Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Karambelkar, Vivek V.' 'Krishnamurthy, Divya' 'Stern, Charlotte L.' 'Zakharov, Lev N.' 'Rheingold, Arnold L.' 'Goldberg, David P.' _publ_contact_author_name 'Prof David P. Goldberg' _publ_contact_author_address ; Department of Chemistry The Johns Hopkins University 3400 N. Charles St. Baltimore Maryland 21218 UNITED STATES OF AMERICA ; _publ_contact_author_email 'dpg@jhu.edu' _publ_section_title ; A New Bis(imidazolyl)(alkylthiolate) Tripodal Ligand and the Spontaneous Formation of a Disulfide-Linked, Hydroxo-Bridged Dinuclear Zinc Complex ; data_4 _database_code_CSD 191657 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H76 B3 F12 N10 O4 S2 Zn2' _chemical_formula_weight 1672.83 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' 'B' 'B' 0.0013 0.0007 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.526(10) _cell_length_b 14.601(5) _cell_length_c 25.161(9) _cell_angle_alpha 90.00 _cell_angle_beta 121.576(5) _cell_angle_gamma 90.00 _cell_volume 8928(5) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.246 _exptl_crystal_size_mid 0.242 _exptl_crystal_size_min 0.080 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3592 _exptl_absorpt_coefficient_mu 0.668 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8441 _exptl_absorpt_correction_T_max 0.9492 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40192 _diffrn_reflns_av_R_equivalents 0.1065 _diffrn_reflns_av_sigmaI/netI 0.0953 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.26 _reflns_number_total 10690 _reflns_number_gt 5598 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.2000P)^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 idealized _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10690 _refine_ls_number_parameters 485 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2080 _refine_ls_R_factor_gt 0.1248 _refine_ls_wR_factor_ref 0.4179 _refine_ls_wR_factor_gt 0.3547 _refine_ls_goodness_of_fit_ref 1.390 _refine_ls_restrained_S_all 1.390 _refine_ls_shift/su_max 0.010 _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 0.01720(3) 0.74535(5) 0.68865(4) 0.0370(3) Uani 1 1 d . . . S1 S 0.04219(7) 0.55207(11) 0.77451(10) 0.0410(5) Uani 1 1 d . . . O1 O 0.0000 0.7796(5) 0.7500 0.0353(14) Uani 1 2 d S . . O2 O 0.0747(2) 0.4702(4) 0.6432(3) 0.0593(17) Uani 1 1 d . . . O3 O 0.2827(10) 0.4609(16) 0.8831(11) 0.145(8) Uiso 0.50 1 d P . . N1 N -0.0226(3) 0.6436(4) 0.6297(3) 0.0456(15) Uani 1 1 d . . . N2 N 0.0904(2) 0.6962(4) 0.7113(3) 0.0389(13) Uani 1 1 d . . . N3 N -0.0418(3) 0.5072(5) 0.5872(3) 0.0528(18) Uani 1 1 d . . . N4 N 0.1543(3) 0.6080(4) 0.7135(4) 0.064(2) Uani 1 1 d . . . N5 N 0.0095(3) 0.8678(5) 0.6471(3) 0.065(2) Uani 1 1 d . . . C1 C -0.1448(4) 0.5179(7) 0.5101(5) 0.063(3) Uani 1 1 d . . . C2 C -0.1747(4) 0.5615(7) 0.4525(4) 0.066(3) Uani 1 1 d . . . H2 H -0.1609 0.6156 0.4446 0.080 Uiso 1 1 calc R . . C3 C -0.2251(5) 0.5254(9) 0.4066(5) 0.084(3) Uani 1 1 d . . . H3 H -0.2459 0.5544 0.3670 0.101 Uiso 1 1 calc R . . C4 C -0.2445(5) 0.4471(10) 0.4192(8) 0.113(6) Uani 1 1 d . . . H4 H -0.2790 0.4228 0.3879 0.136 Uiso 1 1 calc R . . C5 C -0.2162(5) 0.4042(8) 0.4743(8) 0.101(4) Uani 1 1 d . . . H5 H -0.2301 0.3497 0.4817 0.121 Uiso 1 1 calc R . . C6 C -0.1658(4) 0.4406(7) 0.5208(6) 0.085(3) Uani 1 1 d . . . H6 H -0.1460 0.4114 0.5603 0.102 Uiso 1 1 calc R . . C7 C -0.1172(4) 0.7216(8) 0.5720(4) 0.067(3) Uani 1 1 d . . . C8 C -0.1600(4) 0.7091(11) 0.5829(5) 0.100(5) Uani 1 1 d . . . H8 H -0.1652 0.6542 0.5995 0.120 Uiso 1 1 calc R . . C9 C -0.1984(4) 0.7936(9) 0.5655(5) 0.073(3) Uani 1 1 d . . . H9 H -0.2287 0.7930 0.5712 0.088 Uiso 1 1 calc R . . C10 C -0.1879(6) 0.8637(11) 0.5432(7) 0.108(4) Uani 1 1 d . . . H10 H -0.2108 0.9157 0.5350 0.130 Uiso 1 1 calc R . . C11 C -0.1492(6) 0.8717(10) 0.5305(7) 0.109(4) Uani 1 1 d . . . H11 H -0.1465 0.9250 0.5106 0.131 Uiso 1 1 calc R . . C12 C -0.1118(6) 0.7996(8) 0.5470(7) 0.096(4) Uani 1 1 d . . . H12 H -0.0821 0.8056 0.5404 0.115 Uiso 1 1 calc R . . C13 C 0.1409(3) 0.8457(5) 0.7481(3) 0.0402(16) Uani 1 1 d . . . C14 C 0.1217(3) 0.8771(5) 0.7858(4) 0.0472(18) Uani 1 1 d . . . H14 H 0.1109 0.8341 0.8057 0.057 Uiso 1 1 calc R . . C15 C 0.1182(4) 0.9694(6) 0.7946(5) 0.067(3) Uani 1 1 d . . . H15 H 0.1032 0.9909 0.8182 0.080 Uiso 1 1 calc R . . C16 C 0.1382(4) 1.0327(6) 0.7666(5) 0.073(3) Uani 1 1 d . . . H16 H 0.1373 1.0966 0.7731 0.087 Uiso 1 1 calc R . . C17 C 0.1580(4) 1.0019(6) 0.7311(5) 0.072(3) Uani 1 1 d . . . H17 H 0.1707 1.0438 0.7125 0.086 Uiso 1 1 calc R . . C18 C 0.1596(3) 0.9088(6) 0.7227(4) 0.053(2) Uani 1 1 d . . . H18 H 0.1741 0.8874 0.6985 0.063 Uiso 1 1 calc R . . C19 C 0.2366(5) 0.7141(7) 0.7588(9) 0.107(5) Uani 1 1 d . . . C20 C 0.2528(6) 0.7270(7) 0.7167(11) 0.149(8) Uani 1 1 d . . . H20 H 0.2281 0.7211 0.6730 0.179 Uiso 1 1 calc R . . C21 C 0.3149(8) 0.7522(7) 0.7460(15) 0.161(12) Uani 1 1 d . . . H21 H 0.3318 0.7652 0.7227 0.194 Uiso 1 1 calc R . . C22 C 0.3430(10) 0.7531(10) 0.8132(13) 0.167(11) Uani 1 1 d . . . H22 H 0.3792 0.7770 0.8311 0.200 Uiso 1 1 calc R . . C23 C 0.3318(7) 0.7281(12) 0.8602(9) 0.122(5) Uiso 1 1 d . . . H23 H 0.3562 0.7204 0.9039 0.147 Uiso 1 1 calc R . . C24 C 0.2737(5) 0.7180(13) 0.8235(11) 0.193(12) Uani 1 1 d . . . H24 H 0.2567 0.7130 0.8473 0.232 Uiso 1 1 calc R . . C25 C -0.0918(3) 0.5560(6) 0.5597(4) 0.056(2) Uani 1 1 d . . . C26 C -0.0794(3) 0.6395(6) 0.5860(4) 0.0484(19) Uani 1 1 d . . . C27 C 0.1383(3) 0.7486(5) 0.7335(4) 0.0445(18) Uani 1 1 d . . . C28 C 0.1782(4) 0.6938(6) 0.7356(5) 0.070(3) Uani 1 1 d . . . C29 C 0.0084(6) 0.9307(10) 0.6245(6) 0.122(6) Uani 1 1 d . . . C30 C 0.0104(13) 1.0180(18) 0.5950(10) 0.35(3) Uani 1 1 d . . . H30A H 0.0144 1.0696 0.6220 0.519 Uiso 1 1 calc R . . H30B H -0.0237 1.0251 0.5544 0.519 Uiso 1 1 calc R . . H30C H 0.0418 1.0167 0.5893 0.519 Uiso 1 1 calc R . . C31 C -0.0005(3) 0.5624(5) 0.6295(4) 0.0397(17) Uani 1 1 d . . . C32 C -0.0400(4) 0.4130(6) 0.5658(4) 0.059(2) Uani 1 1 d . . . H32A H -0.0016 0.3954 0.5821 0.089 Uiso 1 1 calc R . . H32B H -0.0604 0.4115 0.5201 0.089 Uiso 1 1 calc R . . H32C H -0.0567 0.3700 0.5811 0.089 Uiso 1 1 calc R . . C33 C 0.1004(3) 0.6139(5) 0.6990(4) 0.0445(18) Uani 1 1 d . . . C34 C 0.1883(4) 0.5322(6) 0.7144(5) 0.070(3) Uani 1 1 d . . . H34A H 0.1678 0.4747 0.7055 0.105 Uiso 1 1 calc R . . H34B H 0.2221 0.5286 0.7556 0.105 Uiso 1 1 calc R . . H34C H 0.1977 0.5427 0.6826 0.105 Uiso 1 1 calc R . . C35 C 0.0701(4) 0.5066(7) 0.5865(5) 0.081(4) Uani 1 1 d . . . H35A H 0.0357 0.5413 0.5627 0.122 Uiso 1 1 calc R . . H35B H 0.0701 0.4559 0.5610 0.122 Uiso 1 1 calc R . . H35C H 0.1013 0.5471 0.5978 0.122 Uiso 1 1 calc R . . C36 C 0.0656(3) 0.4781(5) 0.7326(4) 0.049(2) Uani 1 1 d . . . C37 C 0.0359(3) 0.3861(5) 0.7146(5) 0.057(2) Uani 1 1 d . . . H37A H 0.0441 0.3538 0.6862 0.086 Uiso 1 1 calc R . . H37B H -0.0039 0.3962 0.6937 0.086 Uiso 1 1 calc R . . H37C H 0.0483 0.3491 0.7522 0.086 Uiso 1 1 calc R . . C38 C 0.1256(3) 0.4624(6) 0.7843(5) 0.067(3) Uani 1 1 d . . . H38A H 0.1445 0.4282 0.7675 0.100 Uiso 1 1 calc R . . H38B H 0.1269 0.4274 0.8183 0.100 Uiso 1 1 calc R . . H38C H 0.1438 0.5216 0.8003 0.100 Uiso 1 1 calc R . . C39 C 0.0598(3) 0.5327(5) 0.6752(4) 0.0464(19) Uani 1 1 d . . . B1 B 0.3793(9) 0.7154(15) 0.6224(10) 0.054(5) Uiso 0.50 1 d P . . B2 B 0.5003(9) 0.7263(15) 0.5065(10) 0.118(6) Uiso 1 1 d . . . F1 F 0.3298(10) 0.7315(15) 0.5740(11) 0.164(8) Uiso 0.50 1 d P . . F2 F 0.3764(8) 0.7135(14) 0.6718(9) 0.137(6) Uiso 0.50 1 d P . . F3 F 0.4085(5) 0.7831(9) 0.6277(6) 0.083(3) Uiso 0.50 1 d P . . F4 F 0.3844(6) 0.6284(11) 0.6111(7) 0.114(5) Uiso 0.50 1 d P . . F5 F 0.4503(9) 0.7436(12) 0.4502(11) 0.268(8) Uiso 1 1 d . . . F6 F 0.5366(7) 0.6630(11) 0.5108(7) 0.100(4) Uiso 0.50 1 d P . . F7 F 0.5401(6) 0.7824(10) 0.5228(7) 0.083(4) Uiso 0.50 1 d P . . F8 F 0.4897(6) 0.7131(11) 0.5530(7) 0.106(4) Uiso 0.50 1 d P . . F9 F 0.5065(9) 0.6408(14) 0.4876(9) 0.131(6) Uiso 0.50 1 d P . . F10 F 0.5157(7) 0.8115(11) 0.4948(8) 0.105(5) Uiso 0.50 1 d P . . F11 F 0.5393(9) 0.7515(12) 0.5789(10) 0.142(7) Uiso 0.50 1 d P . . 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 0.0426(5) 0.0309(5) 0.0468(5) -0.0051(3) 0.0300(4) -0.0026(3) S1 0.0429(10) 0.0224(8) 0.0736(13) -0.0060(8) 0.0415(10) -0.0032(7) O1 0.035(4) 0.037(3) 0.040(4) 0.000 0.024(3) 0.000 O2 0.056(3) 0.048(3) 0.101(5) -0.044(3) 0.060(3) -0.020(3) N1 0.052(4) 0.043(3) 0.058(4) -0.022(3) 0.040(3) -0.011(3) N2 0.043(3) 0.031(3) 0.052(4) -0.008(3) 0.031(3) -0.004(2) N3 0.050(4) 0.049(4) 0.077(5) -0.036(3) 0.045(4) -0.021(3) N4 0.052(4) 0.037(4) 0.131(7) -0.032(4) 0.066(5) -0.015(3) N5 0.066(5) 0.056(4) 0.056(4) 0.023(4) 0.020(4) -0.003(4) C1 0.052(5) 0.069(6) 0.080(7) -0.038(5) 0.042(5) -0.014(4) C2 0.054(5) 0.085(7) 0.060(6) -0.035(5) 0.030(5) 0.001(5) C3 0.067(7) 0.089(8) 0.081(7) -0.030(6) 0.029(6) 0.017(6) C4 0.058(7) 0.093(10) 0.156(14) -0.066(10) 0.033(8) 0.010(7) C5 0.060(7) 0.064(7) 0.157(13) -0.029(8) 0.040(8) -0.016(6) C6 0.062(6) 0.060(6) 0.127(10) -0.023(6) 0.045(7) -0.012(5) C7 0.047(5) 0.094(7) 0.063(6) -0.035(5) 0.032(5) -0.008(5) C8 0.056(6) 0.168(12) 0.067(7) -0.064(8) 0.025(5) 0.015(7) C9 0.057(6) 0.097(8) 0.065(6) -0.016(6) 0.032(5) 0.009(6) C10 0.119(12) 0.109(12) 0.103(10) -0.043(9) 0.062(9) -0.014(9) C11 0.099(9) 0.085(9) 0.135(12) 0.008(8) 0.056(9) 0.026(7) C12 0.106(9) 0.057(7) 0.138(11) 0.011(7) 0.072(9) 0.019(6) C13 0.041(4) 0.029(3) 0.051(4) -0.006(3) 0.024(3) -0.008(3) C14 0.056(5) 0.032(4) 0.051(4) 0.000(3) 0.027(4) 0.001(3) C15 0.073(6) 0.044(5) 0.088(7) -0.021(5) 0.044(6) 0.004(4) C16 0.085(7) 0.028(4) 0.090(7) -0.006(4) 0.035(6) 0.001(4) C17 0.061(6) 0.035(4) 0.120(8) 0.019(5) 0.048(6) -0.007(4) C18 0.044(4) 0.050(5) 0.067(5) -0.002(4) 0.031(4) 0.001(4) C19 0.064(7) 0.043(5) 0.238(16) -0.058(8) 0.096(10) -0.025(5) C20 0.136(12) 0.034(5) 0.38(3) 0.007(9) 0.205(17) -0.004(6) C21 0.151(16) 0.032(6) 0.40(4) 0.034(12) 0.22(2) 0.022(7) C22 0.20(2) 0.053(8) 0.24(3) -0.054(12) 0.10(2) -0.068(10) C24 0.048(7) 0.172(15) 0.33(3) -0.200(19) 0.083(12) -0.052(8) C25 0.047(5) 0.068(6) 0.071(6) -0.032(4) 0.043(4) -0.018(4) C26 0.041(4) 0.060(5) 0.054(5) -0.026(4) 0.031(4) -0.007(4) C27 0.051(4) 0.033(4) 0.067(5) -0.023(3) 0.043(4) -0.019(3) C28 0.053(5) 0.047(5) 0.135(9) -0.039(5) 0.067(6) -0.022(4) C29 0.117(11) 0.101(9) 0.072(8) 0.043(7) -0.004(7) -0.040(8) C30 0.39(4) 0.23(3) 0.160(18) 0.145(18) -0.04(2) -0.17(3) C31 0.039(4) 0.038(4) 0.059(5) -0.018(3) 0.038(4) -0.009(3) C32 0.065(5) 0.051(5) 0.083(6) -0.036(4) 0.053(5) -0.022(4) C33 0.043(4) 0.035(4) 0.069(5) -0.023(3) 0.039(4) -0.015(3) C34 0.061(5) 0.045(5) 0.135(9) -0.034(5) 0.072(6) -0.011(4) C35 0.084(7) 0.089(7) 0.116(8) -0.066(7) 0.084(7) -0.042(6) C36 0.042(4) 0.027(3) 0.092(6) -0.011(4) 0.046(4) -0.004(3) C37 0.053(5) 0.030(4) 0.096(7) -0.012(4) 0.044(5) -0.004(3) C38 0.042(5) 0.054(5) 0.102(7) -0.020(5) 0.036(5) -0.004(4) C39 0.046(4) 0.035(4) 0.075(5) -0.030(4) 0.043(4) -0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.915(2) . ? Zn1 N1 1.983(6) . ? Zn1 N2 1.989(6) . ? Zn1 N5 2.025(7) . ? S1 C36 1.860(7) . ? S1 S1 2.051(4) 2_556 ? O1 Zn1 1.915(2) 2_556 ? O2 C39 1.423(8) . ? O2 C35 1.462(12) . ? N1 C31 1.344(9) . ? N1 C26 1.404(10) . ? N2 C33 1.310(9) . ? N2 C27 1.402(9) . ? N3 C31 1.363(9) . ? N3 C25 1.409(11) . ? N3 C32 1.489(10) . ? N4 C33 1.383(9) . ? N4 C28 1.394(10) . ? N4 C34 1.464(10) . ? N5 C29 1.072(12) . ? C1 C6 1.369(14) . ? C1 C2 1.392(14) . ? C1 C25 1.476(12) . ? C2 C3 1.393(14) . ? C3 C4 1.377(19) . ? C4 C5 1.34(2) . ? C5 C6 1.397(15) . ? C7 C12 1.348(16) . ? C7 C8 1.397(15) . ? C7 C26 1.525(13) . ? C8 C9 1.551(17) . ? C9 C10 1.274(18) . ? C10 C11 1.308(18) . ? C11 C12 1.397(16) . ? C13 C18 1.379(11) . ? C13 C14 1.397(10) . ? C13 C27 1.457(9) . ? C14 C15 1.378(11) . ? C15 C16 1.446(14) . ? C16 C17 1.360(14) . ? C17 C18 1.380(12) . ? C19 C20 1.37(2) . ? C19 C24 1.40(3) . ? C19 C28 1.479(12) . ? C20 C21 1.57(2) . ? C21 C22 1.44(3) . ? C22 C23 1.43(3) . ? C23 C24 1.42(2) . ? C25 C26 1.343(11) . ? C27 C28 1.369(11) . ? C29 C30 1.490(19) . ? C31 C39 1.548(11) . ? C33 C39 1.542(9) . ? C36 C37 1.525(10) . ? C36 C38 1.531(12) . ? C36 C39 1.581(12) . ? B1 F3 1.26(2) . ? B1 F2 1.29(2) . ? B1 F1 1.31(3) . ? B1 F4 1.33(2) . ? B2 F7 1.28(2) . ? B2 F6 1.35(2) . ? B2 F8 1.37(2) . ? B2 F9 1.38(3) . ? B2 F10 1.40(2) . ? B2 F5 1.41(3) . ? B2 F11 1.60(3) . ? F6 F9 0.81(2) . ? F6 F7 1.76(2) . ? F7 F10 0.806(17) . ? F7 F11 1.49(2) . ? F8 F11 1.33(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 O1 Zn1 N1 120.7(2) . . ? O1 Zn1 N2 122.48(18) . . ? N1 Zn1 N2 92.8(2) . . ? O1 Zn1 N5 100.5(3) . . ? N1 Zn1 N5 114.2(3) . . ? N2 Zn1 N5 106.2(3) . . ? C36 S1 S1 108.4(3) . 2_556 ? Zn1 O1 Zn1 149.8(4) . 2_556 ? C39 O2 C35 114.7(7) . . ? C31 N1 C26 108.1(6) . . ? C31 N1 Zn1 125.3(5) . . ? C26 N1 Zn1 126.2(5) . . ? C33 N2 C27 107.9(6) . . ? C33 N2 Zn1 126.1(5) . . ? C27 N2 Zn1 125.1(5) . . ? C31 N3 C25 108.8(6) . . ? C31 N3 C32 130.5(7) . . ? C25 N3 C32 120.5(6) . . ? C33 N4 C28 107.1(6) . . ? C33 N4 C34 133.3(6) . . ? C28 N4 C34 119.4(6) . . ? C29 N5 Zn1 174.9(13) . . ? C6 C1 C2 119.2(9) . . ? C6 C1 C25 120.4(10) . . ? C2 C1 C25 120.4(9) . . ? C1 C2 C3 119.6(11) . . ? C4 C3 C2 119.2(13) . . ? C5 C4 C3 121.9(12) . . ? C4 C5 C6 119.2(13) . . ? C1 C6 C5 120.8(13) . . ? C12 C7 C8 121.8(12) . . ? C12 C7 C26 122.1(9) . . ? C8 C7 C26 116.0(11) . . ? C7 C8 C9 113.6(14) . . ? C10 C9 C8 118.1(12) . . ? C9 C10 C11 127.0(16) . . ? C10 C11 C12 118.1(16) . . ? C7 C12 C11 121.3(13) . . ? C18 C13 C14 118.7(7) . . ? C18 C13 C27 120.9(7) . . ? C14 C13 C27 120.3(6) . . ? C15 C14 C13 121.1(8) . . ? C14 C15 C16 117.9(8) . . ? C17 C16 C15 120.9(8) . . ? C16 C17 C18 119.0(8) . . ? C13 C18 C17 122.4(8) . . ? C20 C19 C24 122.4(13) . . ? C20 C19 C28 119.2(15) . . ? C24 C19 C28 118.3(14) . . ? C19 C20 C21 115(2) . . ? C22 C21 C20 110.5(18) . . ? C23 C22 C21 137.8(19) . . ? C22 C23 C24 100.3(19) . . ? C19 C24 C23 132.3(19) . . ? C26 C25 N3 106.3(7) . . ? C26 C25 C1 130.4(8) . . ? N3 C25 C1 123.3(7) . . ? C25 C26 N1 108.8(7) . . ? C25 C26 C7 128.9(8) . . ? N1 C26 C7 122.3(7) . . ? C28 C27 N2 108.2(6) . . ? C28 C27 C13 128.9(7) . . ? N2 C27 C13 122.8(6) . . ? C27 C28 N4 106.7(6) . . ? C27 C28 C19 129.8(7) . . ? N4 C28 C19 123.5(7) . . ? N5 C29 C30 176.6(19) . . ? N1 C31 N3 108.0(6) . . ? N1 C31 C39 125.8(6) . . ? N3 C31 C39 125.8(6) . . ? N2 C33 N4 110.1(6) . . ? N2 C33 C39 125.7(6) . . ? N4 C33 C39 124.1(6) . . ? C37 C36 C38 108.7(7) . . ? C37 C36 C39 113.4(7) . . ? C38 C36 C39 112.8(7) . . ? C37 C36 S1 111.9(5) . . ? C38 C36 S1 100.3(6) . . ? C39 C36 S1 109.1(5) . . ? O2 C39 C33 108.9(5) . . ? O2 C39 C31 107.7(6) . . ? C33 C39 C31 113.0(6) . . ? O2 C39 C36 105.9(6) . . ? C33 C39 C36 109.6(6) . . ? C31 C39 C36 111.3(6) . . ? F3 B1 F2 106.8(19) . . ? F3 B1 F1 106.8(19) . . ? F2 B1 F1 109(2) . . ? F3 B1 F4 129.4(19) . . ? F2 B1 F4 104.8(19) . . ? F1 B1 F4 99.2(19) . . ? F7 B2 F6 84.0(17) . . ? F7 B2 F8 112.0(18) . . ? F6 B2 F8 109.9(18) . . ? F7 B2 F9 116(2) . . ? F6 B2 F9 34.5(10) . . ? F8 B2 F9 107.1(18) . . ? F7 B2 F10 34.6(9) . . ? F6 B2 F10 108.2(19) . . ? F8 B2 F10 122.8(19) . . ? F9 B2 F10 128(2) . . ? F7 B2 F5 118(2) . . ? F6 B2 F5 122(2) . . ? F8 B2 F5 109(2) . . ? F9 B2 F5 93.4(18) . . ? F10 B2 F5 83.8(16) . . ? F7 B2 F11 61.3(13) . . ? F6 B2 F11 91.2(17) . . ? F8 B2 F11 52.7(12) . . ? F9 B2 F11 117.5(19) . . ? F10 B2 F11 85.9(15) . . ? F5 B2 F11 147(2) . . ? F9 F6 B2 75(2) . . ? F9 F6 F7 117(2) . . ? B2 F6 F7 46.3(11) . . ? F10 F7 B2 81(2) . . ? F10 F7 F11 123(2) . . ? B2 F7 F11 70.0(14) . . ? F10 F7 F6 115.2(19) . . ? B2 F7 F6 49.7(12) . . ? F11 F7 F6 80.6(11) . . ? F11 F8 B2 72.8(15) . . ? F6 F9 B2 71(2) . . ? F7 F10 B2 64.6(18) . . ? F8 F11 F7 101.8(16) . . ? F8 F11 B2 54.6(12) . . ? F7 F11 B2 48.8(11) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.676 _refine_diff_density_min -0.992 _refine_diff_density_rms 0.184 #===END data_5 _database_code_CSD 191658 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H84 F12 N12 O15 S6 Zn2' _chemical_formula_weight 2076.75 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' '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.5067(16) _cell_length_b 14.7799(8) _cell_length_c 26.0837(15) _cell_angle_alpha 90.00 _cell_angle_beta 122.9810(10) _cell_angle_gamma 90.00 _cell_volume 9218.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4272 _exptl_absorpt_coefficient_mu 0.750 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.751 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28570 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0692 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 28.30 _reflns_number_total 10778 _reflns_number_gt 7751 _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^)+(0.1414P)^2^+81.8141P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10778 _refine_ls_number_parameters 533 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1417 _refine_ls_R_factor_gt 0.1141 _refine_ls_wR_factor_ref 0.3026 _refine_ls_wR_factor_gt 0.2852 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.473 _refine_ls_shift/su_mean 0.006 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 0.07493(3) 1.00624(4) 0.30737(3) 0.0247(2) Uani 1 1 d . . . S1 S 0.01788(6) 0.81685(9) 0.22517(7) 0.0240(3) Uani 1 1 d . . . S2 S 0.24180(9) 0.51525(13) -0.01525(10) 0.0516(5) Uani 1 1 d . . . S3 S -0.0057(3) 0.5060(4) -0.1306(3) 0.1362(17) Uiso 1 1 d D . . F1 F 0.2047(3) 0.6080(4) 0.0399(3) 0.0762(17) Uani 1 1 d . . . F2 F 0.1909(2) 0.4644(4) 0.0381(3) 0.0699(15) Uani 1 1 d . . . F3 F 0.2723(3) 0.5203(5) 0.0983(2) 0.0808(18) Uani 1 1 d . . . F4 F 0.0340(13) 0.655(2) -0.0884(14) 0.408(15) Uiso 1 1 d D . . F5 F 0.0523(9) 0.5754(14) -0.1648(9) 0.276(8) Uiso 1 1 d D . . F6 F 0.0942(8) 0.5639(12) -0.0641(8) 0.240(7) Uiso 1 1 d D . . O1 O 0.0000 1.0468(3) 0.2500 0.0273(13) Uani 1 2 d S . . H1A H 0.0000 1.1097 0.2500 0.033 Uiso 1 2 calc SR . . O2 O 0.17685(16) 0.7364(3) 0.3486(2) 0.0297(9) Uani 1 1 d . . . O3 O 0.1871(3) 0.5170(4) -0.0712(3) 0.071(2) Uani 1 1 d . . . O4 O 0.2692(3) 0.4294(4) -0.0015(3) 0.0649(17) Uani 1 1 d . . . O5 O 0.2760(3) 0.5936(4) -0.0052(3) 0.0718(19) Uani 1 1 d . . . O6 O -0.0538(10) 0.540(2) -0.1883(10) 0.335(14) Uiso 1 1 d D . . O7 O -0.0032(15) 0.495(2) -0.0705(11) 0.370(17) Uiso 1 1 d D . . O8 O 0.0161(6) 0.4186(9) -0.1335(6) 0.154(5) Uiso 1 1 d D . . N1 N 0.09366(18) 0.9066(3) 0.3660(2) 0.0236(10) Uani 1 1 d . . . N2 N 0.1264(2) 0.9609(3) 0.2838(2) 0.0278(11) Uani 1 1 d . . . N3 N 0.1197(2) 0.7722(3) 0.4093(2) 0.0269(10) Uani 1 1 d . . . N4 N 0.1865(2) 0.8738(3) 0.2790(3) 0.0324(12) Uani 1 1 d . . . N5 N 0.1115(2) 1.1226(4) 0.3527(3) 0.0372(13) Uani 1 1 d . . . C1 C 0.0828(2) 0.9019(4) 0.4118(3) 0.0298(13) Uani 1 1 d . . . C2 C 0.0990(2) 0.8193(4) 0.4390(3) 0.0275(12) Uani 1 1 d . . . C3 C 0.1163(2) 0.8271(4) 0.3656(3) 0.0254(12) Uani 1 1 d . . . C4 C 0.1318(2) 0.7988(3) 0.3198(3) 0.0238(11) Uani 1 1 d . . . C5 C 0.1482(2) 0.8783(4) 0.2951(3) 0.0262(12) Uani 1 1 d . . . C6 C 0.1888(3) 0.9582(4) 0.2573(3) 0.0346(14) Uani 1 1 d . . . C7 C 0.1516(3) 1.0122(4) 0.2606(3) 0.0319(13) Uani 1 1 d . . . C8 C 0.0815(2) 0.7452(4) 0.2648(3) 0.0245(11) Uani 1 1 d . . . C9 C 0.0903(3) 0.7286(5) 0.2124(3) 0.0352(14) Uani 1 1 d . . . H9A H 0.1228 0.6913 0.2268 0.053 Uiso 1 1 calc R . . H9B H 0.0956 0.7854 0.1984 0.053 Uiso 1 1 calc R . . H9C H 0.0581 0.6986 0.1794 0.053 Uiso 1 1 calc R . . C10 C 0.0706(3) 0.6548(4) 0.2853(3) 0.0353(15) Uani 1 1 d . . . H10A H 0.1044 0.6196 0.3056 0.053 Uiso 1 1 calc R . . H10B H 0.0419 0.6224 0.2503 0.053 Uiso 1 1 calc R . . H10C H 0.0589 0.6660 0.3129 0.053 Uiso 1 1 calc R . . C11 C 0.2277(3) 0.7706(5) 0.4022(3) 0.0408(16) Uani 1 1 d . . . H11A H 0.2558 0.7242 0.4186 0.061 Uiso 1 1 calc R . . H11B H 0.2202 0.7883 0.4325 0.061 Uiso 1 1 calc R . . H11C H 0.2408 0.8221 0.3910 0.061 Uiso 1 1 calc R . . C12 C 0.1444(3) 0.6810(4) 0.4308(3) 0.0347(14) Uani 1 1 d . . . H12A H 0.1566 0.6582 0.4055 0.052 Uiso 1 1 calc R . . H12B H 0.1168 0.6409 0.4286 0.052 Uiso 1 1 calc R . . H12C H 0.1757 0.6847 0.4724 0.052 Uiso 1 1 calc R . . C13 C 0.2194(3) 0.7992(5) 0.2774(4) 0.0415(17) Uani 1 1 d . . . H13A H 0.2134 0.7457 0.2940 0.062 Uiso 1 1 calc R . . H13B H 0.2584 0.8149 0.3013 0.062 Uiso 1 1 calc R . . H13C H 0.2081 0.7881 0.2360 0.062 Uiso 1 1 calc R . . C14 C 0.0997(3) 0.7825(5) 0.4918(3) 0.0387(15) Uani 1 1 d . . . C15 C 0.0694(4) 0.7054(6) 0.4862(5) 0.057(2) Uani 1 1 d . . . H15A H 0.0465 0.6780 0.4483 0.068 Uiso 1 1 calc R . . C16 C 0.0739(6) 0.6698(8) 0.5381(6) 0.084(4) Uani 1 1 d . . . H16A H 0.0547 0.6170 0.5350 0.101 Uiso 1 1 calc R . . C17 C 0.1061(6) 0.7114(10) 0.5939(6) 0.089(5) Uani 1 1 d . . . H17A H 0.1091 0.6870 0.6285 0.106 Uiso 1 1 calc R . . C18 C 0.1330(5) 0.7876(10) 0.5978(4) 0.080(4) Uani 1 1 d . . . H18A H 0.1534 0.8170 0.6353 0.097 Uiso 1 1 calc R . . C19 C 0.1318(3) 0.8250(6) 0.5477(4) 0.053(2) Uani 1 1 d . . . H19A H 0.1520 0.8770 0.5519 0.064 Uiso 1 1 calc R . . C20 C 0.0567(3) 0.9760(5) 0.4258(3) 0.0345(14) Uani 1 1 d . . . C21 C 0.0030(3) 0.9685(7) 0.4123(4) 0.052(2) Uani 1 1 d . . . H21A H -0.0181 0.9171 0.3926 0.062 Uiso 1 1 calc R . . C22 C -0.0196(4) 1.0375(10) 0.4281(5) 0.079(4) Uani 1 1 d . . . H22A H -0.0558 1.0317 0.4190 0.095 Uiso 1 1 calc R . . C23 C 0.0098(5) 1.1130(7) 0.4563(5) 0.075(3) Uani 1 1 d . . . H23A H -0.0061 1.1583 0.4667 0.090 Uiso 1 1 calc R . . C24 C 0.0630(6) 1.1231(6) 0.4697(6) 0.082(3) Uani 1 1 d . . . H24A H 0.0831 1.1758 0.4882 0.099 Uiso 1 1 calc R . . C25 C 0.0868(4) 1.0538(6) 0.4552(5) 0.059(2) Uani 1 1 d . . . H25A H 0.1234 1.0596 0.4654 0.071 Uiso 1 1 calc R . . C26 C 0.2247(3) 0.9777(4) 0.2339(4) 0.0452(19) Uani 1 1 d . . . C27 C 0.2803(4) 0.9978(7) 0.2726(6) 0.078(3) Uani 1 1 d . . . H27A H 0.2965 0.9992 0.3146 0.093 Uiso 1 1 calc R . . C28 C 0.3125(5) 1.0164(7) 0.2481(7) 0.083(4) Uani 1 1 d . . . H28A H 0.3499 1.0319 0.2743 0.099 Uiso 1 1 calc R . . C29 C 0.2915(6) 1.0125(6) 0.1896(8) 0.091(5) Uani 1 1 d . . . H29A H 0.3140 1.0246 0.1747 0.109 Uiso 1 1 calc R . . C30 C 0.2367(7) 0.9906(10) 0.1504(8) 0.114(6) Uani 1 1 d . . . H30A H 0.2217 0.9877 0.1086 0.137 Uiso 1 1 calc R . . C31 C 0.2031(5) 0.9726(9) 0.1726(6) 0.087(4) Uani 1 1 d . . . H31A H 0.1658 0.9571 0.1457 0.105 Uiso 1 1 calc R . . C32 C 0.1400(3) 1.1093(4) 0.2485(3) 0.0356(15) Uani 1 1 d . . . C33 C 0.0875(4) 1.1422(5) 0.2144(4) 0.0485(19) Uani 1 1 d . . . H33A H 0.0577 1.1021 0.1938 0.058 Uiso 1 1 calc R . . C34 C 0.0769(5) 1.2349(6) 0.2092(5) 0.068(3) Uani 1 1 d . . . H34A H 0.0405 1.2570 0.1865 0.082 Uiso 1 1 calc R . . C35 C 0.1222(6) 1.2931(6) 0.2390(5) 0.082(4) Uani 1 1 d . . . H35A H 0.1160 1.3552 0.2358 0.099 Uiso 1 1 calc R . . C36 C 0.1757(5) 1.2616(6) 0.2727(5) 0.069(3) Uani 1 1 d . . . H36A H 0.2056 1.3019 0.2923 0.083 Uiso 1 1 calc R . . C37 C 0.1852(4) 1.1712(5) 0.2775(4) 0.051(2) Uani 1 1 d . . . H37A H 0.2217 1.1495 0.3000 0.062 Uiso 1 1 calc R . . C38 C 0.1391(4) 1.1829(5) 0.3791(4) 0.0494(19) Uani 1 1 d . . . C39 C 0.1755(5) 1.2598(6) 0.4146(5) 0.088(4) Uani 1 1 d . . . H39A H 0.2124 1.2380 0.4441 0.131 Uiso 1 1 calc R . . H39B H 0.1605 1.2899 0.4353 0.131 Uiso 1 1 calc R . . H39C H 0.1772 1.3016 0.3875 0.131 Uiso 1 1 calc R . . C42 C 0.2267(4) 0.5268(6) 0.0425(4) 0.051(2) Uani 1 1 d . . . C43 C 0.0470(10) 0.5925(19) -0.1173(11) 0.71(7) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0236(3) 0.0173(3) 0.0316(4) -0.0009(3) 0.0140(3) 0.0003(2) S1 0.0204(6) 0.0201(6) 0.0289(7) 0.0014(5) 0.0118(5) 0.0008(5) S2 0.0535(11) 0.0362(10) 0.0507(11) -0.0001(8) 0.0191(9) -0.0075(8) F1 0.094(4) 0.045(3) 0.092(4) -0.004(3) 0.052(4) 0.008(3) F2 0.068(3) 0.062(3) 0.082(4) -0.004(3) 0.042(3) -0.013(3) F3 0.065(3) 0.102(5) 0.045(3) 0.002(3) 0.010(3) -0.006(3) O1 0.022(3) 0.010(2) 0.043(3) 0.000 0.013(3) 0.000 O2 0.0207(19) 0.0220(19) 0.042(2) 0.0013(18) 0.0144(19) 0.0037(15) O3 0.075(4) 0.050(4) 0.047(3) 0.000(3) 0.007(3) -0.015(3) O4 0.061(4) 0.047(3) 0.081(5) -0.001(3) 0.035(4) 0.001(3) O5 0.077(4) 0.050(4) 0.084(5) -0.009(3) 0.041(4) -0.021(3) N1 0.018(2) 0.024(2) 0.027(2) -0.0018(19) 0.0113(19) 0.0008(17) N2 0.024(2) 0.021(2) 0.035(3) 0.000(2) 0.013(2) -0.0010(18) N3 0.023(2) 0.023(2) 0.029(3) 0.0019(19) 0.010(2) 0.0013(18) N4 0.031(3) 0.024(2) 0.050(3) 0.002(2) 0.027(3) -0.001(2) N5 0.041(3) 0.023(3) 0.041(3) -0.007(2) 0.018(3) -0.002(2) C1 0.019(3) 0.038(3) 0.026(3) -0.001(2) 0.008(2) 0.004(2) C2 0.021(3) 0.025(3) 0.030(3) 0.001(2) 0.010(2) 0.003(2) C3 0.012(2) 0.025(3) 0.029(3) 0.004(2) 0.003(2) 0.0033(19) C4 0.027(3) 0.012(2) 0.034(3) -0.001(2) 0.017(2) 0.0022(19) C5 0.021(3) 0.023(3) 0.031(3) 0.002(2) 0.011(2) 0.000(2) C6 0.037(3) 0.024(3) 0.050(4) -0.004(3) 0.028(3) -0.004(2) C7 0.033(3) 0.024(3) 0.042(4) -0.002(3) 0.023(3) -0.003(2) C8 0.020(2) 0.016(2) 0.032(3) -0.003(2) 0.011(2) 0.0017(19) C9 0.030(3) 0.037(3) 0.041(4) -0.012(3) 0.021(3) -0.002(3) C10 0.029(3) 0.018(3) 0.049(4) 0.002(3) 0.014(3) 0.003(2) C11 0.025(3) 0.039(4) 0.049(4) -0.001(3) 0.013(3) 0.006(3) C12 0.039(3) 0.024(3) 0.035(3) 0.011(3) 0.016(3) 0.012(2) C13 0.037(4) 0.032(3) 0.071(5) -0.002(3) 0.040(4) 0.003(3) C14 0.040(4) 0.043(4) 0.038(4) 0.014(3) 0.024(3) 0.016(3) C15 0.062(5) 0.057(5) 0.069(6) 0.017(4) 0.047(5) 0.010(4) C16 0.115(9) 0.074(7) 0.115(10) 0.051(7) 0.096(9) 0.043(7) C17 0.113(9) 0.115(10) 0.081(8) 0.067(8) 0.081(8) 0.078(8) C18 0.079(7) 0.122(10) 0.039(5) 0.025(6) 0.031(5) 0.064(7) C19 0.044(4) 0.069(5) 0.039(4) 0.009(4) 0.018(3) 0.029(4) C20 0.045(4) 0.035(3) 0.031(3) 0.007(3) 0.026(3) 0.013(3) C21 0.039(4) 0.070(5) 0.043(4) 0.002(4) 0.019(3) 0.015(4) C22 0.057(6) 0.132(10) 0.053(5) 0.015(6) 0.034(5) 0.052(7) C23 0.107(9) 0.062(6) 0.070(7) 0.010(5) 0.058(7) 0.041(6) C24 0.133(11) 0.037(5) 0.107(9) -0.013(5) 0.084(9) 0.010(6) C25 0.073(6) 0.042(4) 0.082(6) -0.013(4) 0.055(5) -0.002(4) C26 0.053(4) 0.024(3) 0.081(6) 0.005(3) 0.051(4) 0.001(3) C27 0.072(6) 0.070(6) 0.119(9) -0.043(6) 0.070(7) -0.039(5) C28 0.082(7) 0.061(6) 0.149(12) -0.046(7) 0.091(9) -0.035(5) C29 0.118(10) 0.040(5) 0.192(15) 0.034(7) 0.134(12) 0.022(6) C30 0.123(12) 0.139(12) 0.148(13) 0.092(11) 0.117(11) 0.072(10) C31 0.067(6) 0.132(10) 0.093(8) 0.062(8) 0.063(6) 0.054(7) C32 0.056(4) 0.021(3) 0.048(4) 0.001(3) 0.040(4) -0.005(3) C33 0.069(5) 0.033(4) 0.059(5) 0.014(3) 0.045(4) 0.013(3) C34 0.105(8) 0.036(4) 0.075(6) 0.017(4) 0.056(6) 0.022(5) C35 0.153(12) 0.023(4) 0.079(7) 0.010(4) 0.068(8) 0.010(5) C36 0.121(9) 0.028(4) 0.069(6) -0.004(4) 0.057(7) -0.021(5) C37 0.076(6) 0.035(4) 0.055(5) -0.005(3) 0.044(5) -0.013(4) C38 0.055(5) 0.041(4) 0.040(4) 0.000(3) 0.018(4) 0.003(3) C39 0.096(8) 0.036(5) 0.073(7) -0.012(4) 0.009(6) -0.015(5) C42 0.049(4) 0.041(4) 0.046(4) -0.003(3) 0.015(4) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.9187(17) . ? Zn1 N1 1.976(5) . ? Zn1 N2 1.991(5) . ? Zn1 N5 2.025(5) . ? S1 C8 1.855(5) . ? S1 S1 2.038(3) 2 ? S2 O4 1.430(6) . ? S2 O5 1.442(6) . ? S2 O3 1.444(6) . ? S2 C42 1.786(10) . ? S3 O8 1.453(12) . ? S3 O6 1.464(17) . ? S3 O7 1.540(18) . ? S3 C43 1.85(2) . ? F1 C42 1.339(10) . ? F2 C42 1.334(10) . ? F3 C42 1.327(9) . ? F4 C43 1.369(19) . ? F5 C43 1.351(19) . ? F6 C43 1.37(2) . ? O1 Zn1 1.9187(17) 2 ? O1 H1A 0.9300 . ? O2 C4 1.420(6) . ? O2 C11 1.451(8) . ? N1 C3 1.342(7) . ? N1 C1 1.391(8) . ? N2 C5 1.327(7) . ? N2 C7 1.390(8) . ? N3 C3 1.360(8) . ? N3 C2 1.390(8) . ? N3 C12 1.482(7) . ? N4 C5 1.368(8) . ? N4 C6 1.386(8) . ? N4 C13 1.462(8) . ? N5 C38 1.140(10) . ? C1 C2 1.360(8) . ? C1 C20 1.478(9) . ? C2 C14 1.470(9) . ? C3 C4 1.540(8) . ? C4 C5 1.530(8) . ? C4 C8 1.582(8) . ? C6 C7 1.369(9) . ? C6 C26 1.476(10) . ? C7 C32 1.467(8) . ? C8 C10 1.532(8) . ? C8 C9 1.535(9) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C19 1.379(11) . ? C14 C15 1.389(12) . ? C15 C16 1.393(13) . ? C15 H15A 0.9300 . ? C16 C17 1.373(19) . ? C16 H16A 0.9300 . ? C17 C18 1.334(18) . ? C17 H17A 0.9300 . ? C18 C19 1.403(14) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.377(11) . ? C20 C25 1.389(11) . ? C21 C22 1.382(13) . ? C21 H21A 0.9300 . ? C22 C23 1.348(17) . ? C22 H22A 0.9300 . ? C23 C24 1.367(17) . ? C23 H23A 0.9300 . ? C24 C25 1.388(12) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 C31 1.367(15) . ? C26 C27 1.369(13) . ? C27 C28 1.403(15) . ? C27 H27A 0.9300 . ? C28 C29 1.301(19) . ? C28 H28A 0.9300 . ? C29 C30 1.36(2) . ? C29 H29A 0.9300 . ? C30 C31 1.388(14) . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? C32 C33 1.350(11) . ? C32 C37 1.416(10) . ? C33 C34 1.394(11) . ? C33 H33A 0.9300 . ? C34 C35 1.385(16) . ? C34 H34A 0.9300 . ? C35 C36 1.362(17) . ? C35 H35A 0.9300 . ? C36 C37 1.356(12) . ? C36 H36A 0.9300 . ? C37 H37A 0.9300 . ? C38 C39 1.476(11) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? 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 N1 123.63(17) . . ? O1 Zn1 N2 123.98(15) . . ? N1 Zn1 N2 93.1(2) . . ? O1 Zn1 N5 101.0(2) . . ? N1 Zn1 N5 110.2(2) . . ? N2 Zn1 N5 103.6(2) . . ? C8 S1 S1 108.8(2) . 2 ? O4 S2 O5 116.3(4) . . ? O4 S2 O3 114.3(4) . . ? O5 S2 O3 114.8(4) . . ? O4 S2 C42 102.9(4) . . ? O5 S2 C42 102.7(4) . . ? O3 S2 C42 103.1(5) . . ? O8 S3 O6 115.8(14) . . ? O8 S3 O7 100.0(13) . . ? O6 S3 O7 125.5(18) . . ? O8 S3 C43 107.3(11) . . ? O6 S3 C43 99.8(15) . . ? O7 S3 C43 107.5(14) . . ? Zn1 O1 Zn1 143.6(3) 2 . ? Zn1 O1 H1A 108.2 2 . ? Zn1 O1 H1A 108.2 . . ? C4 O2 C11 115.2(4) . . ? C3 N1 C1 107.2(5) . . ? C3 N1 Zn1 125.1(4) . . ? C1 N1 Zn1 127.6(4) . . ? C5 N2 C7 108.0(5) . . ? C5 N2 Zn1 125.1(4) . . ? C7 N2 Zn1 126.3(4) . . ? C3 N3 C2 108.1(5) . . ? C3 N3 C12 131.6(5) . . ? C2 N3 C12 120.2(5) . . ? C5 N4 C6 107.8(5) . . ? C5 N4 C13 132.6(5) . . ? C6 N4 C13 119.5(5) . . ? C38 N5 Zn1 169.6(7) . . ? C2 C1 N1 108.8(5) . . ? C2 C1 C20 127.7(6) . . ? N1 C1 C20 123.5(6) . . ? C1 C2 N3 106.6(5) . . ? C1 C2 C14 130.4(6) . . ? N3 C2 C14 122.9(5) . . ? N1 C3 N3 109.4(5) . . ? N1 C3 C4 125.8(5) . . ? N3 C3 C4 124.6(5) . . ? O2 C4 C5 109.0(4) . . ? O2 C4 C3 108.9(5) . . ? C5 C4 C3 113.6(4) . . ? O2 C4 C8 105.4(4) . . ? C5 C4 C8 109.7(5) . . ? C3 C4 C8 109.8(5) . . ? N2 C5 N4 109.4(5) . . ? N2 C5 C4 125.9(5) . . ? N4 C5 C4 124.7(5) . . ? C7 C6 N4 106.7(6) . . ? C7 C6 C26 130.4(6) . . ? N4 C6 C26 122.9(6) . . ? C6 C7 N2 108.1(5) . . ? C6 C7 C32 130.4(6) . . ? N2 C7 C32 121.3(6) . . ? C10 C8 C9 109.5(5) . . ? C10 C8 C4 112.0(5) . . ? C9 C8 C4 112.4(5) . . ? C10 C8 S1 111.7(4) . . ? C9 C8 S1 100.4(4) . . ? C4 C8 S1 110.3(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O2 C11 H11A 109.5 . . ? O2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N3 C12 H12A 109.5 . . ? N3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 H13A 109.5 . . ? N4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 120.1(8) . . ? C19 C14 C2 119.0(7) . . ? C15 C14 C2 120.8(7) . . ? C14 C15 C16 119.0(10) . . ? C14 C15 H15A 120.5 . . ? C16 C15 H15A 120.5 . . ? C17 C16 C15 121.1(12) . . ? C17 C16 H16A 119.5 . . ? C15 C16 H16A 119.5 . . ? C18 C17 C16 118.9(9) . . ? C18 C17 H17A 120.5 . . ? C16 C17 H17A 120.5 . . ? C17 C18 C19 122.7(11) . . ? C17 C18 H18A 118.6 . . ? C19 C18 H18A 118.7 . . ? C14 C19 C18 118.1(10) . . ? C14 C19 H19A 121.0 . . ? C18 C19 H19A 120.9 . . ? C21 C20 C25 118.3(7) . . ? C21 C20 C1 121.1(7) . . ? C25 C20 C1 120.5(7) . . ? C20 C21 C22 119.8(10) . . ? C20 C21 H21A 120.1 . . ? C22 C21 H21A 120.1 . . ? C23 C22 C21 121.4(10) . . ? C23 C22 H22A 119.3 . . ? C21 C22 H22A 119.3 . . ? C22 C23 C24 120.3(9) . . ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 . . ? C23 C24 C25 119.1(10) . . ? C23 C24 H24A 120.4 . . ? C25 C24 H24A 120.4 . . ? C24 C25 C20 121.0(9) . . ? C24 C25 H25A 119.5 . . ? C20 C25 H25A 119.5 . . ? C31 C26 C27 118.5(9) . . ? C31 C26 C6 120.0(8) . . ? C27 C26 C6 121.5(9) . . ? C26 C27 C28 119.2(12) . . ? C26 C27 H27A 120.4 . . ? C28 C27 H27A 120.4 . . ? C29 C28 C27 121.9(11) . . ? C29 C28 H28A 119.0 . . ? C27 C28 H28A 119.0 . . ? C28 C29 C30 119.9(10) . . ? C28 C29 H29A 120.1 . . ? C30 C29 H29A 120.1 . . ? C29 C30 C31 120.1(14) . . ? C29 C30 H30A 119.9 . . ? C31 C30 H30A 120.0 . . ? C26 C31 C30 120.3(13) . . ? C26 C31 H31A 119.9 . . ? C30 C31 H31A 119.9 . . ? C33 C32 C37 118.7(7) . . ? C33 C32 C7 122.2(6) . . ? C37 C32 C7 119.0(7) . . ? C32 C33 C34 121.4(9) . . ? C32 C33 H33A 119.3 . . ? C34 C33 H33A 119.3 . . ? C35 C34 C33 118.1(10) . . ? C35 C34 H34A 121.0 . . ? C33 C34 H34A 121.0 . . ? C36 C35 C34 121.6(8) . . ? C36 C35 H35A 119.2 . . ? C34 C35 H35A 119.2 . . ? C37 C36 C35 119.5(10) . . ? C37 C36 H36A 120.2 . . ? C35 C36 H36A 120.2 . . ? C36 C37 C32 120.7(9) . . ? C36 C37 H37A 119.7 . . ? C32 C37 H37A 119.7 . . ? N5 C38 C39 178.7(9) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? F3 C42 F2 106.9(7) . . ? F3 C42 F1 105.8(7) . . ? F2 C42 F1 107.4(8) . . ? F3 C42 S2 112.2(7) . . ? F2 C42 S2 112.8(6) . . ? F1 C42 S2 111.4(6) . . ? F5 C43 F4 146(3) . . ? F5 C43 F6 109(2) . . ? F4 C43 F6 94(2) . . ? F5 C43 S3 100.5(16) . . ? F4 C43 S3 98.0(19) . . ? F6 C43 S3 103.1(17) . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 1.649 _refine_diff_density_min -2.245 _refine_diff_density_rms 0.154 #===END