Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Zong-Wan Mao' _publ_contact_author_address ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Xin Gang Xi Lu 135 Guangzhou Guangzhou 510275 CHINA ; _publ_contact_author_email CESMZW@MAIL.SYSU.EDU.CN _publ_section_title ; Double-strand DNA cleavage by zinc complexes of dicationic 2, 2'-dipyridyl derivatives ; loop_ _publ_author_name 'Zong-Wan Mao.' 'Yan An.' 'Liang-Nian Ji.' 'Yan-Yong Lin.' 'Hongzhe Sun.' ; Ming-Liang Tong ; 'Hui Wang.' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 627515' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H128 Cl8 N12 O36 Zn' _chemical_formula_weight 2086.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 18.7486(7) _cell_length_b 52.014(2) _cell_length_c 13.1492(5) _cell_angle_alpha 90.00 _cell_angle_beta 131.918(3) _cell_angle_gamma 90.00 _cell_volume 9541.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 12435 _cell_measurement_theta_min 3.1624 _cell_measurement_theta_max 62.1091 _exptl_crystal_description polyhedral _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4392 _exptl_absorpt_coefficient_mu 3.177 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.69403 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22997 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -58 _diffrn_reflns_limit_k_max 59 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 62.41 _reflns_number_total 10104 _reflns_number_gt 8364 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1644P)^2^+5.5103P] 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 -0.02(2) _refine_ls_number_reflns 10104 _refine_ls_number_parameters 1180 _refine_ls_number_restraints 135 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0735 _refine_ls_wR_factor_ref 0.2149 _refine_ls_wR_factor_gt 0.2039 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.092 _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 Zn1 Zn -0.18150(7) 0.875750(17) -0.66012(8) 0.0284(3) Uani 1 1 d . . . N1 N -0.0933(4) 0.87491(11) -0.4385(6) 0.0284(14) Uani 1 1 d . . . N2 N -0.2379(5) 0.90725(12) -0.6203(6) 0.0305(14) Uani 1 1 d . . . N3 N 0.1958(5) 0.83720(14) -0.0488(7) 0.0401(16) Uani 1 1 d . . . N4 N -0.5157(5) 0.95775(13) -0.8564(7) 0.0375(15) Uani 1 1 d . . . N5 N -0.2713(5) 0.84490(13) -0.6873(7) 0.0307(14) Uani 1 1 d . . . N6 N -0.3051(4) 0.87684(11) -0.8778(6) 0.0266(13) Uani 1 1 d . . . N7 N -0.3084(6) 0.79392(13) -0.4336(7) 0.0390(16) Uani 1 1 d . . . N8 N -0.4121(6) 0.90446(14) -1.2979(7) 0.0420(17) Uani 1 1 d . . . N9 N -0.0839(5) 0.84950(13) -0.6433(6) 0.0334(15) Uani 1 1 d . . . N10 N -0.0884(4) 0.90055(13) -0.6562(6) 0.0291(13) Uani 1 1 d . . . N11 N -0.0669(7) 0.76327(17) -0.7288(10) 0.059(2) Uani 1 1 d . . . N12 N 0.0029(5) 0.98825(14) -0.5684(7) 0.0404(16) Uani 1 1 d . . . C1 C -0.0247(6) 0.85741(16) -0.3493(8) 0.0348(18) Uani 1 1 d . . . H1 H -0.0105 0.8445 -0.3845 0.042 Uiso 1 1 calc R . . C2 C 0.0248(6) 0.85711(15) -0.2134(8) 0.0327(17) Uani 1 1 d . . . C3 C 0.0049(6) 0.87600(16) -0.1615(8) 0.0361(18) Uani 1 1 d . . . H3 H 0.0377 0.8763 -0.0669 0.043 Uiso 1 1 calc R . . C4 C -0.0633(6) 0.89442(15) -0.2489(8) 0.0338(17) Uani 1 1 d . . . H4 H -0.0767 0.9077 -0.2141 0.041 Uiso 1 1 calc R . . C5 C -0.1123(6) 0.89358(15) -0.3871(8) 0.0315(17) Uani 1 1 d . . . C6 C -0.1914(5) 0.91146(14) -0.4875(8) 0.0282(15) Uani 1 1 d . . . C7 C -0.2140(6) 0.93160(17) -0.4455(9) 0.0364(18) Uani 1 1 d . . . H7 H -0.1792 0.9343 -0.3511 0.044 Uiso 1 1 calc R . . C8 C -0.2885(6) 0.94796(14) -0.5430(8) 0.0341(17) Uani 1 1 d . . . H8 H -0.3059 0.9617 -0.5157 0.041 Uiso 1 1 calc R . . C9 C -0.3380(6) 0.94422(15) -0.6813(9) 0.0325(17) Uani 1 1 d . . . C10 C -0.3078(6) 0.92338(15) -0.7124(8) 0.0317(16) Uani 1 1 d . . . H10 H -0.3395 0.9206 -0.8056 0.038 Uiso 1 1 calc R . . C11 C 0.0891(6) 0.83444(16) -0.1252(8) 0.0353(18) Uani 1 1 d . . . H11A H 0.0644 0.8190 -0.1844 0.042 Uiso 1 1 calc R . . H11B H 0.0831 0.8312 -0.0570 0.042 Uiso 1 1 calc R . . C12 C -0.4131(6) 0.96284(15) -0.7904(9) 0.0339(17) Uani 1 1 d . . . H12A H -0.4107 0.9631 -0.8634 0.041 Uiso 1 1 calc R . . H12B H -0.3954 0.9803 -0.7497 0.041 Uiso 1 1 calc R . . C13 C 0.2106(7) 0.83941(19) -0.1484(11) 0.053(2) Uani 1 1 d . . . H13A H 0.1743 0.8545 -0.2075 0.063 Uiso 1 1 calc R . . H13B H 0.2794 0.8428 -0.0956 0.063 Uiso 1 1 calc R . . C14 C 0.1814(10) 0.8165(3) -0.2393(14) 0.069(3) Uani 1 1 d . . . H14A H 0.1990 0.8194 -0.2938 0.104 Uiso 1 1 calc R . . H14B H 0.1120 0.8140 -0.3004 0.104 Uiso 1 1 calc R . . H14C H 0.2144 0.8011 -0.1828 0.104 Uiso 1 1 calc R . . C15 C 0.2439(8) 0.81262(18) 0.0395(11) 0.062(3) Uani 1 1 d . . . H15A H 0.2347 0.8121 0.1053 0.075 Uiso 1 1 calc R . . H15B H 0.2116 0.7974 -0.0206 0.075 Uiso 1 1 calc R . . C16 C 0.3499(9) 0.8110(2) 0.1174(18) 0.093(6) Uani 1 1 d . . . H16A H 0.3730 0.7936 0.1547 0.140 Uiso 1 1 calc R . . H16B H 0.3846 0.8235 0.1925 0.140 Uiso 1 1 calc R . . H16C H 0.3608 0.8148 0.0558 0.140 Uiso 1 1 calc R . . C17 C 0.2375(7) 0.86094(16) 0.0407(10) 0.052(3) Uani 1 1 d . . . H17A H 0.3036 0.8634 0.0780 0.063 Uiso 1 1 calc R . . H17B H 0.1994 0.8760 -0.0176 0.063 Uiso 1 1 calc R . . C18 C 0.2407(10) 0.8608(2) 0.1576(12) 0.081(5) Uani 1 1 d . . . H18A H 0.2715 0.8766 0.2111 0.122 Uiso 1 1 calc R . . H18B H 0.2775 0.8459 0.2160 0.122 Uiso 1 1 calc R . . H18C H 0.1753 0.8598 0.1223 0.122 Uiso 1 1 calc R . . C19 C -0.5213(7) 0.95691(19) -0.7468(11) 0.047(2) Uani 1 1 d . . . H19A H -0.4852 0.9416 -0.6891 0.057 Uiso 1 1 calc R . . H19B H -0.4875 0.9722 -0.6880 0.057 Uiso 1 1 calc R . . C20 C -0.6179(8) 0.9560(3) -0.7912(14) 0.068(3) Uani 1 1 d . . . H20A H -0.6124 0.9495 -0.7163 0.102 Uiso 1 1 calc R . . H20B H -0.6596 0.9446 -0.8705 0.102 Uiso 1 1 calc R . . H20C H -0.6453 0.9734 -0.8160 0.102 Uiso 1 1 calc R . . C21 C -0.5765(8) 0.9802(2) -0.9523(14) 0.066(3) Uani 1 1 d . . . H21A H -0.6430 0.9737 -1.0215 0.079 Uiso 1 1 calc R . . H21B H -0.5768 0.9932 -0.8976 0.079 Uiso 1 1 calc R . . C22 C -0.5565(12) 0.9939(3) -1.0262(17) 0.088(4) Uani 1 1 d . . . H22A H -0.6006 1.0085 -1.0748 0.132 Uiso 1 1 calc R . . H22B H -0.5649 0.9823 -1.0922 0.132 Uiso 1 1 calc R . . H22C H -0.4903 1.0002 -0.9619 0.132 Uiso 1 1 calc R . . C23 C -0.5509(7) 0.93207(17) -0.9313(10) 0.045(2) Uani 1 1 d . . . H23A H -0.5056 0.9185 -0.8660 0.054 Uiso 1 1 calc R . . H23B H -0.6138 0.9282 -0.9600 0.054 Uiso 1 1 calc R . . C24 C -0.5612(9) 0.9305(3) -1.0528(12) 0.072(3) Uani 1 1 d . . . H24A H -0.5767 0.9127 -1.0869 0.108 Uiso 1 1 calc R . . H24B H -0.5010 0.9356 -1.0279 0.108 Uiso 1 1 calc R . . H24C H -0.6129 0.9419 -1.1242 0.108 Uiso 1 1 calc R . . C25 C -0.2503(6) 0.82800(15) -0.5946(8) 0.0315(16) Uani 1 1 d . . . H25 H -0.1911 0.8300 -0.5033 0.038 Uiso 1 1 calc R . . C26 C -0.3097(6) 0.80745(14) -0.6224(8) 0.0299(16) Uani 1 1 d . . . C27 C -0.3947(6) 0.80485(16) -0.7575(9) 0.0364(18) Uani 1 1 d . . . H27 H -0.4365 0.7909 -0.7828 0.044 Uiso 1 1 calc R . . C28 C -0.4188(6) 0.82227(17) -0.8544(9) 0.0372(18) Uani 1 1 d . . . H28 H -0.4775 0.8206 -0.9464 0.045 Uiso 1 1 calc R . . C29 C -0.3567(6) 0.84247(13) -0.8173(7) 0.0293(16) Uani 1 1 d D . . C30 C -0.3774(6) 0.86173(15) -0.9181(8) 0.0354(18) Uani 1 1 d D . . C31 C -0.4680(6) 0.86369(19) -1.0470(9) 0.041(2) Uani 1 1 d . . . H31 H -0.5192 0.8533 -1.0715 0.050 Uiso 1 1 calc R . . C32 C -0.4824(6) 0.88096(18) -1.1392(8) 0.0380(19) Uani 1 1 d . . . H32 H -0.5441 0.8826 -1.2279 0.046 Uiso 1 1 calc R . . C33 C -0.4062(6) 0.89603(15) -1.1018(8) 0.0338(17) Uani 1 1 d . . . C34 C -0.3205(6) 0.89344(14) -0.9702(8) 0.0300(16) Uani 1 1 d . . . H34 H -0.2686 0.9040 -0.9419 0.036 Uiso 1 1 calc R . . C35 C -0.2777(6) 0.78831(15) -0.5144(8) 0.0337(17) Uani 1 1 d . . . H35A H -0.2068 0.7873 -0.4490 0.040 Uiso 1 1 calc R . . H35B H -0.3029 0.7712 -0.5579 0.040 Uiso 1 1 calc R . . C36 C -0.4206(6) 0.91563(15) -1.1996(8) 0.0349(17) Uani 1 1 d . . . H36A H -0.3725 0.9295 -1.1458 0.042 Uiso 1 1 calc R . . H36B H -0.4849 0.9235 -1.2530 0.042 Uiso 1 1 calc R . . C37 C -0.2668(7) 0.81920(15) -0.3596(9) 0.0395(19) Uani 1 1 d . . . H37A H -0.2892 0.8328 -0.4281 0.047 Uiso 1 1 calc R . . H37B H -0.2932 0.8232 -0.3167 0.047 Uiso 1 1 calc R . . C38 C -0.1596(8) 0.8207(2) -0.2513(11) 0.056(3) Uani 1 1 d . . . H38A H -0.1403 0.8384 -0.2179 0.083 Uiso 1 1 calc R . . H38B H -0.1318 0.8154 -0.2900 0.083 Uiso 1 1 calc R . . H38C H -0.1366 0.8093 -0.1754 0.083 Uiso 1 1 calc R . . C39 C -0.2671(8) 0.77233(17) -0.3279(10) 0.048(2) Uani 1 1 d . . . H39A H -0.1984 0.7701 -0.2791 0.057 Uiso 1 1 calc R . . H39B H -0.2715 0.7775 -0.2598 0.057 Uiso 1 1 calc R . . C40 C -0.3184(12) 0.7467(2) -0.3910(14) 0.077(4) Uani 1 1 d U . . H40A H -0.2832 0.7331 -0.3214 0.116 Uiso 1 1 calc R . . H40B H -0.3215 0.7425 -0.4665 0.116 Uiso 1 1 calc R . . H40C H -0.3835 0.7479 -0.4255 0.116 Uiso 1 1 calc R . . C41 C -0.4175(6) 0.7951(2) -0.5343(10) 0.046(2) Uani 1 1 d . . . H41A H -0.4432 0.7787 -0.5861 0.055 Uiso 1 1 calc R . . H41B H -0.4392 0.8091 -0.6006 0.055 Uiso 1 1 calc R . . C42 C -0.4610(9) 0.7997(3) -0.4679(15) 0.077(4) Uani 1 1 d U . . H42A H -0.5311 0.8000 -0.5393 0.116 Uiso 1 1 calc R . . H42B H -0.4382 0.8162 -0.4195 0.116 Uiso 1 1 calc R . . H42C H -0.4410 0.7858 -0.4031 0.116 Uiso 1 1 calc R . . C43 C -0.4814(8) 0.88211(19) -1.3829(10) 0.051(2) Uani 1 1 d . . . H43A H -0.4676 0.8748 -1.4377 0.061 Uiso 1 1 calc R . . H43B H -0.4684 0.8685 -1.3197 0.061 Uiso 1 1 calc R . . C44 C -0.5868(9) 0.8889(3) -1.4786(11) 0.069(3) Uani 1 1 d . . . H44A H -0.6253 0.8734 -1.5251 0.103 Uiso 1 1 calc R . . H44B H -0.6019 0.9014 -1.5467 0.103 Uiso 1 1 calc R . . H44C H -0.6015 0.8965 -1.4261 0.103 Uiso 1 1 calc R . . C45 C -0.4358(8) 0.92642(19) -1.3961(10) 0.050(2) Uani 1 1 d . . . H45A H -0.4378 0.9190 -1.4673 0.060 Uiso 1 1 calc R . . H45B H -0.5009 0.9329 -1.4424 0.060 Uiso 1 1 calc R . . C46 C -0.3700(9) 0.9485(2) -1.3344(12) 0.058(3) Uani 1 1 d . . . H46A H -0.3915 0.9610 -1.4057 0.087 Uiso 1 1 calc R . . H46B H -0.3053 0.9426 -1.2898 0.087 Uiso 1 1 calc R . . H46C H -0.3694 0.9566 -1.2665 0.087 Uiso 1 1 calc R . . C47 C -0.3099(8) 0.89537(18) -1.2147(11) 0.049(2) Uani 1 1 d . . . H47A H -0.2662 0.9096 -1.1537 0.059 Uiso 1 1 calc R . . H47B H -0.2981 0.8810 -1.1559 0.059 Uiso 1 1 calc R . . C48 C -0.2844(9) 0.8867(2) -1.2960(12) 0.060(3) Uani 1 1 d . . . H48A H -0.2152 0.8887 -1.2408 0.090 Uiso 1 1 calc R . . H48B H -0.3192 0.8971 -1.3790 0.090 Uiso 1 1 calc R . . H48C H -0.3020 0.8685 -1.3211 0.090 Uiso 1 1 calc R . . C49 C -0.0845(7) 0.82322(16) -0.6392(9) 0.0366(18) Uani 1 1 d . . . H49 H -0.1344 0.8150 -0.6500 0.044 Uiso 1 1 calc R . . C50 C -0.0146(8) 0.80801(18) -0.6197(9) 0.045(2) Uani 1 1 d . . . C51 C 0.0571(8) 0.8205(2) -0.6033(12) 0.055(2) Uani 1 1 d . . . H51 H 0.1066 0.8109 -0.5880 0.066 Uiso 1 1 calc R . . C52 C 0.0574(8) 0.8470(2) -0.6091(12) 0.054(2) Uani 1 1 d . . . H52 H 0.1062 0.8557 -0.5996 0.065 Uiso 1 1 calc R . . C53 C -0.0125(6) 0.86052(14) -0.6284(9) 0.0386(19) Uani 1 1 d D . . C54 C -0.0146(6) 0.88942(14) -0.6324(8) 0.0394(19) Uani 1 1 d D . . C55 C 0.0565(6) 0.9030(2) -0.6145(10) 0.047(2) Uani 1 1 d . . . H55 H 0.1099 0.8943 -0.5925 0.056 Uiso 1 1 calc R . . C56 C 0.0484(6) 0.92992(17) -0.6296(10) 0.042(2) Uani 1 1 d . . . H56 H 0.0945 0.9397 -0.6221 0.051 Uiso 1 1 calc R . . C57 C -0.0300(7) 0.94188(17) -0.6561(9) 0.0387(19) Uani 1 1 d . . . C58 C -0.0960(6) 0.92689(16) -0.6707(8) 0.0316(17) Uani 1 1 d . . . H58 H -0.1500 0.9350 -0.6921 0.038 Uiso 1 1 calc R . . C59 C -0.0112(8) 0.77931(18) -0.5998(11) 0.051(2) Uani 1 1 d . . . H59A H -0.0362 0.7756 -0.5547 0.061 Uiso 1 1 calc R . . H59B H 0.0566 0.7737 -0.5368 0.061 Uiso 1 1 calc R . . C60 C -0.0467(7) 0.97028(16) -0.6899(9) 0.043(2) Uani 1 1 d . . . H60A H -0.1165 0.9736 -0.7534 0.051 Uiso 1 1 calc R . . H60B H -0.0249 0.9746 -0.7388 0.051 Uiso 1 1 calc R . . C61 C -0.1709(7) 0.7667(2) -0.8147(11) 0.057(3) Uani 1 1 d . . . H61A H -0.2039 0.7573 -0.9015 0.068 Uiso 1 1 calc R . . H61B H -0.1859 0.7852 -0.8375 0.068 Uiso 1 1 calc R . . C62 C -0.2127(10) 0.7578(3) -0.7538(19) 0.086(4) Uani 1 1 d . . . H62A H -0.2814 0.7616 -0.8176 0.130 Uiso 1 1 calc R . . H62B H -0.1806 0.7668 -0.6673 0.130 Uiso 1 1 calc R . . H62C H -0.2029 0.7392 -0.7370 0.130 Uiso 1 1 calc R . . C63 C -0.0410(11) 0.7355(2) -0.6879(18) 0.087(4) Uani 1 1 d U . . H63A H -0.0897 0.7244 -0.7674 0.105 Uiso 1 1 calc R . . H63B H -0.0418 0.7317 -0.6149 0.105 Uiso 1 1 calc R . . C64 C 0.0590(13) 0.7288(3) -0.6361(18) 0.107(6) Uani 1 1 d . . . H64A H 0.0715 0.7104 -0.6152 0.160 Uiso 1 1 calc R . . H64B H 0.1081 0.7388 -0.5534 0.160 Uiso 1 1 calc R . . H64C H 0.0609 0.7331 -0.7070 0.160 Uiso 1 1 calc R . . C65 C -0.0388(9) 0.7719(3) -0.8113(13) 0.071(3) Uani 1 1 d . . . H65A H -0.0545 0.7904 -0.8324 0.085 Uiso 1 1 calc R . . H65B H 0.0317 0.7703 -0.7500 0.085 Uiso 1 1 calc R . . C66 C -0.0826(13) 0.7582(3) -0.9442(15) 0.090(5) Uani 1 1 d . . . H66A H -0.0589 0.7661 -0.9845 0.135 Uiso 1 1 calc R . . H66B H -0.1526 0.7597 -1.0080 0.135 Uiso 1 1 calc R . . H66C H -0.0645 0.7400 -0.9256 0.135 Uiso 1 1 calc R . . C67 C 0.1098(7) 0.9831(2) -0.4669(12) 0.059(3) Uani 1 1 d . . . H67A H 0.1330 0.9835 -0.5159 0.070 Uiso 1 1 calc R . . H67B H 0.1211 0.9655 -0.4294 0.070 Uiso 1 1 calc R . . C68 C 0.1691(10) 1.0024(3) -0.3469(17) 0.092(5) Uani 1 1 d . . . H68A H 0.2375 0.9985 -0.2891 0.138 Uiso 1 1 calc R . . H68B H 0.1508 1.0010 -0.2926 0.138 Uiso 1 1 calc R . . H68C H 0.1566 1.0199 -0.3830 0.138 Uiso 1 1 calc R . . C69 C -0.0199(9) 1.01566(19) -0.6239(12) 0.056(3) Uani 1 1 d . . . H69A H -0.0898 1.0171 -0.7017 0.068 Uiso 1 1 calc R . . H69B H -0.0027 1.0276 -0.5517 0.068 Uiso 1 1 calc R . . C70 C 0.0306(14) 1.0241(3) -0.6704(17) 0.085(4) Uani 1 1 d U . . H70A H 0.0271 1.0429 -0.6794 0.127 Uiso 1 1 calc R . . H70B H -0.0001 1.0163 -0.7590 0.127 Uiso 1 1 calc R . . H70C H 0.0979 1.0188 -0.6032 0.127 Uiso 1 1 calc R . . C71 C -0.0349(9) 0.9841(2) -0.4972(12) 0.057(3) Uani 1 1 d . . . H71A H -0.0228 0.9660 -0.4667 0.068 Uiso 1 1 calc R . . H71B H 0.0032 0.9950 -0.4142 0.068 Uiso 1 1 calc R . . C72 C -0.1372(10) 0.9896(3) -0.5768(18) 0.077(4) Uani 1 1 d . . . H72A H -0.1551 0.9838 -0.5254 0.116 Uiso 1 1 calc R . . H72B H -0.1761 0.9805 -0.6643 0.116 Uiso 1 1 calc R . . H72C H -0.1485 1.0081 -0.5936 0.116 Uiso 1 1 calc R . . Cl1 Cl -0.47409(16) 0.87386(4) -0.6919(2) 0.0409(5) Uani 1 1 d D . . O1 O -0.5259(7) 0.86909(15) -0.8320(8) 0.066(2) Uani 1 1 d . . . O2 O -0.4826(9) 0.85323(19) -0.6312(11) 0.093(3) Uani 1 1 d U . . O3 O -0.3757(7) 0.8747(4) -0.6185(17) 0.142(5) Uani 1 1 d DU . . O4 O -0.5115(13) 0.8959(2) -0.6817(14) 0.121(4) Uani 1 1 d U . . Cl5 Cl 0.1458(2) 0.92229(5) -0.2273(3) 0.0636(7) Uani 1 1 d . . . O17 O 0.0481(8) 0.9269(2) -0.3338(10) 0.086(3) Uani 1 1 d . . . O18 O 0.1973(10) 0.9423(3) -0.2224(19) 0.165(9) Uani 1 1 d . . . O19 O 0.1654(9) 0.91966(19) -0.1035(10) 0.102(4) Uani 1 1 d . . . O20 O 0.1572(13) 0.8976(3) -0.2666(17) 0.128(4) Uani 1 1 d U . . Cl7 Cl -0.2660(3) 0.82551(6) -1.0400(3) 0.0840(11) Uani 1 1 d D . . O25 O -0.2819(8) 0.81842(19) -0.9533(10) 0.080(2) Uani 1 1 d . . . O26 O -0.2383(10) 0.8037(2) -1.0690(12) 0.103(3) Uani 1 1 d U . . O27 O -0.1982(10) 0.8467(2) -0.9699(14) 0.113(4) Uani 1 1 d D . . O28 O -0.3515(7) 0.83589(19) -1.1693(9) 0.095(3) Uani 1 1 d DU . . Cl3 Cl -0.32911(16) 0.98006(4) -0.9960(2) 0.0436(5) Uani 1 1 d D . . O9 O -0.3127(6) 0.95579(12) -0.9311(8) 0.0582(19) Uani 1 1 d . . . O10 O -0.3233(11) 0.99981(18) -0.9198(12) 0.102(3) Uani 1 1 d DU . . O11 O -0.2583(9) 0.9841(3) -1.0020(15) 0.113(4) Uani 1 1 d . . . O12 O -0.4172(9) 0.9797(2) -1.1358(11) 0.110(5) Uani 1 1 d . . . Cl2 Cl -0.01824(16) 0.76431(4) -0.3176(2) 0.0482(5) Uani 1 1 d . . . O5 O -0.0516(5) 0.78897(11) -0.3856(7) 0.0495(16) Uani 1 1 d . . . O6 O 0.0816(6) 0.76324(15) -0.2254(9) 0.073(2) Uani 1 1 d . . . O7 O -0.0548(8) 0.74458(14) -0.4143(10) 0.090(3) Uani 1 1 d . . . O8 O -0.0505(8) 0.7606(2) -0.2475(12) 0.092(3) Uani 1 1 d . . . Cl4 Cl -0.06376(19) 0.92971(5) -0.9751(2) 0.0539(6) Uani 1 1 d . . . O13 O -0.1240(6) 0.93579(16) -1.1169(8) 0.067(2) Uani 1 1 d . . . O14 O -0.0141(7) 0.95221(16) -0.8946(8) 0.071(2) Uani 1 1 d . . . O15 O 0.0049(8) 0.9107(2) -0.9430(10) 0.092(3) Uani 1 1 d . . . O16 O -0.1189(8) 0.9194(3) -0.9473(9) 0.094(3) Uani 1 1 d . . . Cl6 Cl -0.6874(2) 0.95588(7) -1.4493(4) 0.0846(10) Uani 1 1 d D . . O21 O -0.6695(10) 0.9744(2) -1.3518(13) 0.152(6) Uani 1 1 d D . . O22 O -0.7730(6) 0.9633(3) -1.5772(10) 0.120(4) Uani 1 1 d DU . . O23 O -0.6111(6) 0.9562(2) -1.4433(12) 0.107(4) Uani 1 1 d DU . . O24 O -0.6972(10) 0.9318(2) -1.4119(15) 0.156(6) Uani 1 1 d DU . . Cl8 Cl -0.7157(3) 0.80616(8) -0.5619(4) 0.0911(11) Uani 1 1 d . . . O29 O -0.7748(8) 0.8286(2) -0.6139(13) 0.098(3) Uani 1 1 d . . . O30 O -0.7683(9) 0.7849(2) -0.5726(17) 0.122(4) Uani 1 1 d U . . O31 O -0.7015(8) 0.7987(3) -0.6472(12) 0.098(3) Uani 1 1 d . . . O32 O -0.6234(10) 0.8117(3) -0.4282(12) 0.122(5) Uani 1 1 d . . . O1W O -0.0416(12) 0.8582(3) -0.9524(15) 0.122(4) Uani 1 1 d U . . H1WA H -0.0045 0.8712 -0.9159 0.147 Uiso 1 1 d R . . H1WB H -0.0725 0.8561 -0.9267 0.147 Uiso 1 1 d R . . O2W O 0.0551(10) 0.8156(3) -0.9132(14) 0.116(4) Uani 1 1 d . . . H2WA H 0.0189 0.8284 -0.9361 0.140 Uiso 1 1 d R . . H2WB H 0.1057 0.8173 -0.8296 0.140 Uiso 1 1 d R . . O3W O 0.2694(11) 0.8873(4) -0.3357(16) 0.133(5) Uani 1 1 d U . . H3WA H 0.2506 0.8914 -0.2944 0.159 Uiso 1 1 d R . . H3WB H 0.3079 0.8979 -0.3267 0.159 Uiso 1 1 d R . . O4W O 0.3353(12) 0.8343(4) -0.2629(19) 0.147(5) Uani 1 1 d U . . H4WA H 0.3165 0.8498 -0.2870 0.176 Uiso 1 1 d R . . H4WB H 0.3468 0.8281 -0.3104 0.176 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0298(5) 0.0303(5) 0.0235(4) -0.0017(4) 0.0171(4) -0.0008(4) N1 0.029(3) 0.026(3) 0.027(3) -0.004(2) 0.017(3) -0.003(2) N2 0.039(4) 0.034(3) 0.023(3) 0.001(3) 0.023(3) 0.005(3) N3 0.025(3) 0.037(4) 0.039(4) 0.008(3) 0.013(3) 0.006(3) N4 0.035(4) 0.034(3) 0.043(4) 0.008(3) 0.026(3) 0.010(3) N5 0.029(3) 0.041(4) 0.031(3) 0.006(3) 0.024(3) 0.005(3) N6 0.029(3) 0.027(3) 0.026(3) -0.004(2) 0.019(3) -0.002(2) N7 0.051(4) 0.030(3) 0.036(4) 0.005(3) 0.029(3) -0.003(3) N8 0.058(5) 0.039(4) 0.034(4) -0.001(3) 0.033(3) -0.003(3) N9 0.038(4) 0.035(3) 0.025(3) -0.009(3) 0.020(3) -0.002(3) N10 0.028(3) 0.036(3) 0.026(3) -0.003(3) 0.019(3) -0.004(3) N11 0.059(5) 0.049(5) 0.069(5) -0.016(4) 0.042(5) 0.003(4) N12 0.046(4) 0.035(4) 0.041(4) -0.003(3) 0.029(3) -0.006(3) C1 0.035(4) 0.032(4) 0.031(4) -0.001(3) 0.019(4) 0.001(3) C2 0.028(4) 0.033(4) 0.025(4) -0.001(3) 0.013(3) 0.001(3) C3 0.030(4) 0.046(5) 0.026(4) 0.001(3) 0.017(3) -0.003(3) C4 0.038(4) 0.033(4) 0.035(4) -0.003(3) 0.027(4) 0.005(3) C5 0.031(4) 0.031(4) 0.032(4) 0.001(3) 0.021(3) -0.005(3) C6 0.025(4) 0.026(3) 0.037(4) -0.001(3) 0.022(3) -0.003(3) C7 0.044(5) 0.041(5) 0.035(4) -0.006(3) 0.031(4) -0.001(4) C8 0.044(4) 0.025(3) 0.040(4) 0.000(3) 0.031(4) 0.002(3) C9 0.028(4) 0.034(4) 0.034(4) 0.003(3) 0.020(3) 0.002(3) C10 0.034(4) 0.036(4) 0.033(4) 0.003(3) 0.026(3) 0.006(3) C11 0.036(4) 0.037(4) 0.024(4) 0.004(3) 0.017(3) 0.002(3) C12 0.033(4) 0.027(4) 0.045(4) 0.007(3) 0.028(4) 0.006(3) C13 0.043(5) 0.047(5) 0.065(6) 0.006(5) 0.035(5) 0.001(4) C14 0.078(8) 0.077(8) 0.070(7) -0.004(6) 0.056(7) -0.002(6) C15 0.048(6) 0.035(5) 0.042(5) 0.007(4) 0.005(4) 0.010(4) C16 0.045(6) 0.048(6) 0.119(12) 0.020(7) 0.026(7) 0.015(5) C17 0.042(5) 0.026(4) 0.052(6) 0.001(4) 0.016(4) -0.004(3) C18 0.081(8) 0.044(6) 0.047(6) -0.008(5) 0.014(6) 0.000(5) C19 0.055(5) 0.045(5) 0.056(5) -0.008(4) 0.043(5) -0.002(4) C20 0.048(6) 0.092(8) 0.076(7) -0.015(7) 0.047(6) 0.001(6) C21 0.049(6) 0.041(5) 0.091(8) 0.038(6) 0.040(6) 0.021(4) C22 0.081(9) 0.086(9) 0.085(9) 0.035(8) 0.051(8) 0.022(7) C23 0.045(5) 0.038(4) 0.047(5) -0.003(4) 0.028(4) 0.000(4) C24 0.061(7) 0.092(9) 0.052(6) -0.022(6) 0.034(5) 0.000(6) C25 0.032(4) 0.038(4) 0.033(4) 0.003(3) 0.025(3) 0.002(3) C26 0.034(4) 0.025(3) 0.038(4) -0.005(3) 0.027(4) -0.003(3) C27 0.044(5) 0.035(4) 0.037(4) -0.002(3) 0.030(4) -0.006(3) C28 0.036(4) 0.041(4) 0.037(4) -0.001(4) 0.025(4) -0.006(3) C29 0.033(4) 0.026(3) 0.028(4) -0.005(3) 0.020(3) -0.004(3) C30 0.042(5) 0.037(4) 0.032(4) 0.004(3) 0.027(4) 0.002(3) C31 0.029(4) 0.057(5) 0.030(4) 0.004(4) 0.016(3) -0.005(4) C32 0.027(4) 0.056(5) 0.028(4) 0.004(3) 0.017(3) 0.000(3) C33 0.045(5) 0.032(4) 0.028(4) 0.002(3) 0.027(4) 0.000(3) C34 0.036(4) 0.028(4) 0.034(4) -0.002(3) 0.027(4) -0.003(3) C35 0.036(4) 0.028(4) 0.041(4) -0.001(3) 0.028(4) -0.002(3) C36 0.043(4) 0.033(4) 0.029(4) 0.004(3) 0.024(3) 0.007(3) C37 0.054(5) 0.027(4) 0.046(5) -0.007(3) 0.037(4) -0.008(3) C38 0.067(7) 0.050(6) 0.051(6) -0.017(4) 0.040(5) -0.016(5) C39 0.072(6) 0.034(4) 0.041(5) 0.008(4) 0.039(5) -0.002(4) C40 0.114(8) 0.041(5) 0.065(6) 0.005(4) 0.055(5) -0.010(5) C41 0.030(4) 0.070(6) 0.049(5) -0.001(4) 0.032(4) -0.009(4) C42 0.057(6) 0.111(8) 0.094(7) 0.006(6) 0.064(5) -0.010(5) C43 0.068(6) 0.046(5) 0.041(5) -0.010(4) 0.037(5) -0.009(4) C44 0.064(7) 0.074(7) 0.035(5) -0.012(5) 0.019(5) -0.020(6) C45 0.073(7) 0.042(5) 0.051(5) 0.013(4) 0.048(5) 0.009(4) C46 0.090(8) 0.042(5) 0.060(6) 0.010(4) 0.057(6) 0.003(5) C47 0.065(6) 0.038(4) 0.052(5) 0.012(4) 0.043(5) 0.007(4) C48 0.079(7) 0.048(5) 0.059(6) 0.014(5) 0.048(6) 0.014(5) C49 0.050(5) 0.030(4) 0.045(5) -0.005(3) 0.038(4) 0.000(3) C50 0.056(5) 0.036(4) 0.038(5) -0.004(4) 0.029(4) 0.001(4) C51 0.050(5) 0.054(6) 0.074(7) 0.004(5) 0.047(5) 0.008(5) C52 0.047(5) 0.049(5) 0.077(7) -0.005(5) 0.046(5) 0.002(4) C53 0.040(4) 0.037(4) 0.037(4) -0.001(3) 0.025(4) 0.001(4) C54 0.036(4) 0.042(5) 0.033(4) 0.002(3) 0.021(3) 0.007(4) C55 0.029(4) 0.062(6) 0.057(5) -0.006(4) 0.032(4) 0.002(4) C56 0.036(4) 0.042(5) 0.055(5) -0.010(4) 0.033(4) -0.011(4) C57 0.048(5) 0.036(4) 0.036(4) -0.010(3) 0.030(4) -0.016(4) C58 0.030(4) 0.038(4) 0.032(4) 0.002(3) 0.023(3) 0.007(3) C59 0.062(6) 0.041(5) 0.056(6) -0.002(4) 0.042(5) 0.010(4) C60 0.046(5) 0.037(4) 0.041(5) -0.006(4) 0.028(4) -0.005(4) C61 0.049(6) 0.063(6) 0.063(6) -0.013(5) 0.040(5) 0.005(5) C62 0.061(8) 0.093(10) 0.119(12) 0.014(9) 0.066(8) 0.010(7) C63 0.085(7) 0.051(6) 0.106(8) -0.020(6) 0.055(6) 0.005(5) C64 0.112(12) 0.080(10) 0.091(11) 0.007(8) 0.052(9) 0.050(9) C65 0.057(6) 0.105(9) 0.072(7) -0.026(7) 0.053(6) -0.011(6) C66 0.112(12) 0.071(8) 0.067(8) -0.015(6) 0.052(8) 0.015(8) C67 0.041(5) 0.052(6) 0.072(7) -0.025(5) 0.033(5) -0.012(4) C68 0.056(7) 0.090(9) 0.092(10) -0.056(8) 0.033(7) -0.030(7) C69 0.082(7) 0.037(5) 0.061(6) 0.004(4) 0.052(6) 0.003(5) C70 0.130(9) 0.068(7) 0.091(7) 0.004(5) 0.088(7) -0.007(6) C71 0.089(8) 0.046(5) 0.064(6) -0.008(5) 0.063(6) -0.013(5) C72 0.081(9) 0.062(7) 0.124(11) -0.025(7) 0.084(9) -0.017(6) Cl1 0.0576(12) 0.0291(9) 0.0503(11) -0.0048(8) 0.0420(10) -0.0041(8) O1 0.097(6) 0.055(4) 0.057(4) 0.005(3) 0.056(4) 0.010(4) O2 0.131(7) 0.058(4) 0.078(5) 0.011(4) 0.065(5) -0.012(4) O3 0.112(8) 0.189(10) 0.143(9) -0.035(7) 0.093(7) -0.036(7) O4 0.192(9) 0.091(6) 0.108(6) 0.013(5) 0.113(6) 0.058(6) Cl5 0.0622(15) 0.0427(12) 0.0872(19) 0.0206(12) 0.0505(15) 0.0104(10) O17 0.090(7) 0.094(7) 0.069(5) 0.003(5) 0.050(5) -0.016(5) O18 0.102(9) 0.128(10) 0.171(14) 0.070(10) 0.052(9) -0.040(8) O19 0.121(8) 0.064(5) 0.060(5) 0.011(4) 0.035(5) 0.003(5) O20 0.162(9) 0.112(7) 0.146(8) 0.016(6) 0.119(7) 0.037(6) Cl7 0.141(3) 0.0644(17) 0.0769(19) 0.0247(15) 0.085(2) 0.0365(19) O25 0.098(6) 0.077(5) 0.074(5) 0.008(4) 0.061(5) 0.019(5) O26 0.161(8) 0.089(6) 0.102(6) 0.017(5) 0.106(6) 0.047(6) O27 0.134(10) 0.093(8) 0.112(9) -0.028(7) 0.082(8) -0.033(7) O28 0.118(7) 0.065(5) 0.079(5) 0.018(4) 0.056(5) 0.014(5) Cl3 0.0571(13) 0.0342(10) 0.0409(11) 0.0029(8) 0.0333(10) -0.0018(8) O9 0.097(6) 0.026(3) 0.064(4) 0.009(3) 0.059(4) 0.004(3) O10 0.165(8) 0.068(5) 0.101(6) 0.000(4) 0.101(6) 0.005(5) O11 0.086(7) 0.156(12) 0.125(9) 0.028(8) 0.082(7) 0.004(7) O12 0.102(8) 0.069(6) 0.069(6) 0.009(5) 0.019(5) 0.008(5) Cl2 0.0467(12) 0.0375(10) 0.0465(12) 0.0074(9) 0.0253(10) 0.0132(9) O5 0.055(4) 0.027(3) 0.052(4) 0.012(3) 0.029(3) 0.014(3) O6 0.049(4) 0.054(4) 0.077(5) 0.011(4) 0.026(4) 0.007(3) O7 0.103(7) 0.034(4) 0.073(5) -0.004(4) 0.034(5) 0.002(4) O8 0.112(8) 0.087(6) 0.122(8) 0.050(6) 0.096(7) 0.046(6) Cl4 0.0670(15) 0.0544(12) 0.0421(11) -0.0086(10) 0.0372(11) -0.0083(11) O13 0.084(5) 0.070(5) 0.045(4) -0.006(3) 0.042(4) -0.002(4) O14 0.100(6) 0.058(4) 0.054(4) -0.019(3) 0.051(4) -0.025(4) O15 0.090(6) 0.087(6) 0.075(6) -0.003(5) 0.046(5) 0.025(5) O16 0.090(6) 0.143(9) 0.057(5) -0.031(5) 0.052(5) -0.051(6) Cl6 0.0655(18) 0.0751(19) 0.113(3) 0.0016(18) 0.0598(19) -0.0005(14) O21 0.170(15) 0.125(11) 0.194(17) -0.052(12) 0.135(14) 0.004(10) O22 0.091(7) 0.152(9) 0.113(7) 0.025(6) 0.067(6) 0.016(6) O23 0.065(5) 0.110(7) 0.140(8) -0.013(6) 0.066(5) -0.003(4) O24 0.172(10) 0.160(10) 0.172(10) 0.015(8) 0.130(8) 0.008(8) Cl8 0.091(2) 0.101(3) 0.103(3) 0.038(2) 0.074(2) 0.031(2) O29 0.090(7) 0.092(7) 0.115(8) 0.036(6) 0.070(6) 0.027(6) O30 0.086(6) 0.078(6) 0.162(9) -0.008(6) 0.067(6) 0.013(5) O31 0.083(7) 0.135(9) 0.092(7) -0.013(7) 0.065(6) -0.013(6) O32 0.102(8) 0.164(12) 0.070(6) 0.002(7) 0.045(6) 0.047(9) O1W 0.152(9) 0.096(7) 0.120(8) -0.005(6) 0.091(6) -0.003(6) O2W 0.117(9) 0.129(11) 0.100(8) 0.003(7) 0.071(8) -0.020(8) O3W 0.105(7) 0.167(9) 0.130(8) -0.027(7) 0.080(6) -0.008(7) O4W 0.129(8) 0.175(10) 0.166(10) -0.057(8) 0.111(7) -0.037(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N10 2.144(6) . ? Zn1 N6 2.169(6) . ? Zn1 N9 2.172(7) . ? Zn1 N5 2.176(7) . ? Zn1 N1 2.189(6) . ? Zn1 N2 2.195(6) . ? N1 C1 1.357(11) . ? N1 C5 1.359(11) . ? N2 C10 1.330(11) . ? N2 C6 1.350(10) . ? N3 C13 1.514(15) . ? N3 C17 1.514(12) . ? N3 C11 1.533(11) . ? N3 C15 1.548(11) . ? N4 C19 1.513(13) . ? N4 C12 1.514(11) . ? N4 C23 1.523(12) . ? N4 C21 1.528(11) . ? N5 C25 1.332(11) . ? N5 C29 1.358(11) . ? N6 C30 1.333(11) . ? N6 C34 1.355(10) . ? N7 C37 1.507(11) . ? N7 C41 1.524(12) . ? N7 C39 1.534(11) . ? N7 C35 1.537(12) . ? N8 C47 1.514(14) . ? N8 C36 1.520(11) . ? N8 C43 1.532(12) . ? N8 C45 1.549(11) . ? N9 C53 1.345(12) . ? N9 C49 1.369(11) . ? N10 C54 1.330(11) . ? N10 C58 1.378(11) . ? N11 C61 1.471(14) . ? N11 C63 1.507(16) . ? N11 C59 1.516(14) . ? N11 C65 1.556(17) . ? N12 C67 1.515(13) . ? N12 C60 1.518(11) . ? N12 C71 1.521(13) . ? N12 C69 1.527(12) . ? C1 C2 1.356(12) . ? C1 H1 0.9500 . ? C2 C3 1.383(13) . ? C2 C11 1.523(11) . ? C3 C4 1.382(12) . ? C3 H3 0.9500 . ? C4 C5 1.385(12) . ? C4 H4 0.9500 . ? C5 C6 1.480(11) . ? C6 C7 1.377(12) . ? C7 C8 1.388(13) . ? C7 H7 0.9500 . ? C8 C9 1.397(13) . ? C8 H8 0.9500 . ? C9 C10 1.404(12) . ? C9 C12 1.510(11) . ? C10 H10 0.9500 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.509(17) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.511(18) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.50(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.487(15) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.44(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.477(17) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.404(12) . ? C25 H25 0.9500 . ? C26 C27 1.390(13) . ? C26 C35 1.493(12) . ? C27 C28 1.372(13) . ? C27 H27 0.9500 . ? C28 C29 1.393(12) . ? C28 H28 0.9500 . ? C29 C30 1.491(8) . ? C30 C31 1.386(12) . ? C31 C32 1.383(13) . ? C31 H31 0.9500 . ? C32 C33 1.400(13) . ? C32 H32 0.9500 . ? C33 C34 1.371(12) . ? C33 C36 1.516(11) . ? C34 H34 0.9500 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.500(15) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.527(15) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.562(15) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.515(18) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.469(16) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.504(16) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.401(14) . ? C49 H49 0.9500 . ? C50 C51 1.375(16) . ? C50 C59 1.510(14) . ? C51 C52 1.381(16) . ? C51 H51 0.9500 . ? C52 C53 1.353(14) . ? C52 H52 0.9500 . ? C53 C54 1.503(8) . ? C54 C55 1.383(14) . ? C55 C56 1.407(14) . ? C55 H55 0.9500 . ? C56 C57 1.410(14) . ? C56 H56 0.9500 . ? C57 C58 1.363(13) . ? C57 C60 1.514(13) . ? C58 H58 0.9500 . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.52(2) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.55(2) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.521(18) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C68 1.547(15) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C70 1.496(19) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C72 1.47(2) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? Cl1 O4 1.396(11) . ? Cl1 O3 1.399(9) . ? Cl1 O2 1.408(10) . ? Cl1 O1 1.417(8) . ? Cl5 O18 1.391(12) . ? Cl5 O17 1.395(11) . ? Cl5 O19 1.415(13) . ? Cl5 O20 1.452(15) . ? Cl7 O26 1.404(10) . ? Cl7 O25 1.406(11) . ? Cl7 O28 1.452(8) . ? Cl7 O27 1.453(8) . ? Cl3 O10 1.387(8) . ? Cl3 O11 1.397(11) . ? Cl3 O12 1.432(11) . ? Cl3 O9 1.437(7) . ? Cl2 O6 1.395(9) . ? Cl2 O7 1.405(9) . ? Cl2 O8 1.413(10) . ? Cl2 O5 1.445(6) . ? Cl4 O16 1.412(10) . ? Cl4 O13 1.428(8) . ? Cl4 O14 1.428(8) . ? Cl4 O15 1.445(11) . ? Cl6 O23 1.380(8) . ? Cl6 O22 1.395(8) . ? Cl6 O24 1.402(9) . ? Cl6 O21 1.452(8) . ? Cl8 O31 1.372(12) . ? Cl8 O30 1.423(15) . ? Cl8 O29 1.430(11) . ? Cl8 O32 1.450(14) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8499 . ? O2W H2WB 0.8499 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8499 . ? O4W H4WA 0.8501 . ? O4W H4WB 0.8500 . ? 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 N10 Zn1 N6 98.7(2) . . ? N10 Zn1 N9 76.0(3) . . ? N6 Zn1 N9 103.6(2) . . ? N10 Zn1 N5 167.5(3) . . ? N6 Zn1 N5 77.0(2) . . ? N9 Zn1 N5 93.4(3) . . ? N10 Zn1 N1 95.8(2) . . ? N6 Zn1 N1 161.5(2) . . ? N9 Zn1 N1 90.9(2) . . ? N5 Zn1 N1 91.0(2) . . ? N10 Zn1 N2 93.4(3) . . ? N6 Zn1 N2 92.0(2) . . ? N9 Zn1 N2 162.2(2) . . ? N5 Zn1 N2 98.4(3) . . ? N1 Zn1 N2 75.7(2) . . ? C1 N1 C5 117.5(7) . . ? C1 N1 Zn1 126.9(5) . . ? C5 N1 Zn1 115.6(5) . . ? C10 N2 C6 117.9(7) . . ? C10 N2 Zn1 126.3(5) . . ? C6 N2 Zn1 115.6(5) . . ? C13 N3 C17 108.3(8) . . ? C13 N3 C11 110.7(7) . . ? C17 N3 C11 110.8(7) . . ? C13 N3 C15 111.1(8) . . ? C17 N3 C15 110.6(7) . . ? C11 N3 C15 105.4(7) . . ? C19 N4 C12 109.2(7) . . ? C19 N4 C23 108.3(7) . . ? C12 N4 C23 111.0(7) . . ? C19 N4 C21 108.7(8) . . ? C12 N4 C21 107.5(7) . . ? C23 N4 C21 112.0(8) . . ? C25 N5 C29 118.0(7) . . ? C25 N5 Zn1 127.9(5) . . ? C29 N5 Zn1 114.0(5) . . ? C30 N6 C34 117.9(6) . . ? C30 N6 Zn1 114.5(5) . . ? C34 N6 Zn1 126.9(5) . . ? C37 N7 C41 110.0(7) . . ? C37 N7 C39 108.9(7) . . ? C41 N7 C39 112.9(7) . . ? C37 N7 C35 109.9(7) . . ? C41 N7 C35 108.2(7) . . ? C39 N7 C35 106.9(7) . . ? C47 N8 C36 107.8(7) . . ? C47 N8 C43 109.7(7) . . ? C36 N8 C43 113.0(7) . . ? C47 N8 C45 110.7(7) . . ? C36 N8 C45 107.0(7) . . ? C43 N8 C45 108.7(7) . . ? C53 N9 C49 117.0(7) . . ? C53 N9 Zn1 115.8(5) . . ? C49 N9 Zn1 127.1(6) . . ? C54 N10 C58 117.5(7) . . ? C54 N10 Zn1 116.5(5) . . ? C58 N10 Zn1 126.0(5) . . ? C61 N11 C63 109.7(10) . . ? C61 N11 C59 111.2(8) . . ? C63 N11 C59 108.2(10) . . ? C61 N11 C65 108.8(10) . . ? C63 N11 C65 110.3(11) . . ? C59 N11 C65 108.7(9) . . ? C67 N12 C60 109.7(7) . . ? C67 N12 C71 108.6(9) . . ? C60 N12 C71 110.5(7) . . ? C67 N12 C69 111.8(8) . . ? C60 N12 C69 107.0(7) . . ? C71 N12 C69 109.2(8) . . ? C2 C1 N1 124.5(8) . . ? C2 C1 H1 117.8 . . ? N1 C1 H1 117.8 . . ? C1 C2 C3 118.0(8) . . ? C1 C2 C11 120.6(7) . . ? C3 C2 C11 120.8(7) . . ? C4 C3 C2 119.1(7) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 120.2(8) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? N1 C5 C4 120.7(7) . . ? N1 C5 C6 116.4(7) . . ? C4 C5 C6 122.7(7) . . ? N2 C6 C7 122.5(7) . . ? N2 C6 C5 116.6(7) . . ? C7 C6 C5 121.0(7) . . ? C6 C7 C8 119.0(8) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? C7 C8 C9 120.1(7) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 C10 116.1(7) . . ? C8 C9 C12 122.3(7) . . ? C10 C9 C12 121.3(8) . . ? N2 C10 C9 124.5(7) . . ? N2 C10 H10 117.8 . . ? C9 C10 H10 117.8 . . ? C2 C11 N3 116.7(7) . . ? C2 C11 H11A 108.1 . . ? N3 C11 H11A 108.1 . . ? C2 C11 H11B 108.1 . . ? N3 C11 H11B 108.1 . . ? H11A C11 H11B 107.3 . . ? C9 C12 N4 117.0(7) . . ? C9 C12 H12A 108.0 . . ? N4 C12 H12A 108.0 . . ? C9 C12 H12B 108.0 . . ? N4 C12 H12B 108.0 . . ? H12A C12 H12B 107.3 . . ? C14 C13 N3 116.5(9) . . ? C14 C13 H13A 108.2 . . ? N3 C13 H13A 108.2 . . ? C14 C13 H13B 108.2 . . ? N3 C13 H13B 108.2 . . ? H13A C13 H13B 107.3 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 N3 113.5(10) . . ? C16 C15 H15A 108.9 . . ? N3 C15 H15A 108.9 . . ? C16 C15 H15B 108.9 . . ? N3 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 N3 116.1(9) . . ? C18 C17 H17A 108.3 . . ? N3 C17 H17A 108.3 . . ? C18 C17 H17B 108.3 . . ? N3 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 N4 117.9(9) . . ? C20 C19 H19A 107.8 . . ? N4 C19 H19A 107.8 . . ? C20 C19 H19B 107.8 . . ? N4 C19 H19B 107.8 . . ? H19A C19 H19B 107.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 N4 123.2(11) . . ? C22 C21 H21A 106.5 . . ? N4 C21 H21A 106.5 . . ? C22 C21 H21B 106.5 . . ? N4 C21 H21B 106.5 . . ? H21A C21 H21B 106.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 N4 115.9(9) . . ? C24 C23 H23A 108.3 . . ? N4 C23 H23A 108.3 . . ? C24 C23 H23B 108.3 . . ? N4 C23 H23B 108.3 . . ? H23A C23 H23B 107.4 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 C26 124.5(7) . . ? N5 C25 H25 117.8 . . ? C26 C25 H25 117.8 . . ? C27 C26 C25 116.1(7) . . ? C27 C26 C35 122.7(7) . . ? C25 C26 C35 121.0(7) . . ? C28 C27 C26 120.5(8) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 119.6(8) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? N5 C29 C28 121.2(7) . . ? N5 C29 C30 116.4(7) . . ? C28 C29 C30 122.4(7) . . ? N6 C30 C31 122.2(7) . . ? N6 C30 C29 116.8(7) . . ? C31 C30 C29 121.0(8) . . ? C32 C31 C30 118.8(8) . . ? C32 C31 H31 120.6 . . ? C30 C31 H31 120.6 . . ? C31 C32 C33 120.0(7) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C34 C33 C32 116.6(7) . . ? C34 C33 C36 122.1(8) . . ? C32 C33 C36 121.1(7) . . ? N6 C34 C33 124.3(7) . . ? N6 C34 H34 117.9 . . ? C33 C34 H34 117.9 . . ? C26 C35 N7 115.6(6) . . ? C26 C35 H35A 108.4 . . ? N7 C35 H35A 108.4 . . ? C26 C35 H35B 108.4 . . ? N7 C35 H35B 108.4 . . ? H35A C35 H35B 107.4 . . ? C33 C36 N8 113.8(7) . . ? C33 C36 H36A 108.8 . . ? N8 C36 H36A 108.8 . . ? C33 C36 H36B 108.8 . . ? N8 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? C38 C37 N7 116.4(8) . . ? C38 C37 H37A 108.2 . . ? N7 C37 H37A 108.2 . . ? C38 C37 H37B 108.2 . . ? N7 C37 H37B 108.2 . . ? H37A C37 H37B 107.3 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 N7 113.2(8) . . ? C40 C39 H39A 108.9 . . ? N7 C39 H39A 108.9 . . ? C40 C39 H39B 108.9 . . ? N7 C39 H39B 108.9 . . ? H39A C39 H39B 107.7 . . ? 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 . . ? N7 C41 C42 114.8(9) . . ? N7 C41 H41A 108.6 . . ? C42 C41 H41A 108.6 . . ? N7 C41 H41B 108.6 . . ? C42 C41 H41B 108.6 . . ? H41A C41 H41B 107.5 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 N8 115.3(9) . . ? C44 C43 H43A 108.4 . . ? N8 C43 H43A 108.4 . . ? C44 C43 H43B 108.4 . . ? N8 C43 H43B 108.4 . . ? H43A C43 H43B 107.5 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 N8 116.6(8) . . ? C46 C45 H45A 108.1 . . ? N8 C45 H45A 108.1 . . ? C46 C45 H45B 108.1 . . ? N8 C45 H45B 108.1 . . ? H45A C45 H45B 107.3 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 N8 115.5(9) . . ? C48 C47 H47A 108.4 . . ? N8 C47 H47A 108.4 . . ? C48 C47 H47B 108.4 . . ? N8 C47 H47B 108.4 . . ? H47A C47 H47B 107.5 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N9 C49 C50 122.7(8) . . ? N9 C49 H49 118.7 . . ? C50 C49 H49 118.7 . . ? C51 C50 C49 117.3(9) . . ? C51 C50 C59 121.2(10) . . ? C49 C50 C59 121.0(9) . . ? C50 C51 C52 120.3(9) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C53 C52 C51 119.2(9) . . ? C53 C52 H52 120.4 . . ? C51 C52 H52 120.4 . . ? N9 C53 C52 123.5(8) . . ? N9 C53 C54 114.9(7) . . ? C52 C53 C54 121.6(8) . . ? N10 C54 C55 123.4(8) . . ? N10 C54 C53 116.2(8) . . ? C55 C54 C53 120.4(8) . . ? C54 C55 C56 118.9(8) . . ? C54 C55 H55 120.5 . . ? C56 C55 H55 120.5 . . ? C55 C56 C57 118.0(8) . . ? C55 C56 H56 121.0 . . ? C57 C56 H56 121.0 . . ? C58 C57 C56 118.8(8) . . ? C58 C57 C60 121.7(9) . . ? C56 C57 C60 118.7(8) . . ? C57 C58 N10 123.3(7) . . ? C57 C58 H58 118.4 . . ? N10 C58 H58 118.4 . . ? C50 C59 N11 115.6(9) . . ? C50 C59 H59A 108.4 . . ? N11 C59 H59A 108.4 . . ? C50 C59 H59B 108.4 . . ? N11 C59 H59B 108.4 . . ? H59A C59 H59B 107.4 . . ? C57 C60 N12 115.5(7) . . ? C57 C60 H60A 108.4 . . ? N12 C60 H60A 108.4 . . ? C57 C60 H60B 108.4 . . ? N12 C60 H60B 108.4 . . ? H60A C60 H60B 107.5 . . ? N11 C61 C62 116.3(11) . . ? N11 C61 H61A 108.2 . . ? C62 C61 H61A 108.2 . . ? N11 C61 H61B 108.2 . . ? C62 C61 H61B 108.2 . . ? H61A C61 H61B 107.4 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N11 C63 C64 112.3(13) . . ? N11 C63 H63A 109.2 . . ? C64 C63 H63A 109.2 . . ? N11 C63 H63B 109.2 . . ? C64 C63 H63B 109.2 . . ? H63A C63 H63B 107.9 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 N11 119.5(12) . . ? C66 C65 H65A 107.4 . . ? N11 C65 H65A 107.4 . . ? C66 C65 H65B 107.4 . . ? N11 C65 H65B 107.4 . . ? H65A C65 H65B 107.0 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N12 C67 C68 114.1(9) . . ? N12 C67 H67A 108.7 . . ? C68 C67 H67A 108.7 . . ? N12 C67 H67B 108.7 . . ? C68 C67 H67B 108.7 . . ? H67A C67 H67B 107.6 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C70 C69 N12 114.8(10) . . ? C70 C69 H69A 108.6 . . ? N12 C69 H69A 108.6 . . ? C70 C69 H69B 108.6 . . ? N12 C69 H69B 108.6 . . ? H69A C69 H69B 107.6 . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C72 C71 N12 117.2(10) . . ? C72 C71 H71A 108.0 . . ? N12 C71 H71A 108.0 . . ? C72 C71 H71B 108.0 . . ? N12 C71 H71B 108.0 . . ? H71A C71 H71B 107.3 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? O4 Cl1 O3 115.0(11) . . ? O4 Cl1 O2 108.5(9) . . ? O3 Cl1 O2 103.2(10) . . ? O4 Cl1 O1 108.4(7) . . ? O3 Cl1 O1 110.2(8) . . ? O2 Cl1 O1 111.4(6) . . ? O18 Cl5 O17 108.9(8) . . ? O18 Cl5 O19 112.3(11) . . ? O17 Cl5 O19 109.2(8) . . ? O18 Cl5 O20 114.5(13) . . ? O17 Cl5 O20 101.6(9) . . ? O19 Cl5 O20 109.7(8) . . ? O26 Cl7 O25 108.9(6) . . ? O26 Cl7 O28 107.6(7) . . ? O25 Cl7 O28 112.4(7) . . ? O26 Cl7 O27 117.4(9) . . ? O25 Cl7 O27 104.7(7) . . ? O28 Cl7 O27 106.0(8) . . ? O10 Cl3 O11 108.0(9) . . ? O10 Cl3 O12 113.7(8) . . ? O11 Cl3 O12 104.7(9) . . ? O10 Cl3 O9 109.8(6) . . ? O11 Cl3 O9 109.5(7) . . ? O12 Cl3 O9 110.9(6) . . ? O6 Cl2 O7 108.5(6) . . ? O6 Cl2 O8 109.8(7) . . ? O7 Cl2 O8 109.2(8) . . ? O6 Cl2 O5 110.4(5) . . ? O7 Cl2 O5 109.9(5) . . ? O8 Cl2 O5 109.1(5) . . ? O16 Cl4 O13 110.2(6) . . ? O16 Cl4 O14 110.4(6) . . ? O13 Cl4 O14 110.0(5) . . ? O16 Cl4 O15 109.2(8) . . ? O13 Cl4 O15 107.8(6) . . ? O14 Cl4 O15 109.3(7) . . ? O23 Cl6 O22 112.3(6) . . ? O23 Cl6 O24 111.4(6) . . ? O22 Cl6 O24 110.8(6) . . ? O23 Cl6 O21 108.8(6) . . ? O22 Cl6 O21 106.5(6) . . ? O24 Cl6 O21 106.9(6) . . ? O31 Cl8 O30 101.6(9) . . ? O31 Cl8 O29 110.5(8) . . ? O30 Cl8 O29 108.8(7) . . ? O31 Cl8 O32 108.6(8) . . ? O30 Cl8 O32 117.4(10) . . ? O29 Cl8 O32 109.6(9) . . ? H1WA O1W H1WB 113.2 . . ? H2WA O2W H2WB 108.1 . . ? H3WA O3W H3WB 115.1 . . ? H4WA O4W H4WB 109.4 . . ? 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 O1W H1WA O15 0.85 2.12 2.846(19) 143.7 . O1W H1WB O27 0.85 2.08 2.85(2) 150.5 . O2W H2WA O1W 0.85 1.85 2.69(2) 169.2 . O2W H2WB O29 0.85 2.22 3.057(19) 169.5 1_655 O3W H3WA O20 0.85 2.04 2.84(2) 158.1 . O3W H3WB O24 0.85 2.06 2.75(2) 138.8 1_656 O4W H4WA O3W 0.85 2.06 2.91(3) 175.9 . O4W H4WB O32 0.85 2.14 2.99(2) 178.9 1_655 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 62.41 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.532 _refine_diff_density_min -0.889 _refine_diff_density_rms 0.116 # Attachment 'revised cif for complex 2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 627516' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H129 Br Cl5 N8 O20.50 Zn' _chemical_formula_weight 1757.36 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 17.340(3) _cell_length_b 37.132(6) _cell_length_c 13.715(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8830(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3724 _exptl_absorpt_coefficient_mu 0.950 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7571 _exptl_absorpt_correction_T_max 0.8254 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 53915 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -47 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 27.00 _reflns_number_total 16656 _reflns_number_gt 13777 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 1998' _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^)+(0.0920P)^2^+9.8482P] 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 0.048(10) _refine_ls_number_reflns 16656 _refine_ls_number_parameters 1023 _refine_ls_number_restraints 174 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1652 _refine_ls_wR_factor_gt 0.1515 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.074 _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 Zn1 Zn -0.55969(3) -0.118497(13) -0.52506(5) 0.02992(13) Uani 1 1 d . . . Br1 Br -0.51005(3) -0.125355(18) -0.68535(5) 0.04982(16) Uani 1 1 d . . . N1 N -0.5526(2) -0.07074(10) -0.4425(3) 0.0260(8) Uani 1 1 d . . . N2 N -0.4507(2) -0.12378(11) -0.4506(4) 0.0353(10) Uani 1 1 d . . . N3 N -0.7271(2) 0.01886(10) -0.3424(3) 0.0282(8) Uani 1 1 d . . . N4 N -0.2130(2) -0.17964(11) -0.5076(3) 0.0332(9) Uani 1 1 d . . . N5 N -0.6802(2) -0.11598(10) -0.5632(3) 0.0283(9) Uani 1 1 d . . . N6 N -0.6095(2) -0.15852(10) -0.4351(3) 0.0328(9) Uani 1 1 d . . . N7 N -0.8152(2) -0.09829(11) -0.8495(3) 0.0331(9) Uani 1 1 d . . . N8 N -0.5398(3) -0.21686(11) -0.1455(4) 0.0463(12) Uani 1 1 d . . . C1 C -0.4358(3) -0.09854(13) -0.3841(4) 0.0312(10) Uani 1 1 d . . . C2 C -0.3674(3) -0.09823(14) -0.3317(4) 0.0340(11) Uani 1 1 d . . . H2 H -0.3572 -0.0798 -0.2855 0.041 Uiso 1 1 calc R . . C3 C -0.3145(3) -0.12530(14) -0.3484(4) 0.0370(12) Uani 1 1 d . . . H3 H -0.2676 -0.1257 -0.3125 0.044 Uiso 1 1 calc R . . C4 C -0.3291(3) -0.15204(13) -0.4173(4) 0.0304(10) Uani 1 1 d . . . C5 C -0.3983(3) -0.14979(14) -0.4678(4) 0.0335(11) Uani 1 1 d . . . H5 H -0.4091 -0.1673 -0.5164 0.040 Uiso 1 1 calc R . . C6 C -0.4956(2) -0.06973(12) -0.3755(4) 0.0266(9) Uani 1 1 d . . . C7 C -0.4922(3) -0.04317(14) -0.3055(4) 0.0339(11) Uani 1 1 d . . . H7 H -0.4541 -0.0442 -0.2557 0.041 Uiso 1 1 calc R . . C8 C -0.5443(3) -0.01506(13) -0.3077(4) 0.0339(11) Uani 1 1 d . . . H8 H -0.5419 0.0037 -0.2606 0.041 Uiso 1 1 calc R . . C9 C -0.6006(3) -0.01467(13) -0.3805(4) 0.0282(10) Uani 1 1 d . . . C10 C -0.6030(3) -0.04362(12) -0.4439(4) 0.0283(9) Uani 1 1 d . . . H10 H -0.6429 -0.0442 -0.4912 0.034 Uiso 1 1 calc R . . C11 C -0.2779(3) -0.18398(14) -0.4327(4) 0.0337(11) Uani 1 1 d . . . H11A H -0.3105 -0.2045 -0.4530 0.040 Uiso 1 1 calc R . . H11B H -0.2543 -0.1904 -0.3692 0.040 Uiso 1 1 calc R . . C12 C -0.1558(3) -0.15084(15) -0.4764(5) 0.0411(13) Uani 1 1 d . . . H12A H -0.1182 -0.1474 -0.5299 0.049 Uiso 1 1 calc R . . H12B H -0.1842 -0.1279 -0.4684 0.049 Uiso 1 1 calc R . . C13 C -0.1112(3) -0.15805(18) -0.3833(5) 0.0494(15) Uani 1 1 d . . . H13A H -0.1478 -0.1628 -0.3294 0.059 Uiso 1 1 calc R . . H13B H -0.0786 -0.1797 -0.3919 0.059 Uiso 1 1 calc R . . C14 C -0.0610(5) -0.1263(2) -0.3573(8) 0.073(2) Uani 1 1 d . . . H14A H -0.0942 -0.1060 -0.3366 0.087 Uiso 1 1 calc R . . H14B H -0.0322 -0.1186 -0.4161 0.087 Uiso 1 1 calc R . . C15 C -0.0034(5) -0.1347(3) -0.2758(8) 0.085(3) Uani 1 1 d . . . H15A H 0.0273 -0.1132 -0.2617 0.128 Uiso 1 1 calc R . . H15B H 0.0307 -0.1543 -0.2965 0.128 Uiso 1 1 calc R . . H15C H -0.0315 -0.1420 -0.2170 0.128 Uiso 1 1 calc R . . C16 C -0.2443(3) -0.16780(15) -0.6068(4) 0.0411(13) Uani 1 1 d . . . H16A H -0.2760 -0.1459 -0.5971 0.049 Uiso 1 1 calc R . . H16B H -0.2000 -0.1610 -0.6485 0.049 Uiso 1 1 calc R . . C17 C -0.2919(3) -0.19497(16) -0.6611(4) 0.0443(13) Uani 1 1 d . . . H17A H -0.3394 -0.2004 -0.6238 0.053 Uiso 1 1 calc R . . H17B H -0.2623 -0.2176 -0.6688 0.053 Uiso 1 1 calc R . . C18 C -0.3131(4) -0.1799(2) -0.7612(5) 0.0650(19) Uani 1 1 d . . . H18A H -0.3467 -0.1586 -0.7525 0.078 Uiso 1 1 calc R . . H18B H -0.2655 -0.1718 -0.7945 0.078 Uiso 1 1 calc R . . C19 C -0.3543(5) -0.2072(3) -0.8260(7) 0.081(2) Uani 1 1 d U . . H19A H -0.3418 -0.2024 -0.8945 0.122 Uiso 1 1 calc R . . H19B H -0.4102 -0.2051 -0.8164 0.122 Uiso 1 1 calc R . . H19C H -0.3375 -0.2316 -0.8088 0.122 Uiso 1 1 calc R . . C20 C -0.1750(3) -0.21644(13) -0.5144(4) 0.0367(11) Uani 1 1 d . . . H20A H -0.1538 -0.2226 -0.4495 0.044 Uiso 1 1 calc R . . H20B H -0.2152 -0.2344 -0.5300 0.044 Uiso 1 1 calc R . . C21 C -0.1113(3) -0.21984(16) -0.5884(5) 0.0472(14) Uani 1 1 d . . . H21A H -0.0658 -0.2059 -0.5666 0.057 Uiso 1 1 calc R . . H21B H -0.1287 -0.2099 -0.6517 0.057 Uiso 1 1 calc R . . C22 C -0.0890(4) -0.25962(17) -0.6007(5) 0.0492(15) Uani 1 1 d . . . H22A H -0.0753 -0.2697 -0.5363 0.059 Uiso 1 1 calc R . . H22B H -0.1341 -0.2731 -0.6256 0.059 Uiso 1 1 calc R . . C23 C -0.0216(4) -0.26483(19) -0.6703(6) 0.0608(17) Uani 1 1 d . . . H23A H -0.0115 -0.2906 -0.6783 0.091 Uiso 1 1 calc R . . H23B H 0.0243 -0.2530 -0.6436 0.091 Uiso 1 1 calc R . . H23C H -0.0343 -0.2542 -0.7337 0.091 Uiso 1 1 calc R . . C24 C -0.6508(3) 0.01798(12) -0.3962(3) 0.0260(9) Uani 1 1 d . . . H24A H -0.6615 0.0200 -0.4669 0.031 Uiso 1 1 calc R . . H24B H -0.6209 0.0396 -0.3770 0.031 Uiso 1 1 calc R . . C25 C -0.7148(3) 0.01829(15) -0.2325(4) 0.0382(12) Uani 1 1 d . . . H25A H -0.6848 -0.0035 -0.2154 0.046 Uiso 1 1 calc R . . H25B H -0.7656 0.0163 -0.2002 0.046 Uiso 1 1 calc R . . C26 C -0.6730(4) 0.05114(16) -0.1918(4) 0.0471(13) Uani 1 1 d . . . H26A H -0.7091 0.0718 -0.1881 0.056 Uiso 1 1 calc R . . H26B H -0.6300 0.0579 -0.2355 0.056 Uiso 1 1 calc R . . C27 C -0.6404(6) 0.0421(3) -0.0854(7) 0.088(3) Uani 1 1 d DU . . H27A H -0.6048 0.0214 -0.0898 0.106 Uiso 1 1 calc R . . H27B H -0.6106 0.0630 -0.0611 0.106 Uiso 1 1 calc R . . C28 C -0.7018(6) 0.0338(3) -0.0159(9) 0.111(3) Uani 1 1 d DU . . H28A H -0.6801 0.0321 0.0499 0.166 Uiso 1 1 calc R . . H28B H -0.7256 0.0107 -0.0334 0.166 Uiso 1 1 calc R . . H28C H -0.7409 0.0528 -0.0177 0.166 Uiso 1 1 calc R . . C29 C -0.7696(3) 0.05330(13) -0.3712(4) 0.0340(11) Uani 1 1 d . . . H29A H -0.8151 0.0559 -0.3282 0.041 Uiso 1 1 calc R . . H29B H -0.7351 0.0740 -0.3580 0.041 Uiso 1 1 calc R . . C30 C -0.7962(3) 0.05574(14) -0.4746(4) 0.0394(12) Uani 1 1 d . . . H30A H -0.8338 0.0363 -0.4879 0.047 Uiso 1 1 calc R . . H30B H -0.7517 0.0524 -0.5189 0.047 Uiso 1 1 calc R . . C31 C -0.8337(5) 0.09236(19) -0.4942(7) 0.075(3) Uani 1 1 d . . . H31A H -0.8813 0.0945 -0.4547 0.090 Uiso 1 1 calc R . . H31B H -0.7980 0.1117 -0.4737 0.090 Uiso 1 1 calc R . . C32 C -0.8532(7) 0.0972(3) -0.5979(9) 0.107(3) Uani 1 1 d U . . H32A H -0.8805 0.1201 -0.6065 0.160 Uiso 1 1 calc R . . H32B H -0.8862 0.0774 -0.6195 0.160 Uiso 1 1 calc R . . H32C H -0.8057 0.0975 -0.6368 0.160 Uiso 1 1 calc R . . C33 C -0.7729(3) -0.01438(13) -0.3719(4) 0.0318(10) Uani 1 1 d . . . H33A H -0.7461 -0.0359 -0.3462 0.038 Uiso 1 1 calc R . . H33B H -0.7725 -0.0161 -0.4440 0.038 Uiso 1 1 calc R . . C34 C -0.8566(3) -0.01530(17) -0.3372(4) 0.0435(13) Uani 1 1 d . . . H34A H -0.8836 0.0069 -0.3577 0.052 Uiso 1 1 calc R . . H34B H -0.8584 -0.0168 -0.2651 0.052 Uiso 1 1 calc R . . C35 C -0.8961(4) -0.0485(2) -0.3821(7) 0.067(2) Uani 1 1 d . . . H35A H -0.8628 -0.0699 -0.3729 0.080 Uiso 1 1 calc R . . H35B H -0.9455 -0.0530 -0.3481 0.080 Uiso 1 1 calc R . . C36 C -0.9112(5) -0.0432(3) -0.4893(7) 0.081(2) Uani 1 1 d U . . H36A H -0.9327 -0.0653 -0.5170 0.122 Uiso 1 1 calc R . . H36B H -0.8628 -0.0373 -0.5225 0.122 Uiso 1 1 calc R . . H36C H -0.9480 -0.0234 -0.4982 0.122 Uiso 1 1 calc R . . C37 C -0.7261(3) -0.13781(12) -0.5096(4) 0.0296(10) Uani 1 1 d . . . C38 C -0.8047(3) -0.14042(14) -0.5299(4) 0.0356(10) Uani 1 1 d . . . H38 H -0.8372 -0.1548 -0.4901 0.043 Uiso 1 1 calc R . . C39 C -0.8347(3) -0.12197(14) -0.6079(4) 0.0369(12) Uani 1 1 d . . . H39 H -0.8881 -0.1237 -0.6225 0.044 Uiso 1 1 calc R . . C40 C -0.7868(3) -0.10062(13) -0.6657(4) 0.0315(10) Uani 1 1 d . . . C41 C -0.7091(3) -0.09814(12) -0.6384(4) 0.0283(10) Uani 1 1 d . . . H41 H -0.6758 -0.0831 -0.6753 0.034 Uiso 1 1 calc R . . C42 C -0.8178(3) -0.07937(14) -0.7502(4) 0.0343(11) Uani 1 1 d . . . H42A H -0.7882 -0.0566 -0.7551 0.041 Uiso 1 1 calc R . . H42B H -0.8720 -0.0729 -0.7359 0.041 Uiso 1 1 calc R . . C43 C -0.8548(3) -0.13465(15) -0.8465(4) 0.0393(12) Uani 1 1 d . . . H43A H -0.8334 -0.1486 -0.7912 0.047 Uiso 1 1 calc R . . H43B H -0.8420 -0.1478 -0.9071 0.047 Uiso 1 1 calc R . . C44 C -0.9418(4) -0.1335(2) -0.8362(5) 0.0552(16) Uani 1 1 d . . . H44A H -0.9651 -0.1249 -0.8978 0.066 Uiso 1 1 calc R . . H44B H -0.9561 -0.1164 -0.7837 0.066 Uiso 1 1 calc R . . C45 C -0.9729(5) -0.1712(2) -0.8117(6) 0.073(2) Uani 1 1 d . . . H45A H -0.9641 -0.1763 -0.7418 0.088 Uiso 1 1 calc R . . H45B H -0.9445 -0.1894 -0.8502 0.088 Uiso 1 1 calc R . . C46 C -1.0596(5) -0.1742(3) -0.8342(7) 0.081(2) Uani 1 1 d U . . H46A H -1.0795 -0.1969 -0.8083 0.121 Uiso 1 1 calc R . . H46B H -1.0675 -0.1734 -0.9050 0.121 Uiso 1 1 calc R . . H46C H -1.0870 -0.1540 -0.8037 0.121 Uiso 1 1 calc R . . C47 C -0.7309(3) -0.10517(15) -0.8809(4) 0.0383(12) Uani 1 1 d . . . H47A H -0.7046 -0.1184 -0.8278 0.046 Uiso 1 1 calc R . . H47B H -0.7315 -0.1211 -0.9388 0.046 Uiso 1 1 calc R . . C48 C -0.6843(3) -0.07242(18) -0.9048(5) 0.0497(15) Uani 1 1 d . . . H48A H -0.6854 -0.0555 -0.8491 0.060 Uiso 1 1 calc R . . H48B H -0.7069 -0.0601 -0.9621 0.060 Uiso 1 1 calc R . . C49 C -0.6011(4) -0.0830(2) -0.9270(6) 0.0596(17) Uani 1 1 d U . . H49A H -0.5775 -0.0934 -0.8677 0.072 Uiso 1 1 calc R . . H49B H -0.6008 -0.1017 -0.9784 0.072 Uiso 1 1 calc R . . C50 C -0.5540(5) -0.0515(3) -0.9600(8) 0.083(2) Uani 1 1 d U . . H50A H -0.5008 -0.0593 -0.9718 0.125 Uiso 1 1 calc R . . H50B H -0.5545 -0.0329 -0.9095 0.125 Uiso 1 1 calc R . . H50C H -0.5758 -0.0418 -1.0204 0.125 Uiso 1 1 calc R . . C51 C -0.8548(3) -0.07312(15) -0.9212(4) 0.0401(12) Uani 1 1 d . . . H51A H -0.9083 -0.0689 -0.8986 0.048 Uiso 1 1 calc R . . H51B H -0.8277 -0.0497 -0.9201 0.048 Uiso 1 1 calc R . . C52 C -0.8577(3) -0.08639(16) -1.0256(5) 0.0474(13) Uani 1 1 d . . . H52A H -0.8061 -0.0954 -1.0448 0.057 Uiso 1 1 calc R . . H52B H -0.8945 -0.1067 -1.0304 0.057 Uiso 1 1 calc R . . C53 C -0.8816(6) -0.0573(3) -1.0929(6) 0.079(2) Uani 1 1 d . . . H53A H -0.8407 -0.0387 -1.0927 0.095 Uiso 1 1 calc R . . H53B H -0.8837 -0.0675 -1.1595 0.095 Uiso 1 1 calc R . . C54 C -0.9531(8) -0.0399(4) -1.0745(11) 0.133(5) Uani 1 1 d U . . H54A H -0.9689 -0.0263 -1.1324 0.199 Uiso 1 1 calc R . . H54B H -0.9474 -0.0233 -1.0192 0.199 Uiso 1 1 calc R . . H54C H -0.9925 -0.0580 -1.0590 0.199 Uiso 1 1 calc R . . C55 C -0.6879(3) -0.16003(12) -0.4336(4) 0.0312(10) Uani 1 1 d . . . C56 C -0.7269(3) -0.18153(14) -0.3706(4) 0.0399(12) Uani 1 1 d . . . H56 H -0.7817 -0.1811 -0.3694 0.048 Uiso 1 1 calc R . . C57 C -0.6871(4) -0.20405(15) -0.3083(4) 0.0431(13) Uani 1 1 d . A . H57 H -0.7142 -0.2199 -0.2661 0.052 Uiso 1 1 calc R . . C58 C -0.6079(3) -0.20334(14) -0.3079(4) 0.0416(14) Uani 1 1 d . . . C59 C -0.5716(3) -0.17980(13) -0.3731(4) 0.0365(12) Uani 1 1 d . A . H59 H -0.5169 -0.1789 -0.3731 0.044 Uiso 1 1 calc R . . C60 C -0.5590(4) -0.22891(15) -0.2488(5) 0.0501(16) Uani 1 1 d . A . H60A H -0.5100 -0.2329 -0.2842 0.060 Uiso 1 1 calc R . . H60B H -0.5860 -0.2523 -0.2451 0.060 Uiso 1 1 calc R . . C61 C -0.6144(4) -0.21345(16) -0.0890(5) 0.0514(17) Uani 1 1 d . A . H61A H -0.6487 -0.2318 -0.1124 0.062 Uiso 1 1 d R . . H61B H -0.6374 -0.1907 -0.1051 0.062 Uiso 1 1 d R . . C62 C -0.6122(5) -0.2165(2) 0.0231(6) 0.072(2) Uani 1 1 d . . . H62A H -0.5943 -0.2408 0.0420 0.086 Uiso 1 1 calc R A . H62B H -0.5754 -0.1987 0.0498 0.086 Uiso 1 1 calc R . . C63 C -0.6919(6) -0.2098(2) 0.0650(6) 0.077(2) Uani 1 1 d . A . H63A H -0.7279 -0.2276 0.0367 0.093 Uiso 1 1 calc R . . H63B H -0.7093 -0.1856 0.0440 0.093 Uiso 1 1 calc R . . C64 C -0.6975(7) -0.2119(3) 0.1756(7) 0.091(3) Uani 1 1 d . . . H64A H -0.7513 -0.2088 0.1956 0.137 Uiso 1 1 calc R A . H64B H -0.6659 -0.1928 0.2047 0.137 Uiso 1 1 calc R . . H64C H -0.6787 -0.2354 0.1978 0.137 Uiso 1 1 calc R . . C65 C -0.4988(3) -0.18107(15) -0.1524(4) 0.0396(12) Uani 1 1 d . A . H65A H -0.4555 -0.1837 -0.1990 0.047 Uiso 1 1 calc R . . H65B H -0.5351 -0.1633 -0.1804 0.047 Uiso 1 1 calc R . . C66 C -0.4673(4) -0.16585(17) -0.0595(5) 0.0500(15) Uani 1 1 d . . . H66A H -0.4285 -0.1825 -0.0318 0.060 Uiso 1 1 calc R A . H66B H -0.5094 -0.1630 -0.0114 0.060 Uiso 1 1 calc R . . C67 C -0.4299(4) -0.12911(18) -0.0797(5) 0.0524(15) Uani 1 1 d . A . H67A H -0.3936 -0.1314 -0.1351 0.063 Uiso 1 1 calc R . . H67B H -0.4703 -0.1116 -0.0982 0.063 Uiso 1 1 calc R . . C68 C -0.3867(5) -0.1153(2) 0.0092(6) 0.070(2) Uani 1 1 d . . . H68A H -0.3669 -0.0911 -0.0040 0.105 Uiso 1 1 calc R A . H68B H -0.3436 -0.1315 0.0239 0.105 Uiso 1 1 calc R . . H68C H -0.4218 -0.1145 0.0652 0.105 Uiso 1 1 calc R . . Cl1 Cl -0.08185(13) -0.08070(6) -0.6573(2) 0.0929(9) Uani 1 1 d . . . O1 O -0.1093(5) -0.0620(3) -0.5842(10) 0.169(4) Uani 1 1 d U . . O2 O -0.0420(6) -0.0618(3) -0.7388(9) 0.151(4) Uani 1 1 d U . . O3 O -0.1473(4) -0.09889(19) -0.6931(7) 0.117(3) Uani 1 1 d U . . O4 O -0.0277(3) -0.10504(19) -0.6270(4) 0.0798(16) Uani 1 1 d U . . Cl2 Cl -0.90235(8) -0.23330(4) -0.43664(15) 0.0568(4) Uani 1 1 d . . . O5 O -0.9428(5) -0.2027(2) -0.4403(9) 0.150(3) Uani 1 1 d U . . O6 O -0.8672(5) -0.2367(2) -0.3429(5) 0.119(3) Uani 1 1 d U . . O7 O -0.8416(3) -0.23200(13) -0.5063(4) 0.0778(17) Uani 1 1 d . . . O8 O -0.9434(4) -0.26560(17) -0.4506(6) 0.097(2) Uani 1 1 d . . . Cl3 Cl -0.67095(8) 0.00202(3) -0.68000(10) 0.0385(3) Uani 1 1 d . . . O9 O -0.7298(2) -0.01422(10) -0.6194(3) 0.0408(9) Uani 1 1 d . . . O10 O -0.6448(3) 0.03483(13) -0.6367(4) 0.0646(14) Uani 1 1 d . . . O11 O -0.6077(3) -0.02244(12) -0.6897(4) 0.0637(13) Uani 1 1 d . . . O12 O -0.7014(4) 0.01008(17) -0.7739(4) 0.0838(17) Uani 1 1 d . . . Cl4 Cl -0.67848(8) -0.10159(3) -0.20260(10) 0.0406(3) Uani 1 1 d . . . O13 O -0.6061(3) -0.11034(14) -0.2452(5) 0.0810(18) Uani 1 1 d . . . O14 O -0.6767(3) -0.06670(11) -0.1592(4) 0.0612(13) Uani 1 1 d U . . O15 O -0.6963(4) -0.12809(12) -0.1314(4) 0.0739(15) Uani 1 1 d U . . O16 O -0.7331(5) -0.10082(18) -0.2774(6) 0.112(3) Uani 1 1 d U . . Cl5 Cl -0.23810(8) -0.19768(4) -0.13025(14) 0.0519(4) Uani 1 1 d . . . O17 O -0.1995(5) -0.2144(2) -0.2107(6) 0.114(2) Uani 1 1 d U . . O18 O -0.2848(6) -0.2226(3) -0.0927(9) 0.168(4) Uani 1 1 d U . . O19 O -0.2674(7) -0.1663(3) -0.1611(8) 0.173(4) Uani 1 1 d U . . O20 O -0.1811(6) -0.1929(3) -0.0601(8) 0.155(4) Uani 1 1 d U . . C69' C -0.5096(8) -0.2492(4) -0.0864(10) 0.046(3) Uani 0.50 1 d PDU A 1 H69A H -0.4928 -0.2413 -0.0208 0.055 Uiso 0.50 1 calc PR A 1 H69B H -0.5509 -0.2674 -0.0784 0.055 Uiso 0.50 1 calc PR A 1 C70' C -0.4431(7) -0.2652(4) -0.1406(10) 0.062(4) Uani 0.50 1 d PD A 1 H70A H -0.4064 -0.2461 -0.1606 0.074 Uiso 0.50 1 calc PR A 1 H70B H -0.4613 -0.2779 -0.1997 0.074 Uiso 0.50 1 calc PR A 1 C71' C -0.4051(8) -0.2911(4) -0.0714(10) 0.055(3) Uani 0.50 1 d PDU A 1 H71A H -0.3815 -0.2780 -0.0160 0.066 Uiso 0.50 1 calc PR A 1 H71B H -0.4431 -0.3085 -0.0457 0.066 Uiso 0.50 1 calc PR A 1 C72' C -0.3479(9) -0.3089(4) -0.1269(10) 0.044(3) Uani 0.50 1 d PU A 1 H72D H -0.3288 -0.3298 -0.0904 0.065 Uiso 0.50 1 calc PR A 1 H72E H -0.3052 -0.2923 -0.1398 0.065 Uiso 0.50 1 calc PR A 1 H72F H -0.3702 -0.3170 -0.1888 0.065 Uiso 0.50 1 calc PR A 1 O1W O -1.0973(11) -0.0160(6) -0.2886(17) 0.151(7) Uani 0.50 1 d PU B 1 H1WA H -1.1248 -0.0348 -0.2833 0.182 Uiso 0.50 1 d PR B 1 H1WB H -1.1122 -0.0039 -0.3377 0.182 Uiso 0.50 1 d PR B 1 C69 C -0.4723(6) -0.2421(2) -0.1103(9) 0.028(2) Uani 0.50 1 d P A 2 H69C H -0.4585 -0.2362 -0.0422 0.033 Uiso 0.50 1 calc PR A 2 H69D H -0.4262 -0.2382 -0.1516 0.033 Uiso 0.50 1 calc PR A 2 C70 C -0.4979(5) -0.2829(2) -0.1170(9) 0.034(2) Uani 0.50 1 d P A 2 H70C H -0.5475 -0.2864 -0.0826 0.041 Uiso 0.50 1 calc PR A 2 H70D H -0.5049 -0.2899 -0.1861 0.041 Uiso 0.50 1 calc PR A 2 C71 C -0.4341(6) -0.3066(3) -0.0691(8) 0.039(2) Uani 0.50 1 d PDU A 2 H71C H -0.4130 -0.2937 -0.0118 0.046 Uiso 0.50 1 calc PR A 2 H71D H -0.4579 -0.3292 -0.0453 0.046 Uiso 0.50 1 calc PR A 2 C72 C -0.3664(15) -0.3163(8) -0.139(2) 0.136(14) Uani 0.50 1 d PDU A 2 H72A H -0.3240 -0.3268 -0.1012 0.204 Uiso 0.50 1 calc PR A 2 H72B H -0.3483 -0.2944 -0.1718 0.204 Uiso 0.50 1 calc PR A 2 H72C H -0.3842 -0.3337 -0.1876 0.204 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0273(2) 0.0292(2) 0.0333(3) -0.0038(3) -0.0115(2) 0.0053(2) Br1 0.0455(3) 0.0668(4) 0.0372(3) -0.0052(3) -0.0050(3) 0.0158(3) N1 0.0221(17) 0.0271(18) 0.029(2) -0.0024(17) -0.0066(15) 0.0028(14) N2 0.031(2) 0.035(2) 0.040(3) -0.005(2) -0.0113(18) 0.0063(16) N3 0.032(2) 0.0288(19) 0.024(2) 0.0043(17) 0.0064(16) 0.0010(16) N4 0.0286(19) 0.037(2) 0.034(2) 0.0075(19) 0.0051(17) 0.0038(16) N5 0.0274(19) 0.0270(18) 0.030(2) -0.0023(16) -0.0097(16) 0.0035(15) N6 0.036(2) 0.0264(18) 0.036(2) -0.0061(18) -0.0079(18) 0.0055(16) N7 0.033(2) 0.038(2) 0.028(2) 0.0020(18) -0.0064(17) 0.0064(17) N8 0.064(3) 0.026(2) 0.049(3) 0.002(2) -0.030(2) 0.006(2) C1 0.029(2) 0.036(2) 0.028(3) -0.003(2) -0.0070(19) 0.0019(19) C2 0.029(2) 0.038(3) 0.035(3) -0.005(2) -0.012(2) -0.0019(19) C3 0.027(2) 0.044(3) 0.040(3) 0.004(2) -0.010(2) 0.008(2) C4 0.026(2) 0.034(2) 0.031(3) 0.004(2) -0.0015(19) 0.0041(18) C5 0.033(2) 0.035(2) 0.033(3) -0.003(2) -0.006(2) 0.0046(19) C6 0.025(2) 0.029(2) 0.026(2) 0.0029(19) -0.0082(18) 0.0025(17) C7 0.027(2) 0.041(3) 0.033(3) 0.000(2) -0.013(2) 0.0029(19) C8 0.035(3) 0.031(2) 0.035(3) -0.013(2) -0.007(2) 0.0021(19) C9 0.027(2) 0.029(2) 0.029(2) 0.001(2) -0.0019(19) -0.0021(18) C10 0.026(2) 0.031(2) 0.028(2) 0.000(2) -0.0031(19) 0.0019(17) C11 0.028(2) 0.039(3) 0.035(3) 0.010(2) 0.001(2) 0.0028(19) C12 0.031(2) 0.040(3) 0.053(3) 0.009(3) 0.006(2) -0.002(2) C13 0.031(3) 0.060(4) 0.057(4) 0.007(3) 0.000(3) 0.004(2) C14 0.070(5) 0.065(4) 0.083(6) -0.004(4) -0.021(4) -0.009(4) C15 0.083(6) 0.081(6) 0.092(7) -0.017(5) -0.024(5) -0.019(4) C16 0.046(3) 0.044(3) 0.034(3) 0.015(2) 0.004(2) 0.009(2) C17 0.050(3) 0.047(3) 0.036(3) 0.012(3) 0.005(2) 0.002(2) C18 0.064(4) 0.084(5) 0.046(4) 0.019(4) -0.011(3) 0.003(4) C19 0.083(4) 0.096(4) 0.065(4) 0.002(4) -0.004(3) 0.001(4) C20 0.034(2) 0.036(2) 0.039(3) 0.007(2) 0.001(2) 0.0098(19) C21 0.044(3) 0.046(3) 0.052(4) 0.008(3) 0.018(3) 0.015(2) C22 0.046(3) 0.054(4) 0.048(4) 0.003(3) 0.002(3) 0.014(3) C23 0.065(4) 0.062(4) 0.056(4) -0.007(4) 0.007(3) 0.021(3) C24 0.030(2) 0.023(2) 0.025(2) 0.0024(18) 0.0053(19) -0.0027(17) C25 0.051(3) 0.039(3) 0.025(3) -0.001(2) 0.005(2) -0.007(2) C26 0.064(3) 0.050(3) 0.027(3) -0.006(3) -0.003(3) -0.010(3) C27 0.096(4) 0.093(4) 0.077(4) -0.011(4) -0.012(4) -0.028(4) C28 0.113(4) 0.115(4) 0.104(4) -0.003(3) -0.003(3) -0.004(3) C29 0.030(2) 0.029(2) 0.042(3) -0.006(2) 0.007(2) 0.0073(18) C30 0.036(3) 0.034(3) 0.049(3) 0.006(2) 0.004(2) 0.008(2) C31 0.064(4) 0.046(3) 0.114(7) 0.010(4) -0.031(4) 0.018(3) C32 0.110(4) 0.102(4) 0.107(4) 0.011(3) -0.011(3) 0.006(3) C33 0.032(2) 0.031(2) 0.032(3) -0.003(2) 0.004(2) -0.0063(19) C34 0.038(3) 0.057(3) 0.036(3) -0.002(3) 0.012(2) -0.018(2) C35 0.048(4) 0.062(4) 0.090(6) -0.012(4) 0.011(4) -0.024(3) C36 0.075(3) 0.087(3) 0.082(4) -0.008(3) -0.002(3) -0.003(3) C37 0.034(2) 0.028(2) 0.027(3) 0.004(2) -0.011(2) -0.0008(17) C38 0.029(2) 0.042(3) 0.037(3) 0.005(3) -0.003(2) -0.0040(18) C39 0.028(2) 0.044(3) 0.039(3) 0.006(2) -0.008(2) 0.005(2) C40 0.031(2) 0.031(2) 0.033(3) 0.000(2) -0.008(2) 0.0081(18) C41 0.032(2) 0.022(2) 0.030(3) -0.0009(19) -0.007(2) 0.0017(17) C42 0.034(2) 0.036(3) 0.033(3) 0.000(2) -0.010(2) 0.004(2) C43 0.045(3) 0.042(3) 0.031(3) 0.002(2) -0.001(2) -0.005(2) C44 0.047(3) 0.080(5) 0.039(3) 0.005(3) -0.004(3) -0.016(3) C45 0.085(5) 0.090(6) 0.044(4) 0.018(4) -0.006(4) -0.045(4) C46 0.072(4) 0.090(4) 0.081(4) 0.006(4) -0.002(3) -0.029(3) C47 0.039(3) 0.041(3) 0.035(3) -0.001(2) -0.001(2) 0.007(2) C48 0.045(3) 0.061(4) 0.043(4) -0.010(3) -0.001(3) -0.007(3) C49 0.050(3) 0.073(3) 0.056(3) -0.001(2) -0.004(2) -0.005(2) C50 0.068(4) 0.093(4) 0.088(4) -0.013(4) 0.007(3) -0.024(3) C51 0.039(3) 0.044(3) 0.038(3) 0.003(2) -0.011(2) 0.004(2) C52 0.053(3) 0.054(3) 0.035(3) 0.002(3) -0.008(3) -0.007(2) C53 0.107(7) 0.090(6) 0.041(4) 0.011(4) -0.024(4) -0.005(5) C54 0.133(5) 0.139(5) 0.127(5) 0.005(3) -0.003(3) 0.009(3) C55 0.036(2) 0.024(2) 0.034(3) -0.005(2) -0.016(2) 0.0035(18) C56 0.041(3) 0.036(3) 0.043(3) 0.003(2) -0.016(3) -0.005(2) C57 0.063(4) 0.033(3) 0.034(3) 0.003(2) -0.015(3) -0.006(2) C58 0.057(3) 0.027(2) 0.041(3) 0.000(2) -0.024(3) 0.005(2) C59 0.042(3) 0.030(2) 0.037(3) 0.000(2) -0.019(2) 0.007(2) C60 0.078(4) 0.030(3) 0.042(3) 0.000(2) -0.027(3) 0.011(3) C61 0.076(4) 0.038(3) 0.040(3) 0.006(3) -0.028(3) -0.022(3) C62 0.102(6) 0.064(4) 0.051(4) 0.021(4) -0.035(4) -0.036(4) C63 0.122(7) 0.069(5) 0.040(4) 0.014(4) -0.020(4) -0.021(5) C64 0.127(8) 0.094(7) 0.053(5) 0.024(5) -0.017(5) -0.014(6) C65 0.038(3) 0.040(3) 0.041(3) 0.000(2) -0.010(2) 0.003(2) C66 0.062(4) 0.046(3) 0.042(3) -0.007(3) -0.010(3) -0.007(3) C67 0.051(3) 0.058(4) 0.048(4) -0.004(3) -0.004(3) -0.010(3) C68 0.082(5) 0.063(4) 0.064(5) -0.014(4) -0.011(4) -0.035(4) Cl1 0.0682(11) 0.0720(12) 0.138(2) 0.0346(14) -0.0507(14) -0.0124(10) O1 0.084(5) 0.182(7) 0.243(9) -0.061(7) 0.002(6) 0.048(5) O2 0.154(6) 0.116(6) 0.185(8) 0.061(6) -0.022(6) -0.032(5) O3 0.102(4) 0.102(4) 0.147(6) 0.055(4) -0.069(4) -0.040(3) O4 0.051(3) 0.123(4) 0.066(3) 0.005(3) -0.005(3) 0.010(3) Cl2 0.0397(7) 0.0462(7) 0.0846(13) -0.0182(8) 0.0072(8) -0.0070(6) O5 0.108(5) 0.100(5) 0.243(9) 0.018(6) 0.066(6) 0.037(4) O6 0.134(5) 0.157(6) 0.066(4) -0.019(4) -0.009(4) -0.066(5) O7 0.092(4) 0.060(3) 0.082(4) 0.009(3) 0.039(3) 0.009(3) O8 0.095(4) 0.087(4) 0.109(5) 0.017(4) -0.030(4) -0.051(3) Cl3 0.0558(7) 0.0345(6) 0.0252(6) 0.0008(5) 0.0097(6) -0.0039(5) O9 0.0414(19) 0.043(2) 0.038(2) 0.0027(17) 0.0049(16) -0.0077(16) O10 0.087(3) 0.055(3) 0.051(3) -0.017(2) 0.035(3) -0.031(2) O11 0.055(2) 0.052(2) 0.085(4) 0.007(3) 0.029(3) 0.0025(19) O12 0.129(5) 0.085(4) 0.038(3) 0.014(3) -0.008(3) 0.009(4) Cl4 0.0570(8) 0.0323(6) 0.0325(7) 0.0012(5) -0.0039(6) 0.0036(5) O13 0.077(4) 0.060(3) 0.105(5) 0.009(3) 0.041(3) 0.014(3) O14 0.094(3) 0.035(2) 0.054(3) -0.005(2) 0.003(2) -0.002(2) O15 0.107(4) 0.043(2) 0.071(4) 0.009(2) 0.025(3) -0.006(2) O16 0.132(5) 0.088(4) 0.114(5) -0.023(4) -0.077(4) 0.038(4) Cl5 0.0486(8) 0.0393(7) 0.0679(10) 0.0021(7) 0.0016(8) 0.0120(6) O17 0.154(6) 0.102(5) 0.087(5) 0.001(4) -0.003(4) 0.050(4) O18 0.131(6) 0.186(7) 0.188(8) 0.065(7) 0.015(6) -0.051(6) O19 0.213(8) 0.137(6) 0.169(8) 0.047(6) 0.020(6) 0.114(6) O20 0.150(6) 0.153(7) 0.163(8) -0.029(6) -0.071(6) -0.006(5) C69' 0.050(5) 0.044(5) 0.045(5) 0.005(4) -0.007(4) 0.004(4) C70' 0.061(8) 0.076(10) 0.048(8) 0.012(8) -0.003(7) 0.003(8) C71' 0.055(5) 0.051(5) 0.059(5) 0.007(4) -0.007(4) 0.006(4) C72' 0.058(5) 0.033(4) 0.040(5) 0.002(4) -0.014(4) 0.007(4) O1W 0.152(8) 0.148(8) 0.153(8) 0.010(5) 0.005(5) 0.009(5) C69 0.017(4) 0.024(5) 0.041(6) 0.019(4) -0.007(4) 0.002(4) C70 0.029(4) 0.021(4) 0.052(7) 0.018(4) -0.009(4) 0.000(3) C71 0.046(4) 0.028(4) 0.042(4) 0.012(4) -0.011(4) 0.003(4) C72 0.138(15) 0.133(15) 0.138(15) 0.005(5) -0.004(5) 0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.107(4) . ? Zn1 N6 2.115(4) . ? Zn1 N5 2.157(4) . ? Zn1 N2 2.158(4) . ? Zn1 Br1 2.3746(9) . ? N1 C10 1.333(6) . ? N1 C6 1.350(6) . ? N2 C1 1.333(7) . ? N2 C5 1.347(6) . ? N3 C24 1.515(6) . ? N3 C33 1.523(6) . ? N3 C25 1.523(7) . ? N3 C29 1.527(6) . ? N4 C12 1.520(7) . ? N4 C20 1.520(6) . ? N4 C16 1.530(7) . ? N4 C11 1.532(6) . ? N5 C41 1.325(6) . ? N5 C37 1.353(6) . ? N6 C59 1.334(6) . ? N6 C55 1.361(6) . ? N7 C43 1.515(7) . ? N7 C51 1.521(7) . ? N7 C42 1.533(7) . ? N7 C47 1.545(7) . ? N8 C65 1.510(7) . ? N8 C61 1.514(9) . ? N8 C60 1.523(8) . ? N8 C69' 1.542(13) . ? N8 C69 1.575(10) . ? C1 C2 1.386(7) . ? C1 C6 1.495(6) . ? C2 C3 1.381(7) . ? C2 H2 0.9500 . ? C3 C4 1.394(8) . ? C3 H3 0.9500 . ? C4 C5 1.388(7) . ? C4 C11 1.496(7) . ? C5 H5 0.9500 . ? C6 C7 1.378(7) . ? C7 C8 1.381(7) . ? C7 H7 0.9500 . ? C8 C9 1.396(7) . ? C8 H8 0.9500 . ? C9 C10 1.383(7) . ? C9 C24 1.508(6) . ? C10 H10 0.9500 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.517(9) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.508(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.530(13) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.501(9) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.528(9) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.524(12) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.505(8) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.536(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.520(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.524(8) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.600(11) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.462(9) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.495(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.532(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.473(15) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.528(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.539(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.506(13) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.394(6) . ? C37 C55 1.486(6) . ? C38 C39 1.373(8) . ? C38 H38 0.9500 . ? C39 C40 1.396(8) . ? C39 H39 0.9500 . ? C40 C41 1.401(7) . ? C40 C42 1.501(7) . ? C41 H41 0.9500 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.515(8) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.539(10) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.538(11) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.497(8) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.525(9) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.496(11) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.514(9) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.480(10) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.422(16) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.357(8) . ? C56 C57 1.381(8) . ? C56 H56 0.9500 . ? C57 C58 1.372(9) . ? C57 H57 0.9500 . ? C58 C59 1.400(8) . ? C58 C60 1.510(7) . ? C59 H59 0.9500 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.542(9) . ? C61 H61A 0.9597 . ? C61 H61B 0.9603 . ? C62 C63 1.517(13) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.522(11) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.497(8) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.536(9) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.520(9) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? Cl1 O1 1.309(11) . ? Cl1 O4 1.368(6) . ? Cl1 O3 1.409(6) . ? Cl1 O2 1.491(10) . ? Cl2 O5 1.336(8) . ? Cl2 O8 1.407(6) . ? Cl2 O7 1.422(5) . ? Cl2 O6 1.428(8) . ? Cl3 O12 1.423(5) . ? Cl3 O10 1.429(4) . ? Cl3 O11 1.430(4) . ? Cl3 O9 1.448(4) . ? Cl4 O16 1.396(6) . ? Cl4 O15 1.420(5) . ? Cl4 O13 1.422(5) . ? Cl4 O14 1.426(4) . ? Cl5 O18 1.334(9) . ? Cl5 O19 1.338(7) . ? Cl5 O20 1.390(9) . ? Cl5 O17 1.432(8) . ? C69' C70' 1.494(9) . ? C69' H69A 0.9900 . ? C69' H69B 0.9900 . ? C70' C71' 1.504(9) . ? C70' H70A 0.9900 . ? C70' H70B 0.9900 . ? C71' C72' 1.414(18) . ? C71' H71A 0.9900 . ? C71' H71B 0.9900 . ? C72' H72D 0.9800 . ? C72' H72E 0.9800 . ? C72' H72F 0.9800 . ? O1W H1WA 0.8499 . ? O1W H1WB 0.8499 . ? C69 C70 1.579(12) . ? C69 H69C 0.9900 . ? C69 H69D 0.9900 . ? C70 C71 1.559(13) . ? C70 H70C 0.9900 . ? C70 H70D 0.9900 . ? C71 C72 1.556(10) . ? C71 H71C 0.9900 . ? C71 H71D 0.9900 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? 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 N1 Zn1 N6 107.56(16) . . ? N1 Zn1 N5 98.64(14) . . ? N6 Zn1 N5 77.07(15) . . ? N1 Zn1 N2 76.77(15) . . ? N6 Zn1 N2 91.01(17) . . ? N5 Zn1 N2 165.43(18) . . ? N1 Zn1 Br1 124.50(11) . . ? N6 Zn1 Br1 127.76(11) . . ? N5 Zn1 Br1 97.56(12) . . ? N2 Zn1 Br1 96.38(13) . . ? C10 N1 C6 117.9(4) . . ? C10 N1 Zn1 126.2(3) . . ? C6 N1 Zn1 115.6(3) . . ? C1 N2 C5 119.6(4) . . ? C1 N2 Zn1 115.5(3) . . ? C5 N2 Zn1 124.9(3) . . ? C24 N3 C33 108.0(3) . . ? C24 N3 C25 111.0(4) . . ? C33 N3 C25 109.0(4) . . ? C24 N3 C29 108.3(3) . . ? C33 N3 C29 111.0(4) . . ? C25 N3 C29 109.6(4) . . ? C12 N4 C20 111.5(4) . . ? C12 N4 C16 106.2(4) . . ? C20 N4 C16 110.9(4) . . ? C12 N4 C11 111.4(4) . . ? C20 N4 C11 105.4(4) . . ? C16 N4 C11 111.5(4) . . ? C41 N5 C37 120.0(4) . . ? C41 N5 Zn1 125.2(3) . . ? C37 N5 Zn1 114.4(3) . . ? C59 N6 C55 117.2(5) . . ? C59 N6 Zn1 126.0(4) . . ? C55 N6 Zn1 116.5(3) . . ? C43 N7 C51 111.1(4) . . ? C43 N7 C42 111.8(4) . . ? C51 N7 C42 106.3(4) . . ? C43 N7 C47 106.8(4) . . ? C51 N7 C47 110.4(4) . . ? C42 N7 C47 110.5(4) . . ? C65 N8 C61 111.2(4) . . ? C65 N8 C60 107.6(5) . . ? C61 N8 C60 108.3(5) . . ? C65 N8 C69' 124.0(7) . . ? C61 N8 C69' 95.0(7) . . ? C60 N8 C69' 109.5(6) . . ? C65 N8 C69 101.2(5) . . ? C61 N8 C69 121.9(6) . . ? C60 N8 C69 105.8(6) . . ? C69' N8 C69 28.6(5) . . ? N2 C1 C2 121.7(4) . . ? N2 C1 C6 115.0(4) . . ? C2 C1 C6 123.2(4) . . ? C3 C2 C1 118.5(5) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 120.6(4) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 116.9(4) . . ? C5 C4 C11 119.4(5) . . ? C3 C4 C11 123.5(4) . . ? N2 C5 C4 122.6(5) . . ? N2 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? N1 C6 C7 121.7(4) . . ? N1 C6 C1 115.8(4) . . ? C7 C6 C1 122.5(4) . . ? C6 C7 C8 119.8(4) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C7 C8 C9 118.8(4) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C10 C9 C8 117.5(4) . . ? C10 C9 C24 121.2(4) . . ? C8 C9 C24 120.9(4) . . ? N1 C10 C9 124.0(4) . . ? N1 C10 H10 118.0 . . ? C9 C10 H10 118.0 . . ? C4 C11 N4 116.5(4) . . ? C4 C11 H11A 108.2 . . ? N4 C11 H11A 108.2 . . ? C4 C11 H11B 108.2 . . ? N4 C11 H11B 108.2 . . ? H11A C11 H11B 107.3 . . ? C13 C12 N4 116.4(5) . . ? C13 C12 H12A 108.2 . . ? N4 C12 H12A 108.2 . . ? C13 C12 H12B 108.2 . . ? N4 C12 H12B 108.2 . . ? H12A C12 H12B 107.3 . . ? C14 C13 C12 110.8(6) . . ? C14 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C13 C14 C15 112.9(7) . . ? C13 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? C13 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N4 116.3(4) . . ? C17 C16 H16A 108.2 . . ? N4 C16 H16A 108.2 . . ? C17 C16 H16B 108.2 . . ? N4 C16 H16B 108.2 . . ? H16A C16 H16B 107.4 . . ? C16 C17 C18 109.4(5) . . ? C16 C17 H17A 109.8 . . ? C18 C17 H17A 109.8 . . ? C16 C17 H17B 109.8 . . ? C18 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? C19 C18 C17 113.2(7) . . ? C19 C18 H18A 108.9 . . ? C17 C18 H18A 108.9 . . ? C19 C18 H18B 108.9 . . ? C17 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? 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 . . ? C21 C20 N4 115.8(4) . . ? C21 C20 H20A 108.3 . . ? N4 C20 H20A 108.3 . . ? C21 C20 H20B 108.3 . . ? N4 C20 H20B 108.3 . . ? H20A C20 H20B 107.4 . . ? C20 C21 C22 109.8(5) . . ? C20 C21 H21A 109.7 . . ? C22 C21 H21A 109.7 . . ? C20 C21 H21B 109.7 . . ? C22 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? C23 C22 C21 112.6(5) . . ? C23 C22 H22A 109.1 . . ? C21 C22 H22A 109.1 . . ? C23 C22 H22B 109.1 . . ? C21 C22 H22B 109.1 . . ? H22A C22 H22B 107.8 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C9 C24 N3 116.9(4) . . ? C9 C24 H24A 108.1 . . ? N3 C24 H24A 108.1 . . ? C9 C24 H24B 108.1 . . ? N3 C24 H24B 108.1 . . ? H24A C24 H24B 107.3 . . ? N3 C25 C26 114.7(4) . . ? N3 C25 H25A 108.6 . . ? C26 C25 H25A 108.6 . . ? N3 C25 H25B 108.6 . . ? C26 C25 H25B 108.6 . . ? H25A C25 H25B 107.6 . . ? C25 C26 C27 109.6(5) . . ? C25 C26 H26A 109.8 . . ? C27 C26 H26A 109.8 . . ? C25 C26 H26B 109.8 . . ? C27 C26 H26B 109.8 . . ? H26A C26 H26B 108.2 . . ? C28 C27 C26 112.4(8) . . ? C28 C27 H27A 109.1 . . ? C26 C27 H27A 109.1 . . ? C28 C27 H27B 109.1 . . ? C26 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 N3 116.4(4) . . ? C30 C29 H29A 108.2 . . ? N3 C29 H29A 108.2 . . ? C30 C29 H29B 108.2 . . ? N3 C29 H29B 108.2 . . ? H29A C29 H29B 107.3 . . ? C29 C30 C31 110.6(5) . . ? C29 C30 H30A 109.5 . . ? C31 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? C32 C31 C30 112.1(8) . . ? C32 C31 H31A 109.2 . . ? C30 C31 H31A 109.2 . . ? C32 C31 H31B 109.2 . . ? C30 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? 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 . . ? N3 C33 C34 115.5(4) . . ? N3 C33 H33A 108.4 . . ? C34 C33 H33A 108.4 . . ? N3 C33 H33B 108.4 . . ? C34 C33 H33B 108.4 . . ? H33A C33 H33B 107.5 . . ? C33 C34 C35 108.4(5) . . ? C33 C34 H34A 110.0 . . ? C35 C34 H34A 110.0 . . ? C33 C34 H34B 110.0 . . ? C35 C34 H34B 110.0 . . ? H34A C34 H34B 108.4 . . ? C36 C35 C34 111.3(7) . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35B 109.4 . . ? C34 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? 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 . . ? N5 C37 C38 120.5(4) . . ? N5 C37 C55 116.8(4) . . ? C38 C37 C55 122.5(4) . . ? C39 C38 C37 119.4(5) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C38 C39 C40 120.1(5) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C39 C40 C41 117.3(4) . . ? C39 C40 C42 121.5(4) . . ? C41 C40 C42 121.1(5) . . ? N5 C41 C40 122.6(5) . . ? N5 C41 H41 118.7 . . ? C40 C41 H41 118.7 . . ? C40 C42 N7 115.7(4) . . ? C40 C42 H42A 108.3 . . ? N7 C42 H42A 108.3 . . ? C40 C42 H42B 108.3 . . ? N7 C42 H42B 108.3 . . ? H42A C42 H42B 107.4 . . ? N7 C43 C44 115.3(5) . . ? N7 C43 H43A 108.5 . . ? C44 C43 H43A 108.5 . . ? N7 C43 H43B 108.5 . . ? C44 C43 H43B 108.5 . . ? H43A C43 H43B 107.5 . . ? C43 C44 C45 110.1(6) . . ? C43 C44 H44A 109.6 . . ? C45 C44 H44A 109.6 . . ? C43 C44 H44B 109.6 . . ? C45 C44 H44B 109.6 . . ? H44A C44 H44B 108.2 . . ? C44 C45 C46 111.4(7) . . ? C44 C45 H45A 109.3 . . ? C46 C45 H45A 109.3 . . ? C44 C45 H45B 109.3 . . ? C46 C45 H45B 109.3 . . ? H45A C45 H45B 108.0 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 N7 116.0(5) . . ? C48 C47 H47A 108.3 . . ? N7 C47 H47A 108.3 . . ? C48 C47 H47B 108.3 . . ? N7 C47 H47B 108.3 . . ? H47A C47 H47B 107.4 . . ? C47 C48 C49 110.2(6) . . ? C47 C48 H48A 109.6 . . ? C49 C48 H48A 109.6 . . ? C47 C48 H48B 109.6 . . ? C49 C48 H48B 109.6 . . ? H48A C48 H48B 108.1 . . ? C50 C49 C48 112.1(7) . . ? C50 C49 H49A 109.2 . . ? C48 C49 H49A 109.2 . . ? C50 C49 H49B 109.2 . . ? C48 C49 H49B 109.2 . . ? H49A C49 H49B 107.9 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 N7 115.2(5) . . ? C52 C51 H51A 108.5 . . ? N7 C51 H51A 108.5 . . ? C52 C51 H51B 108.5 . . ? N7 C51 H51B 108.5 . . ? H51A C51 H51B 107.5 . . ? C53 C52 C51 111.2(6) . . ? C53 C52 H52A 109.4 . . ? C51 C52 H52A 109.4 . . ? C53 C52 H52B 109.4 . . ? C51 C52 H52B 109.4 . . ? H52A C52 H52B 108.0 . . ? C54 C53 C52 117.8(10) . . ? C54 C53 H53A 107.9 . . ? C52 C53 H53A 107.9 . . ? C54 C53 H53B 107.9 . . ? C52 C53 H53B 107.9 . . ? H53A C53 H53B 107.2 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 N6 122.2(4) . . ? C56 C55 C37 123.4(4) . . ? N6 C55 C37 114.3(4) . . ? C55 C56 C57 120.0(5) . . ? C55 C56 H56 120.0 . . ? C57 C56 H56 120.0 . . ? C58 C57 C56 119.4(5) . . ? C58 C57 H57 120.3 . . ? C56 C57 H57 120.3 . . ? C57 C58 C59 117.3(5) . . ? C57 C58 C60 123.5(6) . . ? C59 C58 C60 118.9(5) . . ? N6 C59 C58 123.8(5) . . ? N6 C59 H59 118.1 . . ? C58 C59 H59 118.1 . . ? C58 C60 N8 116.0(5) . . ? C58 C60 H60A 108.3 . . ? N8 C60 H60A 108.3 . . ? C58 C60 H60B 108.3 . . ? N8 C60 H60B 108.3 . . ? H60A C60 H60B 107.4 . . ? N8 C61 C62 118.8(6) . . ? N8 C61 H61A 107.4 . . ? C62 C61 H61A 107.2 . . ? N8 C61 H61B 108.1 . . ? C62 C61 H61B 107.7 . . ? H61A C61 H61B 107.1 . . ? C63 C62 C61 110.0(7) . . ? C63 C62 H62A 109.7 . . ? C61 C62 H62A 109.7 . . ? C63 C62 H62B 109.7 . . ? C61 C62 H62B 109.7 . . ? H62A C62 H62B 108.2 . . ? C62 C63 C64 115.3(8) . . ? C62 C63 H63A 108.5 . . ? C64 C63 H63A 108.5 . . ? C62 C63 H63B 108.5 . . ? C64 C63 H63B 108.5 . . ? H63A C63 H63B 107.5 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 N8 116.8(5) . . ? C66 C65 H65A 108.1 . . ? N8 C65 H65A 108.1 . . ? C66 C65 H65B 108.1 . . ? N8 C65 H65B 108.1 . . ? H65A C65 H65B 107.3 . . ? C65 C66 C67 109.6(5) . . ? C65 C66 H66A 109.7 . . ? C67 C66 H66A 109.7 . . ? C65 C66 H66B 109.7 . . ? C67 C66 H66B 109.7 . . ? H66A C66 H66B 108.2 . . ? C68 C67 C66 111.3(6) . . ? C68 C67 H67A 109.4 . . ? C66 C67 H67A 109.4 . . ? C68 C67 H67B 109.4 . . ? C66 C67 H67B 109.4 . . ? H67A C67 H67B 108.0 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O1 Cl1 O4 111.6(6) . . ? O1 Cl1 O3 103.2(6) . . ? O4 Cl1 O3 110.0(4) . . ? O1 Cl1 O2 119.5(8) . . ? O4 Cl1 O2 102.7(5) . . ? O3 Cl1 O2 109.7(6) . . ? O5 Cl2 O8 117.0(5) . . ? O5 Cl2 O7 109.6(5) . . ? O8 Cl2 O7 108.2(4) . . ? O5 Cl2 O6 109.5(7) . . ? O8 Cl2 O6 105.2(4) . . ? O7 Cl2 O6 106.9(4) . . ? O12 Cl3 O10 108.3(4) . . ? O12 Cl3 O11 109.5(4) . . ? O10 Cl3 O11 109.7(3) . . ? O12 Cl3 O9 110.2(3) . . ? O10 Cl3 O9 109.9(2) . . ? O11 Cl3 O9 109.2(3) . . ? O16 Cl4 O15 111.8(5) . . ? O16 Cl4 O13 107.6(5) . . ? O15 Cl4 O13 108.4(3) . . ? O16 Cl4 O14 107.6(3) . . ? O15 Cl4 O14 110.3(3) . . ? O13 Cl4 O14 111.1(3) . . ? O18 Cl5 O19 119.7(7) . . ? O18 Cl5 O20 104.6(7) . . ? O19 Cl5 O20 112.2(8) . . ? O18 Cl5 O17 106.4(7) . . ? O19 Cl5 O17 108.0(6) . . ? O20 Cl5 O17 104.8(6) . . ? C70' C69' N8 108.0(10) . . ? C70' C69' H69A 110.1 . . ? N8 C69' H69A 110.1 . . ? C70' C69' H69B 110.1 . . ? N8 C69' H69B 110.1 . . ? H69A C69' H69B 108.4 . . ? C69' C70' C71' 106.1(10) . . ? C69' C70' H70A 110.5 . . ? C71' C70' H70A 110.5 . . ? C69' C70' H70B 110.5 . . ? C71' C70' H70B 110.5 . . ? H70A C70' H70B 108.7 . . ? C72' C71' C70' 105.5(11) . . ? C72' C71' H71A 110.6 . . ? C70' C71' H71A 110.6 . . ? C72' C71' H71B 110.6 . . ? C70' C71' H71B 110.6 . . ? H71A C71' H71B 108.8 . . ? H1WA O1W H1WB 109.5 . . ? N8 C69 C70 110.2(7) . . ? N8 C69 H69C 109.6 . . ? C70 C69 H69C 109.6 . . ? N8 C69 H69D 109.6 . . ? C70 C69 H69D 109.6 . . ? H69C C69 H69D 108.1 . . ? C71 C70 C69 108.5(8) . . ? C71 C70 H70C 110.0 . . ? C69 C70 H70C 110.0 . . ? C71 C70 H70D 110.0 . . ? C69 C70 H70D 110.0 . . ? H70C C70 H70D 108.4 . . ? C72 C71 C70 114.0(16) . . ? C72 C71 H71C 108.8 . . ? C70 C71 H71C 108.8 . . ? C72 C71 H71D 108.8 . . ? C70 C71 H71D 108.8 . . ? H71C C71 H71D 107.7 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.161 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.090