.8(6) . . ? C4 C3 C2 119.9(6) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 118.6(6) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C6 C5 C4 121.9(6) . . ? C6 C5 S3 118.2(5) . . ? C4 C5 S3 119.7(5) . . ? C7 C6 C5 118.5(6) . . ? C7 C6 H6 120.8 . . ? C5 C6 H6 120.8 . . ? C2 C7 C6 120.8(6) . . ? C2 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C13 C8 C9 121.6(6) . . ? C13 C8 S3 120.6(5) . . ? C9 C8 S3 117.6(5) . . ? C10 C9 C8 119.1(6) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C9 C10 C11 120.9(6) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 118.7(6) . . ? C12 C11 C14 121.8(6) . . ? C10 C11 C14 119.1(6) . . ? C11 C12 C13 121.4(6) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C8 C13 C12 118.2(6) . . ? C8 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? O3 C14 O4 127.5(7) . . ? O3 C14 C11 116.3(6) . . ? O4 C14 C11 116.1(6) . . ? O7 C15 O8 124.9(6) . . ? O7 C15 C16 117.7(6) . . ? O8 C15 C16 117.3(6) . . ? C17 C16 C21 119.1(6) . . ? C17 C16 C15 122.3(6) . . ? C21 C16 C15 118.6(6) . . ? C16 C17 C18 120.2(6) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C19 C18 C17 119.3(6) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 120.9(6) . . ? C18 C19 S4 121.4(5) . . ? C20 C19 S4 117.7(5) . . ? C21 C20 C19 119.8(6) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C16 120.5(6) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? C27 C22 C23 122.1(6) . . ? C27 C22 S4 120.0(5) . . ? C23 C22 S4 117.9(5) . . ? C24 C23 C22 118.5(6) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C23 C24 C25 120.3(7) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 119.4(6) . . ? C26 C25 C28 121.3(6) . . ? C24 C25 C28 119.3(6) . . ? C25 C26 C27 121.6(6) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C22 C27 C26 117.6(6) . . ? C22 C27 H27 121.2 . . ? C26 C27 H27 121.2 . . ? O9 C28 O10 125.4(7) . . ? O9 C28 C25 116.7(6) . . ? O10 C28 C25 117.9(6) . . ? N1 C29 C30 124.5(7) . . ? N1 C29 H29 117.7 . . ? C30 C29 H29 117.7 . . ? C29 C30 C31 118.9(7) . . ? C29 C30 H30 120.6 . . ? C31 C30 H30 120.6 . . ? C30 C31 C32 117.6(6) . . ? C30 C31 C34 120.8(7) . . ? C32 C31 C34 121.6(7) . . ? C33 C32 C31 118.9(7) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? N1 C33 C32 123.1(7) . . ? N1 C33 H33 118.4 . . ? C32 C33 H33 118.4 . . ? C35 C34 C31 127.4(6) . . ? C35 C34 S1 110.8(5) . . ? C31 C34 S1 121.8(5) . . ? C34 C35 C36 112.5(7) . . ? C34 C35 H35 123.8 . . ? C36 C35 H35 123.8 . . ? C37 C36 C35 114.3(7) . . ? C37 C36 H36 122.8 . . ? C35 C36 H36 122.8 . . ? C36 C37 C38 129.1(6) . . ? C36 C37 S1 110.9(5) . . ? C38 C37 S1 119.7(5) . . ? C39 C38 C37 128.4(7) . . ? C39 C38 S2 110.9(6) . . ? C37 C38 S2 120.7(5) . . ? C38 C39 C40 112.7(7) . . ? C38 C39 H39 123.7 . . ? C40 C39 H39 123.7 . . ? C41 C40 C39 113.9(7) . . ? C41 C40 H40 123.1 . . ? C39 C40 H40 123.1 . . ? C40 C41 C42 126.5(7) . . ? C40 C41 S2 110.8(5) . . ? C42 C41 S2 122.7(5) . . ? C43 C42 C46 115.3(6) . . ? C43 C42 C41 121.2(6) . . ? C46 C42 C41 123.5(6) . . ? C44 C43 C42 121.1(7) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? N2 C44 C43 123.8(7) . . ? N2 C44 H44 118.1 . . ? C43 C44 H44 118.1 . . ? N2 C45 C46 120.9(7) . . ? N2 C45 H45 119.5 . . ? C46 C45 H45 119.5 . . ? C42 C46 C45 121.1(7) . . ? C42 C46 H46 119.5 . . ? C45 C46 H46 119.5 . . ? C29 N1 C33 117.0(6) . . ? C29 N1 Zn1 120.9(5) . . ? C33 N1 Zn1 122.1(5) . . ? C44 N2 C45 117.7(6) . . ? C44 N2 Zn2 121.1(4) . 1_565 ? C45 N2 Zn2 121.2(5) . 1_565 ? C1 O1 Zn1 136.3(5) . . ? C1 O2 Zn2 116.5(4) . . ? C14 O3 Zn1 117.5(5) . 1_655 ? C14 O4 Zn2 134.7(4) . 1_655 ? C15 O7 Zn1 131.0(4) . . ? C15 O8 Zn2 122.5(4) . . ? C28 O9 Zn1 122.6(5) . 1_455 ? C28 O10 Zn2 129.9(4) . 1_455 ? C34 S1 C37 91.5(3) . . ? C41 S2 C38 91.7(3) . . ? O5 S3 O6 119.2(3) . . ? O5 S3 C8 107.3(3) . . ? O6 S3 C8 108.5(3) . . ? O5 S3 C5 107.2(3) . . ? O6 S3 C5 107.5(3) . . ? C8 S3 C5 106.4(3) . . ? O12 S4 O11 119.9(3) . . ? O12 S4 C19 107.4(3) . . ? O11 S4 C19 107.7(3) . . ? O12 S4 C22 107.2(3) . . ? O11 S4 C22 106.4(3) . . ? C19 S4 C22 107.7(3) . . ? N1 Zn1 O3 99.0(2) . 1_455 ? N1 Zn1 O7 106.5(2) . . ? O3 Zn1 O7 87.4(2) 1_455 . ? N1 Zn1 O1 104.6(2) . . ? O3 Zn1 O1 90.4(2) 1_455 . ? O7 Zn1 O1 148.8(2) . . ? N1 Zn1 O9 95.2(2) . 1_655 ? O3 Zn1 O9 165.7(2) 1_455 1_655 ? O7 Zn1 O9 88.4(2) . 1_655 ? O1 Zn1 O9 86.2(2) . 1_655 ? O10 Zn2 N2 103.8(2) 1_655 1_545 ? O10 Zn2 O4 148.72(19) 1_655 1_455 ? N2 Zn2 O4 107.5(2) 1_545 1_455 ? O10 Zn2 O2 85.71(19) 1_655 . ? N2 Zn2 O2 99.1(2) 1_545 . ? O4 Zn2 O2 89.57(19) 1_455 . ? O10 Zn2 O8 90.24(19) 1_655 . ? N2 Zn2 O8 94.68(19) 1_545 . ? O4 Zn2 O8 87.04(18) 1_455 . ? O2 Zn2 O8 166.15(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 -166.1(6) . . . . ? O1 C1 C2 C7 11.8(9) . . . . ? O2 C1 C2 C3 9.9(10) . . . . ? O1 C1 C2 C3 -172.2(6) . . . . ? C7 C2 C3 C4 -3.0(10) . . . . ? C1 C2 C3 C4 -179.0(6) . . . . ? C2 C3 C4 C5 1.7(10) . . . . ? C3 C4 C5 C6 1.8(10) . . . . ? C3 C4 C5 S3 -173.0(5) . . . . ? C4 C5 C6 C7 -3.9(10) . . . . ? S3 C5 C6 C7 171.0(5) . . . . ? C3 C2 C7 C6 0.9(11) . . . . ? C1 C2 C7 C6 176.9(6) . . . . ? C5 C6 C7 C2 2.6(11) . . . . ? C13 C8 C9 C10 -2.9(11) . . . . ? S3 C8 C9 C10 172.3(5) . . . . ? C8 C9 C10 C11 3.2(10) . . . . ? C9 C10 C11 C12 0.1(11) . . . . ? C9 C10 C11 C14 173.1(6) . . . . ? C10 C11 C12 C13 -3.9(10) . . . . ? C14 C11 C12 C13 -176.7(6) . . . . ? C9 C8 C13 C12 -0.8(10) . . . . ? S3 C8 C13 C12 -175.8(5) . . . . ? C11 C12 C13 C8 4.3(10) . . . . ? C12 C11 C14 O3 7.1(10) . . . . ? C10 C11 C14 O3 -165.7(7) . . . . ? C12 C11 C14 O4 -173.4(6) . . . . ? C10 C11 C14 O4 13.8(10) . . . . ? O7 C15 C16 C17 177.4(6) . . . . ? O8 C15 C16 C17 0.9(10) . . . . ? O7 C15 C16 C21 -1.5(10) . . . . ? O8 C15 C16 C21 -178.0(6) . . . . ? C21 C16 C17 C18 1.8(10) . . . . ? C15 C16 C17 C18 -177.1(6) . . . . ? C16 C17 C18 C19 -0.1(10) . . . . ? C17 C18 C19 C20 0.5(10) . . . . ? C17 C18 C19 S4 -178.4(5) . . . . ? C18 C19 C20 C21 -2.7(11) . . . . ? S4 C19 C20 C21 176.2(6) . . . . ? C19 C20 C21 C16 4.5(12) . . . . ? C17 C16 C21 C20 -4.0(11) . . . . ? C15 C16 C21 C20 174.9(7) . . . . ? C27 C22 C23 C24 -7.7(10) . . . . ? S4 C22 C23 C24 169.1(5) . . . . ? C22 C23 C24 C25 6.6(10) . . . . ? C23 C24 C25 C26 -1.7(10) . . . . ? C23 C24 C25 C28 176.8(6) . . . . ? C24 C25 C26 C27 -2.6(11) . . . . ? C28 C25 C26 C27 179.0(7) . . . . ? C23 C22 C27 C26 3.5(10) . . . . ? S4 C22 C27 C26 -173.2(5) . . . . ? C25 C26 C27 C22 1.7(11) . . . . ? C26 C25 C28 O9 5.8(10) . . . . ? C24 C25 C28 O9 -172.6(7) . . . . ? C26 C25 C28 O10 -177.6(7) . . . . ? C24 C25 C28 O10 4.0(10) . . . . ? N1 C29 C30 C31 -3.1(11) . . . . ? C29 C30 C31 C32 0.7(10) . . . . ? C29 C30 C31 C34 -177.7(6) . . . . ? C30 C31 C32 C33 1.2(10) . . . . ? C34 C31 C32 C33 179.6(6) . . . . ? C31 C32 C33 N1 -1.0(11) . . . . ? C30 C31 C34 C35 15.6(11) . . . . ? C32 C31 C34 C35 -162.7(7) . . . . ? C30 C31 C34 S1 -164.5(5) . . . . ? C32 C31 C34 S1 17.2(10) . . . . ? C31 C34 C35 C36 -179.7(7) . . . . ? S1 C34 C35 C36 0.4(8) . . . . ? C34 C35 C36 C37 -1.1(10) . . . . ? C35 C36 C37 C38 174.4(7) . . . . ? C35 C36 C37 S1 1.3(8) . . . . ? C36 C37 C38 C39 -156.7(8) . . . . ? S1 C37 C38 C39 16.0(10) . . . . ? C36 C37 C38 S2 23.1(10) . . . . ? S1 C37 C38 S2 -164.2(4) . . . . ? C37 C38 C39 C40 176.4(7) . . . . ? S2 C38 C39 C40 -3.4(8) . . . . ? C38 C39 C40 C41 2.8(10) . . . . ? C39 C40 C41 C42 178.4(7) . . . . ? C39 C40 C41 S2 -0.8(9) . . . . ? C40 C41 C42 C43 24.2(11) . . . . ? S2 C41 C42 C43 -156.6(6) . . . . ? C40 C41 C42 C46 -154.8(8) . . . . ? S2 C41 C42 C46 24.4(10) . . . . ? C46 C42 C43 C44 2.8(10) . . . . ? C41 C42 C43 C44 -176.3(7) . . . . ? C42 C43 C44 N2 -3.7(12) . . . . ? C43 C42 C46 C45 -1.9(10) . . . . ? C41 C42 C46 C45 177.1(7) . . . . ? N2 C45 C46 C42 1.8(11) . . . . ? C30 C29 N1 C33 3.3(10) . . . . ? C30 C29 N1 Zn1 -179.6(5) . . . . ? C32 C33 N1 C29 -1.2(10) . . . . ? C32 C33 N1 Zn1 -178.2(5) . . . . ? C43 C44 N2 C45 3.3(10) . . . . ? C43 C44 N2 Zn2 -177.8(6) . . . 1_565 ? C46 C45 N2 C44 -2.3(10) . . . . ? C46 C45 N2 Zn2 178.7(5) . . . 1_565 ? O2 C1 O1 Zn1 -0.4(12) . . . . ? C2 C1 O1 Zn1 -178.1(5) . . . . ? O1 C1 O2 Zn2 -17.9(9) . . . . ? C2 C1 O2 Zn2 159.8(4) . . . . ? O4 C14 O3 Zn1 -13.6(10) . . . 1_655 ? C11 C14 O3 Zn1 165.8(4) . . . 1_655 ? O3 C14 O4 Zn2 -3.8(12) . . . 1_655 ? C11 C14 O4 Zn2 176.7(4) . . . 1_655 ? O8 C15 O7 Zn1 -2.2(11) . . . . ? C16 C15 O7 Zn1 -178.5(5) . . . . ? O7 C15 O8 Zn2 -17.7(9) . . . . ? C16 C15 O8 Zn2 158.5(4) . . . . ? O10 C28 O9 Zn1 -18.2(10) . . . 1_455 ? C25 C28 O9 Zn1 158.2(5) . . . 1_455 ? O9 C28 O10 Zn2 -4.8(11) . . . 1_455 ? C25 C28 O10 Zn2 178.8(4) . . . 1_455 ? C35 C34 S1 C37 0.2(6) . . . . ? C31 C34 S1 C37 -179.7(6) . . . . ? C36 C37 S1 C34 -0.8(6) . . . . ? C38 C37 S1 C34 -174.7(6) . . . . ? C40 C41 S2 C38 -0.9(6) . . . . ? C42 C41 S2 C38 179.8(6) . . . . ? C39 C38 S2 C41 2.5(5) . . . . ? C37 C38 S2 C41 -177.4(6) . . . . ? C13 C8 S3 O5 -4.2(7) . . . . ? C9 C8 S3 O5 -179.4(5) . . . . ? C13 C8 S3 O6 125.8(6) . . . . ? C9 C8 S3 O6 -49.4(6) . . . . ? C13 C8 S3 C5 -118.8(6) . . . . ? C9 C8 S3 C5 66.0(6) . . . . ? C6 C5 S3 O5 -47.8(6) . . . . ? C4 C5 S3 O5 127.3(6) . . . . ? C6 C5 S3 O6 -177.1(5) . . . . ? C4 C5 S3 O6 -2.1(7) . . . . ? C6 C5 S3 C8 66.8(6) . . . . ? C4 C5 S3 C8 -118.1(6) . . . . ? C18 C19 S4 O12 10.7(7) . . . . ? C20 C19 S4 O12 -168.2(6) . . . . ? C18 C19 S4 O11 141.1(6) . . . . ? C20 C19 S4 O11 -37.8(6) . . . . ? C18 C19 S4 C22 -104.5(6) . . . . ? C20 C19 S4 C22 76.6(6) . . . . ? C27 C22 S4 O12 130.6(6) . . . . ? C23 C22 S4 O12 -46.3(6) . . . . ? C27 C22 S4 O11 1.2(6) . . . . ? C23 C22 S4 O11 -175.7(5) . . . . ? C27 C22 S4 C19 -114.0(6) . . . . ? C23 C22 S4 C19 69.1(6) . . . . ? C29 N1 Zn1 O3 -159.9(5) . . . 1_455 ? C33 N1 Zn1 O3 17.0(5) . . . 1_455 ? C29 N1 Zn1 O7 110.2(5) . . . . ? C33 N1 Zn1 O7 -72.9(5) . . . . ? C29 N1 Zn1 O1 -67.1(5) . . . . ? C33 N1 Zn1 O1 109.8(5) . . . . ? C29 N1 Zn1 O9 20.3(5) . . . 1_655 ? C33 N1 Zn1 O9 -162.8(5) . . . 1_655 ? C15 O7 Zn1 N1 -162.9(6) . . . . ? C15 O7 Zn1 O3 98.5(6) . . . 1_455 ? C15 O7 Zn1 O1 12.1(8) . . . . ? C15 O7 Zn1 O9 -67.9(6) . . . 1_655 ? C1 O1 Zn1 N1 -172.4(7) . . . . ? C1 O1 Zn1 O3 -73.0(7) . . . 1_455 ? C1 O1 Zn1 O7 12.5(9) . . . . ? C1 O1 Zn1 O9 93.1(7) . . . 1_655 ? C1 O2 Zn2 O10 -58.5(5) . . . 1_655 ? C1 O2 Zn2 N2 -161.8(5) . . . 1_545 ? C1 O2 Zn2 O4 90.5(5) . . . 1_455 ? C1 O2 Zn2 O8 14.8(11) . . . . ? C15 O8 Zn2 O10 95.7(5) . . . 1_655 ? C15 O8 Zn2 N2 -160.5(5) . . . 1_545 ? C15 O8 Zn2 O4 -53.2(5) . . . 1_455 ? C15 O8 Zn2 O2 22.8(11) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.273 _refine_diff_density_min -1.404 _refine_diff_density_rms 0.208 # === END data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H28 N2 O10 S2 Zn2' _chemical_formula_sum 'C46 H28 N2 O10 S2 Zn2' _chemical_formula_weight 963.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.3794(12) _cell_length_b 23.893(2) _cell_length_c 15.9117(11) _cell_angle_alpha 90.00 _cell_angle_beta 117.102(6) _cell_angle_gamma 90.00 _cell_volume 4866.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3709 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 24.61 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 1.126 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7288 _exptl_absorpt_correction_T_max 0.8231 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25436 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8541 _reflns_number_gt 5880 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.1000P] 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 8541 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1747 _refine_ls_wR_factor_gt 0.1647 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.89285(4) 0.83877(2) -0.00521(4) 0.02395(17) Uani 1 1 d . . . Zn2 Zn 0.76404(5) 0.83570(2) -0.24912(4) 0.02939(18) Uani 1 1 d . . . S1 S 1.15675(11) 0.78295(6) 0.50786(10) 0.0403(3) Uani 1 1 d . . . S2 S 1.42208(11) 0.78969(7) 0.78315(10) 0.0451(4) Uani 1 1 d . . . O1 O 0.7547(2) 0.87135(14) -0.0387(2) 0.0302(8) Uani 1 1 d . . . O2 O 0.6785(3) 0.87370(15) -0.1971(2) 0.0334(8) Uani 1 1 d . . . O3 O 0.3257(3) 0.98751(15) -0.1246(2) 0.0350(8) Uani 1 1 d . . . O4 O 0.0006(3) 0.83748(17) -0.0560(3) 0.0455(10) Uani 1 1 d . . . O5 O -0.0333(3) 0.92044(18) -0.0180(3) 0.0475(10) Uani 1 1 d . . . O6 O 0.8932(3) 0.82558(14) -0.2994(3) 0.0387(9) Uani 1 1 d . . . O7 O 0.8391(3) 0.90289(14) -0.2610(2) 0.0371(9) Uani 1 1 d . . . O8 O 1.1822(3) 1.00139(14) -0.3690(2) 0.0317(8) Uani 1 1 d . . . O9 O 1.1503(3) 1.25872(13) -0.4678(2) 0.0288(7) Uani 1 1 d . . . O10 O 1.1976(3) 1.26297(14) -0.3123(2) 0.0330(8) Uani 1 1 d . . . N1 N 0.9710(3) 0.83827(16) 0.1393(3) 0.0258(9) Uani 1 1 d . . . N2 N 1.6485(3) 0.6902(2) 1.1227(3) 0.0354(10) Uani 1 1 d . . . C1 C 0.6802(4) 0.8833(2) -0.1195(3) 0.0279(10) Uani 1 1 d U . . C2 C 0.5872(4) 0.9106(2) -0.1194(3) 0.0262(10) Uani 1 1 d U . . C3 C 0.5680(4) 0.9057(2) -0.0417(3) 0.0285(10) Uani 1 1 d U . . H3 H 0.6144 0.8858 0.0111 0.034 Uiso 1 1 calc R . . C4 C 0.4800(4) 0.9303(2) -0.0421(3) 0.0304(10) Uani 1 1 d U . . H4 H 0.4673 0.9273 0.0101 0.037 Uiso 1 1 calc R . . C5 C 0.4115(4) 0.9593(2) -0.1218(3) 0.0278(10) Uani 1 1 d U . . C6 C 0.4304(4) 0.9650(2) -0.2007(3) 0.0302(10) Uani 1 1 d U . . H6 H 0.3845 0.9848 -0.2538 0.036 Uiso 1 1 calc R . . C7 C 0.5182(4) 0.9405(2) -0.1971(3) 0.0279(10) Uani 1 1 d U . . H7 H 0.5319 0.9442 -0.2485 0.033 Uiso 1 1 calc R . . C8 C 0.2578(4) 0.9605(2) -0.0993(3) 0.0304(10) Uani 1 1 d U . . C9 C 0.1998(4) 0.9948(2) -0.0703(3) 0.0344(11) Uani 1 1 d U . . H9 H 0.2131 1.0330 -0.0624 0.041 Uiso 1 1 calc R . . C10 C 0.1221(4) 0.9714(2) -0.0534(3) 0.0316(10) Uani 1 1 d U . . H10 H 0.0820 0.9943 -0.0352 0.038 Uiso 1 1 calc R . . C11 C 0.1029(4) 0.9142(2) -0.0631(3) 0.0305(10) Uani 1 1 d U . . C12 C 0.1635(4) 0.8807(2) -0.0911(4) 0.0371(11) Uani 1 1 d U . . H12 H 0.1522 0.8422 -0.0968 0.044 Uiso 1 1 calc R . . C13 C 0.2386(4) 0.9033(2) -0.1103(4) 0.0335(10) Uani 1 1 d U . . H13 H 0.2768 0.8806 -0.1307 0.040 Uiso 1 1 calc R . . C14 C 0.0192(4) 0.8894(2) -0.0442(4) 0.0352(11) Uani 1 1 d U . . C15 C 0.8988(4) 0.8774(2) -0.2882(3) 0.0299(10) Uani 1 1 d U . . C16 C 0.9735(4) 0.9114(2) -0.3083(3) 0.0298(10) Uani 1 1 d U . . C17 C 0.9693(4) 0.9693(2) -0.3083(3) 0.0311(10) Uani 1 1 d U . . H17 H 0.9209 0.9871 -0.2938 0.037 Uiso 1 1 calc R . . C18 C 1.0371(4) 1.0013(2) -0.3299(4) 0.0334(10) Uani 1 1 d U . . H18 H 1.0329 1.0401 -0.3313 0.040 Uiso 1 1 calc R . . C19 C 1.1096(4) 0.9746(2) -0.3490(3) 0.0294(10) Uani 1 1 d U . . C20 C 1.1131(4) 0.9163(2) -0.3514(4) 0.0362(11) Uani 1 1 d U . . H20 H 1.1605 0.8984 -0.3671 0.043 Uiso 1 1 calc R . . C21 C 1.0459(4) 0.8858(2) -0.3305(4) 0.0349(11) Uani 1 1 d U . . H21 H 1.0490 0.8469 -0.3311 0.042 Uiso 1 1 calc R . . C22 C 1.1820(4) 1.0599(2) -0.3710(3) 0.0309(10) Uani 1 1 d U . . C23 C 1.2066(4) 1.0906(2) -0.2896(4) 0.0356(11) Uani 1 1 d U . . H23 H 1.2238 1.0726 -0.2326 0.043 Uiso 1 1 calc R . . C24 C 1.2050(4) 1.1479(2) -0.2947(4) 0.0323(11) Uani 1 1 d U . . H24 H 1.2209 1.1691 -0.2408 0.039 Uiso 1 1 calc R . . C25 C 1.1796(4) 1.1747(2) -0.3809(3) 0.0282(10) Uani 1 1 d U . . C26 C 1.1584(4) 1.1428(2) -0.4593(4) 0.0365(11) Uani 1 1 d U . . H26 H 1.1438 1.1604 -0.5161 0.044 Uiso 1 1 calc R . . C27 C 1.1584(4) 1.0846(2) -0.4554(4) 0.0377(11) Uani 1 1 d U . . H27 H 1.1426 1.0632 -0.5091 0.045 Uiso 1 1 calc R . . C28 C 1.1758(3) 1.2368(2) -0.3873(3) 0.0255(10) Uani 1 1 d U . . C29 C 0.9674(4) 0.7948(2) 0.1920(3) 0.0269(10) Uani 1 1 d U . . H29 H 0.9237 0.7648 0.1618 0.032 Uiso 1 1 calc R . . C30 C 1.0256(4) 0.7931(2) 0.2883(3) 0.0305(10) Uani 1 1 d U . . H30 H 1.0205 0.7624 0.3219 0.037 Uiso 1 1 calc R . . C31 C 1.0930(4) 0.8377(2) 0.3366(3) 0.0271(10) Uani 1 1 d U . . C32 C 1.0938(4) 0.8824(2) 0.2801(4) 0.0329(11) Uani 1 1 d U . . H32 H 1.1370 0.9130 0.3081 0.039 Uiso 1 1 calc R . . C33 C 1.0328(4) 0.8820(2) 0.1855(3) 0.0307(11) Uani 1 1 d U . . H33 H 1.0334 0.9131 0.1507 0.037 Uiso 1 1 calc R . . C34 C 1.1608(4) 0.8371(2) 0.4371(4) 0.0339(10) Uani 1 1 d U . . C35 C 1.2407(4) 0.8739(2) 0.4906(4) 0.0380(11) Uani 1 1 d U . . H35 H 1.2553 0.9059 0.4657 0.046 Uiso 1 1 calc R . . C36 C 1.2975(4) 0.8582(3) 0.5861(4) 0.0376(11) Uani 1 1 d U . . H36 H 1.3537 0.8785 0.6304 0.045 Uiso 1 1 calc R . . C37 C 1.2617(4) 0.8108(3) 0.6064(4) 0.0401(12) Uani 1 1 d U . . C38 C 1.2970(4) 0.7818(3) 0.6970(4) 0.0453(12) Uani 1 1 d U . . C39 C 1.2492(5) 0.7442(4) 0.7250(5) 0.0791(18) Uani 1 1 d U . . H39 H 1.1801 0.7337 0.6878 0.095 Uiso 1 1 calc R . . C40 C 1.3089(5) 0.7217(4) 0.8129(5) 0.0806(18) Uani 1 1 d U . . H40 H 1.2848 0.6940 0.8390 0.097 Uiso 1 1 calc R . . C41 C 1.4067(4) 0.7439(3) 0.8582(4) 0.0519(13) Uani 1 1 d U . . C42 C 1.4703(5) 0.6960(3) 1.0106(4) 0.0666(16) Uani 1 1 d U . . H42 H 1.4016 0.6863 0.9946 0.080 Uiso 1 1 calc R . . C43 C 1.5496(5) 0.6778(3) 1.0960(4) 0.0602(15) Uani 1 1 d U . . H43 H 1.5326 0.6561 1.1356 0.072 Uiso 1 1 calc R . . C44 C 1.6687(4) 0.7220(3) 1.0632(4) 0.0428(12) Uani 1 1 d U . . H44 H 1.7379 0.7316 1.0810 0.051 Uiso 1 1 calc R . . C45 C 1.5937(4) 0.7413(3) 0.9779(4) 0.0430(12) Uani 1 1 d U . . H45 H 1.6125 0.7633 0.9399 0.052 Uiso 1 1 calc R . . C46 C 1.4905(4) 0.7280(3) 0.9490(4) 0.0458(12) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0219(3) 0.0251(3) 0.0236(3) -0.0034(2) 0.0093(2) 0.0001(2) Zn2 0.0382(3) 0.0279(3) 0.0278(3) 0.0000(2) 0.0200(3) 0.0002(3) S1 0.0359(7) 0.0471(8) 0.0294(7) 0.0030(6) 0.0076(6) -0.0025(6) S2 0.0376(8) 0.0560(9) 0.0309(8) 0.0040(7) 0.0062(6) -0.0092(7) O1 0.0237(17) 0.0324(19) 0.032(2) -0.0079(15) 0.0103(16) 0.0026(15) O2 0.038(2) 0.041(2) 0.0280(19) -0.0026(16) 0.0212(17) 0.0042(17) O3 0.0315(18) 0.0325(19) 0.048(2) 0.0127(17) 0.0247(17) 0.0077(16) O4 0.041(2) 0.054(3) 0.048(2) 0.000(2) 0.026(2) -0.0104(19) O5 0.041(2) 0.059(3) 0.056(3) 0.020(2) 0.034(2) 0.011(2) O6 0.047(2) 0.029(2) 0.048(2) 0.0088(17) 0.027(2) 0.0020(16) O7 0.052(2) 0.033(2) 0.038(2) -0.0042(17) 0.0308(19) -0.0024(17) O8 0.0356(19) 0.0259(18) 0.036(2) 0.0028(15) 0.0187(17) 0.0022(15) O9 0.0339(18) 0.0272(18) 0.0240(18) 0.0047(14) 0.0121(15) 0.0026(15) O10 0.047(2) 0.0244(18) 0.0274(19) -0.0003(15) 0.0169(17) 0.0024(16) N1 0.023(2) 0.026(2) 0.028(2) -0.0056(17) 0.0101(18) -0.0013(17) N2 0.035(2) 0.046(3) 0.031(2) 0.002(2) 0.020(2) -0.003(2) C1 0.031(2) 0.027(2) 0.029(2) -0.0021(19) 0.016(2) -0.0032(19) C2 0.023(2) 0.029(2) 0.029(2) -0.0028(18) 0.0137(18) -0.0016(18) C3 0.022(2) 0.031(2) 0.029(2) 0.0002(19) 0.0091(18) 0.0006(18) C4 0.032(2) 0.035(2) 0.026(2) 0.0014(19) 0.0149(18) 0.0008(19) C5 0.024(2) 0.034(2) 0.028(2) 0.0007(18) 0.0140(17) 0.0021(18) C6 0.030(2) 0.033(2) 0.026(2) 0.0068(19) 0.0111(18) 0.0025(19) C7 0.030(2) 0.031(2) 0.027(2) 0.0002(19) 0.0163(18) -0.0033(19) C8 0.023(2) 0.037(2) 0.030(2) 0.0039(19) 0.0106(18) 0.0034(19) C9 0.033(2) 0.035(2) 0.031(2) 0.004(2) 0.0116(19) 0.004(2) C10 0.030(2) 0.042(2) 0.028(2) 0.004(2) 0.0168(19) 0.006(2) C11 0.024(2) 0.042(2) 0.028(2) 0.001(2) 0.0138(18) -0.0004(19) C12 0.037(2) 0.035(2) 0.038(2) -0.003(2) 0.016(2) -0.003(2) C13 0.031(2) 0.036(2) 0.035(2) -0.0007(19) 0.0163(19) 0.0022(19) C14 0.034(2) 0.046(3) 0.025(2) 0.004(2) 0.012(2) -0.001(2) C15 0.040(2) 0.028(2) 0.026(2) -0.0003(19) 0.019(2) 0.003(2) C16 0.035(2) 0.028(2) 0.029(2) 0.0012(19) 0.0163(19) -0.0008(19) C17 0.038(2) 0.030(2) 0.033(2) 0.0029(19) 0.023(2) 0.004(2) C18 0.041(2) 0.027(2) 0.037(2) -0.0038(19) 0.0223(19) 0.0000(19) C19 0.034(2) 0.025(2) 0.029(2) 0.0041(18) 0.0150(18) 0.0047(18) C20 0.042(2) 0.029(2) 0.043(2) 0.002(2) 0.023(2) 0.005(2) C21 0.043(2) 0.025(2) 0.039(2) 0.002(2) 0.021(2) 0.004(2) C22 0.036(2) 0.026(2) 0.034(2) 0.0027(19) 0.0184(19) 0.0027(19) C23 0.044(2) 0.035(2) 0.031(2) 0.0079(19) 0.0197(19) 0.004(2) C24 0.039(2) 0.027(2) 0.028(2) 0.0006(19) 0.014(2) 0.006(2) C25 0.030(2) 0.024(2) 0.029(2) -0.0023(18) 0.0123(19) -0.0001(18) C26 0.046(3) 0.032(2) 0.028(2) 0.006(2) 0.014(2) 0.000(2) C27 0.050(2) 0.032(2) 0.028(2) -0.0006(19) 0.014(2) -0.003(2) C28 0.024(2) 0.026(2) 0.028(2) 0.0027(19) 0.0125(18) 0.0020(18) C29 0.023(2) 0.027(2) 0.027(2) -0.0031(19) 0.0089(18) -0.0040(18) C30 0.028(2) 0.031(2) 0.030(2) -0.004(2) 0.0111(19) -0.0011(19) C31 0.024(2) 0.032(2) 0.027(2) -0.0055(18) 0.0125(17) 0.0043(18) C32 0.033(2) 0.025(2) 0.032(2) -0.0036(19) 0.0074(19) 0.0013(19) C33 0.032(2) 0.022(2) 0.030(2) -0.0039(19) 0.0068(19) -0.0014(19) C34 0.032(2) 0.039(2) 0.032(2) -0.009(2) 0.0161(18) 0.0006(19) C35 0.034(2) 0.048(3) 0.030(2) -0.007(2) 0.013(2) 0.002(2) C36 0.028(2) 0.058(3) 0.027(2) -0.004(2) 0.0120(19) 0.000(2) C37 0.029(2) 0.064(3) 0.028(2) -0.004(2) 0.0138(19) 0.007(2) C38 0.030(2) 0.080(3) 0.029(2) 0.002(2) 0.016(2) -0.005(2) C39 0.047(3) 0.114(4) 0.050(3) 0.026(3) 0.000(3) -0.015(3) C40 0.047(3) 0.116(4) 0.053(3) 0.029(3) 0.000(2) -0.020(3) C41 0.037(2) 0.087(3) 0.033(2) 0.008(2) 0.017(2) -0.011(2) C42 0.045(3) 0.106(4) 0.042(3) 0.021(3) 0.014(2) -0.018(3) C43 0.044(3) 0.101(4) 0.038(3) 0.021(3) 0.020(2) -0.016(3) C44 0.029(2) 0.060(3) 0.038(3) 0.011(2) 0.014(2) -0.004(2) C45 0.034(2) 0.067(3) 0.027(2) 0.012(2) 0.012(2) -0.008(2) C46 0.031(2) 0.080(3) 0.029(2) 0.011(2) 0.016(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.967(3) . ? Zn1 O9 1.996(3) 2_744 ? Zn1 N1 2.048(4) . ? Zn1 O4 2.048(4) 1_655 ? Zn1 O5 2.274(4) 1_655 ? Zn1 C14 2.486(5) 1_655 ? Zn2 O10 1.946(3) 2_744 ? Zn2 O2 1.987(3) . ? Zn2 O7 1.990(3) . ? Zn2 N2 2.054(4) 4_474 ? Zn2 O6 2.346(4) . ? Zn2 C15 2.497(5) . ? S1 C34 1.733(6) . ? S1 C37 1.738(6) . ? S2 C38 1.704(6) . ? S2 C41 1.706(6) . ? O1 C1 1.275(6) . ? O2 C1 1.246(6) . ? O3 C8 1.375(6) . ? O3 C5 1.389(5) . ? O4 C14 1.266(6) . ? O4 Zn1 2.048(4) 1_455 ? O5 C14 1.258(6) . ? O5 Zn1 2.274(4) 1_455 ? O6 C15 1.248(6) . ? O7 C15 1.280(6) . ? O8 C19 1.380(6) . ? O8 C22 1.397(6) . ? O9 C28 1.274(5) . ? O9 Zn1 1.996(3) 2_754 ? O10 C28 1.254(6) . ? O10 Zn2 1.946(3) 2_754 ? N1 C33 1.351(6) . ? N1 C29 1.351(6) . ? N2 C43 1.320(7) . ? N2 C44 1.344(7) . ? N2 Zn2 2.054(4) 4_677 ? C1 C2 1.489(6) . ? C2 C7 1.381(7) . ? C2 C3 1.388(7) . ? C3 C4 1.393(6) . ? C3 H3 0.9300 . ? C4 C5 1.385(7) . ? C4 H4 0.9300 . ? C5 C6 1.408(7) . ? C6 C7 1.369(7) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C13 1.389(7) . ? C8 C9 1.390(7) . ? C9 C10 1.381(7) . ? C9 H9 0.9300 . ? C10 C11 1.389(7) . ? C10 H10 0.9300 . ? C11 C12 1.397(7) . ? C11 C14 1.489(7) . ? C12 C13 1.361(7) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 Zn1 2.486(5) 1_455 ? C15 C16 1.493(7) . ? C16 C21 1.385(7) . ? C16 C17 1.385(7) . ? C17 C18 1.398(7) . ? C17 H17 0.9300 . ? C18 C19 1.370(7) . ? C18 H18 0.9300 . ? C19 C20 1.394(7) . ? C20 C21 1.367(7) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C27 1.362(7) . ? C22 C23 1.387(7) . ? C23 C24 1.371(7) . ? C23 H23 0.9300 . ? C24 C25 1.403(7) . ? C24 H24 0.9300 . ? C25 C26 1.372(7) . ? C25 C28 1.487(7) . ? C26 C27 1.391(7) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C29 C30 1.371(7) . ? C29 H29 0.9300 . ? C30 C31 1.409(7) . ? C30 H30 0.9300 . ? C31 C32 1.400(7) . ? C31 C34 1.445(7) . ? C32 C33 1.355(7) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.388(7) . ? C35 C36 1.410(7) . ? C35 H35 0.9300 . ? C36 C37 1.342(8) . ? C36 H36 0.9300 . ? C37 C38 1.468(8) . ? C38 C39 1.325(9) . ? C39 C40 1.373(9) . ? C39 H39 0.9300 . ? C40 C41 1.361(9) . ? C40 H40 0.9300 . ? C41 C46 1.448(8) . ? C42 C46 1.374(8) . ? C42 C43 1.387(9) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 C45 1.373(7) . ? C44 H44 0.9300 . ? C45 C46 1.376(7) . ? C45 H45 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O9 98.28(14) . 2_744 ? O1 Zn1 N1 106.07(14) . . ? O9 Zn1 N1 101.17(14) 2_744 . ? O1 Zn1 O4 138.66(15) . 1_655 ? O9 Zn1 O4 96.77(15) 2_744 1_655 ? N1 Zn1 O4 108.40(16) . 1_655 ? O1 Zn1 O5 95.21(14) . 1_655 ? O9 Zn1 O5 156.21(14) 2_744 1_655 ? N1 Zn1 O5 93.75(15) . 1_655 ? O4 Zn1 O5 60.66(15) 1_655 1_655 ? O1 Zn1 C14 120.14(16) . 1_655 ? O9 Zn1 C14 127.16(16) 2_744 1_655 ? N1 Zn1 C14 101.15(16) . 1_655 ? O4 Zn1 C14 30.51(16) 1_655 1_655 ? O5 Zn1 C14 30.23(15) 1_655 1_655 ? O10 Zn2 O2 106.67(14) 2_744 . ? O10 Zn2 O7 136.54(15) 2_744 . ? O2 Zn2 O7 97.80(14) . . ? O10 Zn2 N2 98.35(16) 2_744 4_474 ? O2 Zn2 N2 100.22(15) . 4_474 ? O7 Zn2 N2 112.16(16) . 4_474 ? O10 Zn2 O6 89.52(13) 2_744 . ? O2 Zn2 O6 157.75(13) . . ? O7 Zn2 O6 60.23(13) . . ? N2 Zn2 O6 92.17(15) 4_474 . ? O10 Zn2 C15 113.99(15) 2_744 . ? O2 Zn2 C15 128.27(15) . . ? O7 Zn2 C15 30.56(14) . . ? N2 Zn2 C15 103.97(16) 4_474 . ? O6 Zn2 C15 29.66(13) . . ? C34 S1 C37 91.6(3) . . ? C38 S2 C41 93.8(3) . . ? C1 O1 Zn1 130.0(3) . . ? C1 O2 Zn2 139.5(3) . . ? C8 O3 C5 120.1(4) . . ? C14 O4 Zn1 94.2(3) . 1_455 ? C14 O5 Zn1 84.2(3) . 1_455 ? C15 O6 Zn2 81.9(3) . . ? C15 O7 Zn2 97.2(3) . . ? C19 O8 C22 118.3(4) . . ? C28 O9 Zn1 121.9(3) . 2_754 ? C28 O10 Zn2 144.4(3) . 2_754 ? C33 N1 C29 117.2(4) . . ? C33 N1 Zn1 119.7(3) . . ? C29 N1 Zn1 123.1(3) . . ? C43 N2 C44 116.6(5) . . ? C43 N2 Zn2 121.1(4) . 4_677 ? C44 N2 Zn2 122.2(3) . 4_677 ? O2 C1 O1 125.9(4) . . ? O2 C1 C2 118.0(4) . . ? O1 C1 C2 116.1(4) . . ? C7 C2 C3 119.2(4) . . ? C7 C2 C1 120.3(4) . . ? C3 C2 C1 120.5(4) . . ? C2 C3 C4 120.5(5) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 118.8(4) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 O3 121.6(4) . . ? C4 C5 C6 121.3(4) . . ? O3 C5 C6 117.0(4) . . ? C7 C6 C5 118.0(4) . . ? C7 C6 H6 121.0 . . ? C5 C6 H6 121.0 . . ? C6 C7 C2 122.1(4) . . ? C6 C7 H7 118.9 . . ? C2 C7 H7 118.9 . . ? O3 C8 C13 123.5(4) . . ? O3 C8 C9 115.7(5) . . ? C13 C8 C9 120.4(5) . . ? C10 C9 C8 119.2(5) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 120.9(5) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C12 118.6(5) . . ? C10 C11 C14 120.3(4) . . ? C12 C11 C14 121.1(5) . . ? C13 C12 C11 121.2(5) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C8 119.7(5) . . ? C12 C13 H13 120.2 . . ? C8 C13 H13 120.2 . . ? O5 C14 O4 120.6(5) . . ? O5 C14 C11 119.8(5) . . ? O4 C14 C11 119.7(5) . . ? O5 C14 Zn1 65.5(3) . 1_455 ? O4 C14 Zn1 55.3(3) . 1_455 ? C11 C14 Zn1 173.5(4) . 1_455 ? O6 C15 O7 120.7(5) . . ? O6 C15 C16 121.0(4) . . ? O7 C15 C16 118.3(4) . . ? O6 C15 Zn2 68.4(3) . . ? O7 C15 Zn2 52.3(2) . . ? C16 C15 Zn2 170.5(4) . . ? C21 C16 C17 118.6(5) . . ? C21 C16 C15 120.8(4) . . ? C17 C16 C15 120.5(4) . . ? C16 C17 C18 120.7(5) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 119.1(5) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 O8 124.6(4) . . ? C18 C19 C20 120.7(5) . . ? O8 C19 C20 114.6(4) . . ? C21 C20 C19 119.2(5) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 C16 121.6(5) . . ? C20 C21 H21 119.2 . . ? C16 C21 H21 119.2 . . ? C27 C22 C23 122.3(5) . . ? C27 C22 O8 117.0(4) . . ? C23 C22 O8 120.8(4) . . ? C24 C23 C22 118.9(5) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C23 C24 C25 120.2(5) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 119.1(5) . . ? C26 C25 C28 120.5(4) . . ? C24 C25 C28 120.5(4) . . ? C25 C26 C27 121.3(5) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C22 C27 C26 118.2(5) . . ? C22 C27 H27 120.9 . . ? C26 C27 H27 120.9 . . ? O10 C28 O9 125.8(4) . . ? O10 C28 C25 116.6(4) . . ? O9 C28 C25 117.6(4) . . ? N1 C29 C30 122.8(4) . . ? N1 C29 H29 118.6 . . ? C30 C29 H29 118.6 . . ? C29 C30 C31 120.3(5) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C32 C31 C30 115.7(4) . . ? C32 C31 C34 121.3(5) . . ? C30 C31 C34 123.0(5) . . ? C33 C32 C31 121.1(5) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? N1 C33 C32 123.0(5) . . ? N1 C33 H33 118.5 . . ? C32 C33 H33 118.5 . . ? C35 C34 C31 128.7(5) . . ? C35 C34 S1 109.7(4) . . ? C31 C34 S1 121.4(4) . . ? C34 C35 C36 113.9(5) . . ? C34 C35 H35 123.1 . . ? C36 C35 H35 123.1 . . ? C37 C36 C35 112.6(5) . . ? C37 C36 H36 123.7 . . ? C35 C36 H36 123.7 . . ? C36 C37 C38 129.5(5) . . ? C36 C37 S1 112.2(4) . . ? C38 C37 S1 118.3(5) . . ? C39 C38 C37 130.6(5) . . ? C39 C38 S2 108.9(5) . . ? C37 C38 S2 120.2(4) . . ? C38 C39 C40 115.3(6) . . ? C38 C39 H39 122.3 . . ? C40 C39 H39 122.3 . . ? C41 C40 C39 113.8(7) . . ? C41 C40 H40 123.1 . . ? C39 C40 H40 123.1 . . ? C40 C41 C46 128.0(6) . . ? C40 C41 S2 108.1(5) . . ? C46 C41 S2 123.5(4) . . ? C46 C42 C43 121.8(6) . . ? C46 C42 H42 119.1 . . ? C43 C42 H42 119.1 . . ? N2 C43 C42 121.9(5) . . ? N2 C43 H43 119.0 . . ? C42 C43 H43 119.0 . . ? N2 C44 C45 124.2(5) . . ? N2 C44 H44 117.9 . . ? C45 C44 H44 117.9 . . ? C44 C45 C46 119.7(5) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C42 C46 C45 115.9(5) . . ? C42 C46 C41 120.5(5) . . ? C45 C46 C41 123.6(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 O9 Zn1 O1 C1 -80.0(4) 2_744 . . . ? N1 Zn1 O1 C1 175.8(4) . . . . ? O4 Zn1 O1 C1 30.2(5) 1_655 . . . ? O5 Zn1 O1 C1 80.4(4) 1_655 . . . ? C14 Zn1 O1 C1 62.2(4) 1_655 . . . ? O10 Zn2 O2 C1 46.9(5) 2_744 . . . ? O7 Zn2 O2 C1 -96.8(5) . . . . ? N2 Zn2 O2 C1 148.9(5) 4_474 . . . ? O6 Zn2 O2 C1 -88.2(6) . . . . ? C15 Zn2 O2 C1 -94.0(5) . . . . ? O10 Zn2 O6 C15 -146.7(3) 2_744 . . . ? O2 Zn2 O6 C15 -9.2(5) . . . . ? O7 Zn2 O6 C15 0.5(3) . . . . ? N2 Zn2 O6 C15 114.9(3) 4_474 . . . ? O10 Zn2 O7 C15 51.4(4) 2_744 . . . ? O2 Zn2 O7 C15 175.8(3) . . . . ? N2 Zn2 O7 C15 -79.8(3) 4_474 . . . ? O6 Zn2 O7 C15 -0.5(3) . . . . ? O1 Zn1 N1 C33 -92.5(4) . . . . ? O9 Zn1 N1 C33 165.4(3) 2_744 . . . ? O4 Zn1 N1 C33 64.3(4) 1_655 . . . ? O5 Zn1 N1 C33 4.0(4) 1_655 . . . ? C14 Zn1 N1 C33 33.6(4) 1_655 . . . ? O1 Zn1 N1 C29 90.1(4) . . . . ? O9 Zn1 N1 C29 -12.0(4) 2_744 . . . ? O4 Zn1 N1 C29 -113.1(4) 1_655 . . . ? O5 Zn1 N1 C29 -173.4(4) 1_655 . . . ? C14 Zn1 N1 C29 -143.8(4) 1_655 . . . ? Zn2 O2 C1 O1 5.2(9) . . . . ? Zn2 O2 C1 C2 -174.1(3) . . . . ? Zn1 O1 C1 O2 3.7(7) . . . . ? Zn1 O1 C1 C2 -176.9(3) . . . . ? O2 C1 C2 C7 -21.0(7) . . . . ? O1 C1 C2 C7 159.6(4) . . . . ? O2 C1 C2 C3 158.3(5) . . . . ? O1 C1 C2 C3 -21.1(7) . . . . ? C7 C2 C3 C4 0.5(7) . . . . ? C1 C2 C3 C4 -178.8(4) . . . . ? C2 C3 C4 C5 0.5(7) . . . . ? C3 C4 C5 O3 -176.2(4) . . . . ? C3 C4 C5 C6 -1.0(7) . . . . ? C8 O3 C5 C4 -51.1(6) . . . . ? C8 O3 C5 C6 133.5(5) . . . . ? C4 C5 C6 C7 0.6(7) . . . . ? O3 C5 C6 C7 175.9(4) . . . . ? C5 C6 C7 C2 0.5(7) . . . . ? C3 C2 C7 C6 -1.0(7) . . . . ? C1 C2 C7 C6 178.3(4) . . . . ? C5 O3 C8 C13 -29.6(7) . . . . ? C5 O3 C8 C9 156.9(4) . . . . ? O3 C8 C9 C10 173.1(4) . . . . ? C13 C8 C9 C10 -0.6(7) . . . . ? C8 C9 C10 C11 1.3(7) . . . . ? C9 C10 C11 C12 -0.5(7) . . . . ? C9 C10 C11 C14 179.7(4) . . . . ? C10 C11 C12 C13 -1.1(8) . . . . ? C14 C11 C12 C13 178.6(5) . . . . ? C11 C12 C13 C8 1.9(8) . . . . ? O3 C8 C13 C12 -174.2(4) . . . . ? C9 C8 C13 C12 -1.0(8) . . . . ? Zn1 O5 C14 O4 5.3(5) 1_455 . . . ? Zn1 O5 C14 C11 -175.7(4) 1_455 . . . ? Zn1 O4 C14 O5 -5.8(5) 1_455 . . . ? Zn1 O4 C14 C11 175.1(4) 1_455 . . . ? C10 C11 C14 O5 -1.1(7) . . . . ? C12 C11 C14 O5 179.2(5) . . . . ? C10 C11 C14 O4 178.0(5) . . . . ? C12 C11 C14 O4 -1.8(7) . . . . ? Zn2 O6 C15 O7 -0.8(4) . . . . ? Zn2 O6 C15 C16 -179.4(4) . . . . ? Zn2 O7 C15 O6 1.0(5) . . . . ? Zn2 O7 C15 C16 179.6(4) . . . . ? O10 Zn2 C15 O6 36.9(3) 2_744 . . . ? O2 Zn2 C15 O6 175.6(3) . . . . ? O7 Zn2 C15 O6 -179.1(5) . . . . ? N2 Zn2 C15 O6 -69.0(3) 4_474 . . . ? O10 Zn2 C15 O7 -144.0(3) 2_744 . . . ? O2 Zn2 C15 O7 -5.3(4) . . . . ? N2 Zn2 C15 O7 110.1(3) 4_474 . . . ? O6 Zn2 C15 O7 179.1(5) . . . . ? O6 C15 C16 C21 -6.7(8) . . . . ? O7 C15 C16 C21 174.7(5) . . . . ? O6 C15 C16 C17 171.0(5) . . . . ? O7 C15 C16 C17 -7.6(7) . . . . ? C21 C16 C17 C18 -0.3(8) . . . . ? C15 C16 C17 C18 -178.1(4) . . . . ? C16 C17 C18 C19 -1.5(8) . . . . ? C17 C18 C19 O8 -178.4(4) . . . . ? C17 C18 C19 C20 3.1(8) . . . . ? C22 O8 C19 C18 -0.6(7) . . . . ? C22 O8 C19 C20 178.0(4) . . . . ? C18 C19 C20 C21 -2.8(8) . . . . ? O8 C19 C20 C21 178.5(4) . . . . ? C19 C20 C21 C16 1.0(8) . . . . ? C17 C16 C21 C20 0.5(8) . . . . ? C15 C16 C21 C20 178.3(5) . . . . ? C19 O8 C22 C27 -115.6(5) . . . . ? C19 O8 C22 C23 65.4(6) . . . . ? C27 C22 C23 C24 1.3(8) . . . . ? O8 C22 C23 C24 -179.8(5) . . . . ? C22 C23 C24 C25 -0.4(8) . . . . ? C23 C24 C25 C26 -1.3(8) . . . . ? C23 C24 C25 C28 178.8(5) . . . . ? C24 C25 C26 C27 2.1(8) . . . . ? C28 C25 C26 C27 -177.9(5) . . . . ? C23 C22 C27 C26 -0.5(8) . . . . ? O8 C22 C27 C26 -179.4(5) . . . . ? C25 C26 C27 C22 -1.3(8) . . . . ? Zn2 O10 C28 O9 -16.4(9) 2_754 . . . ? Zn2 O10 C28 C25 164.0(4) 2_754 . . . ? Zn1 O9 C28 O10 -15.3(6) 2_754 . . . ? Zn1 O9 C28 C25 164.3(3) 2_754 . . . ? C26 C25 C28 O10 -179.0(5) . . . . ? C24 C25 C28 O10 0.9(7) . . . . ? C26 C25 C28 O9 1.4(7) . . . . ? C24 C25 C28 O9 -178.7(4) . . . . ? C33 N1 C29 C30 -2.0(7) . . . . ? Zn1 N1 C29 C30 175.4(3) . . . . ? N1 C29 C30 C31 -0.2(7) . . . . ? C29 C30 C31 C32 1.1(7) . . . . ? C29 C30 C31 C34 -176.3(4) . . . . ? C30 C31 C32 C33 0.2(7) . . . . ? C34 C31 C32 C33 177.7(5) . . . . ? C29 N1 C33 C32 3.5(7) . . . . ? Zn1 N1 C33 C32 -174.0(4) . . . . ? C31 C32 C33 N1 -2.6(8) . . . . ? C32 C31 C34 C35 -7.5(8) . . . . ? C30 C31 C34 C35 169.8(5) . . . . ? C32 C31 C34 S1 177.7(4) . . . . ? C30 C31 C34 S1 -5.0(7) . . . . ? C37 S1 C34 C35 -0.2(4) . . . . ? C37 S1 C34 C31 175.5(4) . . . . ? C31 C34 C35 C36 -174.7(5) . . . . ? S1 C34 C35 C36 0.6(6) . . . . ? C34 C35 C36 C37 -0.8(7) . . . . ? C35 C36 C37 C38 -178.1(5) . . . . ? C35 C36 C37 S1 0.6(6) . . . . ? C34 S1 C37 C36 -0.2(4) . . . . ? C34 S1 C37 C38 178.6(4) . . . . ? C36 C37 C38 C39 160.6(8) . . . . ? S1 C37 C38 C39 -18.0(10) . . . . ? C36 C37 C38 S2 -25.6(9) . . . . ? S1 C37 C38 S2 155.8(4) . . . . ? C41 S2 C38 C39 -2.2(6) . . . . ? C41 S2 C38 C37 -177.2(5) . . . . ? C37 C38 C39 C40 174.5(7) . . . . ? S2 C38 C39 C40 0.2(10) . . . . ? C38 C39 C40 C41 2.6(12) . . . . ? C39 C40 C41 C46 -176.7(8) . . . . ? C39 C40 C41 S2 -4.1(10) . . . . ? C38 S2 C41 C40 3.6(6) . . . . ? C38 S2 C41 C46 176.6(6) . . . . ? C44 N2 C43 C42 0.6(10) . . . . ? Zn2 N2 C43 C42 178.5(6) 4_677 . . . ? C46 C42 C43 N2 0.1(12) . . . . ? C43 N2 C44 C45 -0.6(9) . . . . ? Zn2 N2 C44 C45 -178.4(5) 4_677 . . . ? N2 C44 C45 C46 -0.2(10) . . . . ? C43 C42 C46 C45 -0.9(11) . . . . ? C43 C42 C46 C41 176.8(7) . . . . ? C44 C45 C46 C42 0.9(10) . . . . ? C44 C45 C46 C41 -176.7(6) . . . . ? C40 C41 C46 C42 -15.9(12) . . . . ? S2 C41 C46 C42 172.5(6) . . . . ? C40 C41 C46 C45 161.6(8) . . . . ? S2 C41 C46 C45 -10.0(10) . . . . ? 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 0.500 0.000 0.500 575 845 ' ' 2 0.500 0.500 1.000 575 865 ' ' _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.818 _refine_diff_density_min -0.910 _refine_diff_density_rms 0.089 # === END