# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1439 data_cks10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H42 B Cl6 I N6 S3 Zn' _chemical_formula_weight 1094.74 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.9632(9) _cell_length_b 22.3542(11) _cell_length_c 22.7952(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9663.0(8) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4400 _exptl_absorpt_coefficient_mu 1.643 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5595 _exptl_absorpt_correction_T_max 0.6385 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 67247 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 28.34 _reflns_number_total 11592 _reflns_number_gt 8543 _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^)+(0.0759P)^2^+33.6460P] 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 SHELXL _refine_ls_extinction_coef 0.00008(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11592 _refine_ls_number_parameters 519 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1751 _refine_ls_wR_factor_gt 0.1552 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.003 _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 Zn Zn 0.52528(3) 0.29544(2) 0.76172(2) 0.03792(14) Uani 1 1 d . . . I I 0.405336(17) 0.281187(19) 0.811886(17) 0.05816(13) Uani 1 1 d . . . S11 S 0.52430(6) 0.24404(5) 0.67120(5) 0.0388(2) Uani 1 1 d . . . S21 S 0.54359(6) 0.39765(5) 0.74197(6) 0.0428(3) Uani 1 1 d . . . S31 S 0.62366(6) 0.26033(6) 0.81424(5) 0.0432(3) Uani 1 1 d . . . B B 0.6851(3) 0.3194(2) 0.6806(2) 0.0387(10) Uani 1 1 d . . . H1 H 0.733(2) 0.326(2) 0.6562(19) 0.033(11) Uiso 1 1 d . . . N11 N 0.62381(19) 0.32763(16) 0.63598(16) 0.0375(8) Uani 1 1 d . . . N21 N 0.68461(18) 0.36664(17) 0.73060(17) 0.0386(8) Uani 1 1 d . . . N12 N 0.5303(2) 0.32137(17) 0.58003(16) 0.0398(8) Uani 1 1 d . . . N22 N 0.66245(19) 0.43687(17) 0.79477(18) 0.0415(8) Uani 1 1 d . . . N31 N 0.68949(18) 0.25492(17) 0.70502(17) 0.0378(8) Uani 1 1 d . . . N32 N 0.6919(2) 0.17235(17) 0.75605(16) 0.0399(8) Uani 1 1 d . . . C11 C 0.5622(2) 0.29882(18) 0.62892(19) 0.0357(9) Uani 1 1 d . . . C12 C 0.6312(3) 0.3682(2) 0.5900(2) 0.0487(11) Uani 1 1 d . . . H12A H 0.6699 0.3936 0.5838 0.058 Uiso 1 1 calc R . . C13 C 0.5739(3) 0.3649(2) 0.5563(2) 0.0490(11) Uani 1 1 d . . . H13A H 0.5648 0.3878 0.5225 0.059 Uiso 1 1 calc R . . C21 C 0.6325(2) 0.39994(19) 0.7552(2) 0.0385(9) Uani 1 1 d . . . C22 C 0.7479(2) 0.3834(2) 0.7571(2) 0.0482(11) Uani 1 1 d . . . H22A H 0.7925 0.3670 0.7490 0.058 Uiso 1 1 calc R . . C23 C 0.7344(2) 0.4268(2) 0.7961(2) 0.0490(12) Uani 1 1 d . . . H23A H 0.7676 0.4467 0.8198 0.059 Uiso 1 1 calc R . . C31 C 0.6696(2) 0.2299(2) 0.75637(19) 0.0374(9) Uani 1 1 d . . . C32 C 0.7234(3) 0.2112(2) 0.6723(2) 0.0449(11) Uani 1 1 d . . . H32A H 0.7419 0.2164 0.6344 0.054 Uiso 1 1 calc R . . C33 C 0.7256(3) 0.1607(2) 0.7033(2) 0.0468(11) Uani 1 1 d . . . H33A H 0.7460 0.1243 0.6916 0.056 Uiso 1 1 calc R . . C41 C 0.4624(2) 0.3039(2) 0.5579(2) 0.0406(10) Uani 1 1 d . . . C42 C 0.4589(3) 0.2638(2) 0.5112(2) 0.0472(11) Uani 1 1 d . . . C43 C 0.3922(3) 0.2473(3) 0.4913(2) 0.0586(14) Uani 1 1 d . . . H43A H 0.3884 0.2206 0.4596 0.070 Uiso 1 1 calc R . . C44 C 0.3310(3) 0.2696(3) 0.5176(3) 0.0614(15) Uani 1 1 d . . . C45 C 0.3373(3) 0.3101(3) 0.5625(2) 0.0553(13) Uani 1 1 d . . . H45A H 0.2961 0.3262 0.5791 0.066 Uiso 1 1 calc R . . C46 C 0.4021(3) 0.3283(2) 0.5845(2) 0.0458(11) Uani 1 1 d . . . C51 C 0.6254(2) 0.4791(2) 0.8314(2) 0.0412(10) Uani 1 1 d . . . C52 C 0.6059(2) 0.5341(2) 0.8072(2) 0.0445(10) Uani 1 1 d . . . C53 C 0.5702(3) 0.5742(2) 0.8427(2) 0.0487(11) Uani 1 1 d . . . H53A H 0.5557 0.6111 0.8271 0.058 Uiso 1 1 calc R . . C54 C 0.5555(3) 0.5611(2) 0.9008(3) 0.0525(12) Uani 1 1 d . . . C55 C 0.5775(3) 0.5068(2) 0.9235(3) 0.0561(13) Uani 1 1 d . . . H55A H 0.5690 0.4983 0.9633 0.067 Uiso 1 1 calc R . . C56 C 0.6120(3) 0.4644(2) 0.8890(2) 0.0505(12) Uani 1 1 d . . . C61 C 0.6901(3) 0.1314(2) 0.8052(2) 0.0424(10) Uani 1 1 d . . . C62 C 0.6368(3) 0.0889(2) 0.8077(2) 0.0520(12) Uani 1 1 d . . . C63 C 0.6389(3) 0.0494(3) 0.8550(3) 0.0604(14) Uani 1 1 d . . . H63A H 0.6036 0.0201 0.8582 0.072 Uiso 1 1 calc R . . C64 C 0.6906(3) 0.0519(3) 0.8971(3) 0.0602(14) Uani 1 1 d . . . C65 C 0.7425(3) 0.0954(2) 0.8922(2) 0.0554(13) Uani 1 1 d . . . H65A H 0.7782 0.0971 0.9208 0.066 Uiso 1 1 calc R . . C66 C 0.7435(3) 0.1364(2) 0.8468(2) 0.0460(11) Uani 1 1 d . . . C72 C 0.5247(3) 0.2393(3) 0.4831(3) 0.0632(15) Uani 1 1 d . . . H72A H 0.5499 0.2714 0.4637 0.095 Uiso 1 1 calc R . . H72B H 0.5119 0.2090 0.4546 0.095 Uiso 1 1 calc R . . H72C H 0.5545 0.2216 0.5130 0.095 Uiso 1 1 calc R . . C74 C 0.2593(4) 0.2490(4) 0.4962(3) 0.091(2) Uani 1 1 d . . . H74A H 0.2335 0.2312 0.5286 0.137 Uiso 1 1 calc R . . H74B H 0.2653 0.2196 0.4654 0.137 Uiso 1 1 calc R . . H74C H 0.2333 0.2830 0.4811 0.137 Uiso 1 1 calc R . . C76 C 0.4070(3) 0.3708(3) 0.6350(3) 0.0598(14) Uani 1 1 d . . . H76A H 0.3647 0.3951 0.6366 0.090 Uiso 1 1 calc R . . H76B H 0.4478 0.3964 0.6299 0.090 Uiso 1 1 calc R . . H76C H 0.4117 0.3483 0.6712 0.090 Uiso 1 1 calc R . . C82 C 0.6223(3) 0.5499(2) 0.7447(2) 0.0565(13) Uani 1 1 d . . . H82A H 0.6722 0.5437 0.7374 0.085 Uiso 1 1 calc R . . H82B H 0.6105 0.5915 0.7377 0.085 Uiso 1 1 calc R . . H82C H 0.5949 0.5246 0.7187 0.085 Uiso 1 1 calc R . . C84 C 0.5163(4) 0.6055(3) 0.9389(3) 0.078(2) Uani 1 1 d . . . H84A H 0.5138 0.5905 0.9787 0.116 Uiso 1 1 calc R . . H84B H 0.4689 0.6110 0.9237 0.116 Uiso 1 1 calc R . . H84C H 0.5409 0.6435 0.9386 0.116 Uiso 1 1 calc R . . C86 C 0.6316(4) 0.4040(3) 0.9140(3) 0.0730(18) Uani 1 1 d . . . H86A H 0.6006 0.3736 0.8979 0.109 Uiso 1 1 calc R . . H86B H 0.6268 0.4048 0.9563 0.109 Uiso 1 1 calc R . . H86C H 0.6800 0.3947 0.9037 0.109 Uiso 1 1 calc R . . C92 C 0.5796(4) 0.0862(3) 0.7621(3) 0.0772(19) Uani 1 1 d . . . H92A H 0.5507 0.1220 0.7646 0.116 Uiso 1 1 calc R . . H92B H 0.5504 0.0513 0.7688 0.116 Uiso 1 1 calc R . . H92C H 0.6007 0.0838 0.7234 0.116 Uiso 1 1 calc R . . C94 C 0.6908(5) 0.0084(3) 0.9483(3) 0.087(2) Uani 1 1 d . . . H94A H 0.7347 -0.0139 0.9484 0.131 Uiso 1 1 calc R . . H94B H 0.6515 -0.0191 0.9444 0.131 Uiso 1 1 calc R . . H94C H 0.6864 0.0304 0.9847 0.131 Uiso 1 1 calc R . . C96 C 0.7991(3) 0.1837(3) 0.8424(3) 0.0606(14) Uani 1 1 d . . . H96A H 0.8217 0.1814 0.8043 0.091 Uiso 1 1 calc R . . H96B H 0.8341 0.1776 0.8729 0.091 Uiso 1 1 calc R . . H96C H 0.7777 0.2228 0.8472 0.091 Uiso 1 1 calc R . . C11S C 0.5851(5) 0.5960(3) 0.5662(3) 0.093(3) Uani 1 1 d . . . H11A H 0.5811 0.6114 0.5255 0.111 Uiso 1 1 calc R . . Cl11 Cl 0.5552(2) 0.52401(15) 0.5674(2) 0.208(2) Uani 1 1 d . . . Cl12 Cl 0.66894(19) 0.5994(2) 0.58625(16) 0.1829(18) Uani 1 1 d . . . Cl13 Cl 0.5274(3) 0.63625(12) 0.61046(13) 0.1775(19) Uani 1 1 d . . . C21S C 0.3444(3) 0.4369(3) 0.8782(3) 0.0728(17) Uani 1 1 d . . . H21A H 0.3394 0.4019 0.8520 0.087 Uiso 1 1 calc R . . Cl21 Cl 0.42395(18) 0.46472(19) 0.8671(3) 0.248(3) Uani 1 1 d . . . Cl22 Cl 0.27651(16) 0.48559(12) 0.86148(17) 0.1426(12) Uani 1 1 d . . . Cl23 Cl 0.3311(2) 0.41172(16) 0.94881(12) 0.1465(12) 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 Zn 0.0311(2) 0.0436(3) 0.0390(3) -0.0014(2) 0.00076(19) 0.0029(2) I 0.03532(17) 0.0809(3) 0.0582(2) 0.01411(18) 0.00850(14) 0.00435(15) S11 0.0444(6) 0.0357(5) 0.0364(5) 0.0017(4) -0.0016(4) -0.0053(4) S21 0.0303(5) 0.0387(6) 0.0594(7) -0.0077(5) -0.0035(5) 0.0031(4) S31 0.0403(6) 0.0520(7) 0.0372(6) -0.0029(5) 0.0006(4) 0.0151(5) B 0.032(2) 0.040(3) 0.044(3) -0.001(2) 0.001(2) 0.0048(19) N11 0.0361(18) 0.0354(18) 0.041(2) 0.0026(15) 0.0024(15) 0.0016(14) N21 0.0290(16) 0.0405(19) 0.046(2) -0.0047(16) -0.0006(15) 0.0018(14) N12 0.0403(19) 0.041(2) 0.038(2) 0.0054(15) -0.0014(15) 0.0008(15) N22 0.0325(18) 0.041(2) 0.051(2) -0.0090(17) -0.0047(16) 0.0027(15) N31 0.0323(17) 0.0387(19) 0.042(2) -0.0026(15) 0.0001(15) 0.0065(15) N32 0.043(2) 0.0388(19) 0.0382(19) -0.0012(15) -0.0023(16) 0.0077(16) C11 0.040(2) 0.0303(19) 0.037(2) -0.0025(16) 0.0002(17) 0.0034(17) C12 0.049(3) 0.041(2) 0.057(3) 0.014(2) 0.004(2) 0.000(2) C13 0.049(3) 0.047(3) 0.051(3) 0.017(2) -0.001(2) -0.003(2) C21 0.0307(19) 0.037(2) 0.048(2) -0.0024(18) -0.0021(17) 0.0017(16) C22 0.030(2) 0.055(3) 0.060(3) -0.007(2) -0.006(2) 0.004(2) C23 0.030(2) 0.055(3) 0.061(3) -0.014(2) -0.009(2) 0.0011(19) C31 0.0307(19) 0.041(2) 0.040(2) -0.0047(18) -0.0032(16) 0.0065(17) C32 0.049(3) 0.044(3) 0.041(2) -0.0068(19) 0.005(2) 0.010(2) C33 0.053(3) 0.043(2) 0.044(3) -0.007(2) 0.003(2) 0.011(2) C41 0.045(2) 0.040(2) 0.036(2) 0.0071(18) -0.0038(18) 0.0004(19) C42 0.060(3) 0.045(3) 0.037(2) 0.0056(19) -0.001(2) -0.001(2) C43 0.083(4) 0.055(3) 0.038(3) 0.000(2) -0.015(3) -0.015(3) C44 0.057(3) 0.074(4) 0.054(3) 0.015(3) -0.018(3) -0.010(3) C45 0.048(3) 0.068(3) 0.050(3) 0.013(3) -0.009(2) -0.002(2) C46 0.047(3) 0.050(3) 0.040(2) 0.007(2) -0.006(2) 0.006(2) C51 0.036(2) 0.040(2) 0.048(3) -0.0086(19) -0.0038(19) 0.0015(18) C52 0.041(2) 0.039(2) 0.054(3) -0.002(2) -0.005(2) -0.0045(18) C53 0.048(3) 0.037(2) 0.060(3) -0.003(2) -0.005(2) 0.003(2) C54 0.054(3) 0.043(3) 0.061(3) -0.012(2) 0.006(2) 0.006(2) C55 0.069(3) 0.050(3) 0.049(3) -0.005(2) 0.008(3) 0.003(3) C56 0.057(3) 0.039(2) 0.055(3) -0.004(2) -0.001(2) 0.005(2) C61 0.044(2) 0.039(2) 0.044(2) -0.0017(19) -0.0011(19) 0.0099(19) C62 0.049(3) 0.054(3) 0.053(3) -0.002(2) -0.001(2) 0.003(2) C63 0.063(3) 0.052(3) 0.066(4) 0.005(3) 0.008(3) -0.002(3) C64 0.078(4) 0.052(3) 0.050(3) 0.004(2) 0.008(3) 0.016(3) C65 0.064(3) 0.058(3) 0.044(3) -0.001(2) -0.009(2) 0.017(3) C66 0.047(2) 0.044(2) 0.047(3) -0.004(2) -0.004(2) 0.012(2) C72 0.081(4) 0.056(3) 0.052(3) -0.005(3) 0.014(3) 0.004(3) C74 0.072(4) 0.119(6) 0.083(5) 0.014(5) -0.035(4) -0.029(4) C76 0.052(3) 0.068(4) 0.059(3) -0.012(3) -0.004(2) 0.020(3) C82 0.062(3) 0.048(3) 0.059(3) 0.004(2) 0.003(3) 0.001(2) C84 0.092(5) 0.060(4) 0.081(5) -0.015(3) 0.022(4) 0.018(3) C86 0.098(5) 0.053(3) 0.068(4) 0.009(3) 0.007(4) 0.018(3) C92 0.059(4) 0.086(5) 0.086(5) 0.009(4) -0.016(3) -0.018(3) C94 0.123(7) 0.074(4) 0.065(4) 0.021(3) 0.008(4) 0.014(4) C96 0.061(3) 0.052(3) 0.069(4) -0.002(3) -0.021(3) 0.004(3) C11S 0.149(8) 0.075(5) 0.053(4) 0.003(3) -0.019(4) 0.002(5) Cl11 0.194(3) 0.122(2) 0.307(5) -0.116(3) 0.120(4) -0.072(2) Cl12 0.142(3) 0.261(5) 0.146(3) 0.071(3) -0.074(2) -0.075(3) Cl13 0.346(6) 0.0832(15) 0.1028(19) 0.0238(14) 0.078(3) 0.063(2) C21S 0.063(4) 0.076(4) 0.079(4) -0.010(3) -0.002(3) -0.005(3) Cl21 0.098(2) 0.171(3) 0.475(9) 0.031(5) 0.104(4) -0.039(2) Cl22 0.126(2) 0.0940(16) 0.208(3) 0.0201(19) -0.058(2) 0.0104(15) Cl23 0.199(3) 0.159(3) 0.0819(15) 0.0015(16) -0.0119(18) 0.037(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn S31 2.3517(12) . ? Zn S21 2.3545(13) . ? Zn S11 2.3617(12) . ? Zn I 2.5657(6) . ? S11 C11 1.716(4) . ? S21 C21 1.714(4) . ? S31 C31 1.721(4) . ? B N31 1.548(6) . ? B N21 1.553(6) . ? B N11 1.556(6) . ? N11 C11 1.344(6) . ? N11 C12 1.393(6) . ? N21 C21 1.358(5) . ? N21 C22 1.396(6) . ? N12 C11 1.364(6) . ? N12 C13 1.387(6) . ? N12 C41 1.437(6) . ? N22 C21 1.348(6) . ? N22 C23 1.384(6) . ? N22 C51 1.444(6) . ? N31 C31 1.351(6) . ? N31 C32 1.388(6) . ? N32 C31 1.354(6) . ? N32 C33 1.387(6) . ? N32 C61 1.447(6) . ? C12 C13 1.332(7) . ? C22 C23 1.341(7) . ? C32 C33 1.332(7) . ? C41 C42 1.392(7) . ? C41 C46 1.405(7) . ? C42 C43 1.393(8) . ? C42 C72 1.505(8) . ? C43 C44 1.398(9) . ? C44 C45 1.374(9) . ? C44 C74 1.514(8) . ? C45 C46 1.387(7) . ? C46 C76 1.494(7) . ? C51 C56 1.378(7) . ? C51 C52 1.396(7) . ? C52 C53 1.385(7) . ? C52 C82 1.501(7) . ? C53 C54 1.384(8) . ? C54 C55 1.383(8) . ? C54 C84 1.515(7) . ? C55 C56 1.395(7) . ? C56 C86 1.513(8) . ? C61 C62 1.388(7) . ? C61 C66 1.392(7) . ? C62 C63 1.394(8) . ? C62 C92 1.504(8) . ? C63 C64 1.372(9) . ? C64 C65 1.389(9) . ? C64 C94 1.519(8) . ? C65 C66 1.383(7) . ? C66 C96 1.497(8) . ? C11S Cl12 1.657(10) . ? C11S Cl11 1.707(8) . ? C11S Cl13 1.738(9) . ? C21S Cl21 1.652(7) . ? C21S Cl23 1.722(8) . ? C21S Cl22 1.729(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S31 Zn S21 107.71(5) . . ? S31 Zn S11 106.78(4) . . ? S21 Zn S11 107.83(5) . . ? S31 Zn I 115.78(4) . . ? S21 Zn I 109.66(3) . . ? S11 Zn I 108.79(3) . . ? C11 S11 Zn 98.06(15) . . ? C21 S21 Zn 98.08(16) . . ? C31 S31 Zn 98.24(15) . . ? N31 B N21 111.7(4) . . ? N31 B N11 112.6(4) . . ? N21 B N11 113.3(4) . . ? C11 N11 C12 108.0(4) . . ? C11 N11 B 132.2(4) . . ? C12 N11 B 119.6(4) . . ? C21 N21 C22 107.4(4) . . ? C21 N21 B 132.9(4) . . ? C22 N21 B 119.7(4) . . ? C11 N12 C13 108.3(4) . . ? C11 N12 C41 125.6(4) . . ? C13 N12 C41 126.1(4) . . ? C21 N22 C23 109.3(4) . . ? C21 N22 C51 125.7(4) . . ? C23 N22 C51 125.0(4) . . ? C31 N31 C32 107.7(4) . . ? C31 N31 B 133.0(4) . . ? C32 N31 B 119.2(4) . . ? C31 N32 C33 109.1(4) . . ? C31 N32 C61 126.1(4) . . ? C33 N32 C61 124.3(4) . . ? N11 C11 N12 107.8(4) . . ? N11 C11 S11 129.7(3) . . ? N12 C11 S11 122.5(3) . . ? C13 C12 N11 108.4(4) . . ? C12 C13 N12 107.5(4) . . ? N22 C21 N21 107.8(4) . . ? N22 C21 S21 123.4(3) . . ? N21 C21 S21 128.8(3) . . ? C23 C22 N21 108.5(4) . . ? C22 C23 N22 106.9(4) . . ? N31 C31 N32 107.6(4) . . ? N31 C31 S31 129.9(3) . . ? N32 C31 S31 122.5(4) . . ? C33 C32 N31 109.0(4) . . ? C32 C33 N32 106.6(4) . . ? C42 C41 C46 122.8(5) . . ? C42 C41 N12 119.1(4) . . ? C46 C41 N12 118.1(4) . . ? C41 C42 C43 117.5(5) . . ? C41 C42 C72 121.3(5) . . ? C43 C42 C72 121.1(5) . . ? C42 C43 C44 121.4(5) . . ? C45 C44 C43 118.8(5) . . ? C45 C44 C74 121.2(6) . . ? C43 C44 C74 120.0(6) . . ? C44 C45 C46 122.7(6) . . ? C45 C46 C41 116.8(5) . . ? C45 C46 C76 121.3(5) . . ? C41 C46 C76 121.9(4) . . ? C56 C51 C52 122.5(4) . . ? C56 C51 N22 119.0(4) . . ? C52 C51 N22 118.4(4) . . ? C53 C52 C51 117.9(5) . . ? C53 C52 C82 120.3(5) . . ? C51 C52 C82 121.8(5) . . ? C54 C53 C52 121.3(5) . . ? C55 C54 C53 119.0(5) . . ? C55 C54 C84 120.5(5) . . ? C53 C54 C84 120.5(5) . . ? C54 C55 C56 121.7(5) . . ? C51 C56 C55 117.5(5) . . ? C51 C56 C86 121.8(5) . . ? C55 C56 C86 120.7(5) . . ? C62 C61 C66 123.8(5) . . ? C62 C61 N32 118.8(4) . . ? C66 C61 N32 117.4(4) . . ? C61 C62 C63 116.4(5) . . ? C61 C62 C92 121.6(5) . . ? C63 C62 C92 122.0(5) . . ? C64 C63 C62 122.4(6) . . ? C63 C64 C65 118.6(5) . . ? C63 C64 C94 120.9(6) . . ? C65 C64 C94 120.5(6) . . ? C66 C65 C64 122.2(5) . . ? C65 C66 C61 116.6(5) . . ? C65 C66 C96 121.8(5) . . ? C61 C66 C96 121.6(5) . . ? Cl12 C11S Cl11 110.9(5) . . ? Cl12 C11S Cl13 114.8(5) . . ? Cl11 C11S Cl13 105.6(5) . . ? Cl21 C21S Cl23 113.6(5) . . ? Cl21 C21S Cl22 114.1(5) . . ? Cl23 C21S Cl22 107.7(4) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.818 _refine_diff_density_min -1.451 _refine_diff_density_rms 0.104 data_new _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H48 B Cl N6 O6 S3 Zn' _chemical_formula_weight 892.63 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.5920(11) _cell_length_b 16.3598(12) _cell_length_c 20.1484(15) _cell_angle_alpha 90.00 _cell_angle_beta 92.037(2) _cell_angle_gamma 90.00 _cell_volume 4477.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 0.797 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8569 _exptl_absorpt_correction_T_max 0.9246 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30788 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0692 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.23 _reflns_number_total 10237 _reflns_number_gt 5578 _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^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00016(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10237 _refine_ls_number_parameters 566 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.1113 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1194 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.002 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 Zn Zn 0.78744(3) 0.63464(2) 0.197950(17) 0.04630(13) Uani 1 1 d . . . S11 S 0.79810(6) 0.67204(5) 0.08643(4) 0.0514(2) Uani 1 1 d . . . S12 S 0.74386(6) 0.49821(5) 0.20788(4) 0.0477(2) Uani 1 1 d . . . S13 S 0.93743(6) 0.65727(4) 0.25273(4) 0.0476(2) Uani 1 1 d . . . B B 0.9654(3) 0.5159(2) 0.12578(18) 0.0473(9) Uani 1 1 d . . . H01 H 1.0185(17) 0.4807(14) 0.0994(11) 0.029(6) Uiso 1 1 d . . . N11 N 0.98482(18) 0.60610(14) 0.10551(12) 0.0443(6) Uani 1 1 d . . . N12 N 0.9814(2) 0.73385(15) 0.07473(13) 0.0510(7) Uani 1 1 d . . . N21 N 0.86274(19) 0.48398(14) 0.09987(12) 0.0458(6) Uani 1 1 d . . . N22 N 0.70971(19) 0.44712(14) 0.08067(12) 0.0471(6) Uani 1 1 d . . . N31 N 0.98621(17) 0.50470(14) 0.20092(12) 0.0462(6) Uani 1 1 d . . . N32 N 1.01936(19) 0.52241(14) 0.30692(12) 0.0498(7) Uani 1 1 d . . . C1 C 0.6686(4) 0.7862(3) 0.2384(2) 0.1131(16) Uani 1 1 d . . . H1A H 0.7310 0.8134 0.2477 0.170 Uiso 1 1 calc R . . H1B H 0.6215 0.8030 0.2708 0.170 Uiso 1 1 calc R . . H1C H 0.6440 0.8010 0.1942 0.170 Uiso 1 1 calc R . . O1 O 0.6825(2) 0.69742(17) 0.24216(14) 0.0722(8) Uani 1 1 d . . . H1 H 0.642(3) 0.666(2) 0.2498(19) 0.068(15) Uiso 1 1 d . . . C2 C 0.4830(6) 0.5594(3) 0.2632(4) 0.195(4) Uani 1 1 d D . . H2A H 0.4713 0.5368 0.3067 0.292 Uiso 1 1 calc R . . H2B H 0.5350 0.5289 0.2427 0.292 Uiso 1 1 calc R . . H2C H 0.4232 0.5559 0.2357 0.292 Uiso 1 1 calc R . . O2 O 0.5114(3) 0.6418(3) 0.2699(2) 0.1536(16) Uani 1 1 d D . . H2 H 0.4896 0.6681 0.2373 0.230 Uiso 1 1 calc R . . C11 C 0.9245(2) 0.66845(18) 0.08856(14) 0.0450(7) Uani 1 1 d . . . C12 C 1.0808(2) 0.6348(2) 0.10519(15) 0.0510(8) Uani 1 1 d . . . H12A H 1.1377 0.6044 0.1166 0.061 Uiso 1 1 calc R . . C13 C 1.0787(2) 0.7130(2) 0.08583(16) 0.0562(9) Uani 1 1 d . . . H13A H 1.1334 0.7473 0.0808 0.067 Uiso 1 1 calc R . . C21 C 0.7749(2) 0.47628(16) 0.12792(14) 0.0445(7) Uani 1 1 d . . . C22 C 0.8519(3) 0.45850(19) 0.03433(16) 0.0560(9) Uani 1 1 d . . . H22A H 0.9020 0.4574 0.0033 0.067 Uiso 1 1 calc R . . C23 C 0.7590(3) 0.43589(19) 0.02266(16) 0.0592(9) Uani 1 1 d . . . H23A H 0.7318 0.4159 -0.0177 0.071 Uiso 1 1 calc R . . C31 C 0.9806(2) 0.55849(17) 0.25162(14) 0.0424(7) Uani 1 1 d . . . C32 C 1.0298(2) 0.43382(18) 0.22618(18) 0.0571(9) Uani 1 1 d . . . H32A H 1.0425 0.3862 0.2019 0.068 Uiso 1 1 calc R . . C33 C 1.0506(3) 0.44485(19) 0.29068(18) 0.0625(9) Uani 1 1 d . . . H33A H 1.0809 0.4068 0.3198 0.075 Uiso 1 1 calc R . . C41 C 0.9469(2) 0.81064(19) 0.04914(18) 0.0563(9) Uani 1 1 d . . . C42 C 0.9422(3) 0.8211(2) -0.0199(2) 0.0674(10) Uani 1 1 d . . . C43 C 0.9095(3) 0.8961(3) -0.0439(2) 0.0815(12) Uani 1 1 d . . . H43A H 0.9063 0.9048 -0.0900 0.098 Uiso 1 1 calc R . . C44 C 0.8819(3) 0.9579(3) -0.0029(3) 0.0787(13) Uani 1 1 d . . . C45 C 0.8885(3) 0.9453(2) 0.0652(3) 0.0810(12) Uani 1 1 d . . . H45A H 0.8696 0.9875 0.0936 0.097 Uiso 1 1 calc R . . C46 C 0.9223(3) 0.8719(2) 0.0928(2) 0.0677(10) Uani 1 1 d . . . C51 C 0.6083(2) 0.42583(19) 0.09214(15) 0.0505(8) Uani 1 1 d . . . C52 C 0.5869(3) 0.3438(2) 0.10290(16) 0.0590(9) Uani 1 1 d . . . C55 C 0.4425(3) 0.4628(2) 0.10541(18) 0.0722(10) Uani 1 1 d . . . H55A H 0.3930 0.5029 0.1063 0.087 Uiso 1 1 calc R . . C53 C 0.4901(3) 0.3247(2) 0.11594(18) 0.0730(11) Uani 1 1 d . . . H53A H 0.4737 0.2698 0.1240 0.088 Uiso 1 1 calc R . . C54 C 0.4177(3) 0.3824(3) 0.1175(2) 0.0765(11) Uani 1 1 d . . . C56 C 0.5383(3) 0.4866(2) 0.09198(16) 0.0557(9) Uani 1 1 d . . . C61 C 1.0345(2) 0.56233(18) 0.37019(15) 0.0493(8) Uani 1 1 d . . . C62 C 1.1249(2) 0.5999(2) 0.38264(17) 0.0580(9) Uani 1 1 d . . . C63 C 1.1386(3) 0.6397(2) 0.44360(19) 0.0646(10) Uani 1 1 d . . . H63A H 1.1991 0.6655 0.4537 0.078 Uiso 1 1 calc R . . C64 C 1.0650(3) 0.6420(2) 0.48970(17) 0.0636(10) Uani 1 1 d . . . C65 C 0.9771(3) 0.6032(2) 0.47419(17) 0.0616(9) Uani 1 1 d . . . H65A H 0.9272 0.6042 0.5052 0.074 Uiso 1 1 calc R . . C66 C 0.9599(2) 0.56304(18) 0.41465(16) 0.0524(8) Uani 1 1 d . . . C72 C 0.9689(4) 0.7523(3) -0.0664(2) 0.1008(15) Uani 1 1 d . . . H72A H 0.9257 0.7061 -0.0598 0.151 Uiso 1 1 calc R . . H72B H 1.0366 0.7359 -0.0572 0.151 Uiso 1 1 calc R . . H72C H 0.9616 0.7710 -0.1120 0.151 Uiso 1 1 calc R . . C74 C 0.8447(3) 1.0391(2) -0.0301(3) 0.1142(18) Uani 1 1 d . . . H74A H 0.7762 1.0336 -0.0446 0.171 Uiso 1 1 calc R . . H74B H 0.8834 1.0551 -0.0675 0.171 Uiso 1 1 calc R . . H74C H 0.8506 1.0804 0.0043 0.171 Uiso 1 1 calc R . . C76 C 0.9313(4) 0.8603(2) 0.1669(2) 0.1042(16) Uani 1 1 d . . . H76A H 0.9001 0.8092 0.1788 0.156 Uiso 1 1 calc R . . H76B H 0.8992 0.9053 0.1888 0.156 Uiso 1 1 calc R . . H76C H 1.0003 0.8588 0.1809 0.156 Uiso 1 1 calc R . . C82 C 0.6651(3) 0.2786(2) 0.1000(2) 0.0787(11) Uani 1 1 d . . . H82A H 0.6438 0.2303 0.1235 0.118 Uiso 1 1 calc R . . H82B H 0.7259 0.2988 0.1205 0.118 Uiso 1 1 calc R . . H82C H 0.6758 0.2647 0.0540 0.118 Uiso 1 1 calc R . . C84 C 0.3124(3) 0.3595(3) 0.1320(3) 0.127(2) Uani 1 1 d . . . H84A H 0.2824 0.3322 0.0936 0.190 Uiso 1 1 calc R . . H84B H 0.2754 0.4086 0.1415 0.190 Uiso 1 1 calc R . . H84C H 0.3120 0.3232 0.1700 0.190 Uiso 1 1 calc R . . C86 C 0.5607(3) 0.57492(19) 0.07759(18) 0.0678(10) Uani 1 1 d . . . H86A H 0.5004 0.6029 0.0637 0.102 Uiso 1 1 calc R . . H86B H 0.6074 0.5781 0.0424 0.102 Uiso 1 1 calc R . . H86C H 0.5885 0.6007 0.1173 0.102 Uiso 1 1 calc R . . C92 C 1.2023(3) 0.6032(3) 0.33145(19) 0.0853(12) Uani 1 1 d . . . H92A H 1.2287 0.5488 0.3249 0.128 Uiso 1 1 calc R . . H92B H 1.2548 0.6396 0.3465 0.128 Uiso 1 1 calc R . . H92C H 1.1734 0.6232 0.2899 0.128 Uiso 1 1 calc R . . C94 C 1.0810(3) 0.6885(3) 0.55392(19) 0.0946(14) Uani 1 1 d . . . H94A H 1.1482 0.6807 0.5705 0.142 Uiso 1 1 calc R . . H94B H 1.0359 0.6684 0.5864 0.142 Uiso 1 1 calc R . . H94C H 1.0690 0.7462 0.5461 0.142 Uiso 1 1 calc R . . C96 C 0.8610(3) 0.5247(2) 0.39783(18) 0.0760(11) Uani 1 1 d . . . H96A H 0.8171 0.5656 0.3784 0.114 Uiso 1 1 calc R . . H96B H 0.8331 0.5033 0.4380 0.114 Uiso 1 1 calc R . . H96C H 0.8692 0.4806 0.3664 0.114 Uiso 1 1 calc R . . Cl1 Cl 0.3380(12) 0.7271(10) 0.1534(7) 0.1017(9) Uani 0.232(5) 1 d PD A 1 O11 O 0.4350(11) 0.7514(10) 0.1706(9) 0.077(7) Uani 0.232(5) 1 d PD A 1 O12 O 0.2694(10) 0.7854(9) 0.1720(10) 0.096(7) Uani 0.232(5) 1 d PD A 1 O13 O 0.3310(11) 0.7141(10) 0.0843(5) 0.099(5) Uani 0.232(5) 1 d PD A 1 O14 O 0.3183(13) 0.6550(10) 0.1872(8) 0.121(8) Uani 0.232(5) 1 d PD A 1 Cl2 Cl 0.3278(3) 0.7357(3) 0.1569(2) 0.1017(9) Uani 0.77 1 d PD A 2 O21 O 0.4196(5) 0.7448(5) 0.1861(5) 0.173(4) Uani 0.768(5) 1 d PD A 2 O22 O 0.2589(7) 0.7481(8) 0.2061(4) 0.244(6) Uani 0.768(5) 1 d PD A 2 O23 O 0.3081(6) 0.7993(5) 0.1129(5) 0.218(4) Uani 0.768(5) 1 d PD A 2 O24 O 0.3127(5) 0.6600(4) 0.1329(6) 0.217(6) Uani 0.768(5) 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 Zn 0.0505(2) 0.0395(2) 0.0491(2) -0.00270(16) 0.00378(16) 0.00302(17) S11 0.0479(5) 0.0520(5) 0.0543(5) 0.0094(4) -0.0002(4) -0.0066(4) S12 0.0588(5) 0.0435(4) 0.0412(4) -0.0025(3) 0.0094(4) -0.0049(4) S13 0.0567(5) 0.0372(4) 0.0487(5) -0.0046(3) -0.0040(4) 0.0061(4) B 0.053(2) 0.041(2) 0.049(2) -0.0077(16) 0.0092(18) 0.0011(17) N11 0.0473(16) 0.0429(14) 0.0432(15) -0.0040(11) 0.0056(12) -0.0043(12) N12 0.0522(18) 0.0451(15) 0.0560(17) 0.0039(12) 0.0063(13) -0.0096(13) N21 0.0562(17) 0.0388(14) 0.0428(15) -0.0077(11) 0.0075(13) -0.0055(12) N22 0.0537(17) 0.0441(14) 0.0437(16) -0.0050(11) 0.0057(13) -0.0114(12) N31 0.0507(16) 0.0374(13) 0.0507(16) -0.0031(12) 0.0046(12) 0.0061(12) N32 0.0597(17) 0.0386(14) 0.0509(17) 0.0025(12) -0.0027(13) 0.0094(12) C1 0.122(4) 0.097(4) 0.121(4) -0.020(3) 0.004(3) 0.025(3) O1 0.070(2) 0.0545(17) 0.093(2) -0.0139(14) 0.0148(15) 0.0117(15) C2 0.273(10) 0.167(7) 0.143(6) -0.018(6) -0.014(6) 0.086(7) O2 0.098(3) 0.241(5) 0.121(3) 0.029(4) 0.008(2) 0.009(3) C11 0.0486(19) 0.0470(17) 0.0395(18) -0.0029(14) 0.0025(14) -0.0084(16) C12 0.043(2) 0.055(2) 0.055(2) -0.0115(16) 0.0068(15) -0.0031(16) C13 0.047(2) 0.055(2) 0.067(2) -0.0080(17) 0.0094(17) -0.0128(16) C21 0.058(2) 0.0317(15) 0.0446(18) -0.0007(13) 0.0071(16) -0.0057(14) C22 0.069(2) 0.055(2) 0.044(2) -0.0134(15) 0.0135(17) -0.0122(18) C23 0.076(3) 0.061(2) 0.041(2) -0.0142(16) 0.0091(18) -0.0143(18) C31 0.0428(18) 0.0398(17) 0.0444(18) 0.0005(14) 0.0000(14) 0.0021(13) C32 0.063(2) 0.0408(18) 0.068(2) -0.0024(16) 0.0080(18) 0.0100(16) C33 0.072(2) 0.049(2) 0.066(3) 0.0073(17) -0.0008(19) 0.0204(18) C41 0.050(2) 0.0472(19) 0.072(3) 0.0126(18) 0.0043(17) -0.0127(16) C42 0.058(2) 0.066(2) 0.078(3) 0.018(2) -0.0049(19) -0.0197(19) C43 0.069(3) 0.083(3) 0.092(3) 0.030(3) -0.013(2) -0.022(2) C44 0.046(2) 0.069(3) 0.120(4) 0.038(3) -0.004(2) -0.017(2) C45 0.064(3) 0.052(2) 0.128(4) 0.010(2) 0.018(3) -0.0090(19) C46 0.067(3) 0.052(2) 0.085(3) 0.012(2) 0.013(2) -0.0024(18) C51 0.059(2) 0.0488(19) 0.0439(19) -0.0019(15) 0.0020(16) -0.0173(17) C52 0.071(3) 0.053(2) 0.053(2) 0.0000(16) -0.0024(18) -0.0179(18) C55 0.061(3) 0.077(3) 0.079(3) -0.007(2) 0.003(2) -0.009(2) C53 0.080(3) 0.064(2) 0.075(3) 0.009(2) 0.000(2) -0.033(2) C54 0.064(3) 0.081(3) 0.084(3) 0.001(2) 0.007(2) -0.028(2) C56 0.059(2) 0.056(2) 0.052(2) -0.0041(16) -0.0019(16) -0.0127(18) C61 0.054(2) 0.0488(18) 0.0443(19) 0.0048(15) -0.0055(16) 0.0070(16) C62 0.050(2) 0.070(2) 0.053(2) 0.0074(18) -0.0029(17) 0.0077(18) C63 0.058(2) 0.066(2) 0.069(3) 0.0056(19) -0.012(2) -0.0009(18) C64 0.073(3) 0.060(2) 0.056(2) 0.0000(18) -0.005(2) 0.008(2) C65 0.068(3) 0.066(2) 0.052(2) 0.0032(18) 0.0095(18) 0.0022(19) C66 0.054(2) 0.053(2) 0.050(2) 0.0081(16) 0.0022(17) 0.0004(16) C72 0.133(4) 0.103(3) 0.066(3) 0.005(2) -0.002(3) -0.022(3) C74 0.074(3) 0.083(3) 0.185(5) 0.070(3) -0.002(3) -0.004(2) C76 0.157(5) 0.058(2) 0.100(4) 0.000(2) 0.036(3) 0.006(3) C82 0.090(3) 0.048(2) 0.099(3) 0.012(2) 0.002(2) -0.012(2) C84 0.080(4) 0.129(4) 0.172(6) 0.013(4) 0.021(3) -0.042(3) C86 0.070(3) 0.055(2) 0.079(3) 0.0018(18) -0.0017(19) -0.0070(18) C92 0.059(3) 0.123(4) 0.074(3) -0.003(2) 0.001(2) -0.002(2) C94 0.122(4) 0.088(3) 0.074(3) -0.027(2) -0.005(3) -0.002(3) C96 0.073(3) 0.084(3) 0.071(3) 0.000(2) 0.009(2) -0.020(2) Cl1 0.0732(14) 0.0825(15) 0.1486(16) -0.0117(11) -0.0074(10) -0.0177(11) O11 0.050(10) 0.058(10) 0.128(14) -0.017(8) 0.052(10) -0.042(7) O12 0.058(9) 0.090(12) 0.140(17) -0.090(13) -0.010(9) 0.029(8) O13 0.173(14) 0.079(10) 0.045(7) -0.022(6) 0.003(7) -0.041(10) O14 0.160(17) 0.098(13) 0.107(12) -0.020(10) 0.041(12) -0.094(12) Cl2 0.0732(14) 0.0825(15) 0.1486(16) -0.0117(11) -0.0074(10) -0.0177(11) O21 0.133(7) 0.113(5) 0.263(9) 0.033(5) -0.112(6) -0.024(5) O22 0.251(10) 0.342(14) 0.142(7) -0.022(7) 0.060(7) -0.040(9) O23 0.205(7) 0.164(7) 0.276(9) 0.128(7) -0.093(7) -0.063(5) O24 0.109(5) 0.115(5) 0.420(16) -0.132(8) -0.074(8) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn O1 1.993(3) . ? Zn S13 2.3134(9) . ? Zn S12 2.3197(8) . ? Zn S11 2.3381(9) . ? S11 C11 1.718(3) . ? S12 C21 1.718(3) . ? S13 C31 1.720(3) . ? B N31 1.541(4) . ? B N11 1.557(4) . ? B N21 1.562(4) . ? N11 C11 1.345(4) . ? N11 C12 1.387(4) . ? N12 C11 1.355(4) . ? N12 C13 1.376(4) . ? N12 C41 1.431(4) . ? N21 C21 1.344(4) . ? N21 C22 1.388(4) . ? N22 C21 1.364(3) . ? N22 C23 1.380(4) . ? N22 C51 1.448(4) . ? N31 C31 1.353(3) . ? N31 C32 1.391(4) . ? N32 C31 1.351(3) . ? N32 C33 1.381(4) . ? N32 C61 1.441(4) . ? C1 O1 1.467(5) . ? O1 H1 0.77(3) . ? C2 O2 1.4062(10) . ? C12 C13 1.338(4) . ? C22 C23 1.330(4) . ? C32 C33 1.332(4) . ? C41 C46 1.381(5) . ? C41 C42 1.400(5) . ? C42 C43 1.386(5) . ? C42 C72 1.518(5) . ? C43 C44 1.366(6) . ? C44 C45 1.387(5) . ? C44 C74 1.516(5) . ? C45 C46 1.394(5) . ? C46 C76 1.508(5) . ? C51 C56 1.376(4) . ? C51 C52 1.392(4) . ? C52 C53 1.386(5) . ? C52 C82 1.509(5) . ? C55 C54 1.382(5) . ? C55 C56 1.395(5) . ? C53 C54 1.365(5) . ? C54 C84 1.518(5) . ? C56 C86 1.507(4) . ? C61 C66 1.376(4) . ? C61 C62 1.389(4) . ? C62 C63 1.397(5) . ? C62 C92 1.500(5) . ? C63 C64 1.389(5) . ? C64 C65 1.379(5) . ? C64 C94 1.510(5) . ? C65 C66 1.381(4) . ? C66 C96 1.512(4) . ? Cl1 O14 1.392(15) . ? Cl1 O12 1.395(14) . ? Cl1 O11 1.409(15) . ? Cl1 O13 1.410(15) . ? Cl2 O24 1.343(6) . ? Cl2 O21 1.368(6) . ? Cl2 O23 1.387(7) . ? Cl2 O22 1.402(8) . ? 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 Zn S13 109.68(9) . . ? O1 Zn S12 105.56(10) . . ? S13 Zn S12 109.64(3) . . ? O1 Zn S11 111.37(9) . . ? S13 Zn S11 109.45(3) . . ? S12 Zn S11 111.06(3) . . ? C11 S11 Zn 93.62(10) . . ? C21 S12 Zn 92.75(10) . . ? C31 S13 Zn 97.97(10) . . ? N31 B N11 110.1(2) . . ? N31 B N21 114.8(3) . . ? N11 B N21 112.8(3) . . ? C11 N11 C12 107.9(2) . . ? C11 N11 B 132.7(3) . . ? C12 N11 B 119.4(3) . . ? C11 N12 C13 108.9(3) . . ? C11 N12 C41 125.8(3) . . ? C13 N12 C41 125.2(3) . . ? C21 N21 C22 107.8(2) . . ? C21 N21 B 133.4(3) . . ? C22 N21 B 118.8(3) . . ? C21 N22 C23 108.4(3) . . ? C21 N22 C51 124.9(3) . . ? C23 N22 C51 126.6(3) . . ? C31 N31 C32 107.5(2) . . ? C31 N31 B 130.7(2) . . ? C32 N31 B 121.3(3) . . ? C31 N32 C33 108.7(3) . . ? C31 N32 C61 124.8(2) . . ? C33 N32 C61 126.2(3) . . ? H1 O1 C1 125(3) . . ? H1 O1 Zn 106(3) . . ? C1 O1 Zn 125.5(3) . . ? N11 C11 N12 107.7(3) . . ? N11 C11 S11 129.2(2) . . ? N12 C11 S11 123.1(2) . . ? C13 C12 N11 108.3(3) . . ? C12 C13 N12 107.2(3) . . ? N21 C21 N22 107.7(3) . . ? N21 C21 S12 128.8(2) . . ? N22 C21 S12 123.5(2) . . ? C23 C22 N21 108.6(3) . . ? C22 C23 N22 107.5(3) . . ? N32 C31 N31 107.9(2) . . ? N32 C31 S13 121.5(2) . . ? N31 C31 S13 130.5(2) . . ? C33 C32 N31 108.5(3) . . ? C32 C33 N32 107.4(3) . . ? C46 C41 C42 122.6(3) . . ? C46 C41 N12 119.4(3) . . ? C42 C41 N12 117.9(3) . . ? C43 C42 C41 117.3(4) . . ? C43 C42 C72 121.4(4) . . ? C41 C42 C72 121.3(3) . . ? C44 C43 C42 122.4(4) . . ? C43 C44 C45 118.5(4) . . ? C43 C44 C74 121.7(5) . . ? C45 C44 C74 119.8(5) . . ? C44 C45 C46 122.1(4) . . ? C41 C46 C45 117.0(4) . . ? C41 C46 C76 121.7(3) . . ? C45 C46 C76 121.2(4) . . ? C56 C51 C52 123.3(3) . . ? C56 C51 N22 119.2(3) . . ? C52 C51 N22 117.5(3) . . ? C53 C52 C51 116.9(3) . . ? C53 C52 C82 121.5(3) . . ? C51 C52 C82 121.6(3) . . ? C54 C55 C56 122.3(4) . . ? C54 C53 C52 122.6(4) . . ? C53 C54 C55 118.3(4) . . ? C53 C54 C84 121.3(4) . . ? C55 C54 C84 120.4(4) . . ? C51 C56 C55 116.6(3) . . ? C51 C56 C86 123.3(3) . . ? C55 C56 C86 120.1(3) . . ? C66 C61 C62 123.1(3) . . ? C66 C61 N32 119.7(3) . . ? C62 C61 N32 117.3(3) . . ? C61 C62 C63 117.1(3) . . ? C61 C62 C92 122.0(3) . . ? C63 C62 C92 120.8(3) . . ? C64 C63 C62 121.6(3) . . ? C65 C64 C63 118.3(3) . . ? C65 C64 C94 121.5(4) . . ? C63 C64 C94 120.1(4) . . ? C64 C65 C66 122.3(3) . . ? C61 C66 C65 117.6(3) . . ? C61 C66 C96 121.4(3) . . ? C65 C66 C96 120.9(3) . . ? O14 Cl1 O12 107.9(12) . . ? O14 Cl1 O11 108.3(11) . . ? O12 Cl1 O11 111.7(11) . . ? O14 Cl1 O13 110.3(11) . . ? O12 Cl1 O13 110.3(11) . . ? O11 Cl1 O13 108.3(11) . . ? O24 Cl2 O21 112.5(5) . . ? O24 Cl2 O23 116.0(6) . . ? O21 Cl2 O23 110.2(5) . . ? O24 Cl2 O22 106.9(6) . . ? O21 Cl2 O22 107.6(6) . . ? O23 Cl2 O22 102.9(6) . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 28.23 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.505 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.055 data_zncls10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H42 B Cl N6 O0.50 S3 Zn' _chemical_formula_weight 774.57 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.6233(18) _cell_length_b 24.930(2) _cell_length_c 33.100(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16193(2) _cell_formula_units_Z 16 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6464 _exptl_absorpt_coefficient_mu 0.861 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8466 _exptl_absorpt_correction_T_max 0.9188 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 107971 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 28.18 _reflns_number_total 19041 _reflns_number_gt 10046 _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^)+(0.0494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00006(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 19041 _refine_ls_number_parameters 898 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1151 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1208 _refine_ls_wR_factor_gt 0.1048 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.715 _refine_ls_shift/su_mean 0.018 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 0.065882(18) 0.435280(15) 0.234027(10) 0.04094(10) Uani 1 1 d . . . Zn2 Zn -0.033802(18) 0.250376(15) -0.016445(10) 0.04267(11) Uani 1 1 d . . . Cl1 Cl -0.03933(5) 0.40306(4) 0.22260(3) 0.0654(3) Uani 1 1 d . . . Cl2 Cl 0.07650(5) 0.27020(5) -0.01037(4) 0.0866(4) Uani 1 1 d . . . B1 B 0.22954(19) 0.50390(15) 0.24622(10) 0.0401(9) Uani 1 1 d . . . H1 H 0.2804(13) 0.5257(10) 0.2533(7) 0.031(7) Uiso 1 1 d . . . B2 B -0.21334(19) 0.21959(15) -0.02895(10) 0.0389(9) Uani 1 1 d . . . H2 H -0.2674(13) 0.2143(10) -0.0341(7) 0.030(7) Uiso 1 1 d . . . S11 S 0.07268(4) 0.48797(3) 0.29367(2) 0.04092(19) Uani 1 1 d . . . S12 S 0.15770(4) 0.37466(3) 0.24134(2) 0.0463(2) Uani 1 1 d . . . S13 S 0.09230(4) 0.49303(3) 0.17934(2) 0.0429(2) Uani 1 1 d . . . S21 S -0.05408(4) 0.20064(3) -0.07573(2) 0.0468(2) Uani 1 1 d . . . S22 S -0.10116(4) 0.32866(3) -0.01834(2) 0.0437(2) Uani 1 1 d . . . S23 S -0.07653(4) 0.19640(3) 0.03696(2) 0.04158(19) Uani 1 1 d . . . N11 N 0.17233(12) 0.54638(10) 0.25351(7) 0.0369(6) Uani 1 1 d . . . N21 N 0.08106(12) 0.59208(10) 0.26954(7) 0.0399(6) Uani 1 1 d . . . N12 N 0.22983(12) 0.45800(10) 0.27813(7) 0.0394(6) Uani 1 1 d . . . N22 N 0.22019(13) 0.38472(10) 0.31396(7) 0.0438(6) Uani 1 1 d . . . N13 N 0.22833(11) 0.48152(10) 0.20212(7) 0.0377(6) Uani 1 1 d . . . N23 N 0.20391(13) 0.45591(10) 0.14055(7) 0.0433(6) Uani 1 1 d . . . N41 N -0.18680(12) 0.24005(10) -0.07069(7) 0.0417(6) Uani 1 1 d . . . N42 N -0.13264(14) 0.25806(11) -0.12687(7) 0.0530(7) Uani 1 1 d . . . N51 N -0.20831(12) 0.26258(10) 0.00511(6) 0.0370(6) Uani 1 1 d . . . N52 N -0.18406(12) 0.32734(10) 0.04719(7) 0.0414(6) Uani 1 1 d . . . N61 N -0.17960(12) 0.16580(9) -0.01642(6) 0.0371(6) Uani 1 1 d . . . N62 N -0.11893(13) 0.09997(10) 0.00921(7) 0.0430(6) Uani 1 1 d . . . C11 C 0.11107(15) 0.54268(12) 0.27159(8) 0.0365(7) Uani 1 1 d . . . C12 C 0.12341(17) 0.62711(13) 0.24948(9) 0.0474(8) Uani 1 1 d . . . H12J H 0.1148 0.6634 0.2438 0.057 Uiso 1 1 calc R . . C13 C 0.17972(17) 0.59910(13) 0.23948(9) 0.0472(8) Uani 1 1 d . . . H13J H 0.2176 0.6127 0.2254 0.057 Uiso 1 1 calc R . . C21 C 0.20367(15) 0.40755(13) 0.27816(8) 0.0398(7) Uani 1 1 d . . . C22 C 0.25720(17) 0.42090(14) 0.33660(10) 0.0556(9) Uani 1 1 d . . . H22A H 0.2749 0.4151 0.3626 0.067 Uiso 1 1 calc R . . C23 C 0.26311(16) 0.46553(14) 0.31476(9) 0.0495(9) Uani 1 1 d . . . H23A H 0.2860 0.4969 0.3228 0.059 Uiso 1 1 calc R . . C31 C 0.17740(15) 0.47739(12) 0.17471(8) 0.0397(7) Uani 1 1 d . . . C32 C 0.27252(17) 0.44655(14) 0.14655(10) 0.0545(9) Uani 1 1 d . . . H32A H 0.3031 0.4320 0.1276 0.065 Uiso 1 1 calc R . . C33 C 0.28741(16) 0.46194(13) 0.18417(10) 0.0500(9) Uani 1 1 d . . . H33A H 0.3305 0.4599 0.1964 0.060 Uiso 1 1 calc R . . C41 C -0.12706(16) 0.23351(12) -0.09041(8) 0.0419(8) Uani 1 1 d . . . C42 C -0.1965(2) 0.28044(17) -0.12969(11) 0.0730(12) Uani 1 1 d . . . H42A H -0.2138 0.2999 -0.1517 0.088 Uiso 1 1 calc R . . C43 C -0.22971(18) 0.26933(15) -0.09509(10) 0.0626(10) Uani 1 1 d . . . H43A H -0.2745 0.2798 -0.0887 0.075 Uiso 1 1 calc R . . C51 C -0.16634(15) 0.30447(12) 0.01131(8) 0.0366(7) Uani 1 1 d . . . C52 C -0.23807(16) 0.29849(14) 0.06349(9) 0.0532(9) Uani 1 1 d . . . H52A H -0.2603 0.3057 0.0881 0.064 Uiso 1 1 calc R . . C53 C -0.25259(16) 0.25891(13) 0.03806(9) 0.0466(8) Uani 1 1 d . . . H53A H -0.2868 0.2329 0.0416 0.056 Uiso 1 1 calc R . . C61 C -0.12672(15) 0.15414(12) 0.00870(8) 0.0368(7) Uani 1 1 d . . . C62 C -0.16777(18) 0.07753(14) -0.01598(9) 0.0532(9) Uani 1 1 d . . . H62A H -0.1739 0.0408 -0.0212 0.064 Uiso 1 1 calc R . . C63 C -0.20450(17) 0.11777(13) -0.03151(9) 0.0466(8) Uani 1 1 d . . . H63A H -0.2411 0.1141 -0.0496 0.056 Uiso 1 1 calc R . . C71 C 0.01749(16) 0.60499(12) 0.29002(9) 0.0432(8) Uani 1 1 d . . . C72 C -0.04431(17) 0.58818(13) 0.27286(10) 0.0507(9) Uani 1 1 d . . . C73 C -0.10267(19) 0.59770(15) 0.29474(12) 0.0687(11) Uani 1 1 d . . . H73A H -0.1447 0.5870 0.2838 0.082 Uiso 1 1 calc R . . C74 C -0.1020(2) 0.62230(18) 0.33198(14) 0.0813(13) Uani 1 1 d . . . C75 C -0.0404(2) 0.63999(16) 0.34738(12) 0.0760(12) Uani 1 1 d . . . H75A H -0.0398 0.6579 0.3724 0.091 Uiso 1 1 calc R . . C76 C 0.02120(18) 0.63193(13) 0.32676(10) 0.0534(9) Uani 1 1 d . . . C77 C -0.04897(18) 0.55983(14) 0.23254(10) 0.0617(10) Uani 1 1 d . . . H77A H -0.0465 0.5214 0.2367 0.093 Uiso 1 1 calc R . . H77B H -0.0115 0.5712 0.2154 0.093 Uiso 1 1 calc R . . H77C H -0.0919 0.5688 0.2196 0.093 Uiso 1 1 calc R . . C78 C -0.1663(3) 0.6304(3) 0.35687(18) 0.166(3) Uani 1 1 d . . . H78A H -0.1539 0.6380 0.3847 0.249 Uiso 1 1 calc R . . H78B H -0.1938 0.5981 0.3559 0.249 Uiso 1 1 calc R . . H78C H -0.1921 0.6602 0.3460 0.249 Uiso 1 1 calc R . . C79 C 0.0880(2) 0.65061(16) 0.34416(11) 0.0753(12) Uani 1 1 d . . . H79A H 0.1220 0.6227 0.3408 0.113 Uiso 1 1 calc R . . H79B H 0.0824 0.6583 0.3727 0.113 Uiso 1 1 calc R . . H79C H 0.1028 0.6828 0.3302 0.113 Uiso 1 1 calc R . . C81 C 0.20485(17) 0.33063(13) 0.32646(9) 0.0466(8) Uani 1 1 d . . . C82 C 0.14582(17) 0.32073(14) 0.34890(10) 0.0516(9) Uani 1 1 d . . . C83 C 0.13514(19) 0.26877(16) 0.36273(10) 0.0607(10) Uani 1 1 d . . . H83A H 0.0958 0.2614 0.3780 0.073 Uiso 1 1 calc R . . C84 C 0.1798(2) 0.22809(16) 0.35494(12) 0.0691(11) Uani 1 1 d . . . C85 C 0.2369(2) 0.23894(16) 0.33244(12) 0.0771(12) Uani 1 1 d . . . H85A H 0.2675 0.2110 0.3267 0.093 Uiso 1 1 calc R . . C86 C 0.25102(19) 0.29074(15) 0.31763(11) 0.0640(10) Uani 1 1 d . . . C87 C 0.0950(2) 0.36463(16) 0.35784(12) 0.0773(12) Uani 1 1 d . . . H87A H 0.0597 0.3508 0.3755 0.116 Uiso 1 1 calc R . . H87B H 0.0747 0.3769 0.3328 0.116 Uiso 1 1 calc R . . H87C H 0.1181 0.3943 0.3710 0.116 Uiso 1 1 calc R . . C88 C 0.1677(2) 0.17167(16) 0.37139(15) 0.1052(17) Uani 1 1 d . . . H88A H 0.1206 0.1683 0.3801 0.158 Uiso 1 1 calc R . . H88B H 0.1977 0.1653 0.3942 0.158 Uiso 1 1 calc R . . H88C H 0.1770 0.1456 0.3504 0.158 Uiso 1 1 calc R . . C89 C 0.3142(2) 0.30207(18) 0.29179(14) 0.1023(16) Uani 1 1 d . . . H89A H 0.3003 0.3097 0.2643 0.153 Uiso 1 1 calc R . . H89B H 0.3438 0.2709 0.2920 0.153 Uiso 1 1 calc R . . H89C H 0.3384 0.3327 0.3027 0.153 Uiso 1 1 calc R . . C91 C 0.16638(16) 0.44783(14) 0.10352(8) 0.0452(8) Uani 1 1 d . . . C92 C 0.13814(18) 0.39811(14) 0.09564(10) 0.0535(9) Uani 1 1 d . . . C93 C 0.10187(19) 0.39251(16) 0.05948(11) 0.0652(11) Uani 1 1 d . . . H93A H 0.0834 0.3588 0.0529 0.078 Uiso 1 1 calc R . . C94 C 0.0923(2) 0.43478(18) 0.03314(11) 0.0690(11) Uani 1 1 d . . . C95 C 0.12109(19) 0.48387(17) 0.04248(10) 0.0672(11) Uani 1 1 d . . . H95A H 0.1151 0.5127 0.0245 0.081 Uiso 1 1 calc R . . C96 C 0.15903(18) 0.49215(15) 0.07802(9) 0.0542(9) Uani 1 1 d . . . C97 C 0.1465(2) 0.35159(15) 0.12467(11) 0.0827(13) Uani 1 1 d . . . H97A H 0.1728 0.3631 0.1479 0.124 Uiso 1 1 calc R . . H97B H 0.1701 0.3225 0.1112 0.124 Uiso 1 1 calc R . . H97C H 0.1020 0.3394 0.1335 0.124 Uiso 1 1 calc R . . C98 C 0.0511(3) 0.4272(2) -0.00576(13) 0.1128(19) Uani 1 1 d . . . H98A H 0.0349 0.3905 -0.0073 0.169 Uiso 1 1 calc R . . H98B H 0.0799 0.4348 -0.0289 0.169 Uiso 1 1 calc R . . H98C H 0.0125 0.4515 -0.0057 0.169 Uiso 1 1 calc R . . C99 C 0.1888(2) 0.54628(14) 0.08786(10) 0.0715(11) Uani 1 1 d . . . H99A H 0.2129 0.5443 0.1134 0.107 Uiso 1 1 calc R . . H99B H 0.1525 0.5725 0.0898 0.107 Uiso 1 1 calc R . . H99C H 0.2203 0.5568 0.0667 0.107 Uiso 1 1 calc R . . C111 C -0.08131(18) 0.25942(15) -0.15824(9) 0.0519(9) Uani 1 1 d . . . C112 C -0.0761(2) 0.21697(15) -0.18468(10) 0.0641(11) Uani 1 1 d . . . C113 C -0.0276(2) 0.21892(16) -0.21483(10) 0.0732(12) Uani 1 1 d . . . H11J H -0.0240 0.1902 -0.2331 0.088 Uiso 1 1 calc R . . C114 C 0.0158(2) 0.26232(16) -0.21874(10) 0.0621(10) Uani 1 1 d . . . C115 C 0.00912(19) 0.30405(15) -0.19195(10) 0.0597(10) Uani 1 1 d . . . H11K H 0.0383 0.3338 -0.1946 0.072 Uiso 1 1 calc R . . C116 C -0.03905(19) 0.30420(14) -0.16100(10) 0.0547(9) Uani 1 1 d . . . C117 C -0.1212(3) 0.16774(17) -0.17994(12) 0.1049(18) Uani 1 1 d . . . H11A H -0.1101 0.1497 -0.1548 0.157 Uiso 1 1 calc R . . H11B H -0.1135 0.1435 -0.2024 0.157 Uiso 1 1 calc R . . H11C H -0.1686 0.1786 -0.1796 0.157 Uiso 1 1 calc R . . C118 C 0.0705(2) 0.26268(17) -0.25153(13) 0.0930(15) Uani 1 1 d . . . H11D H 0.1115 0.2457 -0.2413 0.140 Uiso 1 1 calc R . . H11E H 0.0805 0.2994 -0.2592 0.140 Uiso 1 1 calc R . . H11F H 0.0542 0.2431 -0.2749 0.140 Uiso 1 1 calc R . . C119 C -0.0434(2) 0.35051(15) -0.13114(13) 0.0883(14) Uani 1 1 d . . . H11G H -0.0894 0.3647 -0.1309 0.132 Uiso 1 1 calc R . . H11H H -0.0119 0.3785 -0.1392 0.132 Uiso 1 1 calc R . . H11I H -0.0316 0.3378 -0.1043 0.132 Uiso 1 1 calc R . . C121 C -0.15471(15) 0.37570(13) 0.06421(8) 0.0419(8) Uani 1 1 d . . . C122 C -0.10040(17) 0.37124(13) 0.09129(9) 0.0484(8) Uani 1 1 d . . . C123 C -0.07416(17) 0.41824(15) 0.10748(10) 0.0547(9) Uani 1 1 d . . . H12K H -0.0373 0.4161 0.1256 0.066 Uiso 1 1 calc R . . C124 C -0.10058(18) 0.46858(14) 0.09785(9) 0.0532(9) Uani 1 1 d . . . C125 C -0.15535(17) 0.47113(14) 0.07077(9) 0.0508(9) Uani 1 1 d . . . H12L H -0.1737 0.5048 0.0640 0.061 Uiso 1 1 calc R . . C126 C -0.18332(16) 0.42514(13) 0.05362(9) 0.0462(8) Uani 1 1 d . . . C127 C -0.0700(2) 0.31746(15) 0.10222(11) 0.0738(12) Uani 1 1 d . . . H12A H -0.0422 0.3046 0.0800 0.111 Uiso 1 1 calc R . . H12B H -0.1063 0.2920 0.1075 0.111 Uiso 1 1 calc R . . H12C H -0.0420 0.3212 0.1262 0.111 Uiso 1 1 calc R . . C128 C -0.0711(2) 0.51933(15) 0.11644(12) 0.0787(12) Uani 1 1 d . . . H12D H -0.0664 0.5146 0.1454 0.118 Uiso 1 1 calc R . . H12E H -0.1013 0.5493 0.1110 0.118 Uiso 1 1 calc R . . H12F H -0.0267 0.5265 0.1047 0.118 Uiso 1 1 calc R . . C129 C -0.24340(18) 0.42867(15) 0.02519(10) 0.0644(10) Uani 1 1 d . . . H12G H -0.2346 0.4069 0.0015 0.097 Uiso 1 1 calc R . . H12H H -0.2502 0.4657 0.0171 0.097 Uiso 1 1 calc R . . H12I H -0.2840 0.4156 0.0387 0.097 Uiso 1 1 calc R . . C131 C -0.07322(18) 0.07069(12) 0.03523(9) 0.0454(8) Uani 1 1 d . . . C132 C -0.00528(18) 0.06559(13) 0.02449(10) 0.0517(9) Uani 1 1 d . . . C133 C 0.0365(2) 0.03785(14) 0.05132(11) 0.0653(11) Uani 1 1 d . . . H13K H 0.0828 0.0339 0.0447 0.078 Uiso 1 1 calc R . . C134 C 0.0135(2) 0.01585(15) 0.08704(11) 0.0658(11) Uani 1 1 d . . . C135 C -0.0554(2) 0.02166(15) 0.09620(10) 0.0638(10) Uani 1 1 d . . . H13L H -0.0724 0.0063 0.1201 0.077 Uiso 1 1 calc R . . C136 C -0.10018(18) 0.04958(13) 0.07095(9) 0.0503(9) Uani 1 1 d . . . C137 C 0.02298(19) 0.08971(15) -0.01452(11) 0.0699(11) Uani 1 1 d . . . H13A H 0.0322 0.1276 -0.0105 0.105 Uiso 1 1 calc R . . H13B H -0.0102 0.0855 -0.0360 0.105 Uiso 1 1 calc R . . H13C H 0.0648 0.0714 -0.0218 0.105 Uiso 1 1 calc R . . C138 C 0.0610(2) -0.0140(2) 0.11499(12) 0.1012(16) Uani 1 1 d . . . H13D H 0.0586 -0.0521 0.1092 0.152 Uiso 1 1 calc R . . H13E H 0.0476 -0.0077 0.1428 0.152 Uiso 1 1 calc R . . H13F H 0.1073 -0.0015 0.1109 0.152 Uiso 1 1 calc R . . C139 C -0.17319(19) 0.05741(16) 0.08275(10) 0.0714(11) Uani 1 1 d . . . H13G H -0.1815 0.0402 0.1086 0.107 Uiso 1 1 calc R . . H13H H -0.2025 0.0416 0.0624 0.107 Uiso 1 1 calc R . . H13I H -0.1828 0.0955 0.0849 0.107 Uiso 1 1 calc R . . O1 O -0.3762(2) 0.3084(3) -0.05762(15) 0.265(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0388(2) 0.0458(2) 0.03818(19) 0.00239(17) -0.00404(16) -0.00538(18) Zn2 0.0353(2) 0.0471(2) 0.0456(2) -0.00439(17) 0.00352(16) 0.00101(18) Cl1 0.0549(6) 0.0687(6) 0.0726(6) 0.0217(5) -0.0212(4) -0.0266(5) Cl2 0.0359(5) 0.1016(9) 0.1223(9) -0.0257(7) 0.0070(5) -0.0105(6) B1 0.038(2) 0.043(2) 0.0387(19) 0.0068(16) -0.0004(16) -0.0029(18) B2 0.035(2) 0.045(2) 0.0368(19) -0.0002(16) -0.0038(15) 0.0043(18) S11 0.0436(5) 0.0443(5) 0.0349(4) 0.0028(4) 0.0046(3) -0.0058(4) S12 0.0505(5) 0.0435(5) 0.0451(5) 0.0004(4) -0.0113(4) -0.0002(4) S13 0.0370(4) 0.0575(5) 0.0342(4) 0.0066(4) 0.0036(3) 0.0088(4) S21 0.0498(5) 0.0538(5) 0.0370(4) -0.0030(4) 0.0018(4) 0.0157(4) S22 0.0444(5) 0.0416(5) 0.0452(4) -0.0005(4) 0.0122(4) 0.0005(4) S23 0.0446(5) 0.0416(5) 0.0385(4) -0.0008(4) -0.0087(3) -0.0015(4) N11 0.0348(15) 0.0377(15) 0.0382(13) 0.0025(11) 0.0021(11) -0.0040(12) N21 0.0367(15) 0.0398(15) 0.0433(14) -0.0007(12) -0.0007(11) -0.0016(13) N12 0.0364(15) 0.0443(16) 0.0376(13) 0.0046(12) -0.0045(11) -0.0047(13) N22 0.0427(16) 0.0466(17) 0.0421(14) 0.0116(13) -0.0104(12) -0.0046(13) N13 0.0293(14) 0.0429(15) 0.0411(14) 0.0034(12) 0.0040(11) 0.0028(12) N23 0.0393(16) 0.0521(17) 0.0386(14) -0.0034(12) 0.0086(12) 0.0038(13) N41 0.0404(15) 0.0477(17) 0.0370(13) 0.0021(12) -0.0043(11) 0.0087(13) N42 0.0576(19) 0.0610(19) 0.0406(15) 0.0113(14) -0.0025(13) 0.0099(16) N51 0.0310(14) 0.0430(16) 0.0370(13) 0.0004(11) 0.0011(11) 0.0015(12) N52 0.0376(15) 0.0448(16) 0.0418(14) -0.0073(12) 0.0051(11) 0.0001(13) N61 0.0397(15) 0.0358(15) 0.0358(13) -0.0033(12) -0.0052(11) -0.0016(12) N62 0.0495(17) 0.0378(16) 0.0418(14) -0.0014(12) -0.0082(12) -0.0005(13) C11 0.0362(18) 0.0417(19) 0.0316(16) -0.0004(13) -0.0017(13) -0.0023(15) C12 0.046(2) 0.040(2) 0.0563(19) 0.0085(16) 0.0020(16) -0.0040(17) C13 0.041(2) 0.049(2) 0.0518(19) 0.0111(16) 0.0044(15) -0.0070(17) C21 0.0339(17) 0.044(2) 0.0410(17) 0.0052(15) -0.0022(13) 0.0004(15) C22 0.058(2) 0.065(2) 0.0440(18) 0.0128(18) -0.0184(16) -0.0133(19) C23 0.048(2) 0.056(2) 0.0452(18) 0.0025(17) -0.0118(15) -0.0123(17) C31 0.0375(18) 0.045(2) 0.0369(16) 0.0077(14) 0.0063(14) 0.0023(15) C32 0.040(2) 0.067(3) 0.056(2) -0.0151(18) 0.0150(16) 0.0053(18) C33 0.0345(18) 0.055(2) 0.060(2) 0.0021(18) 0.0088(16) 0.0065(17) C41 0.051(2) 0.0397(19) 0.0353(16) -0.0020(14) -0.0039(14) 0.0023(16) C42 0.070(3) 0.098(3) 0.051(2) 0.030(2) -0.0055(19) 0.021(2) C43 0.048(2) 0.080(3) 0.059(2) 0.018(2) -0.0062(18) 0.019(2) C51 0.0333(17) 0.0378(18) 0.0388(16) -0.0016(14) 0.0022(13) 0.0078(15) C52 0.046(2) 0.069(2) 0.0450(18) -0.0067(18) 0.0169(15) -0.0088(19) C53 0.0383(18) 0.055(2) 0.0467(18) -0.0066(16) 0.0090(15) -0.0075(16) C61 0.0390(18) 0.0364(19) 0.0350(16) 0.0005(14) 0.0006(13) 0.0013(15) C62 0.062(2) 0.041(2) 0.056(2) -0.0104(17) -0.0099(18) -0.0057(18) C63 0.046(2) 0.047(2) 0.0459(18) -0.0065(16) -0.0127(15) -0.0047(17) C71 0.0413(19) 0.0423(19) 0.0458(18) -0.0020(15) 0.0064(14) 0.0045(16) C72 0.044(2) 0.040(2) 0.068(2) -0.0056(17) 0.0012(17) 0.0054(16) C73 0.042(2) 0.063(3) 0.101(3) -0.017(2) 0.009(2) 0.005(2) C74 0.058(3) 0.075(3) 0.111(4) -0.021(3) 0.023(3) 0.002(2) C75 0.091(3) 0.068(3) 0.069(3) -0.019(2) 0.029(2) 0.008(3) C76 0.062(2) 0.049(2) 0.049(2) -0.0032(17) 0.0023(17) -0.0005(19) C77 0.050(2) 0.058(2) 0.078(3) -0.011(2) -0.0134(18) 0.0039(18) C78 0.092(4) 0.210(7) 0.197(6) -0.088(5) 0.082(4) -0.002(4) C79 0.085(3) 0.083(3) 0.058(2) -0.014(2) -0.005(2) -0.012(3) C81 0.045(2) 0.048(2) 0.0466(18) 0.0152(16) -0.0140(15) -0.0033(18) C82 0.047(2) 0.056(2) 0.052(2) 0.0114(17) -0.0140(16) -0.0100(18) C83 0.056(2) 0.066(3) 0.060(2) 0.017(2) -0.0144(18) -0.017(2) C84 0.069(3) 0.054(3) 0.085(3) 0.023(2) -0.022(2) -0.013(2) C85 0.077(3) 0.058(3) 0.097(3) 0.019(2) -0.007(2) 0.011(2) C86 0.050(2) 0.062(3) 0.080(3) 0.020(2) -0.0038(19) 0.003(2) C87 0.064(3) 0.074(3) 0.093(3) 0.010(2) 0.019(2) -0.004(2) C88 0.105(4) 0.066(3) 0.144(4) 0.043(3) -0.024(3) -0.017(3) C89 0.068(3) 0.099(4) 0.139(4) 0.042(3) 0.028(3) 0.024(3) C91 0.0438(19) 0.059(2) 0.0327(16) -0.0073(16) 0.0093(14) -0.0009(17) C92 0.059(2) 0.055(2) 0.0463(19) -0.0071(18) 0.0131(17) -0.0038(19) C93 0.071(3) 0.065(3) 0.059(2) -0.009(2) 0.012(2) -0.019(2) C94 0.066(3) 0.087(3) 0.053(2) -0.005(2) 0.0009(19) -0.027(2) C95 0.073(3) 0.077(3) 0.052(2) 0.011(2) -0.0037(19) -0.016(2) C96 0.060(2) 0.065(2) 0.0377(18) -0.0009(18) 0.0039(16) -0.009(2) C97 0.111(4) 0.061(3) 0.075(3) 0.001(2) -0.002(2) -0.011(3) C98 0.124(4) 0.137(5) 0.078(3) 0.007(3) -0.040(3) -0.054(4) C99 0.094(3) 0.064(3) 0.056(2) 0.003(2) -0.008(2) -0.021(2) C111 0.064(2) 0.055(2) 0.0367(18) 0.0099(17) -0.0017(16) 0.0065(19) C112 0.093(3) 0.059(2) 0.0405(19) -0.0001(18) 0.0030(19) -0.015(2) C113 0.120(4) 0.055(3) 0.045(2) -0.0022(19) 0.016(2) 0.003(3) C114 0.084(3) 0.054(2) 0.049(2) 0.0132(18) 0.0127(19) 0.019(2) C115 0.065(2) 0.051(2) 0.063(2) 0.0169(19) 0.0051(19) 0.004(2) C116 0.066(2) 0.048(2) 0.050(2) 0.0101(17) 0.0017(18) 0.009(2) C117 0.159(5) 0.091(4) 0.065(3) -0.010(3) 0.013(3) -0.053(3) C118 0.115(4) 0.077(3) 0.086(3) 0.022(3) 0.045(3) 0.030(3) C119 0.114(4) 0.057(3) 0.093(3) -0.018(2) 0.025(3) -0.006(3) C121 0.0379(18) 0.047(2) 0.0406(17) -0.0094(15) 0.0062(14) -0.0003(16) C122 0.051(2) 0.050(2) 0.0438(18) -0.0049(16) -0.0003(15) 0.0061(18) C123 0.045(2) 0.068(3) 0.052(2) -0.0124(18) -0.0069(16) 0.0006(19) C124 0.055(2) 0.058(2) 0.0468(19) -0.0119(17) -0.0005(17) -0.0041(19) C125 0.057(2) 0.046(2) 0.0491(19) -0.0056(16) 0.0003(17) 0.0011(18) C126 0.044(2) 0.053(2) 0.0419(17) -0.0072(16) 0.0006(15) 0.0033(17) C127 0.078(3) 0.066(3) 0.078(3) -0.006(2) -0.022(2) 0.016(2) C128 0.091(3) 0.066(3) 0.079(3) -0.023(2) -0.021(2) -0.013(2) C129 0.062(2) 0.061(2) 0.070(2) -0.0033(19) -0.0176(19) 0.003(2) C131 0.059(2) 0.0315(18) 0.0454(18) -0.0018(15) -0.0071(16) 0.0063(17) C132 0.055(2) 0.046(2) 0.054(2) -0.0029(17) -0.0011(17) 0.0110(19) C133 0.063(3) 0.058(2) 0.075(3) -0.005(2) -0.005(2) 0.022(2) C134 0.091(3) 0.059(2) 0.048(2) -0.0003(19) -0.011(2) 0.024(2) C135 0.087(3) 0.061(3) 0.0437(19) 0.0041(18) -0.0012(19) 0.015(2) C136 0.063(2) 0.043(2) 0.0440(19) -0.0025(16) -0.0045(17) 0.0023(18) C137 0.068(3) 0.071(3) 0.070(2) 0.010(2) 0.014(2) 0.016(2) C138 0.109(4) 0.120(4) 0.075(3) 0.007(3) -0.024(3) 0.055(3) C139 0.072(3) 0.083(3) 0.060(2) 0.003(2) 0.005(2) -0.004(2) O1 0.144(4) 0.430(9) 0.220(5) 0.216(6) 0.100(4) 0.130(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 Cl1 2.2475(9) . ? Zn1 S12 2.3640(9) . ? Zn1 S13 2.3702(8) . ? Zn1 S11 2.3751(8) . ? Zn2 Cl2 2.2293(10) . ? Zn2 S21 2.3552(9) . ? Zn2 S22 2.3580(9) . ? Zn2 S23 2.3745(9) . ? B1 N11 1.562(4) . ? B1 N12 1.557(4) . ? B1 N13 1.563(4) . ? B2 N61 1.552(4) . ? B2 N51 1.559(4) . ? B2 N41 1.562(4) . ? S11 C11 1.721(3) . ? S12 C21 1.724(3) . ? S13 C31 1.722(3) . ? S21 C41 1.720(3) . ? S22 C51 1.721(3) . ? S23 C61 1.719(3) . ? N11 C11 1.346(4) . ? N11 C13 1.401(4) . ? N21 C11 1.367(4) . ? N21 C12 1.376(4) . ? N21 C71 1.456(4) . ? N12 C21 1.359(4) . ? N12 C23 1.390(3) . ? N22 C21 1.354(3) . ? N22 C22 1.379(4) . ? N22 C81 1.442(4) . ? N13 C31 1.354(3) . ? N13 C33 1.391(4) . ? N23 C31 1.355(3) . ? N23 C32 1.381(4) . ? N23 C91 1.444(4) . ? N41 C41 1.352(4) . ? N41 C43 1.376(4) . ? N42 C41 1.358(4) . ? N42 C42 1.375(4) . ? N42 C111 1.447(4) . ? N51 C51 1.346(4) . ? N51 C53 1.397(3) . ? N52 C51 1.363(3) . ? N52 C52 1.390(4) . ? N52 C121 1.450(4) . ? N61 C61 1.361(3) . ? N61 C63 1.386(4) . ? N62 C61 1.359(4) . ? N62 C62 1.388(4) . ? N62 C131 1.442(4) . ? C12 C13 1.348(4) . ? C22 C23 1.332(4) . ? C32 C33 1.335(4) . ? C42 C43 1.347(4) . ? C52 C53 1.328(4) . ? C62 C63 1.338(4) . ? C71 C76 1.391(4) . ? C71 C72 1.403(4) . ? C72 C73 1.376(4) . ? C72 C77 1.513(4) . ? C73 C74 1.377(5) . ? C74 C75 1.385(6) . ? C74 C78 1.520(5) . ? C75 C76 1.402(5) . ? C76 C79 1.506(5) . ? C81 C86 1.377(5) . ? C81 C82 1.398(4) . ? C82 C83 1.390(5) . ? C82 C87 1.509(5) . ? C83 C84 1.365(5) . ? C84 C85 1.372(5) . ? C84 C88 1.527(5) . ? C85 C86 1.409(5) . ? C86 C89 1.532(5) . ? C91 C92 1.383(4) . ? C91 C96 1.398(4) . ? C92 C93 1.400(5) . ? C92 C97 1.515(5) . ? C93 C94 1.381(5) . ? C94 C95 1.383(5) . ? C94 C98 1.532(5) . ? C95 C96 1.407(4) . ? C96 C99 1.506(5) . ? C111 C112 1.377(5) . ? C111 C116 1.394(5) . ? C112 C113 1.381(5) . ? C112 C117 1.520(5) . ? C113 C114 1.383(5) . ? C114 C115 1.373(5) . ? C114 C118 1.527(5) . ? C115 C116 1.394(5) . ? C116 C119 1.522(5) . ? C121 C122 1.397(4) . ? C121 C126 1.399(4) . ? C122 C123 1.388(4) . ? C122 C127 1.511(5) . ? C123 C124 1.395(5) . ? C124 C125 1.401(4) . ? C124 C128 1.521(5) . ? C125 C126 1.392(4) . ? C126 C129 1.511(4) . ? C131 C132 1.386(5) . ? C131 C136 1.398(4) . ? C132 C133 1.393(5) . ? C132 C137 1.529(5) . ? C133 C134 1.379(5) . ? C134 C135 1.393(5) . ? C134 C138 1.510(5) . ? C135 C136 1.398(5) . ? C136 C139 1.498(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Zn1 S12 119.27(4) . . ? Cl1 Zn1 S13 106.83(3) . . ? S12 Zn1 S13 107.44(3) . . ? Cl1 Zn1 S11 112.91(4) . . ? S12 Zn1 S11 103.04(3) . . ? S13 Zn1 S11 106.66(3) . . ? Cl2 Zn2 S21 110.86(4) . . ? Cl2 Zn2 S22 111.30(4) . . ? S21 Zn2 S22 108.60(3) . . ? Cl2 Zn2 S23 113.66(4) . . ? S21 Zn2 S23 105.20(3) . . ? S22 Zn2 S23 106.91(3) . . ? N11 B1 N12 113.3(2) . . ? N11 B1 N13 112.0(2) . . ? N12 B1 N13 111.8(3) . . ? N61 B2 N51 111.9(2) . . ? N61 B2 N41 112.1(2) . . ? N51 B2 N41 113.2(3) . . ? C11 S11 Zn1 96.30(9) . . ? C21 S12 Zn1 99.62(11) . . ? C31 S13 Zn1 98.19(10) . . ? C41 S21 Zn2 97.19(10) . . ? C51 S22 Zn2 96.40(10) . . ? C61 S23 Zn2 98.31(10) . . ? C11 N11 C13 107.7(3) . . ? C11 N11 B1 131.6(3) . . ? C13 N11 B1 120.7(2) . . ? C11 N21 C12 109.6(2) . . ? C11 N21 C71 123.1(2) . . ? C12 N21 C71 127.0(3) . . ? C21 N12 C23 107.6(2) . . ? C21 N12 B1 132.8(2) . . ? C23 N12 B1 119.6(3) . . ? C21 N22 C22 109.1(3) . . ? C21 N22 C81 126.4(3) . . ? C22 N22 C81 124.4(2) . . ? C31 N13 C33 107.6(2) . . ? C31 N13 B1 131.6(2) . . ? C33 N13 B1 120.8(3) . . ? C31 N23 C32 108.7(3) . . ? C31 N23 C91 124.6(3) . . ? C32 N23 C91 126.6(3) . . ? C41 N41 C43 108.1(2) . . ? C41 N41 B2 132.6(2) . . ? C43 N41 B2 119.2(3) . . ? C41 N42 C42 108.5(3) . . ? C41 N42 C111 126.3(3) . . ? C42 N42 C111 125.2(3) . . ? C51 N51 C53 108.2(2) . . ? C51 N51 B2 133.0(2) . . ? C53 N51 B2 118.7(3) . . ? C51 N52 C52 108.4(2) . . ? C51 N52 C121 125.8(2) . . ? C52 N52 C121 125.6(2) . . ? C61 N61 C63 107.7(2) . . ? C61 N61 B2 132.3(3) . . ? C63 N61 B2 120.0(2) . . ? C61 N62 C62 108.4(3) . . ? C61 N62 C131 125.5(2) . . ? C62 N62 C131 125.8(3) . . ? N11 C11 N21 107.5(2) . . ? N11 C11 S11 129.3(2) . . ? N21 C11 S11 123.1(2) . . ? C13 C12 N21 106.5(3) . . ? C12 C13 N11 108.6(3) . . ? N12 C21 N22 107.4(2) . . ? N12 C21 S12 129.6(2) . . ? N22 C21 S12 123.0(2) . . ? C23 C22 N22 107.3(3) . . ? C22 C23 N12 108.6(3) . . ? N13 C31 N23 107.8(3) . . ? N13 C31 S13 129.7(2) . . ? N23 C31 S13 122.4(2) . . ? C33 C32 N23 107.4(3) . . ? C32 C33 N13 108.5(3) . . ? N41 C41 N42 107.8(3) . . ? N41 C41 S21 130.0(2) . . ? N42 C41 S21 122.2(2) . . ? C43 C42 N42 107.5(3) . . ? C42 C43 N41 108.2(3) . . ? N51 C51 N52 107.5(2) . . ? N51 C51 S22 129.8(2) . . ? N52 C51 S22 122.7(2) . . ? C53 C52 N52 107.6(3) . . ? C52 C53 N51 108.2(3) . . ? N61 C61 N62 107.8(3) . . ? N61 C61 S23 129.7(2) . . ? N62 C61 S23 122.5(2) . . ? C63 C62 N62 107.5(3) . . ? C62 C63 N61 108.6(3) . . ? C76 C71 C72 122.9(3) . . ? C76 C71 N21 118.0(3) . . ? C72 C71 N21 119.1(3) . . ? C73 C72 C71 117.1(3) . . ? C73 C72 C77 119.6(3) . . ? C71 C72 C77 123.3(3) . . ? C74 C73 C72 122.7(4) . . ? C73 C74 C75 118.7(4) . . ? C73 C74 C78 122.4(4) . . ? C75 C74 C78 118.9(4) . . ? C74 C75 C76 121.8(4) . . ? C71 C76 C75 116.7(3) . . ? C71 C76 C79 121.9(3) . . ? C75 C76 C79 121.3(3) . . ? C86 C81 C82 122.0(3) . . ? C86 C81 N22 118.5(3) . . ? C82 C81 N22 119.4(3) . . ? C83 C82 C81 117.7(3) . . ? C83 C82 C87 120.8(3) . . ? C81 C82 C87 121.6(3) . . ? C84 C83 C82 122.2(4) . . ? C85 C84 C83 118.7(4) . . ? C85 C84 C88 120.2(4) . . ? C83 C84 C88 121.1(4) . . ? C84 C85 C86 122.0(4) . . ? C81 C86 C85 117.3(4) . . ? C81 C86 C89 121.2(3) . . ? C85 C86 C89 121.5(4) . . ? C92 C91 C96 123.6(3) . . ? C92 C91 N23 119.3(3) . . ? C96 C91 N23 117.1(3) . . ? C91 C92 C93 117.0(3) . . ? C91 C92 C97 121.6(3) . . ? C93 C92 C97 121.4(3) . . ? C94 C93 C92 122.2(4) . . ? C93 C94 C95 118.6(3) . . ? C93 C94 C98 120.6(4) . . ? C95 C94 C98 120.8(4) . . ? C94 C95 C96 122.2(4) . . ? C91 C96 C95 116.3(3) . . ? C91 C96 C99 122.5(3) . . ? C95 C96 C99 121.2(3) . . ? C112 C111 C116 122.0(3) . . ? C112 C111 N42 119.3(3) . . ? C116 C111 N42 118.7(3) . . ? C111 C112 C113 118.9(4) . . ? C111 C112 C117 120.8(3) . . ? C113 C112 C117 120.3(4) . . ? C114 C113 C112 121.3(4) . . ? C115 C114 C113 118.3(3) . . ? C115 C114 C118 121.4(4) . . ? C113 C114 C118 120.3(4) . . ? C114 C115 C116 122.8(4) . . ? C115 C116 C111 116.7(3) . . ? C115 C116 C119 121.1(4) . . ? C111 C116 C119 122.1(3) . . ? C122 C121 C126 122.5(3) . . ? C122 C121 N52 119.1(3) . . ? C126 C121 N52 118.4(3) . . ? C123 C122 C121 117.6(3) . . ? C123 C122 C127 120.7(3) . . ? C121 C122 C127 121.7(3) . . ? C122 C123 C124 122.2(3) . . ? C123 C124 C125 118.2(3) . . ? C123 C124 C128 121.0(3) . . ? C125 C124 C128 120.9(3) . . ? C126 C125 C124 121.7(3) . . ? C125 C126 C121 117.7(3) . . ? C125 C126 C129 120.9(3) . . ? C121 C126 C129 121.4(3) . . ? C132 C131 C136 123.1(3) . . ? C132 C131 N62 119.4(3) . . ? C136 C131 N62 117.4(3) . . ? C131 C132 C133 116.6(3) . . ? C131 C132 C137 122.0(3) . . ? C133 C132 C137 121.4(3) . . ? C134 C133 C132 123.4(4) . . ? C133 C134 C135 117.6(3) . . ? C133 C134 C138 121.3(4) . . ? C135 C134 C138 121.1(4) . . ? C134 C135 C136 122.1(3) . . ? C131 C136 C135 117.1(3) . . ? C131 C136 C139 122.2(3) . . ? C135 C136 C139 120.7(3) . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 28.18 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.890 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.060 data_zns10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H23 B Cl3 N7 O3 S3 Zn' _chemical_formula_weight 784.24 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' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.216(5) _cell_length_b 9.756(3) _cell_length_c 20.381(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.089(5) _cell_angle_gamma 90.00 _cell_volume 3397.1(17) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 1.185 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7175 _exptl_absorpt_correction_T_max 0.8907 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17637 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 28.25 _reflns_number_total 7622 _reflns_number_gt 6327 _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^)+(0.1153P)^2^+10.6214P] 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 SHELXL _refine_ls_extinction_coef 0.0000(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7622 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0823 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.2167 _refine_ls_wR_factor_gt 0.2019 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.473 _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 Zn Zn 0.26715(3) 0.80406(5) 0.61287(2) 0.03221(17) Uani 1 1 d . . . S11 S 0.35521(6) 0.89236(12) 0.70125(5) 0.0395(3) Uani 1 1 d . . . S21 S 0.17129(6) 0.67855(11) 0.65605(6) 0.0367(3) Uani 1 1 d . . . S31 S 0.34236(7) 0.66907(13) 0.55192(6) 0.0434(3) Uani 1 1 d . . . B B 0.3551(3) 0.5368(6) 0.7123(3) 0.0462(12) Uani 1 1 d . . . N11 N 0.3277(2) 0.6454(4) 0.76081(19) 0.0425(9) Uani 1 1 d . . . N12 N 0.2877(2) 0.8253(5) 0.81202(19) 0.0453(9) Uani 1 1 d . . . N21 N 0.2840(2) 0.4718(4) 0.6687(2) 0.0435(9) Uani 1 1 d . . . N22 N 0.1683(2) 0.4087(4) 0.6208(2) 0.0457(9) Uani 1 1 d . . . N31 N 0.4203(2) 0.5908(4) 0.6731(2) 0.0459(9) Uani 1 1 d . . . N32 N 0.4958(2) 0.6793(5) 0.6049(2) 0.0501(10) Uani 1 1 d . . . N1 N 0.1992(2) 0.9681(4) 0.51102(19) 0.0424(8) Uani 1 1 d . . . O1 O 0.1735(3) 1.0706(5) 0.4805(2) 0.0861(15) Uani 1 1 d . . . O2 O 0.1976(3) 0.8540(4) 0.48607(19) 0.0629(10) Uani 1 1 d . . . O3 O 0.2287(2) 0.9818(3) 0.57193(16) 0.0458(8) Uani 1 1 d . . . C11 C 0.3230(2) 0.7839(5) 0.7589(2) 0.0384(9) Uani 1 1 d . . . C12 C 0.2946(3) 0.6012(6) 0.8162(3) 0.0561(13) Uani 1 1 d . . . H11A H 0.2902 0.5095 0.8294 0.067 Uiso 1 1 calc R . . C13 C 0.2701(4) 0.7102(6) 0.8477(3) 0.0569(14) Uani 1 1 d . . . H23A H 0.2456 0.7092 0.8865 0.068 Uiso 1 1 calc R . . C21 C 0.2100(3) 0.5162(5) 0.6493(2) 0.0379(9) Uani 1 1 d . . . C22 C 0.2875(4) 0.3344(6) 0.6503(3) 0.0562(13) Uani 1 1 d . . . H9A H 0.3319 0.2780 0.6574 0.067 Uiso 1 1 calc R . . C23 C 0.2169(4) 0.2963(5) 0.6206(3) 0.0585(14) Uani 1 1 d . . . H3B H 0.2032 0.2094 0.6030 0.070 Uiso 1 1 calc R . . C31 C 0.4205(3) 0.6437(5) 0.6118(2) 0.0428(10) Uani 1 1 d . . . C32 C 0.4972(3) 0.5947(7) 0.7046(3) 0.0612(15) Uani 1 1 d . . . H17A H 0.5138 0.5640 0.7478 0.073 Uiso 1 1 calc R . . C33 C 0.5433(3) 0.6493(7) 0.6631(3) 0.0632(15) Uani 1 1 d . . . H8A H 0.5975 0.6644 0.6718 0.076 Uiso 1 1 calc R . . C41 C 0.2695(3) 0.9627(6) 0.8307(2) 0.0476(11) Uani 1 1 d . . . C42 C 0.2317(4) 1.0513(7) 0.7845(3) 0.0598(14) Uani 1 1 d . . . H15A H 0.2185 1.0239 0.7403 0.072 Uiso 1 1 calc R . . C43 C 0.2137(5) 1.1818(8) 0.8051(4) 0.0742(18) Uani 1 1 d . . . H5A H 0.1889 1.2442 0.7742 0.089 Uiso 1 1 calc R . . C44 C 0.2315(5) 1.2213(8) 0.8698(4) 0.077(2) Uani 1 1 d . . . H51A H 0.2187 1.3100 0.8829 0.093 Uiso 1 1 calc R . . C45 C 0.2684(4) 1.1310(8) 0.9159(3) 0.0724(19) Uani 1 1 d . . . H13A H 0.2796 1.1573 0.9605 0.087 Uiso 1 1 calc R . . C46 C 0.2885(3) 1.0011(7) 0.8957(3) 0.0598(14) Uani 1 1 d . . . H21A H 0.3149 0.9397 0.9263 0.072 Uiso 1 1 calc R . . C51 C 0.0849(3) 0.4041(5) 0.5980(3) 0.0516(12) Uani 1 1 d . . . C52 C 0.0594(4) 0.3407(6) 0.5379(3) 0.0665(16) Uani 1 1 d . . . H4A H 0.0957 0.3058 0.5114 0.080 Uiso 1 1 calc R . . C53 C -0.0203(5) 0.3295(7) 0.5177(4) 0.078(2) Uani 1 1 d . . . H18A H -0.0379 0.2852 0.4777 0.093 Uiso 1 1 calc R . . C54 C -0.0747(4) 0.3839(8) 0.5565(4) 0.084(2) Uani 1 1 d . . . H10A H -0.1286 0.3784 0.5422 0.101 Uiso 1 1 calc R . . C55 C -0.0479(4) 0.4448(8) 0.6153(4) 0.0754(19) Uani 1 1 d . . . H19A H -0.0841 0.4807 0.6417 0.091 Uiso 1 1 calc R . . C56 C 0.0315(3) 0.4549(6) 0.6369(3) 0.0586(14) Uani 1 1 d . . . H27A H 0.0487 0.4960 0.6778 0.070 Uiso 1 1 calc R . . C61 C 0.5230(3) 0.7478(6) 0.5496(3) 0.0537(13) Uani 1 1 d . . . C62 C 0.5064(4) 0.6945(6) 0.4863(4) 0.0668(17) Uani 1 1 d . . . H7A H 0.4761 0.6146 0.4787 0.080 Uiso 1 1 calc R . . C63 C 0.5353(5) 0.7617(9) 0.4343(4) 0.084(2) Uani 1 1 d . . . H6A H 0.5243 0.7269 0.3911 0.101 Uiso 1 1 calc R . . C64 C 0.5799(5) 0.8789(8) 0.4452(5) 0.090(3) Uani 1 1 d . . . H1A H 0.5988 0.9238 0.4096 0.108 Uiso 1 1 calc R . . C65 C 0.5965(4) 0.9296(8) 0.5082(5) 0.086(3) Uani 1 1 d . . . H2A H 0.6280 1.0082 0.5155 0.104 Uiso 1 1 calc R . . C66 C 0.5674(3) 0.8665(7) 0.5614(4) 0.0655(16) Uani 1 1 d . . . H14A H 0.5775 0.9031 0.6042 0.079 Uiso 1 1 calc R . . C1 C -0.0262(4) 0.9988(9) 0.6398(4) 0.082(2) Uani 1 1 d . . . H10B H -0.0589 1.0049 0.5963 0.099 Uiso 1 1 calc R . . Cl1 Cl 0.0649(2) 1.0196(5) 0.6243(4) 0.261(4) Uani 1 1 d . . . Cl2 Cl -0.0318(2) 0.8282(4) 0.6644(3) 0.194(2) Uani 1 1 d . . . Cl3 Cl -0.0689(4) 1.0960(5) 0.68922(17) 0.255(4) Uani 1 1 d . . . H1 H 0.383(3) 0.453(6) 0.744(3) 0.060(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0351(3) 0.0300(3) 0.0314(3) 0.00040(17) 0.00363(18) -0.00202(17) S11 0.0426(6) 0.0455(6) 0.0301(5) 0.0010(4) 0.0030(4) -0.0147(4) S21 0.0333(5) 0.0304(5) 0.0472(6) -0.0007(4) 0.0082(4) -0.0019(4) S31 0.0404(6) 0.0512(7) 0.0397(6) -0.0055(5) 0.0095(4) 0.0035(5) B 0.039(3) 0.048(3) 0.053(3) 0.014(2) 0.007(2) 0.006(2) N11 0.0374(18) 0.050(2) 0.0396(19) 0.0127(17) 0.0028(15) -0.0020(16) N12 0.049(2) 0.056(2) 0.0320(18) 0.0050(17) 0.0083(16) -0.0063(18) N21 0.045(2) 0.034(2) 0.054(2) 0.0022(17) 0.0157(17) 0.0031(16) N22 0.055(2) 0.034(2) 0.049(2) -0.0064(16) 0.0128(18) -0.0044(17) N31 0.0360(19) 0.050(2) 0.052(2) 0.0097(18) 0.0060(16) 0.0074(16) N32 0.0342(19) 0.052(3) 0.066(3) 0.012(2) 0.0150(18) 0.0060(17) N1 0.046(2) 0.042(2) 0.0387(19) 0.0052(16) 0.0037(16) -0.0011(16) O1 0.119(4) 0.066(3) 0.066(3) 0.028(2) -0.019(3) 0.010(3) O2 0.080(3) 0.058(2) 0.050(2) -0.0126(18) 0.0007(19) 0.000(2) O3 0.064(2) 0.0347(17) 0.0368(16) 0.0009(13) -0.0015(14) 0.0012(15) C11 0.035(2) 0.049(3) 0.0308(19) 0.0043(17) 0.0012(16) -0.0069(18) C12 0.059(3) 0.061(3) 0.050(3) 0.022(3) 0.012(2) -0.002(3) C13 0.067(3) 0.068(4) 0.038(2) 0.014(2) 0.016(2) -0.006(3) C21 0.039(2) 0.034(2) 0.042(2) 0.0008(17) 0.0114(17) -0.0040(17) C22 0.061(3) 0.040(3) 0.071(4) 0.002(2) 0.025(3) 0.012(2) C23 0.071(4) 0.035(3) 0.072(4) -0.010(2) 0.020(3) -0.001(2) C31 0.037(2) 0.041(2) 0.053(3) 0.004(2) 0.0135(19) 0.0078(18) C32 0.038(2) 0.076(4) 0.068(3) 0.018(3) 0.003(2) 0.015(2) C33 0.031(2) 0.081(4) 0.078(4) 0.017(3) 0.009(2) 0.011(2) C41 0.049(3) 0.057(3) 0.038(2) -0.002(2) 0.0115(19) -0.010(2) C42 0.069(3) 0.070(4) 0.042(3) -0.001(2) 0.010(2) 0.006(3) C43 0.088(5) 0.076(4) 0.063(4) 0.005(3) 0.025(3) 0.011(4) C44 0.087(5) 0.073(4) 0.080(4) -0.023(4) 0.043(4) -0.015(4) C45 0.075(4) 0.091(5) 0.055(3) -0.031(4) 0.026(3) -0.030(4) C46 0.062(3) 0.082(4) 0.037(2) -0.006(3) 0.009(2) -0.016(3) C51 0.060(3) 0.037(3) 0.056(3) -0.001(2) 0.000(2) -0.016(2) C52 0.089(4) 0.041(3) 0.066(4) -0.010(3) -0.005(3) -0.004(3) C53 0.089(5) 0.054(4) 0.080(5) -0.010(3) -0.028(4) -0.019(3) C54 0.067(4) 0.069(4) 0.109(6) 0.003(4) -0.016(4) -0.026(3) C55 0.054(3) 0.078(5) 0.094(5) -0.002(4) 0.013(3) -0.021(3) C56 0.050(3) 0.067(4) 0.061(3) -0.005(3) 0.015(2) -0.018(3) C61 0.038(2) 0.052(3) 0.075(4) 0.013(3) 0.026(2) 0.012(2) C62 0.073(4) 0.053(3) 0.084(4) 0.008(3) 0.044(3) 0.009(3) C63 0.095(5) 0.085(5) 0.083(5) 0.007(4) 0.054(4) 0.014(4) C64 0.086(5) 0.074(5) 0.123(7) 0.032(5) 0.065(5) 0.013(4) C65 0.051(3) 0.068(4) 0.145(8) 0.034(5) 0.034(4) 0.001(3) C66 0.043(3) 0.058(3) 0.097(5) 0.009(3) 0.017(3) -0.001(2) C1 0.056(3) 0.122(7) 0.068(4) 0.017(4) 0.003(3) 0.012(4) Cl1 0.106(2) 0.168(4) 0.524(10) 0.182(5) 0.100(4) 0.014(2) Cl2 0.130(3) 0.100(2) 0.354(7) 0.036(3) 0.037(3) -0.0280(19) Cl3 0.468(8) 0.211(4) 0.106(2) 0.060(2) 0.118(4) 0.239(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn O3 2.001(3) . ? Zn S31 2.3132(13) . ? Zn S21 2.3144(12) . ? Zn S11 2.3686(12) . ? S11 C11 1.722(4) . ? S21 C21 1.731(5) . ? S31 C31 1.719(5) . ? B N31 1.549(7) . ? B N21 1.556(7) . ? B N11 1.561(8) . ? N11 C11 1.355(6) . ? N11 C12 1.395(6) . ? N12 C11 1.367(6) . ? N12 C13 1.392(7) . ? N12 C41 1.438(7) . ? N21 C21 1.358(6) . ? N21 C22 1.395(7) . ? N22 C21 1.359(6) . ? N22 C23 1.380(7) . ? N22 C51 1.453(7) . ? N31 C31 1.352(6) . ? N31 C32 1.399(6) . ? N32 C31 1.367(6) . ? N32 C33 1.386(7) . ? N32 C61 1.438(7) . ? N1 O2 1.223(6) . ? N1 O1 1.231(6) . ? N1 O3 1.289(5) . ? C12 C13 1.336(9) . ? C22 C23 1.340(9) . ? C32 C33 1.340(8) . ? C41 C46 1.378(7) . ? C41 C42 1.379(8) . ? C42 C43 1.388(9) . ? C43 C44 1.372(10) . ? C44 C45 1.384(11) . ? C45 C46 1.390(10) . ? C51 C56 1.379(8) . ? C51 C52 1.394(8) . ? C52 C53 1.386(10) . ? C53 C54 1.401(12) . ? C54 C55 1.366(11) . ? C55 C56 1.387(8) . ? C61 C62 1.387(10) . ? C61 C66 1.392(9) . ? C62 C63 1.390(9) . ? C63 C64 1.380(12) . ? C64 C65 1.372(13) . ? C65 C66 1.394(10) . ? C1 Cl3 1.624(9) . ? C1 Cl1 1.652(8) . ? C1 Cl2 1.744(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn S31 116.59(11) . . ? O3 Zn S21 113.73(11) . . ? S31 Zn S21 112.06(5) . . ? O3 Zn S11 98.60(10) . . ? S31 Zn S11 105.50(5) . . ? S21 Zn S11 108.83(5) . . ? C11 S11 Zn 93.77(15) . . ? C21 S21 Zn 98.89(15) . . ? C31 S31 Zn 98.15(16) . . ? N31 B N21 114.4(4) . . ? N31 B N11 113.0(4) . . ? N21 B N11 111.1(4) . . ? C11 N11 C12 107.7(4) . . ? C11 N11 B 132.9(4) . . ? C12 N11 B 119.3(4) . . ? C11 N12 C13 108.8(4) . . ? C11 N12 C41 128.1(4) . . ? C13 N12 C41 123.1(4) . . ? C21 N21 C22 107.3(4) . . ? C21 N21 B 132.9(4) . . ? C22 N21 B 119.2(4) . . ? C21 N22 C23 109.0(4) . . ? C21 N22 C51 127.5(4) . . ? C23 N22 C51 123.4(4) . . ? C31 N31 C32 107.7(4) . . ? C31 N31 B 133.8(4) . . ? C32 N31 B 118.5(4) . . ? C31 N32 C33 109.0(4) . . ? C31 N32 C61 127.1(5) . . ? C33 N32 C61 123.7(4) . . ? O2 N1 O1 122.8(4) . . ? O2 N1 O3 118.7(4) . . ? O1 N1 O3 118.5(4) . . ? N1 O3 Zn 112.5(3) . . ? N11 C11 N12 107.6(4) . . ? N11 C11 S11 127.6(4) . . ? N12 C11 S11 124.8(4) . . ? C13 C12 N11 109.1(5) . . ? C12 C13 N12 106.8(4) . . ? N21 C21 N22 107.8(4) . . ? N21 C21 S21 128.7(3) . . ? N22 C21 S21 123.5(3) . . ? C23 C22 N21 108.8(5) . . ? C22 C23 N22 107.1(5) . . ? N31 C31 N32 107.6(4) . . ? N31 C31 S31 128.3(4) . . ? N32 C31 S31 124.1(4) . . ? C33 C32 N31 108.7(5) . . ? C32 C33 N32 107.0(5) . . ? C46 C41 C42 121.5(6) . . ? C46 C41 N12 118.3(5) . . ? C42 C41 N12 120.2(5) . . ? C41 C42 C43 118.3(6) . . ? C44 C43 C42 121.1(7) . . ? C43 C44 C45 120.3(7) . . ? C44 C45 C46 119.3(6) . . ? C41 C46 C45 119.6(6) . . ? C56 C51 C52 120.2(6) . . ? C56 C51 N22 120.5(5) . . ? C52 C51 N22 119.2(5) . . ? C53 C52 C51 119.3(7) . . ? C52 C53 C54 120.5(6) . . ? C55 C54 C53 118.9(6) . . ? C54 C55 C56 121.5(7) . . ? C51 C56 C55 119.6(6) . . ? C62 C61 C66 121.2(6) . . ? C62 C61 N32 120.3(5) . . ? C66 C61 N32 118.4(6) . . ? C61 C62 C63 118.7(7) . . ? C64 C63 C62 120.8(8) . . ? C65 C64 C63 119.9(7) . . ? C64 C65 C66 121.0(7) . . ? C61 C66 C65 118.4(7) . . ? Cl3 C1 Cl1 124.0(7) . . ? Cl3 C1 Cl2 109.5(5) . . ? Cl1 C1 Cl2 105.0(5) . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 2.279 _refine_diff_density_min -1.870 _refine_diff_density_rms 0.113 data_zns33 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H23 B Cl3 I N6 S3 Zn' _chemical_formula_weight 849.13 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' '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' '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 18.6903(15) _cell_length_b 12.3699(10) _cell_length_c 14.2711(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3299.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 2.143 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6738 _exptl_absorpt_correction_T_max 0.8142 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23786 _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_av_sigmaI/netI 0.0802 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 28.29 _reflns_number_total 6487 _reflns_number_gt 4619 _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^)+(0.0239P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00023(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(15) _refine_ls_number_reflns 6487 _refine_ls_number_parameters 393 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0693 _refine_ls_wR_factor_gt 0.0614 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _refine_ls_shift/su_max 0.042 _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 Zn Zn 0.72365(3) -0.24817(5) 0.75611(5) 0.02472(14) Uani 1 1 d . . . I I 0.641322(18) -0.26973(3) 0.61401(2) 0.02999(10) Uani 1 1 d . . . S1 S 0.65590(7) -0.24807(11) 0.89642(10) 0.0267(4) Uani 1 1 d . . . S2 S 0.79386(7) -0.09038(10) 0.75922(10) 0.0258(3) Uani 1 1 d . . . S3 S 0.80564(8) -0.39203(11) 0.77174(9) 0.0247(3) Uani 1 1 d . . . N11 N 0.7713(2) -0.1453(3) 0.9783(3) 0.0220(10) Uani 1 1 d . . . N12 N 0.6744(2) -0.0484(4) 0.9738(3) 0.0265(11) Uani 1 1 d . . . N21 N 0.8824(2) -0.2015(4) 0.8842(3) 0.0233(11) Uani 1 1 d . . . N22 N 0.9319(2) -0.1567(4) 0.7508(3) 0.0253(11) Uani 1 1 d . . . N31 N 0.8035(2) -0.3470(3) 0.9620(3) 0.0246(11) Uani 1 1 d . . . N32 N 0.7525(3) -0.4999(3) 0.9224(3) 0.0252(11) Uani 1 1 d . . . C11 C 0.7032(3) -0.1457(4) 0.9502(3) 0.0236(12) Uani 1 1 d . . . C12 C 0.7853(3) -0.0460(4) 1.0205(4) 0.0283(14) Uani 1 1 d . . . H12A H 0.8292 -0.0246 1.0468 0.034 Uiso 1 1 calc R . . C13 C 0.7260(3) 0.0136(5) 1.0172(4) 0.0301(15) Uani 1 1 d . . . H13A H 0.7204 0.0844 1.0400 0.036 Uiso 1 1 calc R . . C21 C 0.8709(3) -0.1512(4) 0.8003(3) 0.0211(12) Uani 1 1 d . . . C22 C 0.9528(3) -0.2374(5) 0.8839(4) 0.0281(13) Uani 1 1 d . . . H22A H 0.9755 -0.2740 0.9334 0.034 Uiso 1 1 calc R . . C23 C 0.9832(3) -0.2116(4) 0.8021(4) 0.0292(13) Uani 1 1 d . . . H23A H 1.0301 -0.2275 0.7831 0.035 Uiso 1 1 calc R . . C31 C 0.7869(3) -0.4114(4) 0.8895(3) 0.0215(12) Uani 1 1 d . . . C32 C 0.7783(3) -0.3967(4) 1.0431(4) 0.0283(14) Uani 1 1 d . . . H32A H 0.7827 -0.3690 1.1042 0.034 Uiso 1 1 calc R . . C33 C 0.7467(3) -0.4901(5) 1.0203(4) 0.0300(15) Uani 1 1 d . . . H33A H 0.7250 -0.5395 1.0615 0.036 Uiso 1 1 calc R . . C41 C 0.6023(3) -0.0149(5) 0.9591(5) 0.0349(15) Uani 1 1 d . . . C42 C 0.5612(4) 0.0176(5) 1.0346(5) 0.053(2) Uani 1 1 d . . . H42A H 0.5803 0.0164 1.0955 0.063 Uiso 1 1 calc R . . C43 C 0.4924(5) 0.0514(6) 1.0198(8) 0.076(3) Uani 1 1 d . . . H43A H 0.4644 0.0738 1.0710 0.092 Uiso 1 1 calc R . . C44 C 0.4635(4) 0.0529(7) 0.9303(9) 0.086(3) Uani 1 1 d . . . H44A H 0.4164 0.0772 0.9208 0.103 Uiso 1 1 calc R . . C45 C 0.5038(5) 0.0190(6) 0.8558(8) 0.068(2) Uani 1 1 d . . . H45A H 0.4836 0.0174 0.7955 0.081 Uiso 1 1 calc R . . C46 C 0.5736(4) -0.0129(5) 0.8683(5) 0.0464(18) Uani 1 1 d . . . H46A H 0.6018 -0.0330 0.8167 0.056 Uiso 1 1 calc R . . C51 C 0.9425(3) -0.1192(4) 0.6560(4) 0.0256(13) Uani 1 1 d . . . C52 C 0.9770(4) -0.0237(5) 0.6403(4) 0.0447(19) Uani 1 1 d . . . H52A H 0.9916 0.0194 0.6910 0.054 Uiso 1 1 calc R . . C53 C 0.9904(4) 0.0093(6) 0.5492(5) 0.051(2) Uani 1 1 d . . . H53A H 1.0134 0.0755 0.5378 0.061 Uiso 1 1 calc R . . C54 C 0.9699(4) -0.0550(6) 0.4763(5) 0.050(2) Uani 1 1 d . . . H54A H 0.9778 -0.0317 0.4145 0.061 Uiso 1 1 calc R . . C55 C 0.9379(4) -0.1532(7) 0.4919(4) 0.049(2) Uani 1 1 d . . . H55A H 0.9258 -0.1984 0.4414 0.059 Uiso 1 1 calc R . . C56 C 0.9237(4) -0.1847(5) 0.5824(4) 0.0409(17) Uani 1 1 d . . . H56A H 0.9011 -0.2512 0.5939 0.049 Uiso 1 1 calc R . . C71 C 0.7210(3) -0.5861(4) 0.8699(4) 0.0268(13) Uani 1 1 d . . . C72 C 0.6724(3) -0.5637(5) 0.7997(4) 0.0274(13) Uani 1 1 d . . . H72A H 0.6611 -0.4918 0.7843 0.033 Uiso 1 1 calc R . . C73 C 0.6401(3) -0.6493(5) 0.7520(4) 0.0328(13) Uani 1 1 d . . . H73A H 0.6065 -0.6348 0.7046 0.039 Uiso 1 1 calc R . . C74 C 0.6570(4) -0.7543(6) 0.7736(4) 0.0390(17) Uani 1 1 d . . . H74A H 0.6345 -0.8114 0.7417 0.047 Uiso 1 1 calc R . . C75 C 0.7072(4) -0.7760(5) 0.8427(4) 0.0402(16) Uani 1 1 d . . . H75A H 0.7198 -0.8479 0.8565 0.048 Uiso 1 1 calc R . . C76 C 0.7389(3) -0.6913(5) 0.8913(4) 0.0313(14) Uani 1 1 d . . . H76A H 0.7725 -0.7058 0.9387 0.038 Uiso 1 1 calc R . . B B 0.8328(3) -0.2307(5) 0.9680(4) 0.0215(14) Uani 1 1 d . . . H1 H 0.862(3) -0.229(4) 1.032(4) 0.026 Uiso 1 1 d . . . C01 C 0.8974(3) -0.7742(6) 0.6917(5) 0.0509(19) Uani 1 1 d . . . H01A H 0.8809 -0.8357 0.6529 0.061 Uiso 1 1 calc R . . Cl1 Cl 0.90845(12) -0.81878(17) 0.80764(14) 0.0705(6) Uani 1 1 d . . . Cl2 Cl 0.83417(10) -0.67118(17) 0.68508(13) 0.0621(6) Uani 1 1 d . . . Cl3 Cl 0.98034(10) -0.72687(16) 0.64692(13) 0.0644(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 Zn 0.0238(3) 0.0285(3) 0.0218(3) -0.0002(3) -0.0017(3) 0.0006(3) I 0.02593(16) 0.0418(2) 0.02221(15) -0.0005(3) -0.0036(2) 0.00130(18) S1 0.0246(8) 0.0299(10) 0.0255(6) -0.0051(6) 0.0007(6) -0.0018(6) S2 0.0224(8) 0.0268(7) 0.0281(7) 0.0051(7) -0.0030(7) 0.0015(6) S3 0.0298(8) 0.0267(8) 0.0176(7) 0.0007(6) 0.0018(6) 0.0024(6) N11 0.020(3) 0.030(3) 0.016(2) -0.0064(19) -0.002(2) -0.004(2) N12 0.028(3) 0.023(3) 0.029(3) -0.002(2) 0.004(2) 0.002(2) N21 0.021(3) 0.024(3) 0.025(2) 0.000(2) -0.0039(19) 0.0034(19) N22 0.021(3) 0.031(3) 0.024(2) -0.002(2) 0.002(2) -0.001(2) N31 0.027(3) 0.028(3) 0.018(2) 0.0014(19) -0.001(2) 0.000(2) N32 0.034(3) 0.023(3) 0.019(2) 0.0030(19) -0.004(2) -0.002(2) C11 0.031(3) 0.021(3) 0.019(3) 0.003(2) 0.003(2) -0.006(2) C12 0.032(4) 0.026(4) 0.027(3) -0.003(3) -0.005(3) -0.004(3) C13 0.040(4) 0.027(4) 0.023(3) -0.004(3) 0.001(3) -0.010(3) C21 0.024(3) 0.018(3) 0.021(3) 0.001(2) -0.001(2) 0.001(2) C22 0.021(3) 0.031(4) 0.032(3) 0.002(3) -0.006(2) 0.005(3) C23 0.023(3) 0.034(4) 0.030(3) 0.000(3) -0.002(3) 0.008(3) C31 0.026(3) 0.024(3) 0.014(3) 0.005(2) 0.000(2) 0.002(2) C32 0.032(4) 0.034(4) 0.019(3) 0.005(2) -0.002(3) -0.004(3) C33 0.041(4) 0.031(4) 0.018(3) 0.001(3) 0.000(3) -0.004(3) C41 0.034(4) 0.016(4) 0.054(4) 0.004(3) -0.001(3) 0.002(3) C42 0.050(5) 0.040(5) 0.068(5) -0.001(4) 0.009(4) 0.011(4) C43 0.043(6) 0.048(5) 0.139(9) 0.005(6) 0.040(6) 0.017(4) C44 0.031(5) 0.040(5) 0.186(12) 0.000(7) -0.011(7) 0.003(4) C45 0.045(5) 0.045(6) 0.112(7) 0.015(5) -0.026(5) -0.001(4) C46 0.034(4) 0.035(4) 0.070(5) 0.007(3) -0.009(4) 0.000(3) C51 0.021(3) 0.025(3) 0.031(3) 0.002(3) -0.001(3) 0.006(3) C52 0.070(5) 0.031(4) 0.034(4) 0.000(3) 0.006(3) -0.003(3) C53 0.069(6) 0.042(5) 0.042(4) 0.008(4) 0.018(4) -0.008(4) C54 0.041(4) 0.078(6) 0.032(4) 0.019(4) 0.009(3) 0.019(4) C55 0.048(5) 0.075(6) 0.025(4) -0.012(4) 0.002(3) 0.004(4) C56 0.048(4) 0.045(4) 0.030(4) 0.002(3) -0.003(3) -0.004(3) C71 0.032(3) 0.026(3) 0.022(3) 0.001(2) 0.002(3) -0.007(3) C72 0.027(3) 0.030(3) 0.025(3) 0.004(2) 0.000(3) -0.002(3) C73 0.035(3) 0.040(4) 0.023(3) 0.000(3) -0.004(3) -0.012(3) C74 0.055(4) 0.035(4) 0.028(4) -0.003(3) 0.007(3) -0.029(3) C75 0.055(5) 0.025(4) 0.042(4) 0.001(3) 0.007(3) -0.001(3) C76 0.034(4) 0.031(4) 0.028(3) 0.005(3) -0.002(3) 0.004(3) B 0.023(3) 0.021(4) 0.021(3) 0.001(3) 0.001(3) 0.002(3) C01 0.042(4) 0.051(5) 0.061(4) -0.001(4) 0.006(4) 0.018(4) Cl1 0.0896(17) 0.0668(15) 0.0552(11) 0.0173(10) -0.0075(11) 0.0237(13) Cl2 0.0545(12) 0.0796(14) 0.0521(10) 0.0193(10) 0.0099(9) 0.0289(10) Cl3 0.0475(11) 0.0649(13) 0.0808(14) 0.0061(10) 0.0057(9) 0.0093(10) _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 Zn S2 2.3523(15) . ? Zn S3 2.3590(15) . ? Zn S1 2.3692(15) . ? Zn I 2.5596(7) . ? S1 C11 1.725(5) . ? S2 C21 1.727(5) . ? S3 C31 1.734(5) . ? N11 C11 1.334(6) . ? N11 C12 1.393(7) . ? N11 B 1.568(7) . ? N12 C11 1.361(6) . ? N12 C13 1.379(7) . ? N12 C41 1.426(7) . ? N21 C21 1.366(6) . ? N21 C22 1.388(6) . ? N21 B 1.556(8) . ? N22 C21 1.344(6) . ? N22 C23 1.383(7) . ? N22 C51 1.445(7) . ? N31 C31 1.343(6) . ? N31 C32 1.393(6) . ? N31 B 1.542(8) . ? N32 C31 1.353(6) . ? N32 C33 1.406(6) . ? N32 C71 1.430(7) . ? C12 C13 1.332(8) . ? C22 C23 1.337(7) . ? C32 C33 1.338(8) . ? C41 C42 1.383(9) . ? C41 C46 1.402(9) . ? C42 C43 1.368(10) . ? C43 C44 1.388(12) . ? C44 C45 1.369(13) . ? C45 C46 1.374(10) . ? C51 C52 1.364(8) . ? C51 C56 1.372(7) . ? C52 C53 1.384(8) . ? C53 C54 1.364(10) . ? C54 C55 1.373(10) . ? C55 C56 1.374(8) . ? C71 C76 1.378(7) . ? C71 C72 1.381(7) . ? C72 C73 1.396(7) . ? C73 C74 1.371(9) . ? C74 C75 1.388(9) . ? C75 C76 1.390(8) . ? C01 Cl2 1.740(6) . ? C01 Cl1 1.756(7) . ? C01 Cl3 1.777(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Zn S3 105.17(5) . . ? S2 Zn S1 106.37(6) . . ? S3 Zn S1 105.53(5) . . ? S2 Zn I 115.90(5) . . ? S3 Zn I 112.76(4) . . ? S1 Zn I 110.39(4) . . ? C11 S1 Zn 95.86(17) . . ? C21 S2 Zn 96.33(18) . . ? C31 S3 Zn 93.72(18) . . ? C11 N11 C12 108.2(5) . . ? C11 N11 B 132.0(5) . . ? C12 N11 B 119.8(5) . . ? C11 N12 C13 109.1(5) . . ? C11 N12 C41 126.5(5) . . ? C13 N12 C41 124.4(5) . . ? C21 N21 C22 107.1(4) . . ? C21 N21 B 133.2(4) . . ? C22 N21 B 119.5(4) . . ? C21 N22 C23 109.6(5) . . ? C21 N22 C51 126.3(5) . . ? C23 N22 C51 124.0(5) . . ? C31 N31 C32 107.5(4) . . ? C31 N31 B 132.8(4) . . ? C32 N31 B 119.1(5) . . ? C31 N32 C33 108.1(4) . . ? C31 N32 C71 128.1(4) . . ? C33 N32 C71 123.6(5) . . ? N11 C11 N12 107.4(4) . . ? N11 C11 S1 128.7(4) . . ? N12 C11 S1 123.8(4) . . ? C13 C12 N11 108.4(5) . . ? C12 C13 N12 106.8(5) . . ? N22 C21 N21 107.6(5) . . ? N22 C21 S2 123.5(4) . . ? N21 C21 S2 128.9(4) . . ? C23 C22 N21 109.1(5) . . ? C22 C23 N22 106.6(5) . . ? N31 C31 N32 108.8(4) . . ? N31 C31 S3 128.2(4) . . ? N32 C31 S3 123.0(4) . . ? C33 C32 N31 109.1(5) . . ? C32 C33 N32 106.5(5) . . ? C42 C41 C46 120.2(6) . . ? C42 C41 N12 119.7(6) . . ? C46 C41 N12 120.1(6) . . ? C43 C42 C41 119.4(8) . . ? C42 C43 C44 120.8(8) . . ? C45 C44 C43 119.7(8) . . ? C44 C45 C46 120.7(10) . . ? C45 C46 C41 119.2(8) . . ? C52 C51 C56 120.4(5) . . ? C52 C51 N22 119.8(5) . . ? C56 C51 N22 119.5(5) . . ? C51 C52 C53 119.7(6) . . ? C54 C53 C52 119.5(7) . . ? C53 C54 C55 121.0(7) . . ? C54 C55 C56 119.1(7) . . ? C51 C56 C55 120.2(6) . . ? C76 C71 C72 120.7(5) . . ? C76 C71 N32 119.2(5) . . ? C72 C71 N32 120.1(5) . . ? C71 C72 C73 119.1(5) . . ? C74 C73 C72 120.6(6) . . ? C73 C74 C75 119.9(6) . . ? C74 C75 C76 119.8(6) . . ? C71 C76 C75 119.8(6) . . ? N31 B N21 112.7(5) . . ? N31 B N11 111.9(5) . . ? N21 B N11 110.7(5) . . ? Cl2 C01 Cl1 111.2(4) . . ? Cl2 C01 Cl3 109.4(4) . . ? Cl1 C01 Cl3 109.8(4) . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.527 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.099