# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Qin-Yu Zhu' 'Jin-Po Wang' 'Yu-Rong Qin' 'Zheng Shi' 'Qiong-Hua Han' ; Guo-Qing Bian ; 'Jie Dai' _publ_contact_author_name 'Qin-Yu Zhu' _publ_contact_author_email zhuqinyu@suda.edu.cn data_l _database_code_depnum_ccdc_archive 'CCDC 772444' #TrackingRef '- 1-4-revised.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H14 Cu N2 O4 S6' _chemical_formula_weight 602.23 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.276(5) _cell_length_b 8.8492(11) _cell_length_c 19.470(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.260(3) _cell_angle_gamma 90.00 _cell_volume 4792.4(12) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9465 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Platelet _exptl_crystal_colour Red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2440 _exptl_absorpt_coefficient_mu 1.466 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.768 _exptl_absorpt_correction_T_max 0.889 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11224 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4192 _reflns_number_gt 3395 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The disorder atom was split into two positions. ; _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^)+(0.0742P)^2^+39.0263P] 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 4192 _refine_ls_number_parameters 275 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1032 _refine_ls_R_factor_gt 0.0824 _refine_ls_wR_factor_ref 0.1968 _refine_ls_wR_factor_gt 0.1831 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.114 _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 Cu1 Cu 0.20799(3) 0.29909(9) 0.25520(4) 0.0322(3) Uani 1 1 d . . . S1 S 0.37847(6) 0.3977(2) 0.42402(10) 0.0387(5) Uani 1 1 d . . . S2 S 0.40958(7) 0.6897(2) 0.50177(11) 0.0451(5) Uani 1 1 d . . . S3 S 0.47283(8) 0.2360(3) 0.53870(13) 0.0598(7) Uani 1 1 d U . . S4 S 0.50941(7) 0.5244(2) 0.61672(11) 0.0454(5) Uani 1 1 d U . . S5 S 0.5514(2) 0.0554(7) 0.6589(3) 0.0658(15) Uiso 0.50 1 d PU . . S5' S 0.55893(17) 0.0591(5) 0.6338(3) 0.0515(11) Uiso 0.50 1 d P . . S6 S 0.59599(7) 0.3806(3) 0.73471(12) 0.0514(6) Uani 1 1 d U . . O1 O 0.28382(17) 0.3792(5) 0.3210(3) 0.0400(12) Uani 1 1 d . . . O2 O 0.27328(16) 0.6083(5) 0.2712(3) 0.0376(12) Uani 1 1 d . . . O3 O 0.3443(3) 0.9267(7) 0.4615(3) 0.079(2) Uani 1 1 d . . . O4 O 0.30388(18) 0.8818(6) 0.3412(3) 0.0396(12) Uani 1 1 d . . . N1 N 0.20629(19) 0.2153(6) 0.3496(3) 0.0328(13) Uani 1 1 d . . . N2 N 0.1783(2) 0.4735(6) 0.2850(3) 0.0341(13) Uani 1 1 d . . . C1 C 0.3426(2) 0.5565(8) 0.3852(4) 0.0305(15) Uani 1 1 d . . . C2 C 0.3567(2) 0.6908(8) 0.4195(4) 0.0335(15) Uani 1 1 d . . . C3 C 0.4229(2) 0.4972(8) 0.4961(4) 0.0355(16) Uani 1 1 d . . . C4 C 0.4621(3) 0.4306(11) 0.5444(5) 0.0638(11) Uani 1 1 d U . . C5 C 0.5262(3) 0.2304(11) 0.6206(5) 0.0638(11) Uani 1 1 d U . . C6 C 0.5423(3) 0.3602(11) 0.6553(5) 0.0638(11) Uani 1 1 d U . . C7 C 0.5098(3) -0.0626(10) 0.6403(5) 0.0638(11) Uani 1 1 d U . . H7A H 0.4913 -0.0412 0.6699 0.096 Uiso 1 1 calc R . . H7B H 0.5234 -0.1634 0.6517 0.096 Uiso 1 1 calc R . . H7C H 0.4891 -0.0563 0.5876 0.096 Uiso 1 1 calc R . . C8 C 0.5743(3) 0.3829(11) 0.8067(5) 0.0638(11) Uani 1 1 d . . . H8A H 0.5482 0.4550 0.7944 0.096 Uiso 1 1 calc R . . H8B H 0.6001 0.4120 0.8534 0.096 Uiso 1 1 calc R . . H8C H 0.5628 0.2830 0.8119 0.096 Uiso 1 1 calc R . . C9 C 0.2964(2) 0.5132(8) 0.3207(3) 0.0311(15) Uani 1 1 d . . . C10 C 0.3327(3) 0.8443(9) 0.4052(4) 0.0419(18) Uani 1 1 d . . . C11 C 0.2235(3) 0.0786(9) 0.3791(4) 0.0423(18) Uani 1 1 d . . . H11 H 0.2374 0.0152 0.3543 0.051 Uiso 1 1 calc R . . C12 C 0.2211(3) 0.0302(10) 0.4453(4) 0.047(2) Uani 1 1 d . . . H12 H 0.2333 -0.0647 0.4656 0.057 Uiso 1 1 calc R . . C13 C 0.2004(3) 0.1247(10) 0.4806(4) 0.052(2) Uani 1 1 d . . . H13 H 0.1984 0.0933 0.5254 0.062 Uiso 1 1 calc R . . C14 C 0.1827(3) 0.2633(10) 0.4514(4) 0.0456(19) Uani 1 1 d . . . H14 H 0.1687 0.3278 0.4756 0.055 Uiso 1 1 calc R . . C15 C 0.1862(2) 0.3060(8) 0.3844(4) 0.0343(16) Uani 1 1 d . . . C16 C 0.1658(3) 0.6053(8) 0.2488(5) 0.0443(19) Uani 1 1 d . . . H16 H 0.1720 0.6190 0.2055 0.053 Uiso 1 1 calc R . . C17 C 0.1445(3) 0.7218(9) 0.2711(5) 0.055(2) Uani 1 1 d . . . H17 H 0.1363 0.8131 0.2444 0.066 Uiso 1 1 calc R . . C18 C 0.1356(4) 0.6985(10) 0.3350(6) 0.065(3) Uani 1 1 d . . . H18 H 0.1205 0.7744 0.3516 0.078 Uiso 1 1 calc R . . C19 C 0.1486(3) 0.5670(10) 0.3737(5) 0.056(2) Uani 1 1 d . . . H19 H 0.1433 0.5522 0.4177 0.067 Uiso 1 1 calc R . . C20 C 0.1698(3) 0.4547(9) 0.3469(4) 0.0396(17) 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 Cu1 0.0271(5) 0.0375(5) 0.0265(5) -0.0005(4) 0.0046(4) 0.0008(4) S1 0.0255(9) 0.0421(10) 0.0365(10) -0.0013(8) -0.0006(8) 0.0021(8) S2 0.0359(11) 0.0469(11) 0.0350(10) -0.0051(8) -0.0046(8) 0.0043(8) S3 0.0398(12) 0.0501(12) 0.0619(14) -0.0061(11) -0.0095(10) 0.0058(10) S4 0.0309(10) 0.0468(11) 0.0410(11) 0.0062(9) -0.0046(8) 0.0014(8) S6 0.0299(10) 0.0607(13) 0.0459(12) 0.0077(10) -0.0041(9) 0.0008(9) O1 0.029(3) 0.037(3) 0.041(3) 0.003(2) 0.001(2) -0.006(2) O2 0.027(3) 0.042(3) 0.032(3) 0.004(2) -0.001(2) -0.005(2) O3 0.105(6) 0.064(4) 0.037(3) -0.008(3) -0.003(3) 0.036(4) O4 0.039(3) 0.047(3) 0.030(3) 0.003(2) 0.011(2) 0.009(2) N1 0.022(3) 0.039(3) 0.031(3) 0.000(3) 0.004(2) -0.003(2) N2 0.031(3) 0.035(3) 0.034(3) -0.002(3) 0.011(3) -0.003(3) C1 0.023(3) 0.036(4) 0.026(3) 0.007(3) 0.004(3) 0.004(3) C2 0.027(4) 0.042(4) 0.025(3) -0.002(3) 0.004(3) 0.000(3) C3 0.021(3) 0.044(4) 0.034(4) -0.004(3) 0.004(3) 0.005(3) C4 0.049(2) 0.063(2) 0.063(3) 0.006(2) 0.0052(19) 0.003(2) C5 0.049(2) 0.063(2) 0.063(3) 0.006(2) 0.0052(19) 0.003(2) C6 0.049(2) 0.063(2) 0.063(3) 0.006(2) 0.0052(19) 0.003(2) C7 0.049(2) 0.063(2) 0.063(3) 0.006(2) 0.0052(19) 0.003(2) C8 0.049(2) 0.063(2) 0.063(3) 0.006(2) 0.0052(19) 0.003(2) C9 0.024(3) 0.046(4) 0.022(3) -0.003(3) 0.008(3) 0.002(3) C10 0.039(4) 0.049(4) 0.035(4) -0.003(4) 0.012(4) 0.011(4) C11 0.040(4) 0.045(4) 0.037(4) 0.006(3) 0.010(3) 0.002(3) C12 0.041(4) 0.054(5) 0.048(5) 0.019(4) 0.018(4) 0.005(4) C13 0.043(5) 0.072(6) 0.038(4) 0.016(4) 0.013(4) 0.000(4) C14 0.034(4) 0.065(5) 0.035(4) 0.006(4) 0.010(3) 0.003(4) C15 0.019(3) 0.043(4) 0.036(4) -0.005(3) 0.005(3) 0.000(3) C16 0.037(4) 0.044(4) 0.047(4) 0.006(4) 0.011(4) -0.003(3) C17 0.060(6) 0.038(4) 0.069(6) 0.004(4) 0.027(5) 0.007(4) C18 0.072(7) 0.052(5) 0.075(7) -0.010(5) 0.034(6) 0.018(5) C19 0.068(6) 0.057(5) 0.047(5) 0.000(4) 0.028(5) 0.016(5) C20 0.031(4) 0.046(4) 0.031(4) -0.001(3) 0.001(3) 0.003(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 Cu1 O4 1.912(5) 4_545 ? Cu1 O2 1.915(5) 4_545 ? Cu1 N2 1.984(6) . ? Cu1 N1 2.001(6) . ? Cu1 O1 2.256(5) . ? S1 C3 1.750(7) . ? S1 C1 1.754(7) . ? S2 C2 1.762(7) . ? S2 C3 1.763(7) . ? S3 C4 1.764(10) . ? S3 C5 1.767(9) . ? S4 C6 1.754(9) . ? S4 C4 1.769(10) . ? S5 C7 1.562(10) . ? S5 C5 1.758(11) . ? S5' C5 1.774(11) . ? S6 C6 1.754(9) . ? S6 C8 1.767(10) . ? O1 C9 1.245(8) . ? O2 C9 1.264(8) . ? O2 Cu1 1.915(5) 4 ? O3 C10 1.246(9) . ? O4 C10 1.250(8) . ? O4 Cu1 1.912(5) 4 ? N1 C15 1.341(9) . ? N1 C11 1.353(9) . ? N2 C16 1.338(9) . ? N2 C20 1.339(9) . ? C1 C2 1.347(9) . ? C1 C9 1.514(9) . ? C2 C10 1.514(10) . ? C3 C4 1.327(11) . ? C5 C6 1.324(13) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C11 C12 1.387(10) . ? C11 H11 0.9400 . ? C12 C13 1.381(12) . ? C12 H12 0.9400 . ? C13 C14 1.369(12) . ? C13 H13 0.9400 . ? C14 C15 1.402(10) . ? C14 H14 0.9400 . ? C15 C20 1.491(10) . ? C16 C17 1.375(11) . ? C16 H16 0.9400 . ? C17 C18 1.388(13) . ? C17 H17 0.9400 . ? C18 C19 1.356(12) . ? C18 H18 0.9400 . ? C19 C20 1.392(11) . ? C19 H19 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cu1 O2 92.0(2) 4_545 4_545 ? O4 Cu1 N2 93.3(2) 4_545 . ? O2 Cu1 N2 168.7(2) 4_545 . ? O4 Cu1 N1 168.6(2) 4_545 . ? O2 Cu1 N1 92.2(2) 4_545 . ? N2 Cu1 N1 80.8(2) . . ? O4 Cu1 O1 101.04(19) 4_545 . ? O2 Cu1 O1 94.97(19) 4_545 . ? N2 Cu1 O1 93.8(2) . . ? N1 Cu1 O1 89.1(2) . . ? C3 S1 C1 95.2(3) . . ? C2 S2 C3 95.5(3) . . ? C4 S3 C5 95.5(4) . . ? C6 S4 C4 95.5(4) . . ? C7 S5 C5 108.4(6) . . ? C6 S6 C8 101.3(5) . . ? C9 O1 Cu1 122.8(4) . . ? C9 O2 Cu1 131.2(4) . 4 ? C10 O4 Cu1 131.5(5) . 4 ? C15 N1 C11 119.8(6) . . ? C15 N1 Cu1 115.1(5) . . ? C11 N1 Cu1 125.1(5) . . ? C16 N2 C20 117.9(7) . . ? C16 N2 Cu1 126.2(5) . . ? C20 N2 Cu1 115.9(5) . . ? C2 C1 C9 129.9(6) . . ? C2 C1 S1 118.2(5) . . ? C9 C1 S1 111.5(5) . . ? C1 C2 C10 131.7(6) . . ? C1 C2 S2 116.2(5) . . ? C10 C2 S2 111.7(5) . . ? C4 C3 S1 122.3(7) . . ? C4 C3 S2 123.2(6) . . ? S1 C3 S2 114.5(4) . . ? C3 C4 S3 121.6(7) . . ? C3 C4 S4 124.9(7) . . ? S3 C4 S4 113.4(5) . . ? C6 C5 S5 122.5(8) . . ? C6 C5 S3 117.3(7) . . ? S5 C5 S3 119.8(6) . . ? C6 C5 S5' 126.5(8) . . ? S5 C5 S5' 20.1(2) . . ? S3 C5 S5' 114.5(6) . . ? C5 C6 S4 117.8(7) . . ? C5 C6 S6 124.5(8) . . ? S4 C6 S6 117.6(6) . . ? S5 C7 H7A 109.5 . . ? S5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? S5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? S6 C8 H8A 109.5 . . ? S6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C9 O2 123.9(6) . . ? O1 C9 C1 115.0(6) . . ? O2 C9 C1 121.1(6) . . ? O3 C10 O4 124.4(7) . . ? O3 C10 C2 114.5(6) . . ? O4 C10 C2 121.1(6) . . ? N1 C11 C12 121.2(7) . . ? N1 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C13 C12 C11 118.5(7) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C14 C13 C12 121.0(7) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 117.9(8) . . ? C13 C14 H14 121.1 . . ? C15 C14 H14 121.1 . . ? N1 C15 C14 121.6(7) . . ? N1 C15 C20 114.2(6) . . ? C14 C15 C20 124.1(7) . . ? N2 C16 C17 123.9(8) . . ? N2 C16 H16 118.1 . . ? C17 C16 H16 118.1 . . ? C16 C17 C18 117.0(8) . . ? C16 C17 H17 121.5 . . ? C18 C17 H17 121.5 . . ? C19 C18 C17 120.6(8) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 118.6(8) . . ? C18 C19 H19 120.7 . . ? C20 C19 H19 120.7 . . ? N2 C20 C19 122.0(7) . . ? N2 C20 C15 113.9(6) . . ? C19 C20 C15 124.1(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Cu1 O1 C9 49.8(6) 4_545 . . . ? O2 Cu1 O1 C9 142.8(5) 4_545 . . . ? N2 Cu1 O1 C9 -44.3(5) . . . . ? N1 Cu1 O1 C9 -125.1(5) . . . . ? O4 Cu1 N1 C15 -57.7(13) 4_545 . . . ? O2 Cu1 N1 C15 -169.0(5) 4_545 . . . ? N2 Cu1 N1 C15 2.1(5) . . . . ? O1 Cu1 N1 C15 96.0(5) . . . . ? O4 Cu1 N1 C11 122.4(11) 4_545 . . . ? O2 Cu1 N1 C11 11.0(6) 4_545 . . . ? N2 Cu1 N1 C11 -177.9(6) . . . . ? O1 Cu1 N1 C11 -83.9(6) . . . . ? O4 Cu1 N2 C16 -11.4(6) 4_545 . . . ? O2 Cu1 N2 C16 -129.3(10) 4_545 . . . ? N1 Cu1 N2 C16 178.4(6) . . . . ? O1 Cu1 N2 C16 89.9(6) . . . . ? O4 Cu1 N2 C20 167.8(5) 4_545 . . . ? O2 Cu1 N2 C20 49.9(13) 4_545 . . . ? N1 Cu1 N2 C20 -2.4(5) . . . . ? O1 Cu1 N2 C20 -90.9(5) . . . . ? C3 S1 C1 C2 -2.5(6) . . . . ? C3 S1 C1 C9 -176.2(5) . . . . ? C9 C1 C2 C10 -1.7(13) . . . . ? S1 C1 C2 C10 -174.1(6) . . . . ? C9 C1 C2 S2 171.0(5) . . . . ? S1 C1 C2 S2 -1.5(8) . . . . ? C3 S2 C2 C1 4.5(6) . . . . ? C3 S2 C2 C10 178.7(5) . . . . ? C1 S1 C3 C4 -177.6(8) . . . . ? C1 S1 C3 S2 5.5(5) . . . . ? C2 S2 C3 C4 177.0(8) . . . . ? C2 S2 C3 S1 -6.1(5) . . . . ? S1 C3 C4 S3 0.8(12) . . . . ? S2 C3 C4 S3 177.5(5) . . . . ? S1 C3 C4 S4 177.8(5) . . . . ? S2 C3 C4 S4 -5.5(12) . . . . ? C5 S3 C4 C3 -176.1(9) . . . . ? C5 S3 C4 S4 6.5(7) . . . . ? C6 S4 C4 C3 176.2(9) . . . . ? C6 S4 C4 S3 -6.6(7) . . . . ? C7 S5 C5 C6 141.9(10) . . . . ? C7 S5 C5 S3 -30.0(9) . . . . ? C7 S5 C5 S5' -110.0(10) . . . . ? C4 S3 C5 C6 -4.0(10) . . . . ? C4 S3 C5 S5 168.3(7) . . . . ? C4 S3 C5 S5' -169.9(6) . . . . ? S5 C5 C6 S4 -172.1(6) . . . . ? S3 C5 C6 S4 -0.1(13) . . . . ? S5' C5 C6 S4 163.9(6) . . . . ? S5 C5 C6 S6 11.1(15) . . . . ? S3 C5 C6 S6 -176.9(6) . . . . ? S5' C5 C6 S6 -12.9(16) . . . . ? C4 S4 C6 C5 4.1(10) . . . . ? C4 S4 C6 S6 -178.9(6) . . . . ? C8 S6 C6 C5 -99.0(10) . . . . ? C8 S6 C6 S4 84.2(7) . . . . ? Cu1 O1 C9 O2 -19.0(9) . . . . ? Cu1 O1 C9 C1 161.1(4) . . . . ? Cu1 O2 C9 O1 -162.6(5) 4 . . . ? Cu1 O2 C9 C1 17.2(9) 4 . . . ? C2 C1 C9 O1 -150.4(7) . . . . ? S1 C1 C9 O1 22.4(7) . . . . ? C2 C1 C9 O2 29.8(11) . . . . ? S1 C1 C9 O2 -157.4(5) . . . . ? Cu1 O4 C10 O3 163.2(7) 4 . . . ? Cu1 O4 C10 C2 -16.3(11) 4 . . . ? C1 C2 C10 O3 152.2(8) . . . . ? S2 C2 C10 O3 -20.8(9) . . . . ? C1 C2 C10 O4 -28.3(13) . . . . ? S2 C2 C10 O4 158.7(6) . . . . ? C15 N1 C11 C12 -0.5(10) . . . . ? Cu1 N1 C11 C12 179.5(5) . . . . ? N1 C11 C12 C13 0.3(12) . . . . ? C11 C12 C13 C14 -0.2(12) . . . . ? C12 C13 C14 C15 0.3(12) . . . . ? C11 N1 C15 C14 0.5(10) . . . . ? Cu1 N1 C15 C14 -179.5(5) . . . . ? C11 N1 C15 C20 178.6(6) . . . . ? Cu1 N1 C15 C20 -1.4(7) . . . . ? C13 C14 C15 N1 -0.4(11) . . . . ? C13 C14 C15 C20 -178.3(7) . . . . ? C20 N2 C16 C17 -0.4(11) . . . . ? Cu1 N2 C16 C17 178.8(6) . . . . ? N2 C16 C17 C18 -0.3(13) . . . . ? C16 C17 C18 C19 1.3(14) . . . . ? C17 C18 C19 C20 -1.7(15) . . . . ? C16 N2 C20 C19 0.0(11) . . . . ? Cu1 N2 C20 C19 -179.2(6) . . . . ? C16 N2 C20 C15 -178.4(6) . . . . ? Cu1 N2 C20 C15 2.3(8) . . . . ? C18 C19 C20 N2 1.0(13) . . . . ? C18 C19 C20 C15 179.3(8) . . . . ? N1 C15 C20 N2 -0.6(9) . . . . ? C14 C15 C20 N2 177.4(6) . . . . ? N1 C15 C20 C19 -179.0(7) . . . . ? C14 C15 C20 C19 -1.0(12) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.010 _refine_diff_density_min -1.964 _refine_diff_density_rms 0.114 ########End data_2 _database_code_depnum_ccdc_archive 'CCDC 772445' #TrackingRef '1-4-revised.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H14 Mn N2 O4 S6' _chemical_formula_weight 593.63 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.153(4) _cell_length_b 10.4726(19) _cell_length_c 16.681(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.026(5) _cell_angle_gamma 90.00 _cell_volume 4621.3(14) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 11208 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_absorpt_coefficient_mu 1.146 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.848 _exptl_absorpt_correction_T_max 0.872 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12955 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5237 _reflns_number_gt 4213 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5237 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 Mn1 Mn 0.515865(14) -0.14257(3) 0.40058(2) 0.02208(11) Uani 1 1 d . . . S1 S 0.35269(3) 0.09793(6) 0.18197(4) 0.02866(16) Uani 1 1 d . . . S2 S 0.36529(3) 0.22978(6) 0.34081(4) 0.02842(16) Uani 1 1 d . . . S3 S 0.27349(3) 0.32163(6) 0.09682(4) 0.03031(16) Uani 1 1 d . . . S4 S 0.29393(3) 0.46149(6) 0.25317(4) 0.03061(17) Uani 1 1 d . . . S5 S 0.24936(3) 0.55504(8) -0.00817(4) 0.0415(2) Uani 1 1 d . . . S6 S 0.27403(3) 0.71947(7) 0.16983(5) 0.0406(2) Uani 1 1 d . . . O1 O 0.42683(6) -0.07475(17) 0.15888(10) 0.0281(4) Uani 1 1 d . . . O2 O 0.45565(7) -0.13645(15) 0.28940(10) 0.0286(4) Uani 1 1 d . . . O3 O 0.43663(7) 0.14346(16) 0.47512(10) 0.0300(4) Uani 1 1 d . . . O4 O 0.49151(7) 0.04910(15) 0.41165(10) 0.0277(4) Uani 1 1 d . . . N1 N 0.45572(8) -0.25893(19) 0.44394(12) 0.0271(5) Uani 1 1 d . . . N2 N 0.52970(9) -0.3511(2) 0.37750(13) 0.0307(5) Uani 1 1 d . . . C1 C 0.40420(9) 0.0504(2) 0.26107(14) 0.0224(5) Uani 1 1 d . . . C2 C 0.41038(9) 0.1125(2) 0.33343(14) 0.0223(5) Uani 1 1 d . . . C3 C 0.33672(9) 0.2297(2) 0.23591(14) 0.0238(5) Uani 1 1 d . . . C4 C 0.30554(10) 0.3227(2) 0.20078(15) 0.0256(6) Uani 1 1 d . . . C5 C 0.27010(10) 0.4896(2) 0.09076(15) 0.0294(6) Uani 1 1 d . . . C6 C 0.28042(10) 0.5546(2) 0.16216(15) 0.0291(6) Uani 1 1 d . . . C7 C 0.18606(11) 0.6055(3) -0.00544(18) 0.0428(8) Uani 1 1 d . . . H7A H 0.1687 0.5365 0.0155 0.064 Uiso 1 1 calc R . . H7B H 0.1677 0.6277 -0.0606 0.064 Uiso 1 1 calc R . . H7C H 0.1878 0.6793 0.0302 0.064 Uiso 1 1 calc R . . C8 C 0.32042(12) 0.7587(3) 0.2618(2) 0.0464(8) Uani 1 1 d . . . H8A H 0.3101 0.7235 0.3093 0.070 Uiso 1 1 calc R . . H8B H 0.3233 0.8508 0.2673 0.070 Uiso 1 1 calc R . . H8C H 0.3529 0.7230 0.2585 0.070 Uiso 1 1 calc R . . C9 C 0.43215(9) -0.0624(2) 0.23588(15) 0.0238(5) Uani 1 1 d . . . C10 C 0.44978(10) 0.0980(2) 0.41274(14) 0.0233(5) Uani 1 1 d . . . C11 C 0.41836(10) -0.2070(3) 0.47346(16) 0.0338(6) Uani 1 1 d . . . H11 H 0.4210 -0.1205 0.4888 0.041 Uiso 1 1 calc R . . C12 C 0.37638(12) -0.2738(3) 0.48240(18) 0.0446(8) Uani 1 1 d . . . H12 H 0.3507 -0.2339 0.5028 0.053 Uiso 1 1 calc R . . C13 C 0.37308(13) -0.4005(3) 0.46063(19) 0.0528(9) Uani 1 1 d . . . H13 H 0.3448 -0.4489 0.4659 0.063 Uiso 1 1 calc R . . C14 C 0.41110(12) -0.4563(3) 0.43117(19) 0.0460(8) Uani 1 1 d . . . H14 H 0.4091 -0.5431 0.4164 0.055 Uiso 1 1 calc R . . C15 C 0.45262(10) -0.3839(2) 0.42318(15) 0.0301(6) Uani 1 1 d . . . C16 C 0.56872(12) -0.3933(3) 0.34840(18) 0.0415(7) Uani 1 1 d . . . H16 H 0.5927 -0.3338 0.3390 0.050 Uiso 1 1 calc R . . C17 C 0.57546(14) -0.5207(3) 0.3315(2) 0.0512(9) Uani 1 1 d . . . H17 H 0.6031 -0.5473 0.3105 0.061 Uiso 1 1 calc R . . C18 C 0.54045(14) -0.6074(3) 0.34636(19) 0.0514(9) Uani 1 1 d . . . H18 H 0.5441 -0.6947 0.3361 0.062 Uiso 1 1 calc R . . C19 C 0.50049(13) -0.5661(3) 0.37598(18) 0.0435(8) Uani 1 1 d . . . H19 H 0.4765 -0.6248 0.3863 0.052 Uiso 1 1 calc R . . C20 C 0.49524(11) -0.4363(2) 0.39100(15) 0.0304(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0251(2) 0.02208(19) 0.01895(19) 0.00167(15) 0.00465(16) 0.00079(16) S1 0.0342(4) 0.0277(3) 0.0201(3) -0.0028(3) -0.0023(3) 0.0083(3) S2 0.0355(4) 0.0278(3) 0.0196(3) -0.0019(3) 0.0014(3) 0.0097(3) S3 0.0343(4) 0.0320(4) 0.0216(3) -0.0004(3) -0.0001(3) 0.0083(3) S4 0.0430(4) 0.0258(3) 0.0218(3) 0.0014(3) 0.0050(3) 0.0081(3) S5 0.0483(5) 0.0516(5) 0.0244(3) 0.0112(3) 0.0077(3) 0.0221(4) S6 0.0565(5) 0.0269(4) 0.0355(4) 0.0040(3) 0.0040(4) 0.0106(3) O1 0.0295(10) 0.0379(10) 0.0165(8) -0.0032(8) 0.0044(7) 0.0067(8) O2 0.0348(10) 0.0240(9) 0.0235(9) 0.0004(8) -0.0009(8) 0.0062(8) O3 0.0350(10) 0.0348(10) 0.0187(9) -0.0014(8) 0.0033(8) 0.0071(8) O4 0.0292(10) 0.0257(9) 0.0258(9) -0.0030(8) 0.0008(8) 0.0039(8) N1 0.0271(12) 0.0289(11) 0.0250(11) 0.0042(9) 0.0056(9) -0.0020(9) N2 0.0345(13) 0.0288(12) 0.0295(12) 0.0023(10) 0.0087(10) 0.0042(10) C1 0.0219(12) 0.0245(12) 0.0196(12) 0.0020(10) 0.0018(10) 0.0023(10) C2 0.0267(13) 0.0194(12) 0.0207(12) 0.0027(10) 0.0052(10) 0.0041(10) C3 0.0285(14) 0.0228(12) 0.0186(11) 0.0003(10) 0.0022(10) 0.0017(11) C4 0.0307(14) 0.0260(13) 0.0195(12) -0.0004(10) 0.0043(11) 0.0019(11) C5 0.0329(14) 0.0306(14) 0.0240(13) 0.0067(11) 0.0051(11) 0.0105(12) C6 0.0324(14) 0.0272(13) 0.0269(13) 0.0055(11) 0.0052(11) 0.0074(12) C7 0.0388(17) 0.0508(19) 0.0355(16) 0.0007(14) 0.0018(14) 0.0116(14) C8 0.0401(18) 0.0365(16) 0.058(2) -0.0083(15) 0.0016(16) -0.0002(14) C9 0.0208(12) 0.0243(13) 0.0260(13) -0.0041(11) 0.0045(11) -0.0012(10) C10 0.0294(14) 0.0178(12) 0.0216(12) 0.0022(10) 0.0035(11) 0.0000(10) C11 0.0303(15) 0.0434(16) 0.0282(14) 0.0020(12) 0.0079(12) -0.0018(13) C12 0.0326(16) 0.066(2) 0.0367(16) -0.0006(16) 0.0120(13) -0.0065(16) C13 0.0425(19) 0.072(2) 0.0459(19) -0.0073(18) 0.0138(16) -0.0275(18) C14 0.052(2) 0.0437(18) 0.0428(17) -0.0090(14) 0.0120(16) -0.0239(16) C15 0.0365(15) 0.0311(14) 0.0211(13) 0.0018(11) 0.0028(12) -0.0088(12) C16 0.0423(17) 0.0406(17) 0.0454(18) 0.0043(14) 0.0180(15) 0.0093(14) C17 0.058(2) 0.0473(19) 0.0494(19) -0.0048(16) 0.0150(17) 0.0237(17) C18 0.071(2) 0.0319(16) 0.0454(19) -0.0096(14) -0.0004(18) 0.0151(17) C19 0.054(2) 0.0270(14) 0.0436(17) -0.0014(13) -0.0006(16) -0.0037(14) C20 0.0388(16) 0.0284(13) 0.0210(13) 0.0021(11) 0.0004(12) -0.0016(12) _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 Mn1 O4 2.1344(17) . ? Mn1 O1 2.1458(18) 2_655 ? Mn1 O2 2.1794(17) . ? Mn1 O3 2.1812(17) 5_656 ? Mn1 N2 2.263(2) . ? Mn1 N1 2.282(2) . ? S1 C3 1.754(2) . ? S1 C1 1.764(2) . ? S2 C3 1.747(2) . ? S2 C2 1.758(2) . ? S3 C4 1.756(2) . ? S3 C5 1.763(3) . ? S4 C4 1.761(3) . ? S4 C6 1.772(3) . ? S5 C5 1.758(2) . ? S5 C7 1.808(3) . ? S6 C6 1.743(3) . ? S6 C8 1.800(3) . ? O1 C9 1.266(3) . ? O1 Mn1 2.1458(18) 2_655 ? O2 C9 1.244(3) . ? O3 C10 1.267(3) . ? O3 Mn1 2.1812(17) 5_656 ? O4 C10 1.247(3) . ? N1 C11 1.339(3) . ? N1 C15 1.351(3) . ? N2 C16 1.336(4) . ? N2 C20 1.348(3) . ? C1 C2 1.348(3) . ? C1 C9 1.514(3) . ? C2 C10 1.510(3) . ? C3 C4 1.336(3) . ? C5 C6 1.345(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C11 C12 1.374(4) . ? C11 H11 0.9400 . ? C12 C13 1.374(4) . ? C12 H12 0.9400 . ? C13 C14 1.370(5) . ? C13 H13 0.9400 . ? C14 C15 1.390(4) . ? C14 H14 0.9400 . ? C15 C20 1.486(4) . ? C16 C17 1.384(4) . ? C16 H16 0.9400 . ? C17 C18 1.376(5) . ? C17 H17 0.9400 . ? C18 C19 1.360(5) . ? C18 H18 0.9400 . ? C19 C20 1.395(4) . ? C19 H19 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn1 O1 89.99(7) . 2_655 ? O4 Mn1 O2 81.86(6) . . ? O1 Mn1 O2 94.59(7) 2_655 . ? O4 Mn1 O3 92.88(6) . 5_656 ? O1 Mn1 O3 96.07(7) 2_655 5_656 ? O2 Mn1 O3 168.11(7) . 5_656 ? O4 Mn1 N2 171.33(7) . . ? O1 Mn1 N2 94.32(8) 2_655 . ? O2 Mn1 N2 90.29(7) . . ? O3 Mn1 N2 94.15(7) 5_656 . ? O4 Mn1 N1 102.53(7) . . ? O1 Mn1 N1 165.58(7) 2_655 . ? O2 Mn1 N1 80.34(7) . . ? O3 Mn1 N1 90.49(7) 5_656 . ? N2 Mn1 N1 72.34(8) . . ? C3 S1 C1 94.85(11) . . ? C3 S2 C2 95.09(11) . . ? C4 S3 C5 93.34(12) . . ? C4 S4 C6 93.13(12) . . ? C5 S5 C7 101.26(13) . . ? C6 S6 C8 103.10(13) . . ? C9 O1 Mn1 125.01(15) . 2_655 ? C9 O2 Mn1 142.54(16) . . ? C10 O3 Mn1 124.30(16) . 5_656 ? C10 O4 Mn1 133.46(16) . . ? C11 N1 C15 118.6(2) . . ? C11 N1 Mn1 123.73(18) . . ? C15 N1 Mn1 116.34(17) . . ? C16 N2 C20 118.6(2) . . ? C16 N2 Mn1 123.82(19) . . ? C20 N2 Mn1 117.53(18) . . ? C2 C1 C9 131.0(2) . . ? C2 C1 S1 116.80(19) . . ? C9 C1 S1 112.04(16) . . ? C1 C2 C10 131.0(2) . . ? C1 C2 S2 116.86(18) . . ? C10 C2 S2 112.08(17) . . ? C4 C3 S2 122.25(19) . . ? C4 C3 S1 123.63(19) . . ? S2 C3 S1 114.12(13) . . ? C3 C4 S3 123.55(19) . . ? C3 C4 S4 123.41(19) . . ? S3 C4 S4 113.01(14) . . ? C6 C5 S5 126.4(2) . . ? C6 C5 S3 117.14(19) . . ? S5 C5 S3 116.37(15) . . ? C5 C6 S6 124.2(2) . . ? C5 C6 S4 116.2(2) . . ? S6 C6 S4 119.15(15) . . ? S5 C7 H7A 109.5 . . ? S5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? S5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? S6 C8 H8A 109.5 . . ? S6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 O1 125.9(2) . . ? O2 C9 C1 119.7(2) . . ? O1 C9 C1 114.3(2) . . ? O4 C10 O3 126.3(2) . . ? O4 C10 C2 119.7(2) . . ? O3 C10 C2 114.0(2) . . ? N1 C11 C12 123.3(3) . . ? N1 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C11 C12 C13 118.0(3) . . ? C11 C12 H12 121.0 . . ? C13 C12 H12 121.0 . . ? C14 C13 C12 119.8(3) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 119.7(3) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? N1 C15 C14 120.6(3) . . ? N1 C15 C20 116.2(2) . . ? C14 C15 C20 123.2(3) . . ? N2 C16 C17 123.0(3) . . ? N2 C16 H16 118.5 . . ? C17 C16 H16 118.5 . . ? C18 C17 C16 118.1(3) . . ? C18 C17 H17 121.0 . . ? C16 C17 H17 121.0 . . ? C19 C18 C17 119.7(3) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 119.8(3) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? N2 C20 C19 120.8(3) . . ? N2 C20 C15 116.2(2) . . ? C19 C20 C15 123.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Mn1 O2 C9 28.3(3) . . . . ? O1 Mn1 O2 C9 -61.1(3) 2_655 . . . ? O3 Mn1 O2 C9 92.6(4) 5_656 . . . ? N2 Mn1 O2 C9 -155.4(3) . . . . ? N1 Mn1 O2 C9 132.6(3) . . . . ? O1 Mn1 O4 C10 149.7(2) 2_655 . . . ? O2 Mn1 O4 C10 55.0(2) . . . . ? O3 Mn1 O4 C10 -114.3(2) 5_656 . . . ? N2 Mn1 O4 C10 29.8(6) . . . . ? N1 Mn1 O4 C10 -23.1(2) . . . . ? O4 Mn1 N1 C11 -4.3(2) . . . . ? O1 Mn1 N1 C11 -154.0(2) 2_655 . . . ? O2 Mn1 N1 C11 -83.62(19) . . . . ? O3 Mn1 N1 C11 88.77(19) 5_656 . . . ? N2 Mn1 N1 C11 -177.0(2) . . . . ? O4 Mn1 N1 C15 162.40(17) . . . . ? O1 Mn1 N1 C15 12.7(4) 2_655 . . . ? O2 Mn1 N1 C15 83.06(17) . . . . ? O3 Mn1 N1 C15 -104.54(17) 5_656 . . . ? N2 Mn1 N1 C15 -10.35(17) . . . . ? O4 Mn1 N2 C16 129.1(5) . . . . ? O1 Mn1 N2 C16 9.5(2) 2_655 . . . ? O2 Mn1 N2 C16 104.1(2) . . . . ? O3 Mn1 N2 C16 -87.0(2) 5_656 . . . ? N1 Mn1 N2 C16 -176.2(2) . . . . ? O4 Mn1 N2 C20 -48.2(6) . . . . ? O1 Mn1 N2 C20 -167.81(18) 2_655 . . . ? O2 Mn1 N2 C20 -73.19(18) . . . . ? O3 Mn1 N2 C20 95.77(18) 5_656 . . . ? N1 Mn1 N2 C20 6.58(17) . . . . ? C3 S1 C1 C2 7.5(2) . . . . ? C3 S1 C1 C9 -176.37(18) . . . . ? C9 C1 C2 C10 5.3(5) . . . . ? S1 C1 C2 C10 -179.4(2) . . . . ? C9 C1 C2 S2 -173.4(2) . . . . ? S1 C1 C2 S2 1.8(3) . . . . ? C3 S2 C2 C1 -10.2(2) . . . . ? C3 S2 C2 C10 170.85(18) . . . . ? C2 S2 C3 C4 -165.0(2) . . . . ? C2 S2 C3 S1 14.97(16) . . . . ? C1 S1 C3 C4 165.8(2) . . . . ? C1 S1 C3 S2 -14.20(16) . . . . ? S2 C3 C4 S3 -176.45(14) . . . . ? S1 C3 C4 S3 3.6(4) . . . . ? S2 C3 C4 S4 5.7(4) . . . . ? S1 C3 C4 S4 -174.28(15) . . . . ? C5 S3 C4 C3 -152.8(2) . . . . ? C5 S3 C4 S4 25.28(17) . . . . ? C6 S4 C4 C3 151.9(2) . . . . ? C6 S4 C4 S3 -26.16(16) . . . . ? C7 S5 C5 C6 -69.5(3) . . . . ? C7 S5 C5 S3 105.91(18) . . . . ? C4 S3 C5 C6 -14.0(2) . . . . ? C4 S3 C5 S5 170.11(17) . . . . ? S5 C5 C6 S6 1.0(4) . . . . ? S3 C5 C6 S6 -174.38(16) . . . . ? S5 C5 C6 S4 173.26(16) . . . . ? S3 C5 C6 S4 -2.1(3) . . . . ? C8 S6 C6 C5 -151.7(3) . . . . ? C8 S6 C6 S4 36.3(2) . . . . ? C4 S4 C6 C5 17.1(2) . . . . ? C4 S4 C6 S6 -170.30(17) . . . . ? Mn1 O2 C9 O1 125.6(3) . . . . ? Mn1 O2 C9 C1 -58.1(4) . . . . ? Mn1 O1 C9 O2 -38.5(3) 2_655 . . . ? Mn1 O1 C9 C1 145.03(17) 2_655 . . . ? C2 C1 C9 O2 22.3(4) . . . . ? S1 C1 C9 O2 -153.1(2) . . . . ? C2 C1 C9 O1 -161.0(3) . . . . ? S1 C1 C9 O1 23.6(3) . . . . ? Mn1 O4 C10 O3 106.7(3) . . . . ? Mn1 O4 C10 C2 -76.3(3) . . . . ? Mn1 O3 C10 O4 -1.8(4) 5_656 . . . ? Mn1 O3 C10 C2 -178.98(14) 5_656 . . . ? C1 C2 C10 O4 22.3(4) . . . . ? S2 C2 C10 O4 -158.90(19) . . . . ? C1 C2 C10 O3 -160.3(3) . . . . ? S2 C2 C10 O3 18.5(3) . . . . ? C15 N1 C11 C12 -1.2(4) . . . . ? Mn1 N1 C11 C12 165.2(2) . . . . ? N1 C11 C12 C13 0.7(4) . . . . ? C11 C12 C13 C14 0.1(5) . . . . ? C12 C13 C14 C15 -0.3(5) . . . . ? C11 N1 C15 C14 1.0(4) . . . . ? Mn1 N1 C15 C14 -166.4(2) . . . . ? C11 N1 C15 C20 -179.8(2) . . . . ? Mn1 N1 C15 C20 12.8(3) . . . . ? C13 C14 C15 N1 -0.2(4) . . . . ? C13 C14 C15 C20 -179.4(3) . . . . ? C20 N2 C16 C17 -0.1(4) . . . . ? Mn1 N2 C16 C17 -177.3(2) . . . . ? N2 C16 C17 C18 -0.7(5) . . . . ? C16 C17 C18 C19 0.7(5) . . . . ? C17 C18 C19 C20 0.1(5) . . . . ? C16 N2 C20 C19 0.8(4) . . . . ? Mn1 N2 C20 C19 178.24(19) . . . . ? C16 N2 C20 C15 -179.9(2) . . . . ? Mn1 N2 C20 C15 -2.5(3) . . . . ? C18 C19 C20 N2 -0.8(4) . . . . ? C18 C19 C20 C15 179.9(3) . . . . ? N1 C15 C20 N2 -6.9(3) . . . . ? C14 C15 C20 N2 172.2(3) . . . . ? N1 C15 C20 C19 172.4(2) . . . . ? C14 C15 C20 C19 -8.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.347 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.073 ########End data_3 _database_code_depnum_ccdc_archive 'CCDC 772446' #TrackingRef '1-4-revised.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H19 Mn N3 O5 S6' _chemical_formula_weight 652.70 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2322(7) _cell_length_b 11.9875(8) _cell_length_c 12.0255(9) _cell_angle_alpha 78.587(5) _cell_angle_beta 81.446(5) _cell_angle_gamma 73.947(4) _cell_volume 1382.55(17) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6143 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 666 _exptl_absorpt_coefficient_mu 0.969 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.565 _exptl_absorpt_correction_T_max 0.785 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12630 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6207 _reflns_number_gt 4825 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The disorder atoms were split into two positions. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6207 _refine_ls_number_parameters 418 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1654 _refine_ls_wR_factor_gt 0.1524 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.008 _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 Mn1 Mn 0.23159(4) -0.00331(3) 0.52116(4) 0.03318(16) Uani 1 1 d . . . S1 S -0.06242(7) 0.29261(7) 0.22060(8) 0.0482(2) Uani 1 1 d . A . S2 S 0.21827(8) 0.31704(7) 0.16300(8) 0.0512(2) Uani 1 1 d . A . S3 S -0.1883(7) 0.5666(5) 0.1646(6) 0.0523(9) Uani 0.590(3) 1 d P A 1 S3' S -0.1655(10) 0.5903(8) 0.1582(10) 0.066(2) Uani 0.410(3) 1 d PD A 2 S4 S 0.0874(8) 0.6042(10) 0.1095(11) 0.0620(12) Uani 0.590(3) 1 d P A 1 S4' S 0.1214(11) 0.5968(14) 0.0938(15) 0.0604(17) Uani 0.410(3) 1 d PD A 2 S5 S -0.3254(2) 0.81462(15) 0.19012(16) 0.0621(6) Uani 0.590(3) 1 d P A 1 S5' S -0.2579(4) 0.8616(3) 0.1192(3) 0.0890(13) Uani 0.410(3) 1 d P A 2 S6 S -0.0204(3) 0.86811(19) 0.1136(4) 0.1237(15) Uani 0.590(3) 1 d P A 1 S6' S 0.0562(4) 0.8557(2) 0.0307(3) 0.0739(10) Uani 0.410(3) 1 d P A 2 O1 O -0.10178(19) 0.07687(17) 0.34319(17) 0.0388(5) Uani 1 1 d . . . O2 O 0.1076(2) -0.01128(16) 0.39591(18) 0.0381(5) Uani 1 1 d . . . O3 O 0.4151(3) 0.0785(4) 0.1906(3) 0.1197(16) Uani 1 1 d . . . O4 O 0.3580(2) 0.05793(19) 0.37568(19) 0.0451(5) Uani 1 1 d . . . O5 O 0.3691(2) -0.0034(2) 0.6407(2) 0.0559(6) Uani 1 1 d . . . N1 N 0.1356(2) 0.1904(2) 0.5358(2) 0.0402(6) Uani 1 1 d . . . N2 N 0.3513(2) -0.1951(2) 0.5078(2) 0.0382(5) Uani 1 1 d . . . C1 C 0.0701(3) 0.1747(2) 0.2746(2) 0.0357(6) Uani 1 1 d . . . C2 C 0.1975(3) 0.1853(2) 0.2480(3) 0.0386(6) Uani 1 1 d . . . C3 C 0.0439(3) 0.3889(3) 0.1760(3) 0.0428(7) Uani 1 1 d . . . C4 C -0.0144(12) 0.5054(13) 0.1439(12) 0.035(2) Uani 0.590(3) 1 d P A 1 C4' C 0.0105(15) 0.508(2) 0.1620(19) 0.039(4) Uani 0.410(3) 1 d PD A 2 C5 C -0.1705(9) 0.7090(6) 0.1612(8) 0.0539(18) Uani 0.590(3) 1 d P A 1 C5' C -0.1249(18) 0.7321(10) 0.1187(13) 0.063(4) Uani 0.410(3) 1 d P A 2 C6 C -0.0458(12) 0.7273(8) 0.1356(11) 0.063(2) Uani 0.590(3) 1 d P A 1 C6' C -0.0007(17) 0.7300(11) 0.0863(11) 0.061(3) Uani 0.410(3) 1 d P A 2 C7 C -0.3582(12) 0.8884(11) 0.0519(8) 0.115(4) Uani 0.590(3) 1 d P A 1 H7A H -0.2995 0.9416 0.0263 0.172 Uiso 0.590(3) 1 calc PR A 1 H7B H -0.4531 0.9329 0.0524 0.172 Uiso 0.590(3) 1 calc PR A 1 H7C H -0.3400 0.8315 0.0008 0.172 Uiso 0.590(3) 1 calc PR A 1 C7' C -0.4109(15) 0.8204(12) 0.1090(14) 0.102(5) Uani 0.410(3) 1 d P A 2 H7'1 H -0.4034 0.7921 0.0376 0.153 Uiso 0.410(3) 1 calc PR A 2 H7'2 H -0.4887 0.8883 0.1118 0.153 Uiso 0.410(3) 1 calc PR A 2 H7'3 H -0.4235 0.7587 0.1721 0.153 Uiso 0.410(3) 1 calc PR A 2 C8 C 0.122(3) 0.880(2) 0.144(2) 0.146(9) Uani 0.590(3) 1 d P A 1 H8A H 0.1436 0.8303 0.2164 0.220 Uiso 0.590(3) 1 calc PR A 1 H8B H 0.1145 0.9608 0.1487 0.220 Uiso 0.590(3) 1 calc PR A 1 H8C H 0.1933 0.8543 0.0847 0.220 Uiso 0.590(3) 1 calc PR A 1 C8' C 0.131(4) 0.851(2) 0.168(2) 0.097(8) Uani 0.410(3) 1 d P A 2 H8'1 H 0.0571 0.8739 0.2260 0.145 Uiso 0.410(3) 1 calc PR A 2 H8'2 H 0.1888 0.9049 0.1540 0.145 Uiso 0.410(3) 1 calc PR A 2 H8'3 H 0.1841 0.7718 0.1927 0.145 Uiso 0.410(3) 1 calc PR A 2 C9 C 0.0221(3) 0.0721(2) 0.3429(2) 0.0347(6) Uani 1 1 d . . . C10 C 0.3334(3) 0.0975(3) 0.2737(3) 0.0492(8) Uani 1 1 d . . . C11 C 0.0028(3) 0.2396(3) 0.5407(3) 0.0538(9) Uani 1 1 d . . . H11 H -0.0567 0.1899 0.5544 0.065 Uiso 1 1 calc R . . C12 C -0.0535(3) 0.3590(3) 0.5267(4) 0.0610(10) Uani 1 1 d . . . H12 H -0.1489 0.3887 0.5299 0.073 Uiso 1 1 calc R . . C13 C 0.0288(3) 0.4355(2) 0.5083(3) 0.0373(6) Uani 1 1 d . . . C14 C 0.1669(4) 0.3846(3) 0.5049(5) 0.0751(14) Uani 1 1 d . . . H14 H 0.2285 0.4322 0.4931 0.090 Uiso 1 1 calc R . . C15 C 0.2153(4) 0.2637(3) 0.5186(4) 0.0719(13) Uani 1 1 d . . . H15 H 0.3104 0.2315 0.5156 0.086 Uiso 1 1 calc R . . C16 C 0.3778(4) -0.2741(3) 0.6022(3) 0.0566(9) Uani 1 1 d . . . H16 H 0.3550 -0.2471 0.6726 0.068 Uiso 1 1 calc R . . C17 C 0.4365(4) -0.3928(3) 0.6033(3) 0.0524(8) Uani 1 1 d . . . H17 H 0.4539 -0.4437 0.6727 0.063 Uiso 1 1 calc R . . C18 C 0.4697(3) -0.4368(2) 0.5013(2) 0.0338(6) Uani 1 1 d . . . C19 C 0.4420(4) -0.3542(3) 0.4036(3) 0.0498(8) Uani 1 1 d . . . H19 H 0.4630 -0.3783 0.3318 0.060 Uiso 1 1 calc R . . C20 C 0.3840(4) -0.2375(3) 0.4107(3) 0.0499(8) Uani 1 1 d . . . H20 H 0.3665 -0.1845 0.3425 0.060 Uiso 1 1 calc R . . C21 C 0.3986(11) 0.7175(10) -0.0865(9) 0.103(3) Uiso 0.590(3) 1 d PD A 1 C22 C 0.4312(13) 0.6640(11) 0.0307(9) 0.115(4) Uiso 0.590(3) 1 d PD A 1 N3 N 0.4601(7) 0.6206(8) 0.1181(6) 0.0784(19) Uiso 0.590(3) 1 d PD A 1 C21' C 0.4172(12) 0.6397(11) -0.1033(9) 0.075(3) Uiso 0.410(3) 1 d PD A 2 C22' C 0.4546(13) 0.5949(13) 0.0303(9) 0.082(3) Uiso 0.410(3) 1 d PD A 2 N3' N 0.4711(11) 0.5591(11) 0.1288(9) 0.082(3) Uiso 0.410(3) 1 d PD A 2 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 Mn1 0.0259(2) 0.0169(2) 0.0540(3) -0.00324(18) -0.00601(19) -0.00179(17) S1 0.0325(4) 0.0312(4) 0.0729(5) 0.0156(4) -0.0150(4) -0.0070(3) S2 0.0340(4) 0.0318(4) 0.0759(6) 0.0111(4) 0.0002(4) -0.0061(3) S3 0.040(2) 0.0290(18) 0.079(2) 0.0010(15) -0.0050(15) -0.0017(10) S3' 0.042(3) 0.041(4) 0.090(2) 0.021(3) 0.006(2) 0.002(2) S4 0.053(3) 0.0327(15) 0.091(3) 0.0067(17) 0.009(2) -0.016(2) S4' 0.055(5) 0.030(3) 0.089(4) 0.007(2) 0.011(3) -0.019(4) S5 0.0696(11) 0.0373(9) 0.0681(11) -0.0153(8) -0.0054(9) 0.0087(8) S5' 0.101(2) 0.0375(15) 0.107(3) -0.0074(15) -0.012(2) 0.0147(15) S6 0.110(2) 0.0318(11) 0.225(4) -0.0062(16) -0.010(2) -0.0252(12) S6' 0.124(3) 0.0258(12) 0.0713(17) 0.0005(11) -0.0078(17) -0.0250(15) O1 0.0326(10) 0.0314(11) 0.0518(11) 0.0014(9) -0.0102(9) -0.0097(9) O2 0.0383(10) 0.0189(10) 0.0563(12) 0.0023(8) -0.0134(9) -0.0073(8) O3 0.068(2) 0.161(4) 0.073(2) -0.014(2) 0.0012(16) 0.057(2) O4 0.0282(10) 0.0362(12) 0.0610(13) 0.0092(10) -0.0056(9) -0.0034(9) O5 0.0339(11) 0.0560(15) 0.0803(16) -0.0256(13) -0.0143(11) -0.0011(11) N1 0.0356(13) 0.0190(12) 0.0650(16) -0.0065(10) -0.0066(11) -0.0050(10) N2 0.0345(12) 0.0218(12) 0.0530(14) -0.0035(10) -0.0062(10) 0.0006(10) C1 0.0316(14) 0.0210(13) 0.0498(15) 0.0026(11) -0.0081(12) -0.0027(11) C2 0.0345(14) 0.0246(14) 0.0504(16) 0.0021(12) -0.0044(12) -0.0031(12) C3 0.0345(15) 0.0278(16) 0.0586(18) 0.0070(13) -0.0067(13) -0.0045(13) C4 0.036(5) 0.023(3) 0.049(5) 0.006(3) -0.020(4) -0.013(4) C4' 0.023(6) 0.042(6) 0.053(7) -0.013(5) -0.022(5) 0.002(5) C5 0.060(5) 0.026(4) 0.069(5) 0.000(3) -0.012(4) -0.004(3) C5' 0.076(11) 0.016(5) 0.067(8) 0.010(4) 0.011(7) 0.014(6) C6 0.062(7) 0.024(4) 0.091(8) 0.002(4) -0.006(6) 0.000(4) C6' 0.083(10) 0.032(5) 0.061(7) -0.003(5) 0.012(5) -0.020(6) C7 0.106(8) 0.153(11) 0.069(5) -0.030(6) -0.020(5) 0.007(8) C7' 0.104(11) 0.062(8) 0.114(11) -0.015(7) 0.019(9) 0.007(7) C8 0.19(2) 0.16(2) 0.101(11) 0.023(11) -0.017(11) -0.088(17) C8' 0.17(2) 0.076(10) 0.086(13) -0.016(11) -0.004(12) -0.098(14) C9 0.0350(14) 0.0231(14) 0.0452(15) -0.0043(11) -0.0057(12) -0.0061(11) C10 0.0301(15) 0.0410(19) 0.065(2) -0.0025(15) -0.0014(14) 0.0037(13) C11 0.0358(16) 0.0205(15) 0.102(3) -0.0113(16) 0.0079(17) -0.0081(13) C12 0.0316(16) 0.0226(16) 0.120(3) -0.0093(18) 0.0071(18) -0.0018(13) C13 0.0340(14) 0.0191(14) 0.0584(17) -0.0081(12) -0.0056(13) -0.0044(11) C14 0.0375(18) 0.0231(17) 0.167(5) -0.014(2) -0.017(2) -0.0095(15) C15 0.0369(18) 0.0196(16) 0.158(4) -0.015(2) -0.021(2) 0.0008(14) C16 0.077(2) 0.0283(17) 0.0487(17) -0.0051(14) -0.0096(17) 0.0129(16) C17 0.073(2) 0.0258(16) 0.0430(16) -0.0023(12) -0.0079(16) 0.0108(15) C18 0.0261(12) 0.0220(14) 0.0476(15) -0.0031(11) -0.0014(11) 0.0002(11) C19 0.070(2) 0.0246(16) 0.0435(16) -0.0031(12) -0.0040(15) 0.0036(15) C20 0.066(2) 0.0273(16) 0.0447(16) 0.0007(12) -0.0055(15) 0.0016(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 Mn1 O2 2.1403(19) . ? Mn1 O4 2.148(2) . ? Mn1 O1 2.153(2) 2_556 ? Mn1 O5 2.156(2) . ? Mn1 N1 2.288(2) . ? Mn1 N2 2.311(2) . ? S1 C3 1.755(3) . ? S1 C1 1.759(3) . ? S2 C2 1.751(3) . ? S2 C3 1.752(3) . ? S3 C4 1.728(14) . ? S3 C5 1.758(9) . ? S3' C4' 1.802(19) . ? S3' C5' 1.816(17) . ? S4 C4 1.738(14) . ? S4 C6 1.754(14) . ? S4' C6' 1.73(2) . ? S4' C4' 1.777(19) . ? S5 C7 1.754(9) . ? S5 C5 1.771(9) . ? S5' C5' 1.759(13) . ? S5' C7' 1.794(17) . ? S6 C8 1.60(3) . ? S6 C6 1.741(10) . ? S6' C6' 1.739(12) . ? S6' C8' 1.90(2) . ? O1 C9 1.253(3) . ? O1 Mn1 2.153(2) 2_556 ? O2 C9 1.265(3) . ? O3 C10 1.218(5) . ? O4 C10 1.260(4) . ? N1 C11 1.321(4) . ? N1 C15 1.325(4) . ? N2 C20 1.325(4) . ? N2 C16 1.335(4) . ? C1 C2 1.330(4) . ? C1 C9 1.498(4) . ? C2 C10 1.526(4) . ? C3 C4 1.360(15) . ? C3 C4' 1.35(3) . ? C5 C6 1.336(14) . ? C5' C6' 1.27(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C7' H7'1 0.9700 . ? C7' H7'2 0.9700 . ? C7' H7'3 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C8' H8'1 0.9700 . ? C8' H8'2 0.9700 . ? C8' H8'3 0.9700 . ? C11 C12 1.374(4) . ? C11 H11 0.9400 . ? C12 C13 1.374(4) . ? C12 H12 0.9400 . ? C13 C14 1.374(4) . ? C13 C13 1.479(5) 2_566 ? C14 C15 1.380(5) . ? C14 H14 0.9400 . ? C15 H15 0.9400 . ? C16 C17 1.382(4) . ? C16 H16 0.9400 . ? C17 C18 1.389(4) . ? C17 H17 0.9400 . ? C18 C19 1.387(4) . ? C18 C18 1.476(5) 2_646 ? C19 C20 1.375(4) . ? C19 H19 0.9400 . ? C20 H20 0.9400 . ? C21 C22 1.474(11) . ? C22 N3 1.119(10) . ? C21' C22' 1.656(13) . ? C22' N3' 1.199(12) . ? 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 Mn1 O4 83.92(8) . . ? O2 Mn1 O1 91.50(7) . 2_556 ? O4 Mn1 O1 174.16(8) . 2_556 ? O2 Mn1 O5 175.75(8) . . ? O4 Mn1 O5 93.60(9) . . ? O1 Mn1 O5 90.74(9) 2_556 . ? O2 Mn1 N1 96.31(8) . . ? O4 Mn1 N1 86.88(9) . . ? O1 Mn1 N1 97.26(9) 2_556 . ? O5 Mn1 N1 86.98(9) . . ? O2 Mn1 N2 88.53(8) . . ? O4 Mn1 N2 89.69(9) . . ? O1 Mn1 N2 86.56(8) 2_556 . ? O5 Mn1 N2 88.00(9) . . ? N1 Mn1 N2 173.73(8) . . ? C3 S1 C1 93.73(13) . . ? C2 S2 C3 94.56(14) . . ? C4 S3 C5 94.0(6) . . ? C4' S3' C5' 94.3(9) . . ? C4 S4 C6 94.9(7) . . ? C6' S4' C4' 96.6(9) . . ? C7 S5 C5 100.9(5) . . ? C5' S5' C7' 105.9(8) . . ? C8 S6 C6 117.2(10) . . ? C6' S6' C8' 92.3(8) . . ? C9 O1 Mn1 127.35(17) . 2_556 ? C9 O2 Mn1 128.29(18) . . ? C10 O4 Mn1 130.97(19) . . ? C11 N1 C15 115.9(3) . . ? C11 N1 Mn1 123.88(19) . . ? C15 N1 Mn1 119.1(2) . . ? C20 N2 C16 115.6(3) . . ? C20 N2 Mn1 123.90(19) . . ? C16 N2 Mn1 120.1(2) . . ? C2 C1 C9 128.4(2) . . ? C2 C1 S1 117.6(2) . . ? C9 C1 S1 113.90(19) . . ? C1 C2 C10 130.5(3) . . ? C1 C2 S2 116.7(2) . . ? C10 C2 S2 112.7(2) . . ? C4' C3 C4 15.6(11) . . ? C4 C3 S2 127.3(5) . . ? C4' C3 S2 117.2(6) . . ? C4 C3 S1 118.8(5) . . ? C4' C3 S1 128.9(6) . . ? S2 C3 S1 113.55(16) . . ? C3 C4 S3 122.9(8) . . ? C3 C4 S4 119.7(9) . . ? S3 C4 S4 115.9(10) . . ? C3 C4' S4' 124.7(14) . . ? C3 C4' S3' 120.5(11) . . ? S4' C4' S3' 110.6(14) . . ? C6 C5 S3 118.3(7) . . ? C6 C5 S5 127.0(7) . . ? S3 C5 S5 114.7(6) . . ? C6' C5' S5' 124.2(12) . . ? C6' C5' S3' 116.4(10) . . ? S5' C5' S3' 119.3(10) . . ? C5 C6 S6 121.6(8) . . ? C5 C6 S4 116.0(8) . . ? S6 C6 S4 122.0(8) . . ? C5' C6' S4' 119.8(10) . . ? C5' C6' S6' 123.5(11) . . ? S4' C6' S6' 116.7(9) . . ? S5' C7' H7'1 109.5 . . ? S5' C7' H7'2 109.5 . . ? H7'1 C7' H7'2 109.5 . . ? S5' C7' H7'3 109.5 . . ? H7'1 C7' H7'3 109.5 . . ? H7'2 C7' H7'3 109.5 . . ? S6' C8' H8'1 109.5 . . ? S6' C8' H8'2 109.5 . . ? H8'1 C8' H8'2 109.5 . . ? S6' C8' H8'3 109.5 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? O1 C9 O2 125.2(2) . . ? O1 C9 C1 116.3(2) . . ? O2 C9 C1 118.5(2) . . ? O3 C10 O4 124.9(3) . . ? O3 C10 C2 115.1(3) . . ? O4 C10 C2 119.7(3) . . ? N1 C11 C12 123.9(3) . . ? N1 C11 H11 118.1 . . ? C12 C11 H11 118.1 . . ? C11 C12 C13 120.4(3) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 115.8(3) . . ? C14 C13 C13 122.5(3) . 2_566 ? C12 C13 C13 121.7(3) . 2_566 ? C13 C14 C15 120.1(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? N1 C15 C14 123.8(3) . . ? N1 C15 H15 118.1 . . ? C14 C15 H15 118.1 . . ? N2 C16 C17 124.4(3) . . ? N2 C16 H16 117.8 . . ? C17 C16 H16 117.8 . . ? C16 C17 C18 119.7(3) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C19 C18 C17 115.6(3) . . ? C19 C18 C18 122.9(3) . 2_646 ? C17 C18 C18 121.5(3) . 2_646 ? C20 C19 C18 120.6(3) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? N2 C20 C19 124.1(3) . . ? N2 C20 H20 117.9 . . ? C19 C20 H20 117.9 . . ? N3 C22 C21 177.4(14) . . ? N3' C22' C21' 174.1(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Mn1 O2 C9 -79.5(2) . . . . ? O1 Mn1 O2 C9 104.1(2) 2_556 . . . ? O5 Mn1 O2 C9 -134.0(11) . . . . ? N1 Mn1 O2 C9 6.7(2) . . . . ? N2 Mn1 O2 C9 -169.4(2) . . . . ? O2 Mn1 O4 C10 16.3(3) . . . . ? O1 Mn1 O4 C10 54.9(8) 2_556 . . . ? O5 Mn1 O4 C10 -167.1(3) . . . . ? N1 Mn1 O4 C10 -80.4(3) . . . . ? N2 Mn1 O4 C10 104.9(3) . . . . ? O2 Mn1 N1 C11 43.2(3) . . . . ? O4 Mn1 N1 C11 126.8(3) . . . . ? O1 Mn1 N1 C11 -49.1(3) 2_556 . . . ? O5 Mn1 N1 C11 -139.5(3) . . . . ? N2 Mn1 N1 C11 -176.3(7) . . . . ? O2 Mn1 N1 C15 -124.3(3) . . . . ? O4 Mn1 N1 C15 -40.8(3) . . . . ? O1 Mn1 N1 C15 143.4(3) 2_556 . . . ? O5 Mn1 N1 C15 53.0(3) . . . . ? N2 Mn1 N1 C15 16.1(10) . . . . ? O2 Mn1 N2 C20 39.0(3) . . . . ? O4 Mn1 N2 C20 -44.9(3) . . . . ? O1 Mn1 N2 C20 130.6(3) 2_556 . . . ? O5 Mn1 N2 C20 -138.5(3) . . . . ? N1 Mn1 N2 C20 -101.7(8) . . . . ? O2 Mn1 N2 C16 -133.1(3) . . . . ? O4 Mn1 N2 C16 143.0(3) . . . . ? O1 Mn1 N2 C16 -41.5(3) 2_556 . . . ? O5 Mn1 N2 C16 49.4(3) . . . . ? N1 Mn1 N2 C16 86.2(9) . . . . ? C3 S1 C1 C2 -12.0(3) . . . . ? C3 S1 C1 C9 170.0(2) . . . . ? C9 C1 C2 C10 2.4(6) . . . . ? S1 C1 C2 C10 -175.3(3) . . . . ? C9 C1 C2 S2 178.4(2) . . . . ? S1 C1 C2 S2 0.7(4) . . . . ? C3 S2 C2 C1 10.9(3) . . . . ? C3 S2 C2 C10 -172.3(3) . . . . ? C2 S2 C3 C4 169.1(9) . . . . ? C2 S2 C3 C4' 155.0(11) . . . . ? C2 S2 C3 S1 -18.7(2) . . . . ? C1 S1 C3 C4 -168.2(8) . . . . ? C1 S1 C3 C4' -154.0(12) . . . . ? C1 S1 C3 S2 18.9(2) . . . . ? C4' C3 C4 S3 -125(6) . . . . ? S2 C3 C4 S3 -178.3(6) . . . . ? S1 C3 C4 S3 9.8(15) . . . . ? C4' C3 C4 S4 41(4) . . . . ? S2 C3 C4 S4 -13.0(16) . . . . ? S1 C3 C4 S4 175.2(8) . . . . ? C5 S3 C4 C3 156.7(11) . . . . ? C5 S3 C4 S4 -9.2(11) . . . . ? C6 S4 C4 C3 -157.4(12) . . . . ? C6 S4 C4 S3 9.0(12) . . . . ? C4 S3 C5 C6 5.9(10) . . . . ? C4 S3 C5 S5 -175.4(7) . . . . ? C7 S5 C5 C6 77.1(10) . . . . ? C7 S5 C5 S3 -101.5(7) . . . . ? S3 C5 C6 S6 172.3(7) . . . . ? S5 C5 C6 S6 -6.2(15) . . . . ? S3 C5 C6 S4 -0.6(13) . . . . ? S5 C5 C6 S4 -179.2(8) . . . . ? C8 S6 C6 C5 150.7(14) . . . . ? C8 S6 C6 S4 -36.8(17) . . . . ? C4 S4 C6 C5 -4.9(13) . . . . ? C4 S4 C6 S6 -177.8(9) . . . . ? C4 C3 C4' S4' -115(6) . . . . ? S2 C3 C4' S4' 19(2) . . . . ? S1 C3 C4' S4' -168.8(11) . . . . ? C4 C3 C4' S3' 39(4) . . . . ? S2 C3 C4' S3' 173.2(10) . . . . ? S1 C3 C4' S3' -14(2) . . . . ? C6' S4' C4' C3 169.5(16) . . . . ? C6' S4' C4' S3' 12.8(17) . . . . ? C5' S3' C4' C3 -172.5(16) . . . . ? C5' S3' C4' S4' -14.7(15) . . . . ? C7' S5' C5' C6' 154.8(14) . . . . ? C7' S5' C5' S3' -21.2(13) . . . . ? C4' S3' C5' C6' 12.8(16) . . . . ? C4' S3' C5' S5' -170.9(11) . . . . ? S5' C5' C6' S4' 178.1(12) . . . . ? S3' C5' C6' S4' -5.8(19) . . . . ? S5' C5' C6' S6' -3(2) . . . . ? S3' C5' C6' S6' 172.9(10) . . . . ? C4' S4' C6' C5' -4.6(19) . . . . ? C4' S4' C6' S6' 176.6(11) . . . . ? C8' S6' C6' C5' 104.8(18) . . . . ? C8' S6' C6' S4' -76.4(16) . . . . ? Mn1 O1 C9 O2 30.9(4) 2_556 . . . ? Mn1 O1 C9 C1 -148.5(2) 2_556 . . . ? Mn1 O2 C9 O1 -122.4(3) . . . . ? Mn1 O2 C9 C1 57.0(3) . . . . ? C2 C1 C9 O1 -170.5(3) . . . . ? S1 C1 C9 O1 7.3(3) . . . . ? C2 C1 C9 O2 10.1(5) . . . . ? S1 C1 C9 O2 -172.1(2) . . . . ? Mn1 O4 C10 O3 -142.8(4) . . . . ? Mn1 O4 C10 C2 43.3(5) . . . . ? C1 C2 C10 O3 124.8(5) . . . . ? S2 C2 C10 O3 -51.3(5) . . . . ? C1 C2 C10 O4 -60.7(5) . . . . ? S2 C2 C10 O4 123.1(3) . . . . ? C15 N1 C11 C12 1.3(6) . . . . ? Mn1 N1 C11 C12 -166.6(3) . . . . ? N1 C11 C12 C13 -1.1(7) . . . . ? C11 C12 C13 C14 0.1(6) . . . . ? C11 C12 C13 C13 179.3(4) . . . 2_566 ? C12 C13 C14 C15 0.5(7) . . . . ? C13 C13 C14 C15 -178.7(5) 2_566 . . . ? C11 N1 C15 C14 -0.7(7) . . . . ? Mn1 N1 C15 C14 167.8(4) . . . . ? C13 C14 C15 N1 -0.2(8) . . . . ? C20 N2 C16 C17 0.6(5) . . . . ? Mn1 N2 C16 C17 173.4(3) . . . . ? N2 C16 C17 C18 -1.1(6) . . . . ? C16 C17 C18 C19 1.0(5) . . . . ? C16 C17 C18 C18 -178.9(4) . . . 2_646 ? C17 C18 C19 C20 -0.7(5) . . . . ? C18 C18 C19 C20 179.3(4) 2_646 . . . ? C16 N2 C20 C19 -0.2(5) . . . . ? Mn1 N2 C20 C19 -172.7(3) . . . . ? C18 C19 C20 N2 0.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.730 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.073 ########End data_4 _database_code_depnum_ccdc_archive 'CCDC 772447' #TrackingRef '1-4-revised.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H19 N3 O5 S6 Zn' _chemical_formula_weight 663.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1856(9) _cell_length_b 11.8627(9) _cell_length_c 12.0826(12) _cell_angle_alpha 78.587(9) _cell_angle_beta 80.800(9) _cell_angle_gamma 73.103(8) _cell_volume 1361.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6367 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 1.402 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.746 _exptl_absorpt_correction_T_max 0.810 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13106 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0746 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6104 _reflns_number_gt 4443 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The disorder atoms were split into two positions. ; _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^)+(0.0678P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6104 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1549 _refine_ls_wR_factor_gt 0.1393 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 0.23027(4) -0.00243(3) 0.52073(4) 0.0460(8) Uani 1 1 d . . . S1 S -0.06121(10) 0.28799(9) 0.21915(11) 0.0600(8) Uani 1 1 d . A . S2 S 0.22159(10) 0.31203(9) 0.16463(12) 0.0624(8) Uani 1 1 d . A . S3 S -0.18239(13) 0.57452(11) 0.15848(14) 0.0770(8) Uani 1 1 d . A . S4 S 0.10054(14) 0.60017(11) 0.10373(15) 0.0821(9) Uani 1 1 d . . . S5 S -0.3265(3) 0.8220(2) 0.1860(3) 0.0747(12) Uani 0.664(6) 1 d P A 1 S5' S -0.2679(7) 0.8631(5) 0.1209(7) 0.104(2) Uani 0.336(6) 1 d P A 2 S6 S -0.0159(4) 0.8698(2) 0.1144(6) 0.139(2) Uani 0.664(6) 1 d P A 1 S6' S 0.0494(8) 0.8575(4) 0.0351(5) 0.086(2) Uani 0.336(6) 1 d P A 2 O1 O -0.1006(2) 0.0717(2) 0.3471(2) 0.0485(10) Uani 1 1 d . . . O2 O 0.1103(2) -0.0150(2) 0.4027(2) 0.0482(10) Uani 1 1 d . . . O3 O 0.4279(19) 0.0910(14) 0.1941(16) 0.095(5) Uani 0.664(6) 1 d P A 1 O3' O 0.414(4) 0.052(3) 0.204(3) 0.083(9) Uani 0.336(6) 1 d P A 2 O4 O 0.3611(3) 0.0515(2) 0.3812(3) 0.0524(10) Uani 1 1 d . A . O5 O 0.3611(3) -0.0056(3) 0.6369(3) 0.0604(11) Uani 1 1 d . . . N1 N 0.1371(3) 0.1853(3) 0.5328(3) 0.0501(11) Uani 1 1 d . . . N2 N 0.3452(3) -0.1906(3) 0.5091(3) 0.0468(10) Uani 1 1 d . . . C1 C 0.0712(4) 0.1701(3) 0.2768(4) 0.0486(11) Uani 1 1 d . . . C2 C 0.1999(4) 0.1811(3) 0.2530(4) 0.0498(12) Uani 1 1 d . A . C3 C 0.0446(4) 0.3855(3) 0.1754(4) 0.0551(12) Uani 1 1 d . . . C4 C -0.0060(4) 0.5035(4) 0.1508(4) 0.0606(13) Uani 1 1 d . A . C5 C -0.1618(7) 0.7161(5) 0.1480(6) 0.097(2) Uani 1 1 d . . . C6 C -0.0490(12) 0.7287(8) 0.1352(10) 0.070(3) Uani 0.664(6) 1 d P A 1 C6' C -0.006(2) 0.7309(19) 0.0866(18) 0.069(5) Uani 0.336(6) 1 d P A 2 C7 C -0.3495(16) 0.9030(13) 0.0446(10) 0.147(6) Uani 0.664(6) 1 d P A 1 C7' C -0.4172(19) 0.8240(19) 0.110(2) 0.102(7) Uani 0.336(6) 1 d P A 2 C8 C 0.148(2) 0.861(2) 0.1532(19) 0.121(6) Uani 0.664(6) 1 d P A 1 C8' C 0.109(4) 0.855(3) 0.180(3) 0.097(10) Uani 0.336(6) 1 d P A 2 C9 C 0.0240(4) 0.0680(3) 0.3476(3) 0.0465(11) Uani 1 1 d . . . C10 C 0.3384(4) 0.0937(4) 0.2806(4) 0.0549(12) Uani 1 1 d . . . C11 C 0.0026(4) 0.2368(3) 0.5352(4) 0.0624(14) Uani 1 1 d . . . H11 H -0.0573 0.1874 0.5460 0.075 Uiso 1 1 calc R . . C12 C -0.0544(4) 0.3586(3) 0.5228(5) 0.0692(16) Uani 1 1 d . . . H12 H -0.1506 0.3899 0.5244 0.083 Uiso 1 1 calc R . . C13 C 0.0285(4) 0.4341(3) 0.5080(4) 0.0503(12) Uani 1 1 d . . . C14 C 0.1682(4) 0.3809(4) 0.5073(5) 0.0793(18) Uani 1 1 d . . . H14 H 0.2301 0.4281 0.4987 0.095 Uiso 1 1 calc R . . C15 C 0.2170(4) 0.2580(4) 0.5191(5) 0.0734(17) Uani 1 1 d . . . H15 H 0.3129 0.2242 0.5173 0.088 Uiso 1 1 calc R . . C16 C 0.3738(4) -0.2698(3) 0.6021(4) 0.0589(13) Uani 1 1 d . . . H16 H 0.3516 -0.2418 0.6722 0.071 Uiso 1 1 calc R . . C17 C 0.4340(5) -0.3906(3) 0.6034(4) 0.0610(13) Uani 1 1 d . . . H17 H 0.4510 -0.4421 0.6725 0.073 Uiso 1 1 calc R . . C18 C 0.4688(4) -0.4350(3) 0.5023(4) 0.0477(11) Uani 1 1 d . . . C19 C 0.4410(5) -0.3526(3) 0.4043(4) 0.0623(13) Uani 1 1 d . . . H19 H 0.4629 -0.3776 0.3329 0.075 Uiso 1 1 calc R . . C20 C 0.3804(4) -0.2330(3) 0.4124(4) 0.0598(13) Uani 1 1 d . . . H20 H 0.3634 -0.1789 0.3447 0.072 Uiso 1 1 calc R . . C21 C 0.3986(11) 0.7167(10) -0.0858(10) 0.112(3) Uiso 0.664(6) 1 d P A 1 C22 C 0.4345(14) 0.6637(13) 0.0307(14) 0.130(4) Uiso 0.664(6) 1 d P A 1 N3 N 0.4646(9) 0.6211(9) 0.1152(8) 0.093(3) Uiso 0.664(6) 1 d P A 1 C21' C 0.4082(13) 0.6380(13) -0.1122(12) 0.061(4) Uiso 0.336(6) 1 d P A 2 C22' C 0.455(2) 0.596(2) 0.0282(19) 0.090(5) Uiso 0.336(6) 1 d P A 2 N3' N 0.4713(14) 0.5611(15) 0.1303(13) 0.077(4) Uiso 0.336(6) 1 d P A 2 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 0.0407(8) 0.0329(8) 0.0628(8) -0.0048(2) -0.0081(2) -0.0079(3) S1 0.0462(9) 0.0446(9) 0.0833(11) 0.0128(5) -0.0180(5) -0.0123(5) S2 0.0469(9) 0.0445(9) 0.0861(12) 0.0086(5) -0.0044(5) -0.0112(5) S3 0.0601(10) 0.0590(10) 0.0957(13) -0.0018(7) -0.0100(7) 0.0031(6) S4 0.0817(11) 0.0476(10) 0.1121(14) 0.0100(7) -0.0093(8) -0.0254(6) O1 0.0417(15) 0.0419(15) 0.0598(19) -0.0019(12) -0.0080(12) -0.0109(11) O2 0.0473(15) 0.0330(14) 0.064(2) -0.0011(12) -0.0127(12) -0.0112(11) O3 0.055(4) 0.114(12) 0.078(6) 0.008(7) 0.006(3) 0.016(7) O3' 0.091(17) 0.076(14) 0.050(10) -0.013(10) -0.019(11) 0.037(11) O4 0.0405(15) 0.0475(16) 0.062(2) 0.0042(13) -0.0056(13) -0.0098(11) O5 0.0431(15) 0.0608(18) 0.080(2) -0.0207(16) -0.0129(14) -0.0083(13) N1 0.0464(18) 0.0344(17) 0.070(2) -0.0103(15) -0.0083(15) -0.0092(13) N2 0.0443(17) 0.0375(17) 0.055(2) -0.0067(14) -0.0083(14) -0.0046(13) C1 0.050(2) 0.0361(19) 0.058(3) -0.0017(17) -0.0105(18) -0.0104(15) C2 0.047(2) 0.0360(19) 0.063(3) -0.0027(17) -0.0034(18) -0.0097(15) C3 0.048(2) 0.045(2) 0.067(3) 0.0027(19) -0.0087(19) -0.0106(17) C4 0.055(2) 0.045(2) 0.073(3) 0.003(2) -0.008(2) -0.0097(18) C5 0.093(4) 0.058(3) 0.137(6) -0.027(3) -0.046(4) 0.012(3) S5 0.0840(17) 0.0529(14) 0.0775(19) -0.0183(12) -0.0119(13) 0.0037(10) S6 0.127(3) 0.0468(15) 0.242(6) -0.010(2) -0.021(3) -0.0308(15) C6 0.089(8) 0.033(3) 0.083(8) -0.003(5) 0.001(6) -0.017(4) C7 0.169(12) 0.155(12) 0.061(7) -0.014(7) -0.028(7) 0.052(10) C8 0.130(14) 0.145(13) 0.112(14) -0.017(10) 0.011(10) -0.091(11) S5' 0.109(4) 0.057(3) 0.122(6) -0.008(3) -0.013(4) 0.012(3) S6' 0.130(5) 0.039(2) 0.087(4) -0.003(2) -0.010(3) -0.025(2) C6' 0.065(11) 0.057(9) 0.065(13) 0.014(9) 0.003(8) -0.006(8) C7' 0.077(11) 0.100(14) 0.113(18) -0.034(13) -0.022(11) 0.017(10) C8' 0.120(19) 0.106(15) 0.103(19) -0.049(14) 0.056(13) -0.102(15) C9 0.051(2) 0.0363(19) 0.053(2) -0.0080(16) -0.0043(17) -0.0120(16) C10 0.043(2) 0.047(2) 0.068(3) -0.007(2) -0.005(2) -0.0035(17) C11 0.050(2) 0.037(2) 0.101(4) -0.013(2) -0.001(2) -0.0145(17) C12 0.044(2) 0.039(2) 0.123(5) -0.016(2) 0.000(2) -0.0108(17) C13 0.050(2) 0.0333(19) 0.068(3) -0.0093(18) -0.0067(19) -0.0108(16) C14 0.051(2) 0.038(2) 0.154(6) -0.014(3) -0.023(3) -0.0132(18) C15 0.047(2) 0.038(2) 0.137(5) -0.017(3) -0.019(3) -0.0074(17) C16 0.071(3) 0.042(2) 0.054(3) -0.0073(18) -0.010(2) 0.0014(19) C17 0.076(3) 0.040(2) 0.055(3) -0.0010(18) -0.011(2) 0.0001(19) C18 0.0420(19) 0.035(2) 0.061(3) -0.0047(17) -0.0031(17) -0.0061(15) C19 0.080(3) 0.041(2) 0.057(3) -0.0071(19) -0.005(2) -0.003(2) C20 0.071(3) 0.041(2) 0.057(3) -0.0016(19) -0.008(2) -0.0013(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 2.073(3) . ? Zn1 O2 2.073(3) . ? Zn1 O4 2.092(3) . ? Zn1 O1 2.100(3) 2_556 ? Zn1 N1 2.176(3) . ? Zn1 N2 2.219(3) . ? S1 C3 1.754(4) . ? S1 C1 1.755(4) . ? S2 C3 1.756(4) . ? S2 C2 1.752(4) . ? S3 C5 1.730(6) . ? S3 C4 1.745(4) . ? S4 C6' 1.61(2) . ? S4 C4 1.756(4) . ? S4 C6 1.867(10) . ? S5 C7 1.801(12) . ? S5 C5 1.833(6) . ? S5' C5 1.763(7) . ? S5' C7' 1.75(2) . ? S6 C6 1.764(9) . ? S6 C8 1.77(2) . ? S6' C6' 1.72(2) . ? S6' C8' 1.93(5) . ? O1 C9 1.257(4) . ? O1 Zn1 2.100(3) 2_556 ? O2 C9 1.269(4) . ? O3 C10 1.271(19) . ? O3' C10 1.20(3) . ? O4 C10 1.249(5) . ? N1 C15 1.320(5) . ? N1 C11 1.327(5) . ? N2 C20 1.320(5) . ? N2 C16 1.326(5) . ? C1 C2 1.336(5) . ? C1 C9 1.492(5) . ? C2 C10 1.530(5) . ? C3 C4 1.334(5) . ? C5 C6 1.183(12) . ? C5 C6' 1.683(19) . ? C11 C12 1.379(5) . ? C11 H11 0.9400 . ? C12 C13 1.370(5) . ? C12 H12 0.9400 . ? C13 C14 1.378(6) . ? C13 C13 1.486(7) 2_566 ? C14 C15 1.383(6) . ? C14 H14 0.9400 . ? C15 H15 0.9400 . ? C16 C17 1.384(5) . ? C16 H16 0.9400 . ? C17 C18 1.379(6) . ? C17 H17 0.9400 . ? C18 C19 1.388(6) . ? C18 C18 1.496(7) 2_646 ? C19 C20 1.389(5) . ? C19 H19 0.9400 . ? C20 H20 0.9400 . ? C21 C22 1.480(18) . ? C22 N3 1.094(15) . ? C21' C22' 1.77(3) . ? C22' N3' 1.24(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn1 O2 174.72(10) . . ? O5 Zn1 O4 93.34(12) . . ? O2 Zn1 O4 86.15(11) . . ? O5 Zn1 O1 89.84(11) . 2_556 ? O2 Zn1 O1 90.23(10) . 2_556 ? O4 Zn1 O1 174.14(10) . 2_556 ? O5 Zn1 N1 87.91(12) . . ? O2 Zn1 N1 97.32(11) . . ? O4 Zn1 N1 87.95(12) . . ? O1 Zn1 N1 97.10(11) 2_556 . ? O5 Zn1 N2 87.71(11) . . ? O2 Zn1 N2 87.03(11) . . ? O4 Zn1 N2 88.72(11) . . ? O1 Zn1 N2 86.48(11) 2_556 . ? N1 Zn1 N2 174.33(11) . . ? C3 S1 C1 93.86(18) . . ? C3 S2 C2 94.23(18) . . ? C5 S3 C4 94.7(3) . . ? C6' S4 C4 104.0(7) . . ? C6' S4 C6 20.7(6) . . ? C4 S4 C6 89.5(3) . . ? C7 S5 C5 96.4(5) . . ? C5 S5' C7' 96.4(8) . . ? C6 S6 C8 112.4(9) . . ? C6' S6' C8' 91.5(11) . . ? C9 O1 Zn1 127.5(3) . 2_556 ? C9 O2 Zn1 128.5(2) . . ? C10 O4 Zn1 130.4(3) . . ? C15 N1 C11 116.0(3) . . ? C15 N1 Zn1 119.4(3) . . ? C11 N1 Zn1 123.7(2) . . ? C20 N2 C16 115.8(3) . . ? C20 N2 Zn1 123.3(3) . . ? C16 N2 Zn1 120.8(3) . . ? C2 C1 C9 127.8(3) . . ? C2 C1 S1 117.6(3) . . ? C9 C1 S1 114.6(3) . . ? C1 C2 C10 131.3(4) . . ? C1 C2 S2 116.7(3) . . ? C10 C2 S2 111.8(3) . . ? C4 C3 S1 122.7(3) . . ? C4 C3 S2 123.9(3) . . ? S1 C3 S2 113.4(2) . . ? C3 C4 S3 123.2(3) . . ? C3 C4 S4 122.4(3) . . ? S3 C4 S4 114.4(2) . . ? C6 C5 C6' 18.5(11) . . ? C6 C5 S3 119.2(6) . . ? C6' C5 S3 114.3(9) . . ? C6 C5 S5' 103.6(7) . . ? C6' C5 S5' 102.4(9) . . ? S3 C5 S5' 135.6(5) . . ? C6 C5 S5 128.9(6) . . ? C6' C5 S5 133.9(9) . . ? S3 C5 S5 110.8(4) . . ? S5' C5 S5 33.5(3) . . ? C5 C6 S6 123.0(8) . . ? C5 C6 S4 118.8(7) . . ? S6 C6 S4 116.8(6) . . ? S4 C6' C5 107.1(12) . . ? S4 C6' S6' 121.8(12) . . ? C5 C6' S6' 130.3(13) . . ? O1 C9 O2 125.1(3) . . ? O1 C9 C1 116.2(3) . . ? O2 C9 C1 118.7(3) . . ? O3' C10 O4 120.6(15) . . ? O3' C10 O3 24(2) . . ? O4 C10 O3 126.4(9) . . ? O3' C10 C2 117.4(16) . . ? O4 C10 C2 120.8(4) . . ? O3 C10 C2 111.3(8) . . ? N1 C11 C12 123.7(4) . . ? N1 C11 H11 118.1 . . ? C12 C11 H11 118.1 . . ? C13 C12 C11 120.3(4) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 116.2(3) . . ? C12 C13 C13 122.0(4) . 2_566 ? C14 C13 C13 121.9(4) . 2_566 ? C13 C14 C15 119.9(4) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? N1 C15 C14 124.0(4) . . ? N1 C15 H15 118.0 . . ? C14 C15 H15 118.0 . . ? N2 C16 C17 124.6(4) . . ? N2 C16 H16 117.7 . . ? C17 C16 H16 117.7 . . ? C16 C17 C18 119.5(4) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C17 C18 C19 116.4(3) . . ? C17 C18 C18 122.3(5) . 2_646 ? C19 C18 C18 121.3(5) . 2_646 ? C18 C19 C20 119.6(4) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? N2 C20 C19 124.1(4) . . ? N2 C20 H20 117.9 . . ? C19 C20 H20 117.9 . . ? N3 C22 C21 177.3(17) . . ? N3' C22' C21' 171.2(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Zn1 O2 C9 -164.3(11) . . . . ? O4 Zn1 O2 C9 -79.7(3) . . . . ? O1 Zn1 O2 C9 104.9(3) 2_556 . . . ? N1 Zn1 O2 C9 7.7(3) . . . . ? N2 Zn1 O2 C9 -168.6(3) . . . . ? O5 Zn1 O4 C10 -164.8(4) . . . . ? O2 Zn1 O4 C10 20.4(3) . . . . ? O1 Zn1 O4 C10 72.4(10) 2_556 . . . ? N1 Zn1 O4 C10 -77.0(4) . . . . ? N2 Zn1 O4 C10 107.6(4) . . . . ? O5 Zn1 N1 C15 51.4(4) . . . . ? O2 Zn1 N1 C15 -127.8(4) . . . . ? O4 Zn1 N1 C15 -42.0(4) . . . . ? O1 Zn1 N1 C15 141.0(4) 2_556 . . . ? N2 Zn1 N1 C15 12.1(15) . . . . ? O5 Zn1 N1 C11 -139.8(4) . . . . ? O2 Zn1 N1 C11 41.0(4) . . . . ? O4 Zn1 N1 C11 126.8(4) . . . . ? O1 Zn1 N1 C11 -50.2(4) 2_556 . . . ? N2 Zn1 N1 C11 -179(60) . . . . ? O5 Zn1 N2 C20 -138.2(3) . . . . ? O2 Zn1 N2 C20 41.4(3) . . . . ? O4 Zn1 N2 C20 -44.8(3) . . . . ? O1 Zn1 N2 C20 131.8(3) 2_556 . . . ? N1 Zn1 N2 C20 -98.8(13) . . . . ? O5 Zn1 N2 C16 46.9(3) . . . . ? O2 Zn1 N2 C16 -133.5(3) . . . . ? O4 Zn1 N2 C16 140.3(3) . . . . ? O1 Zn1 N2 C16 -43.1(3) 2_556 . . . ? N1 Zn1 N2 C16 86.2(14) . . . . ? C3 S1 C1 C2 -11.5(4) . . . . ? C3 S1 C1 C9 168.6(3) . . . . ? C9 C1 C2 C10 5.3(8) . . . . ? S1 C1 C2 C10 -174.6(4) . . . . ? C9 C1 C2 S2 178.9(3) . . . . ? S1 C1 C2 S2 -1.0(5) . . . . ? C3 S2 C2 C1 12.8(4) . . . . ? C3 S2 C2 C10 -172.3(3) . . . . ? C1 S1 C3 C4 -161.5(5) . . . . ? C1 S1 C3 S2 19.7(3) . . . . ? C2 S2 C3 C4 161.0(5) . . . . ? C2 S2 C3 S1 -20.2(3) . . . . ? S1 C3 C4 S3 -0.4(7) . . . . ? S2 C3 C4 S3 178.3(3) . . . . ? S1 C3 C4 S4 -178.4(3) . . . . ? S2 C3 C4 S4 0.2(7) . . . . ? C5 S3 C4 C3 167.3(5) . . . . ? C5 S3 C4 S4 -14.5(4) . . . . ? C6' S4 C4 C3 -179.6(9) . . . . ? C6 S4 C4 C3 -164.7(6) . . . . ? C6' S4 C4 S3 2.1(9) . . . . ? C6 S4 C4 S3 17.1(5) . . . . ? C4 S3 C5 C6 2.8(9) . . . . ? C4 S3 C5 C6' 22.8(9) . . . . ? C4 S3 C5 S5' 165.9(7) . . . . ? C4 S3 C5 S5 -166.6(4) . . . . ? C6 C5 S5 C7 82.6(12) . . . . ? C6' C5 S5 C7 58.8(14) . . . . ? S3 C5 S5 C7 -109.3(7) . . . . ? S5' C5 S5 C7 34.8(7) . . . . ? C6' C5 C6 S6 96(4) . . . . ? S3 C5 C6 S6 175.8(6) . . . . ? S5' C5 C6 S6 7.9(12) . . . . ? S5 C5 C6 S6 -17.0(16) . . . . ? C6' C5 C6 S4 -70(3) . . . . ? S3 C5 C6 S4 9.6(13) . . . . ? S5' C5 C6 S4 -158.3(6) . . . . ? S5 C5 C6 S4 176.8(5) . . . . ? C8 S6 C6 C5 156.6(12) . . . . ? C8 S6 C6 S4 -37.0(11) . . . . ? C6' S4 C6 C5 119(4) . . . . ? C4 S4 C6 C5 -16.5(10) . . . . ? C6' S4 C6 S6 -49(3) . . . . ? C4 S4 C6 S6 176.4(7) . . . . ? C6 C5 S5' C7' 166.4(11) . . . . ? C6' C5 S5' C7' 147.5(12) . . . . ? S3 C5 S5' C7' 1.6(13) . . . . ? S5 C5 S5' C7' -49.9(9) . . . . ? C4 S4 C6' C5 12.3(14) . . . . ? C6 S4 C6' C5 -34(2) . . . . ? C4 S4 C6' S6' -177.4(12) . . . . ? C6 S4 C6' S6' 136(4) . . . . ? C6 C5 C6' S4 85(3) . . . . ? S3 C5 C6' S4 -24.3(15) . . . . ? S5' C5 C6' S4 -178.9(10) . . . . ? S5 C5 C6' S4 167.9(6) . . . . ? C6 C5 C6' S6' -84(4) . . . . ? S3 C5 C6' S6' 166.5(14) . . . . ? S5' C5 C6' S6' 12(2) . . . . ? S5 C5 C6' S6' -1(3) . . . . ? C8' S6' C6' S4 -76.5(18) . . . . ? C8' S6' C6' C5 91(2) . . . . ? Zn1 O1 C9 O2 31.4(5) 2_556 . . . ? Zn1 O1 C9 C1 -148.9(3) 2_556 . . . ? Zn1 O2 C9 O1 -124.2(3) . . . . ? Zn1 O2 C9 C1 56.1(5) . . . . ? C2 C1 C9 O1 -172.0(4) . . . . ? S1 C1 C9 O1 7.9(5) . . . . ? C2 C1 C9 O2 7.8(6) . . . . ? S1 C1 C9 O2 -172.3(3) . . . . ? Zn1 O4 C10 O3' -129(2) . . . . ? Zn1 O4 C10 O3 -157.0(10) . . . . ? Zn1 O4 C10 C2 37.7(5) . . . . ? C1 C2 C10 O3' 108(2) . . . . ? S2 C2 C10 O3' -65(2) . . . . ? C1 C2 C10 O4 -59.0(7) . . . . ? S2 C2 C10 O4 127.1(4) . . . . ? C1 C2 C10 O3 133.7(10) . . . . ? S2 C2 C10 O3 -40.2(10) . . . . ? C15 N1 C11 C12 1.0(8) . . . . ? Zn1 N1 C11 C12 -168.2(4) . . . . ? N1 C11 C12 C13 -0.7(9) . . . . ? C11 C12 C13 C14 -0.4(8) . . . . ? C11 C12 C13 C13 178.7(6) . . . 2_566 ? C12 C13 C14 C15 1.0(8) . . . . ? C13 C13 C14 C15 -178.0(6) 2_566 . . . ? C11 N1 C15 C14 -0.2(8) . . . . ? Zn1 N1 C15 C14 169.4(5) . . . . ? C13 C14 C15 N1 -0.8(10) . . . . ? C20 N2 C16 C17 -1.2(6) . . . . ? Zn1 N2 C16 C17 174.1(4) . . . . ? N2 C16 C17 C18 0.4(7) . . . . ? C16 C17 C18 C19 0.5(6) . . . . ? C16 C17 C18 C18 -178.6(5) . . . 2_646 ? C17 C18 C19 C20 -0.3(6) . . . . ? C18 C18 C19 C20 178.7(4) 2_646 . . . ? C16 N2 C20 C19 1.3(6) . . . . ? Zn1 N2 C20 C19 -173.8(3) . . . . ? C18 C19 C20 N2 -0.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.224 _refine_diff_density_min -0.126 _refine_diff_density_rms 0.023 ########End