# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Mukesh Kumar' 'Elizabeth T. Papish' 'Matthias Zeller' 'Allen D. Hunter' _publ_contact_author_email mk643@drexel.edu _publ_contact_author_name 'Mukesh Kumar' data_09mz262_0m _database_code_depnum_ccdc_archive 'CCDC 764042' #TrackingRef '- combined cifs' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H28 B N9 O2 Zn' _chemical_formula_weight 610.78 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 17.0859(14) _cell_length_b 11.2068(8) _cell_length_c 16.7846(12) _cell_angle_alpha 90.00 _cell_angle_beta 117.7980(10) _cell_angle_gamma 90.00 _cell_volume 2843.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1521 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 24.30 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.909 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.785 _exptl_absorpt_correction_T_max 0.913 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 21918 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 30.51 _reflns_number_total 8411 _reflns_number_gt 5845 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4' _computing_data_reduction 'Apex2 v2008.2-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0328P)^2^+2.0606P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8411 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0823 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1066 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.09020(17) 1.1380(2) 0.98765(18) 0.0249(5) Uani 1 1 d . . . H1A H 0.1447 1.1651 1.0395 0.037 Uiso 1 1 calc R . . H1B H 0.0452 1.1213 1.0069 0.037 Uiso 1 1 calc R . . H1C H 0.0686 1.2004 0.9414 0.037 Uiso 1 1 calc R . . C2 C 0.10847(15) 1.0278(2) 0.95012(15) 0.0186(5) Uani 1 1 d . . . C3 C 0.10101(14) 0.8518(2) 0.90068(15) 0.0180(5) Uani 1 1 d . . . B1 B 0.23607(17) 1.1106(2) 0.92097(18) 0.0179(5) Uani 1 1 d . . . H1 H 0.2273 1.1894 0.9437 0.021 Uiso 1 1 calc R . . C4 C 0.06813(14) 0.7292(2) 0.87346(15) 0.0192(5) Uani 1 1 d . . . C5 C 0.06852(15) 0.6772(2) 0.79827(16) 0.0226(5) Uani 1 1 d . . . H5 H 0.0931 0.7188 0.7659 0.027 Uiso 1 1 calc R . . C6 C 0.03271(16) 0.5642(2) 0.77094(17) 0.0276(6) Uani 1 1 d . . . H6 H 0.0339 0.5279 0.7203 0.033 Uiso 1 1 calc R . . C7 C -0.00463(16) 0.5040(2) 0.81680(18) 0.0296(6) Uani 1 1 d . . . H7 H -0.0294 0.4270 0.7974 0.035 Uiso 1 1 calc R . . C8 C -0.00591(16) 0.5558(2) 0.89077(18) 0.0277(6) Uani 1 1 d . . . H8 H -0.0322 0.5147 0.9218 0.033 Uiso 1 1 calc R . . C9 C 0.03114(15) 0.6681(2) 0.92003(17) 0.0229(5) Uani 1 1 d . . . H9 H 0.0312 0.7030 0.9716 0.027 Uiso 1 1 calc R . . C10 C 0.16246(17) 1.3292(2) 0.78002(17) 0.0251(5) Uani 1 1 d . . . H10A H 0.2113 1.3818 0.8186 0.038 Uiso 1 1 calc R . . H10B H 0.1252 1.3130 0.8089 0.038 Uiso 1 1 calc R . . H10C H 0.1269 1.3679 0.7217 0.038 Uiso 1 1 calc R . . C11 C 0.19870(14) 1.2153(2) 0.76611(16) 0.0190(5) Uani 1 1 d . . . C12 C 0.24127(14) 1.0779(2) 0.70862(15) 0.0169(4) Uani 1 1 d . . . C13 C 0.26608(15) 1.0142(2) 0.64758(15) 0.0184(5) Uani 1 1 d . . . C14 C 0.33997(16) 0.9400(2) 0.68096(17) 0.0263(6) Uani 1 1 d . . . H14 H 0.3744 0.9289 0.7441 0.032 Uiso 1 1 calc R . . C15 C 0.36322(17) 0.8821(3) 0.62178(18) 0.0332(6) Uani 1 1 d . . . H15 H 0.4138 0.8318 0.6446 0.040 Uiso 1 1 calc R . . C16 C 0.31273(17) 0.8976(2) 0.52949(18) 0.0293(6) Uani 1 1 d . . . H16 H 0.3284 0.8574 0.4891 0.035 Uiso 1 1 calc R . . C17 C 0.23978(16) 0.9717(2) 0.49648(16) 0.0243(5) Uani 1 1 d . . . H17 H 0.2052 0.9820 0.4333 0.029 Uiso 1 1 calc R . . C18 C 0.21656(15) 1.0312(2) 0.55485(16) 0.0206(5) Uani 1 1 d . . . H18 H 0.1670 1.0834 0.5317 0.025 Uiso 1 1 calc R . . C19 C 0.37853(17) 1.2055(2) 1.11202(17) 0.0273(6) Uani 1 1 d . . . H19A H 0.3314 1.1938 1.1290 0.041 Uiso 1 1 calc R . . H19B H 0.3633 1.2727 1.0700 0.041 Uiso 1 1 calc R . . H19C H 0.4343 1.2225 1.1660 0.041 Uiso 1 1 calc R . . C20 C 0.38854(15) 1.0952(2) 1.06792(16) 0.0200(5) Uani 1 1 d . . . C21 C 0.43416(14) 0.9310(2) 1.04215(15) 0.0179(5) Uani 1 1 d . . . C22 C 0.48949(15) 0.8251(2) 1.05586(16) 0.0200(5) Uani 1 1 d . . . C23 C 0.47913(15) 0.7526(2) 0.98407(17) 0.0230(5) Uani 1 1 d . . . H23 H 0.4378 0.7741 0.9243 0.028 Uiso 1 1 calc R . . C24 C 0.52863(16) 0.6494(2) 0.99933(18) 0.0259(6) Uani 1 1 d . . . H24 H 0.5208 0.6001 0.9501 0.031 Uiso 1 1 calc R . . C25 C 0.58988(16) 0.6174(2) 1.08659(18) 0.0271(6) Uani 1 1 d . . . H25 H 0.6233 0.5460 1.0971 0.033 Uiso 1 1 calc R . . C26 C 0.60178(15) 0.6902(2) 1.15791(17) 0.0255(5) Uani 1 1 d . . . H26 H 0.6441 0.6693 1.2175 0.031 Uiso 1 1 calc R . . C27 C 0.55237(15) 0.7937(2) 1.14304(16) 0.0227(5) Uani 1 1 d . . . H27 H 0.5613 0.8435 1.1924 0.027 Uiso 1 1 calc R . . C28 C 0.23165(17) 0.7166(2) 0.72615(17) 0.0269(6) Uani 1 1 d . . . C29 C 0.2458(2) 0.6153(3) 0.6753(2) 0.0422(8) Uani 1 1 d . . . H29A H 0.2868 0.5573 0.7181 0.063 Uiso 1 1 calc R . . H29B H 0.2708 0.6464 0.6374 0.063 Uiso 1 1 calc R . . H29C H 0.1891 0.5763 0.6373 0.063 Uiso 1 1 calc R . . N1 N 0.16406(12) 0.90454(16) 0.88737(13) 0.0177(4) Uani 1 1 d . . . N2 N 0.16749(12) 1.01926(16) 0.91900(12) 0.0166(4) Uani 1 1 d . . . N3 N 0.06561(12) 0.92462(17) 0.93976(13) 0.0200(4) Uani 1 1 d . . . N4 N 0.25260(12) 1.03367(17) 0.78729(12) 0.0178(4) Uani 1 1 d . . . N5 N 0.22645(12) 1.12426(16) 0.82507(13) 0.0171(4) Uani 1 1 d . . . N6 N 0.20751(12) 1.19000(17) 0.69284(13) 0.0193(4) Uani 1 1 d . . . N7 N 0.35752(12) 0.95087(17) 0.96868(13) 0.0183(4) Uani 1 1 d . . . N8 N 0.32864(12) 1.05952(17) 0.98514(13) 0.0177(4) Uani 1 1 d . . . N9 N 0.45557(13) 1.01870(18) 1.10507(13) 0.0218(4) Uani 1 1 d . . . O1 O 0.28968(11) 0.72720(15) 0.81057(11) 0.0257(4) Uani 1 1 d . . . O2 O 0.16869(12) 0.78551(16) 0.69004(12) 0.0310(4) Uani 1 1 d . . . Zn1 Zn 0.261047(17) 0.87467(2) 0.848888(18) 0.01786(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0294(13) 0.0216(12) 0.0326(14) -0.0072(11) 0.0220(11) -0.0044(10) C2 0.0195(11) 0.0187(11) 0.0185(11) -0.0003(9) 0.0096(9) 0.0004(9) C3 0.0177(10) 0.0178(11) 0.0162(11) 0.0000(9) 0.0060(9) 0.0002(8) B1 0.0201(12) 0.0143(12) 0.0201(13) -0.0024(10) 0.0101(10) -0.0004(10) C4 0.0166(10) 0.0140(11) 0.0218(12) 0.0008(9) 0.0045(9) 0.0005(8) C5 0.0216(11) 0.0194(12) 0.0213(12) 0.0001(10) 0.0054(10) 0.0026(9) C6 0.0283(13) 0.0199(13) 0.0229(13) -0.0046(10) 0.0020(11) 0.0050(10) C7 0.0205(12) 0.0146(12) 0.0373(15) 0.0002(11) -0.0002(11) -0.0012(9) C8 0.0200(12) 0.0208(13) 0.0387(15) 0.0043(11) 0.0107(11) -0.0005(10) C9 0.0226(12) 0.0188(11) 0.0276(13) -0.0002(10) 0.0122(10) 0.0008(9) C10 0.0286(13) 0.0195(12) 0.0287(14) -0.0026(10) 0.0146(11) 0.0031(10) C11 0.0173(10) 0.0163(11) 0.0227(12) 0.0007(9) 0.0088(9) -0.0014(8) C12 0.0154(10) 0.0182(11) 0.0168(11) 0.0012(9) 0.0074(9) 0.0003(8) C13 0.0185(11) 0.0196(11) 0.0181(11) -0.0001(9) 0.0094(9) -0.0007(9) C14 0.0226(12) 0.0360(15) 0.0197(12) -0.0003(11) 0.0094(10) 0.0075(11) C15 0.0248(12) 0.0428(17) 0.0316(15) -0.0042(13) 0.0129(11) 0.0099(12) C16 0.0323(14) 0.0344(15) 0.0301(14) -0.0104(12) 0.0219(12) -0.0037(11) C17 0.0294(13) 0.0267(13) 0.0182(12) -0.0021(10) 0.0122(10) -0.0090(10) C18 0.0191(11) 0.0188(12) 0.0221(12) 0.0011(10) 0.0081(9) -0.0008(9) C19 0.0287(13) 0.0288(14) 0.0231(13) -0.0091(11) 0.0110(11) -0.0024(11) C20 0.0230(11) 0.0204(12) 0.0192(12) -0.0035(9) 0.0120(10) -0.0066(9) C21 0.0182(10) 0.0193(11) 0.0167(11) 0.0014(9) 0.0085(9) -0.0036(9) C22 0.0188(11) 0.0201(12) 0.0220(12) -0.0001(10) 0.0102(9) -0.0048(9) C23 0.0184(11) 0.0259(13) 0.0228(12) -0.0007(10) 0.0082(10) -0.0031(10) C24 0.0228(12) 0.0262(13) 0.0299(14) -0.0053(11) 0.0133(11) -0.0040(10) C25 0.0204(11) 0.0251(13) 0.0342(14) 0.0009(11) 0.0113(11) -0.0008(10) C26 0.0186(11) 0.0293(14) 0.0252(13) 0.0049(11) 0.0072(10) -0.0020(10) C27 0.0192(11) 0.0258(13) 0.0222(12) -0.0001(10) 0.0089(10) -0.0056(10) C28 0.0316(13) 0.0231(13) 0.0262(14) -0.0049(11) 0.0137(11) -0.0024(11) C29 0.0550(19) 0.0356(17) 0.0326(16) -0.0167(13) 0.0175(15) 0.0024(14) N1 0.0214(9) 0.0146(9) 0.0179(10) -0.0018(7) 0.0096(8) 0.0005(7) N2 0.0202(9) 0.0145(9) 0.0166(9) -0.0026(7) 0.0097(8) -0.0007(7) N3 0.0221(10) 0.0184(10) 0.0214(10) -0.0004(8) 0.0119(8) -0.0001(8) N4 0.0224(10) 0.0161(9) 0.0168(10) -0.0014(8) 0.0108(8) 0.0031(8) N5 0.0198(9) 0.0128(9) 0.0211(10) -0.0026(8) 0.0116(8) 0.0001(7) N6 0.0188(9) 0.0182(10) 0.0200(10) 0.0008(8) 0.0082(8) 0.0015(8) N7 0.0200(9) 0.0158(9) 0.0209(10) -0.0019(8) 0.0111(8) -0.0008(7) N8 0.0210(9) 0.0153(9) 0.0189(10) -0.0020(8) 0.0111(8) -0.0008(7) N9 0.0223(10) 0.0233(11) 0.0181(10) -0.0013(8) 0.0079(8) -0.0027(8) O1 0.0291(9) 0.0242(9) 0.0218(9) -0.0067(7) 0.0102(7) 0.0024(7) O2 0.0322(10) 0.0273(10) 0.0308(10) 0.0014(8) 0.0125(8) 0.0015(8) Zn1 0.02024(13) 0.01587(13) 0.01714(14) -0.00129(11) 0.00844(10) 0.00121(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.484(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N3 1.336(3) . ? C2 N2 1.338(3) . ? C3 N1 1.336(3) . ? C3 N3 1.354(3) . ? C3 C4 1.473(3) . ? B1 N2 1.545(3) . ? B1 N5 1.547(3) . ? B1 N8 1.549(3) . ? B1 H1 1.0000 . ? C4 C5 1.393(3) . ? C4 C9 1.393(3) . ? C5 C6 1.388(3) . ? C5 H5 0.9500 . ? C6 C7 1.383(4) . ? C6 H6 0.9500 . ? C7 C8 1.380(4) . ? C7 H7 0.9500 . ? C8 C9 1.391(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.484(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N6 1.337(3) . ? C11 N5 1.344(3) . ? C12 N4 1.337(3) . ? C12 N6 1.356(3) . ? C12 C13 1.464(3) . ? C13 C14 1.393(3) . ? C13 C18 1.395(3) . ? C14 C15 1.390(3) . ? C14 H14 0.9500 . ? C15 C16 1.388(4) . ? C15 H15 0.9500 . ? C16 C17 1.380(4) . ? C16 H16 0.9500 . ? C17 C18 1.387(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.491(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 N9 1.330(3) . ? C20 N8 1.346(3) . ? C21 N7 1.334(3) . ? C21 N9 1.362(3) . ? C21 C22 1.467(3) . ? C22 C23 1.395(3) . ? C22 C27 1.397(3) . ? C23 C24 1.385(3) . ? C23 H23 0.9500 . ? C24 C25 1.393(4) . ? C24 H24 0.9500 . ? C25 C26 1.384(4) . ? C25 H25 0.9500 . ? C26 C27 1.387(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 O2 1.230(3) . ? C28 O1 1.302(3) . ? C28 C29 1.507(4) . ? C28 Zn1 2.582(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? N1 N2 1.382(2) . ? N1 Zn1 2.0672(19) . ? N4 N5 1.377(2) . ? N4 Zn1 2.0312(19) . ? N7 N8 1.389(3) . ? N7 Zn1 2.0970(19) . ? O1 Zn1 1.9178(17) . ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N3 C2 N2 110.8(2) . . ? N3 C2 C1 124.4(2) . . ? N2 C2 C1 124.8(2) . . ? N1 C3 N3 113.0(2) . . ? N1 C3 C4 125.5(2) . . ? N3 C3 C4 121.4(2) . . ? N2 B1 N5 109.37(18) . . ? N2 B1 N8 106.75(18) . . ? N5 B1 N8 109.77(19) . . ? N2 B1 H1 110.3 . . ? N5 B1 H1 110.3 . . ? N8 B1 H1 110.3 . . ? C5 C4 C9 119.8(2) . . ? C5 C4 C3 120.6(2) . . ? C9 C4 C3 119.4(2) . . ? C6 C5 C4 119.6(2) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C7 C6 C5 120.5(2) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C8 C7 C6 120.0(2) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 120.2(2) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C9 C4 119.8(2) . . ? C8 C9 H9 120.1 . . ? C4 C9 H9 120.1 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N6 C11 N5 111.3(2) . . ? N6 C11 C10 124.1(2) . . ? N5 C11 C10 124.5(2) . . ? N4 C12 N6 112.9(2) . . ? N4 C12 C13 123.7(2) . . ? N6 C12 C13 123.4(2) . . ? C14 C13 C18 119.7(2) . . ? C14 C13 C12 120.9(2) . . ? C18 C13 C12 119.4(2) . . ? C15 C14 C13 119.9(2) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 120.2(2) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 119.9(2) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.5(2) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C13 119.8(2) . . ? C17 C18 H18 120.1 . . ? C13 C18 H18 120.1 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N9 C20 N8 111.5(2) . . ? N9 C20 C19 125.1(2) . . ? N8 C20 C19 123.4(2) . . ? N7 C21 N9 112.9(2) . . ? N7 C21 C22 124.3(2) . . ? N9 C21 C22 122.8(2) . . ? C23 C22 C27 118.9(2) . . ? C23 C22 C21 121.5(2) . . ? C27 C22 C21 119.5(2) . . ? C24 C23 C22 120.4(2) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 120.3(2) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 119.5(2) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 120.4(2) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C22 120.3(2) . . ? C26 C27 H27 119.8 . . ? C22 C27 H27 119.8 . . ? O2 C28 O1 121.8(2) . . ? O2 C28 C29 121.9(2) . . ? O1 C28 C29 116.3(2) . . ? O2 C28 Zn1 76.27(15) . . ? O1 C28 Zn1 45.83(11) . . ? C29 C28 Zn1 161.1(2) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C3 N1 N2 103.93(18) . . ? C3 N1 Zn1 143.80(16) . . ? N2 N1 Zn1 111.98(14) . . ? C2 N2 N1 108.16(18) . . ? C2 N2 B1 130.29(19) . . ? N1 N2 B1 121.38(18) . . ? C2 N3 C3 104.09(19) . . ? C12 N4 N5 104.65(18) . . ? C12 N4 Zn1 140.44(16) . . ? N5 N4 Zn1 111.94(14) . . ? C11 N5 N4 107.40(18) . . ? C11 N5 B1 132.12(19) . . ? N4 N5 B1 120.41(18) . . ? C11 N6 C12 103.70(19) . . ? C21 N7 N8 104.41(18) . . ? C21 N7 Zn1 144.33(16) . . ? N8 N7 Zn1 110.76(13) . . ? C20 N8 N7 107.23(18) . . ? C20 N8 B1 130.2(2) . . ? N7 N8 B1 121.86(18) . . ? C20 N9 C21 103.91(19) . . ? C28 O1 Zn1 105.04(16) . . ? O1 Zn1 N4 123.64(8) . . ? O1 Zn1 N1 127.69(8) . . ? N4 Zn1 N1 98.04(7) . . ? O1 Zn1 N7 117.59(7) . . ? N4 Zn1 N7 88.18(8) . . ? N1 Zn1 N7 91.18(7) . . ? O1 Zn1 C28 29.13(8) . . ? N4 Zn1 C28 104.74(8) . . ? N1 Zn1 C28 118.31(8) . . ? N7 Zn1 C28 144.86(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C3 C4 C5 -29.9(3) . . . . ? N3 C3 C4 C5 147.3(2) . . . . ? N1 C3 C4 C9 154.2(2) . . . . ? N3 C3 C4 C9 -28.5(3) . . . . ? C9 C4 C5 C6 -0.6(3) . . . . ? C3 C4 C5 C6 -176.4(2) . . . . ? C4 C5 C6 C7 1.1(3) . . . . ? C5 C6 C7 C8 -0.5(4) . . . . ? C6 C7 C8 C9 -0.7(4) . . . . ? C7 C8 C9 C4 1.2(4) . . . . ? C5 C4 C9 C8 -0.5(3) . . . . ? C3 C4 C9 C8 175.3(2) . . . . ? N4 C12 C13 C14 -34.3(3) . . . . ? N6 C12 C13 C14 143.0(2) . . . . ? N4 C12 C13 C18 147.7(2) . . . . ? N6 C12 C13 C18 -34.9(3) . . . . ? C18 C13 C14 C15 -0.9(4) . . . . ? C12 C13 C14 C15 -178.8(2) . . . . ? C13 C14 C15 C16 -0.3(4) . . . . ? C14 C15 C16 C17 0.7(4) . . . . ? C15 C16 C17 C18 0.2(4) . . . . ? C16 C17 C18 C13 -1.4(4) . . . . ? C14 C13 C18 C17 1.7(4) . . . . ? C12 C13 C18 C17 179.7(2) . . . . ? N7 C21 C22 C23 17.9(4) . . . . ? N9 C21 C22 C23 -163.6(2) . . . . ? N7 C21 C22 C27 -160.2(2) . . . . ? N9 C21 C22 C27 18.4(3) . . . . ? C27 C22 C23 C24 1.8(3) . . . . ? C21 C22 C23 C24 -176.3(2) . . . . ? C22 C23 C24 C25 -0.5(4) . . . . ? C23 C24 C25 C26 -0.8(4) . . . . ? C24 C25 C26 C27 0.8(4) . . . . ? C25 C26 C27 C22 0.5(4) . . . . ? C23 C22 C27 C26 -1.8(3) . . . . ? C21 C22 C27 C26 176.3(2) . . . . ? N3 C3 N1 N2 -1.0(2) . . . . ? C4 C3 N1 N2 176.4(2) . . . . ? N3 C3 N1 Zn1 171.56(19) . . . . ? C4 C3 N1 Zn1 -11.0(4) . . . . ? N3 C2 N2 N1 -0.6(3) . . . . ? C1 C2 N2 N1 -178.3(2) . . . . ? N3 C2 N2 B1 -175.9(2) . . . . ? C1 C2 N2 B1 6.4(4) . . . . ? C3 N1 N2 C2 1.0(2) . . . . ? Zn1 N1 N2 C2 -174.31(14) . . . . ? C3 N1 N2 B1 176.77(19) . . . . ? Zn1 N1 N2 B1 1.5(2) . . . . ? N5 B1 N2 C2 -128.8(2) . . . . ? N8 B1 N2 C2 112.5(2) . . . . ? N5 B1 N2 N1 56.4(3) . . . . ? N8 B1 N2 N1 -62.3(3) . . . . ? N2 C2 N3 C3 0.0(3) . . . . ? C1 C2 N3 C3 177.7(2) . . . . ? N1 C3 N3 C2 0.7(3) . . . . ? C4 C3 N3 C2 -176.9(2) . . . . ? N6 C12 N4 N5 -1.5(2) . . . . ? C13 C12 N4 N5 176.1(2) . . . . ? N6 C12 N4 Zn1 155.81(18) . . . . ? C13 C12 N4 Zn1 -26.6(4) . . . . ? N6 C11 N5 N4 -1.6(2) . . . . ? C10 C11 N5 N4 178.1(2) . . . . ? N6 C11 N5 B1 175.5(2) . . . . ? C10 C11 N5 B1 -4.8(4) . . . . ? C12 N4 N5 C11 1.8(2) . . . . ? Zn1 N4 N5 C11 -162.82(14) . . . . ? C12 N4 N5 B1 -175.67(19) . . . . ? Zn1 N4 N5 B1 19.7(2) . . . . ? N2 B1 N5 C11 111.9(3) . . . . ? N8 B1 N5 C11 -131.3(2) . . . . ? N2 B1 N5 N4 -71.3(2) . . . . ? N8 B1 N5 N4 45.5(3) . . . . ? N5 C11 N6 C12 0.7(2) . . . . ? C10 C11 N6 C12 -179.0(2) . . . . ? N4 C12 N6 C11 0.6(2) . . . . ? C13 C12 N6 C11 -177.0(2) . . . . ? N9 C21 N7 N8 1.0(2) . . . . ? C22 C21 N7 N8 179.6(2) . . . . ? N9 C21 N7 Zn1 -169.3(2) . . . . ? C22 C21 N7 Zn1 9.4(4) . . . . ? N9 C20 N8 N7 1.8(3) . . . . ? C19 C20 N8 N7 -176.7(2) . . . . ? N9 C20 N8 B1 172.4(2) . . . . ? C19 C20 N8 B1 -6.2(4) . . . . ? C21 N7 N8 C20 -1.6(2) . . . . ? Zn1 N7 N8 C20 172.29(14) . . . . ? C21 N7 N8 B1 -173.2(2) . . . . ? Zn1 N7 N8 B1 0.8(2) . . . . ? N2 B1 N8 C20 -108.9(3) . . . . ? N5 B1 N8 C20 132.6(2) . . . . ? N2 B1 N8 N7 60.4(3) . . . . ? N5 B1 N8 N7 -58.0(3) . . . . ? N8 C20 N9 C21 -1.2(3) . . . . ? C19 C20 N9 C21 177.3(2) . . . . ? N7 C21 N9 C20 0.1(3) . . . . ? C22 C21 N9 C20 -178.6(2) . . . . ? O2 C28 O1 Zn1 -7.7(3) . . . . ? C29 C28 O1 Zn1 172.4(2) . . . . ? C28 O1 Zn1 N4 -55.51(18) . . . . ? C28 O1 Zn1 N1 81.08(18) . . . . ? C28 O1 Zn1 N7 -163.25(15) . . . . ? C12 N4 Zn1 O1 20.5(3) . . . . ? N5 N4 Zn1 O1 176.74(12) . . . . ? C12 N4 Zn1 N1 -126.2(2) . . . . ? N5 N4 Zn1 N1 30.05(15) . . . . ? C12 N4 Zn1 N7 142.8(2) . . . . ? N5 N4 Zn1 N7 -60.88(14) . . . . ? C12 N4 Zn1 C28 -4.0(3) . . . . ? N5 N4 Zn1 C28 152.23(14) . . . . ? C3 N1 Zn1 O1 2.1(3) . . . . ? N2 N1 Zn1 O1 174.28(12) . . . . ? C3 N1 Zn1 N4 146.8(3) . . . . ? N2 N1 Zn1 N4 -41.01(15) . . . . ? C3 N1 Zn1 N7 -124.9(3) . . . . ? N2 N1 Zn1 N7 47.32(14) . . . . ? C3 N1 Zn1 C28 35.2(3) . . . . ? N2 N1 Zn1 C28 -152.60(13) . . . . ? C21 N7 Zn1 O1 -12.9(3) . . . . ? N8 N7 Zn1 O1 177.24(13) . . . . ? C21 N7 Zn1 N4 -140.4(3) . . . . ? N8 N7 Zn1 N4 49.74(14) . . . . ? C21 N7 Zn1 N1 121.6(3) . . . . ? N8 N7 Zn1 N1 -48.27(14) . . . . ? C21 N7 Zn1 C28 -27.0(3) . . . . ? N8 N7 Zn1 C28 163.13(14) . . . . ? O2 C28 Zn1 O1 173.3(3) . . . . ? C29 C28 Zn1 O1 -21.4(6) . . . . ? O2 C28 Zn1 N4 -51.93(16) . . . . ? O1 C28 Zn1 N4 134.80(16) . . . . ? C29 C28 Zn1 N4 113.4(6) . . . . ? O2 C28 Zn1 N1 55.89(17) . . . . ? O1 C28 Zn1 N1 -117.38(16) . . . . ? C29 C28 Zn1 N1 -138.8(6) . . . . ? O2 C28 Zn1 N7 -160.39(14) . . . . ? O1 C28 Zn1 N7 26.3(2) . . . . ? C29 C28 Zn1 N7 4.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.444 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.083 data_09mz207_0m _database_code_depnum_ccdc_archive 'CCDC 764043' #TrackingRef '- combined cifs' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C33 H29 B N10 O3 Zn), 3(C6 H5 N O3), 2(C7 H8)' _chemical_formula_sum 'C131 H118 B3 N33 O18 Zn3' _chemical_formula_weight 2671.12 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5636(12) _cell_length_b 14.5278(13) _cell_length_c 36.290(3) _cell_angle_alpha 87.8045(14) _cell_angle_beta 79.9926(14) _cell_angle_gamma 64.3664(13) _cell_volume 6343.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2807 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 30.19 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 0.644 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.776 _exptl_absorpt_correction_T_max 0.885 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 74300 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 0.57 _diffrn_reflns_theta_max 30.65 _reflns_number_total 37424 _reflns_number_gt 25643 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4' _computing_data_reduction 'Apex2 v2008.2-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0496P)^2^+4.3119P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 37424 _refine_ls_number_parameters 1713 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B -0.2042(2) 0.14715(18) 0.42850(7) 0.0154(5) Uani 1 1 d . . . H1 H -0.2819 0.1541 0.4353 0.018 Uiso 1 1 calc R . . B2 B 0.5055(2) 0.5288(2) 0.13422(7) 0.0189(5) Uani 1 1 d . . . H2 H 0.5016 0.5538 0.1082 0.023 Uiso 1 1 calc R . . B3 B 0.5417(2) 0.9915(2) 0.26218(8) 0.0209(5) Uani 1 1 d . . . H3 H 0.5457 1.0044 0.2886 0.025 Uiso 1 1 calc R . . C1 C -0.2539(2) -0.0023(2) 0.48833(7) 0.0262(5) Uani 1 1 d . . . H1A H -0.2935 -0.0105 0.4695 0.039 Uiso 1 1 calc R . . H1B H -0.2958 0.0659 0.5006 0.039 Uiso 1 1 calc R . . H1C H -0.2461 -0.0542 0.5071 0.039 Uiso 1 1 calc R . . C2 C -0.14176(19) -0.01425(17) 0.46981(6) 0.0186(4) Uani 1 1 d . . . C3 C 0.03279(19) -0.07311(17) 0.45250(6) 0.0170(4) Uani 1 1 d . . . C4 C 0.15029(19) -0.14669(17) 0.44634(6) 0.0189(4) Uani 1 1 d . . . C5 C 0.1777(2) -0.24751(18) 0.45646(7) 0.0238(5) Uani 1 1 d . . . H5 H 0.1213 -0.2654 0.4689 0.029 Uiso 1 1 calc R . . C6 C 0.2865(2) -0.3216(2) 0.44849(7) 0.0286(6) Uani 1 1 d . . . H6 H 0.3039 -0.3902 0.4550 0.034 Uiso 1 1 calc R . . C7 C 0.3699(2) -0.2960(2) 0.43110(7) 0.0280(6) Uani 1 1 d . . . H7 H 0.4444 -0.3469 0.4256 0.034 Uiso 1 1 calc R . . C8 C 0.3441(2) -0.1962(2) 0.42172(8) 0.0298(6) Uani 1 1 d . . . H8 H 0.4016 -0.1784 0.4102 0.036 Uiso 1 1 calc R . . C9 C 0.2352(2) -0.12155(19) 0.42892(7) 0.0251(5) Uani 1 1 d . . . H9 H 0.2184 -0.0533 0.4220 0.030 Uiso 1 1 calc R . . C10 C -0.32331(19) 0.11876(19) 0.36365(7) 0.0217(5) Uani 1 1 d . . . H10A H -0.3822 0.1854 0.3734 0.033 Uiso 1 1 calc R . . H10B H -0.3225 0.0666 0.3817 0.033 Uiso 1 1 calc R . . H10C H -0.3371 0.1014 0.3398 0.033 Uiso 1 1 calc R . . C11 C -0.21416(19) 0.12322(16) 0.35759(6) 0.0173(4) Uani 1 1 d . . . C12 C -0.06271(18) 0.12607(16) 0.33205(6) 0.0168(4) Uani 1 1 d . . . C13 C 0.02703(19) 0.12707(17) 0.30270(6) 0.0184(4) Uani 1 1 d . . . C14 C 0.0369(2) 0.0922(2) 0.26644(7) 0.0260(5) Uani 1 1 d . . . H14 H -0.0117 0.0652 0.2611 0.031 Uiso 1 1 calc R . . C15 C 0.1174(2) 0.0969(2) 0.23818(7) 0.0317(6) Uani 1 1 d . . . H15 H 0.1238 0.0730 0.2135 0.038 Uiso 1 1 calc R . . C16 C 0.1887(2) 0.1362(2) 0.24565(7) 0.0290(6) Uani 1 1 d . . . H16 H 0.2430 0.1405 0.2261 0.035 Uiso 1 1 calc R . . C17 C 0.1805(2) 0.1691(2) 0.28160(8) 0.0337(6) Uani 1 1 d . . . H17 H 0.2299 0.1953 0.2870 0.040 Uiso 1 1 calc R . . C18 C 0.1003(2) 0.1642(2) 0.31006(7) 0.0298(6) Uani 1 1 d . . . H18 H 0.0956 0.1865 0.3348 0.036 Uiso 1 1 calc R . . C19 C -0.39509(18) 0.36459(18) 0.46455(7) 0.0220(5) Uani 1 1 d . . . H19A H -0.4131 0.3255 0.4851 0.033 Uiso 1 1 calc R . . H19B H -0.4178 0.3510 0.4419 0.033 Uiso 1 1 calc R . . H19C H -0.4346 0.4377 0.4715 0.033 Uiso 1 1 calc R . . C20 C -0.27345(18) 0.33359(16) 0.45721(6) 0.0156(4) Uani 1 1 d . . . C21 C -0.11542(17) 0.33362(16) 0.45471(6) 0.0142(4) Uani 1 1 d . . . C22 C -0.02895(18) 0.36525(16) 0.45903(6) 0.0152(4) Uani 1 1 d . . . C23 C -0.03934(18) 0.46232(17) 0.44849(6) 0.0176(4) Uani 1 1 d . . . H23 H -0.1024 0.5080 0.4385 0.021 Uiso 1 1 calc R . . C24 C 0.0427(2) 0.49127(19) 0.45272(6) 0.0227(5) Uani 1 1 d . . . H24 H 0.0359 0.5571 0.4456 0.027 Uiso 1 1 calc R . . C25 C 0.1348(2) 0.42499(19) 0.46727(6) 0.0225(5) Uani 1 1 d . . . H25 H 0.1916 0.4450 0.4697 0.027 Uiso 1 1 calc R . . C26 C 0.14448(19) 0.32926(19) 0.47833(6) 0.0213(5) Uani 1 1 d . . . H26 H 0.2070 0.2845 0.4888 0.026 Uiso 1 1 calc R . . C27 C 0.06297(18) 0.29900(17) 0.47408(6) 0.0184(4) Uani 1 1 d . . . H27 H 0.0699 0.2333 0.4814 0.022 Uiso 1 1 calc R . . C28 C 0.22057(18) 0.16711(16) 0.39371(6) 0.0164(4) Uani 1 1 d . . . C29 C 0.16580(18) 0.26931(17) 0.38378(6) 0.0172(4) Uani 1 1 d . . . H29 H 0.0938 0.2937 0.3775 0.021 Uiso 1 1 calc R . . C30 C 0.21608(18) 0.33411(17) 0.38308(6) 0.0171(4) Uani 1 1 d . . . H30 H 0.1789 0.4031 0.3765 0.020 Uiso 1 1 calc R . . C31 C 0.32173(18) 0.29752(16) 0.39213(6) 0.0151(4) Uani 1 1 d . . . C32 C 0.37900(18) 0.19643(17) 0.40113(6) 0.0169(4) Uani 1 1 d . . . H32 H 0.4515 0.1724 0.4069 0.020 Uiso 1 1 calc R . . C33 C 0.32895(18) 0.13197(17) 0.40152(6) 0.0184(4) Uani 1 1 d . . . H33 H 0.3681 0.0624 0.4071 0.022 Uiso 1 1 calc R . . C34 C 0.2816(2) 0.6016(2) 0.10209(7) 0.0282(5) Uani 1 1 d . . . H34A H 0.3225 0.6425 0.0941 0.042 Uiso 1 1 calc R . . H34B H 0.2026 0.6426 0.1013 0.042 Uiso 1 1 calc R . . H34C H 0.3106 0.5410 0.0853 0.042 Uiso 1 1 calc R . . C35 C 0.2953(2) 0.56940(17) 0.14109(6) 0.0205(5) Uani 1 1 d . . . C36 C 0.26679(19) 0.53024(17) 0.19725(6) 0.0197(5) Uani 1 1 d . . . C37 C 0.21011(19) 0.51188(17) 0.23312(7) 0.0207(5) Uani 1 1 d . . . C38 C 0.1177(2) 0.4928(2) 0.23349(7) 0.0276(5) Uani 1 1 d . . . H38 H 0.0911 0.4938 0.2109 0.033 Uiso 1 1 calc R . . C39 C 0.0642(2) 0.4725(2) 0.26683(8) 0.0353(6) Uani 1 1 d . . . H39 H 0.0019 0.4586 0.2669 0.042 Uiso 1 1 calc R . . C40 C 0.1014(2) 0.4725(2) 0.30001(8) 0.0359(7) Uani 1 1 d . . . H40 H 0.0648 0.4585 0.3228 0.043 Uiso 1 1 calc R . . C41 C 0.1922(2) 0.4930(2) 0.29989(7) 0.0318(6) Uani 1 1 d . . . H41 H 0.2175 0.4935 0.3227 0.038 Uiso 1 1 calc R . . C42 C 0.2463(2) 0.5126(2) 0.26661(7) 0.0258(5) Uani 1 1 d . . . H42 H 0.3085 0.5267 0.2667 0.031 Uiso 1 1 calc R . . C43 C 0.6377(2) 0.3726(2) 0.06404(7) 0.0285(6) Uani 1 1 d . . . H43A H 0.6949 0.3151 0.0479 0.043 Uiso 1 1 calc R . . H43B H 0.6502 0.4338 0.0588 0.043 Uiso 1 1 calc R . . H43C H 0.5643 0.3853 0.0590 0.043 Uiso 1 1 calc R . . C44 C 0.6435(2) 0.34773(18) 0.10401(6) 0.0211(5) Uani 1 1 d . . . C45 C 0.68093(19) 0.26619(17) 0.15360(6) 0.0187(4) Uani 1 1 d . . . C46 C 0.73321(19) 0.18216(17) 0.17784(6) 0.0196(4) Uani 1 1 d . . . C47 C 0.8092(2) 0.08677(19) 0.16139(7) 0.0274(5) Uani 1 1 d . . . H47 H 0.8200 0.0752 0.1351 0.033 Uiso 1 1 calc R . . C48 C 0.8688(2) 0.00889(19) 0.18320(8) 0.0300(6) Uani 1 1 d . . . H48 H 0.9210 -0.0556 0.1718 0.036 Uiso 1 1 calc R . . C49 C 0.8523(2) 0.02515(19) 0.22142(8) 0.0277(5) Uani 1 1 d . . . H49 H 0.8947 -0.0275 0.2363 0.033 Uiso 1 1 calc R . . C50 C 0.7743(2) 0.1178(2) 0.23813(7) 0.0292(6) Uani 1 1 d . . . H50 H 0.7619 0.1282 0.2645 0.035 Uiso 1 1 calc R . . C51 C 0.7139(2) 0.19596(18) 0.21644(7) 0.0238(5) Uani 1 1 d . . . H51 H 0.6591 0.2590 0.2281 0.029 Uiso 1 1 calc R . . C52 C 0.5862(2) 0.7011(2) 0.10782(7) 0.0286(6) Uani 1 1 d . . . H52A H 0.6279 0.6435 0.0896 0.043 Uiso 1 1 calc R . . H52B H 0.6235 0.7462 0.1060 0.043 Uiso 1 1 calc R . . H52C H 0.5107 0.7394 0.1025 0.043 Uiso 1 1 calc R . . C53 C 0.5808(2) 0.66217(18) 0.14627(7) 0.0226(5) Uani 1 1 d . . . C54 C 0.59110(19) 0.63808(17) 0.20361(6) 0.0196(4) Uani 1 1 d . . . C55 C 0.6141(2) 0.64593(17) 0.24117(6) 0.0203(5) Uani 1 1 d . . . C56 C 0.7120(2) 0.65208(18) 0.24458(7) 0.0238(5) Uani 1 1 d . . . H56 H 0.7610 0.6544 0.2228 0.029 Uiso 1 1 calc R . . C57 C 0.7379(2) 0.65488(19) 0.27956(8) 0.0303(6) Uani 1 1 d . . . H57 H 0.8054 0.6576 0.2817 0.036 Uiso 1 1 calc R . . C58 C 0.6657(2) 0.65377(19) 0.31142(7) 0.0315(6) Uani 1 1 d . . . H58 H 0.6838 0.6555 0.3354 0.038 Uiso 1 1 calc R . . C59 C 0.5664(2) 0.65011(19) 0.30839(7) 0.0291(6) Uani 1 1 d . . . H59 H 0.5161 0.6511 0.3303 0.035 Uiso 1 1 calc R . . C60 C 0.5412(2) 0.64497(18) 0.27339(7) 0.0236(5) Uani 1 1 d . . . H60 H 0.4744 0.6408 0.2713 0.028 Uiso 1 1 calc R . . C61 C 0.59570(19) 0.40816(17) 0.28236(6) 0.0177(4) Uani 1 1 d . . . C62 C 0.70294(19) 0.39595(18) 0.26656(6) 0.0195(4) Uani 1 1 d . . . H62 H 0.7241 0.3920 0.2401 0.023 Uiso 1 1 calc R . . C63 C 0.7780(2) 0.38965(17) 0.28888(7) 0.0207(5) Uani 1 1 d . . . H63 H 0.8503 0.3814 0.2779 0.025 Uiso 1 1 calc R . . C64 C 0.7469(2) 0.39551(17) 0.32748(6) 0.0193(4) Uani 1 1 d . . . C65 C 0.6425(2) 0.40409(18) 0.34410(6) 0.0214(5) Uani 1 1 d . . . H65 H 0.6228 0.4062 0.3706 0.026 Uiso 1 1 calc R . . C66 C 0.5684(2) 0.40944(18) 0.32165(6) 0.0206(5) Uani 1 1 d . . . H66 H 0.4976 0.4141 0.3329 0.025 Uiso 1 1 calc R . . C67 C 0.7736(2) 0.8777(2) 0.29159(7) 0.0302(6) Uani 1 1 d . . . H67A H 0.7686 0.9460 0.2957 0.045 Uiso 1 1 calc R . . H67B H 0.8473 0.8260 0.2948 0.045 Uiso 1 1 calc R . . H67C H 0.7167 0.8679 0.3097 0.045 Uiso 1 1 calc R . . C68 C 0.7560(2) 0.86735(18) 0.25285(7) 0.0248(5) Uani 1 1 d . . . C69 C 0.7816(2) 0.82571(17) 0.19569(7) 0.0216(5) Uani 1 1 d . . . C70 C 0.8379(2) 0.77743(19) 0.15838(7) 0.0241(5) Uani 1 1 d . . . C71 C 0.9390(2) 0.6902(2) 0.15491(8) 0.0306(6) Uani 1 1 d . . . H71 H 0.9714 0.6639 0.1765 0.037 Uiso 1 1 calc R . . C72 C 0.9923(2) 0.6420(2) 0.12004(9) 0.0383(7) Uani 1 1 d . . . H72 H 1.0607 0.5823 0.1179 0.046 Uiso 1 1 calc R . . C73 C 0.9467(3) 0.6802(2) 0.08855(9) 0.0405(7) Uani 1 1 d . . . H73 H 0.9832 0.6463 0.0648 0.049 Uiso 1 1 calc R . . C74 C 0.8481(2) 0.7677(3) 0.09138(8) 0.0385(7) Uani 1 1 d . . . H74 H 0.8176 0.7946 0.0695 0.046 Uiso 1 1 calc R . . C75 C 0.7933(2) 0.8166(2) 0.12616(8) 0.0321(6) Uani 1 1 d . . . H75 H 0.7254 0.8767 0.1280 0.039 Uiso 1 1 calc R . . C76 C 0.3971(2) 0.9332(2) 0.33013(7) 0.0286(6) Uani 1 1 d . . . H76A H 0.4732 0.8998 0.3352 0.043 Uiso 1 1 calc R . . H76B H 0.3523 0.9025 0.3450 0.043 Uiso 1 1 calc R . . H76C H 0.3650 1.0062 0.3369 0.043 Uiso 1 1 calc R . . C77 C 0.3983(2) 0.91952(17) 0.28970(7) 0.0222(5) Uani 1 1 d . . . C78 C 0.3622(2) 0.88303(17) 0.23878(7) 0.0206(5) Uani 1 1 d . . . C79 C 0.3073(2) 0.85194(17) 0.21343(7) 0.0227(5) Uani 1 1 d . . . C80 C 0.2231(2) 0.8232(2) 0.22875(8) 0.0314(6) Uani 1 1 d . . . H80 H 0.2063 0.8185 0.2551 0.038 Uiso 1 1 calc R . . C81 C 0.1641(2) 0.8015(2) 0.20551(8) 0.0342(6) Uani 1 1 d . . . H81 H 0.1078 0.7810 0.2160 0.041 Uiso 1 1 calc R . . C82 C 0.1868(2) 0.8096(2) 0.16723(8) 0.0327(6) Uani 1 1 d . . . H82 H 0.1443 0.7971 0.1515 0.039 Uiso 1 1 calc R . . C83 C 0.2719(2) 0.8359(2) 0.15165(8) 0.0304(6) Uani 1 1 d . . . H83 H 0.2885 0.8403 0.1253 0.036 Uiso 1 1 calc R . . C84 C 0.3324(2) 0.85580(19) 0.17482(7) 0.0259(5) Uani 1 1 d . . . H84 H 0.3916 0.8722 0.1641 0.031 Uiso 1 1 calc R . . C85 C 0.4554(2) 1.22629(19) 0.29178(7) 0.0290(6) Uani 1 1 d . . . H85A H 0.5304 1.2086 0.2965 0.043 Uiso 1 1 calc R . . H85B H 0.4201 1.1927 0.3097 0.043 Uiso 1 1 calc R . . H85C H 0.4113 1.3005 0.2946 0.043 Uiso 1 1 calc R . . C86 C 0.4623(2) 1.19152(18) 0.25307(7) 0.0220(5) Uani 1 1 d . . . C87 C 0.4537(2) 1.18975(18) 0.19544(6) 0.0208(5) Uani 1 1 d . . . C88 C 0.4337(2) 1.22271(17) 0.15759(7) 0.0217(5) Uani 1 1 d . . . C89 C 0.3325(2) 1.30372(19) 0.15357(7) 0.0280(5) Uani 1 1 d . . . H89 H 0.2790 1.3380 0.1750 0.034 Uiso 1 1 calc R . . C90 C 0.3107(3) 1.3339(2) 0.11792(8) 0.0349(7) Uani 1 1 d . . . H90 H 0.2420 1.3889 0.1150 0.042 Uiso 1 1 calc R . . C91 C 0.3893(3) 1.2837(2) 0.08660(7) 0.0338(6) Uani 1 1 d . . . H91 H 0.3739 1.3042 0.0623 0.041 Uiso 1 1 calc R . . C92 C 0.4896(3) 1.2041(2) 0.09071(7) 0.0317(6) Uani 1 1 d . . . H92 H 0.5434 1.1706 0.0692 0.038 Uiso 1 1 calc R . . C93 C 0.5121(2) 1.17291(19) 0.12611(7) 0.0249(5) Uani 1 1 d . . . H93 H 0.5809 1.1177 0.1289 0.030 Uiso 1 1 calc R . . C94 C 0.4515(2) 0.98520(18) 0.11116(7) 0.0227(5) Uani 1 1 d . . . C95 C 0.3430(2) 1.05663(19) 0.12510(7) 0.0263(5) Uani 1 1 d . . . H95 H 0.3210 1.0732 0.1512 0.032 Uiso 1 1 calc R . . C96 C 0.2673(2) 1.1034(2) 0.10144(8) 0.0330(6) Uani 1 1 d . . . H96 H 0.1938 1.1519 0.1111 0.040 Uiso 1 1 calc R . . C97 C 0.3001(3) 1.0785(2) 0.06343(8) 0.0366(7) Uani 1 1 d . . . C98 C 0.4064(3) 1.0083(2) 0.04867(8) 0.0355(7) Uani 1 1 d . . . H98 H 0.4272 0.9919 0.0225 0.043 Uiso 1 1 calc R . . C99 C 0.4819(2) 0.9624(2) 0.07228(7) 0.0296(6) Uani 1 1 d . . . H99 H 0.5554 0.9148 0.0622 0.036 Uiso 1 1 calc R . . C100 C 0.63054(18) 0.65540(17) 0.48052(7) 0.0182(4) Uani 1 1 d . . . C101 C 0.58040(19) 0.75047(18) 0.49969(7) 0.0202(5) Uani 1 1 d . . . H101 H 0.5581 0.7547 0.5261 0.024 Uiso 1 1 calc R . . C102 C 0.56299(18) 0.83872(17) 0.48027(7) 0.0199(5) Uani 1 1 d . . . H102 H 0.5300 0.9035 0.4932 0.024 Uiso 1 1 calc R . . C103 C 0.59450(18) 0.83065(17) 0.44180(7) 0.0199(5) Uani 1 1 d . . . C104 C 0.64328(19) 0.73720(18) 0.42210(7) 0.0219(5) Uani 1 1 d . . . H104 H 0.6641 0.7336 0.3956 0.026 Uiso 1 1 calc R . . C105 C 0.66109(19) 0.64933(18) 0.44161(7) 0.0207(5) Uani 1 1 d . . . H105 H 0.6941 0.5848 0.4285 0.025 Uiso 1 1 calc R . . C106 C -0.1108(2) 1.03494(19) 0.05506(7) 0.0254(5) Uani 1 1 d . . . C107 C -0.0820(2) 0.9470(2) 0.03317(7) 0.0286(6) Uani 1 1 d . . . H107 H -0.1365 0.9393 0.0220 0.034 Uiso 1 1 calc R . . C108 C 0.0252(2) 0.87149(19) 0.02772(7) 0.0283(6) Uani 1 1 d . . . H108 H 0.0454 0.8118 0.0127 0.034 Uiso 1 1 calc R . . C109 C 0.1036(2) 0.88394(19) 0.04444(7) 0.0259(5) Uani 1 1 d . . . C110 C 0.0776(2) 0.97137(19) 0.06560(7) 0.0269(5) Uani 1 1 d . . . H110 H 0.1327 0.9790 0.0764 0.032 Uiso 1 1 calc R . . C111 C -0.0301(2) 1.0472(2) 0.07064(7) 0.0275(5) Uani 1 1 d . . . H111 H -0.0492 1.1080 0.0848 0.033 Uiso 1 1 calc R . . C112 C 0.1998(2) 0.76128(18) 0.33970(7) 0.0230(5) Uani 1 1 d . . . C113 C 0.1911(2) 0.68438(19) 0.36195(7) 0.0285(6) Uani 1 1 d . . . H113 H 0.2552 0.6222 0.3630 0.034 Uiso 1 1 calc R . . C114 C 0.0907(2) 0.69752(19) 0.38250(7) 0.0286(6) Uani 1 1 d . . . H114 H 0.0848 0.6447 0.3976 0.034 Uiso 1 1 calc R . . C115 C -0.0024(2) 0.78910(19) 0.38090(7) 0.0235(5) Uani 1 1 d . . . C116 C 0.0046(2) 0.86662(18) 0.35904(7) 0.0255(5) Uani 1 1 d . . . H116 H -0.0596 0.9288 0.3582 0.031 Uiso 1 1 calc R . . C117 C 0.1056(2) 0.85293(18) 0.33849(7) 0.0263(5) Uani 1 1 d . . . H117 H 0.1112 0.9060 0.3234 0.032 Uiso 1 1 calc R . . C118 C 0.1311(3) 0.4010(3) 0.01253(14) 0.0743(13) Uani 1 1 d . . . H11A H 0.1210 0.3613 0.0341 0.111 Uiso 1 1 calc R . . H11B H 0.1142 0.3771 -0.0094 0.111 Uiso 1 1 calc R . . H11C H 0.0809 0.4735 0.0180 0.111 Uiso 1 1 calc R . . C119 C 0.2485(3) 0.3875(3) 0.00469(9) 0.0415(7) Uani 1 1 d . . . C120 C 0.3360(3) 0.2956(2) -0.00976(8) 0.0384(7) Uani 1 1 d . . . H120 H 0.3208 0.2403 -0.0155 0.046 Uiso 1 1 calc R . . C121 C 0.4447(3) 0.2830(2) -0.01596(7) 0.0343(6) Uani 1 1 d . . . H121 H 0.5036 0.2194 -0.0256 0.041 Uiso 1 1 calc R . . C122 C 0.4669(2) 0.3636(2) -0.00798(7) 0.0318(6) Uani 1 1 d . . . H122 H 0.5412 0.3560 -0.0123 0.038 Uiso 1 1 calc R . . C123 C 0.3804(3) 0.4553(2) 0.00634(7) 0.0328(6) Uani 1 1 d . . . H123 H 0.3959 0.5105 0.0120 0.039 Uiso 1 1 calc R . . C124 C 0.2725(3) 0.4678(2) 0.01252(8) 0.0380(7) Uani 1 1 d . . . H124 H 0.2140 0.5315 0.0222 0.046 Uiso 1 1 calc R . . C173 C 0.9340(3) 0.3005(3) 0.12785(15) 0.0706(13) Uani 1 1 d . . . H173 H 0.9452 0.2570 0.1071 0.085 Uiso 1 1 calc R . . C174 C 0.9038(3) 0.4238(3) 0.18810(11) 0.0572(10) Uani 1 1 d . . . H174 H 0.8939 0.4667 0.2088 0.069 Uiso 1 1 calc R . . C176 C 0.9622(3) 0.2584(3) 0.16130(15) 0.0725(13) Uani 1 1 d . . . H176 H 0.9920 0.1864 0.1635 0.087 Uiso 1 1 calc R . . C177 C 0.9479(3) 0.3190(3) 0.19118(13) 0.0676(12) Uani 1 1 d . . . H177 H 0.9681 0.2895 0.2141 0.081 Uiso 1 1 calc R . . C180 C 0.8895(3) 0.4053(3) 0.12390(11) 0.0471(8) Uani 1 1 d . . . C181 C 0.8741(3) 0.4656(2) 0.15465(10) 0.0478(8) Uani 1 1 d . . . H181 H 0.8423 0.5378 0.1528 0.057 Uiso 1 1 calc R . . C182 C 0.8584(4) 0.4509(4) 0.08749(12) 0.0722(12) Uani 1 1 d . . . H18A H 0.7798 0.4690 0.0877 0.108 Uiso 1 1 calc R . . H18B H 0.9040 0.4012 0.0668 0.108 Uiso 1 1 calc R . . H18C H 0.8711 0.5125 0.0841 0.108 Uiso 1 1 calc R . . N1 N -0.00883(15) 0.01481(14) 0.43525(5) 0.0160(4) Uani 1 1 d . . . N2 N -0.12296(15) 0.05192(14) 0.44632(5) 0.0162(4) Uani 1 1 d . . . N3 N -0.04701(16) -0.09318(15) 0.47437(5) 0.0213(4) Uani 1 1 d . . . N4 N -0.06747(15) 0.13775(14) 0.36875(5) 0.0170(4) Uani 1 1 d . . . N5 N -0.16669(15) 0.13640(14) 0.38528(5) 0.0158(4) Uani 1 1 d . . . N6 N -0.15202(16) 0.11649(14) 0.32415(5) 0.0182(4) Uani 1 1 d . . . N7 N -0.09383(15) 0.24255(14) 0.44092(5) 0.0157(4) Uani 1 1 d . . . N8 N -0.19652(15) 0.24253(14) 0.44280(5) 0.0158(4) Uani 1 1 d . . . N9 N -0.22618(15) 0.39244(14) 0.46517(5) 0.0160(4) Uani 1 1 d . . . N10 N 0.37069(16) 0.36765(15) 0.39399(5) 0.0192(4) Uani 1 1 d . . . N11 N 0.37277(16) 0.51488(14) 0.19085(5) 0.0185(4) Uani 1 1 d . . . N12 N 0.39040(17) 0.54141(14) 0.15411(5) 0.0200(4) Uani 1 1 d . . . N13 N 0.21620(17) 0.56374(15) 0.16718(5) 0.0219(4) Uani 1 1 d . . . N14 N 0.61015(16) 0.36139(14) 0.16551(5) 0.0178(4) Uani 1 1 d . . . N15 N 0.58677(16) 0.41371(15) 0.13300(5) 0.0195(4) Uani 1 1 d . . . N16 N 0.70424(17) 0.25508(15) 0.11555(5) 0.0216(4) Uani 1 1 d . . . N17 N 0.55362(17) 0.57305(15) 0.19404(5) 0.0199(4) Uani 1 1 d . . . N18 N 0.54660(16) 0.58953(14) 0.15662(5) 0.0198(4) Uani 1 1 d . . . N19 N 0.60929(18) 0.69479(15) 0.17490(6) 0.0231(4) Uani 1 1 d . . . N20 N 0.82201(18) 0.39772(16) 0.35082(6) 0.0256(4) Uani 1 1 d . . . N21 N 0.67414(16) 0.88974(15) 0.20406(5) 0.0201(4) Uani 1 1 d . . . N22 N 0.65791(17) 0.91718(15) 0.24126(5) 0.0210(4) Uani 1 1 d . . . N23 N 0.83475(17) 0.80970(15) 0.22534(6) 0.0245(4) Uani 1 1 d . . . N24 N 0.43720(16) 0.91963(14) 0.22834(5) 0.0195(4) Uani 1 1 d . . . N25 N 0.45968(17) 0.94348(14) 0.26152(5) 0.0202(4) Uani 1 1 d . . . N26 N 0.33630(17) 0.88219(15) 0.27655(6) 0.0221(4) Uani 1 1 d . . . N27 N 0.49346(16) 1.09183(15) 0.20415(5) 0.0196(4) Uani 1 1 d . . . N28 N 0.50001(17) 1.09321(14) 0.24165(5) 0.0195(4) Uani 1 1 d . . . N29 N 0.43298(18) 1.25394(15) 0.22490(6) 0.0236(4) Uani 1 1 d . . . N30 N 0.2217(3) 1.1264(2) 0.03814(9) 0.0530(8) Uani 1 1 d . . . N31 N 0.57642(16) 0.92278(15) 0.42106(6) 0.0227(4) Uani 1 1 d . . . N32 N 0.2161(2) 0.80288(17) 0.03975(6) 0.0316(5) Uani 1 1 d . . . N33 N -0.10807(18) 0.80434(18) 0.40352(7) 0.0311(5) Uani 1 1 d . . . O1 O 0.17606(13) 0.10154(12) 0.39574(5) 0.0209(3) Uani 1 1 d . . . O2 O 0.31833(15) 0.45750(13) 0.38629(5) 0.0305(4) Uani 1 1 d . . . O3 O 0.46238(14) 0.33608(13) 0.40339(5) 0.0244(4) Uani 1 1 d . . . O4 O 0.51947(13) 0.41890(13) 0.26219(4) 0.0207(3) Uani 1 1 d . . . O5 O 0.91573(16) 0.38603(17) 0.33580(6) 0.0384(5) Uani 1 1 d . . . O6 O 0.78917(17) 0.41323(16) 0.38478(5) 0.0365(5) Uani 1 1 d . . . O7 O 0.52689(14) 0.93706(13) 0.13240(5) 0.0237(4) Uani 1 1 d . . . O8 O 0.1251(2) 1.1831(2) 0.05132(9) 0.0693(8) Uani 1 1 d . . . O9 O 0.2552(3) 1.1086(2) 0.00417(7) 0.0632(8) Uani 1 1 d . . . O10 O 0.64725(14) 0.57245(12) 0.50104(5) 0.0219(3) Uani 1 1 d D . . H10 H 0.688(2) 0.5175(17) 0.4880(7) 0.033 Uiso 1 1 d D . . O11 O 0.55027(15) 1.00275(13) 0.43892(5) 0.0280(4) Uani 1 1 d . . . O12 O 0.58588(16) 0.91747(14) 0.38686(5) 0.0322(4) Uani 1 1 d . . . O13 O -0.21761(16) 1.10456(15) 0.06006(6) 0.0352(5) Uani 1 1 d D . . H13 H -0.234(3) 1.149(2) 0.0773(8) 0.053 Uiso 1 1 d D . . O14 O 0.28541(17) 0.81658(17) 0.05376(6) 0.0438(5) Uani 1 1 d . . . O15 O 0.23704(18) 0.72306(15) 0.02254(6) 0.0405(5) Uani 1 1 d . . . O16 O 0.30066(15) 0.74214(14) 0.32023(5) 0.0332(4) Uani 1 1 d D . . H16A H 0.303(3) 0.790(2) 0.3055(8) 0.050 Uiso 1 1 d D . . O17 O -0.18938(16) 0.88705(16) 0.40247(6) 0.0385(5) Uani 1 1 d . . . O18 O -0.11295(18) 0.73576(18) 0.42331(7) 0.0519(6) Uani 1 1 d . . . Zn1 Zn 0.02826(2) 0.124604(19) 0.408048(7) 0.01537(6) Uani 1 1 d . . . Zn2 Zn 0.51530(2) 0.45420(2) 0.212376(7) 0.01788(6) Uani 1 1 d . . . Zn3 Zn 0.53109(2) 0.94922(2) 0.182976(7) 0.01910(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 B1 0.0131(11) 0.0166(11) 0.0181(12) 0.0021(9) -0.0039(9) -0.0077(9) B2 0.0228(13) 0.0187(12) 0.0154(12) 0.0038(9) -0.0030(10) -0.0094(10) B3 0.0271(14) 0.0180(12) 0.0187(12) 0.0027(10) -0.0046(10) -0.0106(11) C1 0.0208(12) 0.0329(14) 0.0267(13) 0.0083(10) -0.0014(10) -0.0150(11) C2 0.0195(11) 0.0218(11) 0.0173(11) 0.0020(8) -0.0018(9) -0.0121(9) C3 0.0211(11) 0.0187(10) 0.0142(10) 0.0023(8) -0.0043(8) -0.0110(9) C4 0.0186(11) 0.0206(11) 0.0168(11) 0.0017(8) -0.0046(9) -0.0072(9) C5 0.0258(12) 0.0221(12) 0.0216(12) 0.0059(9) -0.0025(10) -0.0095(10) C6 0.0274(13) 0.0232(12) 0.0287(13) 0.0061(10) -0.0043(11) -0.0055(10) C7 0.0190(12) 0.0304(13) 0.0254(13) 0.0045(10) -0.0046(10) -0.0022(10) C8 0.0195(12) 0.0345(14) 0.0363(15) 0.0093(11) -0.0089(11) -0.0117(11) C9 0.0215(12) 0.0236(12) 0.0329(14) 0.0081(10) -0.0088(10) -0.0112(10) C10 0.0185(11) 0.0265(12) 0.0231(12) 0.0019(9) -0.0062(9) -0.0117(10) C11 0.0184(11) 0.0130(10) 0.0202(11) 0.0025(8) -0.0063(9) -0.0054(8) C12 0.0183(11) 0.0131(10) 0.0186(11) 0.0016(8) -0.0030(8) -0.0065(8) C13 0.0192(11) 0.0168(10) 0.0177(11) 0.0033(8) -0.0024(9) -0.0068(9) C14 0.0265(13) 0.0303(13) 0.0217(12) -0.0005(10) -0.0031(10) -0.0131(11) C15 0.0325(14) 0.0372(15) 0.0193(12) -0.0015(11) 0.0020(10) -0.0116(12) C16 0.0234(13) 0.0284(13) 0.0263(13) 0.0056(10) 0.0049(10) -0.0067(11) C17 0.0303(14) 0.0460(17) 0.0321(15) 0.0012(12) 0.0023(11) -0.0260(13) C18 0.0350(15) 0.0421(15) 0.0209(12) -0.0006(11) -0.0002(11) -0.0263(13) C19 0.0136(10) 0.0226(11) 0.0289(13) -0.0016(9) -0.0020(9) -0.0074(9) C20 0.0144(10) 0.0169(10) 0.0165(10) 0.0032(8) -0.0025(8) -0.0081(8) C21 0.0141(10) 0.0142(10) 0.0152(10) 0.0042(8) -0.0028(8) -0.0073(8) C22 0.0145(10) 0.0166(10) 0.0150(10) -0.0010(8) 0.0002(8) -0.0081(8) C23 0.0163(10) 0.0175(10) 0.0173(11) 0.0003(8) 0.0010(8) -0.0073(9) C24 0.0267(12) 0.0240(12) 0.0203(11) -0.0022(9) 0.0051(9) -0.0167(10) C25 0.0204(11) 0.0332(13) 0.0202(11) -0.0061(9) 0.0024(9) -0.0191(10) C26 0.0142(10) 0.0303(13) 0.0189(11) -0.0025(9) -0.0013(9) -0.0095(10) C27 0.0170(11) 0.0188(11) 0.0178(11) 0.0000(8) -0.0008(8) -0.0071(9) C28 0.0160(10) 0.0176(10) 0.0166(10) -0.0014(8) 0.0023(8) -0.0099(9) C29 0.0128(10) 0.0188(10) 0.0174(10) 0.0008(8) -0.0016(8) -0.0047(8) C30 0.0173(10) 0.0174(10) 0.0149(10) 0.0031(8) -0.0020(8) -0.0065(9) C31 0.0167(10) 0.0162(10) 0.0146(10) 0.0019(8) -0.0006(8) -0.0100(8) C32 0.0108(10) 0.0192(11) 0.0187(11) 0.0008(8) -0.0007(8) -0.0054(8) C33 0.0159(10) 0.0164(10) 0.0222(11) 0.0014(8) -0.0024(9) -0.0068(9) C34 0.0332(14) 0.0313(13) 0.0220(12) 0.0072(10) -0.0115(11) -0.0138(12) C35 0.0251(12) 0.0167(10) 0.0190(11) 0.0014(8) -0.0068(9) -0.0074(9) C36 0.0217(11) 0.0167(10) 0.0205(11) 0.0017(8) -0.0055(9) -0.0075(9) C37 0.0196(11) 0.0188(11) 0.0223(12) 0.0038(9) -0.0038(9) -0.0071(9) C38 0.0253(13) 0.0370(14) 0.0243(13) 0.0068(10) -0.0077(10) -0.0162(11) C39 0.0255(14) 0.0499(18) 0.0384(16) 0.0102(13) -0.0083(12) -0.0231(13) C40 0.0318(15) 0.0521(18) 0.0260(14) 0.0133(12) -0.0015(11) -0.0224(14) C41 0.0317(14) 0.0470(17) 0.0209(13) 0.0061(11) -0.0051(11) -0.0211(13) C42 0.0229(12) 0.0335(14) 0.0241(12) 0.0024(10) -0.0032(10) -0.0155(11) C43 0.0349(14) 0.0284(13) 0.0182(12) 0.0012(10) -0.0035(10) -0.0103(11) C44 0.0241(12) 0.0233(12) 0.0177(11) 0.0006(9) -0.0030(9) -0.0122(10) C45 0.0207(11) 0.0197(11) 0.0176(11) 0.0014(8) -0.0037(9) -0.0105(9) C46 0.0213(11) 0.0180(11) 0.0222(11) 0.0036(9) -0.0064(9) -0.0103(9) C47 0.0287(13) 0.0234(12) 0.0263(13) 0.0024(10) -0.0015(10) -0.0092(11) C48 0.0266(13) 0.0192(12) 0.0380(15) 0.0021(10) -0.0048(11) -0.0045(10) C49 0.0291(13) 0.0219(12) 0.0385(15) 0.0121(10) -0.0181(11) -0.0132(11) C50 0.0426(16) 0.0266(13) 0.0264(13) 0.0077(10) -0.0180(12) -0.0184(12) C51 0.0285(13) 0.0196(11) 0.0248(12) 0.0020(9) -0.0093(10) -0.0100(10) C52 0.0440(16) 0.0255(13) 0.0194(12) 0.0056(10) -0.0025(11) -0.0193(12) C53 0.0281(13) 0.0200(11) 0.0192(11) 0.0037(9) -0.0017(9) -0.0111(10) C54 0.0208(11) 0.0165(10) 0.0200(11) 0.0008(8) -0.0019(9) -0.0073(9) C55 0.0267(12) 0.0147(10) 0.0197(11) 0.0018(8) -0.0049(9) -0.0087(9) C56 0.0290(13) 0.0169(11) 0.0278(13) 0.0023(9) -0.0060(10) -0.0118(10) C57 0.0369(15) 0.0222(12) 0.0355(15) 0.0022(11) -0.0154(12) -0.0130(11) C58 0.0472(17) 0.0215(12) 0.0253(13) 0.0002(10) -0.0162(12) -0.0105(12) C59 0.0393(15) 0.0204(12) 0.0219(12) -0.0021(9) -0.0015(11) -0.0089(11) C60 0.0270(13) 0.0182(11) 0.0245(12) -0.0004(9) -0.0029(10) -0.0095(10) C61 0.0221(11) 0.0166(10) 0.0170(11) 0.0041(8) -0.0054(9) -0.0103(9) C62 0.0235(12) 0.0224(11) 0.0142(10) 0.0025(8) -0.0019(9) -0.0121(10) C63 0.0202(11) 0.0205(11) 0.0226(12) 0.0027(9) -0.0012(9) -0.0109(9) C64 0.0256(12) 0.0179(10) 0.0192(11) 0.0062(8) -0.0094(9) -0.0124(9) C65 0.0309(13) 0.0235(12) 0.0139(10) 0.0052(9) -0.0055(9) -0.0152(10) C66 0.0226(12) 0.0249(12) 0.0169(11) 0.0042(9) -0.0019(9) -0.0135(10) C67 0.0340(14) 0.0256(13) 0.0319(14) 0.0043(10) -0.0154(12) -0.0104(11) C68 0.0300(13) 0.0203(11) 0.0297(13) 0.0074(10) -0.0121(11) -0.0140(10) C69 0.0225(12) 0.0173(11) 0.0280(12) 0.0052(9) -0.0061(10) -0.0111(9) C70 0.0232(12) 0.0234(12) 0.0284(13) 0.0030(10) -0.0022(10) -0.0136(10) C71 0.0268(13) 0.0250(13) 0.0386(15) 0.0026(11) -0.0047(11) -0.0105(11) C72 0.0281(15) 0.0333(15) 0.0472(18) -0.0044(13) 0.0020(13) -0.0101(12) C73 0.0354(16) 0.0467(18) 0.0368(16) -0.0095(13) 0.0085(13) -0.0198(14) C74 0.0309(15) 0.0550(19) 0.0285(15) 0.0023(13) -0.0013(12) -0.0190(14) C75 0.0246(13) 0.0376(15) 0.0295(14) 0.0036(11) -0.0017(11) -0.0104(12) C76 0.0385(15) 0.0283(13) 0.0180(12) 0.0028(10) -0.0017(10) -0.0150(12) C77 0.0284(13) 0.0132(10) 0.0207(11) 0.0014(8) -0.0013(9) -0.0063(9) C78 0.0227(12) 0.0135(10) 0.0226(12) 0.0022(8) -0.0019(9) -0.0059(9) C79 0.0237(12) 0.0157(11) 0.0269(12) 0.0013(9) -0.0025(10) -0.0075(9) C80 0.0330(14) 0.0308(14) 0.0317(14) -0.0022(11) 0.0018(11) -0.0176(12) C81 0.0280(14) 0.0343(15) 0.0446(17) -0.0043(12) -0.0020(12) -0.0186(12) C82 0.0270(14) 0.0265(13) 0.0430(16) -0.0065(11) -0.0114(12) -0.0073(11) C83 0.0338(15) 0.0279(13) 0.0298(14) -0.0003(11) -0.0084(11) -0.0125(12) C84 0.0291(13) 0.0233(12) 0.0270(13) 0.0023(10) -0.0050(10) -0.0129(11) C85 0.0438(16) 0.0216(12) 0.0222(12) 0.0009(10) -0.0095(11) -0.0134(12) C86 0.0246(12) 0.0202(11) 0.0203(11) 0.0009(9) -0.0043(9) -0.0089(10) C87 0.0237(12) 0.0202(11) 0.0204(11) 0.0028(9) -0.0070(9) -0.0103(10) C88 0.0316(13) 0.0179(11) 0.0217(12) 0.0048(9) -0.0112(10) -0.0142(10) C89 0.0377(15) 0.0204(12) 0.0263(13) 0.0020(10) -0.0122(11) -0.0108(11) C90 0.0505(18) 0.0215(12) 0.0353(15) 0.0068(11) -0.0226(13) -0.0129(12) C91 0.0555(19) 0.0341(15) 0.0234(13) 0.0118(11) -0.0166(13) -0.0274(14) C92 0.0467(17) 0.0364(15) 0.0221(13) 0.0051(11) -0.0032(12) -0.0285(14) C93 0.0308(13) 0.0246(12) 0.0250(12) 0.0059(10) -0.0064(10) -0.0171(11) C94 0.0340(14) 0.0206(11) 0.0187(11) 0.0025(9) -0.0053(10) -0.0166(10) C95 0.0341(14) 0.0257(12) 0.0235(12) 0.0026(10) -0.0057(10) -0.0169(11) C96 0.0343(15) 0.0314(14) 0.0436(16) 0.0112(12) -0.0155(12) -0.0213(12) C97 0.0563(19) 0.0400(16) 0.0389(16) 0.0208(13) -0.0313(15) -0.0375(15) C98 0.063(2) 0.0384(16) 0.0213(13) 0.0092(11) -0.0162(13) -0.0343(16) C99 0.0434(16) 0.0302(14) 0.0189(12) 0.0005(10) -0.0030(11) -0.0201(12) C100 0.0110(10) 0.0187(11) 0.0262(12) 0.0000(9) -0.0037(8) -0.0074(8) C101 0.0175(11) 0.0232(11) 0.0214(11) -0.0020(9) -0.0011(9) -0.0108(9) C102 0.0141(10) 0.0176(11) 0.0276(12) -0.0024(9) -0.0034(9) -0.0063(9) C103 0.0147(10) 0.0197(11) 0.0269(12) 0.0032(9) -0.0063(9) -0.0081(9) C104 0.0185(11) 0.0233(12) 0.0231(12) -0.0019(9) -0.0043(9) -0.0079(9) C105 0.0163(11) 0.0181(11) 0.0252(12) -0.0049(9) -0.0031(9) -0.0049(9) C106 0.0297(13) 0.0238(12) 0.0212(12) 0.0009(9) -0.0020(10) -0.0112(11) C107 0.0368(15) 0.0284(13) 0.0233(12) -0.0009(10) -0.0058(11) -0.0162(12) C108 0.0390(15) 0.0222(12) 0.0220(12) -0.0021(10) -0.0016(11) -0.0130(11) C109 0.0284(13) 0.0240(12) 0.0190(12) 0.0019(9) 0.0020(10) -0.0079(10) C110 0.0310(14) 0.0265(13) 0.0248(13) 0.0001(10) -0.0039(10) -0.0142(11) C111 0.0343(14) 0.0244(12) 0.0230(12) -0.0034(10) -0.0007(10) -0.0133(11) C112 0.0248(12) 0.0206(11) 0.0213(12) 0.0028(9) 0.0017(9) -0.0099(10) C113 0.0254(13) 0.0199(12) 0.0329(14) 0.0095(10) -0.0001(11) -0.0056(10) C114 0.0277(13) 0.0225(12) 0.0320(14) 0.0103(10) -0.0008(11) -0.0099(11) C115 0.0197(12) 0.0253(12) 0.0261(12) 0.0007(10) -0.0027(9) -0.0106(10) C116 0.0235(12) 0.0162(11) 0.0304(13) 0.0020(9) -0.0035(10) -0.0032(10) C117 0.0293(13) 0.0164(11) 0.0292(13) 0.0069(9) -0.0009(10) -0.0081(10) C118 0.048(2) 0.066(3) 0.112(4) 0.005(3) -0.025(2) -0.023(2) C119 0.0378(17) 0.054(2) 0.0351(16) 0.0143(14) -0.0118(13) -0.0206(15) C120 0.060(2) 0.0438(17) 0.0256(14) 0.0066(12) -0.0139(13) -0.0332(16) C121 0.0475(18) 0.0365(15) 0.0206(13) 0.0000(11) -0.0033(12) -0.0206(14) C122 0.0372(15) 0.0360(15) 0.0231(13) 0.0017(11) -0.0027(11) -0.0177(13) C123 0.0473(17) 0.0287(14) 0.0246(13) 0.0079(10) -0.0066(12) -0.0188(13) C124 0.0431(17) 0.0312(15) 0.0339(15) 0.0107(12) -0.0099(13) -0.0103(13) C173 0.056(2) 0.041(2) 0.119(4) -0.023(2) -0.015(2) -0.0227(19) C174 0.055(2) 0.0399(19) 0.057(2) -0.0038(16) 0.0085(18) -0.0092(17) C176 0.052(2) 0.0344(19) 0.121(4) 0.001(2) 0.002(3) -0.0156(18) C177 0.051(2) 0.045(2) 0.073(3) 0.0080(19) 0.020(2) -0.0013(18) C180 0.0303(16) 0.0485(19) 0.067(2) -0.0071(17) 0.0003(15) -0.0238(15) C181 0.0400(18) 0.0304(16) 0.065(2) -0.0049(15) 0.0048(16) -0.0124(14) C182 0.059(3) 0.080(3) 0.079(3) -0.012(2) -0.016(2) -0.029(2) N1 0.0123(8) 0.0177(9) 0.0180(9) 0.0000(7) -0.0021(7) -0.0067(7) N2 0.0149(9) 0.0174(9) 0.0181(9) 0.0007(7) -0.0002(7) -0.0097(7) N3 0.0194(10) 0.0237(10) 0.0218(10) 0.0040(8) -0.0025(8) -0.0109(8) N4 0.0153(9) 0.0193(9) 0.0184(9) 0.0020(7) -0.0007(7) -0.0104(8) N5 0.0139(9) 0.0160(9) 0.0189(9) 0.0017(7) -0.0029(7) -0.0077(7) N6 0.0183(9) 0.0183(9) 0.0190(9) 0.0020(7) -0.0056(7) -0.0083(8) N7 0.0121(8) 0.0178(9) 0.0196(9) 0.0018(7) -0.0038(7) -0.0084(7) N8 0.0114(8) 0.0179(9) 0.0198(9) -0.0004(7) -0.0022(7) -0.0080(7) N9 0.0133(9) 0.0163(9) 0.0175(9) 0.0000(7) -0.0018(7) -0.0059(7) N10 0.0198(10) 0.0196(9) 0.0192(9) 0.0016(7) -0.0013(8) -0.0103(8) N11 0.0231(10) 0.0188(9) 0.0138(9) 0.0041(7) -0.0040(7) -0.0094(8) N12 0.0271(10) 0.0185(9) 0.0152(9) 0.0043(7) -0.0064(8) -0.0099(8) N13 0.0243(10) 0.0209(10) 0.0205(10) 0.0031(8) -0.0058(8) -0.0094(8) N14 0.0217(10) 0.0179(9) 0.0151(9) 0.0048(7) -0.0046(7) -0.0096(8) N15 0.0237(10) 0.0216(10) 0.0130(9) 0.0041(7) -0.0044(7) -0.0095(8) N16 0.0240(10) 0.0209(10) 0.0185(10) 0.0005(7) -0.0027(8) -0.0087(8) N17 0.0249(10) 0.0191(9) 0.0164(9) 0.0037(7) -0.0049(8) -0.0100(8) N18 0.0244(10) 0.0185(9) 0.0168(9) 0.0036(7) -0.0037(8) -0.0097(8) N19 0.0298(11) 0.0218(10) 0.0196(10) 0.0018(8) -0.0026(8) -0.0136(9) N20 0.0314(12) 0.0249(11) 0.0271(11) 0.0081(8) -0.0133(9) -0.0158(9) N21 0.0238(10) 0.0192(9) 0.0184(9) 0.0035(7) -0.0053(8) -0.0099(8) N22 0.0254(10) 0.0186(9) 0.0210(10) 0.0029(8) -0.0072(8) -0.0102(8) N23 0.0265(11) 0.0195(10) 0.0299(11) 0.0054(8) -0.0085(9) -0.0112(9) N24 0.0243(10) 0.0184(9) 0.0166(9) 0.0002(7) -0.0047(8) -0.0093(8) N25 0.0249(10) 0.0180(9) 0.0173(9) 0.0021(7) -0.0038(8) -0.0089(8) N26 0.0250(10) 0.0170(9) 0.0219(10) 0.0017(8) -0.0014(8) -0.0079(8) N27 0.0247(10) 0.0203(9) 0.0152(9) 0.0035(7) -0.0052(8) -0.0106(8) N28 0.0253(10) 0.0178(9) 0.0175(9) 0.0028(7) -0.0065(8) -0.0103(8) N29 0.0319(11) 0.0191(10) 0.0210(10) 0.0023(8) -0.0082(9) -0.0110(9) N30 0.078(2) 0.0579(18) 0.062(2) 0.0357(15) -0.0509(18) -0.0542(18) N31 0.0163(9) 0.0222(10) 0.0306(11) 0.0063(8) -0.0098(8) -0.0076(8) N32 0.0341(13) 0.0289(12) 0.0232(11) 0.0009(9) -0.0007(9) -0.0074(10) N33 0.0228(11) 0.0315(12) 0.0371(13) 0.0031(10) -0.0011(9) -0.0118(10) O1 0.0150(8) 0.0178(8) 0.0316(9) -0.0014(7) 0.0004(7) -0.0101(6) O2 0.0299(10) 0.0180(8) 0.0478(12) 0.0120(8) -0.0101(8) -0.0139(8) O3 0.0199(8) 0.0259(9) 0.0324(10) 0.0035(7) -0.0070(7) -0.0139(7) O4 0.0219(8) 0.0280(9) 0.0157(8) 0.0047(6) -0.0046(6) -0.0138(7) O5 0.0296(11) 0.0570(13) 0.0379(11) 0.0056(10) -0.0120(9) -0.0252(10) O6 0.0472(12) 0.0542(13) 0.0218(9) 0.0092(9) -0.0158(9) -0.0315(11) O7 0.0280(9) 0.0224(8) 0.0190(8) 0.0002(6) -0.0048(7) -0.0092(7) O8 0.0587(18) 0.0735(19) 0.096(2) 0.0414(16) -0.0522(17) -0.0360(16) O9 0.105(2) 0.0801(18) 0.0534(16) 0.0387(14) -0.0568(15) -0.0722(18) O10 0.0194(8) 0.0164(8) 0.0271(9) -0.0005(6) 0.0004(7) -0.0067(7) O11 0.0268(9) 0.0178(8) 0.0375(10) 0.0024(7) -0.0098(8) -0.0065(7) O12 0.0372(11) 0.0323(10) 0.0276(10) 0.0073(8) -0.0125(8) -0.0134(9) O13 0.0295(10) 0.0337(11) 0.0356(11) -0.0106(8) -0.0058(8) -0.0065(9) O14 0.0315(11) 0.0473(13) 0.0417(12) -0.0040(10) -0.0064(9) -0.0066(10) O15 0.0462(12) 0.0287(10) 0.0314(11) -0.0057(8) -0.0030(9) -0.0031(9) O16 0.0264(10) 0.0249(9) 0.0374(11) 0.0107(8) 0.0088(8) -0.0070(8) O17 0.0228(10) 0.0366(11) 0.0475(12) -0.0004(9) -0.0011(9) -0.0067(9) O18 0.0330(12) 0.0455(13) 0.0712(16) 0.0218(12) 0.0059(11) -0.0184(10) Zn1 0.01257(12) 0.01561(12) 0.01899(13) 0.00029(9) -0.00154(9) -0.00750(10) Zn2 0.02117(13) 0.01953(13) 0.01367(12) 0.00366(10) -0.00415(10) -0.00933(11) Zn3 0.02195(14) 0.01942(13) 0.01605(13) 0.00125(10) -0.00354(10) -0.00901(11) _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 B1 N8 1.549(3) . ? B1 N2 1.551(3) . ? B1 N5 1.555(3) . ? B1 H1 1.0000 . ? B2 N12 1.538(3) . ? B2 N18 1.544(3) . ? B2 N15 1.552(3) . ? B2 H2 1.0000 . ? B3 N28 1.548(3) . ? B3 N22 1.550(3) . ? B3 N25 1.551(3) . ? B3 H3 1.0000 . ? C1 C2 1.490(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N3 1.333(3) . ? C2 N2 1.338(3) . ? C3 N1 1.334(3) . ? C3 N3 1.358(3) . ? C3 C4 1.467(3) . ? C4 C9 1.397(3) . ? C4 C5 1.397(3) . ? C5 C6 1.385(3) . ? C5 H5 0.9500 . ? C6 C7 1.383(4) . ? C6 H6 0.9500 . ? C7 C8 1.381(4) . ? C7 H7 0.9500 . ? C8 C9 1.389(4) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.488(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N6 1.332(3) . ? C11 N5 1.344(3) . ? C12 N4 1.336(3) . ? C12 N6 1.356(3) . ? C12 C13 1.477(3) . ? C13 C18 1.384(3) . ? C13 C14 1.392(3) . ? C14 C15 1.386(4) . ? C14 H14 0.9500 . ? C15 C16 1.384(4) . ? C15 H15 0.9500 . ? C16 C17 1.376(4) . ? C16 H16 0.9500 . ? C17 C18 1.388(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.486(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 N8 1.335(3) . ? C20 N9 1.335(3) . ? C21 N7 1.323(3) . ? C21 N9 1.359(3) . ? C21 C22 1.465(3) . ? C22 C27 1.392(3) . ? C22 C23 1.400(3) . ? C23 C24 1.382(3) . ? C23 H23 0.9500 . ? C24 C25 1.384(3) . ? C24 H24 0.9500 . ? C25 C26 1.389(3) . ? C25 H25 0.9500 . ? C26 C27 1.387(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 O1 1.324(3) . ? C28 C29 1.409(3) . ? C28 C33 1.409(3) . ? C29 C30 1.378(3) . ? C29 H29 0.9500 . ? C30 C31 1.391(3) . ? C30 H30 0.9500 . ? C31 C32 1.390(3) . ? C31 N10 1.446(3) . ? C32 C33 1.373(3) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.491(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 N13 1.331(3) . ? C35 N12 1.340(3) . ? C36 N11 1.334(3) . ? C36 N13 1.353(3) . ? C36 C37 1.469(3) . ? C37 C42 1.390(3) . ? C37 C38 1.394(3) . ? C38 C39 1.390(4) . ? C38 H38 0.9500 . ? C39 C40 1.384(4) . ? C39 H39 0.9500 . ? C40 C41 1.386(4) . ? C40 H40 0.9500 . ? C41 C42 1.388(4) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.489(3) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 N15 1.332(3) . ? C44 N16 1.335(3) . ? C45 N14 1.332(3) . ? C45 N16 1.361(3) . ? C45 C46 1.467(3) . ? C46 C51 1.386(3) . ? C46 C47 1.397(3) . ? C47 C48 1.387(4) . ? C47 H47 0.9500 . ? C48 C49 1.379(4) . ? C48 H48 0.9500 . ? C49 C50 1.381(4) . ? C49 H49 0.9500 . ? C50 C51 1.390(3) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C53 1.488(3) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 N19 1.337(3) . ? C53 N18 1.343(3) . ? C54 N17 1.332(3) . ? C54 N19 1.359(3) . ? C54 C55 1.469(3) . ? C55 C56 1.395(3) . ? C55 C60 1.399(3) . ? C56 C57 1.381(3) . ? C56 H56 0.9500 . ? C57 C58 1.384(4) . ? C57 H57 0.9500 . ? C58 C59 1.393(4) . ? C58 H58 0.9500 . ? C59 C60 1.385(3) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 O4 1.321(3) . ? C61 C62 1.404(3) . ? C61 C66 1.408(3) . ? C62 C63 1.378(3) . ? C62 H62 0.9500 . ? C63 C64 1.386(3) . ? C63 H63 0.9500 . ? C64 C65 1.392(3) . ? C64 N20 1.445(3) . ? C65 C66 1.375(3) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C68 1.490(3) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 N23 1.326(3) . ? C68 N22 1.345(3) . ? C69 N21 1.333(3) . ? C69 N23 1.355(3) . ? C69 C70 1.469(3) . ? C70 C71 1.397(4) . ? C70 C75 1.398(4) . ? C71 C72 1.388(4) . ? C71 H71 0.9500 . ? C72 C73 1.377(4) . ? C72 H72 0.9500 . ? C73 C74 1.381(4) . ? C73 H73 0.9500 . ? C74 C75 1.391(4) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 C77 1.484(3) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 N26 1.335(3) . ? C77 N25 1.337(3) . ? C78 N24 1.334(3) . ? C78 N26 1.356(3) . ? C78 C79 1.472(3) . ? C79 C84 1.388(3) . ? C79 C80 1.401(4) . ? C80 C81 1.387(4) . ? C80 H80 0.9500 . ? C81 C82 1.382(4) . ? C81 H81 0.9500 . ? C82 C83 1.392(4) . ? C82 H82 0.9500 . ? C83 C84 1.388(4) . ? C83 H83 0.9500 . ? C84 H84 0.9500 . ? C85 C86 1.485(3) . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 N29 1.336(3) . ? C86 N28 1.346(3) . ? C87 N27 1.333(3) . ? C87 N29 1.355(3) . ? C87 C88 1.468(3) . ? C88 C93 1.391(4) . ? C88 C89 1.396(3) . ? C89 C90 1.389(4) . ? C89 H89 0.9500 . ? C90 C91 1.389(4) . ? C90 H90 0.9500 . ? C91 C92 1.381(4) . ? C91 H91 0.9500 . ? C92 C93 1.386(3) . ? C92 H92 0.9500 . ? C93 H93 0.9500 . ? C94 O7 1.320(3) . ? C94 C95 1.400(4) . ? C94 C99 1.409(3) . ? C95 C96 1.383(4) . ? C95 H95 0.9500 . ? C96 C97 1.385(4) . ? C96 H96 0.9500 . ? C97 C98 1.381(5) . ? C97 N30 1.451(4) . ? C98 C99 1.378(4) . ? C98 H98 0.9500 . ? C99 H99 0.9500 . ? C100 O10 1.346(3) . ? C100 C105 1.396(3) . ? C100 C101 1.396(3) . ? C101 C102 1.387(3) . ? C101 H101 0.9500 . ? C102 C103 1.381(3) . ? C102 H102 0.9500 . ? C103 C104 1.387(3) . ? C103 N31 1.456(3) . ? C104 C105 1.383(3) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C106 O13 1.345(3) . ? C106 C111 1.393(4) . ? C106 C107 1.398(3) . ? C107 C108 1.376(4) . ? C107 H107 0.9500 . ? C108 C109 1.389(4) . ? C108 H108 0.9500 . ? C109 C110 1.386(4) . ? C109 N32 1.454(3) . ? C110 C111 1.382(4) . ? C110 H110 0.9500 . ? C111 H111 0.9500 . ? C112 O16 1.341(3) . ? C112 C113 1.388(3) . ? C112 C117 1.397(3) . ? C113 C114 1.371(4) . ? C113 H113 0.9500 . ? C114 C115 1.390(3) . ? C114 H114 0.9500 . ? C115 C116 1.380(3) . ? C115 N33 1.452(3) . ? C116 C117 1.375(4) . ? C116 H116 0.9500 . ? C117 H117 0.9500 . ? C118 C119 1.495(5) . ? C118 H11A 0.9800 . ? C118 H11B 0.9800 . ? C118 H11C 0.9800 . ? C119 C120 1.389(5) . ? C119 C124 1.391(5) . ? C120 C121 1.382(4) . ? C120 H120 0.9500 . ? C121 C122 1.381(4) . ? C121 H121 0.9500 . ? C122 C123 1.382(4) . ? C122 H122 0.9500 . ? C123 C124 1.373(4) . ? C123 H123 0.9500 . ? C124 H124 0.9500 . ? C173 C176 1.377(6) . ? C173 C180 1.386(5) . ? C173 H173 0.9500 . ? C174 C181 1.380(5) . ? C174 C177 1.383(5) . ? C174 H174 0.9500 . ? C176 C177 1.357(6) . ? C176 H176 0.9500 . ? C177 H177 0.9500 . ? C180 C181 1.376(5) . ? C180 C182 1.500(6) . ? C181 H181 0.9500 . ? C182 H18A 0.9800 . ? C182 H18B 0.9800 . ? C182 H18C 0.9800 . ? N1 N2 1.388(2) . ? N1 Zn1 2.0427(19) . ? N4 N5 1.383(2) . ? N4 Zn1 2.0406(19) . ? N7 N8 1.383(2) . ? N7 Zn1 2.0288(18) . ? N10 O3 1.231(2) . ? N10 O2 1.235(2) . ? N11 N12 1.383(3) . ? N11 Zn2 2.0304(19) . ? N14 N15 1.387(2) . ? N14 Zn2 2.0689(19) . ? N17 N18 1.382(3) . ? N17 Zn2 2.0647(19) . ? N20 O6 1.230(3) . ? N20 O5 1.233(3) . ? N21 N22 1.375(3) . ? N21 Zn3 2.028(2) . ? N24 N25 1.384(3) . ? N24 Zn3 2.051(2) . ? N27 N28 1.381(3) . ? N27 Zn3 2.0528(19) . ? N30 O8 1.226(4) . ? N30 O9 1.233(4) . ? N31 O12 1.227(3) . ? N31 O11 1.232(3) . ? N32 O14 1.232(3) . ? N32 O15 1.235(3) . ? N33 O18 1.224(3) . ? N33 O17 1.235(3) . ? O1 Zn1 1.8574(16) . ? O4 Zn2 1.8636(15) . ? O7 Zn3 1.8635(16) . ? O10 H10 0.851(17) . ? O13 H13 0.846(18) . ? O16 H16A 0.869(18) . ? 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 N8 B1 N2 108.21(17) . . ? N8 B1 N5 108.10(18) . . ? N2 B1 N5 108.89(17) . . ? N8 B1 H1 110.5 . . ? N2 B1 H1 110.5 . . ? N5 B1 H1 110.5 . . ? N12 B2 N18 109.55(19) . . ? N12 B2 N15 108.00(18) . . ? N18 B2 N15 109.05(19) . . ? N12 B2 H2 110.1 . . ? N18 B2 H2 110.1 . . ? N15 B2 H2 110.1 . . ? N28 B3 N22 109.23(19) . . ? N28 B3 N25 108.46(19) . . ? N22 B3 N25 108.88(19) . . ? N28 B3 H3 110.1 . . ? N22 B3 H3 110.1 . . ? N25 B3 H3 110.1 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N3 C2 N2 111.3(2) . . ? N3 C2 C1 124.1(2) . . ? N2 C2 C1 124.6(2) . . ? N1 C3 N3 112.7(2) . . ? N1 C3 C4 124.9(2) . . ? N3 C3 C4 122.1(2) . . ? C9 C4 C5 118.6(2) . . ? C9 C4 C3 122.7(2) . . ? C5 C4 C3 118.5(2) . . ? C6 C5 C4 120.7(2) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C7 C6 C5 120.3(2) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C8 C7 C6 119.6(2) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 120.8(2) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C8 C9 C4 120.1(2) . . ? C8 C9 H9 120.0 . . ? C4 C9 H9 120.0 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N6 C11 N5 111.4(2) . . ? N6 C11 C10 124.5(2) . . ? N5 C11 C10 124.1(2) . . ? N4 C12 N6 112.68(19) . . ? N4 C12 C13 124.5(2) . . ? N6 C12 C13 122.7(2) . . ? C18 C13 C14 118.9(2) . . ? C18 C13 C12 121.7(2) . . ? C14 C13 C12 119.4(2) . . ? C15 C14 C13 120.1(2) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 120.5(2) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C17 C16 C15 119.5(2) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 120.2(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C13 C18 C17 120.7(2) . . ? C13 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N8 C20 N9 110.77(18) . . ? N8 C20 C19 124.8(2) . . ? N9 C20 C19 124.4(2) . . ? N7 C21 N9 112.15(18) . . ? N7 C21 C22 123.38(19) . . ? N9 C21 C22 124.45(19) . . ? C27 C22 C23 120.0(2) . . ? C27 C22 C21 119.83(19) . . ? C23 C22 C21 120.14(19) . . ? C24 C23 C22 119.6(2) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 120.4(2) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 120.1(2) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C27 C26 C25 120.1(2) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C22 119.8(2) . . ? C26 C27 H27 120.1 . . ? C22 C27 H27 120.1 . . ? O1 C28 C29 123.5(2) . . ? O1 C28 C33 118.0(2) . . ? C29 C28 C33 118.6(2) . . ? C30 C29 C28 120.4(2) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C31 119.4(2) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C32 C31 C30 121.6(2) . . ? C32 C31 N10 119.26(19) . . ? C30 C31 N10 119.07(19) . . ? C33 C32 C31 118.8(2) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C32 C33 C28 121.2(2) . . ? C32 C33 H33 119.4 . . ? C28 C33 H33 119.4 . . ? C35 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C35 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N13 C35 N12 111.5(2) . . ? N13 C35 C34 124.9(2) . . ? N12 C35 C34 123.7(2) . . ? N11 C36 N13 113.2(2) . . ? N11 C36 C37 123.9(2) . . ? N13 C36 C37 122.9(2) . . ? C42 C37 C38 119.2(2) . . ? C42 C37 C36 121.8(2) . . ? C38 C37 C36 119.0(2) . . ? C39 C38 C37 120.3(2) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C40 C39 C38 120.2(3) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 119.8(2) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C40 C41 C42 120.2(2) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C41 C42 C37 120.3(2) . . ? C41 C42 H42 119.8 . . ? C37 C42 H42 119.8 . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N15 C44 N16 111.0(2) . . ? N15 C44 C43 124.8(2) . . ? N16 C44 C43 124.2(2) . . ? N14 C45 N16 112.34(19) . . ? N14 C45 C46 125.1(2) . . ? N16 C45 C46 122.5(2) . . ? C51 C46 C47 119.0(2) . . ? C51 C46 C45 121.9(2) . . ? C47 C46 C45 119.0(2) . . ? C48 C47 C46 120.4(2) . . ? C48 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C49 C48 C47 119.9(2) . . ? C49 C48 H48 120.1 . . ? C47 C48 H48 120.1 . . ? C48 C49 C50 120.1(2) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C49 C50 C51 120.2(2) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? C46 C51 C50 120.2(2) . . ? C46 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C53 C52 H52A 109.5 . . ? C53 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C53 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N19 C53 N18 111.4(2) . . ? N19 C53 C52 124.5(2) . . ? N18 C53 C52 124.1(2) . . ? N17 C54 N19 113.4(2) . . ? N17 C54 C55 123.6(2) . . ? N19 C54 C55 122.9(2) . . ? C56 C55 C60 119.6(2) . . ? C56 C55 C54 119.1(2) . . ? C60 C55 C54 121.2(2) . . ? C57 C56 C55 120.2(2) . . ? C57 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C56 C57 C58 120.1(3) . . ? C56 C57 H57 119.9 . . ? C58 C57 H57 119.9 . . ? C57 C58 C59 120.2(2) . . ? C57 C58 H58 119.9 . . ? C59 C58 H58 119.9 . . ? C60 C59 C58 119.9(3) . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? C59 C60 C55 119.9(2) . . ? C59 C60 H60 120.1 . . ? C55 C60 H60 120.1 . . ? O4 C61 C62 123.2(2) . . ? O4 C61 C66 118.7(2) . . ? C62 C61 C66 118.1(2) . . ? C63 C62 C61 121.0(2) . . ? C63 C62 H62 119.5 . . ? C61 C62 H62 119.5 . . ? C62 C63 C64 119.4(2) . . ? C62 C63 H63 120.3 . . ? C64 C63 H63 120.3 . . ? C63 C64 C65 121.1(2) . . ? C63 C64 N20 119.3(2) . . ? C65 C64 N20 119.5(2) . . ? C66 C65 C64 119.1(2) . . ? C66 C65 H65 120.4 . . ? C64 C65 H65 120.4 . . ? C65 C66 C61 121.2(2) . . ? C65 C66 H66 119.4 . . ? C61 C66 H66 119.4 . . ? C68 C67 H67A 109.5 . . ? C68 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C68 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N23 C68 N22 111.5(2) . . ? N23 C68 C67 124.6(2) . . ? N22 C68 C67 123.9(2) . . ? N21 C69 N23 112.9(2) . . ? N21 C69 C70 124.2(2) . . ? N23 C69 C70 122.9(2) . . ? C71 C70 C75 119.0(2) . . ? C71 C70 C69 119.2(2) . . ? C75 C70 C69 121.8(2) . . ? C72 C71 C70 120.1(3) . . ? C72 C71 H71 119.9 . . ? C70 C71 H71 119.9 . . ? C73 C72 C71 120.4(3) . . ? C73 C72 H72 119.8 . . ? C71 C72 H72 119.8 . . ? C72 C73 C74 120.2(3) . . ? C72 C73 H73 119.9 . . ? C74 C73 H73 119.9 . . ? C73 C74 C75 120.1(3) . . ? C73 C74 H74 119.9 . . ? C75 C74 H74 119.9 . . ? C74 C75 C70 120.1(3) . . ? C74 C75 H75 119.9 . . ? C70 C75 H75 119.9 . . ? C77 C76 H76A 109.5 . . ? C77 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C77 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N26 C77 N25 110.6(2) . . ? N26 C77 C76 124.0(2) . . ? N25 C77 C76 125.4(2) . . ? N24 C78 N26 112.0(2) . . ? N24 C78 C79 125.7(2) . . ? N26 C78 C79 122.3(2) . . ? C84 C79 C80 119.1(2) . . ? C84 C79 C78 121.8(2) . . ? C80 C79 C78 119.1(2) . . ? C81 C80 C79 120.1(3) . . ? C81 C80 H80 120.0 . . ? C79 C80 H80 120.0 . . ? C82 C81 C80 120.3(3) . . ? C82 C81 H81 119.8 . . ? C80 C81 H81 119.8 . . ? C81 C82 C83 120.1(3) . . ? C81 C82 H82 120.0 . . ? C83 C82 H82 120.0 . . ? C84 C83 C82 119.7(3) . . ? C84 C83 H83 120.2 . . ? C82 C83 H83 120.2 . . ? C83 C84 C79 120.7(3) . . ? C83 C84 H84 119.6 . . ? C79 C84 H84 119.6 . . ? C86 C85 H85A 109.5 . . ? C86 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C86 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? N29 C86 N28 111.2(2) . . ? N29 C86 C85 124.2(2) . . ? N28 C86 C85 124.6(2) . . ? N27 C87 N29 113.2(2) . . ? N27 C87 C88 122.3(2) . . ? N29 C87 C88 124.5(2) . . ? C93 C88 C89 120.1(2) . . ? C93 C88 C87 121.1(2) . . ? C89 C88 C87 118.7(2) . . ? C90 C89 C88 119.5(3) . . ? C90 C89 H89 120.2 . . ? C88 C89 H89 120.2 . . ? C91 C90 C89 120.1(3) . . ? C91 C90 H90 120.0 . . ? C89 C90 H90 120.0 . . ? C92 C91 C90 120.3(2) . . ? C92 C91 H91 119.9 . . ? C90 C91 H91 119.9 . . ? C91 C92 C93 120.2(3) . . ? C91 C92 H92 119.9 . . ? C93 C92 H92 119.9 . . ? C92 C93 C88 119.8(2) . . ? C92 C93 H93 120.1 . . ? C88 C93 H93 120.1 . . ? O7 C94 C95 123.7(2) . . ? O7 C94 C99 118.0(2) . . ? C95 C94 C99 118.2(2) . . ? C96 C95 C94 121.0(2) . . ? C96 C95 H95 119.5 . . ? C94 C95 H95 119.5 . . ? C95 C96 C97 119.0(3) . . ? C95 C96 H96 120.5 . . ? C97 C96 H96 120.5 . . ? C98 C97 C96 121.6(2) . . ? C98 C97 N30 118.5(3) . . ? C96 C97 N30 119.9(3) . . ? C99 C98 C97 119.3(3) . . ? C99 C98 H98 120.4 . . ? C97 C98 H98 120.4 . . ? C98 C99 C94 120.9(3) . . ? C98 C99 H99 119.6 . . ? C94 C99 H99 119.6 . . ? O10 C100 C105 122.7(2) . . ? O10 C100 C101 117.4(2) . . ? C105 C100 C101 119.9(2) . . ? C102 C101 C100 120.2(2) . . ? C102 C101 H101 119.9 . . ? C100 C101 H101 119.9 . . ? C103 C102 C101 118.7(2) . . ? C103 C102 H102 120.6 . . ? C101 C102 H102 120.6 . . ? C102 C103 C104 122.1(2) . . ? C102 C103 N31 119.3(2) . . ? C104 C103 N31 118.6(2) . . ? C105 C104 C103 119.0(2) . . ? C105 C104 H104 120.5 . . ? C103 C104 H104 120.5 . . ? C104 C105 C100 120.1(2) . . ? C104 C105 H105 120.0 . . ? C100 C105 H105 120.0 . . ? O13 C106 C111 123.0(2) . . ? O13 C106 C107 117.2(2) . . ? C111 C106 C107 119.8(2) . . ? C108 C107 C106 120.2(2) . . ? C108 C107 H107 119.9 . . ? C106 C107 H107 119.9 . . ? C107 C108 C109 119.0(2) . . ? C107 C108 H108 120.5 . . ? C109 C108 H108 120.5 . . ? C110 C109 C108 121.9(2) . . ? C110 C109 N32 118.9(2) . . ? C108 C109 N32 119.2(2) . . ? C111 C110 C109 118.7(2) . . ? C111 C110 H110 120.7 . . ? C109 C110 H110 120.7 . . ? C110 C111 C106 120.4(2) . . ? C110 C111 H111 119.8 . . ? C106 C111 H111 119.8 . . ? O16 C112 C113 116.8(2) . . ? O16 C112 C117 123.5(2) . . ? C113 C112 C117 119.6(2) . . ? C114 C113 C112 120.5(2) . . ? C114 C113 H113 119.8 . . ? C112 C113 H113 119.8 . . ? C113 C114 C115 119.2(2) . . ? C113 C114 H114 120.4 . . ? C115 C114 H114 120.4 . . ? C116 C115 C114 121.2(2) . . ? C116 C115 N33 119.5(2) . . ? C114 C115 N33 119.2(2) . . ? C117 C116 C115 119.3(2) . . ? C117 C116 H116 120.3 . . ? C115 C116 H116 120.3 . . ? C116 C117 C112 120.2(2) . . ? C116 C117 H117 119.9 . . ? C112 C117 H117 119.9 . . ? C119 C118 H11A 109.5 . . ? C119 C118 H11B 109.5 . . ? H11A C118 H11B 109.5 . . ? C119 C118 H11C 109.5 . . ? H11A C118 H11C 109.5 . . ? H11B C118 H11C 109.5 . . ? C120 C119 C124 118.3(3) . . ? C120 C119 C118 121.9(3) . . ? C124 C119 C118 119.8(3) . . ? C121 C120 C119 121.4(3) . . ? C121 C120 H120 119.3 . . ? C119 C120 H120 119.3 . . ? C122 C121 C120 119.4(3) . . ? C122 C121 H121 120.3 . . ? C120 C121 H121 120.3 . . ? C121 C122 C123 119.6(3) . . ? C121 C122 H122 120.2 . . ? C123 C122 H122 120.2 . . ? C124 C123 C122 121.0(3) . . ? C124 C123 H123 119.5 . . ? C122 C123 H123 119.5 . . ? C123 C124 C119 120.2(3) . . ? C123 C124 H124 119.9 . . ? C119 C124 H124 119.9 . . ? C176 C173 C180 121.2(4) . . ? C176 C173 H173 119.4 . . ? C180 C173 H173 119.4 . . ? C181 C174 C177 119.5(4) . . ? C181 C174 H174 120.2 . . ? C177 C174 H174 120.2 . . ? C177 C176 C173 120.4(4) . . ? C177 C176 H176 119.8 . . ? C173 C176 H176 119.8 . . ? C176 C177 C174 119.7(4) . . ? C176 C177 H177 120.1 . . ? C174 C177 H177 120.1 . . ? C181 C180 C173 117.6(4) . . ? C181 C180 C182 121.4(3) . . ? C173 C180 C182 121.0(4) . . ? C180 C181 C174 121.5(3) . . ? C180 C181 H181 119.2 . . ? C174 C181 H181 119.2 . . ? C180 C182 H18A 109.5 . . ? C180 C182 H18B 109.5 . . ? H18A C182 H18B 109.5 . . ? C180 C182 H18C 109.5 . . ? H18A C182 H18C 109.5 . . ? H18B C182 H18C 109.5 . . ? C3 N1 N2 104.37(18) . . ? C3 N1 Zn1 144.39(16) . . ? N2 N1 Zn1 109.82(13) . . ? C2 N2 N1 107.52(18) . . ? C2 N2 B1 130.95(19) . . ? N1 N2 B1 121.13(17) . . ? C2 N3 C3 104.11(19) . . ? C12 N4 N5 104.70(17) . . ? C12 N4 Zn1 142.67(15) . . ? N5 N4 Zn1 110.58(13) . . ? C11 N5 N4 107.17(18) . . ? C11 N5 B1 131.48(19) . . ? N4 N5 B1 121.34(17) . . ? C11 N6 C12 104.02(18) . . ? C21 N7 N8 105.10(17) . . ? C21 N7 Zn1 140.54(15) . . ? N8 N7 Zn1 112.00(13) . . ? C20 N8 N7 107.53(17) . . ? C20 N8 B1 132.60(18) . . ? N7 N8 B1 119.85(17) . . ? C20 N9 C21 104.44(18) . . ? O3 N10 O2 122.4(2) . . ? O3 N10 C31 119.04(19) . . ? O2 N10 C31 118.55(19) . . ? C36 N11 N12 104.10(18) . . ? C36 N11 Zn2 143.48(16) . . ? N12 N11 Zn2 111.89(14) . . ? C35 N12 N11 107.48(19) . . ? C35 N12 B2 130.76(19) . . ? N11 N12 B2 121.58(18) . . ? C35 N13 C36 103.7(2) . . ? C45 N14 N15 104.53(18) . . ? C45 N14 Zn2 144.29(15) . . ? N15 N14 Zn2 110.89(14) . . ? C44 N15 N14 107.83(19) . . ? C44 N15 B2 130.62(19) . . ? N14 N15 B2 121.54(18) . . ? C44 N16 C45 104.27(19) . . ? C54 N17 N18 104.21(18) . . ? C54 N17 Zn2 144.12(16) . . ? N18 N17 Zn2 111.42(14) . . ? C53 N18 N17 107.59(18) . . ? C53 N18 B2 131.16(19) . . ? N17 N18 B2 121.25(18) . . ? C53 N19 C54 103.38(19) . . ? O6 N20 O5 122.6(2) . . ? O6 N20 C64 118.6(2) . . ? O5 N20 C64 118.7(2) . . ? C69 N21 N22 104.56(18) . . ? C69 N21 Zn3 142.64(17) . . ? N22 N21 Zn3 112.58(14) . . ? C68 N22 N21 107.3(2) . . ? C68 N22 B3 131.8(2) . . ? N21 N22 B3 120.94(19) . . ? C68 N23 C69 103.8(2) . . ? C78 N24 N25 104.84(18) . . ? C78 N24 Zn3 144.06(16) . . ? N25 N24 Zn3 111.07(14) . . ? C77 N25 N24 107.75(19) . . ? C77 N25 B3 130.3(2) . . ? N24 N25 B3 121.92(18) . . ? C77 N26 C78 104.9(2) . . ? C87 N27 N28 104.41(18) . . ? C87 N27 Zn3 141.99(16) . . ? N28 N27 Zn3 113.21(13) . . ? C86 N28 N27 107.47(18) . . ? C86 N28 B3 133.0(2) . . ? N27 N28 B3 119.44(18) . . ? C86 N29 C87 103.7(2) . . ? O8 N30 O9 122.6(3) . . ? O8 N30 C97 118.8(3) . . ? O9 N30 C97 118.5(3) . . ? O12 N31 O11 123.3(2) . . ? O12 N31 C103 118.6(2) . . ? O11 N31 C103 118.1(2) . . ? O14 N32 O15 123.2(2) . . ? O14 N32 C109 118.3(2) . . ? O15 N32 C109 118.5(2) . . ? O18 N33 O17 122.5(2) . . ? O18 N33 C115 119.0(2) . . ? O17 N33 C115 118.5(2) . . ? C28 O1 Zn1 129.81(14) . . ? C61 O4 Zn2 128.60(14) . . ? C94 O7 Zn3 133.73(16) . . ? C100 O10 H10 111(2) . . ? C106 O13 H13 113(2) . . ? C112 O16 H16A 115(2) . . ? O1 Zn1 N7 125.74(7) . . ? O1 Zn1 N4 122.87(7) . . ? N7 Zn1 N4 93.69(7) . . ? O1 Zn1 N1 118.80(7) . . ? N7 Zn1 N1 94.84(7) . . ? N4 Zn1 N1 92.87(7) . . ? O4 Zn2 N11 123.02(7) . . ? O4 Zn2 N17 118.61(7) . . ? N11 Zn2 N17 91.77(8) . . ? O4 Zn2 N14 126.64(7) . . ? N11 Zn2 N14 94.77(7) . . ? N17 Zn2 N14 93.36(8) . . ? O7 Zn3 N21 123.03(8) . . ? O7 Zn3 N24 128.05(8) . . ? N21 Zn3 N24 95.61(8) . . ? O7 Zn3 N27 117.30(7) . . ? N21 Zn3 N27 90.50(8) . . ? N24 Zn3 N27 93.00(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C3 C4 C9 16.5(4) . . . . ? N3 C3 C4 C9 -169.7(2) . . . . ? N1 C3 C4 C5 -159.9(2) . . . . ? N3 C3 C4 C5 13.9(3) . . . . ? C9 C4 C5 C6 -1.7(4) . . . . ? C3 C4 C5 C6 174.8(2) . . . . ? C4 C5 C6 C7 1.4(4) . . . . ? C5 C6 C7 C8 0.0(4) . . . . ? C6 C7 C8 C9 -1.2(4) . . . . ? C7 C8 C9 C4 0.9(4) . . . . ? C5 C4 C9 C8 0.5(4) . . . . ? C3 C4 C9 C8 -175.9(2) . . . . ? N4 C12 C13 C18 -15.7(3) . . . . ? N6 C12 C13 C18 162.0(2) . . . . ? N4 C12 C13 C14 165.9(2) . . . . ? N6 C12 C13 C14 -16.4(3) . . . . ? C18 C13 C14 C15 -1.4(4) . . . . ? C12 C13 C14 C15 177.1(2) . . . . ? C13 C14 C15 C16 0.0(4) . . . . ? C14 C15 C16 C17 1.2(4) . . . . ? C15 C16 C17 C18 -0.9(4) . . . . ? C14 C13 C18 C17 1.6(4) . . . . ? C12 C13 C18 C17 -176.7(2) . . . . ? C16 C17 C18 C13 -0.5(4) . . . . ? N7 C21 C22 C27 -45.0(3) . . . . ? N9 C21 C22 C27 133.2(2) . . . . ? N7 C21 C22 C23 135.8(2) . . . . ? N9 C21 C22 C23 -46.1(3) . . . . ? C27 C22 C23 C24 0.8(3) . . . . ? C21 C22 C23 C24 180.0(2) . . . . ? C22 C23 C24 C25 0.0(3) . . . . ? C23 C24 C25 C26 -1.1(3) . . . . ? C24 C25 C26 C27 1.4(3) . . . . ? C25 C26 C27 C22 -0.6(3) . . . . ? C23 C22 C27 C26 -0.5(3) . . . . ? C21 C22 C27 C26 -179.7(2) . . . . ? O1 C28 C29 C30 178.5(2) . . . . ? C33 C28 C29 C30 -2.3(3) . . . . ? C28 C29 C30 C31 0.2(3) . . . . ? C29 C30 C31 C32 1.4(3) . . . . ? C29 C30 C31 N10 -175.54(19) . . . . ? C30 C31 C32 C33 -0.9(3) . . . . ? N10 C31 C32 C33 176.0(2) . . . . ? C31 C32 C33 C28 -1.3(3) . . . . ? O1 C28 C33 C32 -177.9(2) . . . . ? C29 C28 C33 C32 2.8(3) . . . . ? N11 C36 C37 C42 23.5(4) . . . . ? N13 C36 C37 C42 -157.1(2) . . . . ? N11 C36 C37 C38 -156.2(2) . . . . ? N13 C36 C37 C38 23.1(3) . . . . ? C42 C37 C38 C39 -1.5(4) . . . . ? C36 C37 C38 C39 178.3(2) . . . . ? C37 C38 C39 C40 1.0(4) . . . . ? C38 C39 C40 C41 0.1(5) . . . . ? C39 C40 C41 C42 -0.5(5) . . . . ? C40 C41 C42 C37 -0.1(4) . . . . ? C38 C37 C42 C41 1.1(4) . . . . ? C36 C37 C42 C41 -178.7(2) . . . . ? N14 C45 C46 C51 -1.1(4) . . . . ? N16 C45 C46 C51 176.1(2) . . . . ? N14 C45 C46 C47 -177.7(2) . . . . ? N16 C45 C46 C47 -0.5(3) . . . . ? C51 C46 C47 C48 -3.6(4) . . . . ? C45 C46 C47 C48 173.1(2) . . . . ? C46 C47 C48 C49 0.7(4) . . . . ? C47 C48 C49 C50 1.8(4) . . . . ? C48 C49 C50 C51 -1.5(4) . . . . ? C47 C46 C51 C50 3.9(4) . . . . ? C45 C46 C51 C50 -172.7(2) . . . . ? C49 C50 C51 C46 -1.4(4) . . . . ? N17 C54 C55 C56 135.3(2) . . . . ? N19 C54 C55 C56 -42.7(3) . . . . ? N17 C54 C55 C60 -43.2(3) . . . . ? N19 C54 C55 C60 138.8(2) . . . . ? C60 C55 C56 C57 1.5(3) . . . . ? C54 C55 C56 C57 -177.1(2) . . . . ? C55 C56 C57 C58 -1.4(4) . . . . ? C56 C57 C58 C59 -0.2(4) . . . . ? C57 C58 C59 C60 1.6(4) . . . . ? C58 C59 C60 C55 -1.5(4) . . . . ? C56 C55 C60 C59 0.0(3) . . . . ? C54 C55 C60 C59 178.5(2) . . . . ? O4 C61 C62 C63 177.0(2) . . . . ? C66 C61 C62 C63 -2.7(3) . . . . ? C61 C62 C63 C64 0.0(3) . . . . ? C62 C63 C64 C65 2.2(3) . . . . ? C62 C63 C64 N20 -174.7(2) . . . . ? C63 C64 C65 C66 -1.7(3) . . . . ? N20 C64 C65 C66 175.3(2) . . . . ? C64 C65 C66 C61 -1.1(3) . . . . ? O4 C61 C66 C65 -176.5(2) . . . . ? C62 C61 C66 C65 3.2(3) . . . . ? N21 C69 C70 C71 -160.8(2) . . . . ? N23 C69 C70 C71 19.6(4) . . . . ? N21 C69 C70 C75 19.4(4) . . . . ? N23 C69 C70 C75 -160.2(2) . . . . ? C75 C70 C71 C72 -1.8(4) . . . . ? C69 C70 C71 C72 178.5(2) . . . . ? C70 C71 C72 C73 0.7(4) . . . . ? C71 C72 C73 C74 0.8(5) . . . . ? C72 C73 C74 C75 -1.2(5) . . . . ? C73 C74 C75 C70 0.1(4) . . . . ? C71 C70 C75 C74 1.4(4) . . . . ? C69 C70 C75 C74 -178.9(3) . . . . ? N24 C78 C79 C84 1.8(4) . . . . ? N26 C78 C79 C84 178.2(2) . . . . ? N24 C78 C79 C80 -174.5(2) . . . . ? N26 C78 C79 C80 1.9(3) . . . . ? C84 C79 C80 C81 -1.6(4) . . . . ? C78 C79 C80 C81 174.8(2) . . . . ? C79 C80 C81 C82 -1.0(4) . . . . ? C80 C81 C82 C83 2.4(4) . . . . ? C81 C82 C83 C84 -1.2(4) . . . . ? C82 C83 C84 C79 -1.4(4) . . . . ? C80 C79 C84 C83 2.8(4) . . . . ? C78 C79 C84 C83 -173.5(2) . . . . ? N27 C87 C88 C93 -45.7(3) . . . . ? N29 C87 C88 C93 135.2(3) . . . . ? N27 C87 C88 C89 132.5(3) . . . . ? N29 C87 C88 C89 -46.7(3) . . . . ? C93 C88 C89 C90 0.2(4) . . . . ? C87 C88 C89 C90 -178.0(2) . . . . ? C88 C89 C90 C91 -0.1(4) . . . . ? C89 C90 C91 C92 -0.4(4) . . . . ? C90 C91 C92 C93 0.8(4) . . . . ? C91 C92 C93 C88 -0.7(4) . . . . ? C89 C88 C93 C92 0.2(4) . . . . ? C87 C88 C93 C92 178.3(2) . . . . ? O7 C94 C95 C96 -179.0(2) . . . . ? C99 C94 C95 C96 0.3(4) . . . . ? C94 C95 C96 C97 0.1(4) . . . . ? C95 C96 C97 C98 -0.1(4) . . . . ? C95 C96 C97 N30 179.8(2) . . . . ? C96 C97 C98 C99 -0.4(4) . . . . ? N30 C97 C98 C99 179.7(2) . . . . ? C97 C98 C99 C94 0.8(4) . . . . ? O7 C94 C99 C98 178.5(2) . . . . ? C95 C94 C99 C98 -0.8(4) . . . . ? O10 C100 C101 C102 178.6(2) . . . . ? C105 C100 C101 C102 -1.4(3) . . . . ? C100 C101 C102 C103 1.0(3) . . . . ? C101 C102 C103 C104 -0.3(3) . . . . ? C101 C102 C103 N31 179.8(2) . . . . ? C102 C103 C104 C105 -0.1(3) . . . . ? N31 C103 C104 C105 179.8(2) . . . . ? C103 C104 C105 C100 -0.2(3) . . . . ? O10 C100 C105 C104 -179.0(2) . . . . ? C101 C100 C105 C104 1.0(3) . . . . ? O13 C106 C107 C108 -178.3(2) . . . . ? C111 C106 C107 C108 1.5(4) . . . . ? C106 C107 C108 C109 0.4(4) . . . . ? C107 C108 C109 C110 -1.8(4) . . . . ? C107 C108 C109 N32 178.0(2) . . . . ? C108 C109 C110 C111 1.2(4) . . . . ? N32 C109 C110 C111 -178.6(2) . . . . ? C109 C110 C111 C106 0.8(4) . . . . ? O13 C106 C111 C110 177.7(2) . . . . ? C107 C106 C111 C110 -2.1(4) . . . . ? O16 C112 C113 C114 -179.4(3) . . . . ? C117 C112 C113 C114 0.5(4) . . . . ? C112 C113 C114 C115 -0.3(4) . . . . ? C113 C114 C115 C116 0.1(4) . . . . ? C113 C114 C115 N33 -178.1(2) . . . . ? C114 C115 C116 C117 0.0(4) . . . . ? N33 C115 C116 C117 178.2(2) . . . . ? C115 C116 C117 C112 0.2(4) . . . . ? O16 C112 C117 C116 179.5(2) . . . . ? C113 C112 C117 C116 -0.4(4) . . . . ? C124 C119 C120 C121 0.7(4) . . . . ? C118 C119 C120 C121 -178.2(3) . . . . ? C119 C120 C121 C122 -0.6(4) . . . . ? C120 C121 C122 C123 0.5(4) . . . . ? C121 C122 C123 C124 -0.5(4) . . . . ? C122 C123 C124 C119 0.5(4) . . . . ? C120 C119 C124 C123 -0.6(4) . . . . ? C118 C119 C124 C123 178.3(3) . . . . ? C180 C173 C176 C177 -0.6(6) . . . . ? C173 C176 C177 C174 0.5(6) . . . . ? C181 C174 C177 C176 0.4(6) . . . . ? C176 C173 C180 C181 -0.3(6) . . . . ? C176 C173 C180 C182 -179.7(4) . . . . ? C173 C180 C181 C174 1.3(5) . . . . ? C182 C180 C181 C174 -179.3(3) . . . . ? C177 C174 C181 C180 -1.4(6) . . . . ? N3 C3 N1 N2 -1.3(2) . . . . ? C4 C3 N1 N2 173.0(2) . . . . ? N3 C3 N1 Zn1 162.16(19) . . . . ? C4 C3 N1 Zn1 -23.5(4) . . . . ? N3 C2 N2 N1 -0.9(2) . . . . ? C1 C2 N2 N1 179.6(2) . . . . ? N3 C2 N2 B1 171.7(2) . . . . ? C1 C2 N2 B1 -7.8(4) . . . . ? C3 N1 N2 C2 1.3(2) . . . . ? Zn1 N1 N2 C2 -168.54(14) . . . . ? C3 N1 N2 B1 -172.19(18) . . . . ? Zn1 N1 N2 B1 17.9(2) . . . . ? N8 B1 N2 C2 116.8(2) . . . . ? N5 B1 N2 C2 -125.9(2) . . . . ? N8 B1 N2 N1 -71.4(2) . . . . ? N5 B1 N2 N1 45.9(2) . . . . ? N2 C2 N3 C3 0.1(3) . . . . ? C1 C2 N3 C3 179.6(2) . . . . ? N1 C3 N3 C2 0.8(3) . . . . ? C4 C3 N3 C2 -173.7(2) . . . . ? N6 C12 N4 N5 -0.5(2) . . . . ? C13 C12 N4 N5 177.32(19) . . . . ? N6 C12 N4 Zn1 160.07(19) . . . . ? C13 C12 N4 Zn1 -22.1(4) . . . . ? N6 C11 N5 N4 -0.3(2) . . . . ? C10 C11 N5 N4 -179.2(2) . . . . ? N6 C11 N5 B1 -179.2(2) . . . . ? C10 C11 N5 B1 1.8(4) . . . . ? C12 N4 N5 C11 0.5(2) . . . . ? Zn1 N4 N5 C11 -167.07(14) . . . . ? C12 N4 N5 B1 179.55(18) . . . . ? Zn1 N4 N5 B1 12.0(2) . . . . ? N8 B1 N5 C11 -130.0(2) . . . . ? N2 B1 N5 C11 112.7(2) . . . . ? N8 B1 N5 N4 51.2(2) . . . . ? N2 B1 N5 N4 -66.1(2) . . . . ? N5 C11 N6 C12 0.0(2) . . . . ? C10 C11 N6 C12 178.9(2) . . . . ? N4 C12 N6 C11 0.3(2) . . . . ? C13 C12 N6 C11 -177.6(2) . . . . ? N9 C21 N7 N8 -0.3(2) . . . . ? C22 C21 N7 N8 178.01(19) . . . . ? N9 C21 N7 Zn1 159.43(17) . . . . ? C22 C21 N7 Zn1 -22.2(4) . . . . ? N9 C20 N8 N7 -0.7(2) . . . . ? C19 C20 N8 N7 -178.9(2) . . . . ? N9 C20 N8 B1 -179.3(2) . . . . ? C19 C20 N8 B1 2.5(4) . . . . ? C21 N7 N8 C20 0.6(2) . . . . ? Zn1 N7 N8 C20 -165.68(14) . . . . ? C21 N7 N8 B1 179.41(18) . . . . ? Zn1 N7 N8 B1 13.1(2) . . . . ? N2 B1 N8 C20 -131.6(2) . . . . ? N5 B1 N8 C20 110.6(3) . . . . ? N2 B1 N8 N7 50.0(2) . . . . ? N5 B1 N8 N7 -67.8(2) . . . . ? N8 C20 N9 C21 0.5(2) . . . . ? C19 C20 N9 C21 178.7(2) . . . . ? N7 C21 N9 C20 -0.1(2) . . . . ? C22 C21 N9 C20 -178.4(2) . . . . ? C32 C31 N10 O3 0.3(3) . . . . ? C30 C31 N10 O3 177.3(2) . . . . ? C32 C31 N10 O2 -179.2(2) . . . . ? C30 C31 N10 O2 -2.3(3) . . . . ? N13 C36 N11 N12 0.5(3) . . . . ? C37 C36 N11 N12 179.9(2) . . . . ? N13 C36 N11 Zn2 -169.61(19) . . . . ? C37 C36 N11 Zn2 9.8(4) . . . . ? N13 C35 N12 N11 0.6(3) . . . . ? C34 C35 N12 N11 -178.9(2) . . . . ? N13 C35 N12 B2 175.6(2) . . . . ? C34 C35 N12 B2 -3.8(4) . . . . ? C36 N11 N12 C35 -0.7(2) . . . . ? Zn2 N11 N12 C35 173.03(14) . . . . ? C36 N11 N12 B2 -176.23(19) . . . . ? Zn2 N11 N12 B2 -2.5(2) . . . . ? N18 B2 N12 C35 128.4(2) . . . . ? N15 B2 N12 C35 -113.0(3) . . . . ? N18 B2 N12 N11 -57.2(3) . . . . ? N15 B2 N12 N11 61.5(3) . . . . ? N12 C35 N13 C36 -0.3(3) . . . . ? C34 C35 N13 C36 179.2(2) . . . . ? N11 C36 N13 C35 -0.2(3) . . . . ? C37 C36 N13 C35 -179.6(2) . . . . ? N16 C45 N14 N15 0.3(3) . . . . ? C46 C45 N14 N15 177.7(2) . . . . ? N16 C45 N14 Zn2 172.9(2) . . . . ? C46 C45 N14 Zn2 -9.7(4) . . . . ? N16 C44 N15 N14 -0.9(3) . . . . ? C43 C44 N15 N14 177.4(2) . . . . ? N16 C44 N15 B2 -179.9(2) . . . . ? C43 C44 N15 B2 -1.7(4) . . . . ? C45 N14 N15 C44 0.3(2) . . . . ? Zn2 N14 N15 C44 -175.03(15) . . . . ? C45 N14 N15 B2 179.5(2) . . . . ? Zn2 N14 N15 B2 4.1(2) . . . . ? N12 B2 N15 C44 116.8(3) . . . . ? N18 B2 N15 C44 -124.2(2) . . . . ? N12 B2 N15 N14 -62.1(3) . . . . ? N18 B2 N15 N14 56.8(3) . . . . ? N15 C44 N16 C45 1.0(3) . . . . ? C43 C44 N16 C45 -177.3(2) . . . . ? N14 C45 N16 C44 -0.8(3) . . . . ? C46 C45 N16 C44 -178.3(2) . . . . ? N19 C54 N17 N18 -0.4(3) . . . . ? C55 C54 N17 N18 -178.5(2) . . . . ? N19 C54 N17 Zn2 172.9(2) . . . . ? C55 C54 N17 Zn2 -5.2(4) . . . . ? N19 C53 N18 N17 -0.4(3) . . . . ? C52 C53 N18 N17 179.6(2) . . . . ? N19 C53 N18 B2 179.9(2) . . . . ? C52 C53 N18 B2 -0.1(4) . . . . ? C54 N17 N18 C53 0.4(2) . . . . ? Zn2 N17 N18 C53 -175.34(15) . . . . ? C54 N17 N18 B2 -179.8(2) . . . . ? Zn2 N17 N18 B2 4.4(2) . . . . ? N12 B2 N18 C53 -124.9(3) . . . . ? N15 B2 N18 C53 117.1(3) . . . . ? N12 B2 N18 N17 55.4(3) . . . . ? N15 B2 N18 N17 -62.6(3) . . . . ? N18 C53 N19 C54 0.2(3) . . . . ? C52 C53 N19 C54 -179.9(2) . . . . ? N17 C54 N19 C53 0.1(3) . . . . ? C55 C54 N19 C53 178.3(2) . . . . ? C63 C64 N20 O6 172.8(2) . . . . ? C65 C64 N20 O6 -4.2(3) . . . . ? C63 C64 N20 O5 -5.8(3) . . . . ? C65 C64 N20 O5 177.2(2) . . . . ? N23 C69 N21 N22 0.7(3) . . . . ? C70 C69 N21 N22 -179.0(2) . . . . ? N23 C69 N21 Zn3 -173.00(19) . . . . ? C70 C69 N21 Zn3 7.4(4) . . . . ? N23 C68 N22 N21 0.3(3) . . . . ? C67 C68 N22 N21 179.1(2) . . . . ? N23 C68 N22 B3 179.1(2) . . . . ? C67 C68 N22 B3 -2.1(4) . . . . ? C69 N21 N22 C68 -0.6(2) . . . . ? Zn3 N21 N22 C68 175.29(15) . . . . ? C69 N21 N22 B3 -179.5(2) . . . . ? Zn3 N21 N22 B3 -3.7(2) . . . . ? N28 B3 N22 C68 124.0(3) . . . . ? N25 B3 N22 C68 -117.8(3) . . . . ? N28 B3 N22 N21 -57.4(3) . . . . ? N25 B3 N22 N21 60.9(3) . . . . ? N22 C68 N23 C69 0.1(3) . . . . ? C67 C68 N23 C69 -178.7(2) . . . . ? N21 C69 N23 C68 -0.5(3) . . . . ? C70 C69 N23 C68 179.2(2) . . . . ? N26 C78 N24 N25 -0.1(2) . . . . ? C79 C78 N24 N25 176.6(2) . . . . ? N26 C78 N24 Zn3 177.65(19) . . . . ? C79 C78 N24 Zn3 -5.7(4) . . . . ? N26 C77 N25 N24 -0.6(3) . . . . ? C76 C77 N25 N24 -179.9(2) . . . . ? N26 C77 N25 B3 178.2(2) . . . . ? C76 C77 N25 B3 -1.1(4) . . . . ? C78 N24 N25 C77 0.4(2) . . . . ? Zn3 N24 N25 C77 -178.19(15) . . . . ? C78 N24 N25 B3 -178.4(2) . . . . ? Zn3 N24 N25 B3 2.9(2) . . . . ? N28 B3 N25 C77 -120.2(2) . . . . ? N22 B3 N25 C77 121.0(2) . . . . ? N28 B3 N25 N24 58.4(3) . . . . ? N22 B3 N25 N24 -60.4(3) . . . . ? N25 C77 N26 C78 0.5(3) . . . . ? C76 C77 N26 C78 179.8(2) . . . . ? N24 C78 N26 C77 -0.2(3) . . . . ? C79 C78 N26 C77 -177.0(2) . . . . ? N29 C87 N27 N28 -0.8(3) . . . . ? C88 C87 N27 N28 -180.0(2) . . . . ? N29 C87 N27 Zn3 170.93(19) . . . . ? C88 C87 N27 Zn3 -8.3(4) . . . . ? N29 C86 N28 N27 -0.8(3) . . . . ? C85 C86 N28 N27 179.9(2) . . . . ? N29 C86 N28 B3 -178.5(2) . . . . ? C85 C86 N28 B3 2.2(4) . . . . ? C87 N27 N28 C86 0.9(2) . . . . ? Zn3 N27 N28 C86 -173.55(16) . . . . ? C87 N27 N28 B3 179.0(2) . . . . ? Zn3 N27 N28 B3 4.5(2) . . . . ? N22 B3 N28 C86 -126.6(3) . . . . ? N25 B3 N28 C86 114.9(3) . . . . ? N22 B3 N28 N27 56.0(3) . . . . ? N25 B3 N28 N27 -62.6(3) . . . . ? N28 C86 N29 C87 0.3(3) . . . . ? C85 C86 N29 C87 179.6(2) . . . . ? N27 C87 N29 C86 0.3(3) . . . . ? C88 C87 N29 C86 179.5(2) . . . . ? C98 C97 N30 O8 174.7(3) . . . . ? C96 C97 N30 O8 -5.1(4) . . . . ? C98 C97 N30 O9 -5.4(4) . . . . ? C96 C97 N30 O9 174.8(3) . . . . ? C102 C103 N31 O12 -167.1(2) . . . . ? C104 C103 N31 O12 13.0(3) . . . . ? C102 C103 N31 O11 11.5(3) . . . . ? C104 C103 N31 O11 -168.4(2) . . . . ? C110 C109 N32 O14 -2.5(4) . . . . ? C108 C109 N32 O14 177.7(2) . . . . ? C110 C109 N32 O15 176.2(2) . . . . ? C108 C109 N32 O15 -3.6(4) . . . . ? C116 C115 N33 O18 -178.7(3) . . . . ? C114 C115 N33 O18 -0.5(4) . . . . ? C116 C115 N33 O17 0.1(4) . . . . ? C114 C115 N33 O17 178.3(2) . . . . ? C29 C28 O1 Zn1 -30.6(3) . . . . ? C33 C28 O1 Zn1 150.08(17) . . . . ? C62 C61 O4 Zn2 -17.3(3) . . . . ? C66 C61 O4 Zn2 162.35(16) . . . . ? C95 C94 O7 Zn3 -7.4(4) . . . . ? C99 C94 O7 Zn3 173.33(17) . . . . ? C28 O1 Zn1 N7 -26.5(2) . . . . ? C28 O1 Zn1 N4 97.5(2) . . . . ? C28 O1 Zn1 N1 -147.43(18) . . . . ? C21 N7 Zn1 O1 17.1(3) . . . . ? N8 N7 Zn1 O1 175.95(12) . . . . ? C21 N7 Zn1 N4 -118.7(2) . . . . ? N8 N7 Zn1 N4 40.18(14) . . . . ? C21 N7 Zn1 N1 148.1(2) . . . . ? N8 N7 Zn1 N1 -53.01(14) . . . . ? C12 N4 Zn1 O1 9.4(3) . . . . ? N5 N4 Zn1 O1 169.38(12) . . . . ? C12 N4 Zn1 N7 147.1(3) . . . . ? N5 N4 Zn1 N7 -53.01(14) . . . . ? C12 N4 Zn1 N1 -117.9(3) . . . . ? N5 N4 Zn1 N1 42.03(14) . . . . ? C3 N1 Zn1 O1 9.0(3) . . . . ? N2 N1 Zn1 O1 171.97(12) . . . . ? C3 N1 Zn1 N7 -126.7(3) . . . . ? N2 N1 Zn1 N7 36.30(14) . . . . ? C3 N1 Zn1 N4 139.4(3) . . . . ? N2 N1 Zn1 N4 -57.66(14) . . . . ? C61 O4 Zn2 N11 -157.98(17) . . . . ? C61 O4 Zn2 N17 -44.6(2) . . . . ? C61 O4 Zn2 N14 74.7(2) . . . . ? C36 N11 Zn2 O4 -14.8(3) . . . . ? N12 N11 Zn2 O4 175.50(13) . . . . ? C36 N11 Zn2 N17 -141.1(3) . . . . ? N12 N11 Zn2 N17 49.24(15) . . . . ? C36 N11 Zn2 N14 125.4(3) . . . . ? N12 N11 Zn2 N14 -44.28(15) . . . . ? C54 N17 Zn2 O4 7.0(3) . . . . ? N18 N17 Zn2 O4 -179.95(13) . . . . ? C54 N17 Zn2 N11 136.7(3) . . . . ? N18 N17 Zn2 N11 -50.32(15) . . . . ? C54 N17 Zn2 N14 -128.5(3) . . . . ? N18 N17 Zn2 N14 44.56(15) . . . . ? C45 N14 Zn2 O4 9.0(3) . . . . ? N15 N14 Zn2 O4 -178.69(13) . . . . ? C45 N14 Zn2 N11 -129.0(3) . . . . ? N15 N14 Zn2 N11 43.27(15) . . . . ? C45 N14 Zn2 N17 138.9(3) . . . . ? N15 N14 Zn2 N17 -48.79(15) . . . . ? C94 O7 Zn3 N21 -162.9(2) . . . . ? C94 O7 Zn3 N24 66.1(2) . . . . ? C94 O7 Zn3 N27 -52.6(2) . . . . ? C69 N21 Zn3 O7 -12.9(3) . . . . ? N22 N21 Zn3 O7 173.74(13) . . . . ? C69 N21 Zn3 N24 130.5(3) . . . . ? N22 N21 Zn3 N24 -42.88(15) . . . . ? C69 N21 Zn3 N27 -136.5(3) . . . . ? N22 N21 Zn3 N27 50.18(15) . . . . ? C78 N24 Zn3 O7 5.9(3) . . . . ? N25 N24 Zn3 O7 -176.44(12) . . . . ? C78 N24 Zn3 N21 -134.7(3) . . . . ? N25 N24 Zn3 N21 42.99(15) . . . . ? C78 N24 Zn3 N27 134.5(3) . . . . ? N25 N24 Zn3 N27 -47.81(15) . . . . ? C87 N27 Zn3 O7 9.5(3) . . . . ? N28 N27 Zn3 O7 -179.27(14) . . . . ? C87 N27 Zn3 N21 137.6(3) . . . . ? N28 N27 Zn3 N21 -51.10(16) . . . . ? C87 N27 Zn3 N24 -126.7(3) . . . . ? N28 N27 Zn3 N24 44.54(16) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O16 H16A N26 0.869(18) 1.831(19) 2.688(3) 168(3) . O13 H13 N16 0.846(18) 1.910(19) 2.748(3) 171(3) 1_465 O10 H10 N9 0.851(17) 1.814(18) 2.661(2) 173(3) 1_655 _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.655 _refine_diff_density_min -0.926 _refine_diff_density_rms 0.076 data_09mz244_0m _database_code_depnum_ccdc_archive 'CCDC 764044' #TrackingRef '- combined cifs' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H40 B N10 O4 Zn' _chemical_formula_weight 825.02 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 16.6709(14) _cell_length_b 14.6250(12) _cell_length_c 18.4633(14) _cell_angle_alpha 90.00 _cell_angle_beta 115.455(2) _cell_angle_gamma 90.00 _cell_volume 4064.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5525 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 30.73 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 0.659 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.782 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; One of the two solvate benzene molecules is located atop of a crystallographic inversion center. It shows large thermal motion and was refined as slightly offset from this center and constrained to resemble an ideal hexagon with C-C distances of 1.39 Angstrom. Opposite carbon atoms were constrained to have identical ADPs and all disordered C atoms were restrained to be approximately isotropic. ; _diffrn_ambient_temperature 100(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 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 27607 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 28.28 _reflns_number_total 10059 _reflns_number_gt 7989 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4' _computing_data_reduction 'Apex2 v2008.2-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0673P)^2^+2.4847P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10059 _refine_ls_number_parameters 530 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1252 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.60827(15) 0.24105(15) 0.64282(13) 0.0181(4) Uani 1 1 d . . . H1 H 0.5959 0.2389 0.6912 0.022 Uiso 1 1 calc R . . C1 C 0.56238(15) 0.05629(15) 0.70624(13) 0.0242(4) Uani 1 1 d . . . H1D H 0.5608 -0.0084 0.7195 0.036 Uiso 1 1 calc R . . H1E H 0.5040 0.0839 0.6923 0.036 Uiso 1 1 calc R . . H1C H 0.6073 0.0881 0.7526 0.036 Uiso 1 1 calc R . . C2 C 0.58517(13) 0.06413(13) 0.63689(12) 0.0188(4) Uani 1 1 d . . . C3 C 0.61526(12) 0.03217(13) 0.53894(11) 0.0175(4) Uani 1 1 d . . . C4 C 0.63857(13) -0.02159(13) 0.48328(12) 0.0192(4) Uani 1 1 d . . . C5 C 0.62987(13) -0.11698(14) 0.48179(12) 0.0209(4) Uani 1 1 d . . . H5 H 0.6049 -0.1457 0.5135 0.025 Uiso 1 1 calc R . . C6 C 0.65756(15) -0.16978(15) 0.43420(13) 0.0257(4) Uani 1 1 d . . . H6 H 0.6524 -0.2345 0.4342 0.031 Uiso 1 1 calc R . . C7 C 0.69257(17) -0.12843(16) 0.38685(15) 0.0325(5) Uani 1 1 d . . . H7 H 0.7120 -0.1646 0.3547 0.039 Uiso 1 1 calc R . . C8 C 0.69925(19) -0.03361(17) 0.38637(16) 0.0373(6) Uani 1 1 d . . . H8 H 0.7217 -0.0051 0.3526 0.045 Uiso 1 1 calc R . . C9 C 0.67344(16) 0.01965(15) 0.43483(14) 0.0289(5) Uani 1 1 d . . . H9 H 0.6795 0.0843 0.4351 0.035 Uiso 1 1 calc R . . C10 C 0.75648(14) 0.28375(16) 0.81781(12) 0.0249(4) Uani 1 1 d . . . H10A H 0.8144 0.2778 0.8640 0.037 Uiso 1 1 calc R . . H10B H 0.7191 0.2314 0.8162 0.037 Uiso 1 1 calc R . . H10C H 0.7277 0.3404 0.8227 0.037 Uiso 1 1 calc R . . C11 C 0.76897(13) 0.28637(13) 0.74235(12) 0.0186(4) Uani 1 1 d . . . C12 C 0.82518(13) 0.29771(14) 0.65941(12) 0.0199(4) Uani 1 1 d . . . C13 C 0.89272(15) 0.30614(16) 0.62901(14) 0.0267(5) Uani 1 1 d . . . C14 C 0.98010(16) 0.32923(19) 0.68029(16) 0.0363(6) Uani 1 1 d . . . H14 H 0.9960 0.3405 0.7354 0.044 Uiso 1 1 calc R . . C15 C 1.04410(18) 0.3358(2) 0.65093(19) 0.0506(8) Uani 1 1 d . . . H15 H 1.1036 0.3510 0.6861 0.061 Uiso 1 1 calc R . . C16 C 1.0210(2) 0.3202(3) 0.5709(2) 0.0668(11) Uani 1 1 d . . . H16 H 1.0645 0.3251 0.5508 0.080 Uiso 1 1 calc R . . C17 C 0.9353(2) 0.2975(3) 0.52035(19) 0.0702(12) Uani 1 1 d . . . H17 H 0.9197 0.2878 0.4650 0.084 Uiso 1 1 calc R . . C18 C 0.87092(18) 0.2887(2) 0.54864(16) 0.0462(7) Uani 1 1 d . . . H18 H 0.8122 0.2707 0.5133 0.055 Uiso 1 1 calc R . . C19 C 0.48448(15) 0.38059(15) 0.67188(13) 0.0262(4) Uani 1 1 d . . . H19A H 0.4555 0.4390 0.6717 0.039 Uiso 1 1 calc R . . H19B H 0.5451 0.3809 0.7148 0.039 Uiso 1 1 calc R . . H19C H 0.4507 0.3306 0.6809 0.039 Uiso 1 1 calc R . . C20 C 0.48762(13) 0.36744(13) 0.59329(13) 0.0207(4) Uani 1 1 d . . . C21 C 0.46395(13) 0.37827(13) 0.47144(12) 0.0197(4) Uani 1 1 d . . . C22 C 0.42179(13) 0.40702(13) 0.38671(13) 0.0218(4) Uani 1 1 d . . . C23 C 0.34455(14) 0.46050(14) 0.36085(14) 0.0275(5) Uani 1 1 d . . . H23 H 0.3227 0.4796 0.3982 0.033 Uiso 1 1 calc R . . C24 C 0.29997(15) 0.48551(16) 0.28073(15) 0.0324(5) Uani 1 1 d . . . H24 H 0.2477 0.5217 0.2635 0.039 Uiso 1 1 calc R . . C25 C 0.33115(16) 0.45816(16) 0.22582(15) 0.0340(5) Uani 1 1 d . . . H25 H 0.2999 0.4748 0.1710 0.041 Uiso 1 1 calc R . . C26 C 0.40820(16) 0.40636(15) 0.25101(14) 0.0296(5) Uani 1 1 d . . . H26 H 0.4301 0.3882 0.2135 0.036 Uiso 1 1 calc R . . C27 C 0.45338(14) 0.38106(14) 0.33111(13) 0.0247(4) Uani 1 1 d . . . H27 H 0.5062 0.3458 0.3480 0.030 Uiso 1 1 calc R . . C28 C 0.67952(13) 0.32914(14) 0.38340(12) 0.0209(4) Uani 1 1 d . . . C29 C 0.68481(15) 0.40912(15) 0.42722(13) 0.0259(4) Uani 1 1 d . . . H29 H 0.6742 0.4060 0.4738 0.031 Uiso 1 1 calc R . . C30 C 0.70513(14) 0.49224(15) 0.40378(13) 0.0257(4) Uani 1 1 d . . . H30 H 0.7090 0.5459 0.4341 0.031 Uiso 1 1 calc R . . C31 C 0.71977(14) 0.49639(15) 0.33571(14) 0.0257(4) Uani 1 1 d . . . C32 C 0.71801(17) 0.41829(16) 0.29242(15) 0.0317(5) Uani 1 1 d . . . H32 H 0.7298 0.4221 0.2465 0.038 Uiso 1 1 calc R . . C33 C 0.69898(16) 0.33493(16) 0.31652(14) 0.0289(5) Uani 1 1 d . . . H33 H 0.6990 0.2811 0.2878 0.035 Uiso 1 1 calc R . . C34 C 0.4856(3) 0.7397(3) 0.1406(2) 0.0745(12) Uani 1 1 d . . . H34 H 0.5056 0.6785 0.1539 0.089 Uiso 1 1 calc R . . C35 C 0.3981(3) 0.7563(3) 0.0927(2) 0.0718(11) Uani 1 1 d . . . H35 H 0.3576 0.7067 0.0734 0.086 Uiso 1 1 calc R . . C36 C 0.3686(3) 0.8428(4) 0.0723(2) 0.0770(12) Uani 1 1 d . . . H36 H 0.3075 0.8542 0.0395 0.092 Uiso 1 1 calc R . . C37 C 0.4292(4) 0.9159(4) 0.1003(3) 0.0944(17) Uani 1 1 d . . . H37 H 0.4102 0.9772 0.0860 0.113 Uiso 1 1 calc R . . C38 C 0.5193(4) 0.8953(5) 0.1502(3) 0.0920(16) Uani 1 1 d . . . H38 H 0.5619 0.9431 0.1700 0.110 Uiso 1 1 calc R . . C39 C 0.5439(3) 0.8088(4) 0.1693(2) 0.0810(13) Uani 1 1 d . . . H39 H 0.6041 0.7956 0.2040 0.097 Uiso 1 1 calc R . . N1 N 0.61610(11) 0.12307(11) 0.54257(10) 0.0174(3) Uani 1 1 d . . . N2 N 0.59742(11) 0.14344(11) 0.60665(9) 0.0172(3) Uani 1 1 d . . . N3 N 0.59577(11) -0.00650(11) 0.59618(10) 0.0187(3) Uani 1 1 d . . . N4 N 0.74031(11) 0.27866(11) 0.61385(10) 0.0201(3) Uani 1 1 d . . . N5 N 0.70490(11) 0.27125(11) 0.66854(10) 0.0173(3) Uani 1 1 d . . . N6 N 0.84538(11) 0.30411(12) 0.73926(10) 0.0202(3) Uani 1 1 d . . . N7 N 0.52897(11) 0.31600(11) 0.50273(10) 0.0185(3) Uani 1 1 d . . . N8 N 0.54337(11) 0.30868(11) 0.58173(10) 0.0183(3) Uani 1 1 d . . . N9 N 0.43716(11) 0.41144(12) 0.52556(11) 0.0226(4) Uani 1 1 d . . . N10 N 0.73330(13) 0.58511(14) 0.30751(13) 0.0323(4) Uani 1 1 d . . . O1 O 0.48438(10) 0.16146(10) 0.37948(9) 0.0224(3) Uani 1 1 d D . . H1A H 0.4629(17) 0.1187(15) 0.3937(16) 0.034 Uiso 1 1 d D . . H1B H 0.4482(15) 0.1744(19) 0.3330(11) 0.034 Uiso 1 1 d D . . O2 O 0.65699(10) 0.24911(10) 0.40193(9) 0.0224(3) Uani 1 1 d . . . O3 O 0.73513(13) 0.65389(12) 0.34659(13) 0.0422(4) Uani 1 1 d . . . O4 O 0.74160(15) 0.58897(13) 0.24428(13) 0.0481(5) Uani 1 1 d . . . C40 C 0.0650(19) 0.009(2) 0.5722(18) 0.206(9) Uani 0.50 1 d PGU A -1 H40 H 0.1019 0.0092 0.6282 0.247 Uiso 0.50 1 calc PR A -1 C41 C -0.007(2) 0.068(2) 0.5399(18) 0.248(9) Uani 0.50 1 d PGU A -1 H41 H -0.0199 0.1082 0.5739 0.297 Uiso 0.50 1 calc PR A -1 C42 C -0.0615(19) 0.067(2) 0.4579(18) 0.261(10) Uani 0.50 1 d PGU A -1 H42 H -0.1110 0.1072 0.4358 0.314 Uiso 0.50 1 calc PR A -1 C43 C -0.0432(19) 0.008(2) 0.4081(18) 0.206(9) Uani 0.50 1 d PG A -1 H43 H -0.0802 0.0072 0.3521 0.247 Uiso 0.50 1 calc PR A -1 C44 C 0.0292(19) -0.051(2) 0.4404(19) 0.248(9) Uani 0.50 1 d PG A -1 H44 H 0.0417 -0.0918 0.4064 0.297 Uiso 0.50 1 calc PR A -1 C45 C 0.0833(18) -0.051(2) 0.5224(19) 0.261(10) Uani 0.50 1 d PG A -1 H45 H 0.1327 -0.0908 0.5445 0.314 Uiso 0.50 1 calc PR A -1 Zn1 Zn 0.592213(15) 0.225900(15) 0.462307(14) 0.01838(8) 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 B1 0.0202(10) 0.0185(10) 0.0152(10) -0.0013(8) 0.0071(9) -0.0010(8) C1 0.0319(11) 0.0215(10) 0.0219(10) 0.0012(8) 0.0139(9) -0.0011(8) C2 0.0168(9) 0.0191(9) 0.0166(9) 0.0009(7) 0.0034(8) -0.0003(7) C3 0.0157(9) 0.0177(9) 0.0151(9) 0.0004(7) 0.0028(7) -0.0003(7) C4 0.0204(9) 0.0170(9) 0.0170(9) -0.0006(7) 0.0052(8) 0.0016(7) C5 0.0219(10) 0.0185(9) 0.0184(10) 0.0013(8) 0.0050(8) 0.0001(8) C6 0.0297(11) 0.0172(9) 0.0265(11) -0.0042(8) 0.0086(9) 0.0004(8) C7 0.0450(14) 0.0241(11) 0.0355(13) -0.0069(10) 0.0240(11) 0.0012(10) C8 0.0562(16) 0.0285(12) 0.0450(15) -0.0003(11) 0.0386(13) 0.0014(11) C9 0.0417(13) 0.0174(10) 0.0359(12) -0.0013(9) 0.0245(11) 0.0008(9) C10 0.0244(10) 0.0334(12) 0.0159(10) -0.0030(8) 0.0077(8) -0.0026(9) C11 0.0206(9) 0.0173(9) 0.0153(9) -0.0014(7) 0.0054(8) 0.0006(7) C12 0.0215(9) 0.0180(9) 0.0191(10) 0.0018(7) 0.0079(8) 0.0015(7) C13 0.0261(11) 0.0295(11) 0.0274(11) 0.0073(9) 0.0141(9) 0.0052(9) C14 0.0293(12) 0.0455(15) 0.0375(14) 0.0026(11) 0.0175(11) -0.0037(11) C15 0.0305(13) 0.071(2) 0.0570(19) 0.0142(16) 0.0254(13) -0.0008(13) C16 0.0436(17) 0.115(3) 0.058(2) 0.028(2) 0.0376(16) 0.0152(19) C17 0.0458(18) 0.141(4) 0.0343(16) 0.0196(19) 0.0269(15) 0.021(2) C18 0.0308(13) 0.085(2) 0.0259(13) 0.0098(13) 0.0148(11) 0.0131(13) C19 0.0274(11) 0.0248(10) 0.0272(11) -0.0054(9) 0.0125(9) 0.0016(8) C20 0.0202(9) 0.0161(9) 0.0246(10) -0.0041(8) 0.0085(8) -0.0020(7) C21 0.0175(9) 0.0142(9) 0.0232(10) -0.0019(8) 0.0049(8) -0.0021(7) C22 0.0213(10) 0.0147(9) 0.0234(10) 0.0010(8) 0.0038(8) -0.0018(7) C23 0.0238(10) 0.0194(10) 0.0335(12) 0.0008(9) 0.0069(9) 0.0011(8) C24 0.0231(11) 0.0222(11) 0.0378(13) 0.0050(10) -0.0003(10) 0.0012(8) C25 0.0352(13) 0.0232(11) 0.0260(12) 0.0045(9) -0.0036(10) -0.0034(9) C26 0.0373(12) 0.0216(10) 0.0224(11) 0.0003(9) 0.0057(10) -0.0012(9) C27 0.0270(10) 0.0175(9) 0.0237(11) 0.0021(8) 0.0054(9) 0.0002(8) C28 0.0201(9) 0.0206(10) 0.0219(10) 0.0001(8) 0.0087(8) 0.0003(7) C29 0.0328(11) 0.0249(11) 0.0235(11) -0.0037(9) 0.0152(9) -0.0041(9) C30 0.0289(11) 0.0216(10) 0.0288(11) -0.0054(9) 0.0144(9) -0.0027(8) C31 0.0237(10) 0.0220(10) 0.0361(12) 0.0011(9) 0.0172(10) -0.0025(8) C32 0.0433(13) 0.0287(12) 0.0350(13) -0.0030(10) 0.0282(11) -0.0064(10) C33 0.0384(12) 0.0247(11) 0.0326(12) -0.0062(9) 0.0239(11) -0.0053(9) C34 0.087(3) 0.104(3) 0.048(2) 0.013(2) 0.044(2) 0.007(3) C35 0.072(3) 0.101(3) 0.053(2) 0.010(2) 0.037(2) -0.014(2) C36 0.083(3) 0.109(4) 0.042(2) 0.015(2) 0.030(2) 0.015(3) C37 0.165(5) 0.088(3) 0.066(3) 0.003(2) 0.085(4) 0.020(4) C38 0.105(4) 0.127(5) 0.069(3) -0.044(3) 0.062(3) -0.041(4) C39 0.076(3) 0.131(4) 0.050(2) -0.020(3) 0.040(2) -0.009(3) N1 0.0185(8) 0.0174(8) 0.0144(8) -0.0007(6) 0.0054(6) 0.0005(6) N2 0.0183(8) 0.0180(8) 0.0137(8) -0.0003(6) 0.0054(6) -0.0002(6) N3 0.0202(8) 0.0181(8) 0.0148(8) 0.0003(6) 0.0048(7) -0.0003(6) N4 0.0228(8) 0.0217(8) 0.0173(8) 0.0013(7) 0.0102(7) 0.0011(7) N5 0.0203(8) 0.0175(8) 0.0137(8) -0.0012(6) 0.0068(7) -0.0002(6) N6 0.0215(8) 0.0193(8) 0.0179(8) -0.0015(7) 0.0067(7) 0.0003(6) N7 0.0192(8) 0.0177(8) 0.0163(8) 0.0000(6) 0.0056(7) 0.0004(6) N8 0.0191(8) 0.0165(8) 0.0177(8) -0.0016(6) 0.0063(7) 0.0003(6) N9 0.0211(8) 0.0178(8) 0.0271(9) -0.0022(7) 0.0088(7) 0.0012(7) N10 0.0321(10) 0.0257(10) 0.0465(12) -0.0005(9) 0.0240(10) -0.0056(8) O1 0.0226(7) 0.0206(7) 0.0189(7) 0.0044(6) 0.0039(6) -0.0026(6) O2 0.0287(8) 0.0189(7) 0.0218(7) -0.0003(6) 0.0131(6) -0.0013(6) O3 0.0539(11) 0.0220(8) 0.0626(13) -0.0047(8) 0.0363(10) -0.0057(8) O4 0.0712(14) 0.0378(10) 0.0527(12) 0.0011(9) 0.0431(11) -0.0170(10) C40 0.132(12) 0.178(12) 0.206(13) 0.012(11) -0.024(9) -0.032(10) C41 0.271(14) 0.214(13) 0.157(13) -0.004(10) -0.004(9) 0.119(11) C42 0.207(14) 0.318(16) 0.233(14) -0.106(13) 0.071(11) -0.051(12) C43 0.132(12) 0.178(12) 0.206(13) 0.012(11) -0.024(9) -0.032(10) C44 0.271(14) 0.214(13) 0.157(13) -0.004(10) -0.004(9) 0.119(11) C45 0.207(14) 0.318(16) 0.233(14) -0.106(13) 0.071(11) -0.051(12) Zn1 0.02113(13) 0.01590(12) 0.01897(13) 0.00245(9) 0.00943(10) 0.00167(8) _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 B1 N5 1.536(3) . ? B1 N8 1.540(3) . ? B1 N2 1.553(3) . ? B1 H1 1.0000 . ? C1 C2 1.488(3) . ? C1 H1D 0.9800 . ? C1 H1E 0.9800 . ? C1 H1C 0.9800 . ? C2 N3 1.333(3) . ? C2 N2 1.340(3) . ? C3 N1 1.331(2) . ? C3 N3 1.356(2) . ? C3 C4 1.473(3) . ? C4 C9 1.396(3) . ? C4 C5 1.402(3) . ? C5 C6 1.389(3) . ? C5 H5 0.9500 . ? C6 C7 1.382(3) . ? C6 H6 0.9500 . ? C7 C8 1.392(3) . ? C7 H7 0.9500 . ? C8 C9 1.387(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.495(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N6 1.325(3) . ? C11 N5 1.340(3) . ? C12 N4 1.328(3) . ? C12 N6 1.367(3) . ? C12 C13 1.463(3) . ? C13 C18 1.391(3) . ? C13 C14 1.395(3) . ? C14 C15 1.392(3) . ? C14 H14 0.9500 . ? C15 C16 1.376(5) . ? C15 H15 0.9500 . ? C16 C17 1.369(5) . ? C16 H16 0.9500 . ? C17 C18 1.387(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.487(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 N9 1.335(3) . ? C20 N8 1.348(2) . ? C21 N7 1.342(2) . ? C21 N9 1.348(3) . ? C21 C22 1.474(3) . ? C22 C27 1.393(3) . ? C22 C23 1.403(3) . ? C23 C24 1.389(3) . ? C23 H23 0.9500 . ? C24 C25 1.382(4) . ? C24 H24 0.9500 . ? C25 C26 1.388(3) . ? C25 H25 0.9500 . ? C26 C27 1.391(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 O2 1.319(2) . ? C28 C29 1.403(3) . ? C28 C33 1.408(3) . ? C29 C30 1.381(3) . ? C29 H29 0.9500 . ? C30 C31 1.381(3) . ? C30 H30 0.9500 . ? C31 C32 1.387(3) . ? C31 N10 1.451(3) . ? C32 C33 1.381(3) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.342(7) . ? C34 C35 1.365(6) . ? C34 H34 0.9500 . ? C35 C36 1.350(6) . ? C35 H35 0.9500 . ? C36 C37 1.407(7) . ? C36 H36 0.9500 . ? C37 C38 1.416(7) . ? C37 H37 0.9500 . ? C38 C39 1.331(7) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? N1 N2 1.379(2) . ? N1 Zn1 2.0271(16) . ? N4 N5 1.376(2) . ? N7 N8 1.377(2) . ? N7 Zn1 2.0202(16) . ? N10 O3 1.231(3) . ? N10 O4 1.235(3) . ? O1 Zn1 2.0237(15) . ? O1 H1A 0.818(17) . ? O1 H1B 0.831(17) . ? O2 Zn1 1.8865(15) . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C40 H40 0.9500 . ? C41 C42 1.3900 . ? C41 H41 0.9500 . ? C42 C43 1.3900 . ? C42 H42 0.9500 . ? C43 C44 1.3900 . ? C43 H43 0.9500 . ? C44 C45 1.3900 . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? 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 N5 B1 N8 110.81(16) . . ? N5 B1 N2 108.07(16) . . ? N8 B1 N2 111.10(16) . . ? N5 B1 H1 108.9 . . ? N8 B1 H1 108.9 . . ? N2 B1 H1 108.9 . . ? C2 C1 H1D 109.5 . . ? C2 C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? C2 C1 H1C 109.5 . . ? H1D C1 H1C 109.5 . . ? H1E C1 H1C 109.5 . . ? N3 C2 N2 110.78(17) . . ? N3 C2 C1 124.75(18) . . ? N2 C2 C1 124.47(18) . . ? N1 C3 N3 112.24(17) . . ? N1 C3 C4 124.62(18) . . ? N3 C3 C4 123.01(17) . . ? C9 C4 C5 119.05(19) . . ? C9 C4 C3 121.60(18) . . ? C5 C4 C3 119.27(18) . . ? C6 C5 C4 120.39(19) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C7 C6 C5 120.2(2) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 119.8(2) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C9 C8 C7 120.5(2) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C4 120.1(2) . . ? C8 C9 H9 120.0 . . ? C4 C9 H9 120.0 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N6 C11 N5 110.44(17) . . ? N6 C11 C10 124.53(18) . . ? N5 C11 C10 125.03(18) . . ? N4 C12 N6 113.52(17) . . ? N4 C12 C13 124.10(19) . . ? N6 C12 C13 122.30(19) . . ? C18 C13 C14 119.1(2) . . ? C18 C13 C12 120.1(2) . . ? C14 C13 C12 120.7(2) . . ? C15 C14 C13 120.2(3) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 119.9(3) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C17 C16 C15 120.1(3) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 121.0(3) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C17 C18 C13 119.7(3) . . ? C17 C18 H18 120.2 . . ? C13 C18 H18 120.2 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N9 C20 N8 111.03(18) . . ? N9 C20 C19 125.42(18) . . ? N8 C20 C19 123.55(19) . . ? N7 C21 N9 112.88(18) . . ? N7 C21 C22 125.39(18) . . ? N9 C21 C22 121.69(18) . . ? C27 C22 C23 118.9(2) . . ? C27 C22 C21 123.07(19) . . ? C23 C22 C21 118.0(2) . . ? C24 C23 C22 120.1(2) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 120.5(2) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 119.8(2) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C27 120.1(2) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C22 120.5(2) . . ? C26 C27 H27 119.7 . . ? C22 C27 H27 119.7 . . ? O2 C28 C29 123.00(18) . . ? O2 C28 C33 118.67(18) . . ? C29 C28 C33 118.33(19) . . ? C30 C29 C28 121.09(19) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C31 119.2(2) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C30 C31 C32 121.3(2) . . ? C30 C31 N10 118.8(2) . . ? C32 C31 N10 119.8(2) . . ? C33 C32 C31 119.5(2) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C32 C33 C28 120.5(2) . . ? C32 C33 H33 119.8 . . ? C28 C33 H33 119.8 . . ? C39 C34 C35 120.8(5) . . ? C39 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C36 C35 C34 120.5(5) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C37 119.5(4) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? C36 C37 C38 118.1(5) . . ? C36 C37 H37 121.0 . . ? C38 C37 H37 121.0 . . ? C39 C38 C37 119.6(5) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C39 C34 121.5(5) . . ? C38 C39 H39 119.2 . . ? C34 C39 H39 119.2 . . ? C3 N1 N2 104.93(15) . . ? C3 N1 Zn1 135.22(13) . . ? N2 N1 Zn1 114.90(12) . . ? C2 N2 N1 107.54(16) . . ? C2 N2 B1 128.80(16) . . ? N1 N2 B1 122.68(15) . . ? C2 N3 C3 104.50(16) . . ? C12 N4 N5 103.18(16) . . ? C11 N5 N4 109.12(16) . . ? C11 N5 B1 129.32(17) . . ? N4 N5 B1 121.31(16) . . ? C11 N6 C12 103.73(17) . . ? C21 N7 N8 104.46(16) . . ? C21 N7 Zn1 137.48(14) . . ? N8 N7 Zn1 117.37(12) . . ? C20 N8 N7 107.46(16) . . ? C20 N8 B1 127.48(17) . . ? N7 N8 B1 124.99(16) . . ? C20 N9 C21 104.17(17) . . ? O3 N10 O4 122.2(2) . . ? O3 N10 C31 119.3(2) . . ? O4 N10 C31 118.6(2) . . ? Zn1 O1 H1A 118.9(19) . . ? Zn1 O1 H1B 133(2) . . ? H1A O1 H1B 106(3) . . ? C28 O2 Zn1 127.76(13) . . ? C41 C40 C45 120.0 . . ? C41 C40 H40 120.0 . . ? C45 C40 H40 120.0 . . ? C40 C41 C42 120.0 . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.0 . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C40 120.0 . . ? C44 C45 H45 120.0 . . ? C40 C45 H45 120.0 . . ? O2 Zn1 N7 128.55(6) . . ? O2 Zn1 O1 100.69(6) . . ? N7 Zn1 O1 98.50(6) . . ? O2 Zn1 N1 125.66(6) . . ? N7 Zn1 N1 100.58(7) . . ? O1 Zn1 N1 92.20(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C3 C4 C9 7.2(3) . . . . ? N3 C3 C4 C9 -168.4(2) . . . . ? N1 C3 C4 C5 -176.10(18) . . . . ? N3 C3 C4 C5 8.2(3) . . . . ? C9 C4 C5 C6 1.5(3) . . . . ? C3 C4 C5 C6 -175.23(19) . . . . ? C4 C5 C6 C7 -1.1(3) . . . . ? C5 C6 C7 C8 -0.6(4) . . . . ? C6 C7 C8 C9 1.9(4) . . . . ? C7 C8 C9 C4 -1.4(4) . . . . ? C5 C4 C9 C8 -0.3(3) . . . . ? C3 C4 C9 C8 176.4(2) . . . . ? N4 C12 C13 C18 -3.9(3) . . . . ? N6 C12 C13 C18 172.5(2) . . . . ? N4 C12 C13 C14 177.9(2) . . . . ? N6 C12 C13 C14 -5.7(3) . . . . ? C18 C13 C14 C15 0.9(4) . . . . ? C12 C13 C14 C15 179.1(2) . . . . ? C13 C14 C15 C16 0.5(5) . . . . ? C14 C15 C16 C17 -0.5(6) . . . . ? C15 C16 C17 C18 -1.0(7) . . . . ? C16 C17 C18 C13 2.3(6) . . . . ? C14 C13 C18 C17 -2.2(4) . . . . ? C12 C13 C18 C17 179.5(3) . . . . ? N7 C21 C22 C27 -8.9(3) . . . . ? N9 C21 C22 C27 173.53(19) . . . . ? N7 C21 C22 C23 168.93(19) . . . . ? N9 C21 C22 C23 -8.7(3) . . . . ? C27 C22 C23 C24 1.1(3) . . . . ? C21 C22 C23 C24 -176.85(19) . . . . ? C22 C23 C24 C25 -0.1(3) . . . . ? C23 C24 C25 C26 -0.9(3) . . . . ? C24 C25 C26 C27 0.8(3) . . . . ? C25 C26 C27 C22 0.2(3) . . . . ? C23 C22 C27 C26 -1.1(3) . . . . ? C21 C22 C27 C26 176.65(19) . . . . ? O2 C28 C29 C30 -177.3(2) . . . . ? C33 C28 C29 C30 2.5(3) . . . . ? C28 C29 C30 C31 0.5(3) . . . . ? C29 C30 C31 C32 -2.6(3) . . . . ? C29 C30 C31 N10 174.6(2) . . . . ? C30 C31 C32 C33 1.7(4) . . . . ? N10 C31 C32 C33 -175.5(2) . . . . ? C31 C32 C33 C28 1.4(4) . . . . ? O2 C28 C33 C32 176.4(2) . . . . ? C29 C28 C33 C32 -3.5(3) . . . . ? C39 C34 C35 C36 0.8(5) . . . . ? C34 C35 C36 C37 0.8(5) . . . . ? C35 C36 C37 C38 -1.1(5) . . . . ? C36 C37 C38 C39 -0.1(6) . . . . ? C37 C38 C39 C34 1.7(6) . . . . ? C35 C34 C39 C38 -2.1(6) . . . . ? N3 C3 N1 N2 1.0(2) . . . . ? C4 C3 N1 N2 -175.10(17) . . . . ? N3 C3 N1 Zn1 -151.56(15) . . . . ? C4 C3 N1 Zn1 32.4(3) . . . . ? N3 C2 N2 N1 0.6(2) . . . . ? C1 C2 N2 N1 -179.12(18) . . . . ? N3 C2 N2 B1 -168.10(18) . . . . ? C1 C2 N2 B1 12.2(3) . . . . ? C3 N1 N2 C2 -0.9(2) . . . . ? Zn1 N1 N2 C2 158.09(12) . . . . ? C3 N1 N2 B1 168.62(17) . . . . ? Zn1 N1 N2 B1 -32.4(2) . . . . ? N5 B1 N2 C2 110.0(2) . . . . ? N8 B1 N2 C2 -128.3(2) . . . . ? N5 B1 N2 N1 -57.2(2) . . . . ? N8 B1 N2 N1 64.6(2) . . . . ? N2 C2 N3 C3 0.0(2) . . . . ? C1 C2 N3 C3 179.70(19) . . . . ? N1 C3 N3 C2 -0.6(2) . . . . ? C4 C3 N3 C2 175.52(18) . . . . ? N6 C12 N4 N5 -0.9(2) . . . . ? C13 C12 N4 N5 175.78(19) . . . . ? N6 C11 N5 N4 0.4(2) . . . . ? C10 C11 N5 N4 -179.63(18) . . . . ? N6 C11 N5 B1 174.72(18) . . . . ? C10 C11 N5 B1 -5.3(3) . . . . ? C12 N4 N5 C11 0.3(2) . . . . ? C12 N4 N5 B1 -174.56(17) . . . . ? N8 B1 N5 C11 125.1(2) . . . . ? N2 B1 N5 C11 -113.0(2) . . . . ? N8 B1 N5 N4 -61.2(2) . . . . ? N2 B1 N5 N4 60.7(2) . . . . ? N5 C11 N6 C12 -0.9(2) . . . . ? C10 C11 N6 C12 179.13(19) . . . . ? N4 C12 N6 C11 1.1(2) . . . . ? C13 C12 N6 C11 -175.60(19) . . . . ? N9 C21 N7 N8 0.7(2) . . . . ? C22 C21 N7 N8 -177.03(18) . . . . ? N9 C21 N7 Zn1 170.33(14) . . . . ? C22 C21 N7 Zn1 -7.4(3) . . . . ? N9 C20 N8 N7 0.8(2) . . . . ? C19 C20 N8 N7 -178.85(18) . . . . ? N9 C20 N8 B1 -176.05(18) . . . . ? C19 C20 N8 B1 4.3(3) . . . . ? C21 N7 N8 C20 -0.9(2) . . . . ? Zn1 N7 N8 C20 -173.00(12) . . . . ? C21 N7 N8 B1 176.05(17) . . . . ? Zn1 N7 N8 B1 4.0(2) . . . . ? N5 B1 N8 C20 -110.1(2) . . . . ? N2 B1 N8 C20 129.79(19) . . . . ? N5 B1 N8 N7 73.6(2) . . . . ? N2 B1 N8 N7 -46.6(2) . . . . ? N8 C20 N9 C21 -0.4(2) . . . . ? C19 C20 N9 C21 179.30(19) . . . . ? N7 C21 N9 C20 -0.3(2) . . . . ? C22 C21 N9 C20 177.60(18) . . . . ? C30 C31 N10 O3 3.0(3) . . . . ? C32 C31 N10 O3 -179.7(2) . . . . ? C30 C31 N10 O4 -176.2(2) . . . . ? C32 C31 N10 O4 1.1(3) . . . . ? C29 C28 O2 Zn1 22.2(3) . . . . ? C33 C28 O2 Zn1 -157.67(16) . . . . ? C45 C40 C41 C42 0.0 . . . . ? C40 C41 C42 C43 0.0 . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C40 0.0 . . . . ? C41 C40 C45 C44 0.0 . . . . ? C28 O2 Zn1 N7 7.8(2) . . . . ? C28 O2 Zn1 O1 117.89(17) . . . . ? C28 O2 Zn1 N1 -141.53(16) . . . . ? C21 N7 Zn1 O2 58.8(2) . . . . ? N8 N7 Zn1 O2 -132.60(13) . . . . ? C21 N7 Zn1 O1 -52.3(2) . . . . ? N8 N7 Zn1 O1 116.37(13) . . . . ? C21 N7 Zn1 N1 -146.13(19) . . . . ? N8 N7 Zn1 N1 22.51(14) . . . . ? C3 N1 Zn1 O2 -62.1(2) . . . . ? N2 N1 Zn1 O2 147.31(12) . . . . ? C3 N1 Zn1 N7 141.78(18) . . . . ? N2 N1 Zn1 N7 -8.78(14) . . . . ? C3 N1 Zn1 O1 42.71(19) . . . . ? N2 N1 Zn1 O1 -107.85(13) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A N3 0.818(17) 1.959(18) 2.764(2) 167(3) 3_656 O1 H1B N6 0.831(17) 1.867(18) 2.677(2) 165(3) 4_565 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.003 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.072 ## data_09mz291_0m _database_code_depnum_ccdc_archive 'CCDC 764045' #TrackingRef '- combined cifs' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H27 B F3 N9 O Zn' _chemical_formula_weight 650.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 17.1768(9) _cell_length_b 11.6552(7) _cell_length_c 16.1882(9) _cell_angle_alpha 90.00 _cell_angle_beta 115.8620(10) _cell_angle_gamma 90.00 _cell_volume 2916.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7656 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 31.22 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.704 _exptl_absorpt_correction_T_max 0.784 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; The CH2-CF3 moiety is disordered over two positions in a ratio of 0.8869(17) to 0.1131(17). Equivalent bond distances in the two disorderede sections were restrained to be similar and ADPs of equivalent atoms were constrained to be identical. ; _diffrn_ambient_temperature 100(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 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 19041 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7027 _reflns_number_gt 6090 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4' _computing_data_reduction 'Apex2 v2008.2-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0491P)^2^+1.8131P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7027 _refine_ls_number_parameters 416 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0931 _refine_ls_wR_factor_gt 0.0883 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.24210(13) -0.10766(16) 0.42629(13) 0.0169(4) Uani 1 1 d . . . H1 H 0.2333 -0.1822 0.4516 0.020 Uiso 1 1 calc R . . C1 C 0.16903(13) -0.32121(16) 0.28725(14) 0.0254(4) Uani 1 1 d . . . H1A H 0.2151 -0.3622 0.3378 0.038 Uiso 1 1 calc R . . H1B H 0.1468 -0.3694 0.2321 0.038 Uiso 1 1 calc R . . H1C H 0.1221 -0.3035 0.3041 0.038 Uiso 1 1 calc R . . C2 C 0.20412(11) -0.21261(14) 0.26854(12) 0.0182(3) Uani 1 1 d . . . C3 C 0.24498(11) -0.08388(14) 0.20432(11) 0.0158(3) Uani 1 1 d . . . C4 C 0.26811(11) -0.02388(14) 0.13808(12) 0.0165(3) Uani 1 1 d . . . C5 C 0.21214(11) -0.02864(15) 0.04477(12) 0.0192(3) Uani 1 1 d . . . H5 H 0.1602 -0.0719 0.0242 0.023 Uiso 1 1 calc R . . C6 C 0.23221(13) 0.02978(16) -0.01812(12) 0.0225(4) Uani 1 1 d . . . H6 H 0.1932 0.0282 -0.0815 0.027 Uiso 1 1 calc R . . C7 C 0.30910(13) 0.09040(16) 0.01139(13) 0.0239(4) Uani 1 1 d . . . H7 H 0.3226 0.1306 -0.0318 0.029 Uiso 1 1 calc R . . C8 C 0.36635(13) 0.09244(16) 0.10392(14) 0.0248(4) Uani 1 1 d . . . H8 H 0.4197 0.1324 0.1238 0.030 Uiso 1 1 calc R . . C9 C 0.34588(12) 0.03600(16) 0.16773(12) 0.0210(4) Uani 1 1 d . . . H9 H 0.3847 0.0383 0.2312 0.025 Uiso 1 1 calc R . . C10 C 0.38440(13) -0.19711(16) 0.61810(13) 0.0236(4) Uani 1 1 d . . . H10A H 0.4389 -0.2113 0.6726 0.035 Uiso 1 1 calc R . . H10B H 0.3712 -0.2626 0.5762 0.035 Uiso 1 1 calc R . . H10C H 0.3376 -0.1870 0.6366 0.035 Uiso 1 1 calc R . . C11 C 0.39275(12) -0.09143(15) 0.57087(12) 0.0181(3) Uani 1 1 d . . . C12 C 0.43450(11) 0.06720(14) 0.54089(12) 0.0169(3) Uani 1 1 d . . . C13 C 0.48565(11) 0.17181(14) 0.55095(12) 0.0180(3) Uani 1 1 d . . . C14 C 0.54946(11) 0.20160(15) 0.63743(12) 0.0200(3) Uani 1 1 d . . . H14 H 0.5607 0.1531 0.6886 0.024 Uiso 1 1 calc R . . C15 C 0.59661(12) 0.30216(16) 0.64898(13) 0.0228(4) Uani 1 1 d . . . H15 H 0.6400 0.3221 0.7081 0.027 Uiso 1 1 calc R . . C16 C 0.58079(12) 0.37358(15) 0.57483(14) 0.0235(4) Uani 1 1 d . . . H16 H 0.6132 0.4422 0.5831 0.028 Uiso 1 1 calc R . . C17 C 0.51742(12) 0.34427(16) 0.48853(13) 0.0228(4) Uani 1 1 d . . . H17 H 0.5061 0.3934 0.4377 0.027 Uiso 1 1 calc R . . C18 C 0.47057(11) 0.24358(15) 0.47606(12) 0.0201(3) Uani 1 1 d . . . H18 H 0.4281 0.2232 0.4166 0.024 Uiso 1 1 calc R . . C19 C 0.10117(15) -0.12381(17) 0.50415(17) 0.0314(5) Uani 1 1 d . . . H19A H 0.0557 -0.1063 0.5234 0.047 Uiso 1 1 calc R . . H19B H 0.1547 -0.1434 0.5581 0.047 Uiso 1 1 calc R . . H19C H 0.0831 -0.1888 0.4615 0.047 Uiso 1 1 calc R . . C20 C 0.11632(12) -0.02185(15) 0.45775(13) 0.0214(4) Uani 1 1 d . . . C21 C 0.10756(11) 0.14178(15) 0.39800(12) 0.0184(3) Uani 1 1 d . . . C22 C 0.07407(11) 0.25700(15) 0.36320(13) 0.0207(4) Uani 1 1 d . . . C23 C 0.03020(12) 0.31803(16) 0.40411(14) 0.0258(4) Uani 1 1 d . . . H23 H 0.0236 0.2861 0.4547 0.031 Uiso 1 1 calc R . . C24 C -0.00389(13) 0.42582(17) 0.37058(16) 0.0318(5) Uani 1 1 d . . . H24 H -0.0334 0.4677 0.3986 0.038 Uiso 1 1 calc R . . C25 C 0.00515(13) 0.47195(17) 0.29660(16) 0.0327(5) Uani 1 1 d . . . H25 H -0.0181 0.5457 0.2742 0.039 Uiso 1 1 calc R . . C26 C 0.04777(13) 0.41160(17) 0.25492(15) 0.0295(4) Uani 1 1 d . . . H26 H 0.0535 0.4436 0.2039 0.035 Uiso 1 1 calc R . . C27 C 0.08227(12) 0.30379(16) 0.28810(13) 0.0236(4) Uani 1 1 d . . . H27 H 0.1114 0.2621 0.2595 0.028 Uiso 1 1 calc R . . N1 N 0.25706(9) -0.03874(12) 0.28437(10) 0.0166(3) Uani 1 1 d . . . N2 N 0.23210(10) -0.12389(12) 0.32690(10) 0.0164(3) Uani 1 1 d . . . N3 N 0.21124(10) -0.19104(12) 0.19101(10) 0.0187(3) Uani 1 1 d . . . N4 N 0.35936(9) 0.04601(12) 0.46825(10) 0.0163(3) Uani 1 1 d . . . N5 N 0.33280(9) -0.05799(12) 0.48769(10) 0.0160(3) Uani 1 1 d . . . N6 N 0.45721(10) -0.01636(13) 0.60560(10) 0.0193(3) Uani 1 1 d . . . N7 N 0.16987(9) 0.08833(12) 0.38482(10) 0.0169(3) Uani 1 1 d . . . N8 N 0.17465(9) -0.01833(12) 0.42355(10) 0.0171(3) Uani 1 1 d . . . N9 N 0.07288(10) 0.07686(13) 0.44276(11) 0.0230(3) Uani 1 1 d . . . O1 O 0.27723(9) 0.25763(11) 0.30172(9) 0.0232(3) Uani 1 1 d D . . Zn1 Zn 0.271303(13) 0.115603(16) 0.348921(13) 0.01538(7) Uani 1 1 d . A . C28 C 0.25008(14) 0.28317(18) 0.20907(14) 0.0231(4) Uani 0.8869(17) 1 d PD A 1 H28A H 0.1892 0.3097 0.1819 0.028 Uiso 0.8869(17) 1 calc PR A 1 H28B H 0.2532 0.2134 0.1758 0.028 Uiso 0.8869(17) 1 calc PR A 1 C29 C 0.30634(17) 0.3744(2) 0.19948(16) 0.0326(5) Uani 0.8869(17) 1 d PD A 1 F1 F 0.38976(10) 0.3417(2) 0.23586(12) 0.0606(5) Uani 0.8869(17) 1 d PD A 1 F2 F 0.2844(2) 0.3999(3) 0.11143(18) 0.0433(6) Uani 0.8869(17) 1 d PD A 1 F3 F 0.30350(16) 0.47227(13) 0.23957(12) 0.0653(6) Uani 0.8869(17) 1 d PD A 1 C28B C 0.3141(10) 0.3030(13) 0.2512(10) 0.0231(4) Uani 0.1131(17) 1 d PD A 2 H28C H 0.3462 0.2434 0.2352 0.028 Uiso 0.1131(17) 1 calc PR A 2 H28D H 0.3550 0.3646 0.2859 0.028 Uiso 0.1131(17) 1 calc PR A 2 C29B C 0.2446(10) 0.3492(12) 0.1688(10) 0.0326(5) Uani 0.1131(17) 1 d PD A 2 F1B F 0.1900(12) 0.2622(10) 0.1257(9) 0.0653(6) Uani 0.1131(17) 1 d PD A 2 F2B F 0.267(2) 0.382(3) 0.1034(17) 0.0433(6) Uani 0.1131(17) 1 d PD A 2 F3B F 0.1903(8) 0.4273(14) 0.1725(10) 0.0606(5) Uani 0.1131(17) 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 B1 0.0190(9) 0.0171(8) 0.0176(9) 0.0024(7) 0.0107(8) -0.0001(7) C1 0.0301(10) 0.0220(9) 0.0269(10) -0.0019(7) 0.0149(8) -0.0083(7) C2 0.0172(8) 0.0182(8) 0.0202(8) -0.0003(6) 0.0090(7) -0.0006(6) C3 0.0139(8) 0.0184(7) 0.0152(8) 0.0000(6) 0.0064(6) 0.0001(6) C4 0.0182(8) 0.0173(7) 0.0157(8) -0.0006(6) 0.0091(7) 0.0011(6) C5 0.0177(8) 0.0210(8) 0.0180(8) -0.0023(6) 0.0071(7) -0.0011(6) C6 0.0278(10) 0.0248(9) 0.0151(8) 0.0010(7) 0.0096(7) 0.0041(7) C7 0.0308(10) 0.0237(8) 0.0246(9) 0.0052(7) 0.0190(8) 0.0043(7) C8 0.0217(9) 0.0280(9) 0.0288(10) 0.0007(8) 0.0150(8) -0.0050(7) C9 0.0203(9) 0.0253(8) 0.0174(8) -0.0003(7) 0.0083(7) -0.0031(7) C10 0.0276(10) 0.0257(9) 0.0201(9) 0.0073(7) 0.0128(8) 0.0035(7) C11 0.0218(9) 0.0199(8) 0.0166(8) 0.0025(6) 0.0119(7) 0.0052(6) C12 0.0173(8) 0.0202(8) 0.0157(8) -0.0004(6) 0.0094(7) 0.0037(6) C13 0.0159(8) 0.0202(8) 0.0204(8) -0.0014(6) 0.0102(7) 0.0027(6) C14 0.0181(8) 0.0232(8) 0.0193(8) 0.0004(7) 0.0088(7) 0.0046(7) C15 0.0157(8) 0.0282(9) 0.0226(9) -0.0042(7) 0.0066(7) 0.0000(7) C16 0.0205(9) 0.0221(8) 0.0301(10) -0.0027(7) 0.0130(8) -0.0016(7) C17 0.0230(9) 0.0238(9) 0.0244(9) 0.0036(7) 0.0129(8) 0.0025(7) C18 0.0181(8) 0.0244(8) 0.0185(8) -0.0007(7) 0.0086(7) 0.0006(7) C19 0.0348(11) 0.0276(10) 0.0470(13) 0.0137(9) 0.0321(11) 0.0080(8) C20 0.0216(9) 0.0230(8) 0.0244(9) 0.0040(7) 0.0146(8) 0.0023(7) C21 0.0170(8) 0.0203(8) 0.0188(8) -0.0003(6) 0.0087(7) -0.0010(6) C22 0.0144(8) 0.0188(8) 0.0264(9) 0.0017(7) 0.0065(7) -0.0012(6) C23 0.0210(9) 0.0225(9) 0.0358(11) 0.0006(8) 0.0142(8) 0.0001(7) C24 0.0192(9) 0.0240(9) 0.0503(13) -0.0013(9) 0.0134(9) 0.0036(7) C25 0.0185(9) 0.0218(9) 0.0453(13) 0.0052(8) 0.0024(9) 0.0028(7) C26 0.0231(10) 0.0260(9) 0.0297(10) 0.0087(8) 0.0024(8) -0.0027(8) C27 0.0194(9) 0.0230(8) 0.0245(9) 0.0024(7) 0.0058(7) -0.0009(7) N1 0.0185(7) 0.0179(6) 0.0158(7) 0.0016(5) 0.0097(6) -0.0018(5) N2 0.0180(7) 0.0167(6) 0.0169(7) 0.0016(5) 0.0099(6) -0.0010(5) N3 0.0188(7) 0.0192(7) 0.0188(7) -0.0014(5) 0.0087(6) -0.0020(5) N4 0.0180(7) 0.0166(6) 0.0167(7) 0.0014(5) 0.0098(6) 0.0002(5) N5 0.0194(7) 0.0164(6) 0.0150(7) 0.0021(5) 0.0101(6) 0.0008(5) N6 0.0212(7) 0.0219(7) 0.0167(7) 0.0018(6) 0.0101(6) 0.0041(6) N7 0.0184(7) 0.0157(6) 0.0172(7) 0.0028(5) 0.0084(6) 0.0005(5) N8 0.0201(7) 0.0173(6) 0.0174(7) 0.0029(5) 0.0115(6) 0.0006(5) N9 0.0230(8) 0.0223(7) 0.0291(9) 0.0046(6) 0.0164(7) 0.0029(6) O1 0.0299(7) 0.0199(6) 0.0203(6) 0.0043(5) 0.0115(6) -0.0030(5) Zn1 0.01762(11) 0.01549(10) 0.01417(11) 0.00166(7) 0.00799(8) -0.00089(7) C28 0.0283(11) 0.0224(9) 0.0187(10) 0.0026(8) 0.0104(8) -0.0021(8) C29 0.0369(13) 0.0360(12) 0.0224(11) 0.0059(9) 0.0107(10) -0.0110(10) F1 0.0277(8) 0.1039(15) 0.0458(10) 0.0233(10) 0.0119(7) -0.0138(9) F2 0.0421(17) 0.0597(17) 0.0273(9) 0.0174(9) 0.0144(10) -0.0137(10) F3 0.1205(18) 0.0241(8) 0.0485(10) -0.0047(7) 0.0342(11) -0.0255(9) C28B 0.0283(11) 0.0224(9) 0.0187(10) 0.0026(8) 0.0104(8) -0.0021(8) C29B 0.0369(13) 0.0360(12) 0.0224(11) 0.0059(9) 0.0107(10) -0.0110(10) F1B 0.1205(18) 0.0241(8) 0.0485(10) -0.0047(7) 0.0342(11) -0.0255(9) F2B 0.0421(17) 0.0597(17) 0.0273(9) 0.0174(9) 0.0144(10) -0.0137(10) F3B 0.0277(8) 0.1039(15) 0.0458(10) 0.0233(10) 0.0119(7) -0.0138(9) _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 B1 N8 1.544(2) . ? B1 N5 1.549(2) . ? B1 N2 1.553(2) . ? B1 H1 1.0000 . ? C1 C2 1.489(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N3 1.337(2) . ? C2 N2 1.340(2) . ? C3 N1 1.328(2) . ? C3 N3 1.354(2) . ? C3 C4 1.473(2) . ? C4 C5 1.394(2) . ? C4 C9 1.394(2) . ? C5 C6 1.387(2) . ? C5 H5 0.9500 . ? C6 C7 1.386(3) . ? C6 H6 0.9500 . ? C7 C8 1.388(3) . ? C7 H7 0.9500 . ? C8 C9 1.393(2) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.489(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N6 1.328(2) . ? C11 N5 1.347(2) . ? C12 N4 1.336(2) . ? C12 N6 1.357(2) . ? C12 C13 1.470(2) . ? C13 C14 1.394(2) . ? C13 C18 1.401(2) . ? C14 C15 1.390(3) . ? C14 H14 0.9500 . ? C15 C16 1.387(3) . ? C15 H15 0.9500 . ? C16 C17 1.388(3) . ? C16 H16 0.9500 . ? C17 C18 1.387(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.488(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 N9 1.335(2) . ? C20 N8 1.340(2) . ? C21 N7 1.333(2) . ? C21 N9 1.353(2) . ? C21 C22 1.473(2) . ? C22 C27 1.395(3) . ? C22 C23 1.395(3) . ? C23 C24 1.392(3) . ? C23 H23 0.9500 . ? C24 C25 1.382(3) . ? C24 H24 0.9500 . ? C25 C26 1.384(3) . ? C25 H25 0.9500 . ? C26 C27 1.393(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? N1 N2 1.3785(19) . ? N1 Zn1 2.0407(14) . ? N4 N5 1.3790(19) . ? N4 Zn1 2.0317(14) . ? N7 N8 1.3786(19) . ? N7 Zn1 2.0875(14) . ? O1 C28B 1.342(13) . ? O1 C28 1.395(2) . ? O1 Zn1 1.8446(12) . ? C28 C29 1.490(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 F3 1.324(3) . ? C29 F2 1.339(3) . ? C29 F1 1.345(3) . ? C28B C29B 1.451(16) . ? C28B H28C 0.9900 . ? C28B H28D 0.9900 . ? C29B F3B 1.323(14) . ? C29B F2B 1.333(15) . ? C29B F1B 1.350(13) . ? 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 N8 B1 N5 107.36(14) . . ? N8 B1 N2 108.05(14) . . ? N5 B1 N2 109.63(14) . . ? N8 B1 H1 110.6 . . ? N5 B1 H1 110.6 . . ? N2 B1 H1 110.6 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N3 C2 N2 111.41(15) . . ? N3 C2 C1 124.18(16) . . ? N2 C2 C1 124.41(16) . . ? N1 C3 N3 113.23(15) . . ? N1 C3 C4 123.05(15) . . ? N3 C3 C4 123.71(15) . . ? C5 C4 C9 119.84(16) . . ? C5 C4 C3 119.51(15) . . ? C9 C4 C3 120.64(15) . . ? C6 C5 C4 120.07(16) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C7 C6 C5 120.11(17) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.04(17) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C7 C8 C9 120.20(17) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C9 C4 119.69(17) . . ? C8 C9 H9 120.2 . . ? C4 C9 H9 120.2 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N6 C11 N5 111.41(15) . . ? N6 C11 C10 125.21(16) . . ? N5 C11 C10 123.33(16) . . ? N4 C12 N6 112.88(15) . . ? N4 C12 C13 123.51(15) . . ? N6 C12 C13 123.59(16) . . ? C14 C13 C18 119.21(16) . . ? C14 C13 C12 119.21(16) . . ? C18 C13 C12 121.57(16) . . ? C15 C14 C13 120.12(17) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 120.46(17) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 119.67(17) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 120.35(17) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C13 120.17(17) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N9 C20 N8 110.97(15) . . ? N9 C20 C19 124.97(16) . . ? N8 C20 C19 124.04(16) . . ? N7 C21 N9 113.34(15) . . ? N7 C21 C22 124.87(16) . . ? N9 C21 C22 121.68(16) . . ? C27 C22 C23 119.68(17) . . ? C27 C22 C21 121.25(17) . . ? C23 C22 C21 119.02(17) . . ? C24 C23 C22 119.82(19) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C25 C24 C23 120.11(19) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.52(18) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C27 119.8(2) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C26 C27 C22 120.07(19) . . ? C26 C27 H27 120.0 . . ? C22 C27 H27 120.0 . . ? C3 N1 N2 104.58(13) . . ? C3 N1 Zn1 141.39(12) . . ? N2 N1 Zn1 111.89(10) . . ? C2 N2 N1 107.30(13) . . ? C2 N2 B1 131.88(14) . . ? N1 N2 B1 120.78(13) . . ? C2 N3 C3 103.43(14) . . ? C12 N4 N5 104.49(13) . . ? C12 N4 Zn1 142.71(12) . . ? N5 N4 Zn1 112.63(10) . . ? C11 N5 N4 107.31(14) . . ? C11 N5 B1 130.50(14) . . ? N4 N5 B1 121.49(13) . . ? C11 N6 C12 103.89(15) . . ? C21 N7 N8 103.96(13) . . ? C21 N7 Zn1 143.03(12) . . ? N8 N7 Zn1 111.88(10) . . ? C20 N8 N7 107.98(14) . . ? C20 N8 B1 130.87(14) . . ? N7 N8 B1 121.08(13) . . ? C20 N9 C21 103.75(15) . . ? C28B O1 Zn1 137.1(7) . . ? C28 O1 Zn1 125.73(12) . . ? O1 Zn1 N4 126.83(6) . . ? O1 Zn1 N1 126.51(6) . . ? N4 Zn1 N1 90.47(6) . . ? O1 Zn1 N7 117.10(6) . . ? N4 Zn1 N7 92.30(6) . . ? N1 Zn1 N7 94.59(6) . . ? O1 C28 C29 109.66(18) . . ? O1 C28 H28A 109.7 . . ? C29 C28 H28A 109.7 . . ? O1 C28 H28B 109.7 . . ? C29 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? F3 C29 F2 106.1(2) . . ? F3 C29 F1 106.8(2) . . ? F2 C29 F1 106.3(2) . . ? F3 C29 C28 113.6(2) . . ? F2 C29 C28 112.0(2) . . ? F1 C29 C28 111.6(2) . . ? O1 C28B C29B 106.8(12) . . ? O1 C28B H28C 110.4 . . ? C29B C28B H28C 110.4 . . ? O1 C28B H28D 110.4 . . ? C29B C28B H28D 110.4 . . ? H28C C28B H28D 108.6 . . ? F3B C29B F2B 107(2) . . ? F3B C29B F1B 101.3(14) . . ? F2B C29B F1B 100.6(16) . . ? F3B C29B C28B 121.8(14) . . ? F2B C29B C28B 115(2) . . ? F1B C29B C28B 107.7(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C3 C4 C5 -138.32(17) . . . . ? N3 C3 C4 C5 43.2(2) . . . . ? N1 C3 C4 C9 42.6(2) . . . . ? N3 C3 C4 C9 -135.83(18) . . . . ? C9 C4 C5 C6 -2.5(3) . . . . ? C3 C4 C5 C6 178.47(16) . . . . ? C4 C5 C6 C7 1.8(3) . . . . ? C5 C6 C7 C8 0.2(3) . . . . ? C6 C7 C8 C9 -1.6(3) . . . . ? C7 C8 C9 C4 0.9(3) . . . . ? C5 C4 C9 C8 1.2(3) . . . . ? C3 C4 C9 C8 -179.81(16) . . . . ? N4 C12 C13 C14 162.71(16) . . . . ? N6 C12 C13 C14 -15.2(2) . . . . ? N4 C12 C13 C18 -15.9(3) . . . . ? N6 C12 C13 C18 166.22(16) . . . . ? C18 C13 C14 C15 0.8(2) . . . . ? C12 C13 C14 C15 -177.87(16) . . . . ? C13 C14 C15 C16 -0.1(3) . . . . ? C14 C15 C16 C17 0.0(3) . . . . ? C15 C16 C17 C18 -0.6(3) . . . . ? C16 C17 C18 C13 1.3(3) . . . . ? C14 C13 C18 C17 -1.4(3) . . . . ? C12 C13 C18 C17 177.22(16) . . . . ? N7 C21 C22 C27 22.8(3) . . . . ? N9 C21 C22 C27 -153.14(18) . . . . ? N7 C21 C22 C23 -159.92(18) . . . . ? N9 C21 C22 C23 24.2(3) . . . . ? C27 C22 C23 C24 -1.0(3) . . . . ? C21 C22 C23 C24 -178.32(18) . . . . ? C22 C23 C24 C25 0.4(3) . . . . ? C23 C24 C25 C26 0.2(3) . . . . ? C24 C25 C26 C27 -0.4(3) . . . . ? C25 C26 C27 C22 -0.2(3) . . . . ? C23 C22 C27 C26 0.8(3) . . . . ? C21 C22 C27 C26 178.12(17) . . . . ? N3 C3 N1 N2 2.05(19) . . . . ? C4 C3 N1 N2 -176.57(15) . . . . ? N3 C3 N1 Zn1 -158.57(14) . . . . ? C4 C3 N1 Zn1 22.8(3) . . . . ? N3 C2 N2 N1 1.4(2) . . . . ? C1 C2 N2 N1 -178.26(16) . . . . ? N3 C2 N2 B1 -176.35(16) . . . . ? C1 C2 N2 B1 4.0(3) . . . . ? C3 N1 N2 C2 -2.02(18) . . . . ? Zn1 N1 N2 C2 165.09(11) . . . . ? C3 N1 N2 B1 176.01(15) . . . . ? Zn1 N1 N2 B1 -16.88(18) . . . . ? N8 B1 N2 C2 -111.5(2) . . . . ? N5 B1 N2 C2 131.80(18) . . . . ? N8 B1 N2 N1 71.03(18) . . . . ? N5 B1 N2 N1 -45.7(2) . . . . ? N2 C2 N3 C3 -0.15(19) . . . . ? C1 C2 N3 C3 179.50(17) . . . . ? N1 C3 N3 C2 -1.23(19) . . . . ? C4 C3 N3 C2 177.38(16) . . . . ? N6 C12 N4 N5 -0.38(18) . . . . ? C13 C12 N4 N5 -178.46(15) . . . . ? N6 C12 N4 Zn1 174.13(14) . . . . ? C13 C12 N4 Zn1 -4.0(3) . . . . ? N6 C11 N5 N4 -1.14(18) . . . . ? C10 C11 N5 N4 176.47(15) . . . . ? N6 C11 N5 B1 -171.45(16) . . . . ? C10 C11 N5 B1 6.2(3) . . . . ? C12 N4 N5 C11 0.89(17) . . . . ? Zn1 N4 N5 C11 -175.51(10) . . . . ? C12 N4 N5 B1 172.26(14) . . . . ? Zn1 N4 N5 B1 -4.14(18) . . . . ? N8 B1 N5 C11 111.56(18) . . . . ? N2 B1 N5 C11 -131.29(17) . . . . ? N8 B1 N5 N4 -57.57(19) . . . . ? N2 B1 N5 N4 59.57(19) . . . . ? N5 C11 N6 C12 0.87(18) . . . . ? C10 C11 N6 C12 -176.68(16) . . . . ? N4 C12 N6 C11 -0.28(19) . . . . ? C13 C12 N6 C11 177.80(15) . . . . ? N9 C21 N7 N8 0.4(2) . . . . ? C22 C21 N7 N8 -175.86(16) . . . . ? N9 C21 N7 Zn1 -165.26(15) . . . . ? C22 C21 N7 Zn1 18.5(3) . . . . ? N9 C20 N8 N7 0.5(2) . . . . ? C19 C20 N8 N7 179.17(18) . . . . ? N9 C20 N8 B1 177.48(17) . . . . ? C19 C20 N8 B1 -3.9(3) . . . . ? C21 N7 N8 C20 -0.51(18) . . . . ? Zn1 N7 N8 C20 170.22(12) . . . . ? C21 N7 N8 B1 -177.82(15) . . . . ? Zn1 N7 N8 B1 -7.09(18) . . . . ? N5 B1 N8 C20 -112.4(2) . . . . ? N2 B1 N8 C20 129.43(19) . . . . ? N5 B1 N8 N7 64.21(19) . . . . ? N2 B1 N8 N7 -53.96(19) . . . . ? N8 C20 N9 C21 -0.3(2) . . . . ? C19 C20 N9 C21 -178.92(19) . . . . ? N7 C21 N9 C20 -0.1(2) . . . . ? C22 C21 N9 C20 176.29(17) . . . . ? C28B O1 Zn1 N4 84.2(10) . . . . ? C28 O1 Zn1 N4 142.95(15) . . . . ? C28B O1 Zn1 N1 -40.4(10) . . . . ? C28 O1 Zn1 N1 18.41(18) . . . . ? C28B O1 Zn1 N7 -159.8(10) . . . . ? C28 O1 Zn1 N7 -100.97(16) . . . . ? C12 N4 Zn1 O1 1.0(2) . . . . ? N5 N4 Zn1 O1 175.26(9) . . . . ? C12 N4 Zn1 N1 139.56(19) . . . . ? N5 N4 Zn1 N1 -46.20(11) . . . . ? C12 N4 Zn1 N7 -125.83(19) . . . . ? N5 N4 Zn1 N7 48.41(11) . . . . ? C3 N1 Zn1 O1 -4.2(2) . . . . ? N2 N1 Zn1 O1 -163.91(10) . . . . ? C3 N1 Zn1 N4 -142.90(19) . . . . ? N2 N1 Zn1 N4 57.35(11) . . . . ? C3 N1 Zn1 N7 124.76(19) . . . . ? N2 N1 Zn1 N7 -35.00(11) . . . . ? C21 N7 Zn1 O1 -11.9(2) . . . . ? N8 N7 Zn1 O1 -176.87(10) . . . . ? C21 N7 Zn1 N4 122.1(2) . . . . ? N8 N7 Zn1 N4 -42.89(11) . . . . ? C21 N7 Zn1 N1 -147.3(2) . . . . ? N8 N7 Zn1 N1 47.77(11) . . . . ? C28B O1 C28 C29 -23.5(10) . . . . ? Zn1 O1 C28 C29 -147.23(15) . . . . ? O1 C28 C29 F3 -61.5(3) . . . . ? O1 C28 C29 F2 178.3(3) . . . . ? O1 C28 C29 F1 59.3(3) . . . . ? C28 O1 C28B C29B 23.1(7) . . . . ? Zn1 O1 C28B C29B 120.4(10) . . . . ? O1 C28B C29B F3B 57.4(18) . . . . ? O1 C28B C29B F2B -170(2) . . . . ? O1 C28B C29B F1B -58.6(17) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.750 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.065 data_09mz245_0m _database_code_depnum_ccdc_archive 'CCDC 764046' #TrackingRef '- combined cifs' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H30 B N9 O Zn' _chemical_formula_weight 644.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 16.954(2) _cell_length_b 11.5994(13) _cell_length_c 17.447(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.398(2) _cell_angle_gamma 90.00 _cell_volume 3073.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6394 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 30.64 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.843 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.597 _exptl_absorpt_correction_T_max 0.919 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 20094 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7588 _reflns_number_gt 5446 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4' _computing_data_reduction 'Apex2 v2008.2-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0557P)^2^+1.2563P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7588 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1207 _refine_ls_wR_factor_gt 0.1019 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 B1 B 0.22568(19) 0.6331(2) 0.90272(18) 0.0265(6) Uani 1 1 d . . . H1 H 0.2121 0.7105 0.9191 0.032 Uiso 1 1 calc R . . C1 C 0.3588(2) 0.7485(2) 1.07960(18) 0.0385(7) Uani 1 1 d . . . H1A H 0.3120 0.7422 1.0977 0.058 Uiso 1 1 calc R . . H1B H 0.3424 0.8062 1.0340 0.058 Uiso 1 1 calc R . . H1C H 0.4137 0.7720 1.1284 0.058 Uiso 1 1 calc R . . C2 C 0.37171(17) 0.6347(2) 1.04714(16) 0.0295(6) Uani 1 1 d . . . C3 C 0.42057(16) 0.4700(2) 1.03859(15) 0.0264(5) Uani 1 1 d . . . C4 C 0.47502(16) 0.3656(2) 1.06364(16) 0.0286(5) Uani 1 1 d . . . C5 C 0.53062(17) 0.3470(3) 1.15065(17) 0.0371(7) Uani 1 1 d . . . H5 H 0.5339 0.4027 1.1919 0.044 Uiso 1 1 calc R . . C6 C 0.58036(18) 0.2483(3) 1.17640(19) 0.0427(7) Uani 1 1 d . . . H6 H 0.6177 0.2362 1.2355 0.051 Uiso 1 1 calc R . . C7 C 0.57685(17) 0.1663(3) 1.1175(2) 0.0431(8) Uani 1 1 d . . . H7 H 0.6119 0.0987 1.1361 0.052 Uiso 1 1 calc R . . C8 C 0.52207(17) 0.1831(3) 1.03123(19) 0.0369(6) Uani 1 1 d . . . H8 H 0.5188 0.1265 0.9906 0.044 Uiso 1 1 calc R . . C9 C 0.47189(16) 0.2833(2) 1.00440(17) 0.0304(6) Uani 1 1 d . . . H9 H 0.4352 0.2955 0.9452 0.036 Uiso 1 1 calc R . . C10 C 0.17226(18) 0.8411(2) 0.76543(17) 0.0322(6) Uani 1 1 d . . . H10A H 0.1588 0.8868 0.7138 0.048 Uiso 1 1 calc R . . H10B H 0.2190 0.8792 0.8149 0.048 Uiso 1 1 calc R . . H10C H 0.1193 0.8344 0.7744 0.048 Uiso 1 1 calc R . . C11 C 0.20215(15) 0.7241(2) 0.75499(15) 0.0257(5) Uani 1 1 d . . . C12 C 0.24066(15) 0.5809(2) 0.70456(15) 0.0227(5) Uani 1 1 d . . . C13 C 0.26254(15) 0.5099(2) 0.64656(15) 0.0240(5) Uani 1 1 d . . . C14 C 0.21249(17) 0.5224(2) 0.55852(16) 0.0292(5) Uani 1 1 d . . . H14 H 0.1643 0.5746 0.5369 0.035 Uiso 1 1 calc R . . C15 C 0.23291(18) 0.4588(3) 0.50246(17) 0.0349(6) Uani 1 1 d . . . H15 H 0.1983 0.4670 0.4425 0.042 Uiso 1 1 calc R . . C16 C 0.30327(19) 0.3838(3) 0.53354(19) 0.0379(7) Uani 1 1 d . . . H16 H 0.3173 0.3407 0.4949 0.045 Uiso 1 1 calc R . . C17 C 0.35340(18) 0.3711(3) 0.62078(19) 0.0386(7) Uani 1 1 d . . . H17 H 0.4019 0.3194 0.6420 0.046 Uiso 1 1 calc R . . C18 C 0.33304(17) 0.4338(2) 0.67772(17) 0.0309(6) Uani 1 1 d . . . H18 H 0.3673 0.4245 0.7377 0.037 Uiso 1 1 calc R . . C19 C 0.06970(19) 0.6539(2) 0.95997(19) 0.0362(6) Uani 1 1 d . . . H19A H 0.0215 0.6368 0.9748 0.054 Uiso 1 1 calc R . . H19B H 0.0515 0.7154 0.9170 0.054 Uiso 1 1 calc R . . H19C H 0.1216 0.6790 1.0113 0.054 Uiso 1 1 calc R . . C20 C 0.09178(16) 0.5482(2) 0.92474(15) 0.0262(5) Uani 1 1 d . . . C21 C 0.09318(15) 0.3780(2) 0.88256(14) 0.0239(5) Uani 1 1 d . . . C22 C 0.06783(15) 0.2571(2) 0.85952(15) 0.0258(5) Uani 1 1 d . . . C23 C 0.02014(17) 0.1982(2) 0.89506(17) 0.0319(6) Uani 1 1 d . . . H23 H 0.0050 0.2363 0.9349 0.038 Uiso 1 1 calc R . . C24 C -0.00534(18) 0.0847(2) 0.8729(2) 0.0372(6) Uani 1 1 d . . . H24 H -0.0366 0.0449 0.8984 0.045 Uiso 1 1 calc R . . C25 C 0.01490(17) 0.0294(2) 0.81354(18) 0.0376(7) Uani 1 1 d . . . H25 H -0.0029 -0.0482 0.7978 0.045 Uiso 1 1 calc R . . C26 C 0.06107(19) 0.0875(2) 0.77733(18) 0.0367(6) Uani 1 1 d . . . H26 H 0.0745 0.0497 0.7363 0.044 Uiso 1 1 calc R . . C27 C 0.08788(17) 0.2001(2) 0.80032(16) 0.0309(6) Uani 1 1 d . . . H27 H 0.1202 0.2388 0.7755 0.037 Uiso 1 1 calc R . . C28 C 0.28337(17) 0.1975(2) 0.76511(16) 0.0281(5) Uani 1 1 d . . . C29 C 0.34302(19) 0.1117(2) 0.77001(18) 0.0356(6) Uani 1 1 d . . . H29 H 0.3933 0.0981 0.8229 0.043 Uiso 1 1 calc R . . C30 C 0.3304(2) 0.0461(3) 0.69941(19) 0.0439(7) Uani 1 1 d . . . H30 H 0.3714 -0.0127 0.7043 0.053 Uiso 1 1 calc R . . C31 C 0.2587(2) 0.0657(3) 0.6220(2) 0.0463(8) Uani 1 1 d . . . H31 H 0.2496 0.0200 0.5736 0.056 Uiso 1 1 calc R . . C32 C 0.1999(2) 0.1523(3) 0.61525(18) 0.0432(7) Uani 1 1 d . . . H32 H 0.1507 0.1666 0.5618 0.052 Uiso 1 1 calc R . . C33 C 0.21234(17) 0.2183(2) 0.68570(16) 0.0333(6) Uani 1 1 d . . . H33 H 0.1720 0.2785 0.6799 0.040 Uiso 1 1 calc R . . N1 N 0.34860(13) 0.48329(18) 0.96439(12) 0.0251(4) Uani 1 1 d . . . N2 N 0.31708(14) 0.59114(17) 0.97020(13) 0.0253(4) Uani 1 1 d . . . N3 N 0.43675(15) 0.5622(2) 1.09098(13) 0.0306(5) Uani 1 1 d . . . N4 N 0.24863(13) 0.54514(17) 0.78018(12) 0.0237(4) Uani 1 1 d . . . N5 N 0.22418(13) 0.63914(17) 0.81344(12) 0.0243(4) Uani 1 1 d . . . N6 N 0.21126(13) 0.69046(18) 0.68618(13) 0.0250(4) Uani 1 1 d . . . N7 N 0.15774(13) 0.43151(17) 0.87257(12) 0.0235(4) Uani 1 1 d . . . N8 N 0.15639(13) 0.54325(17) 0.89966(12) 0.0242(4) Uani 1 1 d . . . N9 N 0.05108(13) 0.44724(18) 0.91467(13) 0.0261(4) Uani 1 1 d . . . O1 O 0.29732(12) 0.25572(15) 0.83583(11) 0.0341(4) Uani 1 1 d . . . Zn1 Zn 0.267545(18) 0.40206(2) 0.852964(17) 0.02328(9) 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 B1 0.0387(15) 0.0200(14) 0.0270(14) -0.0040(11) 0.0202(12) 0.0011(11) C1 0.0534(17) 0.0345(16) 0.0330(14) -0.0126(12) 0.0242(13) -0.0104(13) C2 0.0389(13) 0.0304(14) 0.0250(12) -0.0032(10) 0.0195(11) -0.0109(11) C3 0.0305(12) 0.0309(14) 0.0212(11) 0.0023(10) 0.0144(10) -0.0072(10) C4 0.0262(11) 0.0316(14) 0.0269(12) 0.0052(10) 0.0108(10) -0.0079(10) C5 0.0328(13) 0.0445(17) 0.0291(13) 0.0051(12) 0.0093(11) -0.0115(12) C6 0.0288(13) 0.054(2) 0.0335(15) 0.0152(14) 0.0030(11) -0.0079(12) C7 0.0276(13) 0.0433(18) 0.0517(18) 0.0216(15) 0.0116(13) 0.0035(12) C8 0.0300(13) 0.0372(16) 0.0427(16) 0.0091(12) 0.0155(12) 0.0023(11) C9 0.0273(12) 0.0318(14) 0.0308(13) 0.0078(11) 0.0118(10) -0.0006(10) C10 0.0412(14) 0.0233(14) 0.0349(14) -0.0008(11) 0.0196(12) 0.0069(11) C11 0.0290(11) 0.0229(13) 0.0280(12) 0.0001(10) 0.0151(10) 0.0022(9) C12 0.0252(11) 0.0227(13) 0.0222(11) -0.0009(9) 0.0123(9) 0.0018(9) C13 0.0293(11) 0.0222(12) 0.0274(12) -0.0013(9) 0.0187(10) 0.0001(9) C14 0.0324(12) 0.0295(14) 0.0283(12) -0.0003(10) 0.0158(11) 0.0027(10) C15 0.0390(14) 0.0423(17) 0.0238(13) -0.0075(11) 0.0143(11) -0.0033(12) C16 0.0434(15) 0.0420(18) 0.0383(15) -0.0109(12) 0.0271(13) -0.0001(12) C17 0.0380(14) 0.0384(16) 0.0460(16) -0.0034(13) 0.0246(13) 0.0119(12) C18 0.0352(13) 0.0319(14) 0.0298(13) 0.0000(11) 0.0183(11) 0.0065(11) C19 0.0459(15) 0.0289(15) 0.0462(16) -0.0078(12) 0.0317(13) 0.0013(12) C20 0.0332(12) 0.0250(13) 0.0256(12) -0.0015(10) 0.0179(10) 0.0029(10) C21 0.0286(11) 0.0249(13) 0.0189(11) -0.0001(9) 0.0111(9) 0.0035(9) C22 0.0275(11) 0.0229(13) 0.0242(11) -0.0018(9) 0.0090(10) 0.0030(9) C23 0.0345(13) 0.0256(14) 0.0392(14) -0.0065(11) 0.0197(12) -0.0009(10) C24 0.0330(13) 0.0308(15) 0.0499(17) -0.0035(12) 0.0202(13) -0.0049(11) C25 0.0329(13) 0.0246(14) 0.0449(16) -0.0096(12) 0.0079(12) -0.0001(11) C26 0.0443(15) 0.0291(15) 0.0299(13) -0.0082(11) 0.0104(12) 0.0063(12) C27 0.0405(14) 0.0263(13) 0.0262(12) -0.0029(10) 0.0151(11) 0.0041(11) C28 0.0362(13) 0.0233(13) 0.0278(12) -0.0029(10) 0.0170(11) 0.0012(10) C29 0.0473(15) 0.0298(15) 0.0316(14) 0.0019(11) 0.0192(12) 0.0110(12) C30 0.0636(19) 0.0361(17) 0.0430(17) -0.0015(13) 0.0336(16) 0.0170(14) C31 0.0589(19) 0.0509(19) 0.0361(16) -0.0159(14) 0.0274(15) 0.0045(15) C32 0.0440(16) 0.060(2) 0.0274(14) -0.0096(13) 0.0170(13) 0.0000(14) C33 0.0347(13) 0.0385(16) 0.0298(13) -0.0027(11) 0.0171(11) 0.0086(11) N1 0.0321(10) 0.0232(11) 0.0224(10) -0.0012(8) 0.0144(8) -0.0003(8) N2 0.0360(11) 0.0204(10) 0.0241(10) -0.0045(8) 0.0176(9) -0.0030(8) N3 0.0395(12) 0.0325(12) 0.0227(10) -0.0021(9) 0.0164(9) -0.0116(9) N4 0.0326(10) 0.0187(10) 0.0243(10) -0.0021(8) 0.0168(9) 0.0036(8) N5 0.0328(10) 0.0193(10) 0.0257(10) -0.0018(8) 0.0175(9) 0.0045(8) N6 0.0282(10) 0.0233(11) 0.0257(10) 0.0012(8) 0.0139(8) 0.0030(8) N7 0.0321(10) 0.0195(10) 0.0211(10) -0.0042(7) 0.0137(8) 0.0025(8) N8 0.0335(10) 0.0195(10) 0.0241(10) -0.0031(8) 0.0168(9) 0.0026(8) N9 0.0327(10) 0.0233(11) 0.0267(10) -0.0016(8) 0.0170(9) 0.0026(8) O1 0.0458(10) 0.0278(10) 0.0241(9) -0.0029(7) 0.0114(8) 0.0111(8) Zn1 0.03073(15) 0.02047(15) 0.02001(14) -0.00120(11) 0.01252(11) 0.00449(11) _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 B1 N5 1.548(3) . ? B1 N2 1.550(4) . ? B1 N8 1.553(4) . ? B1 H1 1.0000 . ? C1 C2 1.491(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N3 1.326(4) . ? C2 N2 1.345(3) . ? C3 N1 1.336(3) . ? C3 N3 1.353(3) . ? C3 C4 1.466(4) . ? C4 C9 1.391(4) . ? C4 C5 1.403(3) . ? C5 C6 1.374(4) . ? C5 H5 0.9500 . ? C6 C7 1.381(5) . ? C6 H6 0.9500 . ? C7 C8 1.387(4) . ? C7 H7 0.9500 . ? C8 C9 1.393(4) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.488(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N6 1.335(3) . ? C11 N5 1.346(3) . ? C12 N4 1.331(3) . ? C12 N6 1.351(3) . ? C12 C13 1.474(3) . ? C13 C18 1.388(3) . ? C13 C14 1.393(3) . ? C14 C15 1.386(4) . ? C14 H14 0.9500 . ? C15 C16 1.378(4) . ? C15 H15 0.9500 . ? C16 C17 1.382(4) . ? C16 H16 0.9500 . ? C17 C18 1.393(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.492(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 N9 1.331(3) . ? C20 N8 1.349(3) . ? C21 N7 1.335(3) . ? C21 N9 1.350(3) . ? C21 C22 1.469(3) . ? C22 C27 1.390(3) . ? C22 C23 1.397(4) . ? C23 C24 1.386(4) . ? C23 H23 0.9500 . ? C24 C25 1.385(4) . ? C24 H24 0.9500 . ? C25 C26 1.380(4) . ? C25 H25 0.9500 . ? C26 C27 1.383(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 O1 1.332(3) . ? C28 C29 1.394(4) . ? C28 C33 1.394(4) . ? C29 C30 1.381(4) . ? C29 H29 0.9500 . ? C30 C31 1.376(4) . ? C30 H30 0.9500 . ? C31 C32 1.382(4) . ? C31 H31 0.9500 . ? C32 C33 1.383(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? N1 N2 1.382(3) . ? N1 Zn1 2.044(2) . ? N4 N5 1.383(3) . ? N4 Zn1 2.027(2) . ? N7 N8 1.383(3) . ? N7 Zn1 2.065(2) . ? O1 Zn1 1.8330(18) . ? 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 N5 B1 N2 110.0(2) . . ? N5 B1 N8 108.8(2) . . ? N2 B1 N8 107.5(2) . . ? N5 B1 H1 110.2 . . ? N2 B1 H1 110.2 . . ? N8 B1 H1 110.2 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N3 C2 N2 111.4(2) . . ? N3 C2 C1 124.6(2) . . ? N2 C2 C1 124.0(2) . . ? N1 C3 N3 112.8(2) . . ? N1 C3 C4 124.6(2) . . ? N3 C3 C4 122.6(2) . . ? C9 C4 C5 118.9(3) . . ? C9 C4 C3 122.3(2) . . ? C5 C4 C3 118.8(3) . . ? C6 C5 C4 120.1(3) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 120.9(3) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C6 C7 C8 119.8(3) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C7 C8 C9 119.7(3) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C4 C9 C8 120.5(2) . . ? C4 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N6 C11 N5 111.3(2) . . ? N6 C11 C10 124.0(2) . . ? N5 C11 C10 124.7(2) . . ? N4 C12 N6 113.1(2) . . ? N4 C12 C13 124.1(2) . . ? N6 C12 C13 122.8(2) . . ? C18 C13 C14 119.6(2) . . ? C18 C13 C12 121.5(2) . . ? C14 C13 C12 118.9(2) . . ? C15 C14 C13 120.1(2) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 120.2(2) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 120.1(3) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C18 120.2(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C13 C18 C17 119.7(2) . . ? C13 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N9 C20 N8 111.6(2) . . ? N9 C20 C19 124.6(2) . . ? N8 C20 C19 123.9(2) . . ? N7 C21 N9 113.1(2) . . ? N7 C21 C22 124.4(2) . . ? N9 C21 C22 122.5(2) . . ? C27 C22 C23 118.6(2) . . ? C27 C22 C21 121.3(2) . . ? C23 C22 C21 120.1(2) . . ? C24 C23 C22 120.8(3) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C25 C24 C23 119.9(3) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C26 C25 C24 119.7(3) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 120.6(3) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C22 120.5(3) . . ? C26 C27 H27 119.8 . . ? C22 C27 H27 119.8 . . ? O1 C28 C29 118.7(2) . . ? O1 C28 C33 123.5(2) . . ? C29 C28 C33 117.8(2) . . ? C30 C29 C28 121.2(3) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C31 C30 C29 120.2(3) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 119.5(3) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C31 C32 C33 120.5(3) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C32 C33 C28 120.7(3) . . ? C32 C33 H33 119.7 . . ? C28 C33 H33 119.7 . . ? C3 N1 N2 104.47(19) . . ? C3 N1 Zn1 143.76(18) . . ? N2 N1 Zn1 111.64(14) . . ? C2 N2 N1 107.2(2) . . ? C2 N2 B1 130.7(2) . . ? N1 N2 B1 121.15(19) . . ? C2 N3 C3 104.2(2) . . ? C12 N4 N5 104.67(19) . . ? C12 N4 Zn1 142.56(17) . . ? N5 N4 Zn1 112.10(15) . . ? C11 N5 N4 107.06(19) . . ? C11 N5 B1 132.1(2) . . ? N4 N5 B1 120.85(19) . . ? C11 N6 C12 103.9(2) . . ? C21 N7 N8 104.59(19) . . ? C21 N7 Zn1 142.77(17) . . ? N8 N7 Zn1 111.38(15) . . ? C20 N8 N7 106.9(2) . . ? C20 N8 B1 132.1(2) . . ? N7 N8 B1 120.9(2) . . ? C20 N9 C21 103.9(2) . . ? C28 O1 Zn1 132.22(16) . . ? O1 Zn1 N4 129.38(8) . . ? O1 Zn1 N1 117.67(8) . . ? N4 Zn1 N1 94.05(8) . . ? O1 Zn1 N7 120.93(9) . . ? N4 Zn1 N7 93.74(8) . . ? N1 Zn1 N7 92.33(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C3 C4 C9 18.4(4) . . . . ? N3 C3 C4 C9 -164.4(2) . . . . ? N1 C3 C4 C5 -160.0(2) . . . . ? N3 C3 C4 C5 17.1(4) . . . . ? C9 C4 C5 C6 -0.6(4) . . . . ? C3 C4 C5 C6 177.9(2) . . . . ? C4 C5 C6 C7 0.2(4) . . . . ? C5 C6 C7 C8 -0.4(4) . . . . ? C6 C7 C8 C9 0.9(4) . . . . ? C5 C4 C9 C8 1.1(4) . . . . ? C3 C4 C9 C8 -177.4(2) . . . . ? C7 C8 C9 C4 -1.2(4) . . . . ? N4 C12 C13 C18 -36.3(4) . . . . ? N6 C12 C13 C18 142.8(3) . . . . ? N4 C12 C13 C14 145.6(2) . . . . ? N6 C12 C13 C14 -35.3(3) . . . . ? C18 C13 C14 C15 0.2(4) . . . . ? C12 C13 C14 C15 178.4(2) . . . . ? C13 C14 C15 C16 -0.6(4) . . . . ? C14 C15 C16 C17 0.4(4) . . . . ? C15 C16 C17 C18 0.1(5) . . . . ? C14 C13 C18 C17 0.3(4) . . . . ? C12 C13 C18 C17 -177.8(3) . . . . ? C16 C17 C18 C13 -0.5(4) . . . . ? N7 C21 C22 C27 -21.9(3) . . . . ? N9 C21 C22 C27 156.5(2) . . . . ? N7 C21 C22 C23 160.2(2) . . . . ? N9 C21 C22 C23 -21.3(3) . . . . ? C27 C22 C23 C24 1.1(4) . . . . ? C21 C22 C23 C24 179.0(2) . . . . ? C22 C23 C24 C25 -1.4(4) . . . . ? C23 C24 C25 C26 0.6(4) . . . . ? C24 C25 C26 C27 0.5(4) . . . . ? C25 C26 C27 C22 -0.8(4) . . . . ? C23 C22 C27 C26 0.0(4) . . . . ? C21 C22 C27 C26 -177.9(2) . . . . ? O1 C28 C29 C30 177.9(3) . . . . ? C33 C28 C29 C30 -2.6(4) . . . . ? C28 C29 C30 C31 0.9(5) . . . . ? C29 C30 C31 C32 0.7(5) . . . . ? C30 C31 C32 C33 -0.6(5) . . . . ? C31 C32 C33 C28 -1.1(5) . . . . ? O1 C28 C33 C32 -177.9(3) . . . . ? C29 C28 C33 C32 2.7(4) . . . . ? N3 C3 N1 N2 0.0(3) . . . . ? C4 C3 N1 N2 177.4(2) . . . . ? N3 C3 N1 Zn1 -175.1(2) . . . . ? C4 C3 N1 Zn1 2.4(4) . . . . ? N3 C2 N2 N1 0.5(3) . . . . ? C1 C2 N2 N1 -177.8(2) . . . . ? N3 C2 N2 B1 169.4(2) . . . . ? C1 C2 N2 B1 -8.9(4) . . . . ? C3 N1 N2 C2 -0.3(3) . . . . ? Zn1 N1 N2 C2 176.57(16) . . . . ? C3 N1 N2 B1 -170.5(2) . . . . ? Zn1 N1 N2 B1 6.4(3) . . . . ? N5 B1 N2 C2 130.2(3) . . . . ? N8 B1 N2 C2 -111.5(3) . . . . ? N5 B1 N2 N1 -62.1(3) . . . . ? N8 B1 N2 N1 56.2(3) . . . . ? N2 C2 N3 C3 -0.5(3) . . . . ? C1 C2 N3 C3 177.8(2) . . . . ? N1 C3 N3 C2 0.3(3) . . . . ? C4 C3 N3 C2 -177.2(2) . . . . ? N6 C12 N4 N5 -1.2(3) . . . . ? C13 C12 N4 N5 178.0(2) . . . . ? N6 C12 N4 Zn1 167.82(19) . . . . ? C13 C12 N4 Zn1 -13.0(4) . . . . ? N6 C11 N5 N4 -0.2(3) . . . . ? C10 C11 N5 N4 -179.6(2) . . . . ? N6 C11 N5 B1 179.8(2) . . . . ? C10 C11 N5 B1 0.4(4) . . . . ? C12 N4 N5 C11 0.8(2) . . . . ? Zn1 N4 N5 C11 -171.99(15) . . . . ? C12 N4 N5 B1 -179.2(2) . . . . ? Zn1 N4 N5 B1 8.0(3) . . . . ? N2 B1 N5 C11 -127.3(3) . . . . ? N8 B1 N5 C11 115.1(3) . . . . ? N2 B1 N5 N4 52.7(3) . . . . ? N8 B1 N5 N4 -64.9(3) . . . . ? N5 C11 N6 C12 -0.5(3) . . . . ? C10 C11 N6 C12 179.0(2) . . . . ? N4 C12 N6 C11 1.0(3) . . . . ? C13 C12 N6 C11 -178.2(2) . . . . ? N9 C21 N7 N8 -0.5(3) . . . . ? C22 C21 N7 N8 178.1(2) . . . . ? N9 C21 N7 Zn1 164.39(19) . . . . ? C22 C21 N7 Zn1 -17.0(4) . . . . ? N9 C20 N8 N7 -0.6(3) . . . . ? C19 C20 N8 N7 178.9(2) . . . . ? N9 C20 N8 B1 -176.1(2) . . . . ? C19 C20 N8 B1 3.4(4) . . . . ? C21 N7 N8 C20 0.6(2) . . . . ? Zn1 N7 N8 C20 -169.58(15) . . . . ? C21 N7 N8 B1 176.7(2) . . . . ? Zn1 N7 N8 B1 6.5(2) . . . . ? N5 B1 N8 C20 -130.5(3) . . . . ? N2 B1 N8 C20 110.4(3) . . . . ? N5 B1 N8 N7 54.6(3) . . . . ? N2 B1 N8 N7 -64.5(3) . . . . ? N8 C20 N9 C21 0.3(3) . . . . ? C19 C20 N9 C21 -179.2(2) . . . . ? N7 C21 N9 C20 0.1(3) . . . . ? C22 C21 N9 C20 -178.5(2) . . . . ? C29 C28 O1 Zn1 152.0(2) . . . . ? C33 C28 O1 Zn1 -27.5(4) . . . . ? C28 O1 Zn1 N4 -28.1(3) . . . . ? C28 O1 Zn1 N1 -150.3(2) . . . . ? C28 O1 Zn1 N7 98.1(2) . . . . ? C12 N4 Zn1 O1 9.8(3) . . . . ? N5 N4 Zn1 O1 178.25(14) . . . . ? C12 N4 Zn1 N1 141.1(3) . . . . ? N5 N4 Zn1 N1 -50.41(16) . . . . ? C12 N4 Zn1 N7 -126.3(3) . . . . ? N5 N4 Zn1 N7 42.19(15) . . . . ? C3 N1 Zn1 O1 -3.3(3) . . . . ? N2 N1 Zn1 O1 -178.12(14) . . . . ? C3 N1 Zn1 N4 -142.3(3) . . . . ? N2 N1 Zn1 N4 42.83(16) . . . . ? C3 N1 Zn1 N7 123.8(3) . . . . ? N2 N1 Zn1 N7 -51.09(16) . . . . ? C21 N7 Zn1 O1 4.6(3) . . . . ? N8 N7 Zn1 O1 168.84(13) . . . . ? C21 N7 Zn1 N4 145.9(3) . . . . ? N8 N7 Zn1 N4 -49.86(15) . . . . ? C21 N7 Zn1 N1 -119.9(3) . . . . ? N8 N7 Zn1 N1 44.35(15) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.880 _refine_diff_density_min -0.805 _refine_diff_density_rms 0.081 data_09mz359_0m _database_code_depnum_ccdc_archive 'CCDC 764047' #TrackingRef '- combined cifs' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H30 B N9 S Zn' _chemical_formula_sum 'C33 H30 B N9 S Zn' _chemical_formula_weight 660.93 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' 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.842(3) _cell_length_b 15.757(4) _cell_length_c 17.293(5) _cell_angle_alpha 72.951(4) _cell_angle_beta 89.883(4) _cell_angle_gamma 89.978(4) _cell_volume 3085.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4181 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.45 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 0.904 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6416 _exptl_absorpt_correction_T_max 0.7464 _exptl_absorpt_process_details 'Apex2 v2009.7-0 (Bruker, 2009)' _exptl_special_details ; The structure at hand exhibits pseudo-monoclinic symmetry and the crystal at hand was found to be twinned by this symmetry. The structure as presented was refined under application of the twin law 1 0 0, 0 -1 0, 0 0 -1 and the twin ratio refined to 0.4944(9) vs 0.4056(9). The pseudo-symmetry is both metric with two unit cell angles very close to 90 degrees, as well as internal. The two crystallographically independent molecules are related by a pseudo glide plane (in the current setting an n-glide plane through 0.252 0 0 and 9 0.5 0.5) which would converts the space group into P21/n after resorting of the cell axes. The maximum deviation for non-fitting atoms for this pseudo glide plane is above 0.35 Angstrom, but below 0.45 Angstrom. Systematic absences for the glide plane (and the associated 21 screw axis) are clearly not obeyed. Attempts to refine the structure in a monoclinic setting in P21/n results in disorder of two of the phenyl rings in the then single independent molecule, but even under consideration of the disorder R values are persistently high with R1 being ca 13-14%. Thermal parameters of the disordered atoms are not clearly defined with some being non-positive definite and residual electron densities are high. ; _diffrn_ambient_temperature 100(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 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 30509 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 28.28 _reflns_number_total 15017 _reflns_number_gt 11797 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2009.7-0 (Bruker, 2009)' _computing_cell_refinement 'Apex2 v2009.7-0' _computing_data_reduction 'Apex2 v2009.7-0' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0394P)^2^+2.5619P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15017 _refine_ls_number_parameters 818 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.2863(4) 0.0724(3) 0.8921(2) 0.0185(9) Uani 1 1 d . . . H1 H 0.3066 0.0405 0.8519 0.022 Uiso 1 1 calc R . . B2 B 0.7869(5) 0.4189(3) 0.6051(2) 0.0198(9) Uani 1 1 d . . . H2 H 0.8089 0.4459 0.6485 0.024 Uiso 1 1 calc R . . C1 C 0.2596(4) 0.1749(3) 0.7032(2) 0.0268(9) Uani 1 1 d . . . H1A H 0.2122 0.1246 0.7011 0.040 Uiso 1 1 calc R . . H1B H 0.3385 0.1557 0.7114 0.040 Uiso 1 1 calc R . . H1C H 0.2527 0.2226 0.6522 0.040 Uiso 1 1 calc R . . C2 C 0.2220(4) 0.2080(2) 0.7715(2) 0.0201(7) Uani 1 1 d . . . C3 C 0.1523(3) 0.2862(2) 0.8411(2) 0.0202(8) Uani 1 1 d . . . C4 C 0.0998(4) 0.3614(3) 0.8614(2) 0.0308(10) Uani 1 1 d . . . C5 C 0.1415(5) 0.4466(3) 0.8210(3) 0.0460(14) Uani 1 1 d . . . H5 H 0.2007 0.4530 0.7825 0.055 Uiso 1 1 calc R . . C6 C 0.0979(6) 0.5194(4) 0.8366(3) 0.068(2) Uani 1 1 d . . . H6 H 0.1280 0.5766 0.8109 0.082 Uiso 1 1 calc R . . C7 C 0.0089(7) 0.5091(5) 0.8907(4) 0.079(3) Uani 1 1 d . . . H7 H -0.0240 0.5603 0.8998 0.095 Uiso 1 1 calc R . . C8 C -0.0339(5) 0.4255(5) 0.9322(4) 0.072(2) Uani 1 1 d . . . H8 H -0.0937 0.4199 0.9701 0.086 Uiso 1 1 calc R . . C9 C 0.0129(4) 0.3492(4) 0.9172(3) 0.0461(13) Uani 1 1 d . . . H9 H -0.0144 0.2915 0.9445 0.055 Uiso 1 1 calc R . . C10 C 0.1471(4) -0.1004(3) 0.8931(2) 0.0277(9) Uani 1 1 d . . . H10A H 0.1119 -0.0571 0.8468 0.042 Uiso 1 1 calc R . . H10B H 0.1016 -0.1547 0.9088 0.042 Uiso 1 1 calc R . . H10C H 0.2233 -0.1144 0.8782 0.042 Uiso 1 1 calc R . . C11 C 0.1541(4) -0.0624(2) 0.9619(2) 0.0206(8) Uani 1 1 d . . . C12 C 0.1306(3) -0.0387(2) 1.0749(2) 0.0182(8) Uani 1 1 d . . . C13 C 0.1051(3) -0.0587(2) 1.1627(2) 0.0185(8) Uani 1 1 d . . . C14 C 0.0481(4) -0.1369(3) 1.2004(2) 0.0230(9) Uani 1 1 d . . . H14 H 0.0200 -0.1725 1.1689 0.028 Uiso 1 1 calc R . . C15 C 0.0317(4) -0.1636(3) 1.2837(2) 0.0221(8) Uani 1 1 d . . . H15 H -0.0063 -0.2178 1.3090 0.027 Uiso 1 1 calc R . . C16 C 0.0703(3) -0.1116(3) 1.3295(2) 0.0221(8) Uani 1 1 d . . . H16 H 0.0590 -0.1297 1.3864 0.027 Uiso 1 1 calc R . . C17 C 0.1257(3) -0.0329(2) 1.2923(2) 0.0252(8) Uani 1 1 d . . . H17 H 0.1513 0.0036 1.3238 0.030 Uiso 1 1 calc R . . C18 C 0.1442(3) -0.0067(2) 1.2090(2) 0.0228(8) Uani 1 1 d . . . H18 H 0.1836 0.0469 1.1841 0.027 Uiso 1 1 calc R . . C19 C 0.5447(4) 0.0360(3) 0.8603(2) 0.0250(9) Uani 1 1 d . . . H19A H 0.5507 0.0766 0.8053 0.037 Uiso 1 1 calc R . . H19B H 0.4914 -0.0117 0.8607 0.037 Uiso 1 1 calc R . . H19C H 0.6191 0.0105 0.8782 0.037 Uiso 1 1 calc R . . C20 C 0.5039(4) 0.0855(2) 0.9158(2) 0.0197(8) Uani 1 1 d . . . C21 C 0.4969(3) 0.1625(2) 0.9969(2) 0.0191(8) Uani 1 1 d . . . C22 C 0.5349(4) 0.2133(3) 1.0510(2) 0.0229(9) Uani 1 1 d . . . C23 C 0.6366(4) 0.2587(3) 1.0331(3) 0.0353(11) Uani 1 1 d . . . H23 H 0.6779 0.2577 0.9863 0.042 Uiso 1 1 calc R . . C24 C 0.6778(5) 0.3054(3) 1.0831(3) 0.0415(12) Uani 1 1 d . . . H24 H 0.7473 0.3366 1.0708 0.050 Uiso 1 1 calc R . . C25 C 0.6173(5) 0.3068(3) 1.1516(3) 0.0411(13) Uani 1 1 d . . . H25 H 0.6457 0.3391 1.1859 0.049 Uiso 1 1 calc R . . C26 C 0.5153(4) 0.2613(3) 1.1705(3) 0.0362(11) Uani 1 1 d . . . H26 H 0.4741 0.2625 1.2173 0.043 Uiso 1 1 calc R . . C27 C 0.4743(4) 0.2139(3) 1.1198(2) 0.0300(10) Uani 1 1 d . . . H27 H 0.4053 0.1821 1.1322 0.036 Uiso 1 1 calc R . . C28 C 0.2339(4) 0.3274(2) 1.0902(2) 0.0223(8) Uani 1 1 d . . . C29 C 0.2854(4) 0.3709(2) 1.0163(2) 0.0261(9) Uani 1 1 d . . . H29 H 0.2812 0.3456 0.9728 0.031 Uiso 1 1 calc R . . C30 C 0.3428(4) 0.4506(3) 1.0058(2) 0.0310(10) Uani 1 1 d . . . H30 H 0.3773 0.4795 0.9553 0.037 Uiso 1 1 calc R . . C31 C 0.3497(4) 0.4874(3) 1.0689(3) 0.0360(11) Uani 1 1 d . . . H31 H 0.3887 0.5418 1.0620 0.043 Uiso 1 1 calc R . . C32 C 0.2997(5) 0.4450(3) 1.1415(3) 0.0390(12) Uani 1 1 d . . . H32 H 0.3046 0.4704 1.1849 0.047 Uiso 1 1 calc R . . C33 C 0.2422(4) 0.3658(3) 1.1527(2) 0.0301(10) Uani 1 1 d . . . H33 H 0.2083 0.3375 1.2035 0.036 Uiso 1 1 calc R . . C34 C 0.6804(4) 0.6014(3) 0.6096(2) 0.0295(10) Uani 1 1 d . . . H34A H 0.7604 0.6139 0.6158 0.044 Uiso 1 1 calc R . . H34B H 0.6522 0.5599 0.6599 0.044 Uiso 1 1 calc R . . H34C H 0.6372 0.6568 0.5974 0.044 Uiso 1 1 calc R . . C35 C 0.6674(4) 0.5611(2) 0.5422(2) 0.0205(8) Uani 1 1 d . . . C36 C 0.6263(3) 0.5407(2) 0.4306(2) 0.0186(8) Uani 1 1 d . . . C37 C 0.5886(4) 0.5607(3) 0.3468(2) 0.0197(8) Uani 1 1 d . . . C38 C 0.5600(4) 0.6476(2) 0.3054(2) 0.0222(8) Uani 1 1 d . . . H38 H 0.5590 0.6911 0.3335 0.027 Uiso 1 1 calc R . . C39 C 0.5332(4) 0.6719(3) 0.2245(2) 0.0255(9) Uani 1 1 d . . . H39 H 0.5161 0.7321 0.1970 0.031 Uiso 1 1 calc R . . C40 C 0.5311(4) 0.6093(3) 0.1835(3) 0.0340(10) Uani 1 1 d . . . H40 H 0.5160 0.6260 0.1271 0.041 Uiso 1 1 calc R . . C41 C 0.5512(5) 0.5216(3) 0.2255(3) 0.0528(15) Uani 1 1 d . . . H41 H 0.5457 0.4773 0.1985 0.063 Uiso 1 1 calc R . . C42 C 0.5793(5) 0.4980(3) 0.3062(3) 0.0456(13) Uani 1 1 d . . . H42 H 0.5924 0.4373 0.3343 0.055 Uiso 1 1 calc R . . C43 C 1.0455(4) 0.4492(3) 0.6349(2) 0.0230(9) Uani 1 1 d . . . H43A H 1.0250 0.4143 0.6900 0.034 Uiso 1 1 calc R . . H43B H 1.0116 0.5084 0.6229 0.034 Uiso 1 1 calc R . . H43C H 1.1278 0.4548 0.6304 0.034 Uiso 1 1 calc R . . C44 C 1.0032(3) 0.4041(2) 0.5767(2) 0.0181(8) Uani 1 1 d . . . C45 C 0.9915(3) 0.3329(2) 0.4911(2) 0.0191(8) Uani 1 1 d . . . C46 C 1.0257(4) 0.2848(3) 0.4330(2) 0.0228(9) Uani 1 1 d . . . C47 C 1.1137(4) 0.2232(3) 0.4536(2) 0.0278(9) Uani 1 1 d . . . H47 H 1.1511 0.2128 0.5041 0.033 Uiso 1 1 calc R . . C48 C 1.1462(4) 0.1774(3) 0.3998(2) 0.0315(10) Uani 1 1 d . . . H48 H 1.2039 0.1338 0.4146 0.038 Uiso 1 1 calc R . . C49 C 1.0959(4) 0.1946(3) 0.3258(2) 0.0338(11) Uani 1 1 d . . . H49 H 1.1200 0.1640 0.2889 0.041 Uiso 1 1 calc R . . C50 C 1.0106(4) 0.2560(3) 0.3049(2) 0.0312(10) Uani 1 1 d . . . H50 H 0.9754 0.2676 0.2536 0.037 Uiso 1 1 calc R . . C51 C 0.9754(4) 0.3014(3) 0.3588(2) 0.0279(9) Uani 1 1 d . . . H51 H 0.9164 0.3439 0.3440 0.033 Uiso 1 1 calc R . . C52 C 0.7581(4) 0.2982(2) 0.7902(2) 0.0241(9) Uani 1 1 d . . . H52A H 0.7174 0.3499 0.7966 0.036 Uiso 1 1 calc R . . H52B H 0.8389 0.3118 0.7833 0.036 Uiso 1 1 calc R . . H52C H 0.7465 0.2475 0.8384 0.036 Uiso 1 1 calc R . . C53 C 0.7149(4) 0.2760(2) 0.71804(19) 0.0185(7) Uani 1 1 d . . . C54 C 0.6357(3) 0.2115(2) 0.6425(2) 0.0203(8) Uani 1 1 d . . . C55 C 0.5676(4) 0.1481(2) 0.6153(2) 0.0208(8) Uani 1 1 d . . . C56 C 0.5751(3) 0.0578(2) 0.6538(2) 0.0244(8) Uani 1 1 d . . . H56 H 0.6276 0.0367 0.6966 0.029 Uiso 1 1 calc R . . C57 C 0.5075(4) -0.0018(3) 0.6307(3) 0.0347(11) Uani 1 1 d . . . H57 H 0.5135 -0.0636 0.6572 0.042 Uiso 1 1 calc R . . C58 C 0.4311(4) 0.0295(3) 0.5689(3) 0.0365(10) Uani 1 1 d . . . H58 H 0.3835 -0.0109 0.5530 0.044 Uiso 1 1 calc R . . C59 C 0.4234(4) 0.1194(3) 0.5299(3) 0.0350(10) Uani 1 1 d . . . H59 H 0.3713 0.1404 0.4868 0.042 Uiso 1 1 calc R . . C60 C 0.4916(4) 0.1793(3) 0.5533(2) 0.0274(9) Uani 1 1 d . . . H60 H 0.4857 0.2411 0.5268 0.033 Uiso 1 1 calc R . . C61 C 0.7434(4) 0.1794(2) 0.3926(2) 0.0235(9) Uani 1 1 d . . . C62 C 0.7563(4) 0.1434(3) 0.3290(2) 0.0307(11) Uani 1 1 d . . . H62 H 0.7242 0.1729 0.2778 0.037 Uiso 1 1 calc R . . C63 C 0.8150(4) 0.0655(3) 0.3388(2) 0.0311(11) Uani 1 1 d . . . H63 H 0.8222 0.0413 0.2948 0.037 Uiso 1 1 calc R . . C64 C 0.8633(4) 0.0223(3) 0.4125(2) 0.0286(10) Uani 1 1 d . . . H64 H 0.9051 -0.0308 0.4193 0.034 Uiso 1 1 calc R . . C65 C 0.8499(4) 0.0578(3) 0.4761(2) 0.0268(9) Uani 1 1 d . . . H65 H 0.8821 0.0281 0.5271 0.032 Uiso 1 1 calc R . . C66 C 0.7905(4) 0.1357(2) 0.4670(2) 0.0221(8) Uani 1 1 d . . . H66 H 0.7821 0.1591 0.5115 0.027 Uiso 1 1 calc R . . N1 N 0.1841(3) 0.21090(19) 0.89579(17) 0.0176(7) Uani 1 1 d . . . N2 N 0.2287(3) 0.16049(19) 0.84976(16) 0.0180(6) Uani 1 1 d . . . N3 N 0.1740(3) 0.2864(2) 0.76414(18) 0.0227(7) Uani 1 1 d . . . N4 N 0.1895(3) 0.0319(2) 1.03075(17) 0.0178(7) Uani 1 1 d . . . N5 N 0.2063(3) 0.01446(19) 0.95741(16) 0.0181(7) Uani 1 1 d . . . N6 N 0.1068(3) -0.0974(2) 1.03391(19) 0.0222(8) Uani 1 1 d . . . N7 N 0.3887(3) 0.1464(2) 0.98489(17) 0.0170(7) Uani 1 1 d . . . N8 N 0.3940(3) 0.0951(2) 0.93227(17) 0.0180(7) Uani 1 1 d . . . N9 N 0.5698(3) 0.1266(2) 0.95473(19) 0.0224(7) Uani 1 1 d . . . N10 N 0.6818(3) 0.4673(2) 0.47050(17) 0.0181(7) Uani 1 1 d . . . N11 N 0.7092(3) 0.48182(18) 0.54334(16) 0.0164(6) Uani 1 1 d . . . N12 N 0.6145(3) 0.5993(2) 0.47326(19) 0.0216(7) Uani 1 1 d . . . N13 N 0.8857(3) 0.3523(2) 0.50486(17) 0.0190(7) Uani 1 1 d . . . N14 N 0.8932(3) 0.3983(2) 0.56125(17) 0.0171(7) Uani 1 1 d . . . N15 N 1.0673(3) 0.3639(2) 0.53443(18) 0.0197(7) Uani 1 1 d . . . N16 N 0.6746(3) 0.28742(19) 0.59195(17) 0.0182(7) Uani 1 1 d . . . N17 N 0.7246(3) 0.32921(19) 0.64217(16) 0.0176(6) Uani 1 1 d . . . N18 N 0.6605(3) 0.20179(19) 0.72045(18) 0.0197(7) Uani 1 1 d . . . S1 S 0.15841(10) 0.22695(7) 1.10826(6) 0.0281(2) Uani 1 1 d . . . S2 S 0.66871(11) 0.28152(7) 0.37464(6) 0.0296(3) Uani 1 1 d . . . Zn1 Zn 0.22323(4) 0.16491(3) 1.01652(2) 0.01897(10) Uani 1 1 d . . . Zn2 Zn 0.72009(4) 0.33885(3) 0.47211(2) 0.01777(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.024(2) 0.0135(18) 0.0163(17) -0.0019(14) -0.0038(19) 0.0038(19) B2 0.029(3) 0.0152(19) 0.0158(18) -0.0054(15) -0.0009(19) 0.0013(19) C1 0.032(2) 0.030(2) 0.0155(16) -0.0039(15) 0.0006(15) 0.0068(17) C2 0.0181(18) 0.0235(18) 0.0160(15) -0.0015(13) -0.0007(16) -0.0001(16) C3 0.0184(19) 0.0159(17) 0.0253(19) -0.0044(14) -0.0060(15) 0.0026(15) C4 0.039(3) 0.027(2) 0.029(2) -0.0116(18) -0.0207(19) 0.0140(19) C5 0.088(4) 0.022(2) 0.029(2) -0.0104(18) -0.028(2) 0.015(2) C6 0.116(6) 0.040(3) 0.054(3) -0.024(3) -0.048(4) 0.033(3) C7 0.109(6) 0.058(4) 0.087(5) -0.046(4) -0.059(5) 0.058(4) C8 0.057(4) 0.107(6) 0.072(4) -0.060(4) -0.027(3) 0.041(4) C9 0.037(3) 0.063(3) 0.051(3) -0.036(3) -0.013(2) 0.015(3) C10 0.038(3) 0.024(2) 0.0227(19) -0.0108(16) 0.0030(17) -0.0070(18) C11 0.027(2) 0.0162(18) 0.0189(18) -0.0053(14) -0.0051(16) 0.0013(16) C12 0.021(2) 0.0162(18) 0.0179(17) -0.0055(14) -0.0012(15) -0.0009(16) C13 0.022(2) 0.0150(17) 0.0150(17) 0.0003(14) 0.0007(15) 0.0030(15) C14 0.025(2) 0.022(2) 0.0224(19) -0.0071(15) -0.0026(16) -0.0006(16) C15 0.021(2) 0.023(2) 0.0185(18) -0.0004(15) 0.0019(15) -0.0024(16) C16 0.025(2) 0.0239(19) 0.0161(17) -0.0042(15) 0.0017(15) 0.0035(16) C17 0.034(2) 0.0205(18) 0.0203(18) -0.0051(15) -0.0025(16) -0.0009(17) C18 0.029(2) 0.0163(17) 0.0214(18) -0.0029(14) -0.0003(15) -0.0042(15) C19 0.028(2) 0.0188(19) 0.023(2) 0.0009(15) 0.0057(17) 0.0003(17) C20 0.025(2) 0.0143(18) 0.0153(17) 0.0024(14) -0.0018(15) -0.0003(15) C21 0.022(2) 0.0154(18) 0.0159(17) 0.0012(14) -0.0028(15) -0.0004(16) C22 0.029(2) 0.0164(18) 0.0210(18) -0.0011(14) -0.0088(16) 0.0056(16) C23 0.045(3) 0.027(2) 0.031(2) -0.0021(17) -0.013(2) -0.009(2) C24 0.055(3) 0.028(2) 0.037(2) -0.0019(19) -0.014(2) -0.012(2) C25 0.060(4) 0.023(2) 0.042(3) -0.010(2) -0.029(2) 0.003(2) C26 0.044(3) 0.037(2) 0.031(2) -0.0148(19) -0.010(2) 0.013(2) C27 0.032(2) 0.029(2) 0.032(2) -0.0135(18) -0.0102(19) 0.0027(19) C28 0.026(2) 0.0181(17) 0.0239(18) -0.0070(14) -0.0016(16) 0.0008(16) C29 0.031(2) 0.0226(18) 0.0246(18) -0.0067(15) -0.0092(19) 0.0014(19) C30 0.038(3) 0.022(2) 0.029(2) -0.0012(16) -0.0010(19) -0.0084(19) C31 0.045(3) 0.022(2) 0.040(2) -0.0085(18) -0.006(2) -0.007(2) C32 0.059(4) 0.029(2) 0.033(2) -0.0155(18) -0.003(2) -0.005(2) C33 0.033(3) 0.028(2) 0.032(2) -0.0134(17) 0.0059(18) -0.0034(18) C34 0.042(3) 0.024(2) 0.026(2) -0.0128(16) 0.0006(18) 0.0063(18) C35 0.024(2) 0.0161(18) 0.0200(18) -0.0027(14) 0.0033(16) -0.0013(16) C36 0.018(2) 0.0156(18) 0.0198(18) -0.0012(14) 0.0017(15) -0.0003(15) C37 0.021(2) 0.0181(19) 0.0197(18) -0.0051(15) 0.0021(15) 0.0011(15) C38 0.026(2) 0.0159(18) 0.0229(19) -0.0028(15) -0.0003(16) 0.0032(16) C39 0.027(2) 0.0190(19) 0.025(2) 0.0016(15) -0.0012(17) 0.0033(17) C40 0.045(3) 0.032(2) 0.024(2) -0.0075(18) -0.0109(19) 0.008(2) C41 0.089(4) 0.035(3) 0.042(3) -0.023(2) -0.032(3) 0.025(3) C42 0.078(4) 0.022(2) 0.037(2) -0.0071(18) -0.030(3) 0.020(2) C43 0.025(2) 0.0183(18) 0.0224(19) -0.0009(15) -0.0048(16) -0.0018(16) C44 0.021(2) 0.0140(17) 0.0166(17) -0.0003(14) -0.0005(15) -0.0001(15) C45 0.023(2) 0.0134(17) 0.0146(17) 0.0052(13) 0.0006(15) 0.0007(16) C46 0.026(2) 0.0187(19) 0.0202(19) -0.0006(15) 0.0035(16) -0.0009(16) C47 0.031(2) 0.0211(19) 0.029(2) -0.0022(16) -0.0008(17) 0.0025(17) C48 0.039(3) 0.024(2) 0.031(2) -0.0073(17) 0.0012(19) 0.0095(19) C49 0.051(3) 0.023(2) 0.026(2) -0.0063(17) 0.008(2) 0.005(2) C50 0.047(3) 0.027(2) 0.0177(19) -0.0028(16) 0.0035(18) 0.0074(19) C51 0.034(2) 0.026(2) 0.0207(19) -0.0029(16) 0.0043(17) 0.0030(18) C52 0.034(2) 0.0214(18) 0.0162(16) -0.0048(14) -0.0038(15) 0.0010(16) C53 0.025(2) 0.0155(16) 0.0150(15) -0.0037(12) -0.0014(16) 0.0024(16) C54 0.022(2) 0.0178(18) 0.0213(18) -0.0067(14) 0.0012(15) 0.0030(15) C55 0.028(2) 0.0130(16) 0.0226(19) -0.0075(14) 0.0072(16) -0.0028(15) C56 0.026(2) 0.0210(18) 0.027(2) -0.0086(16) 0.0056(16) -0.0055(16) C57 0.047(3) 0.0170(19) 0.040(2) -0.0092(18) 0.007(2) -0.0087(19) C58 0.035(2) 0.034(2) 0.050(3) -0.027(2) 0.008(2) -0.014(2) C59 0.028(2) 0.036(2) 0.047(3) -0.022(2) -0.0062(19) -0.0022(18) C60 0.028(2) 0.0214(19) 0.034(2) -0.0088(17) -0.0016(18) -0.0035(16) C61 0.035(3) 0.0154(17) 0.0208(17) -0.0055(14) -0.0046(16) 0.0007(16) C62 0.052(3) 0.0227(19) 0.0172(17) -0.0062(15) -0.0036(18) 0.0028(19) C63 0.058(3) 0.0181(19) 0.0200(19) -0.0098(15) 0.0040(19) 0.0000(19) C64 0.037(3) 0.0195(19) 0.030(2) -0.0091(16) 0.0038(19) 0.0051(18) C65 0.032(2) 0.0213(19) 0.024(2) -0.0025(16) -0.0066(17) 0.0042(18) C66 0.028(2) 0.0181(17) 0.0206(17) -0.0067(14) -0.0027(17) 0.0016(17) N1 0.0205(17) 0.0154(15) 0.0183(14) -0.0069(12) -0.0020(12) 0.0005(12) N2 0.0202(16) 0.0188(14) 0.0157(13) -0.0063(11) 0.0003(13) 0.0031(14) N3 0.0280(18) 0.0186(16) 0.0202(15) -0.0038(12) -0.0015(14) -0.0025(14) N4 0.0217(18) 0.0170(15) 0.0143(14) -0.0040(11) -0.0004(12) -0.0009(13) N5 0.026(2) 0.0130(14) 0.0141(13) -0.0027(11) -0.0006(13) 0.0012(14) N6 0.030(2) 0.0175(17) 0.0170(15) -0.0019(13) -0.0015(14) -0.0029(15) N7 0.0177(17) 0.0168(15) 0.0134(14) 0.0005(12) 0.0013(12) -0.0010(13) N8 0.0222(18) 0.0168(15) 0.0142(14) -0.0034(12) -0.0008(12) 0.0004(13) N9 0.0266(19) 0.0177(16) 0.0203(16) -0.0017(13) -0.0038(14) 0.0030(14) N10 0.0231(18) 0.0159(15) 0.0142(14) -0.0030(11) -0.0016(12) 0.0003(13) N11 0.0229(18) 0.0129(14) 0.0138(13) -0.0045(11) 0.0010(13) -0.0018(14) N12 0.0242(19) 0.0160(16) 0.0249(17) -0.0063(13) -0.0004(14) 0.0018(14) N13 0.0282(19) 0.0150(15) 0.0151(14) -0.0062(12) -0.0013(13) -0.0006(14) N14 0.0219(18) 0.0159(15) 0.0128(14) -0.0033(12) -0.0022(12) 0.0006(13) N15 0.0232(18) 0.0157(15) 0.0176(15) -0.0008(12) -0.0009(13) 0.0010(13) N16 0.0232(17) 0.0154(15) 0.0177(14) -0.0072(12) -0.0009(13) -0.0042(13) N17 0.0231(16) 0.0146(13) 0.0152(13) -0.0046(11) -0.0024(14) -0.0001(14) N18 0.0253(18) 0.0135(14) 0.0208(15) -0.0056(12) 0.0044(13) -0.0006(13) S1 0.0362(6) 0.0259(5) 0.0261(5) -0.0136(4) 0.0106(4) -0.0087(5) S2 0.0467(7) 0.0207(5) 0.0249(5) -0.0122(4) -0.0176(5) 0.0141(5) Zn1 0.0263(3) 0.0151(2) 0.01567(19) -0.00479(16) 0.0003(2) -0.0008(2) Zn2 0.0249(2) 0.01350(19) 0.01501(19) -0.00440(15) -0.00311(19) 0.0023(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 B1 N2 1.528(5) . ? B1 N8 1.546(6) . ? B1 N5 1.548(5) . ? B1 H1 1.0000 . ? B2 N11 1.534(5) . ? B2 N14 1.551(6) . ? B2 N17 1.556(5) . ? B2 H2 1.0000 . ? C1 C2 1.492(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N3 1.331(5) . ? C2 N2 1.343(4) . ? C3 N1 1.337(5) . ? C3 N3 1.355(5) . ? C3 C4 1.469(5) . ? C4 C9 1.384(7) . ? C4 C5 1.407(6) . ? C5 C6 1.356(7) . ? C5 H5 0.9500 . ? C6 C7 1.386(10) . ? C6 H6 0.9500 . ? C7 C8 1.398(10) . ? C7 H7 0.9500 . ? C8 C9 1.414(7) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.483(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N6 1.327(5) . ? C11 N5 1.342(5) . ? C12 N4 1.345(5) . ? C12 N6 1.350(5) . ? C12 C13 1.487(5) . ? C13 C18 1.384(5) . ? C13 C14 1.388(5) . ? C14 C15 1.391(5) . ? C14 H14 0.9500 . ? C15 C16 1.374(5) . ? C15 H15 0.9500 . ? C16 C17 1.383(5) . ? C16 H16 0.9500 . ? C17 C18 1.394(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.483(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 N9 1.319(5) . ? C20 N8 1.349(5) . ? C21 N7 1.334(5) . ? C21 N9 1.355(5) . ? C21 C22 1.470(5) . ? C22 C23 1.388(6) . ? C22 C27 1.390(6) . ? C23 C24 1.379(6) . ? C23 H23 0.9500 . ? C24 C25 1.388(7) . ? C24 H24 0.9500 . ? C25 C26 1.394(7) . ? C25 H25 0.9500 . ? C26 C27 1.395(6) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.387(5) . ? C28 C29 1.399(5) . ? C28 S1 1.764(4) . ? C29 C30 1.392(6) . ? C29 H29 0.9500 . ? C30 C31 1.381(6) . ? C30 H30 0.9500 . ? C31 C32 1.370(6) . ? C31 H31 0.9500 . ? C32 C33 1.385(6) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.490(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 N12 1.326(5) . ? C35 N11 1.338(5) . ? C36 N10 1.334(5) . ? C36 N12 1.348(5) . ? C36 C37 1.461(5) . ? C37 C42 1.375(6) . ? C37 C38 1.387(5) . ? C38 C39 1.375(5) . ? C38 H38 0.9500 . ? C39 C40 1.375(6) . ? C39 H39 0.9500 . ? C40 C41 1.380(6) . ? C40 H40 0.9500 . ? C41 C42 1.376(6) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.480(5) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 N15 1.335(5) . ? C44 N14 1.339(5) . ? C45 N13 1.327(5) . ? C45 N15 1.350(5) . ? C45 C46 1.480(5) . ? C46 C51 1.370(5) . ? C46 C47 1.398(6) . ? C47 C48 1.388(6) . ? C47 H47 0.9500 . ? C48 C49 1.365(6) . ? C48 H48 0.9500 . ? C49 C50 1.373(6) . ? C49 H49 0.9500 . ? C50 C51 1.393(6) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C53 1.483(5) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 N18 1.326(5) . ? C53 N17 1.338(4) . ? C54 N16 1.339(5) . ? C54 N18 1.345(5) . ? C54 C55 1.465(5) . ? C55 C60 1.378(6) . ? C55 C56 1.386(5) . ? C56 C57 1.380(6) . ? C56 H56 0.9500 . ? C57 C58 1.378(7) . ? C57 H57 0.9500 . ? C58 C59 1.382(6) . ? C58 H58 0.9500 . ? C59 C60 1.390(5) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C62 1.386(5) . ? C61 C66 1.388(5) . ? C61 S2 1.782(4) . ? C62 C63 1.377(6) . ? C62 H62 0.9500 . ? C63 C64 1.382(6) . ? C63 H63 0.9500 . ? C64 C65 1.380(5) . ? C64 H64 0.9500 . ? C65 C66 1.383(5) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? N1 N2 1.383(4) . ? N1 Zn1 2.053(3) . ? N4 N5 1.388(4) . ? N4 Zn1 2.076(3) . ? N7 N8 1.384(4) . ? N7 Zn1 2.077(3) . ? N10 N11 1.384(4) . ? N10 Zn2 2.066(3) . ? N13 N14 1.378(4) . ? N13 Zn2 2.071(4) . ? N16 N17 1.370(4) . ? N16 Zn2 2.062(3) . ? S1 Zn1 2.2283(12) . ? S2 Zn2 2.2193(11) . ? 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 N2 B1 N8 106.7(3) . . ? N2 B1 N5 109.6(4) . . ? N8 B1 N5 110.0(3) . . ? N2 B1 H1 110.2 . . ? N8 B1 H1 110.2 . . ? N5 B1 H1 110.2 . . ? N11 B2 N14 109.4(3) . . ? N11 B2 N17 109.0(4) . . ? N14 B2 N17 106.9(3) . . ? N11 B2 H2 110.5 . . ? N14 B2 H2 110.5 . . ? N17 B2 H2 110.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N3 C2 N2 110.5(3) . . ? N3 C2 C1 125.5(3) . . ? N2 C2 C1 124.0(3) . . ? N1 C3 N3 112.8(3) . . ? N1 C3 C4 124.2(3) . . ? N3 C3 C4 123.0(3) . . ? C9 C4 C5 121.6(4) . . ? C9 C4 C3 121.5(4) . . ? C5 C4 C3 116.9(4) . . ? C6 C5 C4 120.5(6) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 119.0(6) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C6 C7 C8 121.9(6) . . ? C6 C7 H7 119.1 . . ? C8 C7 H7 119.1 . . ? C7 C8 C9 119.2(6) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C4 C9 C8 117.8(6) . . ? C4 C9 H9 121.1 . . ? C8 C9 H9 121.1 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N6 C11 N5 111.6(3) . . ? N6 C11 C10 125.1(4) . . ? N5 C11 C10 123.3(3) . . ? N4 C12 N6 113.0(3) . . ? N4 C12 C13 125.2(3) . . ? N6 C12 C13 121.4(3) . . ? C18 C13 C14 119.0(3) . . ? C18 C13 C12 122.7(3) . . ? C14 C13 C12 118.1(3) . . ? C13 C14 C15 120.7(4) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C14 120.0(4) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 119.7(3) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C18 120.5(3) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C13 C18 C17 120.0(3) . . ? C13 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N9 C20 N8 111.2(4) . . ? N9 C20 C19 124.6(4) . . ? N8 C20 C19 124.2(4) . . ? N7 C21 N9 113.5(3) . . ? N7 C21 C22 123.9(4) . . ? N9 C21 C22 122.6(4) . . ? C23 C22 C27 120.3(4) . . ? C23 C22 C21 117.8(4) . . ? C27 C22 C21 121.9(4) . . ? C24 C23 C22 120.2(5) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 119.8(5) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 120.7(4) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C27 119.2(4) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? C22 C27 C26 119.8(4) . . ? C22 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C33 C28 C29 118.1(4) . . ? C33 C28 S1 118.2(3) . . ? C29 C28 S1 123.7(3) . . ? C30 C29 C28 120.8(4) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C31 C30 C29 119.9(4) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C32 C31 C30 119.5(4) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 121.1(4) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C32 C33 C28 120.5(4) . . ? C32 C33 H33 119.7 . . ? C28 C33 H33 119.7 . . ? C35 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C35 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N12 C35 N11 111.4(3) . . ? N12 C35 C34 124.6(4) . . ? N11 C35 C34 124.0(3) . . ? N10 C36 N12 113.3(3) . . ? N10 C36 C37 124.6(3) . . ? N12 C36 C37 121.9(3) . . ? C42 C37 C38 117.7(4) . . ? C42 C37 C36 123.6(4) . . ? C38 C37 C36 118.7(3) . . ? C39 C38 C37 121.3(4) . . ? C39 C38 H38 119.3 . . ? C37 C38 H38 119.3 . . ? C40 C39 C38 120.1(4) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 118.9(4) . . ? C39 C40 H40 120.5 . . ? C41 C40 H40 120.5 . . ? C42 C41 C40 120.5(4) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C37 C42 C41 121.1(4) . . ? C37 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N15 C44 N14 111.8(3) . . ? N15 C44 C43 125.4(4) . . ? N14 C44 C43 122.8(4) . . ? N13 C45 N15 112.9(3) . . ? N13 C45 C46 124.7(4) . . ? N15 C45 C46 122.4(4) . . ? C51 C46 C47 119.4(4) . . ? C51 C46 C45 121.5(4) . . ? C47 C46 C45 119.1(4) . . ? C48 C47 C46 119.6(4) . . ? C48 C47 H47 120.2 . . ? C46 C47 H47 120.2 . . ? C49 C48 C47 120.5(4) . . ? C49 C48 H48 119.7 . . ? C47 C48 H48 119.7 . . ? C48 C49 C50 120.0(4) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C49 C50 C51 120.2(4) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? C46 C51 C50 120.2(4) . . ? C46 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C53 C52 H52A 109.5 . . ? C53 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C53 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N18 C53 N17 111.4(3) . . ? N18 C53 C52 124.4(3) . . ? N17 C53 C52 124.2(3) . . ? N16 C54 N18 113.3(3) . . ? N16 C54 C55 122.9(3) . . ? N18 C54 C55 123.7(3) . . ? C60 C55 C56 119.9(4) . . ? C60 C55 C54 119.3(3) . . ? C56 C55 C54 120.7(4) . . ? C57 C56 C55 120.9(4) . . ? C57 C56 H56 119.6 . . ? C55 C56 H56 119.6 . . ? C58 C57 C56 119.2(4) . . ? C58 C57 H57 120.4 . . ? C56 C57 H57 120.4 . . ? C57 C58 C59 120.3(4) . . ? C57 C58 H58 119.8 . . ? C59 C58 H58 119.8 . . ? C58 C59 C60 120.3(4) . . ? C58 C59 H59 119.8 . . ? C60 C59 H59 119.8 . . ? C55 C60 C59 119.4(4) . . ? C55 C60 H60 120.3 . . ? C59 C60 H60 120.3 . . ? C62 C61 C66 119.0(4) . . ? C62 C61 S2 118.3(3) . . ? C66 C61 S2 122.7(3) . . ? C63 C62 C61 120.9(4) . . ? C63 C62 H62 119.5 . . ? C61 C62 H62 119.5 . . ? C62 C63 C64 120.3(4) . . ? C62 C63 H63 119.9 . . ? C64 C63 H63 119.9 . . ? C65 C64 C63 118.8(4) . . ? C65 C64 H64 120.6 . . ? C63 C64 H64 120.6 . . ? C64 C65 C66 121.4(4) . . ? C64 C65 H65 119.3 . . ? C66 C65 H65 119.3 . . ? C65 C66 C61 119.5(3) . . ? C65 C66 H66 120.2 . . ? C61 C66 H66 120.2 . . ? C3 N1 N2 104.0(3) . . ? C3 N1 Zn1 139.4(3) . . ? N2 N1 Zn1 114.1(2) . . ? C2 N2 N1 108.2(3) . . ? C2 N2 B1 132.1(3) . . ? N1 N2 B1 119.3(3) . . ? C2 N3 C3 104.6(3) . . ? C12 N4 N5 103.9(3) . . ? C12 N4 Zn1 143.7(3) . . ? N5 N4 Zn1 109.1(2) . . ? C11 N5 N4 107.4(3) . . ? C11 N5 B1 130.8(3) . . ? N4 N5 B1 121.4(3) . . ? C11 N6 C12 104.2(3) . . ? C21 N7 N8 103.5(3) . . ? C21 N7 Zn1 144.8(3) . . ? N8 N7 Zn1 111.6(2) . . ? C20 N8 N7 107.7(3) . . ? C20 N8 B1 130.3(3) . . ? N7 N8 B1 121.1(3) . . ? C20 N9 C21 104.0(4) . . ? C36 N10 N11 103.8(3) . . ? C36 N10 Zn2 144.3(3) . . ? N11 N10 Zn2 111.0(2) . . ? C35 N11 N10 107.6(3) . . ? C35 N11 B2 130.0(3) . . ? N10 N11 B2 122.0(3) . . ? C35 N12 C36 103.9(3) . . ? C45 N13 N14 105.1(3) . . ? C45 N13 Zn2 142.9(3) . . ? N14 N13 Zn2 111.9(2) . . ? C44 N14 N13 106.7(3) . . ? C44 N14 B2 130.9(3) . . ? N13 N14 B2 121.4(3) . . ? C44 N15 C45 103.5(3) . . ? C54 N16 N17 103.8(3) . . ? C54 N16 Zn2 139.2(2) . . ? N17 N16 Zn2 113.8(2) . . ? C53 N17 N16 107.8(3) . . ? C53 N17 B2 132.5(3) . . ? N16 N17 B2 119.4(3) . . ? C53 N18 C54 103.6(3) . . ? C28 S1 Zn1 105.01(14) . . ? C61 S2 Zn2 106.16(13) . . ? N1 Zn1 N4 96.88(11) . . ? N1 Zn1 N7 88.94(12) . . ? N4 Zn1 N7 89.88(13) . . ? N1 Zn1 S1 123.25(9) . . ? N4 Zn1 S1 119.21(9) . . ? N7 Zn1 S1 129.46(9) . . ? N16 Zn2 N10 92.95(12) . . ? N16 Zn2 N13 90.72(12) . . ? N10 Zn2 N13 91.89(13) . . ? N16 Zn2 S2 124.35(9) . . ? N10 Zn2 S2 122.99(9) . . ? N13 Zn2 S2 124.50(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C3 C4 C9 -45.9(6) . . . . ? N3 C3 C4 C9 134.3(4) . . . . ? N1 C3 C4 C5 134.5(4) . . . . ? N3 C3 C4 C5 -45.3(6) . . . . ? C9 C4 C5 C6 0.7(7) . . . . ? C3 C4 C5 C6 -179.6(4) . . . . ? C4 C5 C6 C7 -2.4(7) . . . . ? C5 C6 C7 C8 2.9(9) . . . . ? C6 C7 C8 C9 -1.6(9) . . . . ? C5 C4 C9 C8 0.5(7) . . . . ? C3 C4 C9 C8 -179.1(4) . . . . ? C7 C8 C9 C4 -0.1(8) . . . . ? N4 C12 C13 C18 -2.5(6) . . . . ? N6 C12 C13 C18 169.6(4) . . . . ? N4 C12 C13 C14 -176.8(4) . . . . ? N6 C12 C13 C14 -4.8(6) . . . . ? C18 C13 C14 C15 -1.0(6) . . . . ? C12 C13 C14 C15 173.6(4) . . . . ? C13 C14 C15 C16 1.2(6) . . . . ? C14 C15 C16 C17 -0.1(6) . . . . ? C15 C16 C17 C18 -1.1(6) . . . . ? C14 C13 C18 C17 -0.2(6) . . . . ? C12 C13 C18 C17 -174.5(4) . . . . ? C16 C17 C18 C13 1.2(6) . . . . ? N7 C21 C22 C23 -151.8(4) . . . . ? N9 C21 C22 C23 28.9(5) . . . . ? N7 C21 C22 C27 30.6(6) . . . . ? N9 C21 C22 C27 -148.7(4) . . . . ? C27 C22 C23 C24 -0.5(6) . . . . ? C21 C22 C23 C24 -178.2(4) . . . . ? C22 C23 C24 C25 0.1(7) . . . . ? C23 C24 C25 C26 0.1(7) . . . . ? C24 C25 C26 C27 0.1(7) . . . . ? C23 C22 C27 C26 0.8(6) . . . . ? C21 C22 C27 C26 178.3(4) . . . . ? C25 C26 C27 C22 -0.6(6) . . . . ? C33 C28 C29 C30 -0.4(7) . . . . ? S1 C28 C29 C30 179.4(4) . . . . ? C28 C29 C30 C31 0.2(7) . . . . ? C29 C30 C31 C32 0.0(8) . . . . ? C30 C31 C32 C33 -0.1(8) . . . . ? C31 C32 C33 C28 0.0(8) . . . . ? C29 C28 C33 C32 0.3(7) . . . . ? S1 C28 C33 C32 -179.5(4) . . . . ? N10 C36 C37 C42 17.6(7) . . . . ? N12 C36 C37 C42 -167.3(5) . . . . ? N10 C36 C37 C38 -162.6(4) . . . . ? N12 C36 C37 C38 12.4(6) . . . . ? C42 C37 C38 C39 -5.8(7) . . . . ? C36 C37 C38 C39 174.4(4) . . . . ? C37 C38 C39 C40 1.9(7) . . . . ? C38 C39 C40 C41 2.9(7) . . . . ? C39 C40 C41 C42 -3.6(8) . . . . ? C38 C37 C42 C41 5.0(8) . . . . ? C36 C37 C42 C41 -175.2(5) . . . . ? C40 C41 C42 C37 -0.4(9) . . . . ? N13 C45 C46 C51 40.7(6) . . . . ? N15 C45 C46 C51 -137.5(4) . . . . ? N13 C45 C46 C47 -141.3(4) . . . . ? N15 C45 C46 C47 40.4(5) . . . . ? C51 C46 C47 C48 -2.3(6) . . . . ? C45 C46 C47 C48 179.7(4) . . . . ? C46 C47 C48 C49 2.6(6) . . . . ? C47 C48 C49 C50 -1.6(7) . . . . ? C48 C49 C50 C51 0.4(7) . . . . ? C47 C46 C51 C50 1.1(6) . . . . ? C45 C46 C51 C50 179.0(4) . . . . ? C49 C50 C51 C46 -0.1(7) . . . . ? N16 C54 C55 C60 -35.6(6) . . . . ? N18 C54 C55 C60 140.9(4) . . . . ? N16 C54 C55 C56 147.5(4) . . . . ? N18 C54 C55 C56 -36.0(6) . . . . ? C60 C55 C56 C57 0.2(6) . . . . ? C54 C55 C56 C57 177.0(4) . . . . ? C55 C56 C57 C58 -0.4(6) . . . . ? C56 C57 C58 C59 0.7(7) . . . . ? C57 C58 C59 C60 -0.8(7) . . . . ? C56 C55 C60 C59 -0.3(6) . . . . ? C54 C55 C60 C59 -177.2(4) . . . . ? C58 C59 C60 C55 0.6(7) . . . . ? C66 C61 C62 C63 0.0(7) . . . . ? S2 C61 C62 C63 178.8(4) . . . . ? C61 C62 C63 C64 -0.8(7) . . . . ? C62 C63 C64 C65 1.2(7) . . . . ? C63 C64 C65 C66 -0.8(7) . . . . ? C64 C65 C66 C61 0.0(7) . . . . ? C62 C61 C66 C65 0.5(6) . . . . ? S2 C61 C66 C65 -178.3(3) . . . . ? N3 C3 N1 N2 0.0(4) . . . . ? C4 C3 N1 N2 -179.8(4) . . . . ? N3 C3 N1 Zn1 159.2(3) . . . . ? C4 C3 N1 Zn1 -20.6(7) . . . . ? N3 C2 N2 N1 -0.8(5) . . . . ? C1 C2 N2 N1 -178.6(4) . . . . ? N3 C2 N2 B1 -172.5(4) . . . . ? C1 C2 N2 B1 9.8(7) . . . . ? C3 N1 N2 C2 0.5(4) . . . . ? Zn1 N1 N2 C2 -164.8(3) . . . . ? C3 N1 N2 B1 173.4(3) . . . . ? Zn1 N1 N2 B1 8.1(4) . . . . ? N8 B1 N2 C2 104.3(5) . . . . ? N5 B1 N2 C2 -136.6(4) . . . . ? N8 B1 N2 N1 -66.6(4) . . . . ? N5 B1 N2 N1 52.5(4) . . . . ? N2 C2 N3 C3 0.8(5) . . . . ? C1 C2 N3 C3 178.5(4) . . . . ? N1 C3 N3 C2 -0.5(5) . . . . ? C4 C3 N3 C2 179.4(4) . . . . ? N6 C12 N4 N5 -1.8(4) . . . . ? C13 C12 N4 N5 170.8(4) . . . . ? N6 C12 N4 Zn1 153.1(3) . . . . ? C13 C12 N4 Zn1 -34.3(7) . . . . ? N6 C11 N5 N4 -1.5(4) . . . . ? C10 C11 N5 N4 176.1(4) . . . . ? N6 C11 N5 B1 170.3(4) . . . . ? C10 C11 N5 B1 -12.1(7) . . . . ? C12 N4 N5 C11 1.9(4) . . . . ? Zn1 N4 N5 C11 -162.6(3) . . . . ? C12 N4 N5 B1 -170.8(3) . . . . ? Zn1 N4 N5 B1 24.6(4) . . . . ? N2 B1 N5 C11 113.2(4) . . . . ? N8 B1 N5 C11 -129.8(4) . . . . ? N2 B1 N5 N4 -76.0(4) . . . . ? N8 B1 N5 N4 41.0(5) . . . . ? N5 C11 N6 C12 0.4(5) . . . . ? C10 C11 N6 C12 -177.1(4) . . . . ? N4 C12 N6 C11 0.9(5) . . . . ? C13 C12 N6 C11 -172.0(4) . . . . ? N9 C21 N7 N8 1.1(4) . . . . ? C22 C21 N7 N8 -178.3(3) . . . . ? N9 C21 N7 Zn1 178.3(3) . . . . ? C22 C21 N7 Zn1 -1.1(7) . . . . ? N9 C20 N8 N7 0.5(4) . . . . ? C19 C20 N8 N7 -178.9(3) . . . . ? N9 C20 N8 B1 169.3(3) . . . . ? C19 C20 N8 B1 -10.0(6) . . . . ? C21 N7 N8 C20 -1.0(4) . . . . ? Zn1 N7 N8 C20 -179.2(2) . . . . ? C21 N7 N8 B1 -171.0(3) . . . . ? Zn1 N7 N8 B1 10.7(4) . . . . ? N2 B1 N8 C20 -113.0(4) . . . . ? N5 B1 N8 C20 128.2(4) . . . . ? N2 B1 N8 N7 54.5(4) . . . . ? N5 B1 N8 N7 -64.3(4) . . . . ? N8 C20 N9 C21 0.2(4) . . . . ? C19 C20 N9 C21 179.5(3) . . . . ? N7 C21 N9 C20 -0.8(4) . . . . ? C22 C21 N9 C20 178.6(3) . . . . ? N12 C36 N10 N11 -1.3(4) . . . . ? C37 C36 N10 N11 174.1(4) . . . . ? N12 C36 N10 Zn2 165.8(3) . . . . ? C37 C36 N10 Zn2 -18.8(7) . . . . ? N12 C35 N11 N10 0.0(4) . . . . ? C34 C35 N11 N10 -179.3(4) . . . . ? N12 C35 N11 B2 172.4(4) . . . . ? C34 C35 N11 B2 -6.9(7) . . . . ? C36 N10 N11 C35 0.8(4) . . . . ? Zn2 N10 N11 C35 -171.2(3) . . . . ? C36 N10 N11 B2 -172.3(3) . . . . ? Zn2 N10 N11 B2 15.7(4) . . . . ? N14 B2 N11 C35 -124.2(4) . . . . ? N17 B2 N11 C35 119.2(4) . . . . ? N14 B2 N11 N10 47.2(5) . . . . ? N17 B2 N11 N10 -69.4(4) . . . . ? N11 C35 N12 C36 -0.8(4) . . . . ? C34 C35 N12 C36 178.5(4) . . . . ? N10 C36 N12 C35 1.3(5) . . . . ? C37 C36 N12 C35 -174.2(4) . . . . ? N15 C45 N13 N14 -0.4(4) . . . . ? C46 C45 N13 N14 -178.8(3) . . . . ? N15 C45 N13 Zn2 179.1(3) . . . . ? C46 C45 N13 Zn2 0.7(6) . . . . ? N15 C44 N14 N13 -0.6(4) . . . . ? C43 C44 N14 N13 -179.9(3) . . . . ? N15 C44 N14 B2 167.7(3) . . . . ? C43 C44 N14 B2 -11.6(6) . . . . ? C45 N13 N14 C44 0.6(4) . . . . ? Zn2 N13 N14 C44 -179.0(2) . . . . ? C45 N13 N14 B2 -169.1(3) . . . . ? Zn2 N13 N14 B2 11.3(4) . . . . ? N11 B2 N14 C44 128.0(4) . . . . ? N17 B2 N14 C44 -114.1(4) . . . . ? N11 B2 N14 N13 -65.1(4) . . . . ? N17 B2 N14 N13 52.8(4) . . . . ? N14 C44 N15 C45 0.4(4) . . . . ? C43 C44 N15 C45 179.6(3) . . . . ? N13 C45 N15 C44 0.0(4) . . . . ? C46 C45 N15 C44 178.5(3) . . . . ? N18 C54 N16 N17 -1.7(4) . . . . ? C55 C54 N16 N17 175.1(4) . . . . ? N18 C54 N16 Zn2 155.7(3) . . . . ? C55 C54 N16 Zn2 -27.5(6) . . . . ? N18 C53 N17 N16 -0.4(5) . . . . ? C52 C53 N17 N16 -179.6(4) . . . . ? N18 C53 N17 B2 -174.8(4) . . . . ? C52 C53 N17 B2 6.0(7) . . . . ? C54 N16 N17 C53 1.2(4) . . . . ? Zn2 N16 N17 C53 -162.8(3) . . . . ? C54 N16 N17 B2 176.5(3) . . . . ? Zn2 N16 N17 B2 12.4(4) . . . . ? N11 B2 N17 C53 -136.2(4) . . . . ? N14 B2 N17 C53 105.7(5) . . . . ? N11 B2 N17 N16 50.0(4) . . . . ? N14 B2 N17 N16 -68.2(4) . . . . ? N17 C53 N18 C54 -0.6(5) . . . . ? C52 C53 N18 C54 178.6(4) . . . . ? N16 C54 N18 C53 1.4(5) . . . . ? C55 C54 N18 C53 -175.4(4) . . . . ? C33 C28 S1 Zn1 -157.9(3) . . . . ? C29 C28 S1 Zn1 22.3(4) . . . . ? C62 C61 S2 Zn2 -159.8(3) . . . . ? C66 C61 S2 Zn2 19.0(4) . . . . ? C3 N1 Zn1 N4 156.9(4) . . . . ? N2 N1 Zn1 N4 -45.3(3) . . . . ? C3 N1 Zn1 N7 -113.4(4) . . . . ? N2 N1 Zn1 N7 44.5(3) . . . . ? C3 N1 Zn1 S1 25.0(5) . . . . ? N2 N1 Zn1 S1 -177.1(2) . . . . ? C12 N4 Zn1 N1 -126.5(4) . . . . ? N5 N4 Zn1 N1 27.6(3) . . . . ? C12 N4 Zn1 N7 144.6(4) . . . . ? N5 N4 Zn1 N7 -61.3(2) . . . . ? C12 N4 Zn1 S1 7.9(5) . . . . ? N5 N4 Zn1 S1 162.1(2) . . . . ? C21 N7 Zn1 N1 129.3(4) . . . . ? N8 N7 Zn1 N1 -53.6(2) . . . . ? C21 N7 Zn1 N4 -133.8(4) . . . . ? N8 N7 Zn1 N4 43.3(2) . . . . ? C21 N7 Zn1 S1 -4.7(5) . . . . ? N8 N7 Zn1 S1 172.37(17) . . . . ? C28 S1 Zn1 N1 -72.92(18) . . . . ? C28 S1 Zn1 N4 165.02(17) . . . . ? C28 S1 Zn1 N7 47.82(18) . . . . ? C54 N16 Zn2 N10 152.6(4) . . . . ? N17 N16 Zn2 N10 -51.5(3) . . . . ? C54 N16 Zn2 N13 -115.5(4) . . . . ? N17 N16 Zn2 N13 40.4(3) . . . . ? C54 N16 Zn2 S2 18.5(5) . . . . ? N17 N16 Zn2 S2 174.4(2) . . . . ? C36 N10 Zn2 N16 -130.2(5) . . . . ? N11 N10 Zn2 N16 36.4(3) . . . . ? C36 N10 Zn2 N13 139.0(5) . . . . ? N11 N10 Zn2 N13 -54.5(3) . . . . ? C36 N10 Zn2 S2 4.8(5) . . . . ? N11 N10 Zn2 S2 171.3(2) . . . . ? C45 N13 Zn2 N16 128.1(4) . . . . ? N14 N13 Zn2 N16 -52.4(2) . . . . ? C45 N13 Zn2 N10 -138.9(4) . . . . ? N14 N13 Zn2 N10 40.5(2) . . . . ? C45 N13 Zn2 S2 -5.8(5) . . . . ? N14 N13 Zn2 S2 173.67(17) . . . . ? C61 S2 Zn2 N16 -69.92(19) . . . . ? C61 S2 Zn2 N10 168.89(18) . . . . ? C61 S2 Zn2 N13 49.30(18) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.728 _refine_diff_density_min -1.194 _refine_diff_density_rms 0.085 data_09mz446_0m _database_code_depnum_ccdc_archive 'CCDC 764048' #TrackingRef '- combined cifs' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 B N9 O2 Zn' _chemical_formula_weight 650.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 18.670(8) _cell_length_b 16.257(7) _cell_length_c 10.399(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.551(9) _cell_angle_gamma 90.00 _cell_volume 3129(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1023 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 27.38 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.830 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4045 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details 'Apex2 v2009.7-0 (Bruker, 2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 22814 _diffrn_reflns_av_R_equivalents 0.0773 _diffrn_reflns_av_sigmaI/netI 0.0676 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5511 _reflns_number_gt 3742 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2009.7-0 (Bruker, 2009)' _computing_cell_refinement 'Apex2 v2009.7-0' _computing_data_reduction 'Apex2 v2009.7-0' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0427P)^2^+66.2866P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5511 _refine_ls_number_parameters 411 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1416 _refine_ls_R_factor_gt 0.1014 _refine_ls_wR_factor_ref 0.2837 _refine_ls_wR_factor_gt 0.2569 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.1169(6) 0.5485(6) 0.2258(9) 0.023(2) Uani 1 1 d . . . H1 H 0.0743 0.5650 0.2689 0.028 Uiso 1 1 calc R . . C1 C 0.1254(6) 0.5435(6) 0.5336(10) 0.037(3) Uani 1 1 d . . . H1A H 0.1198 0.6035 0.5302 0.055 Uiso 1 1 calc R . . H1B H 0.1375 0.5261 0.6241 0.055 Uiso 1 1 calc R . . H1C H 0.0801 0.5174 0.4962 0.055 Uiso 1 1 calc R . . C2 C 0.1847(6) 0.5187(5) 0.4581(8) 0.026(2) Uani 1 1 d . . . C3 C 0.2846(6) 0.4766(5) 0.4085(8) 0.027(2) Uani 1 1 d . . . C4 C 0.3575(6) 0.4423(6) 0.4274(9) 0.030(2) Uani 1 1 d . . . C5 C 0.3948(7) 0.4369(7) 0.5520(11) 0.044(3) Uani 1 1 d . . . H5 H 0.3722 0.4556 0.6233 0.053 Uiso 1 1 calc R . . C6 C 0.4633(7) 0.4052(7) 0.5746(11) 0.048(3) Uani 1 1 d . . . H6 H 0.4879 0.4037 0.6606 0.058 Uiso 1 1 calc R . . C7 C 0.4968(7) 0.3753(7) 0.4732(12) 0.046(3) Uani 1 1 d . . . H7 H 0.5439 0.3522 0.4884 0.056 Uiso 1 1 calc R . . C8 C 0.4600(7) 0.3799(8) 0.3493(12) 0.052(3) Uani 1 1 d . . . H8 H 0.4827 0.3605 0.2786 0.062 Uiso 1 1 calc R . . C9 C 0.3911(7) 0.4118(7) 0.3257(10) 0.045(3) Uani 1 1 d . . . H9 H 0.3665 0.4129 0.2397 0.054 Uiso 1 1 calc R . . C10 C 0.0629(6) 0.7350(5) 0.2073(10) 0.033(2) Uani 1 1 d . . . H10A H 0.0470 0.7882 0.1697 0.049 Uiso 1 1 calc R . . H10B H 0.0844 0.7428 0.2976 0.049 Uiso 1 1 calc R . . H10C H 0.0214 0.6979 0.2042 0.049 Uiso 1 1 calc R . . C11 C 0.1170(6) 0.6991(5) 0.1326(9) 0.027(2) Uani 1 1 d . . . C12 C 0.1951(5) 0.6819(5) 0.0029(9) 0.027(2) Uani 1 1 d . . . C13 C 0.2408(5) 0.6975(5) -0.0966(9) 0.028(2) Uani 1 1 d . . . C14 C 0.2671(6) 0.7776(5) -0.1133(9) 0.031(2) Uani 1 1 d . . . H14 H 0.2542 0.8212 -0.0600 0.038 Uiso 1 1 calc R . . C15 C 0.3112(6) 0.7927(6) -0.2063(9) 0.032(2) Uani 1 1 d . . . H15 H 0.3293 0.8467 -0.2155 0.039 Uiso 1 1 calc R . . C16 C 0.3299(6) 0.7301(6) -0.2879(9) 0.037(3) Uani 1 1 d . . . H16 H 0.3602 0.7411 -0.3524 0.044 Uiso 1 1 calc R . . C17 C 0.3031(6) 0.6515(6) -0.2726(9) 0.035(2) Uani 1 1 d . . . H17 H 0.3154 0.6082 -0.3268 0.043 Uiso 1 1 calc R . . C18 C 0.2586(6) 0.6358(5) -0.1792(9) 0.030(2) Uani 1 1 d . . . H18 H 0.2400 0.5819 -0.1713 0.036 Uiso 1 1 calc R . . C19 C -0.0285(5) 0.4433(5) 0.1744(10) 0.031(2) Uani 1 1 d . . . H19A H -0.0687 0.4114 0.1294 0.046 Uiso 1 1 calc R . . H19B H -0.0410 0.5019 0.1707 0.046 Uiso 1 1 calc R . . H19C H -0.0191 0.4257 0.2651 0.046 Uiso 1 1 calc R . . C20 C 0.0365(6) 0.4299(5) 0.1113(10) 0.030(2) Uani 1 1 d . . . C21 C 0.1108(6) 0.3826(5) -0.0071(9) 0.027(2) Uani 1 1 d . . . C22 C 0.1424(5) 0.3355(5) -0.1056(10) 0.029(2) Uani 1 1 d . . . C23 C 0.1347(6) 0.2490(5) -0.1072(9) 0.033(2) Uani 1 1 d . . . H23 H 0.1079 0.2225 -0.0475 0.039 Uiso 1 1 calc R . . C24 C 0.1666(6) 0.2036(6) -0.1966(10) 0.036(2) Uani 1 1 d . . . H24 H 0.1623 0.1454 -0.1967 0.044 Uiso 1 1 calc R . . C25 C 0.2048(6) 0.2410(6) -0.2861(10) 0.035(2) Uani 1 1 d . . . H25 H 0.2270 0.2089 -0.3461 0.042 Uiso 1 1 calc R . . C26 C 0.2101(6) 0.3270(6) -0.2867(9) 0.036(2) Uani 1 1 d . . . H26 H 0.2347 0.3540 -0.3491 0.044 Uiso 1 1 calc R . . C27 C 0.1790(6) 0.3724(5) -0.1952(9) 0.033(2) Uani 1 1 d . . . H27 H 0.1834 0.4306 -0.1949 0.040 Uiso 1 1 calc R . . C28 C 0.4377(6) 0.6196(6) -0.0113(11) 0.041(3) Uani 1 1 d . . . H28A H 0.4101 0.6652 -0.0548 0.061 Uiso 1 1 calc R . . H28B H 0.4725 0.5994 -0.0665 0.061 Uiso 1 1 calc R . . H28C H 0.4634 0.6386 0.0715 0.061 Uiso 1 1 calc R . . C29 C 0.3868(6) 0.5510(6) 0.0132(10) 0.031(2) Uani 1 1 d . . . C30 C 0.3927(6) 0.4746(6) -0.0516(10) 0.038(2) Uani 1 1 d . . . H30 H 0.4271 0.4707 -0.1111 0.045 Uiso 1 1 calc R . . C31 C 0.3513(6) 0.4049(6) -0.0336(10) 0.033(2) Uani 1 1 d . . . C32 C 0.3714(7) 0.3229(6) -0.0876(11) 0.044(3) Uani 1 1 d . . . H32A H 0.4032 0.2929 -0.0211 0.067 Uiso 1 1 calc R . . H32B H 0.3965 0.3320 -0.1634 0.067 Uiso 1 1 calc R . . H32C H 0.3275 0.2906 -0.1133 0.067 Uiso 1 1 calc R . . N1 N 0.2480(4) 0.4910(4) 0.5112(8) 0.0276(18) Uani 1 1 d . . . N2 N 0.1806(4) 0.5220(4) 0.3293(7) 0.0246(17) Uani 1 1 d . . . N3 N 0.2456(4) 0.4954(5) 0.2975(8) 0.0287(18) Uani 1 1 d . . . N4 N 0.1501(5) 0.7389(4) 0.0440(7) 0.0292(19) Uani 1 1 d . . . N5 N 0.1407(4) 0.6201(4) 0.1456(7) 0.0252(17) Uani 1 1 d . . . N6 N 0.1912(4) 0.6093(4) 0.0619(7) 0.0233(17) Uani 1 1 d . . . N7 N 0.0432(5) 0.3714(4) 0.0224(8) 0.0294(19) Uani 1 1 d . . . N8 N 0.0974(4) 0.4745(4) 0.1345(7) 0.0262(18) Uani 1 1 d . . . N9 N 0.1464(4) 0.4447(4) 0.0586(7) 0.0250(17) Uani 1 1 d . . . O1 O 0.3417(4) 0.5657(4) 0.0883(6) 0.0304(15) Uani 1 1 d . . . O2 O 0.2976(4) 0.4034(4) 0.0301(7) 0.0336(16) Uani 1 1 d . . . Zn1 Zn 0.25154(6) 0.50058(6) 0.09844(10) 0.0247(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.045(7) 0.009(5) 0.016(5) -0.001(4) 0.006(4) -0.001(4) C1 0.067(8) 0.017(5) 0.029(5) 0.002(4) 0.013(5) -0.002(5) C2 0.053(6) 0.011(4) 0.015(4) -0.003(3) 0.005(4) -0.005(4) C3 0.049(6) 0.014(4) 0.016(4) -0.002(3) 0.003(4) -0.004(4) C4 0.055(7) 0.013(4) 0.023(5) 0.003(4) 0.005(4) -0.002(4) C5 0.064(8) 0.039(6) 0.029(6) -0.006(5) 0.006(5) 0.003(6) C6 0.065(8) 0.042(7) 0.035(6) 0.004(5) -0.002(6) 0.002(6) C7 0.049(7) 0.035(6) 0.055(8) 0.014(5) 0.006(6) 0.009(5) C8 0.064(8) 0.054(8) 0.040(7) 0.014(6) 0.018(6) 0.017(6) C9 0.064(8) 0.049(7) 0.022(5) 0.003(5) 0.005(5) 0.012(6) C10 0.053(7) 0.007(4) 0.038(6) -0.004(4) 0.007(5) 0.003(4) C11 0.053(6) 0.003(4) 0.023(5) 0.000(3) -0.001(4) 0.001(4) C12 0.047(6) 0.008(4) 0.028(5) 0.000(4) 0.004(4) -0.002(4) C13 0.042(6) 0.013(4) 0.028(5) -0.002(4) 0.003(4) 0.006(4) C14 0.056(7) 0.010(4) 0.028(5) 0.000(4) 0.003(5) -0.002(4) C15 0.058(7) 0.012(4) 0.026(5) 0.007(4) 0.001(5) 0.000(4) C16 0.069(8) 0.024(5) 0.018(5) 0.000(4) 0.008(5) 0.000(5) C17 0.068(7) 0.015(5) 0.024(5) 0.000(4) 0.006(5) 0.003(5) C18 0.057(7) 0.007(4) 0.025(5) -0.005(4) 0.001(5) -0.002(4) C19 0.047(6) 0.009(4) 0.036(6) 0.005(4) 0.006(5) -0.003(4) C20 0.045(6) 0.011(4) 0.034(6) 0.006(4) 0.000(4) -0.002(4) C21 0.049(6) 0.005(4) 0.027(5) 0.001(3) 0.006(4) 0.003(4) C22 0.044(6) 0.008(4) 0.035(6) -0.005(4) 0.000(4) 0.007(4) C23 0.062(7) 0.007(4) 0.028(5) -0.004(4) 0.003(5) -0.004(4) C24 0.065(7) 0.009(4) 0.032(5) -0.006(4) -0.001(5) 0.003(4) C25 0.056(7) 0.017(5) 0.029(5) -0.008(4) -0.001(5) 0.003(4) C26 0.066(7) 0.025(5) 0.019(5) 0.003(4) 0.011(5) 0.002(5) C27 0.071(8) 0.006(4) 0.023(5) 0.002(4) 0.007(5) 0.002(4) C28 0.057(7) 0.025(5) 0.042(6) 0.009(5) 0.010(5) 0.002(5) C29 0.041(6) 0.015(5) 0.037(6) 0.006(4) 0.003(5) 0.006(4) C30 0.049(7) 0.029(5) 0.037(6) -0.004(5) 0.014(5) 0.006(5) C31 0.049(6) 0.011(4) 0.038(6) -0.005(4) 0.004(5) 0.006(4) C32 0.064(8) 0.025(6) 0.046(7) -0.012(5) 0.011(6) 0.007(5) N1 0.046(5) 0.009(4) 0.028(4) -0.001(3) 0.004(4) -0.002(3) N2 0.049(5) 0.007(3) 0.019(4) -0.003(3) 0.008(3) -0.005(3) N3 0.030(4) 0.012(4) 0.044(5) 0.001(3) 0.006(4) -0.003(3) N4 0.059(6) 0.010(4) 0.019(4) 0.005(3) 0.005(4) 0.005(3) N5 0.044(5) 0.005(3) 0.027(4) 0.001(3) 0.008(4) 0.000(3) N6 0.045(5) 0.005(3) 0.020(4) 0.001(3) 0.005(3) -0.001(3) N7 0.053(6) 0.004(3) 0.030(4) 0.002(3) 0.001(4) -0.001(3) N8 0.046(5) 0.007(3) 0.025(4) 0.000(3) 0.005(4) -0.001(3) N9 0.049(5) 0.005(3) 0.023(4) -0.001(3) 0.010(3) 0.000(3) O1 0.050(4) 0.009(3) 0.035(4) -0.001(3) 0.014(3) -0.001(3) O2 0.049(4) 0.013(3) 0.040(4) -0.006(3) 0.010(3) 0.002(3) Zn1 0.0478(7) 0.0056(5) 0.0214(5) 0.0002(4) 0.0076(4) 0.0003(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 B1 N5 1.531(12) . ? B1 N8 1.547(11) . ? B1 N2 1.556(13) . ? B1 H1 1.0000 . ? C1 C2 1.495(14) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.317(13) . ? C2 N2 1.332(11) . ? C3 N3 1.316(12) . ? C3 N1 1.361(12) . ? C3 C4 1.462(14) . ? C4 C9 1.390(14) . ? C4 C5 1.391(14) . ? C5 C6 1.370(16) . ? C5 H5 0.9500 . ? C6 C7 1.383(17) . ? C6 H6 0.9500 . ? C7 C8 1.379(17) . ? C7 H7 0.9500 . ? C8 C9 1.379(16) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.473(14) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N4 1.341(12) . ? C11 N5 1.358(11) . ? C12 N6 1.336(11) . ? C12 N4 1.358(12) . ? C12 C13 1.448(14) . ? C13 C18 1.389(12) . ? C13 C14 1.410(13) . ? C14 C15 1.372(14) . ? C14 H14 0.9500 . ? C15 C16 1.398(14) . ? C15 H15 0.9500 . ? C16 C17 1.389(14) . ? C16 H16 0.9500 . ? C17 C18 1.382(14) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.469(14) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 N8 1.343(12) . ? C20 N7 1.344(12) . ? C21 N9 1.344(12) . ? C21 N7 1.351(13) . ? C21 C22 1.463(13) . ? C22 C27 1.365(14) . ? C22 C23 1.412(12) . ? C23 C24 1.383(14) . ? C23 H23 0.9500 . ? C24 C25 1.385(15) . ? C24 H24 0.9500 . ? C25 C26 1.401(14) . ? C25 H25 0.9500 . ? C26 C27 1.390(14) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.507(14) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 O1 1.245(12) . ? C29 C30 1.425(14) . ? C30 C31 1.399(15) . ? C30 H30 0.9500 . ? C31 O2 1.271(12) . ? C31 C32 1.512(13) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N2 N3 1.369(11) . ? N3 Zn1 2.089(9) . ? N5 N6 1.377(11) . ? N6 Zn1 2.103(7) . ? N8 N9 1.373(11) . ? N9 Zn1 2.154(8) . ? O1 Zn1 2.003(7) . ? O2 Zn1 1.976(6) . ? 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 N5 B1 N8 108.6(7) . . ? N5 B1 N2 109.7(8) . . ? N8 B1 N2 107.8(7) . . ? N5 B1 H1 110.2 . . ? N8 B1 H1 110.2 . . ? N2 B1 H1 110.2 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 N2 111.4(9) . . ? N1 C2 C1 123.9(8) . . ? N2 C2 C1 124.7(9) . . ? N3 C3 N1 111.8(9) . . ? N3 C3 C4 127.2(9) . . ? N1 C3 C4 121.0(8) . . ? C9 C4 C5 117.8(10) . . ? C9 C4 C3 122.6(9) . . ? C5 C4 C3 119.5(9) . . ? C6 C5 C4 121.7(11) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 120.4(11) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C7 C6 118.3(11) . . ? C8 C7 H7 120.9 . . ? C6 C7 H7 120.9 . . ? C7 C8 C9 121.7(11) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C8 C9 C4 120.1(10) . . ? C8 C9 H9 119.9 . . ? C4 C9 H9 119.9 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 N5 110.6(8) . . ? N4 C11 C10 125.5(8) . . ? N5 C11 C10 124.0(8) . . ? N6 C12 N4 112.6(8) . . ? N6 C12 C13 123.8(8) . . ? N4 C12 C13 123.6(8) . . ? C18 C13 C14 118.4(9) . . ? C18 C13 C12 121.8(8) . . ? C14 C13 C12 119.8(8) . . ? C15 C14 C13 120.1(9) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 121.2(9) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C17 C16 C15 118.5(10) . . ? C17 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? C18 C17 C16 120.6(9) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C13 121.0(9) . . ? C17 C18 H18 119.5 . . ? C13 C18 H18 119.5 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N8 C20 N7 110.7(9) . . ? N8 C20 C19 124.7(9) . . ? N7 C20 C19 124.7(9) . . ? N9 C21 N7 113.6(8) . . ? N9 C21 C22 122.1(9) . . ? N7 C21 C22 124.3(8) . . ? C27 C22 C23 119.3(9) . . ? C27 C22 C21 122.1(8) . . ? C23 C22 C21 118.7(9) . . ? C24 C23 C22 119.2(10) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C23 C24 C25 121.5(9) . . ? C23 C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? C24 C25 C26 119.0(10) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C27 C26 C25 119.3(10) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C22 C27 C26 121.7(8) . . ? C22 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O1 C29 C30 124.4(9) . . ? O1 C29 C28 117.2(9) . . ? C30 C29 C28 118.4(9) . . ? C31 C30 C29 124.4(10) . . ? C31 C30 H30 117.8 . . ? C29 C30 H30 117.8 . . ? O2 C31 C30 124.9(9) . . ? O2 C31 C32 115.3(9) . . ? C30 C31 C32 119.7(10) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C2 N1 C3 104.1(8) . . ? C2 N2 N3 107.1(8) . . ? C2 N2 B1 130.0(8) . . ? N3 N2 B1 122.8(7) . . ? C3 N3 N2 105.5(8) . . ? C3 N3 Zn1 141.6(7) . . ? N2 N3 Zn1 113.0(6) . . ? C11 N4 C12 104.3(7) . . ? C11 N5 N6 107.4(7) . . ? C11 N5 B1 131.2(8) . . ? N6 N5 B1 121.3(7) . . ? C12 N6 N5 105.1(7) . . ? C12 N6 Zn1 139.9(7) . . ? N5 N6 Zn1 112.9(5) . . ? C20 N7 C21 103.6(8) . . ? C20 N8 N9 108.6(7) . . ? C20 N8 B1 131.0(8) . . ? N9 N8 B1 120.4(8) . . ? C21 N9 N8 103.6(8) . . ? C21 N9 Zn1 142.3(7) . . ? N8 N9 Zn1 113.6(5) . . ? C29 O1 Zn1 125.0(6) . . ? C31 O2 Zn1 125.6(6) . . ? O2 Zn1 O1 89.7(3) . . ? O2 Zn1 N3 114.0(3) . . ? O1 Zn1 N3 103.2(3) . . ? O2 Zn1 N6 148.8(3) . . ? O1 Zn1 N6 88.8(3) . . ? N3 Zn1 N6 96.7(3) . . ? O2 Zn1 N9 91.3(3) . . ? O1 Zn1 N9 164.6(3) . . ? N3 Zn1 N9 90.5(3) . . ? N6 Zn1 N9 82.4(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 C3 C4 C9 -11.3(15) . . . . ? N1 C3 C4 C9 167.0(9) . . . . ? N3 C3 C4 C5 171.0(10) . . . . ? N1 C3 C4 C5 -10.7(14) . . . . ? C9 C4 C5 C6 2.2(17) . . . . ? C3 C4 C5 C6 180.0(10) . . . . ? C4 C5 C6 C7 -1.8(18) . . . . ? C5 C6 C7 C8 1.3(18) . . . . ? C6 C7 C8 C9 -1.2(19) . . . . ? C7 C8 C9 C4 1.6(19) . . . . ? C5 C4 C9 C8 -2.0(17) . . . . ? C3 C4 C9 C8 -179.8(10) . . . . ? N6 C12 C13 C18 29.5(15) . . . . ? N4 C12 C13 C18 -148.6(10) . . . . ? N6 C12 C13 C14 -151.9(9) . . . . ? N4 C12 C13 C14 30.0(15) . . . . ? C18 C13 C14 C15 -2.2(15) . . . . ? C12 C13 C14 C15 179.2(9) . . . . ? C13 C14 C15 C16 1.3(15) . . . . ? C14 C15 C16 C17 -0.3(16) . . . . ? C15 C16 C17 C18 0.4(16) . . . . ? C16 C17 C18 C13 -1.4(16) . . . . ? C14 C13 C18 C17 2.2(15) . . . . ? C12 C13 C18 C17 -179.1(10) . . . . ? N9 C21 C22 C27 -43.2(14) . . . . ? N7 C21 C22 C27 133.6(10) . . . . ? N9 C21 C22 C23 136.7(10) . . . . ? N7 C21 C22 C23 -46.6(14) . . . . ? C27 C22 C23 C24 2.2(16) . . . . ? C21 C22 C23 C24 -177.6(9) . . . . ? C22 C23 C24 C25 -1.2(16) . . . . ? C23 C24 C25 C26 -0.9(16) . . . . ? C24 C25 C26 C27 2.1(16) . . . . ? C23 C22 C27 C26 -1.1(16) . . . . ? C21 C22 C27 C26 178.7(10) . . . . ? C25 C26 C27 C22 -1.0(17) . . . . ? O1 C29 C30 C31 -3.7(17) . . . . ? C28 C29 C30 C31 177.1(10) . . . . ? C29 C30 C31 O2 8.9(18) . . . . ? C29 C30 C31 C32 -168.6(10) . . . . ? N2 C2 N1 C3 0.0(10) . . . . ? C1 C2 N1 C3 -179.7(8) . . . . ? N3 C3 N1 C2 0.5(10) . . . . ? C4 C3 N1 C2 -178.0(8) . . . . ? N1 C2 N2 N3 -0.5(10) . . . . ? C1 C2 N2 N3 179.2(8) . . . . ? N1 C2 N2 B1 178.5(8) . . . . ? C1 C2 N2 B1 -1.8(14) . . . . ? N5 B1 N2 C2 121.7(9) . . . . ? N8 B1 N2 C2 -120.1(9) . . . . ? N5 B1 N2 N3 -59.4(10) . . . . ? N8 B1 N2 N3 58.8(10) . . . . ? N1 C3 N3 N2 -0.8(10) . . . . ? C4 C3 N3 N2 177.6(8) . . . . ? N1 C3 N3 Zn1 176.9(7) . . . . ? C4 C3 N3 Zn1 -4.7(16) . . . . ? C2 N2 N3 C3 0.8(9) . . . . ? B1 N2 N3 C3 -178.3(7) . . . . ? C2 N2 N3 Zn1 -177.7(5) . . . . ? B1 N2 N3 Zn1 3.2(9) . . . . ? N5 C11 N4 C12 -0.2(10) . . . . ? C10 C11 N4 C12 179.4(9) . . . . ? N6 C12 N4 C11 0.0(11) . . . . ? C13 C12 N4 C11 178.4(9) . . . . ? N4 C11 N5 N6 0.3(10) . . . . ? C10 C11 N5 N6 -179.3(9) . . . . ? N4 C11 N5 B1 -175.4(9) . . . . ? C10 C11 N5 B1 5.0(16) . . . . ? N8 B1 N5 C11 125.7(10) . . . . ? N2 B1 N5 C11 -116.6(10) . . . . ? N8 B1 N5 N6 -49.5(11) . . . . ? N2 B1 N5 N6 68.2(10) . . . . ? N4 C12 N6 N5 0.1(11) . . . . ? C13 C12 N6 N5 -178.2(9) . . . . ? N4 C12 N6 Zn1 -160.8(7) . . . . ? C13 C12 N6 Zn1 20.8(16) . . . . ? C11 N5 N6 C12 -0.2(10) . . . . ? B1 N5 N6 C12 176.0(8) . . . . ? C11 N5 N6 Zn1 166.6(6) . . . . ? B1 N5 N6 Zn1 -17.2(10) . . . . ? N8 C20 N7 C21 -0.1(10) . . . . ? C19 C20 N7 C21 179.9(9) . . . . ? N9 C21 N7 C20 0.1(10) . . . . ? C22 C21 N7 C20 -176.9(8) . . . . ? N7 C20 N8 N9 0.0(10) . . . . ? C19 C20 N8 N9 180.0(8) . . . . ? N7 C20 N8 B1 179.3(8) . . . . ? C19 C20 N8 B1 -0.8(15) . . . . ? N5 B1 N8 C20 -124.2(10) . . . . ? N2 B1 N8 C20 117.0(10) . . . . ? N5 B1 N8 N9 55.0(11) . . . . ? N2 B1 N8 N9 -63.8(10) . . . . ? N7 C21 N9 N8 -0.2(10) . . . . ? C22 C21 N9 N8 176.9(8) . . . . ? N7 C21 N9 Zn1 170.6(7) . . . . ? C22 C21 N9 Zn1 -12.3(15) . . . . ? C20 N8 N9 C21 0.1(9) . . . . ? B1 N8 N9 C21 -179.3(7) . . . . ? C20 N8 N9 Zn1 -173.7(6) . . . . ? B1 N8 N9 Zn1 6.9(9) . . . . ? C30 C29 O1 Zn1 -17.9(14) . . . . ? C28 C29 O1 Zn1 161.3(7) . . . . ? C30 C31 O2 Zn1 8.8(15) . . . . ? C32 C31 O2 Zn1 -173.7(7) . . . . ? C31 O2 Zn1 O1 -20.9(8) . . . . ? C31 O2 Zn1 N3 -125.2(8) . . . . ? C31 O2 Zn1 N6 66.4(10) . . . . ? C31 O2 Zn1 N9 143.7(8) . . . . ? C29 O1 Zn1 O2 25.5(8) . . . . ? C29 O1 Zn1 N3 140.1(8) . . . . ? C29 O1 Zn1 N6 -123.3(8) . . . . ? C29 O1 Zn1 N9 -68.3(13) . . . . ? C3 N3 Zn1 O2 44.6(11) . . . . ? N2 N3 Zn1 O2 -137.8(5) . . . . ? C3 N3 Zn1 O1 -51.1(10) . . . . ? N2 N3 Zn1 O1 126.6(5) . . . . ? C3 N3 Zn1 N6 -141.4(10) . . . . ? N2 N3 Zn1 N6 36.2(6) . . . . ? C3 N3 Zn1 N9 136.2(10) . . . . ? N2 N3 Zn1 N9 -46.2(6) . . . . ? C12 N6 Zn1 O2 -60.2(12) . . . . ? N5 N6 Zn1 O2 139.8(6) . . . . ? C12 N6 Zn1 O1 27.3(10) . . . . ? N5 N6 Zn1 O1 -132.7(6) . . . . ? C12 N6 Zn1 N3 130.5(10) . . . . ? N5 N6 Zn1 N3 -29.6(6) . . . . ? C12 N6 Zn1 N9 -140.0(10) . . . . ? N5 N6 Zn1 N9 60.0(6) . . . . ? C21 N9 Zn1 O2 -14.5(10) . . . . ? N8 N9 Zn1 O2 155.7(6) . . . . ? C21 N9 Zn1 O1 79.1(15) . . . . ? N8 N9 Zn1 O1 -110.7(10) . . . . ? C21 N9 Zn1 N3 -128.5(10) . . . . ? N8 N9 Zn1 N3 41.7(6) . . . . ? C21 N9 Zn1 N6 134.8(10) . . . . ? N8 N9 Zn1 N6 -55.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.692 _refine_diff_density_min -1.791 _refine_diff_density_rms 0.149 data_09mz220_0m _database_code_depnum_ccdc_archive 'CCDC 764049' #TrackingRef '- combined cifs' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H41 B N10 O3 Zn' _chemical_formula_weight 629.90 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 13.9148(16) _cell_length_b 15.3546(16) _cell_length_c 14.7509(15) _cell_angle_alpha 90.00 _cell_angle_beta 103.469(2) _cell_angle_gamma 90.00 _cell_volume 3064.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1518 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 30.94 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.848 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.817 _exptl_absorpt_correction_T_max 0.934 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 20152 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7562 _reflns_number_gt 5589 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4' _computing_data_reduction 'Apex2 v2008.2-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0427P)^2^+0.7447P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7562 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1015 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.79794(18) 0.85499(17) 0.63677(18) 0.0173(5) Uani 1 1 d . . . H1 H 0.7794 0.8835 0.6912 0.021 Uiso 1 1 calc R . . C1 C 0.63972(17) 1.01207(16) 0.59869(17) 0.0247(5) Uani 1 1 d . . . H1A H 0.6648 1.0702 0.5893 0.037 Uiso 1 1 calc R . . H1B H 0.6718 0.9911 0.6611 0.037 Uiso 1 1 calc R . . H1C H 0.5681 1.0150 0.5925 0.037 Uiso 1 1 calc R . . C2 C 0.66155(15) 0.95152(14) 0.52784(15) 0.0179(5) Uani 1 1 d . . . C3 C 0.65743(15) 0.88801(14) 0.39971(15) 0.0171(5) Uani 1 1 d . . . C4 C 0.62060(16) 0.86026(15) 0.29975(15) 0.0199(5) Uani 1 1 d . . . C5 C 0.66009(19) 0.92261(16) 0.23595(17) 0.0278(6) Uani 1 1 d . . . H5A H 0.6413 0.9824 0.2472 0.042 Uiso 1 1 calc R . . H5B H 0.6320 0.9071 0.1707 0.042 Uiso 1 1 calc R . . H5C H 0.7323 0.9182 0.2491 0.042 Uiso 1 1 calc R . . C6 C 0.65199(18) 0.76653(15) 0.28693(16) 0.0233(5) Uani 1 1 d . . . H6A H 0.7242 0.7636 0.2983 0.035 Uiso 1 1 calc R . . H6B H 0.6226 0.7474 0.2231 0.035 Uiso 1 1 calc R . . H6C H 0.6294 0.7285 0.3311 0.035 Uiso 1 1 calc R . . C7 C 0.50753(17) 0.86352(18) 0.27525(17) 0.0292(6) Uani 1 1 d . . . H7A H 0.4822 0.8275 0.3194 0.044 Uiso 1 1 calc R . . H7B H 0.4823 0.8413 0.2119 0.044 Uiso 1 1 calc R . . H7C H 0.4856 0.9238 0.2788 0.044 Uiso 1 1 calc R . . C8 C 0.72060(19) 0.73731(16) 0.78522(17) 0.0259(5) Uani 1 1 d . . . H8A H 0.7791 0.7375 0.8372 0.039 Uiso 1 1 calc R . . H8B H 0.6701 0.6991 0.8003 0.039 Uiso 1 1 calc R . . H8C H 0.6944 0.7966 0.7745 0.039 Uiso 1 1 calc R . . C9 C 0.74823(16) 0.70496(15) 0.69966(16) 0.0191(5) Uani 1 1 d . . . C10 C 0.77949(15) 0.62120(14) 0.59598(15) 0.0171(5) Uani 1 1 d . . . C11 C 0.78831(17) 0.54065(15) 0.54004(16) 0.0211(5) Uani 1 1 d . . . C12 C 0.72194(19) 0.55099(19) 0.44293(19) 0.0368(7) Uani 1 1 d . . . H12A H 0.6543 0.5634 0.4479 0.055 Uiso 1 1 calc R . . H12B H 0.7227 0.4970 0.4076 0.055 Uiso 1 1 calc R . . H12C H 0.7461 0.5992 0.4107 0.055 Uiso 1 1 calc R . . C13 C 0.89533(18) 0.52910(17) 0.53202(18) 0.0280(6) Uani 1 1 d . . . H13A H 0.9145 0.5788 0.4984 0.042 Uiso 1 1 calc R . . H13B H 0.9010 0.4752 0.4980 0.042 Uiso 1 1 calc R . . H13C H 0.9389 0.5259 0.5945 0.042 Uiso 1 1 calc R . . C14 C 0.7569(3) 0.46110(17) 0.5877(2) 0.0487(9) Uani 1 1 d . . . H14A H 0.7985 0.4561 0.6510 0.073 Uiso 1 1 calc R . . H14B H 0.7645 0.4087 0.5521 0.073 Uiso 1 1 calc R . . H14C H 0.6876 0.4673 0.5907 0.073 Uiso 1 1 calc R . . C15 C 0.95758(17) 0.95759(16) 0.78643(16) 0.0255(5) Uani 1 1 d . . . H15A H 1.0170 0.9888 0.8192 0.038 Uiso 1 1 calc R . . H15B H 0.9416 0.9119 0.8270 0.038 Uiso 1 1 calc R . . H15C H 0.9022 0.9985 0.7700 0.038 Uiso 1 1 calc R . . C16 C 0.97559(16) 0.91752(14) 0.70032(15) 0.0181(5) Uani 1 1 d . . . C17 C 1.04323(15) 0.87362(14) 0.59375(15) 0.0166(4) Uani 1 1 d . . . C18 C 1.12053(16) 0.85987(15) 0.53839(16) 0.0200(5) Uani 1 1 d . . . C19 C 1.12733(17) 0.76339(15) 0.51286(18) 0.0250(5) Uani 1 1 d . . . H19A H 1.1458 0.7286 0.5700 0.038 Uiso 1 1 calc R . . H19B H 1.1774 0.7563 0.4764 0.038 Uiso 1 1 calc R . . H19C H 1.0631 0.7437 0.4759 0.038 Uiso 1 1 calc R . . C20 C 1.09257(18) 0.91559(16) 0.45017(17) 0.0273(6) Uani 1 1 d . . . H20A H 1.0286 0.8963 0.4122 0.041 Uiso 1 1 calc R . . H20B H 1.1432 0.9094 0.4142 0.041 Uiso 1 1 calc R . . H20C H 1.0879 0.9768 0.4675 0.041 Uiso 1 1 calc R . . C21 C 1.22093(17) 0.88941(18) 0.59651(18) 0.0299(6) Uani 1 1 d . . . H21A H 1.2188 0.9520 0.6091 0.045 Uiso 1 1 calc R . . H21B H 1.2719 0.8778 0.5621 0.045 Uiso 1 1 calc R . . H21C H 1.2364 0.8574 0.6556 0.045 Uiso 1 1 calc R . . C22 C 0.92064(16) 0.72549(15) 0.30524(16) 0.0192(5) Uani 1 1 d . . . C23 C 0.90493(17) 0.80777(16) 0.26326(17) 0.0245(5) Uani 1 1 d . . . H23 H 0.8810 0.8540 0.2947 0.029 Uiso 1 1 calc R . . C24 C 0.92379(19) 0.82228(18) 0.17705(18) 0.0309(6) Uani 1 1 d . . . H24 H 0.9117 0.8780 0.1486 0.037 Uiso 1 1 calc R . . C25 C 0.96051(19) 0.75541(19) 0.13187(18) 0.0315(6) Uani 1 1 d . . . C26 C 0.97843(19) 0.67432(18) 0.17205(17) 0.0301(6) Uani 1 1 d . . . H26 H 1.0038 0.6289 0.1406 0.036 Uiso 1 1 calc R . . C27 C 0.95941(17) 0.65959(15) 0.25766(17) 0.0232(5) Uani 1 1 d . . . H27 H 0.9726 0.6038 0.2856 0.028 Uiso 1 1 calc R . . N1 N 0.61320(13) 0.95149(12) 0.43852(13) 0.0201(4) Uani 1 1 d . . . N2 N 0.73385(13) 0.89158(12) 0.54432(12) 0.0167(4) Uani 1 1 d . . . N3 N 0.73273(13) 0.85143(12) 0.46012(12) 0.0167(4) Uani 1 1 d . . . N4 N 0.74533(14) 0.62137(12) 0.67476(13) 0.0204(4) Uani 1 1 d . . . N5 N 0.78203(13) 0.75510(12) 0.63970(12) 0.0164(4) Uani 1 1 d . . . N6 N 0.80347(13) 0.70067(12) 0.57235(12) 0.0164(4) Uani 1 1 d . . . N7 N 1.06080(13) 0.91991(12) 0.67354(13) 0.0188(4) Uani 1 1 d . . . N8 N 0.90752(13) 0.87220(12) 0.63916(12) 0.0158(4) Uani 1 1 d . . . N9 N 0.95073(13) 0.84332(11) 0.56940(12) 0.0156(4) Uani 1 1 d . . . N10 N 0.9808(2) 0.7717(2) 0.04126(18) 0.0540(8) Uani 1 1 d . . . O1 O 0.89999(12) 0.70640(10) 0.38550(11) 0.0229(4) Uani 1 1 d . . . O2 O 0.9606(2) 0.8436(2) 0.00558(18) 0.0923(11) Uani 1 1 d . . . O3 O 1.0179(2) 0.71346(19) 0.00422(17) 0.0847(10) Uani 1 1 d . . . Zn1 Zn 0.851048(18) 0.769753(17) 0.473489(17) 0.01639(8) 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 B1 0.0167(11) 0.0196(13) 0.0160(12) -0.0008(10) 0.0048(9) 0.0005(10) C1 0.0207(11) 0.0262(13) 0.0268(13) -0.0078(11) 0.0045(10) 0.0023(10) C2 0.0130(10) 0.0195(11) 0.0212(11) -0.0012(9) 0.0041(8) -0.0014(8) C3 0.0160(10) 0.0161(11) 0.0195(11) 0.0010(9) 0.0050(9) -0.0021(8) C4 0.0220(11) 0.0213(12) 0.0164(11) 0.0000(9) 0.0042(9) 0.0018(9) C5 0.0348(14) 0.0279(13) 0.0214(12) 0.0036(11) 0.0078(10) 0.0046(11) C6 0.0301(12) 0.0215(12) 0.0173(11) -0.0020(10) 0.0036(9) -0.0014(10) C7 0.0242(12) 0.0391(15) 0.0213(12) -0.0062(11) -0.0008(10) 0.0044(11) C8 0.0368(14) 0.0231(12) 0.0227(13) -0.0013(10) 0.0171(11) 0.0000(11) C9 0.0198(11) 0.0211(12) 0.0173(11) 0.0004(9) 0.0060(9) -0.0001(9) C10 0.0155(10) 0.0180(11) 0.0181(11) 0.0002(9) 0.0045(8) -0.0006(9) C11 0.0238(12) 0.0176(11) 0.0243(12) -0.0027(10) 0.0104(10) -0.0017(9) C12 0.0309(14) 0.0380(16) 0.0366(16) -0.0196(13) -0.0020(12) 0.0033(12) C13 0.0261(12) 0.0278(13) 0.0299(14) -0.0057(11) 0.0061(10) 0.0049(10) C14 0.083(2) 0.0180(14) 0.059(2) -0.0059(14) 0.0455(19) -0.0125(15) C15 0.0254(12) 0.0262(13) 0.0228(12) -0.0060(10) 0.0013(10) -0.0016(10) C16 0.0199(11) 0.0153(11) 0.0177(11) 0.0021(9) 0.0014(9) 0.0023(9) C17 0.0183(10) 0.0120(10) 0.0193(11) 0.0049(9) 0.0042(9) 0.0006(8) C18 0.0182(11) 0.0198(12) 0.0234(12) 0.0038(9) 0.0078(9) 0.0006(9) C19 0.0253(12) 0.0214(12) 0.0326(14) 0.0028(11) 0.0150(11) 0.0046(10) C20 0.0316(13) 0.0257(13) 0.0281(13) 0.0076(11) 0.0142(11) 0.0050(11) C21 0.0189(12) 0.0398(16) 0.0324(14) 0.0012(12) 0.0086(10) -0.0055(11) C22 0.0161(10) 0.0233(12) 0.0189(11) -0.0045(10) 0.0054(8) -0.0009(9) C23 0.0272(12) 0.0205(12) 0.0277(13) -0.0026(10) 0.0102(10) 0.0053(10) C24 0.0324(14) 0.0319(15) 0.0311(14) 0.0131(12) 0.0127(11) 0.0101(11) C25 0.0300(13) 0.0451(17) 0.0224(13) 0.0051(12) 0.0119(11) 0.0075(12) C26 0.0316(13) 0.0356(15) 0.0258(14) -0.0070(12) 0.0119(11) 0.0077(11) C27 0.0267(12) 0.0177(12) 0.0263(13) -0.0036(10) 0.0086(10) 0.0017(10) N1 0.0172(9) 0.0198(10) 0.0221(10) -0.0039(8) 0.0020(8) 0.0009(8) N2 0.0169(9) 0.0173(9) 0.0163(9) -0.0030(8) 0.0045(7) -0.0008(7) N3 0.0167(9) 0.0188(10) 0.0152(9) -0.0017(7) 0.0048(7) -0.0002(7) N4 0.0232(10) 0.0190(10) 0.0212(10) 0.0008(8) 0.0098(8) -0.0013(8) N5 0.0181(9) 0.0187(10) 0.0137(9) -0.0010(7) 0.0067(7) -0.0006(7) N6 0.0177(9) 0.0178(9) 0.0145(9) -0.0027(7) 0.0054(7) 0.0002(7) N7 0.0176(9) 0.0159(9) 0.0221(10) 0.0009(8) 0.0030(7) 0.0005(7) N8 0.0175(9) 0.0157(9) 0.0142(9) -0.0006(7) 0.0036(7) 0.0018(7) N9 0.0175(9) 0.0156(9) 0.0149(9) 0.0012(7) 0.0065(7) 0.0011(7) N10 0.0590(17) 0.077(2) 0.0315(14) 0.0189(15) 0.0227(13) 0.0294(16) O1 0.0269(8) 0.0230(9) 0.0223(9) 0.0005(7) 0.0129(7) 0.0034(7) O2 0.125(3) 0.110(2) 0.0615(17) 0.0603(17) 0.0615(17) 0.068(2) O3 0.130(3) 0.098(2) 0.0449(15) 0.0157(14) 0.0591(17) 0.0551(19) Zn1 0.01754(13) 0.01764(14) 0.01511(13) -0.00050(11) 0.00607(9) 0.00044(11) _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 B1 N8 1.540(3) . ? B1 N2 1.550(3) . ? B1 N5 1.552(3) . ? B1 H1 1.0000 . ? C1 C2 1.482(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.332(3) . ? C2 N2 1.343(3) . ? C3 N3 1.331(3) . ? C3 N1 1.349(3) . ? C3 C4 1.505(3) . ? C4 C6 1.529(3) . ? C4 C7 1.531(3) . ? C4 C5 1.531(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.488(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N4 1.333(3) . ? C9 N5 1.338(3) . ? C10 N6 1.333(3) . ? C10 N4 1.354(3) . ? C10 C11 1.508(3) . ? C11 C12 1.521(3) . ? C11 C14 1.523(3) . ? C11 C13 1.531(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.484(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N7 1.335(3) . ? C16 N8 1.341(3) . ? C17 N9 1.337(3) . ? C17 N7 1.348(3) . ? C17 C18 1.509(3) . ? C18 C21 1.528(3) . ? C18 C20 1.530(3) . ? C18 C19 1.537(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 O1 1.315(3) . ? C22 C23 1.401(3) . ? C22 C27 1.408(3) . ? C23 C24 1.375(3) . ? C23 H23 0.9500 . ? C24 C25 1.385(4) . ? C24 H24 0.9500 . ? C25 C26 1.377(4) . ? C25 N10 1.450(3) . ? C26 C27 1.368(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? N2 N3 1.383(2) . ? N3 Zn1 2.0423(18) . ? N5 N6 1.383(2) . ? N6 Zn1 2.0347(19) . ? N8 N9 1.380(2) . ? N9 Zn1 2.0705(18) . ? N10 O3 1.223(3) . ? N10 O2 1.227(3) . ? O1 Zn1 1.8726(16) . ? 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 N8 B1 N2 108.76(18) . . ? N8 B1 N5 108.42(18) . . ? N2 B1 N5 109.03(18) . . ? N8 B1 H1 110.2 . . ? N2 B1 H1 110.2 . . ? N5 B1 H1 110.2 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 N2 111.29(19) . . ? N1 C2 C1 123.9(2) . . ? N2 C2 C1 124.8(2) . . ? N3 C3 N1 112.73(19) . . ? N3 C3 C4 124.9(2) . . ? N1 C3 C4 122.36(19) . . ? C3 C4 C6 110.23(18) . . ? C3 C4 C7 108.58(19) . . ? C6 C4 C7 108.01(19) . . ? C3 C4 C5 109.63(19) . . ? C6 C4 C5 111.03(19) . . ? C7 C4 C5 109.31(19) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N4 C9 N5 111.4(2) . . ? N4 C9 C8 123.9(2) . . ? N5 C9 C8 124.7(2) . . ? N6 C10 N4 112.46(19) . . ? N6 C10 C11 123.42(19) . . ? N4 C10 C11 124.1(2) . . ? C10 C11 C12 108.71(19) . . ? C10 C11 C14 109.7(2) . . ? C12 C11 C14 110.0(2) . . ? C10 C11 C13 109.99(19) . . ? C12 C11 C13 109.1(2) . . ? C14 C11 C13 109.3(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N7 C16 N8 110.63(19) . . ? N7 C16 C15 125.5(2) . . ? N8 C16 C15 123.9(2) . . ? N9 C17 N7 112.69(19) . . ? N9 C17 C18 124.7(2) . . ? N7 C17 C18 122.62(19) . . ? C17 C18 C21 109.19(19) . . ? C17 C18 C20 108.05(18) . . ? C21 C18 C20 109.2(2) . . ? C17 C18 C19 111.08(18) . . ? C21 C18 C19 108.86(19) . . ? C20 C18 C19 110.4(2) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O1 C22 C23 123.7(2) . . ? O1 C22 C27 118.5(2) . . ? C23 C22 C27 117.8(2) . . ? C24 C23 C22 120.7(2) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 119.7(2) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C26 C25 C24 120.9(2) . . ? C26 C25 N10 119.9(3) . . ? C24 C25 N10 119.2(2) . . ? C27 C26 C25 119.5(2) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C26 C27 C22 121.3(2) . . ? C26 C27 H27 119.3 . . ? C22 C27 H27 119.3 . . ? C2 N1 C3 104.16(18) . . ? C2 N2 N3 106.95(17) . . ? C2 N2 B1 131.34(19) . . ? N3 N2 B1 120.80(17) . . ? C3 N3 N2 104.80(17) . . ? C3 N3 Zn1 144.56(16) . . ? N2 N3 Zn1 110.28(13) . . ? C9 N4 C10 104.13(19) . . ? C9 N5 N6 107.15(17) . . ? C9 N5 B1 131.43(19) . . ? N6 N5 B1 121.42(17) . . ? C10 N6 N5 104.86(17) . . ? C10 N6 Zn1 143.89(16) . . ? N5 N6 Zn1 111.13(13) . . ? C16 N7 C17 104.54(18) . . ? C16 N8 N9 107.83(17) . . ? C16 N8 B1 130.18(19) . . ? N9 N8 B1 121.92(17) . . ? C17 N9 N8 104.32(17) . . ? C17 N9 Zn1 145.42(15) . . ? N8 N9 Zn1 110.23(12) . . ? O3 N10 O2 123.0(3) . . ? O3 N10 C25 118.6(3) . . ? O2 N10 C25 118.4(3) . . ? C22 O1 Zn1 134.37(15) . . ? O1 Zn1 N6 117.23(7) . . ? O1 Zn1 N3 131.85(7) . . ? N6 Zn1 N3 89.99(7) . . ? O1 Zn1 N9 117.59(7) . . ? N6 Zn1 N9 94.17(7) . . ? N3 Zn1 N9 97.33(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 C3 C4 C6 21.8(3) . . . . ? N1 C3 C4 C6 -155.2(2) . . . . ? N3 C3 C4 C7 139.9(2) . . . . ? N1 C3 C4 C7 -37.0(3) . . . . ? N3 C3 C4 C5 -100.7(2) . . . . ? N1 C3 C4 C5 82.3(3) . . . . ? N6 C10 C11 C12 -60.9(3) . . . . ? N4 C10 C11 C12 118.2(2) . . . . ? N6 C10 C11 C14 178.8(2) . . . . ? N4 C10 C11 C14 -2.1(3) . . . . ? N6 C10 C11 C13 58.5(3) . . . . ? N4 C10 C11 C13 -122.4(2) . . . . ? N9 C17 C18 C21 -169.8(2) . . . . ? N7 C17 C18 C21 11.3(3) . . . . ? N9 C17 C18 C20 71.5(3) . . . . ? N7 C17 C18 C20 -107.4(2) . . . . ? N9 C17 C18 C19 -49.8(3) . . . . ? N7 C17 C18 C19 131.4(2) . . . . ? O1 C22 C23 C24 -176.9(2) . . . . ? C27 C22 C23 C24 2.2(3) . . . . ? C22 C23 C24 C25 -1.3(4) . . . . ? C23 C24 C25 C26 0.0(4) . . . . ? C23 C24 C25 N10 -179.6(3) . . . . ? C24 C25 C26 C27 0.2(4) . . . . ? N10 C25 C26 C27 179.8(2) . . . . ? C25 C26 C27 C22 0.8(4) . . . . ? O1 C22 C27 C26 177.2(2) . . . . ? C23 C22 C27 C26 -1.9(3) . . . . ? N2 C2 N1 C3 0.8(2) . . . . ? C1 C2 N1 C3 179.1(2) . . . . ? N3 C3 N1 C2 -2.3(2) . . . . ? C4 C3 N1 C2 175.0(2) . . . . ? N1 C2 N2 N3 0.9(2) . . . . ? C1 C2 N2 N3 -177.4(2) . . . . ? N1 C2 N2 B1 -168.0(2) . . . . ? C1 C2 N2 B1 13.8(4) . . . . ? N8 B1 N2 C2 -121.4(2) . . . . ? N5 B1 N2 C2 120.6(2) . . . . ? N8 B1 N2 N3 71.1(2) . . . . ? N5 B1 N2 N3 -47.0(3) . . . . ? N1 C3 N3 N2 2.8(2) . . . . ? C4 C3 N3 N2 -174.4(2) . . . . ? N1 C3 N3 Zn1 -168.97(19) . . . . ? C4 C3 N3 Zn1 13.8(4) . . . . ? C2 N2 N3 C3 -2.2(2) . . . . ? B1 N2 N3 C3 168.08(18) . . . . ? C2 N2 N3 Zn1 172.75(13) . . . . ? B1 N2 N3 Zn1 -17.0(2) . . . . ? N5 C9 N4 C10 0.2(2) . . . . ? C8 C9 N4 C10 -177.8(2) . . . . ? N6 C10 N4 C9 0.4(2) . . . . ? C11 C10 N4 C9 -178.8(2) . . . . ? N4 C9 N5 N6 -0.7(2) . . . . ? C8 C9 N5 N6 177.3(2) . . . . ? N4 C9 N5 B1 179.1(2) . . . . ? C8 C9 N5 B1 -2.9(4) . . . . ? N8 B1 N5 C9 121.6(2) . . . . ? N2 B1 N5 C9 -120.1(2) . . . . ? N8 B1 N5 N6 -58.5(2) . . . . ? N2 B1 N5 N6 59.7(2) . . . . ? N4 C10 N6 N5 -0.8(2) . . . . ? C11 C10 N6 N5 178.40(19) . . . . ? N4 C10 N6 Zn1 -176.01(18) . . . . ? C11 C10 N6 Zn1 3.2(4) . . . . ? C9 N5 N6 C10 0.9(2) . . . . ? B1 N5 N6 C10 -178.96(18) . . . . ? C9 N5 N6 Zn1 177.87(13) . . . . ? B1 N5 N6 Zn1 -2.0(2) . . . . ? N8 C16 N7 C17 -0.5(2) . . . . ? C15 C16 N7 C17 178.4(2) . . . . ? N9 C17 N7 C16 0.6(2) . . . . ? C18 C17 N7 C16 179.56(19) . . . . ? N7 C16 N8 N9 0.3(2) . . . . ? C15 C16 N8 N9 -178.7(2) . . . . ? N7 C16 N8 B1 -176.7(2) . . . . ? C15 C16 N8 B1 4.3(4) . . . . ? N2 B1 N8 C16 120.6(2) . . . . ? N5 B1 N8 C16 -121.0(2) . . . . ? N2 B1 N8 N9 -56.1(2) . . . . ? N5 B1 N8 N9 62.3(2) . . . . ? N7 C17 N9 N8 -0.4(2) . . . . ? C18 C17 N9 N8 -179.36(19) . . . . ? N7 C17 N9 Zn1 -177.91(18) . . . . ? C18 C17 N9 Zn1 3.1(4) . . . . ? C16 N8 N9 C17 0.1(2) . . . . ? B1 N8 N9 C17 177.37(18) . . . . ? C16 N8 N9 Zn1 178.55(13) . . . . ? B1 N8 N9 Zn1 -4.1(2) . . . . ? C26 C25 N10 O3 -3.3(5) . . . . ? C24 C25 N10 O3 176.3(3) . . . . ? C26 C25 N10 O2 177.3(3) . . . . ? C24 C25 N10 O2 -3.1(5) . . . . ? C23 C22 O1 Zn1 -2.3(3) . . . . ? C27 C22 O1 Zn1 178.67(16) . . . . ? C22 O1 Zn1 N6 166.30(19) . . . . ? C22 O1 Zn1 N3 48.9(2) . . . . ? C22 O1 Zn1 N9 -82.5(2) . . . . ? C10 N6 Zn1 O1 -13.1(3) . . . . ? N5 N6 Zn1 O1 171.87(12) . . . . ? C10 N6 Zn1 N3 125.5(3) . . . . ? N5 N6 Zn1 N3 -49.52(13) . . . . ? C10 N6 Zn1 N9 -137.1(2) . . . . ? N5 N6 Zn1 N9 47.83(13) . . . . ? C3 N3 Zn1 O1 -0.9(3) . . . . ? N2 N3 Zn1 O1 -172.44(12) . . . . ? C3 N3 Zn1 N6 -128.8(3) . . . . ? N2 N3 Zn1 N6 59.68(14) . . . . ? C3 N3 Zn1 N9 137.0(3) . . . . ? N2 N3 Zn1 N9 -34.53(14) . . . . ? C17 N9 Zn1 O1 8.8(3) . . . . ? N8 N9 Zn1 O1 -168.65(12) . . . . ? C17 N9 Zn1 N6 132.5(3) . . . . ? N8 N9 Zn1 N6 -44.89(13) . . . . ? C17 N9 Zn1 N3 -136.9(3) . . . . ? N8 N9 Zn1 N3 45.63(14) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.468 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.072 data_09mz218_0m _database_code_depnum_ccdc_archive 'CCDC 764050' #TrackingRef '- combined cifs' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H38 B F6 N9 O Zn' _chemical_formula_weight 658.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 41.250(2) _cell_length_b 44.237(3) _cell_length_c 14.6555(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 26743(3) _cell_formula_units_Z 32 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6659 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 26.73 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10944 _exptl_absorpt_coefficient_mu 0.800 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.779 _exptl_absorpt_correction_T_max 0.916 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; Small solvent filled voids are present in the structure. The positions of the solvent molecules are however not well defined and no satisfying solvent model could be developed. The electron density within in the voids was thus corrected for using the SQUEEZE procedcure implemeneted in Platon (Spek, 2009) (see squeeze report appended to this cif file). ; _diffrn_ambient_temperature 100(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 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 32020 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0684 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -58 _diffrn_reflns_limit_k_max 58 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 28.28 _reflns_number_total 12986 _reflns_number_gt 10738 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4' _computing_data_reduction 'Apex2 v2008.2-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0468P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 4605 Friedel pairs' _refine_ls_abs_structure_Flack 0.012(7) _refine_ls_number_reflns 12986 _refine_ls_number_parameters 782 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.0992 _refine_ls_wR_factor_gt 0.0945 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 B1 B 0.91830(8) 0.10822(7) 0.5574(3) 0.0208(7) Uani 1 1 d . . . H1 H 0.9383 0.0965 0.5732 0.025 Uiso 1 1 calc R . . B2 B 0.93093(8) 0.26373(6) 0.8456(2) 0.0193(7) Uani 1 1 d . . . H2 H 0.9502 0.2740 0.8181 0.023 Uiso 1 1 calc R . . C1 C 0.98243(7) 0.14288(6) 0.6238(2) 0.0281(7) Uani 1 1 d . . . H1A H 0.9906 0.1309 0.5724 0.042 Uiso 1 1 calc R . . H1B H 0.9791 0.1297 0.6766 0.042 Uiso 1 1 calc R . . H1C H 0.9982 0.1586 0.6392 0.042 Uiso 1 1 calc R . . C2 C 0.95066(7) 0.15734(6) 0.5977(2) 0.0196(6) Uani 1 1 d . . . C3 C 0.91467(7) 0.18969(5) 0.56555(19) 0.0171(6) Uani 1 1 d . . . C4 C 0.89780(7) 0.21927(5) 0.5498(2) 0.0204(6) Uani 1 1 d . . . C5 C 0.92188(8) 0.24546(6) 0.5581(3) 0.0310(8) Uani 1 1 d . . . H5A H 0.9392 0.2429 0.5130 0.046 Uiso 1 1 calc R . . H5B H 0.9312 0.2456 0.6196 0.046 Uiso 1 1 calc R . . H5C H 0.9106 0.2646 0.5471 0.046 Uiso 1 1 calc R . . C6 C 0.87098(7) 0.22304(6) 0.6203(2) 0.0268(7) Uani 1 1 d . . . H6A H 0.8589 0.2417 0.6077 0.040 Uiso 1 1 calc R . . H6B H 0.8806 0.2242 0.6814 0.040 Uiso 1 1 calc R . . H6C H 0.8562 0.2057 0.6172 0.040 Uiso 1 1 calc R . . C7 C 0.88369(8) 0.21903(6) 0.4530(2) 0.0266(7) Uani 1 1 d . . . H7A H 0.9013 0.2166 0.4086 0.040 Uiso 1 1 calc R . . H7B H 0.8724 0.2381 0.4415 0.040 Uiso 1 1 calc R . . H7C H 0.8684 0.2022 0.4469 0.040 Uiso 1 1 calc R . . C8 C 0.91536(8) 0.05662(6) 0.7128(2) 0.0311(8) Uani 1 1 d . . . H8A H 0.9091 0.0470 0.7704 0.047 Uiso 1 1 calc R . . H8B H 0.9338 0.0701 0.7234 0.047 Uiso 1 1 calc R . . H8C H 0.9215 0.0410 0.6685 0.047 Uiso 1 1 calc R . . C9 C 0.88744(7) 0.07438(5) 0.6765(2) 0.0231(7) Uani 1 1 d . . . C10 C 0.83972(7) 0.08984(6) 0.6517(2) 0.0213(6) Uani 1 1 d . . . C11 C 0.80318(7) 0.09227(6) 0.6565(2) 0.0245(7) Uani 1 1 d . . . C12 C 0.78885(8) 0.09856(7) 0.5613(2) 0.0299(8) Uani 1 1 d . . . H12A H 0.7968 0.1181 0.5389 0.045 Uiso 1 1 calc R . . H12B H 0.7651 0.0991 0.5652 0.045 Uiso 1 1 calc R . . H12C H 0.7955 0.0825 0.5191 0.045 Uiso 1 1 calc R . . C13 C 0.78935(8) 0.06271(6) 0.6913(2) 0.0313(8) Uani 1 1 d . . . H13A H 0.7970 0.0461 0.6527 0.047 Uiso 1 1 calc R . . H13B H 0.7656 0.0636 0.6894 0.047 Uiso 1 1 calc R . . H13C H 0.7965 0.0594 0.7542 0.047 Uiso 1 1 calc R . . C14 C 0.79463(8) 0.11781(7) 0.7222(3) 0.0359(8) Uani 1 1 d . . . H14A H 0.8018 0.1124 0.7839 0.054 Uiso 1 1 calc R . . H14B H 0.7711 0.1210 0.7222 0.054 Uiso 1 1 calc R . . H14C H 0.8055 0.1364 0.7028 0.054 Uiso 1 1 calc R . . C15 C 0.95783(8) 0.07392(8) 0.4015(3) 0.0394(9) Uani 1 1 d . . . H15A H 0.9542 0.0563 0.4406 0.059 Uiso 1 1 calc R . . H15B H 0.9737 0.0874 0.4304 0.059 Uiso 1 1 calc R . . H15C H 0.9661 0.0672 0.3422 0.059 Uiso 1 1 calc R . . C16 C 0.92693(8) 0.09032(6) 0.3884(2) 0.0279(7) Uani 1 1 d . . . C17 C 0.88467(8) 0.10912(6) 0.3284(2) 0.0241(7) Uani 1 1 d . . . C18 C 0.85934(7) 0.11715(6) 0.2586(2) 0.0244(7) Uani 1 1 d . . . C19 C 0.86662(9) 0.14968(7) 0.2250(3) 0.0356(9) Uani 1 1 d . . . H19A H 0.8651 0.1638 0.2764 0.053 Uiso 1 1 calc R . . H19B H 0.8509 0.1554 0.1780 0.053 Uiso 1 1 calc R . . H19C H 0.8885 0.1505 0.1993 0.053 Uiso 1 1 calc R . . C20 C 0.82542(8) 0.11552(7) 0.2982(3) 0.0340(8) Uani 1 1 d . . . H20A H 0.8212 0.0949 0.3199 0.051 Uiso 1 1 calc R . . H20B H 0.8096 0.1209 0.2510 0.051 Uiso 1 1 calc R . . H20C H 0.8236 0.1297 0.3492 0.051 Uiso 1 1 calc R . . C21 C 0.86237(9) 0.09577(7) 0.1774(3) 0.0380(9) Uani 1 1 d . . . H21A H 0.8837 0.0983 0.1490 0.057 Uiso 1 1 calc R . . H21B H 0.8454 0.1004 0.1326 0.057 Uiso 1 1 calc R . . H21C H 0.8599 0.0748 0.1982 0.057 Uiso 1 1 calc R . . C22 C 0.80386(8) 0.19001(6) 0.4828(3) 0.0326(8) Uani 1 1 d . . . H22 H 0.8199 0.2059 0.5000 0.039 Uiso 1 1 calc R . . C23 C 0.79177(10) 0.19702(8) 0.3863(3) 0.0412(9) Uani 1 1 d . . . C24 C 0.77665(9) 0.19088(7) 0.5517(3) 0.0387(9) Uani 1 1 d . . . C25 C 0.98257(9) 0.29757(9) 0.9708(3) 0.0428(9) Uani 1 1 d . . . H25A H 0.9787 0.3191 0.9590 0.064 Uiso 1 1 calc R . . H25B H 0.9895 0.2876 0.9142 0.064 Uiso 1 1 calc R . . H25C H 0.9996 0.2954 1.0170 0.064 Uiso 1 1 calc R . . C26 C 0.95186(7) 0.28313(6) 1.0047(2) 0.0264(7) Uani 1 1 d . . . C27 C 0.91469(8) 0.26623(6) 1.0892(2) 0.0244(7) Uani 1 1 d . . . C28 C 0.89551(8) 0.26007(6) 1.1742(2) 0.0271(7) Uani 1 1 d . . . C29 C 0.88376(8) 0.22723(6) 1.1763(3) 0.0288(7) Uani 1 1 d . . . H29A H 0.8693 0.2236 1.1243 0.043 Uiso 1 1 calc R . . H29B H 0.8720 0.2235 1.2333 0.043 Uiso 1 1 calc R . . H29C H 0.9024 0.2136 1.1726 0.043 Uiso 1 1 calc R . . C30 C 0.86689(9) 0.28178(7) 1.1765(3) 0.0468(10) Uani 1 1 d . . . H30A H 0.8749 0.3026 1.1758 0.070 Uiso 1 1 calc R . . H30B H 0.8542 0.2784 1.2322 0.070 Uiso 1 1 calc R . . H30C H 0.8531 0.2783 1.1230 0.070 Uiso 1 1 calc R . . C31 C 0.91676(10) 0.26604(8) 1.2581(3) 0.0481(10) Uani 1 1 d . . . H31A H 0.9363 0.2535 1.2549 0.072 Uiso 1 1 calc R . . H31B H 0.9046 0.2610 1.3135 0.072 Uiso 1 1 calc R . . H31C H 0.9230 0.2874 1.2596 0.072 Uiso 1 1 calc R . . C32 C 0.92017(7) 0.31538(6) 0.6925(2) 0.0266(7) Uani 1 1 d . . . H32A H 0.9241 0.3345 0.7242 0.040 Uiso 1 1 calc R . . H32B H 0.9132 0.3195 0.6298 0.040 Uiso 1 1 calc R . . H32C H 0.9402 0.3035 0.6915 0.040 Uiso 1 1 calc R . . C33 C 0.89439(7) 0.29810(5) 0.7412(2) 0.0202(6) Uani 1 1 d . . . C34 C 0.84838(7) 0.28363(6) 0.7870(2) 0.0196(6) Uani 1 1 d . . . C35 C 0.81226(7) 0.28132(7) 0.8000(2) 0.0282(7) Uani 1 1 d . . . C36 C 0.80431(8) 0.28574(7) 0.9006(2) 0.0311(8) Uani 1 1 d . . . H36A H 0.8154 0.2702 0.9368 0.047 Uiso 1 1 calc R . . H36B H 0.7808 0.2840 0.9096 0.047 Uiso 1 1 calc R . . H36C H 0.8116 0.3058 0.9201 0.047 Uiso 1 1 calc R . . C37 C 0.79505(9) 0.30601(9) 0.7461(3) 0.0487(11) Uani 1 1 d . . . H37A H 0.8024 0.3259 0.7675 0.073 Uiso 1 1 calc R . . H37B H 0.7716 0.3042 0.7550 0.073 Uiso 1 1 calc R . . H37C H 0.8001 0.3038 0.6811 0.073 Uiso 1 1 calc R . . C38 C 0.80123(8) 0.25010(8) 0.7667(3) 0.0383(9) Uani 1 1 d . . . H38A H 0.8044 0.2487 0.7006 0.057 Uiso 1 1 calc R . . H38B H 0.7782 0.2473 0.7810 0.057 Uiso 1 1 calc R . . H38C H 0.8140 0.2344 0.7972 0.057 Uiso 1 1 calc R . . C39 C 0.98746(7) 0.22466(6) 0.7562(2) 0.0245(7) Uani 1 1 d . . . H39A H 1.0013 0.2081 0.7352 0.037 Uiso 1 1 calc R . . H39B H 0.9993 0.2369 0.8008 0.037 Uiso 1 1 calc R . . H39C H 0.9813 0.2373 0.7040 0.037 Uiso 1 1 calc R . . C40 C 0.95795(7) 0.21211(6) 0.7992(2) 0.0195(6) Uani 1 1 d . . . C41 C 0.92216(7) 0.18213(5) 0.8507(2) 0.0183(6) Uani 1 1 d . . . C42 C 0.90470(8) 0.15309(6) 0.8738(2) 0.0231(7) Uani 1 1 d . . . C43 C 0.92761(9) 0.12613(6) 0.8568(3) 0.0365(9) Uani 1 1 d . . . H43A H 0.9332 0.1252 0.7918 0.055 Uiso 1 1 calc R . . H43B H 0.9168 0.1073 0.8747 0.055 Uiso 1 1 calc R . . H43C H 0.9474 0.1287 0.8929 0.055 Uiso 1 1 calc R . . C44 C 0.87511(8) 0.15047(7) 0.8110(3) 0.0341(8) Uani 1 1 d . . . H44A H 0.8606 0.1676 0.8216 0.051 Uiso 1 1 calc R . . H44B H 0.8636 0.1316 0.8240 0.051 Uiso 1 1 calc R . . H44C H 0.8823 0.1505 0.7472 0.051 Uiso 1 1 calc R . . C45 C 0.89420(9) 0.15301(7) 0.9739(2) 0.0323(8) Uani 1 1 d . . . H45A H 0.9131 0.1564 1.0129 0.048 Uiso 1 1 calc R . . H45B H 0.8844 0.1334 0.9888 0.048 Uiso 1 1 calc R . . H45C H 0.8783 0.1691 0.9841 0.048 Uiso 1 1 calc R . . C46 C 0.80713(9) 0.20924(8) 0.9818(3) 0.0409(10) Uani 1 1 d . . . H46 H 0.7985 0.2251 0.9395 0.049 Uiso 1 1 calc R . . C47 C 0.79482(10) 0.17847(8) 0.9465(4) 0.0516(12) Uani 1 1 d . . . C48 C 0.79402(9) 0.21665(8) 1.0776(3) 0.0396(9) Uani 1 1 d . . . F1 F 0.78885(6) 0.18684(5) 0.63634(17) 0.0542(6) Uani 1 1 d . . . F2 F 0.75461(5) 0.16904(5) 0.53913(19) 0.0571(7) Uani 1 1 d . . . F3 F 0.76101(6) 0.21682(5) 0.55370(18) 0.0601(7) Uani 1 1 d . . . F4 F 0.77783(7) 0.22417(5) 0.38075(19) 0.0688(8) Uani 1 1 d . . . F5 F 0.77076(6) 0.17729(6) 0.3561(2) 0.0689(8) Uani 1 1 d . . . F6 F 0.81667(6) 0.19739(5) 0.32863(16) 0.0564(6) Uani 1 1 d . . . F7 F 0.80170(7) 0.17654(6) 0.8583(2) 0.0815(9) Uani 1 1 d . . . F8 F 0.81076(6) 0.15553(5) 0.9857(2) 0.0753(9) Uani 1 1 d . . . F9 F 0.76404(6) 0.17497(5) 0.9568(2) 0.0717(9) Uani 1 1 d . . . F10 F 0.80171(8) 0.19437(7) 1.1371(2) 0.0894(10) Uani 1 1 d . . . F11 F 0.76269(6) 0.21887(6) 1.0794(2) 0.0717(8) Uani 1 1 d . . . F12 F 0.80689(6) 0.24231(5) 1.10775(18) 0.0557(7) Uani 1 1 d . . . N1 N 0.90010(6) 0.16276(5) 0.55563(17) 0.0186(5) Uani 1 1 d . . . N2 N 0.92396(6) 0.14213(4) 0.57624(17) 0.0183(5) Uani 1 1 d . . . N3 N 0.94588(6) 0.18721(5) 0.59272(18) 0.0199(5) Uani 1 1 d . . . N4 N 0.85842(6) 0.10706(5) 0.59874(17) 0.0189(5) Uani 1 1 d . . . N5 N 0.88949(6) 0.09654(5) 0.61409(18) 0.0204(5) Uani 1 1 d . . . N6 N 0.85673(6) 0.06973(5) 0.70071(18) 0.0238(6) Uani 1 1 d . . . N7 N 0.88316(6) 0.11701(5) 0.41616(18) 0.0212(5) Uani 1 1 d . . . N8 N 0.91070(6) 0.10456(5) 0.45503(18) 0.0221(6) Uani 1 1 d . . . N9 N 0.91142(7) 0.09288(6) 0.3091(2) 0.0310(7) Uani 1 1 d . . . N10 N 0.90615(6) 0.25797(4) 1.00541(18) 0.0189(5) Uani 1 1 d . . . N11 N 0.93035(6) 0.26908(5) 0.94944(17) 0.0201(6) Uani 1 1 d . . . N12 N 0.94297(7) 0.28201(6) 1.0905(2) 0.0293(6) Uani 1 1 d . . . N13 N 0.86957(6) 0.26665(5) 0.83279(18) 0.0184(5) Uani 1 1 d . . . N14 N 0.89969(6) 0.27624(5) 0.80297(17) 0.0169(5) Uani 1 1 d . . . N15 N 0.86288(6) 0.30321(5) 0.72967(18) 0.0227(6) Uani 1 1 d . . . N16 N 0.90980(6) 0.20978(5) 0.86550(17) 0.0190(5) Uani 1 1 d . . . N17 N 0.93330(5) 0.22927(5) 0.83022(17) 0.0170(5) Uani 1 1 d . . . N18 N 0.95159(6) 0.18294(5) 0.81083(18) 0.0213(5) Uani 1 1 d . . . O1 O 0.81969(5) 0.16280(4) 0.48194(17) 0.0326(6) Uani 1 1 d . . . O2 O 0.83954(5) 0.21060(5) 0.97740(18) 0.0354(6) Uani 1 1 d . . . Zn1 Zn 0.858135(8) 0.143064(6) 0.50965(2) 0.01851(7) Uani 1 1 d . . . Zn2 Zn 0.872971(8) 0.233315(7) 0.92919(2) 0.01911(7) 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 B1 0.0237(16) 0.0191(12) 0.0197(18) -0.0012(12) 0.0006(16) 0.0045(12) B2 0.0211(16) 0.0213(13) 0.0155(18) 0.0005(11) -0.0002(14) -0.0012(12) C1 0.0244(16) 0.0283(13) 0.032(2) 0.0039(12) -0.0059(15) -0.0008(12) C2 0.0219(14) 0.0246(12) 0.0123(16) 0.0014(10) 0.0018(13) -0.0006(11) C3 0.0228(14) 0.0212(11) 0.0073(15) 0.0017(10) 0.0025(12) -0.0023(10) C4 0.0245(15) 0.0160(11) 0.0206(17) 0.0026(10) 0.0011(13) -0.0002(10) C5 0.0311(17) 0.0200(12) 0.042(2) 0.0018(13) -0.0036(17) 0.0004(12) C6 0.0335(17) 0.0251(13) 0.0218(18) -0.0024(12) 0.0013(15) 0.0036(12) C7 0.0305(17) 0.0283(13) 0.0210(19) 0.0055(12) -0.0002(14) 0.0030(12) C8 0.0334(17) 0.0287(14) 0.031(2) 0.0094(13) -0.0048(16) 0.0004(13) C9 0.0299(15) 0.0174(11) 0.0221(17) 0.0012(11) -0.0036(15) 0.0004(10) C10 0.0265(15) 0.0214(12) 0.0159(16) -0.0034(10) -0.0025(13) -0.0032(11) C11 0.0278(16) 0.0271(13) 0.0186(18) 0.0011(11) -0.0016(14) -0.0002(12) C12 0.0297(17) 0.0318(14) 0.028(2) 0.0057(13) -0.0009(16) -0.0047(12) C13 0.0316(17) 0.0389(15) 0.0234(19) 0.0077(13) -0.0032(16) -0.0070(13) C14 0.0318(18) 0.0408(16) 0.035(2) -0.0094(14) -0.0010(17) 0.0055(14) C15 0.0341(18) 0.0451(17) 0.039(2) -0.0191(15) 0.0005(17) 0.0111(15) C16 0.0270(16) 0.0303(14) 0.0264(19) -0.0063(12) 0.0036(15) -0.0001(12) C17 0.0328(17) 0.0197(12) 0.0199(18) -0.0014(11) 0.0008(15) -0.0033(11) C18 0.0314(16) 0.0221(11) 0.0199(17) -0.0042(12) -0.0002(15) -0.0015(11) C19 0.050(2) 0.0270(14) 0.029(2) 0.0046(13) -0.0019(18) -0.0039(14) C20 0.0367(19) 0.0384(16) 0.027(2) -0.0009(13) -0.0058(17) -0.0035(14) C21 0.056(2) 0.0337(15) 0.024(2) -0.0062(14) -0.008(2) 0.0007(15) C22 0.0326(17) 0.0274(14) 0.038(2) 0.0014(13) -0.0040(17) 0.0051(13) C23 0.046(2) 0.0380(17) 0.040(2) -0.0001(15) -0.004(2) 0.0059(16) C24 0.040(2) 0.0315(15) 0.044(2) -0.0017(15) 0.0001(19) 0.0015(14) C25 0.0370(19) 0.062(2) 0.030(2) -0.0096(17) -0.0003(17) -0.0235(17) C26 0.0259(15) 0.0331(13) 0.0203(18) -0.0019(13) -0.0051(15) -0.0045(12) C27 0.0338(17) 0.0211(12) 0.0184(17) 0.0009(11) 0.0019(15) 0.0001(12) C28 0.0423(18) 0.0229(12) 0.0159(17) -0.0009(11) 0.0049(16) -0.0088(12) C29 0.0346(17) 0.0250(12) 0.0269(19) -0.0001(13) 0.0018(17) -0.0043(12) C30 0.057(2) 0.0340(16) 0.049(3) 0.0033(16) 0.023(2) 0.0017(15) C31 0.065(3) 0.055(2) 0.025(2) 0.0026(17) 0.001(2) -0.0272(18) C32 0.0272(16) 0.0265(13) 0.026(2) 0.0009(12) 0.0042(15) -0.0013(11) C33 0.0251(15) 0.0201(11) 0.0153(17) -0.0044(10) 0.0016(13) 0.0010(10) C34 0.0200(14) 0.0222(12) 0.0165(17) -0.0029(10) -0.0018(13) 0.0018(10) C35 0.0185(15) 0.0381(15) 0.028(2) 0.0019(13) 0.0006(15) 0.0040(12) C36 0.0235(16) 0.0390(15) 0.031(2) -0.0013(13) 0.0107(15) 0.0040(13) C37 0.0281(18) 0.077(2) 0.042(3) 0.028(2) 0.0031(19) 0.0105(17) C38 0.0192(15) 0.0591(19) 0.037(2) -0.0096(18) -0.0021(17) -0.0066(14) C39 0.0194(14) 0.0275(12) 0.0264(18) 0.0022(13) 0.0038(15) 0.0045(10) C40 0.0199(14) 0.0270(12) 0.0117(15) 0.0021(11) -0.0008(12) 0.0023(11) C41 0.0217(14) 0.0205(11) 0.0126(16) 0.0008(10) -0.0009(13) 0.0005(10) C42 0.0309(16) 0.0189(11) 0.0195(17) 0.0005(11) 0.0050(14) -0.0025(11) C43 0.043(2) 0.0227(13) 0.043(2) 0.0049(13) 0.0139(18) 0.0019(13) C44 0.041(2) 0.0282(14) 0.033(2) 0.0009(13) 0.0006(18) -0.0100(13) C45 0.047(2) 0.0301(15) 0.0197(19) 0.0028(12) 0.0092(16) -0.0025(14) C46 0.0350(19) 0.0421(17) 0.046(3) 0.0050(16) 0.0060(19) -0.0099(15) C47 0.042(2) 0.0352(17) 0.078(4) -0.0068(19) 0.019(2) -0.0013(15) C48 0.0318(19) 0.0463(18) 0.041(2) 0.0026(16) 0.0029(18) -0.0024(15) F1 0.0656(15) 0.0611(13) 0.0360(14) 0.0048(10) 0.0054(13) -0.0013(12) F2 0.0364(11) 0.0545(12) 0.081(2) -0.0077(11) 0.0086(13) -0.0074(10) F3 0.0653(15) 0.0436(11) 0.0716(18) 0.0006(11) 0.0210(14) 0.0256(11) F4 0.0950(19) 0.0546(12) 0.0566(17) 0.0146(11) -0.0087(16) 0.0358(13) F5 0.0644(16) 0.0801(16) 0.0622(18) -0.0021(13) -0.0361(15) -0.0127(13) F6 0.0648(16) 0.0748(15) 0.0297(14) 0.0055(11) -0.0003(13) 0.0032(12) F7 0.083(2) 0.0788(17) 0.083(2) -0.0392(16) -0.0107(19) 0.0017(15) F8 0.0622(15) 0.0412(11) 0.123(3) 0.0173(14) -0.0214(17) -0.0143(11) F9 0.0423(13) 0.0523(12) 0.121(3) -0.0111(14) -0.0069(16) -0.0137(11) F10 0.110(3) 0.102(2) 0.057(2) 0.0339(16) 0.0092(19) -0.0017(18) F11 0.0416(14) 0.0830(17) 0.090(2) -0.0217(15) 0.0169(15) -0.0042(12) F12 0.0467(13) 0.0663(13) 0.0541(17) -0.0225(12) 0.0043(13) -0.0082(11) N1 0.0208(12) 0.0198(10) 0.0153(14) 0.0005(9) -0.0018(11) 0.0009(9) N2 0.0209(12) 0.0183(9) 0.0157(13) -0.0002(9) -0.0018(11) 0.0018(9) N3 0.0219(12) 0.0209(10) 0.0170(14) 0.0018(9) 0.0019(11) -0.0010(9) N4 0.0202(12) 0.0220(10) 0.0146(13) -0.0016(9) -0.0023(11) 0.0014(9) N5 0.0224(12) 0.0171(9) 0.0217(14) -0.0001(9) -0.0013(11) 0.0005(9) N6 0.0273(13) 0.0229(10) 0.0213(15) 0.0050(9) -0.0053(12) -0.0032(9) N7 0.0255(12) 0.0202(10) 0.0180(15) 0.0002(9) 0.0009(11) 0.0007(9) N8 0.0209(12) 0.0231(11) 0.0224(15) -0.0037(9) 0.0017(11) 0.0003(9) N9 0.0331(15) 0.0349(13) 0.0249(17) -0.0064(11) 0.0061(14) 0.0011(11) N10 0.0233(12) 0.0187(9) 0.0145(13) 0.0007(9) 0.0010(12) -0.0020(9) N11 0.0172(12) 0.0234(10) 0.0197(15) -0.0013(9) 0.0020(11) -0.0018(9) N12 0.0326(15) 0.0358(13) 0.0197(16) -0.0025(11) -0.0040(13) -0.0104(11) N13 0.0150(11) 0.0222(10) 0.0178(14) -0.0026(9) 0.0016(11) -0.0010(9) N14 0.0183(12) 0.0186(9) 0.0137(13) -0.0034(9) 0.0045(10) -0.0026(8) N15 0.0236(13) 0.0278(11) 0.0169(15) 0.0009(9) 0.0019(11) 0.0040(10) N16 0.0203(12) 0.0221(10) 0.0147(14) 0.0009(9) 0.0008(11) -0.0038(9) N17 0.0156(11) 0.0207(10) 0.0147(13) 0.0007(9) 0.0022(10) -0.0027(8) N18 0.0222(12) 0.0242(10) 0.0176(14) 0.0017(9) 0.0012(11) 0.0040(9) O1 0.0300(12) 0.0227(9) 0.0452(16) -0.0033(9) -0.0112(11) 0.0084(8) O2 0.0269(12) 0.0368(11) 0.0426(16) 0.0036(10) 0.0099(12) -0.0033(9) Zn1 0.02111(16) 0.01772(12) 0.01669(17) -0.00031(12) -0.00174(15) 0.00098(12) Zn2 0.01816(15) 0.02145(13) 0.01770(18) -0.00074(12) 0.00194(15) -0.00137(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N5 1.539(4) . ? B1 N8 1.542(4) . ? B1 N2 1.543(4) . ? B1 H1 1.0000 . ? B2 N14 1.535(4) . ? B2 N11 1.541(4) . ? B2 N17 1.544(3) . ? B2 H2 1.0000 . ? C1 C2 1.507(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N2 1.328(4) . ? C2 N3 1.338(3) . ? C3 N1 1.342(3) . ? C3 N3 1.352(4) . ? C3 C4 1.500(4) . ? C4 C6 1.523(4) . ? C4 C5 1.531(4) . ? C4 C7 1.534(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.492(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N6 1.332(4) . ? C9 N5 1.343(4) . ? C10 N4 1.333(4) . ? C10 N6 1.341(4) . ? C10 C11 1.513(4) . ? C11 C13 1.515(4) . ? C11 C14 1.526(4) . ? C11 C12 1.541(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.479(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N9 1.331(4) . ? C16 N8 1.341(4) . ? C17 N7 1.334(4) . ? C17 N9 1.347(4) . ? C17 C18 1.505(5) . ? C18 C20 1.516(5) . ? C18 C21 1.526(4) . ? C18 C19 1.551(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 O1 1.369(3) . ? C22 C24 1.511(5) . ? C22 C23 1.531(5) . ? C22 H22 1.0000 . ? C23 F5 1.307(4) . ? C23 F6 1.330(5) . ? C23 F4 1.334(4) . ? C24 F3 1.317(4) . ? C24 F2 1.340(4) . ? C24 F1 1.350(4) . ? C25 C26 1.503(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 N12 1.311(5) . ? C26 N11 1.352(4) . ? C27 N10 1.328(4) . ? C27 N12 1.359(4) . ? C27 C28 1.501(4) . ? C28 C30 1.522(5) . ? C28 C29 1.532(4) . ? C28 C31 1.533(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.492(4) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 N15 1.330(4) . ? C33 N14 1.343(4) . ? C34 N13 1.334(4) . ? C34 N15 1.347(4) . ? C34 C35 1.505(4) . ? C35 C36 1.523(5) . ? C35 C37 1.523(5) . ? C35 C38 1.534(4) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.479(4) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 N18 1.328(3) . ? C40 N17 1.348(4) . ? C41 N16 1.343(3) . ? C41 N18 1.348(4) . ? C41 C42 1.511(4) . ? C42 C45 1.529(5) . ? C42 C44 1.533(5) . ? C42 C43 1.542(4) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 O2 1.340(4) . ? C46 C48 1.540(6) . ? C46 C47 1.542(5) . ? C46 H46 1.0000 . ? C47 F9 1.288(4) . ? C47 F7 1.326(6) . ? C47 F8 1.339(5) . ? C48 F11 1.296(4) . ? C48 F12 1.329(4) . ? C48 F10 1.353(5) . ? N1 N2 1.376(3) . ? N1 Zn1 2.052(2) . ? N4 N5 1.382(3) . ? N4 Zn1 2.060(2) . ? N7 N8 1.385(3) . ? N7 Zn1 2.067(2) . ? N10 N11 1.382(3) . ? N10 Zn2 2.076(2) . ? N13 N14 1.384(3) . ? N13 Zn2 2.047(2) . ? N16 N17 1.397(3) . ? N16 Zn2 2.065(2) . ? O1 Zn1 1.855(2) . ? O2 Zn2 1.847(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 B1 N8 109.4(2) . . ? N5 B1 N2 110.3(2) . . ? N8 B1 N2 107.9(2) . . ? N5 B1 H1 109.7 . . ? N8 B1 H1 109.7 . . ? N2 B1 H1 109.7 . . ? N14 B2 N11 109.5(2) . . ? N14 B2 N17 110.5(2) . . ? N11 B2 N17 107.2(2) . . ? N14 B2 H2 109.9 . . ? N11 B2 H2 109.9 . . ? N17 B2 H2 109.9 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 N3 111.4(2) . . ? N2 C2 C1 124.5(2) . . ? N3 C2 C1 124.1(2) . . ? N1 C3 N3 112.7(2) . . ? N1 C3 C4 123.4(2) . . ? N3 C3 C4 123.9(2) . . ? C3 C4 C6 109.1(2) . . ? C3 C4 C5 110.3(2) . . ? C6 C4 C5 109.5(2) . . ? C3 C4 C7 108.2(2) . . ? C6 C4 C7 110.7(2) . . ? C5 C4 C7 109.0(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N6 C9 N5 110.7(3) . . ? N6 C9 C8 123.9(3) . . ? N5 C9 C8 125.4(3) . . ? N4 C10 N6 112.8(3) . . ? N4 C10 C11 124.3(3) . . ? N6 C10 C11 122.9(3) . . ? C10 C11 C13 109.2(2) . . ? C10 C11 C14 108.2(2) . . ? C13 C11 C14 109.8(3) . . ? C10 C11 C12 110.7(3) . . ? C13 C11 C12 108.5(2) . . ? C14 C11 C12 110.4(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N9 C16 N8 110.8(3) . . ? N9 C16 C15 124.7(3) . . ? N8 C16 C15 124.5(3) . . ? N7 C17 N9 112.4(3) . . ? N7 C17 C18 124.2(3) . . ? N9 C17 C18 123.5(3) . . ? C17 C18 C20 111.7(3) . . ? C17 C18 C21 109.1(2) . . ? C20 C18 C21 110.2(3) . . ? C17 C18 C19 107.5(2) . . ? C20 C18 C19 110.1(3) . . ? C21 C18 C19 108.1(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O1 C22 C24 112.5(3) . . ? O1 C22 C23 109.0(3) . . ? C24 C22 C23 111.8(3) . . ? O1 C22 H22 107.8 . . ? C24 C22 H22 107.8 . . ? C23 C22 H22 107.8 . . ? F5 C23 F6 107.7(3) . . ? F5 C23 F4 107.1(3) . . ? F6 C23 F4 106.5(3) . . ? F5 C23 C22 113.2(3) . . ? F6 C23 C22 109.7(3) . . ? F4 C23 C22 112.3(3) . . ? F3 C24 F2 107.4(3) . . ? F3 C24 F1 106.1(3) . . ? F2 C24 F1 106.5(3) . . ? F3 C24 C22 113.6(3) . . ? F2 C24 C22 113.2(3) . . ? F1 C24 C22 109.5(3) . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N12 C26 N11 111.9(3) . . ? N12 C26 C25 124.7(3) . . ? N11 C26 C25 123.4(3) . . ? N10 C27 N12 112.5(3) . . ? N10 C27 C28 125.3(3) . . ? N12 C27 C28 122.2(3) . . ? C27 C28 C30 108.2(3) . . ? C27 C28 C29 110.8(3) . . ? C30 C28 C29 110.6(3) . . ? C27 C28 C31 109.5(3) . . ? C30 C28 C31 108.5(3) . . ? C29 C28 C31 109.2(3) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C33 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N15 C33 N14 111.6(2) . . ? N15 C33 C32 123.3(3) . . ? N14 C33 C32 125.1(3) . . ? N13 C34 N15 112.7(2) . . ? N13 C34 C35 123.2(3) . . ? N15 C34 C35 124.2(3) . . ? C34 C35 C36 109.1(3) . . ? C34 C35 C37 110.3(3) . . ? C36 C35 C37 108.0(3) . . ? C34 C35 C38 108.3(2) . . ? C36 C35 C38 111.1(3) . . ? C37 C35 C38 110.0(3) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C40 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N18 C40 N17 110.8(2) . . ? N18 C40 C39 125.6(2) . . ? N17 C40 C39 123.6(2) . . ? N16 C41 N18 112.8(2) . . ? N16 C41 C42 123.8(3) . . ? N18 C41 C42 123.3(2) . . ? C41 C42 C45 110.6(2) . . ? C41 C42 C44 108.0(2) . . ? C45 C42 C44 110.5(3) . . ? C41 C42 C43 109.2(2) . . ? C45 C42 C43 109.1(3) . . ? C44 C42 C43 109.4(3) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O2 C46 C48 112.6(3) . . ? O2 C46 C47 110.6(3) . . ? C48 C46 C47 112.2(3) . . ? O2 C46 H46 107.0 . . ? C48 C46 H46 107.0 . . ? C47 C46 H46 107.0 . . ? F9 C47 F7 108.5(4) . . ? F9 C47 F8 110.0(3) . . ? F7 C47 F8 105.4(3) . . ? F9 C47 C46 113.0(3) . . ? F7 C47 C46 108.3(3) . . ? F8 C47 C46 111.3(4) . . ? F11 C48 F12 109.1(3) . . ? F11 C48 F10 106.0(3) . . ? F12 C48 F10 108.3(3) . . ? F11 C48 C46 112.6(3) . . ? F12 C48 C46 110.1(3) . . ? F10 C48 C46 110.5(3) . . ? C3 N1 N2 104.2(2) . . ? C3 N1 Zn1 142.20(19) . . ? N2 N1 Zn1 113.22(15) . . ? C2 N2 N1 108.0(2) . . ? C2 N2 B1 131.3(2) . . ? N1 N2 B1 119.8(2) . . ? C2 N3 C3 103.7(2) . . ? C10 N4 N5 104.4(2) . . ? C10 N4 Zn1 143.9(2) . . ? N5 N4 Zn1 111.63(17) . . ? C9 N5 N4 107.3(2) . . ? C9 N5 B1 131.3(3) . . ? N4 N5 B1 121.0(2) . . ? C9 N6 C10 104.6(2) . . ? C17 N7 N8 104.7(2) . . ? C17 N7 Zn1 143.9(2) . . ? N8 N7 Zn1 111.03(18) . . ? C16 N8 N7 107.3(3) . . ? C16 N8 B1 131.0(3) . . ? N7 N8 B1 121.7(2) . . ? C16 N9 C17 104.8(3) . . ? C27 N10 N11 105.0(2) . . ? C27 N10 Zn2 144.8(2) . . ? N11 N10 Zn2 110.09(18) . . ? C26 N11 N10 106.4(2) . . ? C26 N11 B2 130.7(3) . . ? N10 N11 B2 122.9(2) . . ? C26 N12 C27 104.2(3) . . ? C34 N13 N14 104.9(2) . . ? C34 N13 Zn2 142.9(2) . . ? N14 N13 Zn2 112.17(17) . . ? C33 N14 N13 106.7(2) . . ? C33 N14 B2 132.1(2) . . ? N13 N14 B2 121.0(2) . . ? C33 N15 C34 104.2(2) . . ? C41 N16 N17 103.8(2) . . ? C41 N16 Zn2 144.27(19) . . ? N17 N16 Zn2 111.51(15) . . ? C40 N17 N16 107.5(2) . . ? C40 N17 B2 130.8(2) . . ? N16 N17 B2 120.8(2) . . ? C40 N18 C41 105.0(2) . . ? C22 O1 Zn1 145.0(2) . . ? C46 O2 Zn2 142.0(2) . . ? O1 Zn1 N1 126.39(9) . . ? O1 Zn1 N4 120.50(10) . . ? N1 Zn1 N4 96.63(9) . . ? O1 Zn1 N7 122.97(10) . . ? N1 Zn1 N7 91.89(10) . . ? N4 Zn1 N7 89.21(9) . . ? O2 Zn2 N13 127.22(10) . . ? O2 Zn2 N16 116.61(9) . . ? N13 Zn2 N16 95.84(9) . . ? O2 Zn2 N10 124.90(11) . . ? N13 Zn2 N10 92.19(9) . . ? N16 Zn2 N10 91.32(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C3 C4 C6 64.9(4) . . . . ? N3 C3 C4 C6 -113.9(3) . . . . ? N1 C3 C4 C5 -174.7(3) . . . . ? N3 C3 C4 C5 6.5(4) . . . . ? N1 C3 C4 C7 -55.6(4) . . . . ? N3 C3 C4 C7 125.6(3) . . . . ? N4 C10 C11 C13 157.6(3) . . . . ? N6 C10 C11 C13 -22.0(4) . . . . ? N4 C10 C11 C14 -82.9(4) . . . . ? N6 C10 C11 C14 97.5(3) . . . . ? N4 C10 C11 C12 38.2(4) . . . . ? N6 C10 C11 C12 -141.4(3) . . . . ? N7 C17 C18 C20 -37.9(4) . . . . ? N9 C17 C18 C20 141.6(3) . . . . ? N7 C17 C18 C21 -160.0(3) . . . . ? N9 C17 C18 C21 19.6(4) . . . . ? N7 C17 C18 C19 83.0(3) . . . . ? N9 C17 C18 C19 -97.5(3) . . . . ? O1 C22 C23 F5 62.5(4) . . . . ? C24 C22 C23 F5 -62.5(4) . . . . ? O1 C22 C23 F6 -57.9(4) . . . . ? C24 C22 C23 F6 177.1(3) . . . . ? O1 C22 C23 F4 -176.1(3) . . . . ? C24 C22 C23 F4 59.0(4) . . . . ? O1 C22 C24 F3 -179.9(3) . . . . ? C23 C22 C24 F3 -56.9(4) . . . . ? O1 C22 C24 F2 -57.0(4) . . . . ? C23 C22 C24 F2 65.9(4) . . . . ? O1 C22 C24 F1 61.6(3) . . . . ? C23 C22 C24 F1 -175.4(3) . . . . ? N10 C27 C28 C30 -75.7(3) . . . . ? N12 C27 C28 C30 102.5(3) . . . . ? N10 C27 C28 C29 45.8(4) . . . . ? N12 C27 C28 C29 -136.0(3) . . . . ? N10 C27 C28 C31 166.3(3) . . . . ? N12 C27 C28 C31 -15.5(4) . . . . ? N13 C34 C35 C36 55.2(4) . . . . ? N15 C34 C35 C36 -123.7(3) . . . . ? N13 C34 C35 C37 173.7(3) . . . . ? N15 C34 C35 C37 -5.2(4) . . . . ? N13 C34 C35 C38 -65.9(4) . . . . ? N15 C34 C35 C38 115.3(3) . . . . ? N16 C41 C42 C45 -54.0(4) . . . . ? N18 C41 C42 C45 127.6(3) . . . . ? N16 C41 C42 C44 67.0(4) . . . . ? N18 C41 C42 C44 -111.3(3) . . . . ? N16 C41 C42 C43 -174.1(3) . . . . ? N18 C41 C42 C43 7.5(4) . . . . ? O2 C46 C47 F9 174.2(4) . . . . ? C48 C46 C47 F9 47.5(5) . . . . ? O2 C46 C47 F7 -65.5(4) . . . . ? C48 C46 C47 F7 167.8(3) . . . . ? O2 C46 C47 F8 49.8(5) . . . . ? C48 C46 C47 F8 -76.9(4) . . . . ? O2 C46 C48 F11 172.3(3) . . . . ? C47 C46 C48 F11 -62.1(4) . . . . ? O2 C46 C48 F12 50.3(4) . . . . ? C47 C46 C48 F12 175.9(3) . . . . ? O2 C46 C48 F10 -69.3(4) . . . . ? C47 C46 C48 F10 56.3(4) . . . . ? N3 C3 N1 N2 -1.2(3) . . . . ? C4 C3 N1 N2 179.9(3) . . . . ? N3 C3 N1 Zn1 -172.5(2) . . . . ? C4 C3 N1 Zn1 8.6(5) . . . . ? N3 C2 N2 N1 0.2(3) . . . . ? C1 C2 N2 N1 -179.5(3) . . . . ? N3 C2 N2 B1 169.3(3) . . . . ? C1 C2 N2 B1 -10.3(5) . . . . ? C3 N1 N2 C2 0.6(3) . . . . ? Zn1 N1 N2 C2 174.83(19) . . . . ? C3 N1 N2 B1 -170.0(3) . . . . ? Zn1 N1 N2 B1 4.2(3) . . . . ? N5 B1 N2 C2 130.1(3) . . . . ? N8 B1 N2 C2 -110.4(3) . . . . ? N5 B1 N2 N1 -61.8(3) . . . . ? N8 B1 N2 N1 57.6(3) . . . . ? N2 C2 N3 C3 -0.9(3) . . . . ? C1 C2 N3 C3 178.8(3) . . . . ? N1 C3 N3 C2 1.3(3) . . . . ? C4 C3 N3 C2 -179.8(3) . . . . ? N6 C10 N4 N5 1.4(3) . . . . ? C11 C10 N4 N5 -178.3(3) . . . . ? N6 C10 N4 Zn1 -175.6(2) . . . . ? C11 C10 N4 Zn1 4.8(5) . . . . ? N6 C9 N5 N4 1.1(3) . . . . ? C8 C9 N5 N4 179.7(3) . . . . ? N6 C9 N5 B1 -172.8(3) . . . . ? C8 C9 N5 B1 5.8(5) . . . . ? C10 N4 N5 C9 -1.5(3) . . . . ? Zn1 N4 N5 C9 176.58(18) . . . . ? C10 N4 N5 B1 173.2(2) . . . . ? Zn1 N4 N5 B1 -8.8(3) . . . . ? N8 B1 N5 C9 119.9(3) . . . . ? N2 B1 N5 C9 -121.6(3) . . . . ? N8 B1 N5 N4 -53.2(3) . . . . ? N2 B1 N5 N4 65.3(3) . . . . ? N5 C9 N6 C10 -0.3(3) . . . . ? C8 C9 N6 C10 -178.9(3) . . . . ? N4 C10 N6 C9 -0.7(3) . . . . ? C11 C10 N6 C9 178.9(3) . . . . ? N9 C17 N7 N8 -0.7(3) . . . . ? C18 C17 N7 N8 178.8(2) . . . . ? N9 C17 N7 Zn1 171.6(2) . . . . ? C18 C17 N7 Zn1 -8.9(5) . . . . ? N9 C16 N8 N7 0.0(3) . . . . ? C15 C16 N8 N7 -179.9(3) . . . . ? N9 C16 N8 B1 180.0(3) . . . . ? C15 C16 N8 B1 0.2(5) . . . . ? C17 N7 N8 C16 0.5(3) . . . . ? Zn1 N7 N8 C16 -174.70(18) . . . . ? C17 N7 N8 B1 -179.6(2) . . . . ? Zn1 N7 N8 B1 5.3(3) . . . . ? N5 B1 N8 C16 -124.4(3) . . . . ? N2 B1 N8 C16 115.6(3) . . . . ? N5 B1 N8 N7 55.6(3) . . . . ? N2 B1 N8 N7 -64.4(3) . . . . ? N8 C16 N9 C17 -0.4(3) . . . . ? C15 C16 N9 C17 179.4(3) . . . . ? N7 C17 N9 C16 0.7(3) . . . . ? C18 C17 N9 C16 -178.8(3) . . . . ? N12 C27 N10 N11 0.0(3) . . . . ? C28 C27 N10 N11 178.3(3) . . . . ? N12 C27 N10 Zn2 174.6(2) . . . . ? C28 C27 N10 Zn2 -7.1(5) . . . . ? N12 C26 N11 N10 -0.6(3) . . . . ? C25 C26 N11 N10 178.0(3) . . . . ? N12 C26 N11 B2 -177.8(3) . . . . ? C25 C26 N11 B2 0.9(5) . . . . ? C27 N10 N11 C26 0.4(3) . . . . ? Zn2 N10 N11 C26 -176.29(17) . . . . ? C27 N10 N11 B2 177.8(2) . . . . ? Zn2 N10 N11 B2 1.1(3) . . . . ? N14 B2 N11 C26 -125.1(3) . . . . ? N17 B2 N11 C26 115.0(3) . . . . ? N14 B2 N11 N10 58.1(3) . . . . ? N17 B2 N11 N10 -61.7(3) . . . . ? N11 C26 N12 C27 0.6(3) . . . . ? C25 C26 N12 C27 -178.0(3) . . . . ? N10 C27 N12 C26 -0.4(3) . . . . ? C28 C27 N12 C26 -178.8(3) . . . . ? N15 C34 N13 N14 0.4(3) . . . . ? C35 C34 N13 N14 -178.5(3) . . . . ? N15 C34 N13 Zn2 179.0(2) . . . . ? C35 C34 N13 Zn2 0.0(5) . . . . ? N15 C33 N14 N13 0.2(3) . . . . ? C32 C33 N14 N13 178.7(3) . . . . ? N15 C33 N14 B2 -174.7(3) . . . . ? C32 C33 N14 B2 3.9(5) . . . . ? C34 N13 N14 C33 -0.4(3) . . . . ? Zn2 N13 N14 C33 -179.41(17) . . . . ? C34 N13 N14 B2 175.2(2) . . . . ? Zn2 N13 N14 B2 -3.9(3) . . . . ? N11 B2 N14 C33 118.1(3) . . . . ? N17 B2 N14 C33 -124.0(3) . . . . ? N11 B2 N14 N13 -56.1(3) . . . . ? N17 B2 N14 N13 61.8(3) . . . . ? N14 C33 N15 C34 0.1(3) . . . . ? C32 C33 N15 C34 -178.5(3) . . . . ? N13 C34 N15 C33 -0.3(3) . . . . ? C35 C34 N15 C33 178.6(3) . . . . ? N18 C41 N16 N17 1.2(3) . . . . ? C42 C41 N16 N17 -177.3(3) . . . . ? N18 C41 N16 Zn2 -170.2(3) . . . . ? C42 C41 N16 Zn2 11.3(5) . . . . ? N18 C40 N17 N16 1.0(3) . . . . ? C39 C40 N17 N16 179.6(3) . . . . ? N18 C40 N17 B2 169.6(3) . . . . ? C39 C40 N17 B2 -11.8(5) . . . . ? C41 N16 N17 C40 -1.3(3) . . . . ? Zn2 N16 N17 C40 173.31(19) . . . . ? C41 N16 N17 B2 -171.3(3) . . . . ? Zn2 N16 N17 B2 3.3(3) . . . . ? N14 B2 N17 C40 131.6(3) . . . . ? N11 B2 N17 C40 -109.2(3) . . . . ? N14 B2 N17 N16 -61.1(3) . . . . ? N11 B2 N17 N16 58.1(3) . . . . ? N17 C40 N18 C41 -0.3(3) . . . . ? C39 C40 N18 C41 -178.8(3) . . . . ? N16 C41 N18 C40 -0.6(3) . . . . ? C42 C41 N18 C40 177.9(3) . . . . ? C24 C22 O1 Zn1 -110.7(4) . . . . ? C23 C22 O1 Zn1 124.8(4) . . . . ? C48 C46 O2 Zn2 -109.7(4) . . . . ? C47 C46 O2 Zn2 123.8(4) . . . . ? C22 O1 Zn1 N1 -5.0(5) . . . . ? C22 O1 Zn1 N4 121.9(4) . . . . ? C22 O1 Zn1 N7 -126.8(4) . . . . ? C3 N1 Zn1 O1 -13.3(4) . . . . ? N2 N1 Zn1 O1 175.86(17) . . . . ? C3 N1 Zn1 N4 -149.4(3) . . . . ? N2 N1 Zn1 N4 39.8(2) . . . . ? C3 N1 Zn1 N7 121.2(3) . . . . ? N2 N1 Zn1 N7 -49.65(19) . . . . ? C10 N4 Zn1 O1 0.0(4) . . . . ? N5 N4 Zn1 O1 -176.78(16) . . . . ? C10 N4 Zn1 N1 139.6(3) . . . . ? N5 N4 Zn1 N1 -37.17(18) . . . . ? C10 N4 Zn1 N7 -128.6(3) . . . . ? N5 N4 Zn1 N7 54.64(18) . . . . ? C17 N7 Zn1 O1 8.9(4) . . . . ? N8 N7 Zn1 O1 -179.12(15) . . . . ? C17 N7 Zn1 N1 -127.9(3) . . . . ? N8 N7 Zn1 N1 44.09(17) . . . . ? C17 N7 Zn1 N4 135.4(3) . . . . ? N8 N7 Zn1 N4 -52.52(17) . . . . ? C46 O2 Zn2 N13 -12.1(4) . . . . ? C46 O2 Zn2 N16 -133.7(4) . . . . ? C46 O2 Zn2 N10 113.9(4) . . . . ? C34 N13 Zn2 O2 9.7(4) . . . . ? N14 N13 Zn2 O2 -171.79(16) . . . . ? C34 N13 Zn2 N16 139.8(3) . . . . ? N14 N13 Zn2 N16 -41.76(18) . . . . ? C34 N13 Zn2 N10 -128.7(3) . . . . ? N14 N13 Zn2 N10 49.79(18) . . . . ? C41 N16 Zn2 O2 -10.2(4) . . . . ? N17 N16 Zn2 O2 178.79(17) . . . . ? C41 N16 Zn2 N13 -147.2(3) . . . . ? N17 N16 Zn2 N13 41.80(19) . . . . ? C41 N16 Zn2 N10 120.5(3) . . . . ? N17 N16 Zn2 N10 -50.53(19) . . . . ? C27 N10 Zn2 O2 -2.2(4) . . . . ? N11 N10 Zn2 O2 172.24(15) . . . . ? C27 N10 Zn2 N13 137.7(3) . . . . ? N11 N10 Zn2 N13 -47.89(17) . . . . ? C27 N10 Zn2 N16 -126.4(3) . . . . ? N11 N10 Zn2 N16 48.01(17) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.621 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.067 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.023 0.169 0.207 199 57 ' ' 2 0.023 0.331 0.707 199 56 ' ' 3 -0.023 0.669 0.707 199 57 ' ' 4 0.023 0.831 0.207 199 56 ' ' 5 0.000 0.500 0.986 13 1 ' ' 6 0.000 1.000 0.486 13 1 ' ' 7 0.227 0.081 0.457 199 56 ' ' 8 0.227 0.581 -0.043 199 56 ' ' 9 0.273 0.419 0.457 199 57 ' ' 10 0.273 0.919 -0.043 199 57 ' ' 11 0.250 0.250 0.736 13 1 ' ' 12 0.250 0.750 0.236 13 1 ' ' 13 0.477 0.169 0.707 199 57 ' ' 14 0.477 0.669 0.207 199 57 ' ' 15 0.523 0.331 0.207 199 56 ' ' 16 0.523 0.831 0.707 199 56 ' ' 17 0.500 0.000 0.986 13 1 ' ' 18 0.500 0.500 0.486 13 1 ' ' 19 0.727 0.081 -0.043 199 56 ' ' 20 0.727 0.581 0.457 199 56 ' ' 21 0.773 0.419 -0.043 199 57 ' ' 22 0.773 0.919 0.457 199 57 ' ' 23 0.750 0.250 0.236 13 1 ' ' 24 0.750 0.750 0.736 13 1 ' ' _platon_squeeze_details ; ; data_09mz458_0m _database_code_depnum_ccdc_archive 'CCDC 764051' #TrackingRef '- combined cifs' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C27 H42 B N9 O Zn), C6 H6 O' _chemical_formula_sum 'C60 H90 B2 N18 O3 Zn2' _chemical_formula_weight 1263.90 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 9.887(3) _cell_length_b 20.091(6) _cell_length_c 16.297(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.627(7) _cell_angle_gamma 90.00 _cell_volume 3236.9(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2113 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 31.55 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6365 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_process_details 'Apex2 v2009.7-0 (Bruker, 2009)' _exptl_special_details ; The phenol solvate molecule is located on an inversion center and the OH group is thus disordered with an H atom in a 1:1 ratio. ; _diffrn_ambient_temperature 100(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 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 16725 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7959 _reflns_number_gt 6247 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2009.7-0 (Bruker, 2009)' _computing_cell_refinement 'Apex2 v2009.7-0' _computing_data_reduction 'Apex2 v2009.7-0' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0516P)^2^+0.0443P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7959 _refine_ls_number_parameters 402 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1114 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 B1 B 0.5739(2) 0.83667(11) 0.26157(13) 0.0155(4) Uani 1 1 d . . . H1 H 0.6179 0.8809 0.2528 0.019 Uiso 1 1 calc R . . C1 C 0.5098(3) 0.95778(10) 0.38226(14) 0.0290(5) Uani 1 1 d . . . H1A H 0.4609 0.9873 0.4195 0.044 Uiso 1 1 calc R . . H1B H 0.4979 0.9734 0.3257 0.044 Uiso 1 1 calc R . . H1C H 0.6063 0.9580 0.3968 0.044 Uiso 1 1 calc R . . C2 C 0.4560(2) 0.88919(10) 0.38947(12) 0.0187(4) Uani 1 1 d . . . C3 C 0.3511(2) 0.80375(10) 0.43196(12) 0.0172(4) Uani 1 1 d . . . C4 C 0.2580(2) 0.75999(10) 0.48017(12) 0.0205(4) Uani 1 1 d . . . C5 C 0.3277(3) 0.69436(12) 0.50060(18) 0.0413(7) Uani 1 1 d . . . H5A H 0.3479 0.6705 0.4497 0.062 Uiso 1 1 calc R . . H5B H 0.2680 0.6671 0.5345 0.062 Uiso 1 1 calc R . . H5C H 0.4121 0.7032 0.5308 0.062 Uiso 1 1 calc R . . C6 C 0.1316(3) 0.74812(16) 0.42760(15) 0.0432(7) Uani 1 1 d . . . H6A H 0.0888 0.7909 0.4146 0.065 Uiso 1 1 calc R . . H6B H 0.0680 0.7202 0.4578 0.065 Uiso 1 1 calc R . . H6C H 0.1568 0.7257 0.3766 0.065 Uiso 1 1 calc R . . C7 C 0.2198(3) 0.79404(11) 0.56056(14) 0.0289(5) Uani 1 1 d . . . H7A H 0.3019 0.8037 0.5926 0.043 Uiso 1 1 calc R . . H7B H 0.1610 0.7646 0.5921 0.043 Uiso 1 1 calc R . . H7C H 0.1719 0.8357 0.5485 0.043 Uiso 1 1 calc R . . C8 C 0.5178(2) 0.91553(10) 0.09170(13) 0.0246(5) Uani 1 1 d . . . H8A H 0.5247 0.9183 0.0319 0.037 Uiso 1 1 calc R . . H8B H 0.6076 0.9214 0.1167 0.037 Uiso 1 1 calc R . . H8C H 0.4571 0.9505 0.1113 0.037 Uiso 1 1 calc R . . C9 C 0.4629(2) 0.84941(9) 0.11482(12) 0.0170(4) Uani 1 1 d . . . C10 C 0.35322(19) 0.75908(9) 0.11134(11) 0.0145(4) Uani 1 1 d . . . C11 C 0.2627(2) 0.70386(9) 0.08156(12) 0.0177(4) Uani 1 1 d . . . C12 C 0.1407(2) 0.69820(11) 0.13844(14) 0.0259(5) Uani 1 1 d . . . H12A H 0.1715 0.6845 0.1932 0.039 Uiso 1 1 calc R . . H12B H 0.0774 0.6650 0.1164 0.039 Uiso 1 1 calc R . . H12C H 0.0953 0.7414 0.1420 0.039 Uiso 1 1 calc R . . C13 C 0.3405(2) 0.63837(10) 0.08084(14) 0.0267(5) Uani 1 1 d . . . H13A H 0.4161 0.6418 0.0427 0.040 Uiso 1 1 calc R . . H13B H 0.2800 0.6024 0.0632 0.040 Uiso 1 1 calc R . . H13C H 0.3753 0.6289 0.1361 0.040 Uiso 1 1 calc R . . C14 C 0.2137(2) 0.71998(12) -0.00540(13) 0.0279(5) Uani 1 1 d . . . H14A H 0.1623 0.7617 -0.0049 0.042 Uiso 1 1 calc R . . H14B H 0.1557 0.6839 -0.0256 0.042 Uiso 1 1 calc R . . H14C H 0.2918 0.7248 -0.0415 0.042 Uiso 1 1 calc R . . C15 C 0.8946(2) 0.84802(11) 0.25760(15) 0.0286(5) Uani 1 1 d . . . H15A H 0.8761 0.8650 0.2022 0.043 Uiso 1 1 calc R . . H15B H 0.9915 0.8387 0.2637 0.043 Uiso 1 1 calc R . . H15C H 0.8678 0.8814 0.2981 0.043 Uiso 1 1 calc R . . C16 C 0.8168(2) 0.78604(10) 0.27076(12) 0.0188(4) Uani 1 1 d . . . C17 C 0.7672(2) 0.68549(10) 0.29155(11) 0.0173(4) Uani 1 1 d . . . C18 C 0.7822(2) 0.61202(10) 0.30882(12) 0.0212(4) Uani 1 1 d . . . C19 C 0.6922(3) 0.57236(10) 0.24985(14) 0.0282(5) Uani 1 1 d . . . H19A H 0.5972 0.5839 0.2590 0.042 Uiso 1 1 calc R . . H19B H 0.7054 0.5246 0.2595 0.042 Uiso 1 1 calc R . . H19C H 0.7161 0.5831 0.1932 0.042 Uiso 1 1 calc R . . C20 C 0.7411(3) 0.59859(11) 0.39725(13) 0.0338(6) Uani 1 1 d . . . H20A H 0.8005 0.6236 0.4347 0.051 Uiso 1 1 calc R . . H20B H 0.7493 0.5509 0.4089 0.051 Uiso 1 1 calc R . . H20C H 0.6473 0.6127 0.4050 0.051 Uiso 1 1 calc R . . C21 C 0.9291(2) 0.59185(12) 0.29655(17) 0.0393(6) Uani 1 1 d . . . H21A H 0.9561 0.6028 0.2405 0.059 Uiso 1 1 calc R . . H21B H 0.9387 0.5438 0.3056 0.059 Uiso 1 1 calc R . . H21C H 0.9869 0.6159 0.3357 0.059 Uiso 1 1 calc R . . C22 C 0.3376(2) 0.56518(10) 0.31459(13) 0.0220(4) Uani 1 1 d . . . C23 C 0.2825(2) 0.52053(11) 0.25833(14) 0.0317(5) Uani 1 1 d . . . H23 H 0.2442 0.5367 0.2085 0.038 Uiso 1 1 calc R . . C24 C 0.2825(3) 0.45263(12) 0.27397(17) 0.0376(6) Uani 1 1 d . . . H24 H 0.2455 0.4230 0.2343 0.045 Uiso 1 1 calc R . . C25 C 0.3350(2) 0.42775(11) 0.34560(16) 0.0347(6) Uani 1 1 d . . . H25 H 0.3337 0.3812 0.3562 0.042 Uiso 1 1 calc R . . C26 C 0.3896(3) 0.47108(13) 0.40199(16) 0.0412(6) Uani 1 1 d . . . H26 H 0.4274 0.4544 0.4517 0.049 Uiso 1 1 calc R . . C27 C 0.3900(3) 0.53895(12) 0.38701(15) 0.0356(6) Uani 1 1 d . . . H27 H 0.4270 0.5682 0.4272 0.043 Uiso 1 1 calc R . . C28 C 0.0465(2) 1.01195(10) 0.57844(13) 0.0253(5) Uani 1 1 d . . . H28 H 0.0783 1.0199 0.6328 0.030 Uiso 1 1 calc R . . C29 C 0.1269(2) 0.97735(10) 0.52401(14) 0.0240(5) Uani 1 1 d . . . H29 H 0.2140 0.9622 0.5405 0.029 Uiso 0.50 1 calc PR A 2 C30 C 0.0791(2) 0.96516(10) 0.44561(14) 0.0257(5) Uani 1 1 d . . . H30 H 0.1330 0.9409 0.4081 0.031 Uiso 1 1 calc R . . O2 O 0.2460(3) 0.95892(15) 0.54817(18) 0.0242(6) Uani 0.50 1 d P B 1 H2 H 0.2803 0.9341 0.5125 0.036 Uiso 0.50 1 calc PR B 1 N1 N 0.37349(18) 0.86876(8) 0.44838(10) 0.0203(4) Uani 1 1 d . . . N2 N 0.48439(16) 0.83922(8) 0.33839(9) 0.0153(3) Uani 1 1 d . . . N3 N 0.41611(17) 0.78360(8) 0.36515(10) 0.0158(3) Uani 1 1 d . . . N4 N 0.38147(17) 0.81358(8) 0.06643(10) 0.0172(3) Uani 1 1 d . . . N5 N 0.48517(16) 0.81869(8) 0.18665(10) 0.0148(3) Uani 1 1 d . . . N6 N 0.41381(16) 0.75970(8) 0.18462(10) 0.0147(3) Uani 1 1 d . . . N7 N 0.87327(17) 0.72674(9) 0.28216(10) 0.0204(4) Uani 1 1 d . . . N8 N 0.68242(17) 0.78259(8) 0.27314(10) 0.0147(3) Uani 1 1 d . . . N9 N 0.64891(17) 0.71682(8) 0.28629(10) 0.0160(3) Uani 1 1 d . . . O1 O 0.33426(16) 0.63021(7) 0.29941(10) 0.0291(4) Uani 1 1 d . . . Zn1 Zn 0.44534(2) 0.702886(11) 0.288703(13) 0.01557(8) 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 B1 0.0194(11) 0.0136(10) 0.0134(10) 0.0005(8) 0.0015(8) -0.0019(8) C1 0.0445(14) 0.0163(10) 0.0265(12) -0.0050(9) 0.0102(10) -0.0031(10) C2 0.0216(10) 0.0170(9) 0.0173(10) -0.0005(8) 0.0013(8) 0.0036(8) C3 0.0165(10) 0.0201(10) 0.0150(9) 0.0019(7) -0.0002(8) 0.0024(7) C4 0.0188(10) 0.0249(11) 0.0178(10) -0.0001(8) 0.0042(8) -0.0019(8) C5 0.0508(17) 0.0274(13) 0.0464(16) 0.0127(11) 0.0282(14) 0.0048(11) C6 0.0283(13) 0.077(2) 0.0247(13) 0.0032(13) 0.0016(10) -0.0238(13) C7 0.0336(13) 0.0328(13) 0.0205(11) 0.0003(9) 0.0093(10) -0.0004(10) C8 0.0346(13) 0.0192(10) 0.0200(11) 0.0033(8) 0.0001(9) -0.0021(9) C9 0.0215(10) 0.0153(9) 0.0145(9) 0.0007(7) 0.0022(8) 0.0026(8) C10 0.0144(9) 0.0153(9) 0.0139(9) -0.0001(7) 0.0022(7) 0.0030(7) C11 0.0169(10) 0.0209(10) 0.0152(10) -0.0009(8) -0.0006(8) -0.0014(8) C12 0.0201(11) 0.0328(12) 0.0249(11) 0.0009(9) 0.0003(9) -0.0064(9) C13 0.0287(12) 0.0203(10) 0.0309(12) -0.0086(9) -0.0037(10) 0.0000(9) C14 0.0308(13) 0.0362(13) 0.0164(10) 0.0011(9) -0.0070(9) -0.0095(10) C15 0.0202(11) 0.0237(11) 0.0421(14) -0.0011(10) 0.0031(10) -0.0066(9) C16 0.0187(10) 0.0217(10) 0.0161(10) -0.0039(8) 0.0018(8) -0.0024(8) C17 0.0206(10) 0.0203(10) 0.0109(9) -0.0026(7) -0.0022(7) 0.0005(8) C18 0.0275(11) 0.0168(10) 0.0192(10) -0.0005(8) -0.0010(8) 0.0030(8) C19 0.0455(14) 0.0157(10) 0.0234(11) -0.0032(8) -0.0049(10) 0.0012(10) C20 0.0625(17) 0.0212(11) 0.0178(11) 0.0021(9) -0.0010(11) 0.0012(11) C21 0.0343(14) 0.0234(12) 0.0600(18) 0.0044(11) 0.0011(13) 0.0110(10) C22 0.0228(11) 0.0196(10) 0.0238(11) 0.0012(8) 0.0034(9) -0.0051(8) C23 0.0397(14) 0.0260(12) 0.0292(12) 0.0000(10) -0.0049(10) -0.0080(10) C24 0.0441(15) 0.0236(12) 0.0452(15) -0.0095(11) 0.0008(12) -0.0106(11) C25 0.0342(14) 0.0190(11) 0.0512(16) 0.0068(11) 0.0170(12) -0.0024(10) C26 0.0580(18) 0.0314(13) 0.0344(14) 0.0109(11) 0.0029(13) 0.0041(12) C27 0.0544(17) 0.0238(12) 0.0284(13) 0.0005(10) -0.0077(12) -0.0037(11) C28 0.0369(13) 0.0171(10) 0.0219(11) 0.0004(8) -0.0037(9) 0.0001(9) C29 0.0259(11) 0.0150(10) 0.0312(12) 0.0031(9) -0.0008(9) -0.0014(8) C30 0.0350(13) 0.0160(10) 0.0261(11) 0.0034(9) 0.0046(10) 0.0035(9) O2 0.0221(16) 0.0267(16) 0.0239(16) -0.0062(13) -0.0003(13) 0.0026(12) N1 0.0230(9) 0.0202(9) 0.0179(9) -0.0011(7) 0.0046(7) 0.0029(7) N2 0.0191(8) 0.0145(8) 0.0124(8) -0.0007(6) -0.0002(6) -0.0019(6) N3 0.0167(8) 0.0164(8) 0.0143(8) 0.0013(6) 0.0017(6) -0.0023(6) N4 0.0210(9) 0.0167(8) 0.0140(8) 0.0008(6) 0.0001(7) 0.0018(7) N5 0.0185(8) 0.0126(7) 0.0132(8) 0.0004(6) 0.0010(6) -0.0024(6) N6 0.0166(8) 0.0132(8) 0.0144(8) 0.0002(6) 0.0006(6) -0.0022(6) N7 0.0197(9) 0.0216(9) 0.0199(9) -0.0019(7) -0.0004(7) 0.0004(7) N8 0.0172(8) 0.0140(8) 0.0131(8) -0.0002(6) 0.0009(6) -0.0036(6) N9 0.0212(9) 0.0120(8) 0.0148(8) -0.0010(6) 0.0004(7) -0.0009(6) O1 0.0285(9) 0.0186(7) 0.0399(9) 0.0063(7) -0.0064(7) -0.0073(6) Zn1 0.01904(13) 0.01420(12) 0.01346(12) 0.00109(8) -0.00053(9) -0.00338(9) _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 B1 N8 1.537(3) . ? B1 N5 1.539(3) . ? B1 N2 1.542(3) . ? B1 H1 1.0000 . ? C1 C2 1.482(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.332(3) . ? C2 N2 1.336(2) . ? C3 N3 1.333(3) . ? C3 N1 1.351(3) . ? C3 C4 1.501(3) . ? C4 C5 1.523(3) . ? C4 C6 1.527(3) . ? C4 C7 1.529(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.485(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N4 1.332(3) . ? C9 N5 1.339(2) . ? C10 N6 1.330(2) . ? C10 N4 1.348(2) . ? C10 C11 1.503(3) . ? C11 C13 1.524(3) . ? C11 C14 1.527(3) . ? C11 C12 1.533(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.481(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N7 1.328(3) . ? C16 N8 1.331(3) . ? C17 N9 1.330(3) . ? C17 N7 1.347(3) . ? C17 C18 1.510(3) . ? C18 C21 1.523(3) . ? C18 C20 1.525(3) . ? C18 C19 1.527(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 O1 1.330(2) . ? C22 C27 1.388(3) . ? C22 C23 1.390(3) . ? C23 C24 1.388(3) . ? C23 H23 0.9500 . ? C24 C25 1.367(4) . ? C24 H24 0.9500 . ? C25 C26 1.372(4) . ? C25 H25 0.9500 . ? C26 C27 1.385(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C30 1.377(3) 3_576 ? C28 C29 1.384(3) . ? C28 H28 0.9500 . ? C29 O2 1.292(4) . ? C29 C30 1.379(3) . ? C29 H29 0.9500 . ? C30 C28 1.377(3) 3_576 ? C30 H30 0.9500 . ? O2 H2 0.8400 . ? N2 N3 1.379(2) . ? N3 Zn1 2.0671(17) . ? N5 N6 1.380(2) . ? N6 Zn1 2.0653(16) . ? N8 N9 1.380(2) . ? N9 Zn1 2.0329(18) . ? O1 Zn1 1.8365(15) . ? 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 N8 B1 N5 108.82(16) . . ? N8 B1 N2 109.27(16) . . ? N5 B1 N2 108.97(16) . . ? N8 B1 H1 109.9 . . ? N5 B1 H1 109.9 . . ? N2 B1 H1 109.9 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 N2 110.61(18) . . ? N1 C2 C1 124.54(18) . . ? N2 C2 C1 124.84(18) . . ? N3 C3 N1 112.09(17) . . ? N3 C3 C4 123.59(17) . . ? N1 C3 C4 124.23(17) . . ? C3 C4 C5 110.08(18) . . ? C3 C4 C6 107.52(17) . . ? C5 C4 C6 110.7(2) . . ? C3 C4 C7 110.20(17) . . ? C5 C4 C7 108.40(19) . . ? C6 C4 C7 109.99(19) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N4 C9 N5 111.15(17) . . ? N4 C9 C8 123.58(18) . . ? N5 C9 C8 125.25(18) . . ? N6 C10 N4 112.69(17) . . ? N6 C10 C11 123.89(17) . . ? N4 C10 C11 123.42(17) . . ? C10 C11 C13 109.95(17) . . ? C10 C11 C14 108.95(16) . . ? C13 C11 C14 109.31(17) . . ? C10 C11 C12 109.23(16) . . ? C13 C11 C12 109.92(17) . . ? C14 C11 C12 109.47(18) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N7 C16 N8 111.56(17) . . ? N7 C16 C15 123.79(19) . . ? N8 C16 C15 124.65(19) . . ? N9 C17 N7 112.74(18) . . ? N9 C17 C18 124.01(18) . . ? N7 C17 C18 123.23(18) . . ? C17 C18 C21 109.12(18) . . ? C17 C18 C20 108.80(16) . . ? C21 C18 C20 109.94(19) . . ? C17 C18 C19 109.72(17) . . ? C21 C18 C19 109.18(19) . . ? C20 C18 C19 110.05(18) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O1 C22 C27 122.7(2) . . ? O1 C22 C23 120.2(2) . . ? C27 C22 C23 117.1(2) . . ? C24 C23 C22 120.9(2) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C25 C24 C23 121.0(2) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 118.9(2) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? C25 C26 C27 120.6(2) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C22 121.5(2) . . ? C26 C27 H27 119.3 . . ? C22 C27 H27 119.3 . . ? C30 C28 C29 120.5(2) 3_576 . ? C30 C28 H28 119.8 3_576 . ? C29 C28 H28 119.8 . . ? O2 C29 C30 122.2(2) . . ? O2 C29 C28 118.4(2) . . ? C30 C29 C28 119.3(2) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C28 C30 C29 120.2(2) 3_576 . ? C28 C30 H30 119.9 3_576 . ? C29 C30 H30 119.9 . . ? C29 O2 H2 109.5 . . ? C2 N1 C3 104.80(16) . . ? C2 N2 N3 107.77(15) . . ? C2 N2 B1 131.08(16) . . ? N3 N2 B1 121.14(15) . . ? C3 N3 N2 104.72(15) . . ? C3 N3 Zn1 143.35(14) . . ? N2 N3 Zn1 111.90(11) . . ? C9 N4 C10 104.19(16) . . ? C9 N5 N6 107.21(15) . . ? C9 N5 B1 132.24(16) . . ? N6 N5 B1 120.50(15) . . ? C10 N6 N5 104.76(15) . . ? C10 N6 Zn1 142.61(13) . . ? N5 N6 Zn1 112.50(11) . . ? C16 N7 C17 103.96(17) . . ? C16 N8 N9 107.21(16) . . ? C16 N8 B1 130.93(16) . . ? N9 N8 B1 121.83(16) . . ? C17 N9 N8 104.53(16) . . ? C17 N9 Zn1 143.47(14) . . ? N8 N9 Zn1 111.99(12) . . ? C22 O1 Zn1 141.71(15) . . ? O1 Zn1 N9 134.79(7) . . ? O1 Zn1 N6 115.62(7) . . ? N9 Zn1 N6 92.78(6) . . ? O1 Zn1 N3 118.60(7) . . ? N9 Zn1 N3 92.78(6) . . ? N6 Zn1 N3 92.32(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 C3 C4 C5 50.7(3) . . . . ? N1 C3 C4 C5 -132.9(2) . . . . ? N3 C3 C4 C6 -69.9(3) . . . . ? N1 C3 C4 C6 106.5(2) . . . . ? N3 C3 C4 C7 170.2(2) . . . . ? N1 C3 C4 C7 -13.4(3) . . . . ? N6 C10 C11 C13 -59.4(2) . . . . ? N4 C10 C11 C13 120.8(2) . . . . ? N6 C10 C11 C14 -179.15(18) . . . . ? N4 C10 C11 C14 1.0(3) . . . . ? N6 C10 C11 C12 61.3(2) . . . . ? N4 C10 C11 C12 -118.5(2) . . . . ? N9 C17 C18 C21 170.8(2) . . . . ? N7 C17 C18 C21 -11.2(3) . . . . ? N9 C17 C18 C20 -69.2(3) . . . . ? N7 C17 C18 C20 108.8(2) . . . . ? N9 C17 C18 C19 51.3(3) . . . . ? N7 C17 C18 C19 -130.7(2) . . . . ? O1 C22 C23 C24 -178.6(2) . . . . ? C27 C22 C23 C24 -1.1(4) . . . . ? C22 C23 C24 C25 1.0(4) . . . . ? C23 C24 C25 C26 -0.8(4) . . . . ? C24 C25 C26 C27 0.8(4) . . . . ? C25 C26 C27 C22 -1.0(4) . . . . ? O1 C22 C27 C26 178.6(2) . . . . ? C23 C22 C27 C26 1.1(4) . . . . ? C30 C28 C29 O2 177.5(2) 3_576 . . . ? C30 C28 C29 C30 -0.9(3) 3_576 . . . ? O2 C29 C30 C28 -177.4(2) . . . 3_576 ? C28 C29 C30 C28 0.9(3) . . . 3_576 ? N2 C2 N1 C3 -0.1(2) . . . . ? C1 C2 N1 C3 -179.5(2) . . . . ? N3 C3 N1 C2 -0.3(2) . . . . ? C4 C3 N1 C2 -177.06(19) . . . . ? N1 C2 N2 N3 0.4(2) . . . . ? C1 C2 N2 N3 179.86(19) . . . . ? N1 C2 N2 B1 -179.82(18) . . . . ? C1 C2 N2 B1 -0.4(3) . . . . ? N8 B1 N2 C2 123.1(2) . . . . ? N5 B1 N2 C2 -118.1(2) . . . . ? N8 B1 N2 N3 -57.1(2) . . . . ? N5 B1 N2 N3 61.7(2) . . . . ? N1 C3 N3 N2 0.5(2) . . . . ? C4 C3 N3 N2 177.33(18) . . . . ? N1 C3 N3 Zn1 -176.99(17) . . . . ? C4 C3 N3 Zn1 -0.2(4) . . . . ? C2 N2 N3 C3 -0.6(2) . . . . ? B1 N2 N3 C3 179.63(17) . . . . ? C2 N2 N3 Zn1 177.84(13) . . . . ? B1 N2 N3 Zn1 -2.0(2) . . . . ? N5 C9 N4 C10 0.2(2) . . . . ? C8 C9 N4 C10 -178.25(18) . . . . ? N6 C10 N4 C9 -0.3(2) . . . . ? C11 C10 N4 C9 179.59(18) . . . . ? N4 C9 N5 N6 -0.1(2) . . . . ? C8 C9 N5 N6 178.33(18) . . . . ? N4 C9 N5 B1 177.35(18) . . . . ? C8 C9 N5 B1 -4.2(3) . . . . ? N8 B1 N5 C9 -117.5(2) . . . . ? N2 B1 N5 C9 123.4(2) . . . . ? N8 B1 N5 N6 59.7(2) . . . . ? N2 B1 N5 N6 -59.4(2) . . . . ? N4 C10 N6 N5 0.2(2) . . . . ? C11 C10 N6 N5 -179.65(17) . . . . ? N4 C10 N6 Zn1 -174.89(15) . . . . ? C11 C10 N6 Zn1 5.3(3) . . . . ? C9 N5 N6 C10 -0.1(2) . . . . ? B1 N5 N6 C10 -177.86(16) . . . . ? C9 N5 N6 Zn1 176.72(12) . . . . ? B1 N5 N6 Zn1 -1.1(2) . . . . ? N8 C16 N7 C17 0.2(2) . . . . ? C15 C16 N7 C17 179.9(2) . . . . ? N9 C17 N7 C16 0.1(2) . . . . ? C18 C17 N7 C16 -178.11(18) . . . . ? N7 C16 N8 N9 -0.5(2) . . . . ? C15 C16 N8 N9 179.87(19) . . . . ? N7 C16 N8 B1 -178.51(18) . . . . ? C15 C16 N8 B1 1.8(3) . . . . ? N5 B1 N8 C16 118.2(2) . . . . ? N2 B1 N8 C16 -122.9(2) . . . . ? N5 B1 N8 N9 -59.6(2) . . . . ? N2 B1 N8 N9 59.3(2) . . . . ? N7 C17 N9 N8 -0.4(2) . . . . ? C18 C17 N9 N8 177.82(17) . . . . ? N7 C17 N9 Zn1 178.21(16) . . . . ? C18 C17 N9 Zn1 -3.6(3) . . . . ? C16 N8 N9 C17 0.5(2) . . . . ? B1 N8 N9 C17 178.75(16) . . . . ? C16 N8 N9 Zn1 -178.59(12) . . . . ? B1 N8 N9 Zn1 -0.3(2) . . . . ? C27 C22 O1 Zn1 60.3(3) . . . . ? C23 C22 O1 Zn1 -122.4(2) . . . . ? C22 O1 Zn1 N9 6.5(3) . . . . ? C22 O1 Zn1 N6 130.1(2) . . . . ? C22 O1 Zn1 N3 -121.7(2) . . . . ? C17 N9 Zn1 O1 -1.1(3) . . . . ? N8 N9 Zn1 O1 177.39(11) . . . . ? C17 N9 Zn1 N6 -132.3(2) . . . . ? N8 N9 Zn1 N6 46.22(12) . . . . ? C17 N9 Zn1 N3 135.2(2) . . . . ? N8 N9 Zn1 N3 -46.25(12) . . . . ? C10 N6 Zn1 O1 -14.7(2) . . . . ? N5 N6 Zn1 O1 170.47(11) . . . . ? C10 N6 Zn1 N9 129.0(2) . . . . ? N5 N6 Zn1 N9 -45.86(12) . . . . ? C10 N6 Zn1 N3 -138.1(2) . . . . ? N5 N6 Zn1 N3 47.04(13) . . . . ? C3 N3 Zn1 O1 11.2(3) . . . . ? N2 N3 Zn1 O1 -166.24(12) . . . . ? C3 N3 Zn1 N9 -134.9(2) . . . . ? N2 N3 Zn1 N9 47.66(13) . . . . ? C3 N3 Zn1 N6 132.2(2) . . . . ? N2 N3 Zn1 N6 -45.24(13) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 N1 0.84 1.92 2.750(3) 169.2 . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.417 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.076 data_09mz450_0m _database_code_depnum_ccdc_archive 'CCDC 764052' #TrackingRef '- combined cifs' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H42 B N9 S Zn' _chemical_formula_sum 'C27 H42 B N9 S Zn' _chemical_formula_weight 600.94 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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' _cell_length_a 9.2539(11) _cell_length_b 17.075(2) _cell_length_c 18.952(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2994.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5751 _cell_measurement_theta_min 2.458 _cell_measurement_theta_max 31.854 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.923 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.511296 _exptl_absorpt_correction_T_max 0.746470 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2007)' _exptl_special_details ; The crystal under investigation was found to be non-merohedrally twinned. The orientation matrices for the two components were identified using the program Cell_Now, and the two components were integrated using Saint, resulting in a total of 22947 reflections. 9546 reflections (7096 unique ones) involved component 1 only (mean I/sigma = 13.9), 9436 reflections (6937 unique ones) involved component 2 only (mean I/sigma = 3.8), and 3961 reflections (3682 unique ones) involved both components (mean I/sigma = 13.1). 4 reflections (4 unique ) involved 3 domains (mean I/sigma 5.3). The exact twin matrix identified by the integration program was found to be 0.99810 0.01028 -0.02859, 0.03667 -0.99969 0.01328, -0.11929 -0.01762 -0.99818. The data were corrected for absorption using twinabs, and the structure was solved using direct methods with only the non-overlapping reflections of component 1. The structure was refined using the hklf 5 routine with all reflections of component 1 (including the overlapping ones) below a d-spacing threshold of 0.75, resulting in a BASF value of 0.085(1). No racemic twinning was observed. The Rint value given is for all reflections before the cutoff at d = 0.75 and is based on agreement between observed single and composite intensities and those calculated from refined unique intensities and twin fractions (TWINABS (Sheldrick, 2007)). ; _diffrn_ambient_temperature 100(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 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 22947 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7240 _reflns_number_gt 6826 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4 ' _computing_data_reduction 'Apex2 v2008.2-4 ' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0458P)^2^+0.6888P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.002(8) _chemical_absolute_configuration ad _refine_ls_number_reflns 7240 _refine_ls_number_parameters 365 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0853 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.8256(3) 0.13088(15) 0.08381(13) 0.0123(5) Uani 1 1 d . . . H1 H 0.8741 0.1766 0.1067 0.015 Uiso 1 1 calc R . . C1 C 1.1282(3) 0.10605(17) 0.16299(14) 0.0232(6) Uani 1 1 d . . . H1A H 1.0846 0.1104 0.2099 0.035 Uiso 1 1 calc R . . H1B H 1.1219 0.1567 0.1388 0.035 Uiso 1 1 calc R . . H1C H 1.2299 0.0909 0.1677 0.035 Uiso 1 1 calc R . . C2 C 1.0495(3) 0.04551(15) 0.12114(12) 0.0143(5) Uani 1 1 d . . . C3 C 0.9944(3) -0.06104(15) 0.07063(12) 0.0141(5) Uani 1 1 d . . . C4 C 1.0004(3) -0.14539(15) 0.04768(12) 0.0146(5) Uani 1 1 d . . . C5 C 1.1530(3) -0.17681(15) 0.05988(14) 0.0210(5) Uani 1 1 d . . . H5A H 1.2218 -0.1468 0.0313 0.031 Uiso 1 1 calc R . . H5B H 1.1570 -0.2321 0.0463 0.031 Uiso 1 1 calc R . . H5C H 1.1781 -0.1716 0.1099 0.031 Uiso 1 1 calc R . . C6 C 0.8918(3) -0.19289(16) 0.09125(14) 0.0218(5) Uani 1 1 d . . . H6A H 0.9174 -0.1897 0.1413 0.033 Uiso 1 1 calc R . . H6B H 0.8940 -0.2477 0.0760 0.033 Uiso 1 1 calc R . . H6C H 0.7945 -0.1716 0.0842 0.033 Uiso 1 1 calc R . . C7 C 0.9628(3) -0.15320(16) -0.03064(12) 0.0213(5) Uani 1 1 d . . . H7A H 0.8640 -0.1345 -0.0386 0.032 Uiso 1 1 calc R . . H7B H 0.9699 -0.2083 -0.0448 0.032 Uiso 1 1 calc R . . H7C H 1.0304 -0.1218 -0.0587 0.032 Uiso 1 1 calc R . . C8 C 0.9062(3) 0.28224(15) -0.00535(14) 0.0236(5) Uani 1 1 d . . . H8A H 0.8515 0.3054 0.0337 0.035 Uiso 1 1 calc R . . H8B H 0.9165 0.3209 -0.0433 0.035 Uiso 1 1 calc R . . H8C H 1.0021 0.2665 0.0114 0.035 Uiso 1 1 calc R . . C9 C 0.8280(3) 0.21244(14) -0.03248(12) 0.0154(4) Uani 1 1 d . . . C10 C 0.7298(3) 0.13155(15) -0.10235(12) 0.0147(5) Uani 1 1 d . . . C11 C 0.6740(3) 0.09788(15) -0.17092(11) 0.0164(5) Uani 1 1 d . . . C12 C 0.7524(3) 0.13774(18) -0.23193(12) 0.0244(6) Uani 1 1 d . . . H12A H 0.7274 0.1935 -0.2328 0.037 Uiso 1 1 calc R . . H12B H 0.7233 0.1134 -0.2765 0.037 Uiso 1 1 calc R . . H12C H 0.8570 0.1320 -0.2257 0.037 Uiso 1 1 calc R . . C13 C 0.5113(3) 0.11473(18) -0.17615(14) 0.0222(5) Uani 1 1 d . . . H13A H 0.4605 0.0874 -0.1381 0.033 Uiso 1 1 calc R . . H13B H 0.4750 0.0963 -0.2218 0.033 Uiso 1 1 calc R . . H13C H 0.4946 0.1712 -0.1719 0.033 Uiso 1 1 calc R . . C14 C 0.7010(3) 0.00958(15) -0.17568(12) 0.0200(5) Uani 1 1 d . . . H14A H 0.8048 -0.0008 -0.1715 0.030 Uiso 1 1 calc R . . H14B H 0.6661 -0.0100 -0.2212 0.030 Uiso 1 1 calc R . . H14C H 0.6495 -0.0170 -0.1374 0.030 Uiso 1 1 calc R . . C15 C 0.4401(3) -0.04823(15) 0.15850(13) 0.0172(5) Uani 1 1 d . . . H15A H 0.3397 -0.0365 0.1457 0.026 Uiso 1 1 calc R . . H15B H 0.4432 -0.0696 0.2065 0.026 Uiso 1 1 calc R . . H15C H 0.4798 -0.0867 0.1254 0.026 Uiso 1 1 calc R . . C16 C 0.5269(2) 0.02456(15) 0.15545(11) 0.0140(5) Uani 1 1 d . . . C17 C 0.6241(3) 0.13217(15) 0.18559(11) 0.0134(5) Uani 1 1 d . . . C18 C 0.6576(3) 0.20600(15) 0.22647(12) 0.0155(5) Uani 1 1 d . . . C19 C 0.5445(3) 0.21510(17) 0.28520(14) 0.0251(6) Uani 1 1 d . . . H19A H 0.4476 0.2163 0.2644 0.038 Uiso 1 1 calc R . . H19B H 0.5620 0.2640 0.3109 0.038 Uiso 1 1 calc R . . H19C H 0.5518 0.1708 0.3179 0.038 Uiso 1 1 calc R . . C20 C 0.8075(3) 0.20069(15) 0.26057(12) 0.0211(5) Uani 1 1 d . . . H20A H 0.8102 0.1560 0.2929 0.032 Uiso 1 1 calc R . . H20B H 0.8273 0.2490 0.2868 0.032 Uiso 1 1 calc R . . H20C H 0.8808 0.1937 0.2238 0.032 Uiso 1 1 calc R . . C21 C 0.6487(3) 0.27758(15) 0.17764(13) 0.0196(5) Uani 1 1 d . . . H21A H 0.7204 0.2725 0.1399 0.029 Uiso 1 1 calc R . . H21B H 0.6681 0.3252 0.2049 0.029 Uiso 1 1 calc R . . H21C H 0.5518 0.2807 0.1570 0.029 Uiso 1 1 calc R . . C22 C 0.3972(3) -0.05573(15) -0.06261(12) 0.0153(5) Uani 1 1 d . . . C23 C 0.3271(2) 0.00386(14) -0.02596(11) 0.0173(4) Uani 1 1 d . . . H23 H 0.3630 0.0202 0.0186 0.021 Uiso 1 1 calc R . . C24 C 0.2048(3) 0.03962(16) -0.05411(13) 0.0222(5) Uani 1 1 d . . . H24 H 0.1579 0.0804 -0.0288 0.027 Uiso 1 1 calc R . . C25 C 0.1514(3) 0.01591(18) -0.11899(14) 0.0250(6) Uani 1 1 d . . . H25 H 0.0688 0.0408 -0.1386 0.030 Uiso 1 1 calc R . . C26 C 0.2188(3) -0.04401(18) -0.15492(14) 0.0254(6) Uani 1 1 d . . . H26 H 0.1810 -0.0611 -0.1989 0.030 Uiso 1 1 calc R . . C27 C 0.3409(3) -0.07939(16) -0.12760(13) 0.0199(5) Uani 1 1 d . . . H27 H 0.3869 -0.1202 -0.1532 0.024 Uiso 1 1 calc R . . N1 N 1.0941(2) -0.02773(13) 0.11343(10) 0.0162(4) Uani 1 1 d . . . N2 N 0.8905(2) -0.01113(12) 0.05274(9) 0.0133(4) Uani 1 1 d . . . N3 N 0.9262(2) 0.05819(12) 0.08563(10) 0.0126(4) Uani 1 1 d . . . N4 N 0.7889(2) 0.20386(13) -0.09982(10) 0.0170(4) Uani 1 1 d . . . N5 N 0.7277(2) 0.09617(12) -0.03932(10) 0.0141(4) Uani 1 1 d . . . N6 N 0.7917(2) 0.14955(11) 0.00573(10) 0.0129(4) Uani 1 1 d . . . N7 N 0.5244(2) 0.08063(12) 0.20580(10) 0.0149(4) Uani 1 1 d . . . N8 N 0.6848(2) 0.10976(11) 0.12404(9) 0.0126(4) Uani 1 1 d . . . N9 N 0.6207(2) 0.04061(12) 0.10460(10) 0.0134(4) Uani 1 1 d . . . S1 S 0.55001(7) -0.10619(4) -0.02856(3) 0.01710(13) Uani 1 1 d . . . Zn1 Zn 0.68650(3) -0.008646(15) 0.011342(13) 0.01222(7) 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 B1 0.0153(12) 0.0081(11) 0.0135(11) -0.0012(9) 0.0027(10) -0.0007(10) C1 0.0187(12) 0.0193(14) 0.0314(13) -0.0102(12) -0.0083(10) 0.0037(11) C2 0.0120(11) 0.0153(12) 0.0158(10) -0.0010(9) -0.0013(9) 0.0013(9) C3 0.0144(11) 0.0146(11) 0.0132(10) 0.0019(9) 0.0002(8) -0.0006(9) C4 0.0174(12) 0.0112(11) 0.0153(10) 0.0000(9) 0.0007(8) 0.0001(9) C5 0.0206(13) 0.0119(11) 0.0303(13) 0.0003(10) 0.0004(10) 0.0028(9) C6 0.0257(14) 0.0149(13) 0.0247(12) 0.0006(10) 0.0075(10) -0.0012(11) C7 0.0325(14) 0.0154(12) 0.0162(11) -0.0024(9) -0.0018(10) 0.0029(11) C8 0.0319(14) 0.0162(12) 0.0226(12) -0.0001(10) 0.0033(11) -0.0070(10) C9 0.0172(11) 0.0108(10) 0.0184(10) -0.0002(8) 0.0027(9) 0.0002(9) C10 0.0132(11) 0.0152(12) 0.0156(10) 0.0029(9) 0.0006(8) 0.0018(9) C11 0.0177(11) 0.0178(12) 0.0137(10) 0.0017(9) 0.0007(9) 0.0005(10) C12 0.0291(14) 0.0295(16) 0.0146(11) 0.0013(11) -0.0002(10) -0.0078(12) C13 0.0187(12) 0.0251(15) 0.0228(12) 0.0011(11) -0.0049(10) 0.0010(11) C14 0.0244(12) 0.0192(12) 0.0165(10) -0.0045(10) -0.0004(9) 0.0021(12) C15 0.0159(12) 0.0157(12) 0.0200(11) 0.0022(9) -0.0003(9) -0.0013(10) C16 0.0123(10) 0.0152(12) 0.0144(10) 0.0024(9) -0.0016(8) 0.0013(9) C17 0.0153(11) 0.0153(12) 0.0098(9) 0.0005(9) -0.0015(8) 0.0035(9) C18 0.0212(13) 0.0115(11) 0.0137(10) -0.0015(9) 0.0016(8) 0.0003(9) C19 0.0354(16) 0.0193(14) 0.0206(12) -0.0047(11) 0.0101(11) -0.0003(12) C20 0.0271(13) 0.0176(12) 0.0188(11) -0.0017(9) -0.0055(11) 0.0000(12) C21 0.0256(14) 0.0136(12) 0.0195(11) -0.0013(10) 0.0014(9) 0.0015(10) C22 0.0168(11) 0.0136(12) 0.0155(10) 0.0049(9) -0.0016(9) -0.0038(9) C23 0.0188(10) 0.0150(11) 0.0182(10) 0.0011(9) -0.0008(8) -0.0037(10) C24 0.0191(13) 0.0208(13) 0.0269(12) 0.0052(10) 0.0029(10) -0.0006(11) C25 0.0152(12) 0.0295(15) 0.0303(13) 0.0142(12) -0.0046(9) -0.0053(11) C26 0.0270(15) 0.0294(15) 0.0197(11) 0.0059(11) -0.0077(10) -0.0113(12) C27 0.0228(14) 0.0196(13) 0.0172(11) -0.0006(10) -0.0040(9) -0.0072(11) N1 0.0146(10) 0.0160(11) 0.0182(9) -0.0037(8) -0.0038(7) 0.0021(8) N2 0.0161(9) 0.0095(9) 0.0144(8) -0.0014(8) 0.0002(7) -0.0011(8) N3 0.0127(10) 0.0111(10) 0.0141(8) -0.0026(7) -0.0011(7) -0.0003(8) N4 0.0218(11) 0.0132(10) 0.0161(9) 0.0014(8) 0.0017(8) -0.0015(9) N5 0.0159(10) 0.0112(10) 0.0150(8) -0.0026(8) -0.0006(7) -0.0005(7) N6 0.0145(9) 0.0092(8) 0.0150(8) -0.0028(7) 0.0008(7) 0.0003(7) N7 0.0152(10) 0.0140(10) 0.0155(9) 0.0015(8) 0.0003(7) 0.0006(8) N8 0.0132(9) 0.0114(9) 0.0132(8) -0.0029(7) -0.0007(8) -0.0007(9) N9 0.0126(9) 0.0106(10) 0.0170(9) -0.0015(8) -0.0006(7) -0.0021(8) S1 0.0193(3) 0.0104(3) 0.0216(3) -0.0014(2) -0.0061(2) -0.0017(2) Zn1 0.01362(11) 0.00985(12) 0.01321(11) -0.00101(9) -0.00217(9) -0.00088(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 B1 N6 1.546(3) . ? B1 N8 1.552(3) . ? B1 N3 1.552(3) . ? B1 H1 1.0000 . ? C1 C2 1.493(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.325(3) . ? C2 N3 1.342(3) . ? C3 N2 1.329(3) . ? C3 N1 1.354(3) . ? C3 C4 1.506(3) . ? C4 C5 1.529(3) . ? C4 C7 1.530(3) . ? C4 C6 1.533(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.486(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N4 1.335(3) . ? C9 N6 1.338(3) . ? C10 N5 1.339(3) . ? C10 N4 1.351(3) . ? C10 C11 1.512(3) . ? C11 C12 1.525(3) . ? C11 C14 1.531(3) . ? C11 C13 1.536(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.481(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N9 1.325(3) . ? C16 N7 1.352(3) . ? C17 N7 1.331(3) . ? C17 N8 1.350(3) . ? C17 C18 1.512(3) . ? C18 C20 1.534(4) . ? C18 C21 1.535(3) . ? C18 C19 1.535(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.392(3) . ? C22 C27 1.397(3) . ? C22 S1 1.777(3) . ? C23 C24 1.392(3) . ? C23 H23 0.9500 . ? C24 C25 1.386(4) . ? C24 H24 0.9500 . ? C25 C26 1.378(4) . ? C25 H25 0.9500 . ? C26 C27 1.382(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? N2 N3 1.378(3) . ? N2 Zn1 2.0451(19) . ? N5 N6 1.382(3) . ? N5 Zn1 2.066(2) . ? N8 N9 1.372(3) . ? N9 Zn1 2.050(2) . ? S1 Zn1 2.2229(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 N6 B1 N8 110.38(19) . . ? N6 B1 N3 107.93(17) . . ? N8 B1 N3 107.87(18) . . ? N6 B1 H1 110.2 . . ? N8 B1 H1 110.2 . . ? N3 B1 H1 110.2 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 N3 111.2(2) . . ? N1 C2 C1 124.1(2) . . ? N3 C2 C1 124.7(2) . . ? N2 C3 N1 112.1(2) . . ? N2 C3 C4 124.5(2) . . ? N1 C3 C4 123.4(2) . . ? C3 C4 C5 109.0(2) . . ? C3 C4 C7 110.8(2) . . ? C5 C4 C7 109.0(2) . . ? C3 C4 C6 109.1(2) . . ? C5 C4 C6 109.8(2) . . ? C7 C4 C6 109.1(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N4 C9 N6 111.2(2) . . ? N4 C9 C8 123.4(2) . . ? N6 C9 C8 125.4(2) . . ? N5 C10 N4 112.7(2) . . ? N5 C10 C11 126.2(2) . . ? N4 C10 C11 121.1(2) . . ? C10 C11 C12 108.6(2) . . ? C10 C11 C14 111.7(2) . . ? C12 C11 C14 108.5(2) . . ? C10 C11 C13 108.6(2) . . ? C12 C11 C13 109.5(2) . . ? C14 C11 C13 109.9(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N9 C16 N7 112.2(2) . . ? N9 C16 C15 123.9(2) . . ? N7 C16 C15 123.9(2) . . ? N7 C17 N8 110.5(2) . . ? N7 C17 C18 123.1(2) . . ? N8 C17 C18 126.4(2) . . ? C17 C18 C20 110.6(2) . . ? C17 C18 C21 110.12(19) . . ? C20 C18 C21 110.5(2) . . ? C17 C18 C19 108.4(2) . . ? C20 C18 C19 108.5(2) . . ? C21 C18 C19 108.7(2) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C27 118.5(2) . . ? C23 C22 S1 122.96(17) . . ? C27 C22 S1 118.5(2) . . ? C24 C23 C22 120.6(2) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 120.1(3) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C26 C25 C24 119.6(2) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 120.6(2) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C22 120.6(3) . . ? C26 C27 H27 119.7 . . ? C22 C27 H27 119.7 . . ? C2 N1 C3 104.5(2) . . ? C3 N2 N3 105.20(18) . . ? C3 N2 Zn1 141.19(17) . . ? N3 N2 Zn1 112.15(14) . . ? C2 N3 N2 106.98(19) . . ? C2 N3 B1 130.6(2) . . ? N2 N3 B1 122.21(18) . . ? C9 N4 C10 104.1(2) . . ? C10 N5 N6 104.31(19) . . ? C10 N5 Zn1 143.91(17) . . ? N6 N5 Zn1 111.30(14) . . ? C9 N6 N5 107.62(18) . . ? C9 N6 B1 129.24(19) . . ? N5 N6 B1 122.83(18) . . ? C17 N7 C16 104.66(19) . . ? C17 N8 N9 107.22(19) . . ? C17 N8 B1 135.1(2) . . ? N9 N8 B1 115.54(18) . . ? C16 N9 N8 105.42(19) . . ? C16 N9 Zn1 137.44(17) . . ? N8 N9 Zn1 117.14(14) . . ? C22 S1 Zn1 102.26(8) . . ? N2 Zn1 N9 87.25(8) . . ? N2 Zn1 N5 91.49(8) . . ? N9 Zn1 N5 95.74(8) . . ? N2 Zn1 S1 129.76(6) . . ? N9 Zn1 S1 115.59(6) . . ? N5 Zn1 S1 126.56(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C3 C4 C5 163.7(2) . . . . ? N1 C3 C4 C5 -17.7(3) . . . . ? N2 C3 C4 C7 43.7(3) . . . . ? N1 C3 C4 C7 -137.7(2) . . . . ? N2 C3 C4 C6 -76.4(3) . . . . ? N1 C3 C4 C6 102.2(3) . . . . ? N5 C10 C11 C12 -155.5(2) . . . . ? N4 C10 C11 C12 24.5(3) . . . . ? N5 C10 C11 C14 -35.9(3) . . . . ? N4 C10 C11 C14 144.2(2) . . . . ? N5 C10 C11 C13 85.5(3) . . . . ? N4 C10 C11 C13 -94.5(3) . . . . ? N7 C17 C18 C20 110.5(2) . . . . ? N8 C17 C18 C20 -71.6(3) . . . . ? N7 C17 C18 C21 -127.1(2) . . . . ? N8 C17 C18 C21 50.8(3) . . . . ? N7 C17 C18 C19 -8.4(3) . . . . ? N8 C17 C18 C19 169.6(2) . . . . ? C27 C22 C23 C24 -0.9(3) . . . . ? S1 C22 C23 C24 -177.79(19) . . . . ? C22 C23 C24 C25 0.2(4) . . . . ? C23 C24 C25 C26 0.9(4) . . . . ? C24 C25 C26 C27 -1.4(4) . . . . ? C25 C26 C27 C22 0.8(4) . . . . ? C23 C22 C27 C26 0.4(4) . . . . ? S1 C22 C27 C26 177.4(2) . . . . ? N3 C2 N1 C3 0.7(3) . . . . ? C1 C2 N1 C3 -178.3(2) . . . . ? N2 C3 N1 C2 -0.6(3) . . . . ? C4 C3 N1 C2 -179.5(2) . . . . ? N1 C3 N2 N3 0.4(3) . . . . ? C4 C3 N2 N3 179.1(2) . . . . ? N1 C3 N2 Zn1 -163.59(18) . . . . ? C4 C3 N2 Zn1 15.2(4) . . . . ? N1 C2 N3 N2 -0.5(3) . . . . ? C1 C2 N3 N2 178.5(2) . . . . ? N1 C2 N3 B1 173.7(2) . . . . ? C1 C2 N3 B1 -7.3(4) . . . . ? C3 N2 N3 C2 0.1(2) . . . . ? Zn1 N2 N3 C2 169.30(15) . . . . ? C3 N2 N3 B1 -174.69(19) . . . . ? Zn1 N2 N3 B1 -5.5(2) . . . . ? N6 B1 N3 C2 132.2(2) . . . . ? N8 B1 N3 C2 -108.6(3) . . . . ? N6 B1 N3 N2 -54.4(3) . . . . ? N8 B1 N3 N2 64.9(2) . . . . ? N6 C9 N4 C10 -1.6(3) . . . . ? C8 C9 N4 C10 176.4(2) . . . . ? N5 C10 N4 C9 1.5(3) . . . . ? C11 C10 N4 C9 -178.5(2) . . . . ? N4 C10 N5 N6 -0.8(3) . . . . ? C11 C10 N5 N6 179.2(2) . . . . ? N4 C10 N5 Zn1 -171.4(2) . . . . ? C11 C10 N5 Zn1 8.7(4) . . . . ? N4 C9 N6 N5 1.2(3) . . . . ? C8 C9 N6 N5 -176.8(2) . . . . ? N4 C9 N6 B1 174.8(2) . . . . ? C8 C9 N6 B1 -3.2(4) . . . . ? C10 N5 N6 C9 -0.2(2) . . . . ? Zn1 N5 N6 C9 173.85(15) . . . . ? C10 N5 N6 B1 -174.3(2) . . . . ? Zn1 N5 N6 B1 -0.3(2) . . . . ? N8 B1 N6 C9 127.6(2) . . . . ? N3 B1 N6 C9 -114.7(2) . . . . ? N8 B1 N6 N5 -59.6(3) . . . . ? N3 B1 N6 N5 58.0(3) . . . . ? N8 C17 N7 C16 1.1(3) . . . . ? C18 C17 N7 C16 179.4(2) . . . . ? N9 C16 N7 C17 -1.7(3) . . . . ? C15 C16 N7 C17 175.6(2) . . . . ? N7 C17 N8 N9 -0.2(3) . . . . ? C18 C17 N8 N9 -178.4(2) . . . . ? N7 C17 N8 B1 -162.0(2) . . . . ? C18 C17 N8 B1 19.9(4) . . . . ? N6 B1 N8 C17 -131.4(3) . . . . ? N3 B1 N8 C17 110.9(3) . . . . ? N6 B1 N8 N9 68.0(2) . . . . ? N3 B1 N8 N9 -49.7(2) . . . . ? N7 C16 N9 N8 1.6(3) . . . . ? C15 C16 N9 N8 -175.7(2) . . . . ? N7 C16 N9 Zn1 -177.98(17) . . . . ? C15 C16 N9 Zn1 4.8(4) . . . . ? C17 N8 N9 C16 -0.8(2) . . . . ? B1 N8 N9 C16 165.02(19) . . . . ? C17 N8 N9 Zn1 178.84(15) . . . . ? B1 N8 N9 Zn1 -15.3(2) . . . . ? C23 C22 S1 Zn1 -46.2(2) . . . . ? C27 C22 S1 Zn1 136.92(18) . . . . ? C3 N2 Zn1 N9 118.2(2) . . . . ? N3 N2 Zn1 N9 -45.09(14) . . . . ? C3 N2 Zn1 N5 -146.2(2) . . . . ? N3 N2 Zn1 N5 50.59(15) . . . . ? C3 N2 Zn1 S1 -3.3(3) . . . . ? N3 N2 Zn1 S1 -166.59(11) . . . . ? C16 N9 Zn1 N2 -121.9(3) . . . . ? N8 N9 Zn1 N2 58.64(17) . . . . ? C16 N9 Zn1 N5 146.9(2) . . . . ? N8 N9 Zn1 N5 -32.58(17) . . . . ? C16 N9 Zn1 S1 11.5(3) . . . . ? N8 N9 Zn1 S1 -167.98(14) . . . . ? C10 N5 Zn1 N2 122.6(3) . . . . ? N6 N5 Zn1 N2 -47.57(15) . . . . ? C10 N5 Zn1 N9 -150.0(3) . . . . ? N6 N5 Zn1 N9 39.82(15) . . . . ? C10 N5 Zn1 S1 -22.1(3) . . . . ? N6 N5 Zn1 S1 167.77(11) . . . . ? C22 S1 Zn1 N2 -174.83(10) . . . . ? C22 S1 Zn1 N9 75.96(10) . . . . ? C22 S1 Zn1 N5 -43.60(11) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.369 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.063 data_09mz289_0m _database_code_depnum_ccdc_archive 'CCDC 764053' #TrackingRef '- combined cifs' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H58 B2 N20 O6 Zn2, C7 H8' _chemical_formula_sum 'C73 H66 B2 N20 O6 Zn2' _chemical_formula_weight 1471.82 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' Zn Zn 0.2839 1.4301 '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 25.0768(17) _cell_length_b 19.0144(13) _cell_length_c 29.281(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13961.9(16) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9957 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 31.25 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6096 _exptl_absorpt_coefficient_mu 0.756 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.739 _exptl_absorpt_correction_T_max 0.815 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 140364 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 28.28 _reflns_number_total 17337 _reflns_number_gt 13729 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4' _computing_data_reduction 'Apex2 v2008.2-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0466P)^2^+12.6632P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17337 _refine_ls_number_parameters 935 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.1025 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 B1 B 0.82299(8) 0.68981(11) 0.42037(7) 0.0197(4) Uani 1 1 d . . . H1 H 0.7903 0.6643 0.4282 0.024 Uiso 1 1 calc R . . B2 B 0.95993(8) 0.87932(11) 0.17957(7) 0.0188(4) Uani 1 1 d . . . H2 H 0.9878 0.9110 0.1909 0.023 Uiso 1 1 calc R . . C1 C 0.82078(8) 0.78932(10) 0.50983(6) 0.0231(4) Uani 1 1 d . . . H1A H 0.8287 0.8253 0.4879 0.035 Uiso 1 1 calc R . . H1B H 0.8263 0.8074 0.5401 0.035 Uiso 1 1 calc R . . H1C H 0.7843 0.7749 0.5065 0.035 Uiso 1 1 calc R . . C2 C 0.85647(7) 0.72787(9) 0.50217(6) 0.0189(3) Uani 1 1 d . . . C3 C 0.91456(7) 0.64639(9) 0.51044(6) 0.0190(3) Uani 1 1 d . . . C4 C 0.95739(7) 0.60272(10) 0.53083(6) 0.0203(4) Uani 1 1 d . . . C5 C 1.00587(8) 0.63374(11) 0.54209(6) 0.0247(4) Uani 1 1 d . . . H5 H 1.0112 0.6813 0.5363 0.030 Uiso 1 1 calc R . . C6 C 1.04639(8) 0.59411(12) 0.56190(7) 0.0302(4) Uani 1 1 d . . . H6 H 1.0791 0.6148 0.5687 0.036 Uiso 1 1 calc R . . C7 C 1.03777(9) 0.52423(12) 0.57134(7) 0.0319(5) Uani 1 1 d . . . H7 H 1.0643 0.4979 0.5855 0.038 Uiso 1 1 calc R . . C8 C 0.98994(9) 0.49291(11) 0.55990(7) 0.0298(4) Uani 1 1 d . . . H8 H 0.9845 0.4456 0.5664 0.036 Uiso 1 1 calc R . . C9 C 0.94985(8) 0.53146(10) 0.53869(6) 0.0243(4) Uani 1 1 d . . . H9 H 0.9183 0.5097 0.5299 0.029 Uiso 1 1 calc R . . C10 C 0.70932(8) 0.76573(12) 0.42003(7) 0.0295(4) Uani 1 1 d . . . H10A H 0.7096 0.7506 0.4513 0.044 Uiso 1 1 calc R . . H10B H 0.7039 0.7259 0.4005 0.044 Uiso 1 1 calc R . . H10C H 0.6810 0.7990 0.4155 0.044 Uiso 1 1 calc R . . C11 C 0.76137(8) 0.79946(10) 0.40881(6) 0.0233(4) Uani 1 1 d . . . C12 C 0.82013(8) 0.87558(10) 0.39382(6) 0.0225(4) Uani 1 1 d . . . C13 C 0.84624(8) 0.94403(10) 0.38729(6) 0.0250(4) Uani 1 1 d . . . C14 C 0.81586(9) 1.00144(11) 0.37325(7) 0.0327(5) Uani 1 1 d . . . H14 H 0.7802 0.9953 0.3656 0.039 Uiso 1 1 calc R . . C15 C 0.83858(11) 1.06763(12) 0.37062(8) 0.0393(5) Uani 1 1 d . . . H15 H 0.8180 1.1057 0.3613 0.047 Uiso 1 1 calc R . . C16 C 0.89134(11) 1.07759(12) 0.38161(8) 0.0395(5) Uani 1 1 d . . . H16 H 0.9061 1.1224 0.3805 0.047 Uiso 1 1 calc R . . C17 C 0.92251(10) 1.02076(12) 0.39433(8) 0.0380(5) Uani 1 1 d . . . H17 H 0.9585 1.0272 0.4009 0.046 Uiso 1 1 calc R . . C18 C 0.90011(9) 0.95399(11) 0.39738(8) 0.0324(5) Uani 1 1 d . . . H18 H 0.9210 0.9159 0.4062 0.039 Uiso 1 1 calc R . . C19 C 0.82177(9) 0.52874(11) 0.40256(8) 0.0301(4) Uani 1 1 d . . . H19A H 0.8210 0.4840 0.3874 0.045 Uiso 1 1 calc R . . H19B H 0.7859 0.5450 0.4072 0.045 Uiso 1 1 calc R . . H19C H 0.8393 0.5240 0.4315 0.045 Uiso 1 1 calc R . . C20 C 0.85118(8) 0.58021(10) 0.37394(6) 0.0224(4) Uani 1 1 d . . . C21 C 0.90403(7) 0.62525(10) 0.32616(6) 0.0207(4) Uani 1 1 d . . . C22 C 0.93968(8) 0.63199(10) 0.28638(6) 0.0222(4) Uani 1 1 d . . . C23 C 0.93266(9) 0.58463(11) 0.25025(7) 0.0276(4) Uani 1 1 d . . . H23 H 0.9061 0.5506 0.2518 0.033 Uiso 1 1 calc R . . C24 C 0.96540(10) 0.58850(12) 0.21212(7) 0.0339(5) Uani 1 1 d . . . H24 H 0.9607 0.5571 0.1881 0.041 Uiso 1 1 calc R . . C25 C 1.00509(9) 0.63906(12) 0.20981(7) 0.0336(5) Uani 1 1 d . . . H25 H 1.0269 0.6417 0.1842 0.040 Uiso 1 1 calc R . . C26 C 1.01236(8) 0.68566(11) 0.24556(7) 0.0302(4) Uani 1 1 d . . . H26 H 1.0390 0.7196 0.2439 0.036 Uiso 1 1 calc R . . C27 C 0.97998(8) 0.68189(10) 0.28388(7) 0.0245(4) Uani 1 1 d . . . H27 H 0.9853 0.7129 0.3080 0.029 Uiso 1 1 calc R . . C28 C 1.01336(8) 0.79012(10) 0.39721(6) 0.0239(4) Uani 1 1 d . . . C29 C 1.06068(8) 0.83040(11) 0.40013(7) 0.0300(4) Uani 1 1 d . . . H29 H 1.0619 0.8745 0.3864 0.036 Uiso 1 1 calc R . . C30 C 1.10490(9) 0.80579(12) 0.42280(8) 0.0323(5) Uani 1 1 d . . . H30 H 1.1360 0.8323 0.4241 0.039 Uiso 1 1 calc R . . C31 C 1.10206(8) 0.74025(11) 0.44385(7) 0.0278(4) Uani 1 1 d . . . C32 C 1.05640(9) 0.69992(11) 0.44214(7) 0.0288(4) Uani 1 1 d . . . H32 H 1.0554 0.6563 0.4565 0.035 Uiso 1 1 calc R . . C33 C 1.01220(8) 0.72439(11) 0.41901(7) 0.0270(4) Uani 1 1 d . . . H33 H 0.9814 0.6971 0.4179 0.032 Uiso 1 1 calc R . . C34 C 0.95066(10) 1.04181(11) 0.17549(9) 0.0380(5) Uani 1 1 d . . . H34A H 0.9418 1.0894 0.1676 0.057 Uiso 1 1 calc R . . H34B H 0.9871 1.0326 0.1676 0.057 Uiso 1 1 calc R . . H34C H 0.9459 1.0350 0.2077 0.057 Uiso 1 1 calc R . . C35 C 0.91524(8) 0.99279(10) 0.15004(7) 0.0246(4) Uani 1 1 d . . . C36 C 0.85547(7) 0.95267(9) 0.10642(6) 0.0198(3) Uani 1 1 d . . . C37 C 0.81215(7) 0.95377(10) 0.07219(6) 0.0212(4) Uani 1 1 d . . . C38 C 0.80314(9) 1.01743(11) 0.04941(7) 0.0288(4) Uani 1 1 d . . . H38 H 0.8238 1.0565 0.0565 0.035 Uiso 1 1 calc R . . C39 C 0.76380(9) 1.02273(12) 0.01642(8) 0.0353(5) Uani 1 1 d . . . H39 H 0.7583 1.0651 0.0013 0.042 Uiso 1 1 calc R . . C40 C 0.73278(9) 0.96493(13) 0.00606(8) 0.0362(5) Uani 1 1 d . . . H40 H 0.7061 0.9685 -0.0159 0.043 Uiso 1 1 calc R . . C41 C 0.74129(8) 0.90159(12) 0.02826(7) 0.0316(5) Uani 1 1 d . . . H41 H 0.7205 0.8627 0.0209 0.038 Uiso 1 1 calc R . . C42 C 0.78074(8) 0.89579(11) 0.06144(7) 0.0249(4) Uani 1 1 d . . . H42 H 0.7861 0.8532 0.0764 0.030 Uiso 1 1 calc R . . C43 C 1.08245(8) 0.84049(13) 0.17229(8) 0.0336(5) Uani 1 1 d . . . H43A H 1.0799 0.8326 0.2046 0.050 Uiso 1 1 calc R . . H43B H 1.0796 0.8899 0.1661 0.050 Uiso 1 1 calc R . . H43C H 1.1161 0.8234 0.1614 0.050 Uiso 1 1 calc R . . C44 C 1.03846(8) 0.80253(11) 0.14866(7) 0.0251(4) Uani 1 1 d . . . C45 C 0.99527(8) 0.72982(10) 0.10891(6) 0.0243(4) Uani 1 1 d . . . C46 C 0.98074(9) 0.67169(11) 0.07784(7) 0.0288(4) Uani 1 1 d . . . C47 C 1.01208(11) 0.65796(12) 0.03928(8) 0.0414(6) Uani 1 1 d . . . H47 H 1.0432 0.6834 0.0341 0.050 Uiso 1 1 calc R . . C48 C 0.99619(14) 0.60591(14) 0.00892(8) 0.0548(8) Uani 1 1 d . . . H48 H 1.0165 0.5971 -0.0170 0.066 Uiso 1 1 calc R . . C49 C 0.95073(14) 0.56732(14) 0.01692(9) 0.0541(8) Uani 1 1 d . . . H49 H 0.9407 0.5324 -0.0036 0.065 Uiso 1 1 calc R . . C50 C 0.91989(12) 0.58004(13) 0.05524(9) 0.0442(6) Uani 1 1 d . . . H50 H 0.8893 0.5536 0.0606 0.053 Uiso 1 1 calc R . . C51 C 0.93499(9) 0.63264(11) 0.08560(8) 0.0323(5) Uani 1 1 d . . . H51 H 0.9143 0.6416 0.1113 0.039 Uiso 1 1 calc R . . C52 C 0.98226(9) 0.89781(12) 0.28629(7) 0.0317(5) Uani 1 1 d . . . H52A H 1.0132 0.8685 0.2898 0.048 Uiso 1 1 calc R . . H52B H 0.9714 0.9151 0.3156 0.048 Uiso 1 1 calc R . . H52C H 0.9907 0.9367 0.2667 0.048 Uiso 1 1 calc R . . C53 C 0.93815(7) 0.85597(10) 0.26573(6) 0.0204(4) Uani 1 1 d . . . C54 C 0.86985(7) 0.79011(9) 0.25529(6) 0.0180(3) Uani 1 1 d . . . C55 C 0.82176(7) 0.74800(10) 0.26395(6) 0.0203(4) Uani 1 1 d . . . C56 C 0.78240(8) 0.77271(12) 0.29317(7) 0.0287(4) Uani 1 1 d . . . H56 H 0.7877 0.8142 0.3094 0.034 Uiso 1 1 calc R . . C57 C 0.73498(9) 0.73536(16) 0.29819(8) 0.0422(6) Uani 1 1 d . . . H57 H 0.7082 0.7526 0.3171 0.051 Uiso 1 1 calc R . . C58 C 0.72771(10) 0.67306(15) 0.27515(8) 0.0428(6) Uani 1 1 d . . . H58 H 0.6961 0.6481 0.2787 0.051 Uiso 1 1 calc R . . C59 C 0.76717(10) 0.64744(12) 0.24668(8) 0.0370(5) Uani 1 1 d . . . H59 H 0.7624 0.6048 0.2317 0.044 Uiso 1 1 calc R . . C60 C 0.81379(9) 0.68522(10) 0.24041(7) 0.0276(4) Uani 1 1 d . . . H60 H 0.8398 0.6687 0.2205 0.033 Uiso 1 1 calc R . . C61 C 0.78403(8) 0.73033(10) 0.13327(6) 0.0209(4) Uani 1 1 d . . . C62 C 0.74619(8) 0.67616(10) 0.12588(6) 0.0250(4) Uani 1 1 d . . . H62 H 0.7561 0.6364 0.1094 0.030 Uiso 1 1 calc R . . C63 C 0.69515(8) 0.68138(11) 0.14267(7) 0.0277(4) Uani 1 1 d . . . H63 H 0.6704 0.6460 0.1372 0.033 Uiso 1 1 calc R . . C64 C 0.68101(8) 0.74064(11) 0.16806(7) 0.0262(4) Uani 1 1 d . . . C65 C 0.71746(8) 0.79391(10) 0.17683(7) 0.0241(4) Uani 1 1 d . . . H65 H 0.7077 0.8326 0.1944 0.029 Uiso 1 1 calc R . . C66 C 0.76828(8) 0.78883(10) 0.15931(6) 0.0209(4) Uani 1 1 d . . . H66 H 0.7926 0.8248 0.1648 0.025 Uiso 1 1 calc R . . C67 C 0.75126(12) 0.98382(13) 0.18375(9) 0.0466(6) Uani 1 1 d . . . H67 H 0.7604 0.9965 0.1541 0.056 Uiso 1 1 calc R . . C68 C 0.79136(14) 0.97430(15) 0.21669(10) 0.0574(8) Uani 1 1 d . . . H68 H 0.8269 0.9806 0.2085 0.069 Uiso 1 1 calc R . . C69 C 0.77906(15) 0.95606(17) 0.26007(11) 0.0620(8) Uani 1 1 d . . . H69 H 0.8057 0.9496 0.2817 0.074 Uiso 1 1 calc R . . C70 C 0.72610(14) 0.94724(15) 0.27145(11) 0.0590(8) Uani 1 1 d . . . H70 H 0.7176 0.9353 0.3014 0.071 Uiso 1 1 calc R . . C71 C 0.68586(14) 0.95525(14) 0.24078(11) 0.0582(8) Uani 1 1 d . . . H71 H 0.6506 0.9483 0.2495 0.070 Uiso 1 1 calc R . . C72 C 0.69850(13) 0.97443(15) 0.19511(12) 0.0587(8) Uani 1 1 d . . . C73 C 0.65661(18) 0.9833(2) 0.16043(16) 0.0976(15) Uani 1 1 d . . . H73A H 0.6474 1.0321 0.1580 0.146 Uiso 1 1 calc R . . H73B H 0.6257 0.9567 0.1692 0.146 Uiso 1 1 calc R . . H73C H 0.6694 0.9667 0.1315 0.146 Uiso 1 1 calc R . . N1 N 0.89761(6) 0.63873(8) 0.46822(5) 0.0211(3) Uani 1 1 d . . . N2 N 0.86035(6) 0.69180(8) 0.46306(5) 0.0194(3) Uani 1 1 d . . . N3 N 0.89015(6) 0.70074(8) 0.53336(5) 0.0185(3) Uani 1 1 d . . . N4 N 0.84669(6) 0.81457(8) 0.39520(5) 0.0201(3) Uani 1 1 d . . . N5 N 0.80823(6) 0.76535(8) 0.40548(5) 0.0195(3) Uani 1 1 d . . . N6 N 0.76730(7) 0.86818(9) 0.40148(5) 0.0254(3) Uani 1 1 d . . . N7 N 0.88804(6) 0.67919(8) 0.35197(5) 0.0197(3) Uani 1 1 d . . . N8 N 0.85267(6) 0.64959(8) 0.38231(5) 0.0196(3) Uani 1 1 d . . . N9 N 0.88227(6) 0.56330(8) 0.33859(6) 0.0231(3) Uani 1 1 d . . . N10 N 1.14792(8) 0.71360(10) 0.46838(6) 0.0334(4) Uani 1 1 d . . . N11 N 0.92030(6) 0.92241(8) 0.15018(5) 0.0186(3) Uani 1 1 d . . . N12 N 0.88093(6) 0.89574(8) 0.12194(5) 0.0175(3) Uani 1 1 d . . . N13 N 0.87523(7) 1.01336(9) 0.12357(6) 0.0255(3) Uani 1 1 d . . . N14 N 0.98643(6) 0.81986(8) 0.15193(5) 0.0197(3) Uani 1 1 d . . . N15 N 0.95829(6) 0.77257(8) 0.12613(5) 0.0200(3) Uani 1 1 d . . . N16 N 1.04528(7) 0.74656(9) 0.12178(6) 0.0276(4) Uani 1 1 d . . . N17 N 0.88624(6) 0.80552(8) 0.21382(5) 0.0194(3) Uani 1 1 d . . . N18 N 0.92991(6) 0.84793(8) 0.22089(5) 0.0190(3) Uani 1 1 d . . . N19 N 0.90068(6) 0.82016(8) 0.28892(5) 0.0191(3) Uani 1 1 d . . . N20 N 0.62733(7) 0.74758(11) 0.18532(7) 0.0340(4) Uani 1 1 d . . . O1 O 0.97285(6) 0.81604(8) 0.37464(5) 0.0291(3) Uani 1 1 d . . . O2 O 1.18963(6) 0.74779(10) 0.46733(6) 0.0450(4) Uani 1 1 d . . . O3 O 1.14374(7) 0.65810(9) 0.48958(6) 0.0451(4) Uani 1 1 d . . . O4 O 0.83228(5) 0.72358(7) 0.11616(4) 0.0227(3) Uani 1 1 d . . . O5 O 0.59402(7) 0.70305(10) 0.17437(7) 0.0465(4) Uani 1 1 d . . . O6 O 0.61615(7) 0.79840(10) 0.20983(7) 0.0442(4) Uani 1 1 d . . . Zn1 Zn 0.906370(8) 0.782264(11) 0.353214(7) 0.01798(5) Uani 1 1 d . . . Zn2 Zn 0.884206(8) 0.793145(11) 0.103216(7) 0.01767(5) 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 B1 0.0195(9) 0.0242(10) 0.0154(9) 0.0005(7) -0.0002(7) 0.0000(8) B2 0.0205(10) 0.0215(9) 0.0143(9) 0.0004(7) -0.0022(7) -0.0015(8) C1 0.0296(10) 0.0227(9) 0.0171(8) 0.0005(7) -0.0015(7) 0.0058(7) C2 0.0202(8) 0.0207(8) 0.0157(8) 0.0018(6) 0.0013(7) -0.0003(7) C3 0.0201(9) 0.0203(8) 0.0166(8) 0.0008(6) 0.0025(6) -0.0005(7) C4 0.0221(9) 0.0261(9) 0.0128(8) -0.0007(7) 0.0017(6) 0.0053(7) C5 0.0267(10) 0.0272(10) 0.0202(9) -0.0042(7) 0.0006(7) 0.0018(8) C6 0.0250(10) 0.0419(12) 0.0236(10) -0.0077(9) -0.0025(8) 0.0056(9) C7 0.0325(11) 0.0382(12) 0.0249(10) -0.0011(8) -0.0025(8) 0.0150(9) C8 0.0383(12) 0.0258(10) 0.0254(10) 0.0018(8) 0.0032(9) 0.0086(9) C9 0.0270(10) 0.0265(9) 0.0193(9) -0.0019(7) 0.0022(7) 0.0033(8) C10 0.0222(10) 0.0396(12) 0.0265(10) 0.0028(9) 0.0019(8) 0.0019(8) C11 0.0245(9) 0.0295(10) 0.0158(8) 0.0006(7) -0.0001(7) 0.0039(8) C12 0.0288(10) 0.0252(9) 0.0134(8) 0.0008(7) 0.0003(7) 0.0032(7) C13 0.0330(10) 0.0238(9) 0.0183(9) -0.0005(7) 0.0045(8) 0.0019(8) C14 0.0366(12) 0.0302(11) 0.0313(11) 0.0026(9) 0.0017(9) 0.0057(9) C15 0.0528(15) 0.0257(11) 0.0393(13) 0.0057(9) 0.0047(11) 0.0076(10) C16 0.0550(15) 0.0254(11) 0.0382(12) 0.0014(9) 0.0093(11) -0.0063(10) C17 0.0393(13) 0.0327(12) 0.0421(13) -0.0045(10) 0.0028(10) -0.0073(10) C18 0.0388(12) 0.0260(10) 0.0323(11) -0.0025(8) 0.0004(9) 0.0005(9) C19 0.0287(10) 0.0258(10) 0.0360(11) 0.0016(8) 0.0026(9) -0.0042(8) C20 0.0226(9) 0.0231(9) 0.0215(9) 0.0001(7) -0.0047(7) -0.0014(7) C21 0.0213(9) 0.0232(9) 0.0177(8) -0.0003(7) -0.0052(7) 0.0030(7) C22 0.0235(9) 0.0250(9) 0.0182(8) 0.0009(7) -0.0015(7) 0.0071(7) C23 0.0336(11) 0.0275(10) 0.0216(9) -0.0012(8) -0.0004(8) 0.0048(8) C24 0.0460(13) 0.0359(11) 0.0197(10) -0.0037(8) 0.0002(9) 0.0129(10) C25 0.0400(12) 0.0389(12) 0.0219(10) 0.0069(9) 0.0086(9) 0.0128(10) C26 0.0275(10) 0.0312(10) 0.0317(11) 0.0080(9) 0.0043(8) 0.0067(8) C27 0.0242(9) 0.0248(9) 0.0245(9) 0.0014(7) 0.0001(7) 0.0074(7) C28 0.0225(9) 0.0282(10) 0.0208(9) -0.0005(7) -0.0022(7) -0.0013(7) C29 0.0289(10) 0.0296(10) 0.0314(11) 0.0067(8) -0.0059(8) -0.0052(8) C30 0.0261(10) 0.0375(12) 0.0334(11) 0.0017(9) -0.0055(9) -0.0069(9) C31 0.0267(10) 0.0332(11) 0.0234(10) -0.0030(8) -0.0053(8) 0.0033(8) C32 0.0351(11) 0.0278(10) 0.0235(10) 0.0021(8) -0.0058(8) -0.0015(8) C33 0.0261(10) 0.0310(10) 0.0240(9) 0.0010(8) -0.0039(8) -0.0056(8) C34 0.0472(14) 0.0225(10) 0.0443(13) -0.0065(9) -0.0196(11) -0.0016(9) C35 0.0298(10) 0.0203(9) 0.0237(9) -0.0030(7) -0.0028(8) -0.0008(7) C36 0.0225(9) 0.0203(8) 0.0165(8) -0.0013(7) 0.0007(7) 0.0016(7) C37 0.0211(9) 0.0252(9) 0.0175(8) -0.0016(7) 0.0007(7) 0.0032(7) C38 0.0307(11) 0.0265(10) 0.0293(10) 0.0010(8) -0.0025(8) 0.0047(8) C39 0.0376(12) 0.0374(12) 0.0308(11) 0.0063(9) -0.0059(9) 0.0114(10) C40 0.0292(11) 0.0520(14) 0.0276(11) -0.0022(10) -0.0080(9) 0.0088(10) C41 0.0245(10) 0.0406(12) 0.0296(11) -0.0054(9) -0.0046(8) -0.0010(9) C42 0.0245(10) 0.0283(10) 0.0219(9) -0.0013(8) 0.0010(7) 0.0008(8) C43 0.0215(10) 0.0429(12) 0.0363(12) 0.0052(10) -0.0022(8) 0.0020(9) C44 0.0233(9) 0.0299(10) 0.0221(9) 0.0068(7) 0.0009(7) 0.0033(8) C45 0.0315(10) 0.0235(9) 0.0179(9) 0.0046(7) 0.0044(7) 0.0077(8) C46 0.0408(12) 0.0242(10) 0.0215(9) 0.0003(8) 0.0010(8) 0.0129(8) C47 0.0632(16) 0.0309(11) 0.0300(11) 0.0039(9) 0.0148(11) 0.0149(11) C48 0.100(2) 0.0379(14) 0.0267(12) -0.0021(10) 0.0142(14) 0.0242(15) C49 0.097(2) 0.0327(13) 0.0331(13) -0.0124(10) -0.0105(14) 0.0162(14) C50 0.0597(16) 0.0310(12) 0.0420(14) -0.0080(10) -0.0099(12) 0.0075(11) C51 0.0428(12) 0.0250(10) 0.0292(11) -0.0049(8) -0.0032(9) 0.0098(9) C52 0.0379(12) 0.0380(11) 0.0192(9) 0.0003(8) -0.0029(8) -0.0168(9) C53 0.0240(9) 0.0208(8) 0.0165(8) -0.0006(7) 0.0000(7) -0.0013(7) C54 0.0184(8) 0.0182(8) 0.0174(8) -0.0019(6) -0.0004(6) 0.0031(6) C55 0.0225(9) 0.0232(9) 0.0151(8) 0.0044(7) -0.0042(7) -0.0004(7) C56 0.0229(10) 0.0434(12) 0.0200(9) -0.0041(8) -0.0006(7) -0.0020(8) C57 0.0254(11) 0.0772(18) 0.0241(11) -0.0015(11) 0.0038(8) -0.0098(11) C58 0.0370(13) 0.0585(16) 0.0328(12) 0.0126(11) -0.0041(10) -0.0239(12) C59 0.0441(13) 0.0284(11) 0.0384(12) 0.0079(9) -0.0115(10) -0.0112(10) C60 0.0318(11) 0.0238(9) 0.0273(10) 0.0020(8) -0.0038(8) -0.0001(8) C61 0.0259(9) 0.0229(9) 0.0140(8) 0.0019(7) -0.0001(7) -0.0029(7) C62 0.0307(10) 0.0231(9) 0.0211(9) -0.0032(7) 0.0013(8) -0.0056(8) C63 0.0299(10) 0.0284(10) 0.0249(10) -0.0011(8) -0.0007(8) -0.0102(8) C64 0.0224(9) 0.0312(10) 0.0250(10) 0.0010(8) 0.0014(8) -0.0035(8) C65 0.0271(10) 0.0241(9) 0.0212(9) -0.0026(7) 0.0001(7) -0.0026(8) C66 0.0232(9) 0.0206(8) 0.0189(8) -0.0006(7) -0.0012(7) -0.0045(7) C67 0.0657(18) 0.0370(13) 0.0370(13) -0.0045(10) 0.0113(12) 0.0151(12) C68 0.072(2) 0.0465(16) 0.0542(17) -0.0044(13) 0.0163(15) 0.0178(14) C69 0.079(2) 0.0585(18) 0.0483(17) -0.0019(14) 0.0046(16) 0.0225(16) C70 0.076(2) 0.0443(15) 0.0570(18) 0.0014(13) 0.0234(16) 0.0165(15) C71 0.075(2) 0.0313(13) 0.068(2) -0.0058(13) 0.0255(17) 0.0079(13) C72 0.067(2) 0.0382(14) 0.071(2) -0.0167(14) -0.0008(16) 0.0137(13) C73 0.100(3) 0.089(3) 0.104(3) -0.035(3) -0.032(3) 0.025(3) N1 0.0232(8) 0.0226(8) 0.0174(7) 0.0014(6) 0.0005(6) 0.0046(6) N2 0.0216(8) 0.0205(7) 0.0159(7) 0.0008(6) 0.0013(6) 0.0025(6) N3 0.0202(7) 0.0192(7) 0.0159(7) 0.0018(6) 0.0008(6) 0.0012(6) N4 0.0237(8) 0.0224(7) 0.0142(7) 0.0007(6) 0.0011(6) 0.0010(6) N5 0.0192(7) 0.0241(8) 0.0153(7) 0.0009(6) -0.0001(6) -0.0004(6) N6 0.0278(9) 0.0282(8) 0.0203(8) 0.0005(6) 0.0020(6) 0.0049(7) N7 0.0203(7) 0.0238(8) 0.0151(7) 0.0013(6) -0.0013(6) 0.0009(6) N8 0.0209(7) 0.0223(8) 0.0156(7) 0.0008(6) -0.0019(6) -0.0009(6) N9 0.0244(8) 0.0229(8) 0.0221(8) -0.0011(6) -0.0039(6) -0.0002(6) N10 0.0349(10) 0.0371(10) 0.0283(9) -0.0067(8) -0.0096(8) 0.0062(8) N11 0.0217(7) 0.0190(7) 0.0150(7) -0.0025(6) -0.0017(6) -0.0014(6) N12 0.0186(7) 0.0201(7) 0.0138(7) -0.0014(6) -0.0003(5) -0.0010(6) N13 0.0314(9) 0.0200(8) 0.0252(8) -0.0029(6) -0.0045(7) 0.0014(7) N14 0.0206(7) 0.0231(7) 0.0155(7) 0.0024(6) 0.0003(6) 0.0004(6) N15 0.0235(8) 0.0215(7) 0.0150(7) 0.0004(6) 0.0014(6) 0.0023(6) N16 0.0268(9) 0.0311(9) 0.0251(8) 0.0063(7) 0.0035(7) 0.0080(7) N17 0.0187(7) 0.0220(7) 0.0175(7) -0.0002(6) -0.0003(6) -0.0020(6) N18 0.0203(7) 0.0212(7) 0.0156(7) -0.0006(6) -0.0011(6) -0.0022(6) N19 0.0217(7) 0.0198(7) 0.0158(7) -0.0012(6) -0.0008(6) -0.0008(6) N20 0.0277(9) 0.0392(10) 0.0352(10) -0.0037(8) 0.0044(8) -0.0049(8) O1 0.0241(7) 0.0297(7) 0.0336(8) 0.0033(6) -0.0084(6) -0.0031(6) O2 0.0288(8) 0.0621(11) 0.0440(10) -0.0021(9) -0.0122(7) 0.0011(8) O3 0.0556(11) 0.0330(9) 0.0466(10) 0.0007(8) -0.0219(9) 0.0087(8) O4 0.0259(7) 0.0216(6) 0.0206(6) -0.0025(5) 0.0051(5) -0.0046(5) O5 0.0299(9) 0.0483(10) 0.0612(12) -0.0081(9) 0.0078(8) -0.0137(8) O6 0.0320(9) 0.0499(10) 0.0506(11) -0.0154(8) 0.0126(8) -0.0038(8) Zn1 0.01896(10) 0.02075(10) 0.01422(10) 0.00051(7) -0.00069(8) 0.00025(8) Zn2 0.02015(11) 0.01787(10) 0.01500(10) -0.00083(7) 0.00119(8) -0.00080(8) _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 B1 N8 1.543(3) . ? B1 N5 1.546(3) . ? B1 N2 1.563(2) . ? B1 H1 0.9800 . ? B2 N14 1.541(3) . ? B2 N18 1.545(2) . ? B2 N11 1.549(2) . ? B2 H2 0.9800 . ? C1 C2 1.489(2) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 N2 1.339(2) . ? C2 N3 1.347(2) . ? C3 N1 1.315(2) . ? C3 N3 1.376(2) . ? C3 C4 1.483(2) . ? C4 C9 1.387(3) . ? C4 C5 1.391(3) . ? C5 C6 1.392(3) . ? C5 H5 0.9300 . ? C6 C7 1.374(3) . ? C6 H6 0.9300 . ? C7 C8 1.381(3) . ? C7 H7 0.9300 . ? C8 C9 1.390(3) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.491(3) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N6 1.332(3) . ? C11 N5 1.346(2) . ? C12 N4 1.338(2) . ? C12 N6 1.351(3) . ? C12 C13 1.469(3) . ? C13 C14 1.393(3) . ? C13 C18 1.396(3) . ? C14 C15 1.384(3) . ? C14 H14 0.9300 . ? C15 C16 1.375(4) . ? C15 H15 0.9300 . ? C16 C17 1.385(3) . ? C16 H16 0.9300 . ? C17 C18 1.391(3) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.484(3) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N9 1.335(3) . ? C20 N8 1.342(2) . ? C21 N7 1.335(2) . ? C21 N9 1.348(2) . ? C21 C22 1.474(3) . ? C22 C27 1.388(3) . ? C22 C23 1.400(3) . ? C23 C24 1.388(3) . ? C23 H23 0.9300 . ? C24 C25 1.385(3) . ? C24 H24 0.9300 . ? C25 C26 1.383(3) . ? C25 H25 0.9300 . ? C26 C27 1.387(3) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 O1 1.309(2) . ? C28 C33 1.404(3) . ? C28 C29 1.415(3) . ? C29 C30 1.374(3) . ? C29 H29 0.9300 . ? C30 C31 1.392(3) . ? C30 H30 0.9300 . ? C31 C32 1.379(3) . ? C31 N10 1.447(3) . ? C32 C33 1.380(3) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.488(3) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 N13 1.327(3) . ? C35 N11 1.344(2) . ? C36 N12 1.336(2) . ? C36 N13 1.353(2) . ? C36 C37 1.478(3) . ? C37 C42 1.391(3) . ? C37 C38 1.400(3) . ? C38 C39 1.384(3) . ? C38 H38 0.9300 . ? C39 C40 1.380(3) . ? C39 H39 0.9300 . ? C40 C41 1.385(3) . ? C40 H40 0.9300 . ? C41 C42 1.391(3) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.489(3) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 N16 1.335(3) . ? C44 N14 1.349(2) . ? C45 N15 1.332(2) . ? C45 N16 1.348(3) . ? C45 C46 1.477(3) . ? C46 C51 1.385(3) . ? C46 C47 1.400(3) . ? C47 C48 1.389(4) . ? C47 H47 0.9300 . ? C48 C49 1.376(5) . ? C48 H48 0.9300 . ? C49 C50 1.384(4) . ? C49 H49 0.9300 . ? C50 C51 1.391(3) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 C53 1.490(3) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 N18 1.338(2) . ? C53 N19 1.345(2) . ? C54 N17 1.315(2) . ? C54 N19 1.376(2) . ? C54 C55 1.470(3) . ? C55 C56 1.388(3) . ? C55 C60 1.393(3) . ? C56 C57 1.393(3) . ? C56 H56 0.9300 . ? C57 C58 1.376(4) . ? C57 H57 0.9300 . ? C58 C59 1.382(4) . ? C58 H58 0.9300 . ? C59 C60 1.384(3) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C61 O4 1.316(2) . ? C61 C66 1.405(3) . ? C61 C62 1.417(3) . ? C62 C63 1.375(3) . ? C62 H62 0.9300 . ? C63 C64 1.396(3) . ? C63 H63 0.9300 . ? C64 C65 1.388(3) . ? C64 N20 1.444(3) . ? C65 C66 1.377(3) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 C72 1.376(4) . ? C67 C68 1.405(4) . ? C67 H67 0.9300 . ? C68 C69 1.352(4) . ? C68 H68 0.9300 . ? C69 C70 1.379(5) . ? C69 H69 0.9300 . ? C70 C71 1.359(5) . ? C70 H70 0.9300 . ? C71 C72 1.422(5) . ? C71 H71 0.9300 . ? C72 C73 1.471(5) . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? N1 N2 1.384(2) . ? N3 Zn2 2.0544(15) 7_576 ? N4 N5 1.377(2) . ? N4 Zn1 2.0319(15) . ? N7 N8 1.376(2) . ? N7 Zn1 2.0134(16) . ? N10 O3 1.229(3) . ? N10 O2 1.232(3) . ? N11 N12 1.384(2) . ? N12 Zn2 2.0281(15) . ? N14 N15 1.370(2) . ? N15 Zn2 2.0136(16) . ? N17 N18 1.376(2) . ? N19 Zn1 2.0207(15) . ? N20 O5 1.232(2) . ? N20 O6 1.236(2) . ? O1 Zn1 1.8934(14) . ? O4 Zn2 1.8945(13) . ? Zn2 N3 2.0543(15) 7_575 ? 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 N8 B1 N5 111.85(15) . . ? N8 B1 N2 107.49(15) . . ? N5 B1 N2 110.28(15) . . ? N8 B1 H1 109.1 . . ? N5 B1 H1 109.1 . . ? N2 B1 H1 109.1 . . ? N14 B2 N18 109.76(15) . . ? N14 B2 N11 111.89(14) . . ? N18 B2 N11 109.08(15) . . ? N14 B2 H2 108.7 . . ? N18 B2 H2 108.7 . . ? N11 B2 H2 108.7 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 N3 109.76(16) . . ? N2 C2 C1 125.08(16) . . ? N3 C2 C1 125.15(16) . . ? N1 C3 N3 113.44(16) . . ? N1 C3 C4 123.39(16) . . ? N3 C3 C4 123.12(16) . . ? C9 C4 C5 119.60(18) . . ? C9 C4 C3 120.99(17) . . ? C5 C4 C3 119.41(17) . . ? C4 C5 C6 120.49(19) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C7 C6 C5 119.5(2) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C8 120.32(19) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C9 120.6(2) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C4 C9 C8 119.37(19) . . ? C4 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N6 C11 N5 111.31(17) . . ? N6 C11 C10 123.71(18) . . ? N5 C11 C10 124.97(18) . . ? N4 C12 N6 113.11(17) . . ? N4 C12 C13 123.37(18) . . ? N6 C12 C13 123.42(17) . . ? C14 C13 C18 119.0(2) . . ? C14 C13 C12 119.26(19) . . ? C18 C13 C12 121.59(18) . . ? C15 C14 C13 120.3(2) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 120.6(2) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 119.9(2) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C18 120.1(2) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 120.1(2) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N9 C20 N8 111.22(17) . . ? N9 C20 C19 124.68(18) . . ? N8 C20 C19 123.97(18) . . ? N7 C21 N9 113.37(17) . . ? N7 C21 C22 124.23(17) . . ? N9 C21 C22 122.32(17) . . ? C27 C22 C23 119.42(18) . . ? C27 C22 C21 122.85(17) . . ? C23 C22 C21 117.72(18) . . ? C24 C23 C22 120.0(2) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 120.1(2) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C24 120.1(2) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C27 120.1(2) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C22 120.28(19) . . ? C26 C27 H27 119.9 . . ? C22 C27 H27 119.9 . . ? O1 C28 C33 123.30(18) . . ? O1 C28 C29 118.54(18) . . ? C33 C28 C29 118.16(18) . . ? C30 C29 C28 121.43(19) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C29 C30 C31 118.5(2) . . ? C29 C30 H30 120.7 . . ? C31 C30 H30 120.7 . . ? C32 C31 C30 121.62(19) . . ? C32 C31 N10 118.88(19) . . ? C30 C31 N10 119.50(19) . . ? C31 C32 C33 119.82(19) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C32 C33 C28 120.45(19) . . ? C32 C33 H33 119.8 . . ? C28 C33 H33 119.8 . . ? C35 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C35 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N13 C35 N11 111.50(17) . . ? N13 C35 C34 124.03(18) . . ? N11 C35 C34 124.46(18) . . ? N12 C36 N13 112.94(16) . . ? N12 C36 C37 126.38(16) . . ? N13 C36 C37 120.59(16) . . ? C42 C37 C38 119.07(18) . . ? C42 C37 C36 123.94(17) . . ? C38 C37 C36 116.99(17) . . ? C39 C38 C37 120.7(2) . . ? C39 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C40 C39 C38 119.8(2) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C39 C40 C41 120.2(2) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C40 C41 C42 120.4(2) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C41 C42 C37 119.87(19) . . ? C41 C42 H42 120.1 . . ? C37 C42 H42 120.1 . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N16 C44 N14 111.14(18) . . ? N16 C44 C43 124.44(18) . . ? N14 C44 C43 124.42(19) . . ? N15 C45 N16 113.44(18) . . ? N15 C45 C46 121.20(19) . . ? N16 C45 C46 125.34(18) . . ? C51 C46 C47 119.8(2) . . ? C51 C46 C45 120.28(18) . . ? C47 C46 C45 119.8(2) . . ? C48 C47 C46 119.2(3) . . ? C48 C47 H47 120.4 . . ? C46 C47 H47 120.4 . . ? C49 C48 C47 120.6(2) . . ? C49 C48 H48 119.7 . . ? C47 C48 H48 119.7 . . ? C48 C49 C50 120.5(2) . . ? C48 C49 H49 119.7 . . ? C50 C49 H49 119.7 . . ? C49 C50 C51 119.4(3) . . ? C49 C50 H50 120.3 . . ? C51 C50 H50 120.3 . . ? C46 C51 C50 120.4(2) . . ? C46 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C53 C52 H52A 109.5 . . ? C53 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C53 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N18 C53 N19 109.26(16) . . ? N18 C53 C52 124.91(17) . . ? N19 C53 C52 125.83(16) . . ? N17 C54 N19 113.13(16) . . ? N17 C54 C55 122.49(16) . . ? N19 C54 C55 124.31(16) . . ? C56 C55 C60 119.55(18) . . ? C56 C55 C54 120.35(17) . . ? C60 C55 C54 119.95(17) . . ? C55 C56 C57 120.0(2) . . ? C55 C56 H56 120.0 . . ? C57 C56 H56 120.0 . . ? C58 C57 C56 120.0(2) . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C57 C58 C59 120.3(2) . . ? C57 C58 H58 119.9 . . ? C59 C58 H58 119.9 . . ? C58 C59 C60 120.1(2) . . ? C58 C59 H59 119.9 . . ? C60 C59 H59 119.9 . . ? C59 C60 C55 120.0(2) . . ? C59 C60 H60 120.0 . . ? C55 C60 H60 120.0 . . ? O4 C61 C66 122.83(17) . . ? O4 C61 C62 119.13(17) . . ? C66 C61 C62 118.04(18) . . ? C63 C62 C61 121.09(18) . . ? C63 C62 H62 119.5 . . ? C61 C62 H62 119.5 . . ? C62 C63 C64 119.03(18) . . ? C62 C63 H63 120.5 . . ? C64 C63 H63 120.5 . . ? C65 C64 C63 121.36(18) . . ? C65 C64 N20 118.84(18) . . ? C63 C64 N20 119.80(18) . . ? C66 C65 C64 119.29(18) . . ? C66 C65 H65 120.4 . . ? C64 C65 H65 120.4 . . ? C65 C66 C61 121.17(17) . . ? C65 C66 H66 119.4 . . ? C61 C66 H66 119.4 . . ? C72 C67 C68 120.4(3) . . ? C72 C67 H67 119.8 . . ? C68 C67 H67 119.8 . . ? C69 C68 C67 121.0(3) . . ? C69 C68 H68 119.5 . . ? C67 C68 H68 119.5 . . ? C68 C69 C70 118.5(3) . . ? C68 C69 H69 120.7 . . ? C70 C69 H69 120.7 . . ? C71 C70 C69 122.8(3) . . ? C71 C70 H70 118.6 . . ? C69 C70 H70 118.6 . . ? C70 C71 C72 119.0(3) . . ? C70 C71 H71 120.5 . . ? C72 C71 H71 120.5 . . ? C67 C72 C71 118.4(3) . . ? C67 C72 C73 120.3(3) . . ? C71 C72 C73 121.3(4) . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C3 N1 N2 103.89(15) . . ? C2 N2 N1 109.23(15) . . ? C2 N2 B1 130.78(16) . . ? N1 N2 B1 118.34(14) . . ? C2 N3 C3 103.66(15) . . ? C2 N3 Zn2 127.44(12) . 7_576 ? C3 N3 Zn2 124.08(12) . 7_576 ? C12 N4 N5 104.32(15) . . ? C12 N4 Zn1 127.61(13) . . ? N5 N4 Zn1 116.27(11) . . ? C11 N5 N4 107.45(15) . . ? C11 N5 B1 129.52(16) . . ? N4 N5 B1 121.70(15) . . ? C11 N6 C12 103.79(16) . . ? C21 N7 N8 104.17(15) . . ? C21 N7 Zn1 133.57(13) . . ? N8 N7 Zn1 122.26(12) . . ? C20 N8 N7 107.59(15) . . ? C20 N8 B1 127.26(16) . . ? N7 N8 B1 125.08(15) . . ? C20 N9 C21 103.60(16) . . ? O3 N10 O2 122.56(19) . . ? O3 N10 C31 118.92(19) . . ? O2 N10 C31 118.52(19) . . ? C35 N11 N12 107.19(15) . . ? C35 N11 B2 126.07(15) . . ? N12 N11 B2 126.57(14) . . ? C36 N12 N11 104.31(14) . . ? C36 N12 Zn2 134.97(12) . . ? N11 N12 Zn2 119.01(11) . . ? C35 N13 C36 104.04(16) . . ? C44 N14 N15 107.38(15) . . ? C44 N14 B2 129.31(16) . . ? N15 N14 B2 123.30(15) . . ? C45 N15 N14 104.52(15) . . ? C45 N15 Zn2 129.39(13) . . ? N14 N15 Zn2 122.09(12) . . ? C44 N16 C45 103.52(16) . . ? C54 N17 N18 103.92(14) . . ? C53 N18 N17 109.72(15) . . ? C53 N18 B2 130.48(15) . . ? N17 N18 B2 119.78(14) . . ? C53 N19 C54 103.97(15) . . ? C53 N19 Zn1 127.00(12) . . ? C54 N19 Zn1 123.94(12) . . ? O5 N20 O6 122.33(19) . . ? O5 N20 C64 118.57(19) . . ? O6 N20 C64 119.09(18) . . ? C28 O1 Zn1 136.32(13) . . ? C61 O4 Zn2 129.80(12) . . ? O1 Zn1 N7 122.49(6) . . ? O1 Zn1 N19 104.47(6) . . ? N7 Zn1 N19 108.31(6) . . ? O1 Zn1 N4 110.21(7) . . ? N7 Zn1 N4 97.88(6) . . ? N19 Zn1 N4 113.82(6) . . ? O4 Zn2 N15 115.58(6) . . ? O4 Zn2 N12 126.13(6) . . ? N15 Zn2 N12 97.72(6) . . ? O4 Zn2 N3 106.78(6) . 7_575 ? N15 Zn2 N3 106.01(6) . 7_575 ? N12 Zn2 N3 102.57(6) . 7_575 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C3 C4 C9 -67.0(2) . . . . ? N3 C3 C4 C9 115.7(2) . . . . ? N1 C3 C4 C5 112.8(2) . . . . ? N3 C3 C4 C5 -64.5(2) . . . . ? C9 C4 C5 C6 -1.2(3) . . . . ? C3 C4 C5 C6 179.01(17) . . . . ? C4 C5 C6 C7 -1.6(3) . . . . ? C5 C6 C7 C8 2.1(3) . . . . ? C6 C7 C8 C9 0.0(3) . . . . ? C5 C4 C9 C8 3.3(3) . . . . ? C3 C4 C9 C8 -176.88(17) . . . . ? C7 C8 C9 C4 -2.8(3) . . . . ? N4 C12 C13 C14 161.62(18) . . . . ? N6 C12 C13 C14 -22.1(3) . . . . ? N4 C12 C13 C18 -22.2(3) . . . . ? N6 C12 C13 C18 154.10(19) . . . . ? C18 C13 C14 C15 -1.7(3) . . . . ? C12 C13 C14 C15 174.50(19) . . . . ? C13 C14 C15 C16 0.2(4) . . . . ? C14 C15 C16 C17 1.7(4) . . . . ? C15 C16 C17 C18 -2.0(4) . . . . ? C16 C17 C18 C13 0.5(3) . . . . ? C14 C13 C18 C17 1.4(3) . . . . ? C12 C13 C18 C17 -174.8(2) . . . . ? N7 C21 C22 C27 33.1(3) . . . . ? N9 C21 C22 C27 -150.20(18) . . . . ? N7 C21 C22 C23 -148.18(18) . . . . ? N9 C21 C22 C23 28.5(3) . . . . ? C27 C22 C23 C24 -0.9(3) . . . . ? C21 C22 C23 C24 -179.62(18) . . . . ? C22 C23 C24 C25 0.2(3) . . . . ? C23 C24 C25 C26 0.2(3) . . . . ? C24 C25 C26 C27 0.1(3) . . . . ? C25 C26 C27 C22 -0.8(3) . . . . ? C23 C22 C27 C26 1.2(3) . . . . ? C21 C22 C27 C26 179.89(18) . . . . ? O1 C28 C29 C30 -179.1(2) . . . . ? C33 C28 C29 C30 1.3(3) . . . . ? C28 C29 C30 C31 -1.1(3) . . . . ? C29 C30 C31 C32 0.4(3) . . . . ? C29 C30 C31 N10 -179.3(2) . . . . ? C30 C31 C32 C33 0.2(3) . . . . ? N10 C31 C32 C33 179.89(19) . . . . ? C31 C32 C33 C28 -0.1(3) . . . . ? O1 C28 C33 C32 179.75(19) . . . . ? C29 C28 C33 C32 -0.7(3) . . . . ? N12 C36 C37 C42 20.5(3) . . . . ? N13 C36 C37 C42 -163.17(18) . . . . ? N12 C36 C37 C38 -159.05(18) . . . . ? N13 C36 C37 C38 17.3(3) . . . . ? C42 C37 C38 C39 -0.4(3) . . . . ? C36 C37 C38 C39 179.16(19) . . . . ? C37 C38 C39 C40 0.5(3) . . . . ? C38 C39 C40 C41 -0.6(3) . . . . ? C39 C40 C41 C42 0.6(3) . . . . ? C40 C41 C42 C37 -0.5(3) . . . . ? C38 C37 C42 C41 0.4(3) . . . . ? C36 C37 C42 C41 -179.16(18) . . . . ? N15 C45 C46 C51 -39.2(3) . . . . ? N16 C45 C46 C51 142.6(2) . . . . ? N15 C45 C46 C47 138.1(2) . . . . ? N16 C45 C46 C47 -40.2(3) . . . . ? C51 C46 C47 C48 1.1(3) . . . . ? C45 C46 C47 C48 -176.2(2) . . . . ? C46 C47 C48 C49 -1.2(4) . . . . ? C47 C48 C49 C50 0.4(4) . . . . ? C48 C49 C50 C51 0.4(4) . . . . ? C47 C46 C51 C50 -0.2(3) . . . . ? C45 C46 C51 C50 177.0(2) . . . . ? C49 C50 C51 C46 -0.5(3) . . . . ? N17 C54 C55 C56 -127.6(2) . . . . ? N19 C54 C55 C56 49.1(3) . . . . ? N17 C54 C55 C60 48.0(3) . . . . ? N19 C54 C55 C60 -135.34(19) . . . . ? C60 C55 C56 C57 -1.1(3) . . . . ? C54 C55 C56 C57 174.55(19) . . . . ? C55 C56 C57 C58 1.7(4) . . . . ? C56 C57 C58 C59 -0.5(4) . . . . ? C57 C58 C59 C60 -1.5(4) . . . . ? C58 C59 C60 C55 2.1(3) . . . . ? C56 C55 C60 C59 -0.8(3) . . . . ? C54 C55 C60 C59 -176.48(18) . . . . ? O4 C61 C62 C63 -179.23(18) . . . . ? C66 C61 C62 C63 1.6(3) . . . . ? C61 C62 C63 C64 -1.2(3) . . . . ? C62 C63 C64 C65 -0.4(3) . . . . ? C62 C63 C64 N20 178.98(19) . . . . ? C63 C64 C65 C66 1.4(3) . . . . ? N20 C64 C65 C66 -177.99(18) . . . . ? C64 C65 C66 C61 -0.8(3) . . . . ? O4 C61 C66 C65 -179.71(17) . . . . ? C62 C61 C66 C65 -0.6(3) . . . . ? C72 C67 C68 C69 -0.2(4) . . . . ? C67 C68 C69 C70 -0.3(5) . . . . ? C68 C69 C70 C71 0.8(5) . . . . ? C69 C70 C71 C72 -0.8(4) . . . . ? C68 C67 C72 C71 0.2(4) . . . . ? C68 C67 C72 C73 -179.0(3) . . . . ? C70 C71 C72 C67 0.3(4) . . . . ? C70 C71 C72 C73 179.5(3) . . . . ? N3 C3 N1 N2 0.7(2) . . . . ? C4 C3 N1 N2 -176.84(16) . . . . ? N3 C2 N2 N1 0.2(2) . . . . ? C1 C2 N2 N1 179.49(17) . . . . ? N3 C2 N2 B1 165.01(17) . . . . ? C1 C2 N2 B1 -15.7(3) . . . . ? C3 N1 N2 C2 -0.58(19) . . . . ? C3 N1 N2 B1 -167.53(15) . . . . ? N8 B1 N2 C2 169.81(17) . . . . ? N5 B1 N2 C2 47.6(3) . . . . ? N8 B1 N2 N1 -26.5(2) . . . . ? N5 B1 N2 N1 -148.72(15) . . . . ? N2 C2 N3 C3 0.20(19) . . . . ? C1 C2 N3 C3 -179.06(17) . . . . ? N2 C2 N3 Zn2 -155.65(12) . . . 7_576 ? C1 C2 N3 Zn2 25.1(3) . . . 7_576 ? N1 C3 N3 C2 -0.6(2) . . . . ? C4 C3 N3 C2 176.97(17) . . . . ? N1 C3 N3 Zn2 156.31(13) . . . 7_576 ? C4 C3 N3 Zn2 -26.1(2) . . . 7_576 ? N6 C12 N4 N5 -1.4(2) . . . . ? C13 C12 N4 N5 175.23(16) . . . . ? N6 C12 N4 Zn1 139.21(14) . . . . ? C13 C12 N4 Zn1 -44.1(2) . . . . ? N6 C11 N5 N4 -0.3(2) . . . . ? C10 C11 N5 N4 -179.30(17) . . . . ? N6 C11 N5 B1 166.40(17) . . . . ? C10 C11 N5 B1 -12.6(3) . . . . ? C12 N4 N5 C11 1.02(18) . . . . ? Zn1 N4 N5 C11 -144.92(12) . . . . ? C12 N4 N5 B1 -166.94(15) . . . . ? Zn1 N4 N5 B1 47.12(19) . . . . ? N8 B1 N5 C11 131.62(19) . . . . ? N2 B1 N5 C11 -108.8(2) . . . . ? N8 B1 N5 N4 -63.3(2) . . . . ? N2 B1 N5 N4 56.2(2) . . . . ? N5 C11 N6 C12 -0.5(2) . . . . ? C10 C11 N6 C12 178.47(18) . . . . ? N4 C12 N6 C11 1.3(2) . . . . ? C13 C12 N6 C11 -175.41(17) . . . . ? N9 C21 N7 N8 -1.4(2) . . . . ? C22 C21 N7 N8 175.54(16) . . . . ? N9 C21 N7 Zn1 177.72(13) . . . . ? C22 C21 N7 Zn1 -5.3(3) . . . . ? N9 C20 N8 N7 -2.3(2) . . . . ? C19 C20 N8 N7 173.59(17) . . . . ? N9 C20 N8 B1 -179.27(16) . . . . ? C19 C20 N8 B1 -3.4(3) . . . . ? C21 N7 N8 C20 2.18(18) . . . . ? Zn1 N7 N8 C20 -177.07(12) . . . . ? C21 N7 N8 B1 179.22(16) . . . . ? Zn1 N7 N8 B1 0.0(2) . . . . ? N5 B1 N8 C20 -148.48(17) . . . . ? N2 B1 N8 C20 90.3(2) . . . . ? N5 B1 N8 N7 35.1(2) . . . . ? N2 B1 N8 N7 -86.13(19) . . . . ? N8 C20 N9 C21 1.4(2) . . . . ? C19 C20 N9 C21 -174.46(18) . . . . ? N7 C21 N9 C20 0.1(2) . . . . ? C22 C21 N9 C20 -176.95(17) . . . . ? C32 C31 N10 O3 -4.9(3) . . . . ? C30 C31 N10 O3 174.8(2) . . . . ? C32 C31 N10 O2 175.4(2) . . . . ? C30 C31 N10 O2 -4.8(3) . . . . ? N13 C35 N11 N12 0.0(2) . . . . ? C34 C35 N11 N12 -178.8(2) . . . . ? N13 C35 N11 B2 -175.56(17) . . . . ? C34 C35 N11 B2 5.7(3) . . . . ? N14 B2 N11 C35 -137.15(18) . . . . ? N18 B2 N11 C35 101.2(2) . . . . ? N14 B2 N11 N12 48.2(2) . . . . ? N18 B2 N11 N12 -73.5(2) . . . . ? N13 C36 N12 N11 -1.3(2) . . . . ? C37 C36 N12 N11 175.29(17) . . . . ? N13 C36 N12 Zn2 -165.46(13) . . . . ? C37 C36 N12 Zn2 11.1(3) . . . . ? C35 N11 N12 C36 0.76(19) . . . . ? B2 N11 N12 C36 176.27(16) . . . . ? C35 N11 N12 Zn2 168.03(12) . . . . ? B2 N11 N12 Zn2 -16.5(2) . . . . ? N11 C35 N13 C36 -0.7(2) . . . . ? C34 C35 N13 C36 178.1(2) . . . . ? N12 C36 N13 C35 1.3(2) . . . . ? C37 C36 N13 C35 -175.53(17) . . . . ? N16 C44 N14 N15 0.4(2) . . . . ? C43 C44 N14 N15 -179.15(18) . . . . ? N16 C44 N14 B2 178.84(17) . . . . ? C43 C44 N14 B2 -0.7(3) . . . . ? N18 B2 N14 C44 -107.4(2) . . . . ? N11 B2 N14 C44 131.32(19) . . . . ? N18 B2 N14 N15 70.8(2) . . . . ? N11 B2 N14 N15 -50.4(2) . . . . ? N16 C45 N15 N14 -0.2(2) . . . . ? C46 C45 N15 N14 -178.61(16) . . . . ? N16 C45 N15 Zn2 157.16(13) . . . . ? C46 C45 N15 Zn2 -21.3(3) . . . . ? C44 N14 N15 C45 -0.10(19) . . . . ? B2 N14 N15 C45 -178.70(16) . . . . ? C44 N14 N15 Zn2 -159.53(12) . . . . ? B2 N14 N15 Zn2 21.9(2) . . . . ? N14 C44 N16 C45 -0.4(2) . . . . ? C43 C44 N16 C45 179.05(19) . . . . ? N15 C45 N16 C44 0.4(2) . . . . ? C46 C45 N16 C44 178.74(18) . . . . ? N19 C54 N17 N18 -0.16(19) . . . . ? C55 C54 N17 N18 176.88(16) . . . . ? N19 C53 N18 N17 -0.4(2) . . . . ? C52 C53 N18 N17 179.27(18) . . . . ? N19 C53 N18 B2 177.92(17) . . . . ? C52 C53 N18 B2 -2.4(3) . . . . ? C54 N17 N18 C53 0.32(19) . . . . ? C54 N17 N18 B2 -178.18(15) . . . . ? N14 B2 N18 C53 116.0(2) . . . . ? N11 B2 N18 C53 -121.1(2) . . . . ? N14 B2 N18 N17 -65.9(2) . . . . ? N11 B2 N18 N17 57.0(2) . . . . ? N18 C53 N19 C54 0.3(2) . . . . ? C52 C53 N19 C54 -179.38(19) . . . . ? N18 C53 N19 Zn1 155.46(13) . . . . ? C52 C53 N19 Zn1 -24.2(3) . . . . ? N17 C54 N19 C53 -0.1(2) . . . . ? C55 C54 N19 C53 -177.04(17) . . . . ? N17 C54 N19 Zn1 -156.25(12) . . . . ? C55 C54 N19 Zn1 26.8(2) . . . . ? C65 C64 N20 O5 174.2(2) . . . . ? C63 C64 N20 O5 -5.2(3) . . . . ? C65 C64 N20 O6 -4.5(3) . . . . ? C63 C64 N20 O6 176.1(2) . . . . ? C33 C28 O1 Zn1 -10.9(3) . . . . ? C29 C28 O1 Zn1 169.46(15) . . . . ? C66 C61 O4 Zn2 -22.1(3) . . . . ? C62 C61 O4 Zn2 158.79(14) . . . . ? C28 O1 Zn1 N7 -12.5(2) . . . . ? C28 O1 Zn1 N19 -135.77(19) . . . . ? C28 O1 Zn1 N4 101.6(2) . . . . ? C21 N7 Zn1 O1 -72.22(18) . . . . ? N8 N7 Zn1 O1 106.78(13) . . . . ? C21 N7 Zn1 N19 49.30(18) . . . . ? N8 N7 Zn1 N19 -131.71(13) . . . . ? C21 N7 Zn1 N4 167.67(17) . . . . ? N8 N7 Zn1 N4 -13.34(14) . . . . ? C53 N19 Zn1 O1 5.22(17) . . . . ? C54 N19 Zn1 O1 155.85(14) . . . . ? C53 N19 Zn1 N7 -126.82(15) . . . . ? C54 N19 Zn1 N7 23.80(15) . . . . ? C53 N19 Zn1 N4 125.49(15) . . . . ? C54 N19 Zn1 N4 -83.89(15) . . . . ? C12 N4 Zn1 O1 85.61(17) . . . . ? N5 N4 Zn1 O1 -137.63(12) . . . . ? C12 N4 Zn1 N7 -145.42(16) . . . . ? N5 N4 Zn1 N7 -8.67(13) . . . . ? C12 N4 Zn1 N19 -31.36(18) . . . . ? N5 N4 Zn1 N19 105.39(12) . . . . ? C61 O4 Zn2 N15 132.05(15) . . . . ? C61 O4 Zn2 N12 9.78(18) . . . . ? C61 O4 Zn2 N3 -110.33(15) . . . 7_575 ? C45 N15 Zn2 O4 77.92(17) . . . . ? N14 N15 Zn2 O4 -128.19(12) . . . . ? C45 N15 Zn2 N12 -145.64(16) . . . . ? N14 N15 Zn2 N12 8.25(14) . . . . ? C45 N15 Zn2 N3 -40.14(17) . . . 7_575 ? N14 N15 Zn2 N3 113.75(13) . . . 7_575 ? C36 N12 Zn2 O4 -78.74(19) . . . . ? N11 N12 Zn2 O4 118.82(12) . . . . ? C36 N12 Zn2 N15 151.57(17) . . . . ? N11 N12 Zn2 N15 -10.86(13) . . . . ? C36 N12 Zn2 N3 43.19(18) . . . 7_575 ? N11 N12 Zn2 N3 -119.24(12) . . . 7_575 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.018 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.067 data_08mz406_0m _database_code_depnum_ccdc_archive 'CCDC 804900' #TrackingRef 'web_deposit_cif_file_0_MukeshKumar_1292470389.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H38 B N9, C H2 Cl2, H2 O' _chemical_formula_sum 'C22 H42 B Cl2 N9 O' _chemical_formula_weight 530.36 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' B B 0.0013 0.0007 '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 16.290(8) _cell_length_b 18.323(9) _cell_length_c 20.877(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.436(11) _cell_angle_gamma 90.00 _cell_volume 6220(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1172 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 30.28 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 0.238 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.631657 _exptl_absorpt_correction_T_max 0.862222 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2007)' _exptl_special_details ; The crystal under investigation was found to be non-merohedrally twinned. The orientation matrices for the two components were identified using the program Cell_Now, and the two components were integrated using Saint, resulting in a total of 43194 reflections. 731 reflections (376 unique ones) involved component 1 only (mean I/sigma = 33.0), 720 reflections (374 unique ones) involved component 2 only (mean I/sigma = 28.2), and 41743 reflections (17588 unique ones) involved both components (mean I/sigma = 5.1). The exact twin matrix identified by the integration program was found to be -0.99923 0.00096 -0.00098, -0.00128 -1.00085 -0.00081, 0.14795 -0.00111 0.99182. The data were corrected for absorption using twinabs, and the structure was solved using direct methods with only the non-overlapping reflections of component 1. The structure was refined using the hklf 5 routine with all reflections of component 1 (including the overlapping ones) below a d-spacing threshold of 0.75, resulting in a BASF value of 0.413(2). The Rint value given is for all reflections before the cutoff at d = 0.84 and is based on agreement between observed single and composite intensities and those calculated from refined unique intensities and twin fractions (TWINABS (Sheldrick, 2007)). One of the methylene chloride molecules is disordered over two positions with an occupancy rate for the major component of 0.65(2). The two disordered carbon atoms were constrained to have identical ADPs and C-Cl distances within the disordered sections were restrained to be the same within a standard deviation of 0.02 Angstrom. ; _diffrn_ambient_temperature 100(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 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 43194 _diffrn_reflns_av_R_equivalents 0.0971 _diffrn_reflns_av_sigmaI/netI 0.1053 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10839 _reflns_number_gt 7000 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4 ' _computing_data_reduction 'Apex2 v2008.2-4 ' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0804P)^2^+37.5810P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10839 _refine_ls_number_parameters 681 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1651 _refine_ls_R_factor_gt 0.1047 _refine_ls_wR_factor_ref 0.2883 _refine_ls_wR_factor_gt 0.2499 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.5327(6) 0.1624(5) 0.0765(4) 0.028(2) Uani 1 1 d . . . H1 H 0.5040 0.1148 0.0685 0.033 Uiso 1 1 calc R . . B2 B 0.9478(6) 0.6365(5) 0.0558(4) 0.026(2) Uani 1 1 d . . . H2 H 0.9743 0.5880 0.0493 0.031 Uiso 1 1 calc R . . C1 C 0.6758(6) 0.2711(5) 0.1328(5) 0.039(2) Uani 1 1 d . . . H1A H 0.6554 0.2945 0.0927 0.058 Uiso 1 1 calc R . . H1B H 0.7300 0.2910 0.1461 0.058 Uiso 1 1 calc R . . H1C H 0.6375 0.2806 0.1662 0.058 Uiso 1 1 calc R . . C2 C 0.6827(5) 0.1897(5) 0.1224(4) 0.0277(19) Uani 1 1 d . . . C3 C 0.7298(5) 0.0834(5) 0.1151(5) 0.035(2) Uani 1 1 d . . . C4 C 0.7896(6) 0.0201(5) 0.1209(5) 0.044(3) Uani 1 1 d . . . C5 C 0.8586(7) 0.0355(7) 0.0777(8) 0.083(5) Uani 1 1 d . . . H5A H 0.8975 -0.0053 0.0798 0.125 Uiso 1 1 calc R . . H5B H 0.8871 0.0804 0.0919 0.125 Uiso 1 1 calc R . . H5C H 0.8360 0.0416 0.0335 0.125 Uiso 1 1 calc R . . C6 C 0.8217(8) 0.0138(6) 0.1915(6) 0.070(4) Uani 1 1 d . . . H6A H 0.7758 0.0024 0.2181 0.105 Uiso 1 1 calc R . . H6B H 0.8468 0.0602 0.2055 0.105 Uiso 1 1 calc R . . H6C H 0.8628 -0.0252 0.1957 0.105 Uiso 1 1 calc R . . C7 C 0.7461(7) -0.0496(5) 0.1027(7) 0.070(4) Uani 1 1 d . . . H7A H 0.7227 -0.0461 0.0584 0.105 Uiso 1 1 calc R . . H7B H 0.7018 -0.0581 0.1316 0.105 Uiso 1 1 calc R . . H7C H 0.7852 -0.0903 0.1061 0.105 Uiso 1 1 calc R . . C8 C 0.4636(7) 0.1048(5) 0.2014(4) 0.043(2) Uani 1 1 d . . . H8A H 0.4512 0.1024 0.2467 0.065 Uiso 1 1 calc R . . H8B H 0.5202 0.0884 0.1966 0.065 Uiso 1 1 calc R . . H8C H 0.4256 0.0732 0.1761 0.065 Uiso 1 1 calc R . . C9 C 0.4544(5) 0.1810(5) 0.1783(4) 0.031(2) Uani 1 1 d . . . C10 C 0.4262(6) 0.2936(5) 0.1686(4) 0.030(2) Uani 1 1 d . . . C11 C 0.3945(6) 0.3685(5) 0.1842(5) 0.037(2) Uani 1 1 d . . . C12 C 0.4434(9) 0.4001(7) 0.2403(8) 0.088(5) Uani 1 1 d . . . H12A H 0.4422 0.3666 0.2768 0.132 Uiso 1 1 calc R . . H12B H 0.4196 0.4471 0.2518 0.132 Uiso 1 1 calc R . . H12C H 0.5004 0.4073 0.2291 0.132 Uiso 1 1 calc R . . C13 C 0.3072(7) 0.3628(6) 0.2017(7) 0.069(4) Uani 1 1 d . . . H13A H 0.2750 0.3369 0.1677 0.104 Uiso 1 1 calc R . . H13B H 0.2846 0.4119 0.2067 0.104 Uiso 1 1 calc R . . H13C H 0.3048 0.3360 0.2421 0.104 Uiso 1 1 calc R . . C14 C 0.3968(11) 0.4167(7) 0.1239(7) 0.099(6) Uani 1 1 d . . . H14A H 0.4536 0.4212 0.1115 0.148 Uiso 1 1 calc R . . H14B H 0.3751 0.4653 0.1332 0.148 Uiso 1 1 calc R . . H14C H 0.3630 0.3944 0.0887 0.148 Uiso 1 1 calc R . . C15 C 0.3818(6) 0.2084(5) -0.0158(4) 0.038(2) Uani 1 1 d . . . H15A H 0.3774 0.1680 0.0146 0.057 Uiso 1 1 calc R . . H15B H 0.3526 0.1956 -0.0567 0.057 Uiso 1 1 calc R . . H15C H 0.3572 0.2523 0.0018 0.057 Uiso 1 1 calc R . . C16 C 0.4658(5) 0.2217(5) -0.0259(4) 0.031(2) Uani 1 1 d . . . C17 C 0.5768(5) 0.2582(4) -0.0718(4) 0.0229(17) Uani 1 1 d . . . C18 C 0.6310(5) 0.2897(4) -0.1195(4) 0.0283(19) Uani 1 1 d . . . C19 C 0.6050(6) 0.3706(5) -0.1330(5) 0.041(2) Uani 1 1 d . . . H19A H 0.5461 0.3725 -0.1456 0.061 Uiso 1 1 calc R . . H19B H 0.6363 0.3902 -0.1677 0.061 Uiso 1 1 calc R . . H19C H 0.6161 0.3997 -0.0941 0.061 Uiso 1 1 calc R . . C20 C 0.6184(6) 0.2465(5) -0.1831(4) 0.038(2) Uani 1 1 d . . . H20A H 0.6348 0.1955 -0.1758 0.057 Uiso 1 1 calc R . . H20B H 0.6521 0.2681 -0.2155 0.057 Uiso 1 1 calc R . . H20C H 0.5603 0.2484 -0.1982 0.057 Uiso 1 1 calc R . . C21 C 0.7206(5) 0.2868(5) -0.0954(5) 0.035(2) Uani 1 1 d . . . H21A H 0.7284 0.3158 -0.0561 0.053 Uiso 1 1 calc R . . H21B H 0.7550 0.3065 -0.1282 0.053 Uiso 1 1 calc R . . H21C H 0.7363 0.2360 -0.0862 0.053 Uiso 1 1 calc R . . C22 C 0.8310(6) 0.7456(5) 0.1292(5) 0.036(2) Uani 1 1 d . . . H22A H 0.7807 0.7701 0.1410 0.054 Uiso 1 1 calc R . . H22B H 0.8549 0.7724 0.0942 0.054 Uiso 1 1 calc R . . H22C H 0.8706 0.7440 0.1664 0.054 Uiso 1 1 calc R . . C23 C 0.8105(5) 0.6679(4) 0.1072(4) 0.0217(17) Uani 1 1 d . . . C24 C 0.7493(5) 0.5695(4) 0.0862(4) 0.0263(19) Uani 1 1 d . . . C25 C 0.6827(5) 0.5117(4) 0.0873(4) 0.032(2) Uani 1 1 d . . . C26 C 0.6821(8) 0.4803(6) 0.1546(5) 0.058(3) Uani 1 1 d . . . H26A H 0.6394 0.4427 0.1557 0.087 Uiso 1 1 calc R . . H26B H 0.6706 0.5192 0.1849 0.087 Uiso 1 1 calc R . . H26C H 0.7358 0.4585 0.1665 0.087 Uiso 1 1 calc R . . C27 C 0.6999(7) 0.4516(5) 0.0396(5) 0.046(3) Uani 1 1 d . . . H27A H 0.7472 0.4226 0.0560 0.069 Uiso 1 1 calc R . . H27B H 0.7121 0.4734 -0.0016 0.069 Uiso 1 1 calc R . . H27C H 0.6515 0.4199 0.0336 0.069 Uiso 1 1 calc R . . C28 C 0.5996(5) 0.5448(6) 0.0693(7) 0.061(3) Uani 1 1 d . . . H28A H 0.6024 0.5723 0.0292 0.092 Uiso 1 1 calc R . . H28B H 0.5839 0.5776 0.1035 0.092 Uiso 1 1 calc R . . H28C H 0.5586 0.5058 0.0633 0.092 Uiso 1 1 calc R . . C29 C 1.0954(6) 0.6593(6) -0.0343(5) 0.042(2) Uani 1 1 d . . . H29A H 1.1220 0.6723 0.0075 0.064 Uiso 1 1 calc R . . H29B H 1.1296 0.6762 -0.0685 0.064 Uiso 1 1 calc R . . H29C H 1.0890 0.6062 -0.0371 0.064 Uiso 1 1 calc R . . C30 C 1.0135(5) 0.6945(5) -0.0417(4) 0.032(2) Uani 1 1 d . . . C31 C 0.9136(5) 0.7625(4) -0.0782(4) 0.0287(19) Uani 1 1 d . . . C32 C 0.8637(5) 0.8168(4) -0.1190(4) 0.032(2) Uani 1 1 d . . . C33 C 0.8606(5) 0.7938(5) -0.1883(4) 0.036(2) Uani 1 1 d . . . H33A H 0.9163 0.7827 -0.2006 0.054 Uiso 1 1 calc R . . H33B H 0.8375 0.8335 -0.2152 0.054 Uiso 1 1 calc R . . H33C H 0.8260 0.7503 -0.1941 0.054 Uiso 1 1 calc R . . C34 C 0.7769(5) 0.8228(5) -0.0964(5) 0.040(2) Uani 1 1 d . . . H34A H 0.7456 0.8585 -0.1229 0.060 Uiso 1 1 calc R . . H34B H 0.7793 0.8385 -0.0515 0.060 Uiso 1 1 calc R . . H34C H 0.7498 0.7751 -0.1003 0.060 Uiso 1 1 calc R . . C35 C 0.9070(7) 0.8928(5) -0.1123(5) 0.048(3) Uani 1 1 d . . . H35A H 0.9630 0.8890 -0.1267 0.072 Uiso 1 1 calc R . . H35B H 0.9093 0.9082 -0.0672 0.072 Uiso 1 1 calc R . . H35C H 0.8760 0.9288 -0.1386 0.072 Uiso 1 1 calc R . . C36 C 0.9914(6) 0.5906(5) 0.1985(5) 0.038(2) Uani 1 1 d . . . H36A H 0.9327 0.5912 0.2065 0.057 Uiso 1 1 calc R . . H36B H 1.0238 0.5828 0.2390 0.057 Uiso 1 1 calc R . . H36C H 1.0023 0.5510 0.1685 0.057 Uiso 1 1 calc R . . C37 C 1.0151(5) 0.6629(4) 0.1696(4) 0.0245(18) Uani 1 1 d . . . C38 C 1.0559(5) 0.7701(5) 0.1558(4) 0.031(2) Uani 1 1 d . . . C39 C 1.0870(6) 0.8469(5) 0.1706(5) 0.038(2) Uani 1 1 d . . . C40 C 1.0231(7) 0.8820(6) 0.2125(7) 0.077(4) Uani 1 1 d . . . H40A H 0.9724 0.8916 0.1863 0.115 Uiso 1 1 calc R . . H40B H 1.0450 0.9280 0.2304 0.115 Uiso 1 1 calc R . . H40C H 1.0114 0.8487 0.2476 0.115 Uiso 1 1 calc R . . C41 C 1.0930(8) 0.8888(5) 0.1084(6) 0.065(3) Uani 1 1 d . . . H41A H 1.1311 0.8636 0.0813 0.097 Uiso 1 1 calc R . . H41B H 1.1134 0.9382 0.1179 0.097 Uiso 1 1 calc R . . H41C H 1.0386 0.8916 0.0859 0.097 Uiso 1 1 calc R . . C42 C 1.1700(6) 0.8449(6) 0.2073(5) 0.049(3) Uani 1 1 d . . . H42A H 1.1657 0.8169 0.2470 0.074 Uiso 1 1 calc R . . H42B H 1.1878 0.8948 0.2179 0.074 Uiso 1 1 calc R . . H42C H 1.2103 0.8216 0.1809 0.074 Uiso 1 1 calc R . . C44 C 0.1363(8) 0.4600(6) 0.0881(6) 0.060(3) Uani 1 1 d . . . H44A H 0.0952 0.4706 0.0524 0.072 Uiso 1 1 calc R . . H44B H 0.1792 0.4282 0.0714 0.072 Uiso 1 1 calc R . . Cl1 Cl 0.4804(2) 0.93373(16) 0.09806(17) 0.0737(10) Uani 1 1 d D . . C43 C 0.3951(7) 0.9698(12) 0.0555(10) 0.063(7) Uani 0.65(2) 1 d PD A 1 H43A H 0.4037 1.0226 0.0485 0.076 Uiso 0.65(2) 1 calc PR A 1 H43B H 0.3884 0.9459 0.0130 0.076 Uiso 0.65(2) 1 calc PR A 1 Cl2 Cl 0.3071(3) 0.9571(6) 0.0964(3) 0.082(3) Uani 0.65(2) 1 d PD A 1 C43B C 0.3866(17) 0.946(3) 0.0556(18) 0.063(7) Uani 0.35(2) 1 d PD A 2 H43C H 0.3983 0.9640 0.0124 0.076 Uiso 0.35(2) 1 calc PR A 2 H43D H 0.3611 0.8972 0.0497 0.076 Uiso 0.35(2) 1 calc PR A 2 Cl2B Cl 0.3132(11) 1.0031(13) 0.0849(7) 0.104(7) Uani 0.35(2) 1 d PD A 2 Cl3 Cl 0.18159(17) 0.54272(14) 0.11632(14) 0.0529(7) Uani 1 1 d . . . Cl4 Cl 0.08801(17) 0.41417(14) 0.14995(13) 0.0482(7) Uani 1 1 d . . . N1 N 0.6217(4) 0.1473(4) 0.0995(3) 0.0286(16) Uani 1 1 d . . . N2 N 0.6526(4) 0.0773(4) 0.0956(3) 0.0278(16) Uani 1 1 d . . . N3 N 0.7526(5) 0.1533(4) 0.1335(3) 0.0310(17) Uani 1 1 d . . . N4 N 0.4858(4) 0.2060(3) 0.1245(3) 0.0278(16) Uani 1 1 d . . . N5 N 0.4665(5) 0.2796(4) 0.1175(4) 0.0332(18) Uani 1 1 d . . . N6 N 0.4150(5) 0.2343(4) 0.2077(3) 0.0328(17) Uani 1 1 d . . . N7 N 0.5316(4) 0.2066(4) 0.0112(3) 0.0262(16) Uani 1 1 d . . . N8 N 0.6016(4) 0.2292(4) -0.0159(3) 0.0279(16) Uani 1 1 d . . . N9 N 0.4941(4) 0.2557(3) -0.0792(3) 0.0249(15) Uani 1 1 d . . . H9 H 0.4636 0.2726 -0.1121 0.030 Uiso 1 1 calc R . . N10 N 0.8614(4) 0.6249(4) 0.0745(3) 0.0242(15) Uani 1 1 d . . . N11 N 0.8203(4) 0.5605(3) 0.0624(3) 0.0253(15) Uani 1 1 d . . . N12 N 0.7408(4) 0.6365(4) 0.1162(3) 0.0275(16) Uani 1 1 d . . . N13 N 0.9501(4) 0.6829(4) -0.0083(3) 0.0254(15) Uani 1 1 d . . . N14 N 0.8851(4) 0.7255(4) -0.0286(3) 0.0285(16) Uani 1 1 d . . . N15 N 0.9918(4) 0.7450(4) -0.0861(3) 0.0278(16) Uani 1 1 d . . . H15 H 1.0233 0.7631 -0.1150 0.033 Uiso 1 1 calc R . . N16 N 0.9991(4) 0.6795(3) 0.1084(3) 0.0227(15) Uani 1 1 d . . . N17 N 1.0268(4) 0.7502(4) 0.0984(3) 0.0301(16) Uani 1 1 d . . . N18 N 1.0525(4) 0.7174(4) 0.2019(3) 0.0316(17) Uani 1 1 d . . . O1 O 0.6169(5) 0.7127(5) 0.1681(3) 0.058(2) Uani 1 1 d D . . H1D H 0.664(4) 0.696(7) 0.163(6) 0.087 Uiso 1 1 d D . . H1E H 0.611(8) 0.716(7) 0.2081(16) 0.087 Uiso 1 1 d D . . O2 O 0.9041(4) 0.2112(4) 0.1686(3) 0.0422(17) Uani 1 1 d D . . H2A H 0.855(3) 0.196(6) 0.169(5) 0.063 Uiso 1 1 d D . . H2B H 0.916(7) 0.211(6) 0.2085(14) 0.063 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.036(6) 0.023(5) 0.024(5) -0.004(4) -0.002(4) 0.000(4) B2 0.033(6) 0.016(4) 0.027(5) -0.003(4) -0.001(4) 0.013(4) C1 0.051(6) 0.023(5) 0.040(5) -0.002(4) -0.009(5) 0.004(4) C2 0.028(5) 0.031(5) 0.024(4) 0.005(4) 0.002(4) -0.003(4) C3 0.036(5) 0.024(5) 0.045(6) 0.010(4) 0.003(4) 0.008(4) C4 0.037(5) 0.017(4) 0.075(7) 0.005(5) -0.012(5) 0.002(4) C5 0.053(8) 0.044(7) 0.152(14) -0.017(8) -0.005(9) 0.015(6) C6 0.069(8) 0.044(7) 0.093(10) 0.028(7) -0.029(7) 0.010(6) C7 0.069(8) 0.013(5) 0.125(11) -0.011(6) -0.014(8) 0.014(5) C8 0.074(7) 0.029(5) 0.027(5) 0.008(4) 0.006(5) 0.009(5) C9 0.036(5) 0.025(5) 0.033(5) 0.001(4) 0.000(4) 0.005(4) C10 0.038(5) 0.023(5) 0.031(5) 0.002(4) 0.003(4) -0.003(4) C11 0.035(5) 0.023(5) 0.052(6) 0.005(4) 0.001(4) 0.001(4) C12 0.080(9) 0.044(7) 0.135(13) -0.038(8) -0.029(9) 0.015(7) C13 0.065(8) 0.024(5) 0.120(11) -0.004(6) 0.016(8) 0.001(5) C14 0.179(16) 0.038(7) 0.084(9) 0.028(7) 0.050(10) 0.047(9) C15 0.037(6) 0.047(6) 0.030(5) 0.007(4) -0.001(4) 0.003(5) C16 0.036(5) 0.031(5) 0.025(4) -0.004(4) -0.007(4) 0.009(4) C17 0.023(4) 0.018(4) 0.028(4) -0.006(3) 0.005(4) 0.003(3) C18 0.029(5) 0.026(4) 0.030(4) 0.002(4) 0.002(4) 0.002(4) C19 0.037(5) 0.021(5) 0.064(7) 0.006(4) 0.005(5) 0.002(4) C20 0.046(6) 0.045(6) 0.025(5) -0.006(4) 0.007(4) 0.004(5) C21 0.026(5) 0.026(5) 0.055(6) 0.007(4) 0.009(4) -0.002(4) C22 0.034(5) 0.020(4) 0.054(6) -0.003(4) 0.000(4) 0.004(4) C23 0.019(4) 0.028(4) 0.019(4) 0.000(3) 0.003(3) 0.002(3) C24 0.018(4) 0.022(4) 0.039(5) 0.004(4) 0.003(4) 0.003(3) C25 0.036(5) 0.021(4) 0.040(5) 0.001(4) 0.016(4) -0.010(4) C26 0.082(9) 0.050(7) 0.044(6) 0.011(5) 0.012(6) -0.022(6) C27 0.054(7) 0.037(6) 0.049(6) -0.012(5) 0.018(5) -0.013(5) C28 0.017(5) 0.049(7) 0.119(10) -0.009(7) 0.003(6) -0.012(5) C29 0.031(5) 0.060(7) 0.036(5) -0.001(5) 0.002(4) 0.003(5) C30 0.024(5) 0.031(5) 0.042(5) -0.010(4) -0.002(4) -0.007(4) C31 0.041(5) 0.020(4) 0.024(4) -0.002(3) -0.005(4) -0.005(4) C32 0.028(5) 0.015(4) 0.051(6) 0.011(4) 0.003(4) 0.002(3) C33 0.022(5) 0.040(5) 0.045(6) 0.012(4) 0.002(4) -0.006(4) C34 0.027(5) 0.035(5) 0.058(6) 0.013(5) -0.001(5) 0.016(4) C35 0.060(7) 0.026(5) 0.058(6) 0.005(5) -0.001(5) -0.005(5) C36 0.045(6) 0.029(5) 0.040(5) 0.003(4) 0.001(4) 0.005(4) C37 0.019(4) 0.024(4) 0.030(5) 0.003(4) 0.002(4) 0.003(4) C38 0.028(5) 0.023(5) 0.043(5) -0.005(4) 0.011(4) 0.012(4) C39 0.029(5) 0.027(5) 0.059(6) -0.013(4) 0.009(5) -0.003(4) C40 0.052(7) 0.034(6) 0.145(13) -0.046(7) 0.006(8) -0.001(5) C41 0.098(10) 0.024(5) 0.071(8) 0.014(5) -0.011(7) 0.000(6) C42 0.044(6) 0.034(6) 0.070(7) -0.012(5) 0.007(5) -0.004(5) C44 0.073(8) 0.041(6) 0.066(7) -0.002(6) 0.004(6) -0.021(6) Cl1 0.089(2) 0.0452(16) 0.084(2) -0.0197(16) -0.0199(18) 0.0132(16) C43 0.049(8) 0.034(17) 0.107(11) -0.018(10) 0.008(8) -0.012(9) Cl2 0.055(3) 0.062(6) 0.130(5) 0.016(4) 0.024(3) 0.000(3) C43B 0.049(8) 0.034(17) 0.107(11) -0.018(10) 0.008(8) -0.012(9) Cl2B 0.172(14) 0.074(14) 0.067(8) -0.027(8) 0.009(7) 0.006(10) Cl3 0.0584(16) 0.0368(13) 0.0638(17) 0.0005(13) 0.0071(13) -0.0122(12) Cl4 0.0612(17) 0.0324(13) 0.0521(15) -0.0028(11) 0.0113(13) -0.0060(12) N1 0.031(4) 0.019(4) 0.036(4) 0.002(3) 0.003(3) -0.003(3) N2 0.021(4) 0.022(4) 0.041(4) 0.005(3) -0.003(3) 0.004(3) N3 0.039(4) 0.016(3) 0.037(4) 0.005(3) 0.001(3) 0.000(3) N4 0.034(4) 0.019(3) 0.030(4) 0.000(3) 0.003(3) 0.007(3) N5 0.040(4) 0.019(4) 0.041(4) 0.009(3) 0.000(4) 0.000(3) N6 0.038(4) 0.024(4) 0.037(4) 0.002(3) 0.008(3) 0.005(3) N7 0.005(3) 0.030(4) 0.044(4) -0.007(3) 0.002(3) -0.001(3) N8 0.025(4) 0.021(4) 0.038(4) -0.005(3) 0.005(3) 0.004(3) N9 0.027(4) 0.019(3) 0.029(4) 0.000(3) 0.000(3) 0.006(3) N10 0.023(4) 0.024(4) 0.025(4) 0.000(3) -0.002(3) 0.004(3) N11 0.028(4) 0.017(3) 0.031(4) -0.002(3) -0.003(3) 0.001(3) N12 0.032(4) 0.024(4) 0.027(4) -0.002(3) 0.000(3) -0.003(3) N13 0.023(4) 0.028(4) 0.025(4) -0.007(3) 0.001(3) -0.003(3) N14 0.030(4) 0.025(4) 0.030(4) -0.008(3) 0.000(3) -0.003(3) N15 0.029(4) 0.024(4) 0.030(4) 0.005(3) -0.003(3) -0.006(3) N16 0.018(3) 0.024(4) 0.027(4) -0.003(3) 0.004(3) 0.003(3) N17 0.030(4) 0.027(4) 0.033(4) 0.002(3) 0.005(3) 0.001(3) N18 0.024(4) 0.029(4) 0.041(4) -0.002(3) -0.006(3) 0.004(3) O1 0.045(4) 0.095(6) 0.032(4) -0.012(4) -0.003(3) 0.037(4) O2 0.033(4) 0.062(5) 0.031(3) 0.006(3) -0.001(3) -0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N4 1.520(11) . ? B1 N1 1.525(12) . ? B1 N7 1.585(12) . ? B1 H1 1.0000 . ? B2 N10 1.499(12) . ? B2 N16 1.555(11) . ? B2 N13 1.587(11) . ? B2 H2 1.0000 . ? C1 C2 1.513(12) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.327(10) . ? C2 N3 1.327(11) . ? C3 N2 1.303(11) . ? C3 N3 1.382(11) . ? C3 C4 1.515(12) . ? C4 C7 1.500(13) . ? C4 C5 1.508(17) . ? C4 C6 1.538(15) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.481(12) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N6 1.338(11) . ? C9 N4 1.342(11) . ? C10 N5 1.311(11) . ? C10 N6 1.377(11) . ? C10 C11 1.508(12) . ? C11 C13 1.492(14) . ? C11 C12 1.493(15) . ? C11 C14 1.540(15) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.419(12) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N7 1.313(10) . ? C16 N9 1.378(11) . ? C17 N8 1.322(10) . ? C17 N9 1.349(10) . ? C17 C18 1.487(11) . ? C18 C21 1.516(12) . ? C18 C20 1.548(12) . ? C18 C19 1.563(12) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.527(11) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 N12 1.297(10) . ? C23 N10 1.356(10) . ? C24 N11 1.296(10) . ? C24 N12 1.389(10) . ? C24 C25 1.517(11) . ? C25 C28 1.509(13) . ? C25 C26 1.518(13) . ? C25 C27 1.524(12) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.482(12) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N13 1.298(11) . ? C30 N15 1.342(11) . ? C31 N15 1.335(11) . ? C31 N14 1.344(10) . ? C31 C32 1.514(11) . ? C32 C33 1.503(13) . ? C32 C34 1.522(12) . ? C32 C35 1.563(12) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.516(11) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 N16 1.323(10) . ? C37 N18 1.332(10) . ? C38 N17 1.312(11) . ? C38 N18 1.368(11) . ? C38 C39 1.521(12) . ? C39 C42 1.515(14) . ? C39 C41 1.516(14) . ? C39 C40 1.540(14) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C44 Cl4 1.765(11) . ? C44 Cl3 1.771(11) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? Cl1 C43 1.735(14) . ? Cl1 C43B 1.736(17) . ? C43 Cl2 1.727(15) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43B Cl2B 1.729(17) . ? C43B H43C 0.9900 . ? C43B H43D 0.9900 . ? N1 N2 1.383(9) . ? N4 N5 1.392(9) . ? N7 N8 1.368(9) . ? N9 H9 0.8800 . ? N10 N11 1.373(9) . ? N13 N14 1.363(9) . ? N15 H15 0.8800 . ? N16 N17 1.392(9) . ? O1 H1D 0.85(2) . ? O1 H1E 0.85(2) . ? O2 H2A 0.85(2) . ? O2 H2B 0.84(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 B1 N1 113.2(7) . . ? N4 B1 N7 108.6(7) . . ? N1 B1 N7 108.9(7) . . ? N4 B1 H1 108.7 . . ? N1 B1 H1 108.7 . . ? N7 B1 H1 108.7 . . ? N10 B2 N16 111.2(7) . . ? N10 B2 N13 111.4(7) . . ? N16 B2 N13 106.6(7) . . ? N10 B2 H2 109.2 . . ? N16 B2 H2 109.2 . . ? N13 B2 H2 109.2 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 N3 112.7(7) . . ? N1 C2 C1 124.6(8) . . ? N3 C2 C1 122.7(8) . . ? N2 C3 N3 113.9(7) . . ? N2 C3 C4 124.2(8) . . ? N3 C3 C4 121.8(8) . . ? C7 C4 C5 111.5(10) . . ? C7 C4 C3 109.9(8) . . ? C5 C4 C3 107.9(8) . . ? C7 C4 C6 107.9(9) . . ? C5 C4 C6 111.3(10) . . ? C3 C4 C6 108.3(9) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N6 C9 N4 110.6(7) . . ? N6 C9 C8 125.5(8) . . ? N4 C9 C8 123.9(8) . . ? N5 C10 N6 114.8(7) . . ? N5 C10 C11 123.2(8) . . ? N6 C10 C11 122.1(7) . . ? C13 C11 C12 107.8(10) . . ? C13 C11 C10 109.5(8) . . ? C12 C11 C10 110.4(8) . . ? C13 C11 C14 108.0(10) . . ? C12 C11 C14 112.4(11) . . ? C10 C11 C14 108.7(8) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N7 C16 N9 105.7(7) . . ? N7 C16 C15 129.6(8) . . ? N9 C16 C15 124.7(7) . . ? N8 C17 N9 109.7(7) . . ? N8 C17 C18 125.8(7) . . ? N9 C17 C18 124.5(7) . . ? C17 C18 C21 111.2(7) . . ? C17 C18 C20 108.8(7) . . ? C21 C18 C20 110.1(7) . . ? C17 C18 C19 108.8(7) . . ? C21 C18 C19 109.8(7) . . ? C20 C18 C19 108.1(7) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N12 C23 N10 112.5(7) . . ? N12 C23 C22 123.2(7) . . ? N10 C23 C22 124.3(7) . . ? N11 C24 N12 113.6(7) . . ? N11 C24 C25 125.0(7) . . ? N12 C24 C25 121.2(7) . . ? C28 C25 C24 110.4(7) . . ? C28 C25 C26 109.1(9) . . ? C24 C25 C26 108.9(8) . . ? C28 C25 C27 108.9(8) . . ? C24 C25 C27 109.6(7) . . ? C26 C25 C27 110.0(8) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N13 C30 N15 107.4(8) . . ? N13 C30 C29 127.8(9) . . ? N15 C30 C29 124.8(8) . . ? N15 C31 N14 110.5(7) . . ? N15 C31 C32 125.0(7) . . ? N14 C31 C32 124.6(8) . . ? C33 C32 C31 110.0(7) . . ? C33 C32 C34 109.9(8) . . ? C31 C32 C34 110.5(7) . . ? C33 C32 C35 109.0(7) . . ? C31 C32 C35 108.1(7) . . ? C34 C32 C35 109.4(8) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 H36A 109.5 . . ? C37 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C37 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N16 C37 N18 112.0(7) . . ? N16 C37 C36 123.0(7) . . ? N18 C37 C36 125.0(8) . . ? N17 C38 N18 114.8(7) . . ? N17 C38 C39 122.7(8) . . ? N18 C38 C39 122.5(8) . . ? C42 C39 C41 110.1(9) . . ? C42 C39 C38 110.9(8) . . ? C41 C39 C38 109.4(8) . . ? C42 C39 C40 109.6(9) . . ? C41 C39 C40 110.9(10) . . ? C38 C39 C40 105.9(7) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Cl4 C44 Cl3 111.0(6) . . ? Cl4 C44 H44A 109.4 . . ? Cl3 C44 H44A 109.4 . . ? Cl4 C44 H44B 109.4 . . ? Cl3 C44 H44B 109.4 . . ? H44A C44 H44B 108.0 . . ? Cl2 C43 Cl1 111.0(11) . . ? Cl2 C43 H43A 109.4 . . ? Cl1 C43 H43A 109.4 . . ? Cl2 C43 H43B 109.4 . . ? Cl1 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? Cl2B C43B Cl1 120.3(18) . . ? Cl2B C43B H43C 107.3 . . ? Cl1 C43B H43C 107.3 . . ? Cl2B C43B H43D 107.3 . . ? Cl1 C43B H43D 107.3 . . ? H43C C43B H43D 106.9 . . ? C2 N1 N2 107.2(7) . . ? C2 N1 B1 133.2(7) . . ? N2 N1 B1 119.5(6) . . ? C3 N2 N1 104.4(7) . . ? C2 N3 C3 101.7(7) . . ? C9 N4 N5 108.9(7) . . ? C9 N4 B1 127.1(7) . . ? N5 N4 B1 124.0(7) . . ? C10 N5 N4 103.0(7) . . ? C9 N6 C10 102.7(7) . . ? C16 N7 N8 111.3(7) . . ? C16 N7 B1 125.6(7) . . ? N8 N7 B1 123.0(6) . . ? C17 N8 N7 105.6(7) . . ? C17 N9 C16 107.6(7) . . ? C17 N9 H9 126.2 . . ? C16 N9 H9 126.2 . . ? C23 N10 N11 106.6(6) . . ? C23 N10 B2 131.4(7) . . ? N11 N10 B2 121.9(6) . . ? C24 N11 N10 104.9(6) . . ? C23 N12 C24 102.4(7) . . ? C30 N13 N14 111.5(7) . . ? C30 N13 B2 126.9(7) . . ? N14 N13 B2 120.8(6) . . ? C31 N14 N13 103.4(7) . . ? C31 N15 C30 107.1(7) . . ? C31 N15 H15 126.4 . . ? C30 N15 H15 126.4 . . ? C37 N16 N17 108.2(6) . . ? C37 N16 B2 129.2(7) . . ? N17 N16 B2 122.1(6) . . ? C38 N17 N16 102.9(7) . . ? C37 N18 C38 102.0(7) . . ? H1D O1 H1E 108(10) . . ? H2A O2 H2B 99(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C3 C4 C7 -1.6(14) . . . . ? N3 C3 C4 C7 175.2(10) . . . . ? N2 C3 C4 C5 120.2(11) . . . . ? N3 C3 C4 C5 -63.0(12) . . . . ? N2 C3 C4 C6 -119.1(10) . . . . ? N3 C3 C4 C6 57.7(12) . . . . ? N5 C10 C11 C13 132.5(10) . . . . ? N6 C10 C11 C13 -47.6(13) . . . . ? N5 C10 C11 C12 -109.0(12) . . . . ? N6 C10 C11 C12 70.9(12) . . . . ? N5 C10 C11 C14 14.7(14) . . . . ? N6 C10 C11 C14 -165.4(11) . . . . ? N8 C17 C18 C21 -1.8(11) . . . . ? N9 C17 C18 C21 177.7(7) . . . . ? N8 C17 C18 C20 119.7(8) . . . . ? N9 C17 C18 C20 -60.9(10) . . . . ? N8 C17 C18 C19 -122.8(8) . . . . ? N9 C17 C18 C19 56.6(10) . . . . ? N11 C24 C25 C28 -137.0(9) . . . . ? N12 C24 C25 C28 48.1(11) . . . . ? N11 C24 C25 C26 103.2(10) . . . . ? N12 C24 C25 C26 -71.7(10) . . . . ? N11 C24 C25 C27 -17.1(12) . . . . ? N12 C24 C25 C27 168.0(8) . . . . ? N15 C31 C32 C33 58.2(10) . . . . ? N14 C31 C32 C33 -122.2(8) . . . . ? N15 C31 C32 C34 179.7(8) . . . . ? N14 C31 C32 C34 -0.7(12) . . . . ? N15 C31 C32 C35 -60.7(11) . . . . ? N14 C31 C32 C35 118.9(9) . . . . ? N17 C38 C39 C42 -131.9(9) . . . . ? N18 C38 C39 C42 51.3(11) . . . . ? N17 C38 C39 C41 -10.3(12) . . . . ? N18 C38 C39 C41 172.9(8) . . . . ? N17 C38 C39 C40 109.2(11) . . . . ? N18 C38 C39 C40 -67.5(11) . . . . ? C43B Cl1 C43 Cl2 62(6) . . . . ? C43 Cl1 C43B Cl2B -60(4) . . . . ? N3 C2 N1 N2 0.9(9) . . . . ? C1 C2 N1 N2 178.5(8) . . . . ? N3 C2 N1 B1 -176.7(8) . . . . ? C1 C2 N1 B1 0.9(14) . . . . ? N4 B1 N1 C2 -51.1(12) . . . . ? N7 B1 N1 C2 69.7(11) . . . . ? N4 B1 N1 N2 131.5(8) . . . . ? N7 B1 N1 N2 -107.6(8) . . . . ? N3 C3 N2 N1 1.5(10) . . . . ? C4 C3 N2 N1 178.6(9) . . . . ? C2 N1 N2 C3 -1.4(9) . . . . ? B1 N1 N2 C3 176.6(7) . . . . ? N1 C2 N3 C3 0.0(9) . . . . ? C1 C2 N3 C3 -177.6(8) . . . . ? N2 C3 N3 C2 -1.0(10) . . . . ? C4 C3 N3 C2 -178.1(9) . . . . ? N6 C9 N4 N5 0.0(10) . . . . ? C8 C9 N4 N5 -179.4(9) . . . . ? N6 C9 N4 B1 -178.1(8) . . . . ? C8 C9 N4 B1 2.5(14) . . . . ? N1 B1 N4 C9 -77.5(11) . . . . ? N7 B1 N4 C9 161.5(8) . . . . ? N1 B1 N4 N5 104.7(9) . . . . ? N7 B1 N4 N5 -16.3(11) . . . . ? N6 C10 N5 N4 -2.2(10) . . . . ? C11 C10 N5 N4 177.7(8) . . . . ? C9 N4 N5 C10 1.3(9) . . . . ? B1 N4 N5 C10 179.4(8) . . . . ? N4 C9 N6 C10 -1.2(9) . . . . ? C8 C9 N6 C10 178.2(9) . . . . ? N5 C10 N6 C9 2.2(10) . . . . ? C11 C10 N6 C9 -177.7(8) . . . . ? N9 C16 N7 N8 0.0(9) . . . . ? C15 C16 N7 N8 -179.3(9) . . . . ? N9 C16 N7 B1 -175.6(7) . . . . ? C15 C16 N7 B1 5.1(14) . . . . ? N4 B1 N7 C16 -64.5(10) . . . . ? N1 B1 N7 C16 171.9(7) . . . . ? N4 B1 N7 N8 120.5(8) . . . . ? N1 B1 N7 N8 -3.2(10) . . . . ? N9 C17 N8 N7 1.5(8) . . . . ? C18 C17 N8 N7 -179.0(7) . . . . ? C16 N7 N8 C17 -0.9(8) . . . . ? B1 N7 N8 C17 174.8(7) . . . . ? N8 C17 N9 C16 -1.5(9) . . . . ? C18 C17 N9 C16 179.0(7) . . . . ? N7 C16 N9 C17 0.9(9) . . . . ? C15 C16 N9 C17 -179.8(8) . . . . ? N12 C23 N10 N11 -0.6(9) . . . . ? C22 C23 N10 N11 -178.6(7) . . . . ? N12 C23 N10 B2 -177.1(7) . . . . ? C22 C23 N10 B2 5.0(13) . . . . ? N16 B2 N10 C23 35.5(11) . . . . ? N13 B2 N10 C23 -83.3(10) . . . . ? N16 B2 N10 N11 -140.5(7) . . . . ? N13 B2 N10 N11 100.8(8) . . . . ? N12 C24 N11 N10 -2.0(9) . . . . ? C25 C24 N11 N10 -177.3(7) . . . . ? C23 N10 N11 C24 1.6(8) . . . . ? B2 N10 N11 C24 178.4(7) . . . . ? N10 C23 N12 C24 -0.5(9) . . . . ? C22 C23 N12 C24 177.5(8) . . . . ? N11 C24 N12 C23 1.6(9) . . . . ? C25 C24 N12 C23 177.1(7) . . . . ? N15 C30 N13 N14 -0.9(9) . . . . ? C29 C30 N13 N14 179.8(8) . . . . ? N15 C30 N13 B2 -170.8(7) . . . . ? C29 C30 N13 B2 9.9(14) . . . . ? N10 B2 N13 C30 -170.5(7) . . . . ? N16 B2 N13 C30 68.0(10) . . . . ? N10 B2 N13 N14 20.4(10) . . . . ? N16 B2 N13 N14 -101.1(8) . . . . ? N15 C31 N14 N13 -1.8(8) . . . . ? C32 C31 N14 N13 178.5(7) . . . . ? C30 N13 N14 C31 1.7(9) . . . . ? B2 N13 N14 C31 172.3(7) . . . . ? N14 C31 N15 C30 1.4(9) . . . . ? C32 C31 N15 C30 -179.0(8) . . . . ? N13 C30 N15 C31 -0.3(9) . . . . ? C29 C30 N15 C31 179.0(8) . . . . ? N18 C37 N16 N17 -0.5(9) . . . . ? C36 C37 N16 N17 178.3(7) . . . . ? N18 C37 N16 B2 -172.0(7) . . . . ? C36 C37 N16 B2 6.8(12) . . . . ? N10 B2 N16 C37 58.4(10) . . . . ? N13 B2 N16 C37 -180.0(7) . . . . ? N10 B2 N16 N17 -112.1(8) . . . . ? N13 B2 N16 N17 9.6(9) . . . . ? N18 C38 N17 N16 2.4(9) . . . . ? C39 C38 N17 N16 -174.6(7) . . . . ? C37 N16 N17 C38 -1.1(8) . . . . ? B2 N16 N17 C38 171.2(7) . . . . ? N16 C37 N18 C38 1.8(9) . . . . ? C36 C37 N18 C38 -177.0(8) . . . . ? N17 C38 N18 C37 -2.7(9) . . . . ? C39 C38 N18 C37 174.3(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2B N18 0.84(2) 1.91(2) 2.754(10) 175(12) 2_745 O2 H2A N3 0.85(2) 1.95(5) 2.746(10) 157(11) . O1 H1E N6 0.85(2) 1.86(3) 2.704(10) 171(13) 2_655 O1 H1D N12 0.85(2) 1.96(7) 2.732(10) 152(13) . N15 H15 O2 0.88 1.74 2.614(9) 171.4 3_765 N9 H9 O1 0.88 1.72 2.578(9) 162.7 3_665 _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.666 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.105