Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_1_free-base _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C133 H148 N16 O22' _chemical_formula_weight 2322.67 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.8938(7) _cell_length_b 22.5940(10) _cell_length_c 35.296(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.776(4) _cell_angle_gamma 90.00 _cell_volume 11627.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4936 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Saphire 3 Xcalibur' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 19.64 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 80307 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0916 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11076 _reflns_number_gt 5409 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,Version 1.171.26' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26' _computing_structure_solution 'SIR-97_(Altomare & al., 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON_(Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11076 _refine_ls_number_parameters 762 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1680 _refine_ls_R_factor_gt 0.1095 _refine_ls_wR_factor_ref 0.3504 _refine_ls_wR_factor_gt 0.3279 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.146 _refine_ls_shift/su_max 2.194 _refine_ls_shift/su_mean 0.075 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 O63 O 0.6282(5) 0.5603(3) 0.0492(2) 0.113(2) Uiso 1 1 d . . . H63 H 0.6659 0.5477 0.0677 0.169 Uiso 1 1 calc R . . C64 C 0.5452(13) 0.5300(9) 0.0466(6) 0.244(8) Uiso 1 1 d . . . H64A H 0.5115 0.5444 0.0219 0.293 Uiso 1 1 calc R . . H64B H 0.5190 0.5514 0.0656 0.293 Uiso 1 1 calc R . . C65 C 0.5026(7) 0.4720(4) 0.0481(3) 0.107(3) Uiso 1 1 d . . . H65A H 0.4383 0.4769 0.0474 0.160 Uiso 1 1 calc R . . H65B H 0.5307 0.4522 0.0716 0.160 Uiso 1 1 calc R . . H65C H 0.5110 0.4487 0.0263 0.160 Uiso 1 1 calc R . . C67 C 0.5000 0.5238(8) 0.2500 0.144(6) Uiso 1 2 d S . . H67A H 0.5022 0.5500 0.2284 0.173 Uiso 0.50 1 calc PR . . H67B H 0.4978 0.5500 0.2716 0.173 Uiso 0.50 1 calc PR . . C68 C 0.4003(6) 0.4991(4) 0.2397(3) 0.079(2) Uiso 1 1 d . . . H68A H 0.4026 0.4696 0.2199 0.095 Uiso 1 1 calc R . . H68B H 0.3939 0.4769 0.2625 0.095 Uiso 1 1 calc R . . C69 C 0.3358(12) 0.5194(8) 0.2305(5) 0.211(7) Uiso 1 1 d . . . H69A H 0.2889 0.4895 0.2258 0.317 Uiso 1 1 calc R . . H69B H 0.3353 0.5411 0.2071 0.317 Uiso 1 1 calc R . . H69C H 0.3244 0.5459 0.2502 0.317 Uiso 1 1 calc R . . O1 O 0.8971(2) 0.36094(17) -0.05460(11) 0.0382(9) Uani 1 1 d . . . O2 O 0.6413(3) 0.35333(17) -0.01203(11) 0.0456(10) Uani 1 1 d . . . O3 O 0.5747(2) 0.33088(16) 0.05553(11) 0.0392(10) Uani 1 1 d . . . O4 O 0.8568(3) 0.3899(2) 0.06397(12) 0.0635(14) Uani 1 1 d D . . O5 O 0.7754(3) 0.2800(2) 0.12489(13) 0.0571(12) Uani 1 1 d D . . O6 O 0.5357(2) 0.34665(18) 0.17098(11) 0.0448(10) Uani 1 1 d . A . O7 O 1.1868(3) 0.01870(17) 0.15690(14) 0.0567(12) Uani 1 1 d . . . O8 O 0.8543(2) 0.01014(16) 0.13079(12) 0.0455(10) Uani 1 1 d . . . N1 N 1.0498(3) 0.29236(18) 0.12213(12) 0.0292(10) Uani 1 1 d . . . N2 N 0.9541(3) 0.28160(17) 0.18512(12) 0.0290(10) Uani 1 1 d . . . H2 H 0.9766 0.3098 0.1736 0.035 Uiso 1 1 calc R . . N3 N 0.9505(3) 0.41060(17) 0.18749(12) 0.0279(10) Uani 1 1 d . . . N4 N 1.0482(3) 0.42209(17) 0.12519(11) 0.0273(10) Uani 1 1 d . . . H4 H 1.0316 0.3938 0.1385 0.033 Uiso 1 1 calc R . . N5 N 0.9742(3) 0.39036(19) 0.00512(12) 0.0312(10) Uani 1 1 d . . . H5 H 0.9658 0.4019 0.0273 0.037 Uiso 1 1 calc R . . N6 N 0.8230(3) 0.4173(2) -0.01789(13) 0.0392(12) Uani 1 1 d . A . N7 N 0.5873(3) 0.2756(2) 0.13516(13) 0.0378(12) Uani 1 1 d . A . N8 N 0.6823(3) 0.31113(18) 0.19018(12) 0.0324(11) Uani 1 1 d . A . H8 H 0.7269 0.2981 0.1805 0.039 Uiso 1 1 calc R . . C1 C 1.0813(3) 0.3041(2) 0.08932(15) 0.0285(12) Uani 1 1 d . . . C2 C 1.0974(4) 0.2504(2) 0.06965(17) 0.0388(14) Uani 1 1 d . . . H2A H 1.1185 0.2475 0.0467 0.047 Uiso 1 1 calc R . . C3 C 1.0759(4) 0.2053(2) 0.09106(17) 0.0411(14) Uani 1 1 d . . . H3A H 1.0796 0.1651 0.0858 0.049 Uiso 1 1 calc R . . C4 C 1.0456(3) 0.2316(2) 0.12402(16) 0.0325(13) Uani 1 1 d . . . C5 C 1.0109(3) 0.1981(2) 0.15176(15) 0.0319(13) Uani 1 1 d . . . C6 C 0.9677(3) 0.2226(2) 0.17943(15) 0.0318(13) Uani 1 1 d . . . C7 C 0.9231(4) 0.1914(3) 0.20611(17) 0.0406(14) Uani 1 1 d . . . H7 H 0.9234 0.1507 0.2100 0.049 Uiso 1 1 calc R . . C8 C 0.8804(4) 0.2326(2) 0.22466(16) 0.0365(14) Uani 1 1 d . . . H8A H 0.8447 0.2246 0.2428 0.044 Uiso 1 1 calc R . . C9 C 0.8996(3) 0.2894(2) 0.21161(15) 0.0296(12) Uani 1 1 d . . . C10 C 0.8679(3) 0.3432(2) 0.22354(15) 0.0296(12) Uani 1 1 d . . . C11 C 0.8952(3) 0.3994(2) 0.21320(15) 0.0300(12) Uani 1 1 d . . . C12 C 0.8696(4) 0.4540(2) 0.23007(16) 0.0363(13) Uani 1 1 d . . . H12 H 0.8329 0.4576 0.2483 0.044 Uiso 1 1 calc R . . C13 C 0.9090(4) 0.4979(2) 0.21421(16) 0.0398(14) Uani 1 1 d . . . H13 H 0.9053 0.5382 0.2193 0.048 Uiso 1 1 calc R . . C14 C 0.9587(3) 0.4705(2) 0.18748(15) 0.0321(13) Uani 1 1 d . . . C15 C 1.0027(4) 0.5039(2) 0.16254(16) 0.0381(14) Uani 1 1 d . . . C16 C 1.0430(3) 0.4808(2) 0.13355(15) 0.0313(12) Uani 1 1 d . . . C17 C 1.0795(4) 0.5124(2) 0.10559(16) 0.0365(13) Uani 1 1 d . . . H17 H 1.0861 0.5532 0.1045 0.044 Uiso 1 1 calc R . . C18 C 1.1035(3) 0.4724(2) 0.08037(15) 0.0320(12) Uani 1 1 d . . . H18 H 1.1284 0.4815 0.0590 0.038 Uiso 1 1 calc R . . C19 C 1.0839(3) 0.4145(2) 0.09246(14) 0.0283(12) Uani 1 1 d . . . C20 C 1.0972(3) 0.3611(2) 0.07514(14) 0.0284(12) Uani 1 1 d . . . C21 C 1.1271(3) 0.3631(2) 0.03702(15) 0.0290(12) Uani 1 1 d . . . C22 C 1.2176(4) 0.3503(3) 0.03507(17) 0.0441(15) Uani 1 1 d . . . H22 H 1.2601 0.3425 0.0577 0.053 Uiso 1 1 calc R . . C23 C 1.2451(4) 0.3490(3) -0.00024(19) 0.0578(19) Uani 1 1 d . . . H23 H 1.3056 0.3402 -0.0012 0.069 Uiso 1 1 calc R . . C24 C 1.1829(4) 0.3606(3) -0.03349(19) 0.0559(18) Uani 1 1 d . . . H24 H 1.2010 0.3590 -0.0572 0.067 Uiso 1 1 calc R . . C25 C 1.0930(4) 0.3748(3) -0.03236(16) 0.0389(14) Uani 1 1 d . . . H25 H 1.0517 0.3838 -0.0552 0.047 Uiso 1 1 calc R . . C26 C 1.0643(3) 0.3757(2) 0.00244(15) 0.0286(12) Uani 1 1 d . . . C27 C 0.8979(3) 0.3880(2) -0.02451(16) 0.0284(12) Uani 1 1 d . . . C28 C 0.7362(4) 0.4077(3) -0.04641(17) 0.0472(16) Uani 1 1 d . . . H28A H 0.7490 0.4104 -0.0722 0.057 Uiso 1 1 calc R . . H28B H 0.6940 0.4394 -0.0437 0.057 Uiso 1 1 calc R . . C29 C 0.6902(4) 0.3501(3) -0.04271(17) 0.0471(16) Uani 1 1 d . . . H29A H 0.6482 0.3409 -0.0668 0.057 Uiso 1 1 calc R . . H29B H 0.7357 0.3189 -0.0375 0.057 Uiso 1 1 calc R . . C30 C 0.6103(4) 0.2953(3) -0.00286(18) 0.0430(15) Uani 1 1 d . . . H30A H 0.6613 0.2730 0.0119 0.052 Uiso 1 1 calc R . . H30B H 0.5863 0.2738 -0.0266 0.052 Uiso 1 1 calc R . . C31 C 0.5382(4) 0.3018(3) 0.01982(17) 0.0439(15) Uani 1 1 d . . . H31A H 0.4878 0.3247 0.0052 0.053 Uiso 1 1 calc R . . H31B H 0.5150 0.2631 0.0249 0.053 Uiso 1 1 calc R . . C32 C 0.5084(4) 0.3365(3) 0.07983(18) 0.0467(16) Uani 1 1 d . . . H32A H 0.4482 0.3428 0.0637 0.056 Uiso 1 1 calc R . . H32B H 0.5233 0.3710 0.0963 0.056 Uiso 1 1 calc R . . C33 C 0.5055(4) 0.2825(3) 0.10491(17) 0.0550(18) Uani 1 1 d . . . H33A H 0.4524 0.2853 0.1168 0.066 Uiso 1 1 calc R . . H33B H 0.4981 0.2475 0.0887 0.066 Uiso 1 1 calc R . . C34 C 0.8244(5) 0.4603(3) 0.01325(19) 0.0589(19) Uani 1 1 d . . . H34A H 0.7845 0.4931 0.0034 0.071 Uiso 1 1 calc R A . H34B H 0.8862 0.4758 0.0212 0.071 Uiso 1 1 calc R . . C35 C 0.7946(5) 0.4351(4) 0.0479(2) 0.083(3) Uani 1 1 d . A . H35A H 0.7937 0.4659 0.0669 0.100 Uiso 1 1 calc R . . H35B H 0.7332 0.4189 0.0404 0.100 Uiso 1 1 calc R . . C36A C 0.8301(9) 0.3279(5) 0.0766(4) 0.037(4) Uani 0.522(11) 1 d PD A 1 H36A H 0.7872 0.3095 0.0555 0.045 Uiso 0.522(11) 1 calc PR A 1 H36B H 0.8844 0.3031 0.0826 0.045 Uiso 0.522(11) 1 calc PR A 1 C36B C 0.7880(8) 0.3324(5) 0.1110(4) 0.028(3) Uani 0.478(11) 1 d PD A 1 H36C H 0.8273 0.3557 0.1307 0.034 Uiso 0.478(11) 1 calc PR A 1 H36D H 0.7295 0.3526 0.1039 0.034 Uiso 0.478(11) 1 calc PR A 1 C37A C 0.8131(11) 0.3089(8) 0.0912(6) 0.054(5) Uani 0.522(11) 1 d P A 2 H37A H 0.8747 0.2945 0.0917 0.065 Uiso 0.522(11) 1 calc PR A 2 H37B H 0.7748 0.2974 0.0666 0.065 Uiso 0.522(11) 1 calc PR A 2 C37B C 0.8148(9) 0.3752(7) 0.0943(4) 0.053(4) Uani 0.478(11) 1 d P A 2 H37C H 0.7535 0.3915 0.0907 0.063 Uiso 0.478(11) 1 calc PR A 2 H37D H 0.8507 0.3883 0.1190 0.063 Uiso 0.478(11) 1 calc PR A 2 C38 C 0.7167(4) 0.2346(2) 0.10910(17) 0.0394(14) Uani 1 1 d . A . H38A H 0.7516 0.1986 0.1078 0.047 Uiso 1 1 calc R . . H38B H 0.6858 0.2450 0.0830 0.047 Uiso 1 1 calc R . . C39 C 0.6470(4) 0.2242(2) 0.13378(18) 0.0454(16) Uani 1 1 d . . . H39A H 0.6093 0.1905 0.1237 0.054 Uiso 1 1 calc R A . H39B H 0.6787 0.2146 0.1599 0.054 Uiso 1 1 calc R . . C40 C 0.5982(3) 0.3132(2) 0.16624(16) 0.0333(13) Uani 1 1 d . . . C41 C 0.7030(3) 0.3285(2) 0.22945(16) 0.0317(13) Uani 1 1 d . . . C42 C 0.6370(3) 0.3308(2) 0.25200(16) 0.0354(14) Uani 1 1 d . A . H42 H 0.5762 0.3227 0.2407 0.042 Uiso 1 1 calc R . . C43 C 0.6592(4) 0.3447(3) 0.29023(18) 0.0440(15) Uani 1 1 d . . . H43 H 0.6135 0.3466 0.3046 0.053 Uiso 1 1 calc R A . C44 C 0.7482(4) 0.3558(3) 0.30772(18) 0.0498(17) Uani 1 1 d . A . H44 H 0.7629 0.3649 0.3339 0.060 Uiso 1 1 calc R . . C45 C 0.8158(4) 0.3534(3) 0.28650(16) 0.0380(14) Uani 1 1 d . . . H45 H 0.8764 0.3604 0.2986 0.046 Uiso 1 1 calc R A . C46 C 0.7952(3) 0.3406(2) 0.24730(16) 0.0331(13) Uani 1 1 d . A . C47 C 1.0140(4) 0.1325(2) 0.14892(15) 0.0323(13) Uani 1 1 d . . . C48 C 1.0978(4) 0.1036(2) 0.15400(18) 0.0433(15) Uani 1 1 d . . . H48 H 1.1522 0.1252 0.1589 0.052 Uiso 1 1 calc R . . C49 C 1.1000(4) 0.0427(2) 0.15170(18) 0.0438(15) Uani 1 1 d . . . C50 C 1.0203(4) 0.0088(2) 0.14425(17) 0.0397(14) Uani 1 1 d . . . H50 H 1.0230 -0.0323 0.1429 0.048 Uiso 1 1 calc R . . C51 C 0.9362(4) 0.0382(2) 0.13895(16) 0.0361(13) Uani 1 1 d . . . C52 C 0.9328(4) 0.0996(2) 0.14121(16) 0.0363(13) Uani 1 1 d . . . H52 H 0.8765 0.1188 0.1376 0.044 Uiso 1 1 calc R . . C53 C 1.1939(4) -0.0435(3) 0.1526(2) 0.067(2) Uani 1 1 d . . . H53A H 1.2574 -0.0545 0.1567 0.101 Uiso 1 1 calc R . . H53B H 1.1635 -0.0548 0.1270 0.101 Uiso 1 1 calc R . . H53C H 1.1655 -0.0632 0.1712 0.101 Uiso 1 1 calc R . . C54 C 0.8538(4) -0.0518(2) 0.1232(2) 0.0587(19) Uani 1 1 d . . . H54A H 0.7918 -0.0661 0.1181 0.088 Uiso 1 1 calc R . . H54B H 0.8887 -0.0720 0.1454 0.088 Uiso 1 1 calc R . . H54C H 0.8806 -0.0591 0.1012 0.088 Uiso 1 1 calc R . . C55 C 0.9957(5) 0.5692(3) 0.1666(2) 0.058(2) Uani 1 1 d . . . C56 C 0.9194(6) 0.5997(3) 0.1484(2) 0.080(3) Uani 1 1 d . . . H56A H 0.8773 0.5792 0.1300 0.096 Uiso 1 1 calc R . . C57 C 0.8994(6) 0.6576(3) 0.1549(3) 0.078(3) Uani 1 1 d . . . C58 C 0.9565(7) 0.6858(4) 0.1792(2) 0.089(4) Uani 1 1 d . . . H58 H 0.9432 0.7251 0.1835 0.107 Uiso 1 1 calc R . . C59 C 1.0408(7) 0.6623(4) 0.2010(2) 0.075(3) Uani 1 1 d . . . C60 C 1.0658(7) 0.5966(3) 0.1945(2) 0.086(3) Uani 1 1 d . . . H60A H 1.1192 0.5779 0.2071 0.103 Uiso 1 1 calc R . . C61 C 0.7907(6) 0.7361(4) 0.1472(3) 0.095(3) Uani 1 1 d . . . H61A H 0.7339 0.7478 0.1308 0.114 Uiso 1 1 calc R . . H61B H 0.8366 0.7656 0.1463 0.114 Uiso 1 1 calc R . . H61C H 0.7820 0.7321 0.1733 0.114 Uiso 1 1 calc R . . C62 C 1.1792(4) 0.6651(3) 0.24787(18) 0.0416(15) Uani 1 1 d . . . H62A H 1.2125 0.6944 0.2649 0.050 Uiso 1 1 calc R . . H62B H 1.2167 0.6510 0.2307 0.050 Uiso 1 1 calc R . . H62C H 1.1634 0.6327 0.2628 0.050 Uiso 1 1 calc R . . O9 O 0.8180(3) 0.6838(2) 0.13497(17) 0.0795(16) Uani 1 1 d . . . O10 O 1.0949(5) 0.6918(2) 0.22515(18) 0.0929(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.036(2) 0.048(2) 0.030(2) -0.0026(19) 0.0051(18) -0.0054(17) O2 0.041(2) 0.054(3) 0.046(3) 0.005(2) 0.018(2) 0.0057(19) O3 0.035(2) 0.047(2) 0.036(2) -0.0045(18) 0.0087(19) -0.0050(17) O4 0.042(3) 0.114(4) 0.036(3) 0.002(3) 0.011(2) -0.017(3) O5 0.042(2) 0.074(3) 0.060(3) -0.025(3) 0.021(2) -0.021(2) O6 0.034(2) 0.061(3) 0.042(3) -0.001(2) 0.0120(19) 0.0082(19) O7 0.037(2) 0.033(2) 0.097(4) -0.003(2) 0.005(2) 0.0100(18) O8 0.037(2) 0.034(2) 0.063(3) 0.003(2) 0.004(2) -0.0029(17) N1 0.027(2) 0.029(2) 0.032(3) -0.001(2) 0.007(2) -0.0009(18) N2 0.028(2) 0.024(2) 0.037(3) -0.0015(19) 0.011(2) -0.0013(17) N3 0.027(2) 0.027(2) 0.031(3) 0.0000(19) 0.008(2) 0.0029(17) N4 0.031(2) 0.026(2) 0.026(3) 0.0043(18) 0.010(2) 0.0021(18) N5 0.029(2) 0.041(3) 0.024(3) -0.008(2) 0.006(2) 0.0001(19) N6 0.029(3) 0.061(3) 0.026(3) 0.006(2) 0.003(2) 0.011(2) N7 0.034(3) 0.049(3) 0.031(3) -0.004(2) 0.009(2) -0.009(2) N8 0.031(2) 0.036(3) 0.032(3) -0.005(2) 0.010(2) 0.0004(19) C1 0.025(3) 0.030(3) 0.031(3) -0.003(2) 0.007(2) -0.003(2) C2 0.044(3) 0.034(3) 0.043(4) -0.007(3) 0.021(3) -0.003(2) C3 0.049(4) 0.030(3) 0.047(4) -0.008(3) 0.018(3) 0.002(3) C4 0.027(3) 0.029(3) 0.042(4) 0.000(2) 0.008(3) -0.001(2) C5 0.027(3) 0.033(3) 0.035(3) 0.002(2) 0.005(3) 0.004(2) C6 0.031(3) 0.030(3) 0.034(3) 0.005(2) 0.003(3) -0.003(2) C7 0.046(3) 0.036(3) 0.041(4) 0.006(3) 0.010(3) -0.007(3) C8 0.041(3) 0.036(3) 0.036(3) -0.003(3) 0.016(3) -0.005(3) C9 0.027(3) 0.030(3) 0.033(3) 0.000(2) 0.008(3) -0.005(2) C10 0.026(3) 0.039(3) 0.024(3) -0.003(2) 0.006(2) -0.003(2) C11 0.031(3) 0.034(3) 0.025(3) 0.000(2) 0.006(2) -0.001(2) C12 0.037(3) 0.037(3) 0.038(3) -0.005(3) 0.014(3) 0.005(2) C13 0.055(4) 0.030(3) 0.038(4) -0.005(3) 0.019(3) 0.003(3) C14 0.037(3) 0.028(3) 0.032(3) 0.001(2) 0.010(3) 0.003(2) C15 0.051(3) 0.029(3) 0.038(3) -0.002(2) 0.018(3) 0.002(2) C16 0.036(3) 0.027(3) 0.031(3) 0.000(2) 0.008(3) 0.003(2) C17 0.048(3) 0.026(3) 0.039(3) 0.006(2) 0.016(3) 0.000(2) C18 0.036(3) 0.033(3) 0.029(3) 0.005(2) 0.012(3) 0.000(2) C19 0.025(3) 0.034(3) 0.025(3) 0.003(2) 0.003(2) 0.001(2) C20 0.025(3) 0.034(3) 0.026(3) -0.003(2) 0.006(2) 0.002(2) C21 0.029(3) 0.029(3) 0.031(3) -0.004(2) 0.012(3) -0.002(2) C22 0.033(3) 0.068(4) 0.033(4) 0.000(3) 0.009(3) 0.005(3) C23 0.034(3) 0.101(6) 0.042(4) -0.003(4) 0.016(3) 0.016(3) C24 0.044(4) 0.096(6) 0.032(4) -0.004(3) 0.017(3) 0.001(3) C25 0.037(3) 0.050(4) 0.031(3) -0.001(3) 0.009(3) -0.002(3) C26 0.028(3) 0.029(3) 0.030(3) -0.005(2) 0.008(3) -0.003(2) C27 0.029(3) 0.030(3) 0.027(3) 0.002(2) 0.007(3) 0.001(2) C28 0.039(3) 0.064(4) 0.039(4) 0.010(3) 0.012(3) 0.004(3) C29 0.035(3) 0.077(5) 0.031(4) 0.003(3) 0.008(3) -0.002(3) C30 0.040(3) 0.048(4) 0.041(4) 0.008(3) 0.008(3) 0.007(3) C31 0.048(4) 0.049(4) 0.037(4) -0.001(3) 0.013(3) -0.006(3) C32 0.034(3) 0.065(4) 0.042(4) -0.012(3) 0.009(3) 0.006(3) C33 0.042(4) 0.090(5) 0.032(4) -0.008(3) 0.006(3) -0.029(3) C34 0.057(4) 0.067(5) 0.053(5) -0.015(4) 0.011(4) 0.022(3) C35 0.038(4) 0.168(9) 0.047(5) -0.028(5) 0.014(4) 0.012(5) C36A 0.029(7) 0.039(9) 0.046(9) 0.008(6) 0.014(6) 0.002(6) C36B 0.027(6) 0.033(7) 0.025(7) -0.004(6) 0.004(6) 0.008(5) C37A 0.033(8) 0.065(13) 0.064(13) 0.000(10) 0.013(8) -0.011(7) C37B 0.058(9) 0.076(11) 0.033(8) 0.018(7) 0.029(7) 0.020(7) C38 0.045(3) 0.035(3) 0.040(4) -0.010(3) 0.011(3) -0.005(3) C39 0.063(4) 0.034(3) 0.043(4) -0.010(3) 0.019(3) -0.017(3) C40 0.026(3) 0.044(3) 0.032(3) -0.006(3) 0.009(3) -0.010(2) C41 0.035(3) 0.029(3) 0.033(3) -0.003(2) 0.010(3) -0.003(2) C42 0.026(3) 0.043(3) 0.039(4) -0.006(3) 0.012(3) -0.009(2) C43 0.034(3) 0.063(4) 0.039(4) -0.010(3) 0.016(3) -0.005(3) C44 0.042(4) 0.073(5) 0.039(4) -0.016(3) 0.018(3) -0.012(3) C45 0.029(3) 0.057(4) 0.029(3) -0.007(3) 0.008(3) -0.009(3) C46 0.027(3) 0.038(3) 0.037(4) -0.003(3) 0.012(3) -0.004(2) C47 0.035(3) 0.029(3) 0.033(3) 0.003(2) 0.006(3) 0.000(2) C48 0.036(3) 0.034(3) 0.061(4) 0.002(3) 0.011(3) -0.001(2) C49 0.039(3) 0.032(3) 0.059(4) 0.005(3) 0.007(3) 0.006(3) C50 0.035(3) 0.027(3) 0.057(4) 0.001(3) 0.007(3) 0.006(2) C51 0.037(3) 0.030(3) 0.038(4) 0.001(2) 0.001(3) -0.005(2) C52 0.033(3) 0.033(3) 0.043(4) 0.003(3) 0.009(3) 0.005(2) C53 0.048(4) 0.042(4) 0.102(6) -0.018(4) -0.008(4) 0.019(3) C54 0.047(4) 0.029(3) 0.093(6) 0.003(3) -0.001(4) -0.009(3) C55 0.103(6) 0.026(3) 0.063(5) 0.003(3) 0.058(5) 0.001(4) C56 0.123(7) 0.040(4) 0.098(6) 0.026(4) 0.072(6) 0.037(4) C57 0.107(7) 0.051(5) 0.093(7) 0.000(4) 0.058(6) 0.005(5) C58 0.128(8) 0.117(7) 0.039(5) -0.053(5) 0.052(5) -0.112(7) C59 0.083(6) 0.104(7) 0.043(5) -0.016(4) 0.024(5) -0.063(5) C60 0.167(9) 0.048(4) 0.066(5) -0.020(4) 0.082(6) -0.049(5) C61 0.090(6) 0.059(5) 0.136(8) -0.007(5) 0.026(6) 0.007(5) C62 0.038(3) 0.041(3) 0.041(4) -0.003(3) -0.002(3) -0.015(3) O9 0.059(3) 0.062(3) 0.110(5) -0.001(3) 0.000(3) 0.029(3) O10 0.120(5) 0.074(4) 0.094(5) -0.011(3) 0.045(4) -0.037(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O63 C64 1.401(18) . ? O63 H63 0.8200 . ? C64 C65 1.462(19) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C67 C68 1.559(10) 2_655 ? C67 C68 1.559(10) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 C69 1.054(16) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? O1 C27 1.223(6) . ? O2 C29 1.425(6) . ? O2 C30 1.450(7) . ? O3 C31 1.427(7) . ? O3 C32 1.439(6) . ? O4 C35 1.418(9) . ? O4 C37B 1.387(12) . ? O4 C36A 1.546(11) . ? O5 C36B 1.309(10) . ? O5 C38 1.390(6) . ? O5 C37A 1.559(19) . ? O6 C40 1.237(6) . ? O7 C49 1.381(6) . ? O7 C53 1.419(7) . ? O8 C51 1.352(6) . ? O8 C54 1.424(7) . ? N1 C1 1.362(6) . ? N1 C4 1.377(6) . ? N2 C9 1.368(6) . ? N2 C6 1.368(6) . ? N2 H2 0.8600 . ? N3 C11 1.368(6) . ? N3 C14 1.360(6) . ? N4 C16 1.366(6) . ? N4 C19 1.377(6) . ? N4 H4 0.8600 . ? N5 C27 1.379(7) . ? N5 C26 1.404(6) . ? N5 H5 0.8600 . ? N6 C27 1.358(6) . ? N6 C28 1.484(7) . ? N6 C34 1.464(7) . ? N7 C40 1.370(7) . ? N7 C33 1.455(7) . ? N7 C39 1.470(7) . ? N8 C40 1.361(7) . ? N8 C41 1.413(7) . ? N8 H8 0.8600 . ? C1 C20 1.418(7) . ? C1 C2 1.443(7) . ? C2 C3 1.346(7) . ? C2 H2A 0.9300 . ? C3 C4 1.457(7) . ? C3 H3A 0.9300 . ? C4 C5 1.417(7) . ? C5 C6 1.390(7) . ? C5 C47 1.487(7) . ? C6 C7 1.442(7) . ? C7 C8 1.368(8) . ? C7 H7 0.9300 . ? C8 C9 1.413(7) . ? C8 H8A 0.9300 . ? C9 C10 1.399(7) . ? C10 C11 1.405(7) . ? C10 C46 1.499(7) . ? C11 C12 1.455(7) . ? C12 C13 1.332(7) . ? C12 H12 0.9300 . ? C13 C14 1.452(7) . ? C13 H13 0.9300 . ? C14 C15 1.417(7) . ? C15 C16 1.390(7) . ? C15 C55 1.488(8) . ? C16 C17 1.413(7) . ? C17 C18 1.365(7) . ? C17 H17 0.9300 . ? C18 C19 1.425(7) . ? C18 H18 0.9300 . ? C19 C20 1.386(7) . ? C20 C21 1.502(7) . ? C21 C22 1.394(7) . ? C21 C26 1.407(7) . ? C22 C23 1.390(8) . ? C22 H22 0.9300 . ? C23 C24 1.364(9) . ? C23 H23 0.9300 . ? C24 C25 1.386(8) . ? C24 H24 0.9300 . ? C25 C26 1.381(7) . ? C25 H25 0.9300 . ? C28 C29 1.488(8) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.471(8) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.513(9) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.497(10) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36A C36B 1.479(18) . ? C36A H36A 0.9700 . ? C36A H36B 0.9700 . ? C36B H36C 0.9700 . ? C36B H36D 0.9700 . ? C37A C37B 1.50(2) . ? C37A H37A 0.9700 . ? C37A H37B 0.9700 . ? C37B H37C 0.9700 . ? C37B H37D 0.9700 . ? C38 C39 1.503(8) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C41 C46 1.416(7) . ? C41 C42 1.387(7) . ? C42 C43 1.359(8) . ? C42 H42 0.9300 . ? C43 C44 1.366(8) . ? C43 H43 0.9300 . ? C44 C45 1.373(7) . ? C44 H44 0.9300 . ? C45 C46 1.385(8) . ? C45 H45 0.9300 . ? C47 C48 1.387(7) . ? C47 C52 1.398(7) . ? C48 C49 1.379(8) . ? C48 H48 0.9300 . ? C49 C50 1.393(8) . ? C50 C51 1.396(7) . ? C50 H50 0.9300 . ? C51 C52 1.392(7) . ? C52 H52 0.9300 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C60 1.423(11) . ? C55 C56 1.370(10) . ? C56 C57 1.372(9) . ? C56 H56A 0.9300 . ? C57 C58 1.253(11) . ? C57 O9 1.402(10) . ? C58 C59 1.433(13) . ? C58 H58 0.9300 . ? C59 O10 1.242(9) . ? C59 C60 1.558(11) . ? C60 H60A 0.9300 . ? C61 O9 1.349(8) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 O10 1.474(8) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C64 O63 H63 109.1 . . ? O63 C64 C65 145.1(16) . . ? O63 C64 H64A 101.5 . . ? C65 C64 H64A 101.5 . . ? O63 C64 H64B 99.5 . . ? C65 C64 H64B 99.6 . . ? H64A C64 H64B 104.7 . . ? C64 C65 H65A 111.5 . . ? C64 C65 H65B 109.3 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 107.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C68 C67 C68 138.0(14) 2_655 . ? C68 C67 H67A 102.5 2_655 . ? C68 C67 H67A 102.7 . . ? C68 C67 H67B 102.7 2_655 . ? C68 C67 H67B 102.5 . . ? H67A C67 H67B 105.0 . . ? C69 C68 C67 133.0(15) . . ? C69 C68 H68A 104.3 . . ? C67 C68 H68A 103.8 . . ? C69 C68 H68B 103.9 . . ? C67 C68 H68B 103.9 . . ? H68A C68 H68B 105.4 . . ? C68 C69 H69A 109.1 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.8 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C29 O2 C30 111.1(4) . . ? C31 O3 C32 112.6(4) . . ? C35 O4 C37B 96.9(7) . . ? C35 O4 C36A 125.6(7) . . ? C37B O4 C36A 51.5(8) . . ? C36B O5 C38 130.1(7) . . ? C36B O5 C37A 40.0(8) . . ? C38 O5 C37A 107.4(8) . . ? C49 O7 C53 117.6(5) . . ? C51 O8 C54 118.0(4) . . ? C1 N1 C4 105.2(4) . . ? C9 N2 C6 110.6(4) . . ? C9 N2 H2 124.7 . . ? C6 N2 H2 124.7 . . ? C11 N3 C14 104.5(4) . . ? C16 N4 C19 110.5(4) . . ? C16 N4 H4 124.7 . . ? C19 N4 H4 124.7 . . ? C27 N5 C26 126.2(4) . . ? C27 N5 H5 116.9 . . ? C26 N5 H5 116.9 . . ? C27 N6 C28 116.4(5) . . ? C27 N6 C34 124.6(5) . . ? C28 N6 C34 118.9(5) . . ? C40 N7 C33 117.8(5) . . ? C40 N7 C39 122.9(5) . . ? C33 N7 C39 118.8(5) . . ? C40 N8 C41 126.1(4) . . ? C40 N8 H8 116.9 . . ? C41 N8 H8 117.0 . . ? N1 C1 C20 126.1(4) . . ? N1 C1 C2 111.4(4) . . ? C20 C1 C2 122.5(5) . . ? C3 C2 C1 106.6(5) . . ? C3 C2 H2A 126.7 . . ? C1 C2 H2A 126.7 . . ? C2 C3 C4 106.7(5) . . ? C2 C3 H3A 126.7 . . ? C4 C3 H3A 126.6 . . ? N1 C4 C5 126.4(5) . . ? N1 C4 C3 110.1(4) . . ? C5 C4 C3 123.3(5) . . ? C6 C5 C4 124.0(5) . . ? C6 C5 C47 118.1(4) . . ? C4 C5 C47 117.7(4) . . ? N2 C6 C5 126.6(5) . . ? N2 C6 C7 106.2(4) . . ? C5 C6 C7 127.1(5) . . ? C8 C7 C6 107.5(5) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.3 . . ? C7 C8 C9 108.5(5) . . ? C7 C8 H8A 125.7 . . ? C9 C8 H8A 125.7 . . ? N2 C9 C10 127.0(4) . . ? N2 C9 C8 107.0(4) . . ? C10 C9 C8 126.0(5) . . ? C11 C10 C9 125.0(4) . . ? C11 C10 C46 117.5(4) . . ? C9 C10 C46 117.5(4) . . ? N3 C11 C10 125.8(4) . . ? N3 C11 C12 111.0(4) . . ? C10 C11 C12 123.1(4) . . ? C13 C12 C11 106.5(5) . . ? C13 C12 H12 126.7 . . ? C11 C12 H12 126.7 . . ? C12 C13 C14 106.4(5) . . ? C12 C13 H13 126.8 . . ? C14 C13 H13 126.8 . . ? N3 C14 C15 125.7(5) . . ? N3 C14 C13 111.5(4) . . ? C15 C14 C13 122.6(5) . . ? C16 C15 C14 125.6(5) . . ? C16 C15 C55 119.5(5) . . ? C14 C15 C55 114.7(4) . . ? N4 C16 C15 125.2(5) . . ? N4 C16 C17 107.0(4) . . ? C15 C16 C17 127.7(5) . . ? C18 C17 C16 108.2(5) . . ? C18 C17 H17 125.9 . . ? C16 C17 H17 125.9 . . ? C17 C18 C19 108.3(4) . . ? C17 C18 H18 125.8 . . ? C19 C18 H18 125.8 . . ? N4 C19 C20 126.4(4) . . ? N4 C19 C18 106.0(4) . . ? C20 C19 C18 127.7(5) . . ? C19 C20 C1 125.9(4) . . ? C19 C20 C21 117.6(4) . . ? C1 C20 C21 116.5(4) . . ? C22 C21 C26 118.5(5) . . ? C22 C21 C20 120.3(5) . . ? C26 C21 C20 121.1(4) . . ? C21 C22 C23 120.9(6) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.6 . . ? C24 C23 C22 119.6(5) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 120.7(5) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.6 . . ? C24 C25 C26 120.4(6) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 119.8(5) . . ? C25 C26 N5 122.5(5) . . ? C21 C26 N5 117.7(4) . . ? O1 C27 N6 122.0(5) . . ? O1 C27 N5 122.6(4) . . ? N6 C27 N5 115.3(5) . . ? N6 C28 C29 114.9(5) . . ? N6 C28 H28A 108.5 . . ? C29 C28 H28A 108.5 . . ? N6 C28 H28B 108.6 . . ? C29 C28 H28B 108.6 . . ? H28A C28 H28B 107.5 . . ? O2 C29 C28 109.7(5) . . ? O2 C29 H29A 109.7 . . ? C28 C29 H29A 109.8 . . ? O2 C29 H29B 109.7 . . ? C28 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? O2 C30 C31 109.4(5) . . ? O2 C30 H30A 109.8 . . ? C31 C30 H30A 109.7 . . ? O2 C30 H30B 109.8 . . ? C31 C30 H30B 109.8 . . ? H30A C30 H30B 108.2 . . ? O3 C31 C30 109.8(5) . . ? O3 C31 H31A 109.7 . . ? C30 C31 H31A 109.7 . . ? O3 C31 H31B 109.7 . . ? C30 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? O3 C32 C33 112.5(5) . . ? O3 C32 H32A 109.1 . . ? C33 C32 H32A 109.1 . . ? O3 C32 H32B 109.1 . . ? C33 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? N7 C33 C32 113.3(5) . . ? N7 C33 H33A 108.9 . . ? C32 C33 H33A 109.0 . . ? N7 C33 H33B 108.9 . . ? C32 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? N6 C34 C35 113.6(6) . . ? N6 C34 H34A 108.8 . . ? C35 C34 H34A 108.8 . . ? N6 C34 H34B 108.9 . . ? C35 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? O4 C35 C34 108.8(5) . . ? O4 C35 H35A 109.9 . . ? C34 C35 H35A 110.0 . . ? O4 C35 H35B 109.9 . . ? C34 C35 H35B 109.9 . . ? H35A C35 H35B 108.3 . . ? C36B C36A O4 110.6(9) . . ? C36B C36A H36A 109.6 . . ? O4 C36A H36A 109.5 . . ? C36B C36A H36B 109.6 . . ? O4 C36A H36B 109.5 . . ? H36A C36A H36B 108.1 . . ? O5 C36B C36A 111.3(11) . . ? O5 C36B H36C 109.4 . . ? C36A C36B H36C 109.4 . . ? O5 C36B H36D 109.4 . . ? C36A C36B H36D 109.4 . . ? H36C C36B H36D 108.0 . . ? C37B C37A O5 111.4(15) . . ? C37B C37A H37A 109.4 . . ? O5 C37A H37A 109.4 . . ? C37B C37A H37B 109.3 . . ? O5 C37A H37B 109.3 . . ? H37A C37A H37B 108.0 . . ? O4 C37B C37A 100.6(12) . . ? O4 C37B H37C 111.6 . . ? C37A C37B H37C 111.7 . . ? O4 C37B H37D 111.7 . . ? C37A C37B H37D 111.6 . . ? H37C C37B H37D 109.5 . . ? O5 C38 C39 109.6(4) . . ? O5 C38 H38A 109.8 . . ? C39 C38 H38A 109.7 . . ? O5 C38 H38B 109.7 . . ? C39 C38 H38B 109.9 . . ? H38A C38 H38B 108.2 . . ? N7 C39 C38 113.0(5) . . ? N7 C39 H39A 109.0 . . ? C38 C39 H39A 109.0 . . ? N7 C39 H39B 109.0 . . ? C38 C39 H39B 109.1 . . ? H39A C39 H39B 107.8 . . ? O6 C40 N7 121.2(5) . . ? O6 C40 N8 124.0(5) . . ? N7 C40 N8 114.8(5) . . ? C46 C41 N8 119.3(4) . . ? C46 C41 C42 118.3(5) . . ? N8 C41 C42 122.3(5) . . ? C43 C42 C41 121.4(5) . . ? C43 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? C42 C43 C44 120.6(5) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C43 C44 C45 119.9(6) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.1 . . ? C44 C45 C46 121.0(5) . . ? C44 C45 H45 119.5 . . ? C46 C45 H45 119.5 . . ? C45 C46 C41 118.8(4) . . ? C45 C46 C10 120.8(5) . . ? C41 C46 C10 120.2(5) . . ? C48 C47 C52 119.7(5) . . ? C48 C47 C5 120.0(5) . . ? C52 C47 C5 120.3(5) . . ? C49 C48 C47 119.5(5) . . ? C49 C48 H48 120.3 . . ? C47 C48 H48 120.3 . . ? C48 C49 O7 114.6(5) . . ? C48 C49 C50 122.2(5) . . ? O7 C49 C50 123.2(5) . . ? C51 C50 C49 118.0(5) . . ? C51 C50 H50 121.0 . . ? C49 C50 H50 121.0 . . ? O8 C51 C52 115.9(5) . . ? O8 C51 C50 123.4(5) . . ? C52 C51 C50 120.6(5) . . ? C51 C52 C47 120.1(5) . . ? C51 C52 H52 120.0 . . ? C47 C52 H52 120.0 . . ? O7 C53 H53A 109.5 . . ? O7 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? O7 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O8 C54 H54A 109.4 . . ? O8 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O8 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C60 C55 C56 121.7(7) . . ? C60 C55 C15 116.2(7) . . ? C56 C55 C15 121.4(7) . . ? C57 C56 C55 126.2(9) . . ? C57 C56 H56A 117.0 . . ? C55 C56 H56A 116.9 . . ? C58 C57 C56 117.2(10) . . ? C58 C57 O9 121.8(8) . . ? C56 C57 O9 121.0(8) . . ? C57 C58 C59 125.3(10) . . ? C57 C58 H58 117.3 . . ? C59 C58 H58 117.4 . . ? O10 C59 C58 122.9(9) . . ? O10 C59 C60 118.2(9) . . ? C58 C59 C60 118.9(7) . . ? C55 C60 C59 110.7(8) . . ? C55 C60 H60A 124.7 . . ? C59 C60 H60A 124.7 . . ? O9 C61 H61A 109.4 . . ? O9 C61 H61B 109.4 . . ? H61A C61 H61B 109.5 . . ? O9 C61 H61C 109.6 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O10 C62 H62A 109.5 . . ? O10 C62 H62B 109.4 . . ? H62A C62 H62B 109.5 . . ? O10 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 O9 C57 119.7(7) . . ? C59 O10 C62 121.0(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C68 C67 C68 C69 -173.5(18) 2_655 . . . ? C4 N1 C1 C20 -179.9(5) . . . . ? C4 N1 C1 C2 0.2(6) . . . . ? N1 C1 C2 C3 -0.4(6) . . . . ? C20 C1 C2 C3 179.7(5) . . . . ? C1 C2 C3 C4 0.4(6) . . . . ? C1 N1 C4 C5 -175.4(5) . . . . ? C1 N1 C4 C3 0.0(6) . . . . ? C2 C3 C4 N1 -0.3(6) . . . . ? C2 C3 C4 C5 175.3(5) . . . . ? N1 C4 C5 C6 6.2(9) . . . . ? C3 C4 C5 C6 -168.7(5) . . . . ? N1 C4 C5 C47 -179.1(5) . . . . ? C3 C4 C5 C47 6.0(8) . . . . ? C9 N2 C6 C5 172.6(5) . . . . ? C9 N2 C6 C7 -3.7(6) . . . . ? C4 C5 C6 N2 -1.9(9) . . . . ? C47 C5 C6 N2 -176.6(5) . . . . ? C4 C5 C6 C7 173.7(5) . . . . ? C47 C5 C6 C7 -1.0(8) . . . . ? N2 C6 C7 C8 3.7(6) . . . . ? C5 C6 C7 C8 -172.6(5) . . . . ? C6 C7 C8 C9 -2.3(6) . . . . ? C6 N2 C9 C10 -177.1(5) . . . . ? C6 N2 C9 C8 2.4(6) . . . . ? C7 C8 C9 N2 0.1(6) . . . . ? C7 C8 C9 C10 179.6(5) . . . . ? N2 C9 C10 C11 -7.4(9) . . . . ? C8 C9 C10 C11 173.2(5) . . . . ? N2 C9 C10 C46 168.9(5) . . . . ? C8 C9 C10 C46 -10.5(8) . . . . ? C14 N3 C11 C10 -179.0(5) . . . . ? C14 N3 C11 C12 -0.9(6) . . . . ? C9 C10 C11 N3 6.0(9) . . . . ? C46 C10 C11 N3 -170.4(5) . . . . ? C9 C10 C11 C12 -172.0(5) . . . . ? C46 C10 C11 C12 11.7(8) . . . . ? N3 C11 C12 C13 0.5(6) . . . . ? C10 C11 C12 C13 178.7(5) . . . . ? C11 C12 C13 C14 0.1(6) . . . . ? C11 N3 C14 C15 -173.7(5) . . . . ? C11 N3 C14 C13 1.0(6) . . . . ? C12 C13 C14 N3 -0.7(7) . . . . ? C12 C13 C14 C15 174.1(5) . . . . ? N3 C14 C15 C16 1.3(9) . . . . ? C13 C14 C15 C16 -172.8(5) . . . . ? N3 C14 C15 C55 175.5(6) . . . . ? C13 C14 C15 C55 1.4(9) . . . . ? C19 N4 C16 C15 173.9(5) . . . . ? C19 N4 C16 C17 -1.8(6) . . . . ? C14 C15 C16 N4 -1.6(9) . . . . ? C55 C15 C16 N4 -175.5(6) . . . . ? C14 C15 C16 C17 173.2(6) . . . . ? C55 C15 C16 C17 -0.7(9) . . . . ? N4 C16 C17 C18 1.7(6) . . . . ? C15 C16 C17 C18 -173.8(5) . . . . ? C16 C17 C18 C19 -1.0(6) . . . . ? C16 N4 C19 C20 -178.6(5) . . . . ? C16 N4 C19 C18 1.2(5) . . . . ? C17 C18 C19 N4 -0.1(6) . . . . ? C17 C18 C19 C20 179.7(5) . . . . ? N4 C19 C20 C1 -3.9(8) . . . . ? C18 C19 C20 C1 176.3(5) . . . . ? N4 C19 C20 C21 173.2(5) . . . . ? C18 C19 C20 C21 -6.6(8) . . . . ? N1 C1 C20 C19 0.5(8) . . . . ? C2 C1 C20 C19 -179.6(5) . . . . ? N1 C1 C20 C21 -176.6(5) . . . . ? C2 C1 C20 C21 3.2(7) . . . . ? C19 C20 C21 C22 104.8(6) . . . . ? C1 C20 C21 C22 -77.8(6) . . . . ? C19 C20 C21 C26 -77.6(6) . . . . ? C1 C20 C21 C26 99.8(6) . . . . ? C26 C21 C22 C23 -1.0(9) . . . . ? C20 C21 C22 C23 176.6(6) . . . . ? C21 C22 C23 C24 0.2(10) . . . . ? C22 C23 C24 C25 1.3(11) . . . . ? C23 C24 C25 C26 -1.9(10) . . . . ? C24 C25 C26 C21 1.1(8) . . . . ? C24 C25 C26 N5 179.4(5) . . . . ? C22 C21 C26 C25 0.4(7) . . . . ? C20 C21 C26 C25 -177.3(5) . . . . ? C22 C21 C26 N5 -178.0(5) . . . . ? C20 C21 C26 N5 4.4(7) . . . . ? C27 N5 C26 C25 21.0(8) . . . . ? C27 N5 C26 C21 -160.7(5) . . . . ? C28 N6 C27 O1 8.8(7) . . . . ? C34 N6 C27 O1 -166.4(5) . . . . ? C28 N6 C27 N5 -170.7(4) . . . . ? C34 N6 C27 N5 14.1(8) . . . . ? C26 N5 C27 O1 15.9(8) . . . . ? C26 N5 C27 N6 -164.7(5) . . . . ? C27 N6 C28 C29 76.4(6) . . . . ? C34 N6 C28 C29 -108.1(6) . . . . ? C30 O2 C29 C28 -169.2(5) . . . . ? N6 C28 C29 O2 79.5(6) . . . . ? C29 O2 C30 C31 -163.0(5) . . . . ? C32 O3 C31 C30 -177.6(5) . . . . ? O2 C30 C31 O3 -62.3(6) . . . . ? C31 O3 C32 C33 86.5(6) . . . . ? C40 N7 C33 C32 73.8(6) . . . . ? C39 N7 C33 C32 -114.8(6) . . . . ? O3 C32 C33 N7 69.5(7) . . . . ? C27 N6 C34 C35 -99.1(7) . . . . ? C28 N6 C34 C35 85.9(7) . . . . ? C37B O4 C35 C34 179.7(9) . . . . ? C36A O4 C35 C34 -133.5(9) . . . . ? N6 C34 C35 O4 62.7(8) . . . . ? C35 O4 C36A C36B -68.5(13) . . . . ? C37B O4 C36A C36B -0.9(10) . . . . ? C38 O5 C36B C36A -67.3(12) . . . . ? C37A O5 C36B C36A -0.6(13) . . . . ? O4 C36A C36B O5 -172.1(8) . . . . ? C36B O5 C37A C37B 5.2(10) . . . . ? C38 O5 C37A C37B 137.7(10) . . . . ? C35 O4 C37B C37A 133.1(10) . . . . ? C36A O4 C37B C37A 2.3(11) . . . . ? O5 C37A C37B O4 175.3(9) . . . . ? C36B O5 C38 C39 -115.5(10) . . . . ? C37A O5 C38 C39 -153.7(8) . . . . ? C40 N7 C39 C38 -103.0(6) . . . . ? C33 N7 C39 C38 86.1(6) . . . . ? O5 C38 C39 N7 63.1(7) . . . . ? C33 N7 C40 O6 9.0(7) . . . . ? C39 N7 C40 O6 -162.1(5) . . . . ? C33 N7 C40 N8 -169.7(4) . . . . ? C39 N7 C40 N8 19.3(7) . . . . ? C41 N8 C40 O6 24.0(8) . . . . ? C41 N8 C40 N7 -157.3(5) . . . . ? C40 N8 C41 C46 -161.3(5) . . . . ? C40 N8 C41 C42 22.5(8) . . . . ? C46 C41 C42 C43 0.4(8) . . . . ? N8 C41 C42 C43 176.6(5) . . . . ? C41 C42 C43 C44 -1.1(9) . . . . ? C42 C43 C44 C45 0.5(10) . . . . ? C43 C44 C45 C46 0.9(9) . . . . ? C44 C45 C46 C41 -1.6(9) . . . . ? C44 C45 C46 C10 174.7(5) . . . . ? N8 C41 C46 C45 -175.4(5) . . . . ? C42 C41 C46 C45 1.0(8) . . . . ? N8 C41 C46 C10 8.3(7) . . . . ? C42 C41 C46 C10 -175.3(5) . . . . ? C11 C10 C46 C45 -76.2(7) . . . . ? C9 C10 C46 C45 107.2(6) . . . . ? C11 C10 C46 C41 100.1(6) . . . . ? C9 C10 C46 C41 -76.5(7) . . . . ? C6 C5 C47 C48 -121.1(6) . . . . ? C4 C5 C47 C48 63.8(7) . . . . ? C6 C5 C47 C52 58.8(7) . . . . ? C4 C5 C47 C52 -116.3(6) . . . . ? C52 C47 C48 C49 -0.6(9) . . . . ? C5 C47 C48 C49 179.3(5) . . . . ? C47 C48 C49 O7 179.5(5) . . . . ? C47 C48 C49 C50 0.2(9) . . . . ? C53 O7 C49 C48 -176.3(6) . . . . ? C53 O7 C49 C50 3.0(9) . . . . ? C48 C49 C50 C51 0.2(9) . . . . ? O7 C49 C50 C51 -179.1(5) . . . . ? C54 O8 C51 C52 172.1(5) . . . . ? C54 O8 C51 C50 -6.8(8) . . . . ? C49 C50 C51 O8 178.6(5) . . . . ? C49 C50 C51 C52 -0.2(8) . . . . ? O8 C51 C52 C47 -179.0(5) . . . . ? C50 C51 C52 C47 -0.1(8) . . . . ? C48 C47 C52 C51 0.5(8) . . . . ? C5 C47 C52 C51 -179.4(5) . . . . ? C16 C15 C55 C60 -96.6(7) . . . . ? C14 C15 C55 C60 88.9(7) . . . . ? C16 C15 C55 C56 92.3(7) . . . . ? C14 C15 C55 C56 -82.3(7) . . . . ? C60 C55 C56 C57 -1.7(11) . . . . ? C15 C55 C56 C57 169.0(6) . . . . ? C55 C56 C57 C58 1.0(11) . . . . ? C55 C56 C57 O9 -178.7(6) . . . . ? C56 C57 C58 C59 -0.3(11) . . . . ? O9 C57 C58 C59 179.5(6) . . . . ? C57 C58 C59 O10 -179.3(7) . . . . ? C57 C58 C59 C60 0.2(10) . . . . ? C56 C55 C60 C59 1.4(8) . . . . ? C15 C55 C60 C59 -169.7(5) . . . . ? O10 C59 C60 C55 178.8(6) . . . . ? C58 C59 C60 C55 -0.7(8) . . . . ? C58 C57 O9 C61 -13.4(11) . . . . ? C56 C57 O9 C61 166.3(7) . . . . ? C58 C59 O10 C62 177.8(6) . . . . ? C60 C59 O10 C62 -1.7(9) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 2.373 _refine_diff_density_min -1.002 _refine_diff_density_rms 0.114 data_1Zn(H2O) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H63 Cl3 N8 O11 Zn' _chemical_formula_weight 1279.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' '-x, -y, -z' 'x-1/2, -y, z' _cell_length_a 23.7550(10) _cell_length_b 8.6928(4) _cell_length_c 30.9120(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.1340(10) _cell_angle_gamma 90.00 _cell_volume 6066.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 0.605 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD Saphire 3 Xcalibur' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 19.64 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41065 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.1248 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11877 _reflns_number_gt 6037 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,Version 1.171.26' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26' _computing_structure_solution 'SIR-97_(Altomare & al., 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON_(Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0507P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11877 _refine_ls_number_parameters 777 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0995 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1073 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 0.861 _refine_ls_restrained_S_all 0.861 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C72 C 0.39100(19) 0.5028(6) 0.79148(15) 0.0591(13) Uani 1 1 d . . . H72 H 0.3914 0.5271 0.8225 0.071 Uiso 1 1 calc R . . Cl1 Cl 0.33315(6) 0.60772(18) 0.75277(4) 0.0815(4) Uani 1 1 d . . . Cl2 Cl 0.37840(7) 0.30100(17) 0.78210(5) 0.0834(5) Uani 1 1 d . . . Cl3 Cl 0.45910(6) 0.55101(16) 0.78593(5) 0.0735(4) Uani 1 1 d . . . Zn1 Zn 0.2500 0.24828(6) 0.5000 0.01638(14) Uani 1 2 d S . . O1 O 0.43381(10) -0.0747(3) 0.65256(8) 0.0285(6) Uani 1 1 d . . . O2 O 0.34352(10) -0.1685(3) 0.49882(8) 0.0275(6) Uani 1 1 d . . . O3 O 0.25204(10) -0.2264(3) 0.41217(8) 0.0282(6) Uani 1 1 d . . . O4 O 0.2500 0.0108(3) 0.5000 0.0296(9) Uani 1 2 d S . . H4 H 0.2212 -0.0544 0.4990 0.050 Uiso 1 1 d . . . O5 O 0.17632(10) 0.6476(3) 0.71065(7) 0.0283(6) Uani 1 1 d . . . O6 O 0.22407(12) 0.1270(3) 0.75363(8) 0.0353(7) Uani 1 1 d . . . N1 N 0.30334(11) 0.2776(3) 0.56557(8) 0.0162(6) Uani 1 1 d . . . N2 N 0.32320(11) 0.2810(3) 0.47862(8) 0.0162(6) Uani 1 1 d . . . N3 N 0.44253(12) -0.0663(3) 0.58082(9) 0.0231(7) Uani 1 1 d . . . H3 H 0.4322 -0.1046 0.5538 0.028 Uiso 1 1 calc R . . N4 N 0.38173(12) -0.2468(3) 0.59936(10) 0.0274(7) Uani 1 1 d . . . C1 C 0.36355(14) 0.2547(3) 0.58039(10) 0.0163(7) Uani 1 1 d . . . C2 C 0.38437(14) 0.2616(4) 0.62944(10) 0.0193(8) Uani 1 1 d . . . H2 H 0.4233 0.2491 0.6479 0.023 Uiso 1 1 calc R . . C3 C 0.33707(14) 0.2895(3) 0.64357(11) 0.0186(8) Uani 1 1 d . . . H3A H 0.3374 0.3015 0.6735 0.022 Uiso 1 1 calc R . . C4 C 0.28628(14) 0.2970(3) 0.60371(10) 0.0156(7) Uani 1 1 d . . . C5 C 0.22761(14) 0.3135(3) 0.60402(10) 0.0170(7) Uani 1 1 d . . . C6 C 0.17674(14) 0.3011(3) 0.56560(11) 0.0169(8) Uani 1 1 d . . . C7 C 0.11635(14) 0.2937(4) 0.56671(11) 0.0225(8) Uani 1 1 d . . . H7 H 0.1039 0.3064 0.5922 0.027 Uiso 1 1 calc R . . C8 C 0.08127(14) 0.2647(4) 0.52374(11) 0.0223(8) Uani 1 1 d . . . H8 H 0.0404 0.2509 0.5144 0.027 Uiso 1 1 calc R . . C9 C 0.38105(13) 0.2593(4) 0.50489(10) 0.0162(7) Uani 1 1 d . . . C10 C 0.39959(13) 0.2394(3) 0.55202(10) 0.0150(7) Uani 1 1 d . . . C11 C 0.46370(14) 0.2083(4) 0.57649(10) 0.0169(7) Uani 1 1 d . . . C12 C 0.50520(15) 0.3274(4) 0.58776(11) 0.0213(8) Uani 1 1 d . . . H12 H 0.4943 0.4252 0.5759 0.026 Uiso 1 1 calc R . . C13 C 0.56210(15) 0.3024(4) 0.61626(11) 0.0239(8) Uani 1 1 d . . . H13 H 0.5888 0.3838 0.6242 0.029 Uiso 1 1 calc R . . C14 C 0.57931(15) 0.1570(4) 0.63290(11) 0.0241(8) Uani 1 1 d . . . H14 H 0.6173 0.1406 0.6527 0.029 Uiso 1 1 calc R . . C15 C 0.54023(15) 0.0362(4) 0.62024(11) 0.0237(8) Uani 1 1 d . . . H15 H 0.5525 -0.0626 0.6304 0.028 Uiso 1 1 calc R . . C16 C 0.48293(15) 0.0607(4) 0.59253(11) 0.0191(8) Uani 1 1 d . . . C17 C 0.42049(15) -0.1258(4) 0.61376(13) 0.0239(8) Uani 1 1 d . . . C18 C 0.38189(17) -0.3474(4) 0.56156(12) 0.0326(10) Uani 1 1 d . . . H18A H 0.3780 -0.4530 0.5703 0.039 Uiso 1 1 calc R . . H18B H 0.4199 -0.3381 0.5563 0.039 Uiso 1 1 calc R . . C19 C 0.33354(16) -0.3145(4) 0.51746(12) 0.0334(10) Uani 1 1 d . . . H19A H 0.3326 -0.3957 0.4957 0.040 Uiso 1 1 calc R . . H19B H 0.2955 -0.3129 0.5229 0.040 Uiso 1 1 calc R . . C20 C 0.35272(16) -0.1734(4) 0.45520(12) 0.0341(10) Uani 1 1 d . . . H20A H 0.3626 -0.2778 0.4491 0.041 Uiso 1 1 calc R . . H20B H 0.3861 -0.1082 0.4559 0.041 Uiso 1 1 calc R . . C21 C 0.29994(16) -0.1219(4) 0.41777(12) 0.0307(9) Uani 1 1 d . . . H21A H 0.2882 -0.0203 0.4246 0.037 Uiso 1 1 calc R . . H21B H 0.3098 -0.1156 0.3896 0.037 Uiso 1 1 calc R . . C22 C 0.20386(16) -0.1909(4) 0.37293(12) 0.0339(10) Uani 1 1 d . . . H22A H 0.2159 -0.2044 0.3459 0.041 Uiso 1 1 calc R . . H22B H 0.1924 -0.0843 0.3742 0.041 Uiso 1 1 calc R . . C23 C 0.15136(16) -0.2947(4) 0.37011(13) 0.0365(10) Uani 1 1 d . . . H23A H 0.1249 -0.2948 0.3391 0.044 Uiso 1 1 calc R . . H23B H 0.1655 -0.3990 0.3776 0.044 Uiso 1 1 calc R . . C24 C 0.21768(14) 0.3367(4) 0.64891(10) 0.0169(8) Uani 1 1 d . . . C25 C 0.20125(14) 0.4797(4) 0.66034(11) 0.0204(8) Uani 1 1 d . . . H25 H 0.1968 0.5618 0.6403 0.025 Uiso 1 1 calc R . . C26 C 0.19126(14) 0.5007(4) 0.70230(11) 0.0212(8) Uani 1 1 d . . . C27 C 0.19836(15) 0.3801(4) 0.73213(11) 0.0243(8) Uani 1 1 d . . . H27 H 0.1910 0.3937 0.7597 0.029 Uiso 1 1 calc R . . C28 C 0.21641(15) 0.2384(4) 0.72110(11) 0.0240(8) Uani 1 1 d . . . C29 C 0.22562(15) 0.2142(4) 0.67943(11) 0.0231(8) Uani 1 1 d . . . H29 H 0.2369 0.1179 0.6720 0.028 Uiso 1 1 calc R . . C30 C 0.16364(17) 0.6757(4) 0.75252(11) 0.0325(9) Uani 1 1 d . . . H30A H 0.1536 0.7821 0.7541 0.049 Uiso 1 1 calc R . . H30B H 0.1979 0.6511 0.7778 0.049 Uiso 1 1 calc R . . H30C H 0.1310 0.6125 0.7536 0.049 Uiso 1 1 calc R . . C31 C 0.25589(19) -0.0064(4) 0.74881(12) 0.0441(11) Uani 1 1 d . . . H31A H 0.2586 -0.0756 0.7736 0.066 Uiso 1 1 calc R . . H31B H 0.2950 0.0222 0.7490 0.066 Uiso 1 1 calc R . . H31C H 0.2357 -0.0564 0.7205 0.066 Uiso 1 1 calc R . . Zn2 Zn 0.7500 -0.19894(6) 1.0000 0.01501(14) Uani 1 2 d S . . O41 O 0.60848(11) -0.6486(3) 1.12132(8) 0.0324(6) Uani 1 1 d . . . O42 O 0.75775(10) -0.7542(3) 1.09126(7) 0.0264(6) Uani 1 1 d . . . O43 O 0.84038(10) -0.7227(2) 1.04684(7) 0.0234(5) Uani 1 1 d . . . O44 O 0.7500 0.0476(3) 1.0000 0.0204(8) Uani 1 2 d S . . H44 H 0.7287 0.1033 0.9755 0.050 Uiso 1 1 d . . . O45 O 0.55810(10) -0.3997(2) 0.73741(7) 0.0245(6) Uani 1 1 d . . . O46 O 0.54491(11) 0.1393(3) 0.77726(7) 0.0326(6) Uani 1 1 d . . . N41 N 0.66014(11) -0.2279(3) 0.96953(8) 0.0149(6) Uani 1 1 d . . . N42 N 0.76343(11) -0.2421(3) 0.93862(8) 0.0149(6) Uani 1 1 d . . . N43 N 0.57311(12) -0.5426(3) 1.05056(9) 0.0208(7) Uani 1 1 d . . . H43 H 0.5653 -0.5590 1.0219 0.025 Uiso 1 1 calc R . . N44 N 0.63060(12) -0.7654(3) 1.06317(9) 0.0211(6) Uani 1 1 d . . . C41 C 0.61677(14) -0.2399(3) 0.98996(10) 0.0146(7) Uani 1 1 d . . . C42 C 0.55996(14) -0.2375(3) 0.95607(11) 0.0181(7) Uani 1 1 d . . . H42 H 0.5235 -0.2448 0.9613 0.022 Uiso 1 1 calc R . . C43 C 0.56857(14) -0.2229(3) 0.91506(11) 0.0181(8) Uani 1 1 d . . . H43A H 0.5394 -0.2171 0.8869 0.022 Uiso 1 1 calc R . . C44 C 0.63217(13) -0.2178(3) 0.92360(10) 0.0150(7) Uani 1 1 d . . . C45 C 0.65985(14) -0.2144(3) 0.88965(10) 0.0150(7) Uani 1 1 d . . . C46 C 0.72080(14) -0.2315(3) 0.89678(10) 0.0138(7) Uani 1 1 d . . . C47 C 0.75209(14) -0.2418(4) 1.13879(11) 0.0200(8) Uani 1 1 d . . . H47 H 0.7713 -0.2358 1.1699 0.024 Uiso 1 1 calc R . . C48 C 0.69320(14) -0.2619(4) 1.11827(10) 0.0202(8) Uani 1 1 d . . . H48 H 0.6647 -0.2754 1.1328 0.024 Uiso 1 1 calc R . . C49 C 0.68274(14) -0.2585(3) 1.06981(10) 0.0146(7) Uani 1 1 d . . . C50 C 0.62692(13) -0.2561(3) 1.03682(10) 0.0145(7) Uani 1 1 d . . . C51 C 0.57442(13) -0.2638(4) 1.05485(10) 0.0154(7) Uani 1 1 d . . . C52 C 0.55073(14) -0.1292(4) 1.06662(11) 0.0219(8) Uani 1 1 d . . . H52 H 0.5623 -0.0346 1.0582 0.026 Uiso 1 1 calc R . . C53 C 0.51048(15) -0.1340(4) 1.09057(12) 0.0256(9) Uani 1 1 d . . . H53 H 0.4956 -0.0430 1.0985 0.031 Uiso 1 1 calc R . . C54 C 0.49231(15) -0.2735(4) 1.10270(11) 0.0265(9) Uani 1 1 d . . . H54 H 0.4664 -0.2770 1.1199 0.032 Uiso 1 1 calc R . . C55 C 0.51275(15) -0.4078(4) 1.08930(11) 0.0228(8) Uani 1 1 d . . . H55 H 0.4994 -0.5020 1.0965 0.027 Uiso 1 1 calc R . . C56 C 0.55302(14) -0.4035(3) 1.06527(10) 0.0168(8) Uani 1 1 d . . . C57 C 0.60481(15) -0.6526(4) 1.08100(12) 0.0215(8) Uani 1 1 d . . . C58 C 0.66995(15) -0.8711(4) 1.09562(11) 0.0258(8) Uani 1 1 d . . . H58A H 0.6779 -0.9592 1.0792 0.031 Uiso 1 1 calc R . . H58B H 0.6499 -0.9080 1.1165 0.031 Uiso 1 1 calc R . . C59 C 0.72769(15) -0.7998(4) 1.12246(11) 0.0257(8) Uani 1 1 d . . . H59A H 0.7207 -0.7111 1.1392 0.031 Uiso 1 1 calc R . . H59B H 0.7514 -0.8734 1.1441 0.031 Uiso 1 1 calc R . . C60 C 0.81020(15) -0.6667(4) 1.11165(11) 0.0242(8) Uani 1 1 d . . . H60A H 0.8411 -0.7322 1.1308 0.029 Uiso 1 1 calc R . . H60B H 0.8022 -0.5851 1.1303 0.029 Uiso 1 1 calc R . . C61 C 0.82917(15) -0.6011(4) 1.07413(11) 0.0237(8) Uani 1 1 d . . . H61A H 0.7984 -0.5342 1.0555 0.028 Uiso 1 1 calc R . . H61B H 0.8648 -0.5404 1.0866 0.028 Uiso 1 1 calc R . . C62 C 0.84486(16) -0.6644(4) 1.00510(11) 0.0251(8) Uani 1 1 d . . . H62A H 0.8661 -0.5675 1.0102 0.030 Uiso 1 1 calc R . . H62B H 0.8057 -0.6469 0.9839 0.030 Uiso 1 1 calc R . . C63 C 0.87783(16) -0.7821(4) 0.98570(11) 0.0248(8) Uani 1 1 d . . . H63A H 0.9198 -0.7742 1.0021 0.030 Uiso 1 1 calc R . . H63B H 0.8650 -0.8842 0.9911 0.030 Uiso 1 1 calc R . . C64 C 0.62074(13) -0.1874(4) 0.84163(10) 0.0151(7) Uani 1 1 d . . . C65 C 0.60650(14) -0.3044(4) 0.80972(10) 0.0180(7) Uani 1 1 d . . . H65 H 0.6211 -0.4032 0.8176 0.022 Uiso 1 1 calc R . . C66 C 0.57029(14) -0.2731(4) 0.76592(11) 0.0190(8) Uani 1 1 d . . . C67 C 0.54848(14) -0.1270(4) 0.75269(11) 0.0200(8) Uani 1 1 d . . . H67 H 0.5249 -0.1070 0.7230 0.024 Uiso 1 1 calc R . . C68 C 0.56322(15) -0.0104(4) 0.78549(11) 0.0212(8) Uani 1 1 d . . . C69 C 0.59863(14) -0.0400(4) 0.82953(11) 0.0209(8) Uani 1 1 d . . . H69 H 0.6076 0.0386 0.8510 0.025 Uiso 1 1 calc R . . C70 C 0.52358(19) -0.3757(4) 0.69117(11) 0.0423(11) Uani 1 1 d . . . H70A H 0.5183 -0.4719 0.6751 0.063 Uiso 1 1 calc R . . H70B H 0.5436 -0.3044 0.6773 0.063 Uiso 1 1 calc R . . H70C H 0.4856 -0.3348 0.6900 0.063 Uiso 1 1 calc R . . C71 C 0.50551(18) 0.1763(4) 0.73302(11) 0.0396(11) Uani 1 1 d . . . H71A H 0.4960 0.2839 0.7318 0.059 Uiso 1 1 calc R . . H71B H 0.4699 0.1168 0.7272 0.059 Uiso 1 1 calc R . . H71C H 0.5243 0.1530 0.7104 0.059 Uiso 1 1 calc 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 C72 0.046(3) 0.091(4) 0.042(3) -0.019(3) 0.015(2) -0.019(3) Cl1 0.0502(8) 0.1154(12) 0.0640(9) 0.0126(8) -0.0039(7) -0.0102(8) Cl2 0.0995(12) 0.0890(11) 0.0706(9) -0.0313(7) 0.0396(9) -0.0333(9) Cl3 0.0508(8) 0.0860(10) 0.0994(11) -0.0039(8) 0.0462(8) -0.0137(7) Zn1 0.0158(3) 0.0178(3) 0.0151(3) 0.000 0.0041(2) 0.000 O1 0.0253(15) 0.0321(15) 0.0232(15) 0.0050(11) 0.0004(12) -0.0005(11) O2 0.0311(15) 0.0250(14) 0.0255(14) -0.0026(11) 0.0072(12) 0.0011(11) O3 0.0251(14) 0.0300(15) 0.0252(14) -0.0046(11) 0.0016(11) -0.0005(12) O4 0.024(2) 0.0151(18) 0.054(2) 0.000 0.0185(18) 0.000 O5 0.0324(15) 0.0338(15) 0.0200(14) -0.0049(11) 0.0101(12) 0.0060(12) O6 0.0580(19) 0.0295(15) 0.0234(15) 0.0072(11) 0.0197(13) 0.0039(13) N1 0.0145(16) 0.0205(16) 0.0140(15) 0.0005(11) 0.0048(12) 0.0007(12) N2 0.0153(16) 0.0173(16) 0.0143(15) -0.0001(11) 0.0020(12) -0.0002(12) N3 0.0247(18) 0.0197(16) 0.0221(17) -0.0044(12) 0.0033(14) -0.0025(13) N4 0.0233(17) 0.0191(16) 0.0350(18) 0.0066(14) 0.0022(14) -0.0020(14) C1 0.0156(19) 0.0145(17) 0.0161(18) 0.0028(14) 0.0011(14) 0.0002(15) C2 0.0157(19) 0.0208(19) 0.0163(18) 0.0028(14) -0.0024(15) 0.0033(15) C3 0.022(2) 0.0205(19) 0.0117(17) 0.0007(14) 0.0030(15) 0.0004(15) C4 0.0188(19) 0.0133(17) 0.0141(18) 0.0022(13) 0.0042(15) 0.0010(14) C5 0.020(2) 0.0162(17) 0.0155(18) 0.0006(14) 0.0062(15) -0.0005(15) C6 0.019(2) 0.0160(18) 0.0183(19) 0.0004(14) 0.0098(16) 0.0003(14) C7 0.021(2) 0.028(2) 0.021(2) -0.0007(15) 0.0096(16) 0.0016(16) C8 0.0114(18) 0.031(2) 0.024(2) 0.0010(16) 0.0052(15) -0.0003(16) C9 0.0115(18) 0.0183(18) 0.0179(19) -0.0014(14) 0.0031(15) 0.0004(15) C10 0.0139(18) 0.0129(17) 0.0181(18) 0.0005(14) 0.0049(14) -0.0014(14) C11 0.0199(19) 0.0217(19) 0.0108(17) -0.0022(14) 0.0073(15) 0.0024(15) C12 0.021(2) 0.0201(19) 0.023(2) -0.0002(15) 0.0079(17) -0.0005(15) C13 0.016(2) 0.030(2) 0.025(2) -0.0028(16) 0.0048(16) -0.0067(16) C14 0.0128(19) 0.037(2) 0.020(2) -0.0039(16) 0.0015(16) 0.0031(16) C15 0.022(2) 0.026(2) 0.023(2) 0.0037(16) 0.0068(17) 0.0064(16) C16 0.020(2) 0.0212(19) 0.0169(19) -0.0022(15) 0.0077(16) -0.0023(15) C17 0.018(2) 0.0159(19) 0.031(2) 0.0058(16) -0.0025(17) 0.0029(15) C18 0.030(2) 0.014(2) 0.048(3) 0.0004(17) 0.005(2) 0.0003(16) C19 0.030(2) 0.023(2) 0.043(2) -0.0087(18) 0.005(2) -0.0058(17) C20 0.025(2) 0.047(3) 0.030(2) -0.0086(18) 0.0087(19) -0.0025(19) C21 0.033(2) 0.034(2) 0.027(2) -0.0070(17) 0.0115(19) -0.0074(18) C22 0.031(2) 0.039(2) 0.029(2) -0.0047(18) 0.0045(19) 0.0094(19) C23 0.027(2) 0.033(2) 0.042(2) -0.0152(18) -0.0008(19) 0.0021(18) C24 0.0137(19) 0.024(2) 0.0105(17) -0.0006(14) 0.0003(14) -0.0004(15) C25 0.018(2) 0.029(2) 0.0149(19) 0.0039(15) 0.0048(15) 0.0015(15) C26 0.017(2) 0.025(2) 0.020(2) -0.0047(15) 0.0031(16) 0.0002(15) C27 0.028(2) 0.033(2) 0.0135(19) -0.0036(16) 0.0079(16) -0.0037(17) C28 0.027(2) 0.029(2) 0.0166(19) 0.0047(16) 0.0076(16) -0.0075(17) C29 0.027(2) 0.024(2) 0.0189(19) -0.0002(15) 0.0067(16) 0.0000(16) C30 0.035(2) 0.038(2) 0.029(2) -0.0130(17) 0.0167(19) -0.0015(18) C31 0.076(3) 0.030(3) 0.029(2) 0.0072(18) 0.021(2) 0.003(2) Zn2 0.0129(3) 0.0176(3) 0.0135(3) 0.000 0.0025(2) 0.000 O41 0.0442(17) 0.0349(16) 0.0206(15) 0.0005(11) 0.0136(13) 0.0105(12) O42 0.0277(14) 0.0293(14) 0.0233(13) -0.0053(11) 0.0097(11) -0.0068(12) O43 0.0307(14) 0.0216(14) 0.0216(13) -0.0003(10) 0.0137(11) -0.0015(11) O44 0.0215(19) 0.0185(18) 0.0149(17) 0.000 -0.0035(15) 0.000 O45 0.0296(15) 0.0237(14) 0.0139(13) -0.0035(10) -0.0023(11) 0.0037(11) O46 0.0465(17) 0.0214(14) 0.0223(14) 0.0040(11) -0.0002(12) 0.0109(12) N41 0.0147(15) 0.0151(15) 0.0149(15) 0.0010(11) 0.0046(12) 0.0005(12) N42 0.0122(14) 0.0146(14) 0.0168(15) 0.0013(11) 0.0031(12) -0.0016(12) N43 0.0278(18) 0.0176(16) 0.0181(16) -0.0022(12) 0.0088(14) -0.0003(13) N44 0.0267(17) 0.0190(16) 0.0197(16) -0.0008(12) 0.0105(13) -0.0005(13) C41 0.0144(18) 0.0117(17) 0.0171(18) 0.0016(14) 0.0043(15) 0.0008(14) C42 0.0110(18) 0.0206(18) 0.0210(19) -0.0002(15) 0.0025(15) -0.0011(15) C43 0.0166(19) 0.0166(19) 0.0160(18) -0.0003(14) -0.0024(15) -0.0006(14) C44 0.0114(18) 0.0127(18) 0.0172(18) -0.0008(13) -0.0010(14) -0.0009(13) C45 0.0150(18) 0.0139(18) 0.0134(17) -0.0004(13) 0.0004(14) -0.0009(14) C46 0.0179(19) 0.0127(18) 0.0097(17) -0.0003(13) 0.0025(14) -0.0008(14) C47 0.022(2) 0.0229(19) 0.0136(17) -0.0010(14) 0.0039(15) 0.0012(16) C48 0.0187(19) 0.0233(19) 0.0196(19) 0.0024(15) 0.0076(15) 0.0002(15) C49 0.0194(19) 0.0104(17) 0.0139(18) 0.0018(13) 0.0050(15) 0.0002(14) C50 0.0151(18) 0.0116(16) 0.0167(18) 0.0001(14) 0.0050(14) -0.0006(14) C51 0.0114(17) 0.0227(19) 0.0097(17) 0.0013(14) -0.0003(13) 0.0000(15) C52 0.019(2) 0.0166(19) 0.029(2) 0.0056(15) 0.0059(17) -0.0003(15) C53 0.022(2) 0.023(2) 0.035(2) -0.0007(16) 0.0141(18) 0.0067(16) C54 0.023(2) 0.032(2) 0.030(2) 0.0024(17) 0.0156(17) 0.0004(17) C55 0.021(2) 0.0195(19) 0.030(2) 0.0021(15) 0.0098(17) -0.0025(15) C56 0.0154(19) 0.0172(19) 0.0165(19) -0.0008(14) 0.0033(15) 0.0016(14) C57 0.022(2) 0.0169(19) 0.028(2) -0.0017(16) 0.0113(18) -0.0047(15) C58 0.031(2) 0.022(2) 0.027(2) 0.0033(16) 0.0131(18) 0.0056(17) C59 0.030(2) 0.0227(19) 0.026(2) 0.0036(16) 0.0108(17) 0.0010(17) C60 0.027(2) 0.021(2) 0.021(2) -0.0067(15) 0.0024(17) -0.0007(16) C61 0.023(2) 0.020(2) 0.029(2) -0.0075(15) 0.0084(17) -0.0035(15) C62 0.027(2) 0.027(2) 0.025(2) 0.0027(16) 0.0117(17) 0.0021(16) C63 0.029(2) 0.022(2) 0.026(2) 0.0014(15) 0.0130(17) -0.0012(16) C64 0.0096(17) 0.0219(18) 0.0131(17) 0.0009(14) 0.0026(14) -0.0010(14) C65 0.0179(19) 0.0175(18) 0.0187(19) 0.0015(14) 0.0058(15) 0.0025(15) C66 0.0175(19) 0.023(2) 0.0160(18) -0.0051(15) 0.0047(15) -0.0031(15) C67 0.0175(19) 0.028(2) 0.0105(18) 0.0028(15) -0.0016(15) 0.0042(16) C68 0.024(2) 0.0174(19) 0.021(2) 0.0046(15) 0.0054(16) 0.0024(15) C69 0.023(2) 0.0194(19) 0.0168(19) -0.0038(14) 0.0017(16) -0.0026(15) C70 0.061(3) 0.035(2) 0.018(2) -0.0102(17) -0.006(2) 0.007(2) C71 0.059(3) 0.031(2) 0.021(2) 0.0060(17) 0.001(2) 0.019(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C72 Cl3 1.731(4) . ? C72 Cl1 1.769(5) . ? C72 Cl2 1.788(5) . ? C72 H72 0.9800 . ? Zn1 N1 2.045(2) 2_556 ? Zn1 N1 2.045(2) . ? Zn1 N2 2.063(3) . ? Zn1 N2 2.063(3) 2_556 ? Zn1 O4 2.065(3) . ? O1 C17 1.224(4) . ? O2 C20 1.432(4) . ? O2 C19 1.444(4) . ? O3 C22 1.419(4) . ? O3 C21 1.424(4) . ? O4 H4 0.8814 . ? O5 C26 1.372(4) . ? O5 C30 1.438(4) . ? O6 C28 1.367(4) . ? O6 C31 1.417(4) . ? N1 C4 1.371(4) . ? N1 C1 1.374(4) . ? N2 C9 1.374(4) . ? N2 C6 1.378(4) 2_556 ? N3 C17 1.383(4) . ? N3 C16 1.433(4) . ? N3 H3 0.8600 . ? N4 C17 1.377(4) . ? N4 C18 1.460(4) . ? N4 C23 1.464(4) 2_556 ? C1 C10 1.410(4) . ? C1 C2 1.442(4) . ? C2 C3 1.348(4) . ? C2 H2 0.9300 . ? C3 C4 1.433(4) . ? C3 H3A 0.9300 . ? C4 C5 1.404(4) . ? C5 C6 1.410(4) . ? C5 C24 1.492(4) . ? C6 N2 1.378(4) 2_556 ? C6 C7 1.447(4) . ? C7 C8 1.354(4) . ? C7 H7 0.9300 . ? C8 C9 1.442(4) 2_556 ? C8 H8 0.9300 . ? C9 C10 1.396(4) . ? C9 C8 1.442(4) 2_556 ? C10 C11 1.499(4) . ? C11 C12 1.397(4) . ? C11 C16 1.400(4) . ? C12 C13 1.382(4) . ? C12 H12 0.9300 . ? C13 C14 1.378(4) . ? C13 H13 0.9300 . ? C14 C15 1.376(4) . ? C14 H14 0.9300 . ? C15 C16 1.381(4) . ? C15 H15 0.9300 . ? C18 C19 1.511(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.486(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.520(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N4 1.464(4) 2_556 ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.381(4) . ? C24 C29 1.396(4) . ? C25 C26 1.401(4) . ? C25 H25 0.9300 . ? C26 C27 1.372(4) . ? C27 C28 1.381(4) . ? C27 H27 0.9300 . ? C28 C29 1.388(4) . ? C29 H29 0.9300 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? Zn2 N42 2.054(2) . ? Zn2 N42 2.054(2) 2_657 ? Zn2 N41 2.063(2) . ? Zn2 N41 2.063(2) 2_657 ? Zn2 O44 2.143(3) . ? O41 C57 1.222(4) . ? O42 C59 1.423(4) . ? O42 C60 1.428(4) . ? O43 C62 1.421(4) . ? O43 C61 1.428(4) . ? O44 H44 0.9087 . ? O45 C66 1.383(4) . ? O45 C70 1.425(4) . ? O46 C68 1.370(4) . ? O46 C71 1.433(4) . ? N41 C44 1.370(4) . ? N41 C41 1.370(4) . ? N42 C46 1.375(4) . ? N42 C49 1.389(4) 2_657 ? N43 C57 1.387(4) . ? N43 C56 1.426(4) . ? N43 H43 0.8600 . ? N44 C57 1.361(4) . ? N44 C58 1.463(4) . ? N44 C63 1.468(4) 2_657 ? C41 C50 1.400(4) . ? C41 C42 1.428(4) . ? C42 C43 1.351(4) . ? C42 H42 0.9300 . ? C43 C44 1.451(4) . ? C43 H43A 0.9300 . ? C44 C45 1.402(4) . ? C45 C46 1.403(4) . ? C45 C64 1.504(4) . ? C46 C47 1.440(4) 2_657 ? C47 C48 1.356(4) . ? C47 C46 1.440(4) 2_657 ? C47 H47 0.9300 . ? C48 C49 1.441(4) . ? C48 H48 0.9300 . ? C49 N42 1.389(4) 2_657 ? C49 C50 1.399(4) . ? C50 C51 1.518(4) . ? C51 C56 1.392(4) . ? C51 C52 1.394(4) . ? C52 C53 1.380(4) . ? C52 H52 0.9300 . ? C53 C54 1.378(4) . ? C53 H53 0.9300 . ? C54 C55 1.376(4) . ? C54 H54 0.9300 . ? C55 C56 1.382(4) . ? C55 H55 0.9300 . ? C58 C59 1.499(5) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C61 1.483(4) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.520(4) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 N44 1.468(4) 2_657 ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 C65 1.384(4) . ? C64 C69 1.391(4) . ? C65 C66 1.386(4) . ? C65 H65 0.9300 . ? C66 C67 1.385(4) . ? C67 C68 1.399(4) . ? C67 H67 0.9300 . ? C68 C69 1.383(4) . ? C69 H69 0.9300 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl3 C72 Cl1 111.2(3) . . ? Cl3 C72 Cl2 109.6(3) . . ? Cl1 C72 Cl2 109.9(2) . . ? Cl3 C72 H72 108.7 . . ? Cl1 C72 H72 108.7 . . ? Cl2 C72 H72 108.7 . . ? N1 Zn1 N1 165.66(14) 2_556 . ? N1 Zn1 N2 89.39(10) 2_556 . ? N1 Zn1 N2 88.64(10) . . ? N1 Zn1 N2 88.64(10) 2_556 2_556 ? N1 Zn1 N2 89.39(10) . 2_556 ? N2 Zn1 N2 164.14(14) . 2_556 ? N1 Zn1 O4 97.17(7) 2_556 . ? N1 Zn1 O4 97.17(7) . . ? N2 Zn1 O4 97.93(7) . . ? N2 Zn1 O4 97.93(7) 2_556 . ? C20 O2 C19 116.2(3) . . ? C22 O3 C21 111.5(3) . . ? Zn1 O4 H4 130.0 . . ? C26 O5 C30 117.8(3) . . ? C28 O6 C31 117.1(3) . . ? C4 N1 C1 106.7(3) . . ? C4 N1 Zn1 127.6(2) . . ? C1 N1 Zn1 124.9(2) . . ? C9 N2 C6 107.1(3) . 2_556 ? C9 N2 Zn1 125.4(2) . . ? C6 N2 Zn1 126.6(2) 2_556 . ? C17 N3 C16 118.7(3) . . ? C17 N3 H3 120.7 . . ? C16 N3 H3 120.7 . . ? C17 N4 C18 123.2(3) . . ? C17 N4 C23 116.6(3) . 2_556 ? C18 N4 C23 118.8(3) . 2_556 ? N1 C1 C10 125.3(3) . . ? N1 C1 C2 109.0(3) . . ? C10 C1 C2 125.6(3) . . ? C3 C2 C1 107.5(3) . . ? C3 C2 H2 126.3 . . ? C1 C2 H2 126.3 . . ? C2 C3 C4 107.1(3) . . ? C2 C3 H3A 126.5 . . ? C4 C3 H3A 126.5 . . ? N1 C4 C5 125.3(3) . . ? N1 C4 C3 109.8(3) . . ? C5 C4 C3 124.8(3) . . ? C4 C5 C6 125.3(3) . . ? C4 C5 C24 117.7(3) . . ? C6 C5 C24 116.8(3) . . ? N2 C6 C5 125.4(3) 2_556 . ? N2 C6 C7 109.0(3) 2_556 . ? C5 C6 C7 125.4(3) . . ? C8 C7 C6 107.3(3) . . ? C8 C7 H7 126.4 . . ? C6 C7 H7 126.4 . . ? C7 C8 C9 107.3(3) . 2_556 ? C7 C8 H8 126.3 . . ? C9 C8 H8 126.3 2_556 . ? N2 C9 C10 124.5(3) . . ? N2 C9 C8 109.3(3) . 2_556 ? C10 C9 C8 126.2(3) . 2_556 ? C9 C10 C1 125.6(3) . . ? C9 C10 C11 119.3(3) . . ? C1 C10 C11 114.9(3) . . ? C12 C11 C16 117.6(3) . . ? C12 C11 C10 121.3(3) . . ? C16 C11 C10 120.8(3) . . ? C13 C12 C11 121.1(3) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C14 C13 C12 120.0(3) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 119.9(3) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 120.4(3) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C11 120.7(3) . . ? C15 C16 N3 119.4(3) . . ? C11 C16 N3 119.8(3) . . ? O1 C17 N4 122.4(3) . . ? O1 C17 N3 123.0(3) . . ? N4 C17 N3 114.6(3) . . ? N4 C18 C19 114.7(3) . . ? N4 C18 H18A 108.6 . . ? C19 C18 H18A 108.6 . . ? N4 C18 H18B 108.6 . . ? C19 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? O2 C19 C18 110.7(3) . . ? O2 C19 H19A 109.5 . . ? C18 C19 H19A 109.5 . . ? O2 C19 H19B 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? O2 C20 C21 112.7(3) . . ? O2 C20 H20A 109.1 . . ? C21 C20 H20A 109.1 . . ? O2 C20 H20B 109.1 . . ? C21 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? O3 C21 C20 110.6(3) . . ? O3 C21 H21A 109.5 . . ? C20 C21 H21A 109.5 . . ? O3 C21 H21B 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? O3 C22 C23 110.4(3) . . ? O3 C22 H22A 109.6 . . ? C23 C22 H22A 109.6 . . ? O3 C22 H22B 109.6 . . ? C23 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? N4 C23 C22 113.0(3) 2_556 . ? N4 C23 H23A 109.0 2_556 . ? C22 C23 H23A 109.0 . . ? N4 C23 H23B 109.0 2_556 . ? C22 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C29 120.2(3) . . ? C25 C24 C5 119.9(3) . . ? C29 C24 C5 119.9(3) . . ? C24 C25 C26 119.8(3) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C27 C26 O5 124.8(3) . . ? C27 C26 C25 120.1(3) . . ? O5 C26 C25 115.1(3) . . ? C26 C27 C28 119.9(3) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? O6 C28 C27 115.5(3) . . ? O6 C28 C29 123.5(3) . . ? C27 C28 C29 121.0(3) . . ? C28 C29 C24 119.0(3) . . ? C28 C29 H29 120.5 . . ? C24 C29 H29 120.5 . . ? O5 C30 H30A 109.5 . . ? O5 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O5 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O6 C31 H31A 109.5 . . ? O6 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O6 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N42 Zn2 N42 158.95(14) . 2_657 ? N42 Zn2 N41 89.54(9) . . ? N42 Zn2 N41 87.90(10) 2_657 . ? N42 Zn2 N41 87.90(9) . 2_657 ? N42 Zn2 N41 89.54(9) 2_657 2_657 ? N41 Zn2 N41 165.97(14) . 2_657 ? N42 Zn2 O44 100.53(7) . . ? N42 Zn2 O44 100.53(7) 2_657 . ? N41 Zn2 O44 97.01(7) . . ? N41 Zn2 O44 97.01(7) 2_657 . ? C59 O42 C60 113.7(2) . . ? C62 O43 C61 110.7(2) . . ? Zn2 O44 H44 122.2 . . ? C66 O45 C70 117.7(2) . . ? C68 O46 C71 117.8(3) . . ? C44 N41 C41 106.9(3) . . ? C44 N41 Zn2 124.4(2) . . ? C41 N41 Zn2 128.2(2) . . ? C46 N42 C49 106.4(2) . 2_657 ? C46 N42 Zn2 125.1(2) . . ? C49 N42 Zn2 127.5(2) 2_657 . ? C57 N43 C56 122.2(3) . . ? C57 N43 H43 118.9 . . ? C56 N43 H43 118.9 . . ? C57 N44 C58 116.5(3) . . ? C57 N44 C63 123.6(3) . 2_657 ? C58 N44 C63 119.8(3) . 2_657 ? N41 C41 C50 124.9(3) . . ? N41 C41 C42 109.6(3) . . ? C50 C41 C42 125.4(3) . . ? C43 C42 C41 107.8(3) . . ? C43 C42 H42 126.1 . . ? C41 C42 H42 126.1 . . ? C42 C43 C44 106.6(3) . . ? C42 C43 H43A 126.7 . . ? C44 C43 H43A 126.7 . . ? N41 C44 C45 126.0(3) . . ? N41 C44 C43 109.2(3) . . ? C45 C44 C43 124.7(3) . . ? C44 C45 C46 125.6(3) . . ? C44 C45 C64 116.9(3) . . ? C46 C45 C64 117.5(3) . . ? N42 C46 C45 125.2(3) . . ? N42 C46 C47 109.9(3) . 2_657 ? C45 C46 C47 124.9(3) . 2_657 ? C48 C47 C46 107.0(3) . 2_657 ? C48 C47 H47 126.5 . . ? C46 C47 H47 126.5 2_657 . ? C47 C48 C49 107.6(3) . . ? C47 C48 H48 126.2 . . ? C49 C48 H48 126.2 . . ? N42 C49 C50 125.5(3) 2_657 . ? N42 C49 C48 109.0(3) 2_657 . ? C50 C49 C48 125.2(3) . . ? C41 C50 C49 125.1(3) . . ? C41 C50 C51 119.2(3) . . ? C49 C50 C51 115.6(3) . . ? C56 C51 C52 117.7(3) . . ? C56 C51 C50 121.6(3) . . ? C52 C51 C50 120.2(3) . . ? C53 C52 C51 121.2(3) . . ? C53 C52 H52 119.4 . . ? C51 C52 H52 119.4 . . ? C54 C53 C52 120.0(3) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C55 C54 C53 119.7(3) . . ? C55 C54 H54 120.2 . . ? C53 C54 H54 120.2 . . ? C54 C55 C56 120.4(3) . . ? C54 C55 H55 119.8 . . ? C56 C55 H55 119.8 . . ? C55 C56 C51 120.8(3) . . ? C55 C56 N43 120.3(3) . . ? C51 C56 N43 118.9(3) . . ? O41 C57 N44 122.3(3) . . ? O41 C57 N43 121.6(3) . . ? N44 C57 N43 116.1(3) . . ? N44 C58 C59 113.5(3) . . ? N44 C58 H58A 108.9 . . ? C59 C58 H58A 108.9 . . ? N44 C58 H58B 108.9 . . ? C59 C58 H58B 108.9 . . ? H58A C58 H58B 107.7 . . ? O42 C59 C58 107.8(3) . . ? O42 C59 H59A 110.1 . . ? C58 C59 H59A 110.1 . . ? O42 C59 H59B 110.1 . . ? C58 C59 H59B 110.1 . . ? H59A C59 H59B 108.5 . . ? O42 C60 C61 107.2(3) . . ? O42 C60 H60A 110.3 . . ? C61 C60 H60A 110.3 . . ? O42 C60 H60B 110.3 . . ? C61 C60 H60B 110.3 . . ? H60A C60 H60B 108.5 . . ? O43 C61 C60 109.6(3) . . ? O43 C61 H61A 109.8 . . ? C60 C61 H61A 109.8 . . ? O43 C61 H61B 109.8 . . ? C60 C61 H61B 109.8 . . ? H61A C61 H61B 108.2 . . ? O43 C62 C63 108.2(3) . . ? O43 C62 H62A 110.1 . . ? C63 C62 H62A 110.1 . . ? O43 C62 H62B 110.1 . . ? C63 C62 H62B 110.1 . . ? H62A C62 H62B 108.4 . . ? N44 C63 C62 114.7(3) 2_657 . ? N44 C63 H63A 108.6 2_657 . ? C62 C63 H63A 108.6 . . ? N44 C63 H63B 108.6 2_657 . ? C62 C63 H63B 108.6 . . ? H63A C63 H63B 107.6 . . ? C65 C64 C69 119.8(3) . . ? C65 C64 C45 121.8(3) . . ? C69 C64 C45 118.3(3) . . ? C64 C65 C66 119.5(3) . . ? C64 C65 H65 120.3 . . ? C66 C65 H65 120.3 . . ? O45 C66 C67 123.8(3) . . ? O45 C66 C65 114.2(3) . . ? C67 C66 C65 122.0(3) . . ? C66 C67 C68 117.7(3) . . ? C66 C67 H67 121.2 . . ? C68 C67 H67 121.2 . . ? O46 C68 C69 114.8(3) . . ? O46 C68 C67 124.0(3) . . ? C69 C68 C67 121.1(3) . . ? C68 C69 C64 119.9(3) . . ? C68 C69 H69 120.0 . . ? C64 C69 H69 120.0 . . ? O45 C70 H70A 109.5 . . ? O45 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? O45 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O46 C71 H71A 109.5 . . ? O46 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? O46 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Zn1 N1 C4 86.6(2) 2_556 . . . ? N2 Zn1 N1 C4 168.8(2) . . . . ? N2 Zn1 N1 C4 4.5(2) 2_556 . . . ? O4 Zn1 N1 C4 -93.4(2) . . . . ? N1 Zn1 N1 C1 -105.4(2) 2_556 . . . ? N2 Zn1 N1 C1 -23.3(2) . . . . ? N2 Zn1 N1 C1 172.5(2) 2_556 . . . ? O4 Zn1 N1 C1 74.6(2) . . . . ? N1 Zn1 N2 C9 -171.6(2) 2_556 . . . ? N1 Zn1 N2 C9 22.6(2) . . . . ? N2 Zn1 N2 C9 105.6(2) 2_556 . . . ? O4 Zn1 N2 C9 -74.4(2) . . . . ? N1 Zn1 N2 C6 -3.9(2) 2_556 . . 2_556 ? N1 Zn1 N2 C6 -169.7(2) . . . 2_556 ? N2 Zn1 N2 C6 -86.8(2) 2_556 . . 2_556 ? O4 Zn1 N2 C6 93.2(2) . . . 2_556 ? C4 N1 C1 C10 -175.8(3) . . . . ? Zn1 N1 C1 C10 14.1(4) . . . . ? C4 N1 C1 C2 -0.5(3) . . . . ? Zn1 N1 C1 C2 -170.6(2) . . . . ? N1 C1 C2 C3 -0.4(4) . . . . ? C10 C1 C2 C3 174.8(3) . . . . ? C1 C2 C3 C4 1.2(3) . . . . ? C1 N1 C4 C5 -175.5(3) . . . . ? Zn1 N1 C4 C5 -5.8(4) . . . . ? C1 N1 C4 C3 1.3(3) . . . . ? Zn1 N1 C4 C3 171.0(2) . . . . ? C2 C3 C4 N1 -1.6(3) . . . . ? C2 C3 C4 C5 175.3(3) . . . . ? N1 C4 C5 C6 5.1(5) . . . . ? C3 C4 C5 C6 -171.3(3) . . . . ? N1 C4 C5 C24 -178.8(3) . . . . ? C3 C4 C5 C24 4.9(5) . . . . ? C4 C5 C6 N2 -4.5(5) . . . 2_556 ? C24 C5 C6 N2 179.3(3) . . . 2_556 ? C4 C5 C6 C7 169.6(3) . . . . ? C24 C5 C6 C7 -6.6(5) . . . . ? N2 C6 C7 C8 1.8(4) 2_556 . . . ? C5 C6 C7 C8 -173.1(3) . . . . ? C6 C7 C8 C9 -2.0(4) . . . 2_556 ? C6 N2 C9 C10 178.0(3) 2_556 . . . ? Zn1 N2 C9 C10 -12.3(4) . . . . ? C6 N2 C9 C8 -0.5(3) 2_556 . . 2_556 ? Zn1 N2 C9 C8 169.2(2) . . . 2_556 ? N2 C9 C10 C1 -7.3(5) . . . . ? C8 C9 C10 C1 171.0(3) 2_556 . . . ? N2 C9 C10 C11 176.8(3) . . . . ? C8 C9 C10 C11 -5.0(5) 2_556 . . . ? N1 C1 C10 C9 6.4(5) . . . . ? C2 C1 C10 C9 -168.1(3) . . . . ? N1 C1 C10 C11 -177.5(3) . . . . ? C2 C1 C10 C11 8.0(4) . . . . ? C9 C10 C11 C12 80.9(4) . . . . ? C1 C10 C11 C12 -95.5(3) . . . . ? C9 C10 C11 C16 -105.1(3) . . . . ? C1 C10 C11 C16 78.5(4) . . . . ? C16 C11 C12 C13 -4.3(5) . . . . ? C10 C11 C12 C13 169.9(3) . . . . ? C11 C12 C13 C14 2.1(5) . . . . ? C12 C13 C14 C15 1.5(5) . . . . ? C13 C14 C15 C16 -2.9(5) . . . . ? C14 C15 C16 C11 0.6(5) . . . . ? C14 C15 C16 N3 -178.3(3) . . . . ? C12 C11 C16 C15 2.9(5) . . . . ? C10 C11 C16 C15 -171.3(3) . . . . ? C12 C11 C16 N3 -178.2(3) . . . . ? C10 C11 C16 N3 7.6(4) . . . . ? C17 N3 C16 C15 72.9(4) . . . . ? C17 N3 C16 C11 -105.9(3) . . . . ? C18 N4 C17 O1 -155.6(3) . . . . ? C23 N4 C17 O1 10.7(5) 2_556 . . . ? C18 N4 C17 N3 25.0(4) . . . . ? C23 N4 C17 N3 -168.7(3) 2_556 . . . ? C16 N3 C17 O1 0.2(5) . . . . ? C16 N3 C17 N4 179.6(3) . . . . ? C17 N4 C18 C19 -102.3(4) . . . . ? C23 N4 C18 C19 91.7(4) 2_556 . . . ? C20 O2 C19 C18 117.8(3) . . . . ? N4 C18 C19 O2 68.4(4) . . . . ? C19 O2 C20 C21 104.1(3) . . . . ? C22 O3 C21 C20 -172.3(3) . . . . ? O2 C20 C21 O3 -65.9(4) . . . . ? C21 O3 C22 C23 -174.9(3) . . . . ? O3 C22 C23 N4 78.4(4) . . . 2_556 ? C4 C5 C24 C25 106.8(4) . . . . ? C6 C5 C24 C25 -76.7(4) . . . . ? C4 C5 C24 C29 -72.6(4) . . . . ? C6 C5 C24 C29 103.9(4) . . . . ? C29 C24 C25 C26 -1.4(5) . . . . ? C5 C24 C25 C26 179.2(3) . . . . ? C30 O5 C26 C27 -4.0(5) . . . . ? C30 O5 C26 C25 178.1(3) . . . . ? C24 C25 C26 C27 0.7(5) . . . . ? C24 C25 C26 O5 178.7(3) . . . . ? O5 C26 C27 C28 -176.7(3) . . . . ? C25 C26 C27 C28 1.1(5) . . . . ? C31 O6 C28 C27 -165.0(3) . . . . ? C31 O6 C28 C29 15.2(5) . . . . ? C26 C27 C28 O6 178.0(3) . . . . ? C26 C27 C28 C29 -2.2(5) . . . . ? O6 C28 C29 C24 -178.7(3) . . . . ? C27 C28 C29 C24 1.5(5) . . . . ? C25 C24 C29 C28 0.4(5) . . . . ? C5 C24 C29 C28 179.7(3) . . . . ? N42 Zn2 N41 C44 -19.9(2) . . . . ? N42 Zn2 N41 C44 -179.0(2) 2_657 . . . ? N41 Zn2 N41 C44 -99.3(2) 2_657 . . . ? O44 Zn2 N41 C44 80.7(2) . . . . ? N42 Zn2 N41 C41 169.4(2) . . . . ? N42 Zn2 N41 C41 10.3(2) 2_657 . . . ? N41 Zn2 N41 C41 90.0(2) 2_657 . . . ? O44 Zn2 N41 C41 -90.0(2) . . . . ? N42 Zn2 N42 C46 102.4(2) 2_657 . . . ? N41 Zn2 N42 C46 19.4(2) . . . . ? N41 Zn2 N42 C46 -174.4(2) 2_657 . . . ? O44 Zn2 N42 C46 -77.6(2) . . . . ? N42 Zn2 N42 C49 -90.6(2) 2_657 . . 2_657 ? N41 Zn2 N42 C49 -173.6(2) . . . 2_657 ? N41 Zn2 N42 C49 -7.4(2) 2_657 . . 2_657 ? O44 Zn2 N42 C49 89.4(2) . . . 2_657 ? C44 N41 C41 C50 178.5(3) . . . . ? Zn2 N41 C41 C50 -9.5(4) . . . . ? C44 N41 C41 C42 0.1(3) . . . . ? Zn2 N41 C41 C42 172.1(2) . . . . ? N41 C41 C42 C43 -0.5(3) . . . . ? C50 C41 C42 C43 -178.9(3) . . . . ? C41 C42 C43 C44 0.7(3) . . . . ? C41 N41 C44 C45 -175.4(3) . . . . ? Zn2 N41 C44 C45 12.2(4) . . . . ? C41 N41 C44 C43 0.3(3) . . . . ? Zn2 N41 C44 C43 -172.04(19) . . . . ? C42 C43 C44 N41 -0.6(3) . . . . ? C42 C43 C44 C45 175.2(3) . . . . ? N41 C44 C45 C46 4.7(5) . . . . ? C43 C44 C45 C46 -170.4(3) . . . . ? N41 C44 C45 C64 -174.2(3) . . . . ? C43 C44 C45 C64 10.7(4) . . . . ? C49 N42 C46 C45 179.7(3) 2_657 . . . ? Zn2 N42 C46 C45 -11.0(4) . . . . ? C49 N42 C46 C47 0.2(3) 2_657 . . 2_657 ? Zn2 N42 C46 C47 169.5(2) . . . 2_657 ? C44 C45 C46 N42 -5.5(5) . . . . ? C64 C45 C46 N42 173.5(3) . . . . ? C44 C45 C46 C47 174.0(3) . . . 2_657 ? C64 C45 C46 C47 -7.1(4) . . . 2_657 ? C46 C47 C48 C49 -2.1(3) 2_657 . . . ? C47 C48 C49 N42 2.3(4) . . . 2_657 ? C47 C48 C49 C50 -171.6(3) . . . . ? N41 C41 C50 C49 1.7(5) . . . . ? C42 C41 C50 C49 179.9(3) . . . . ? N41 C41 C50 C51 178.4(3) . . . . ? C42 C41 C50 C51 -3.4(5) . . . . ? N42 C49 C50 C41 1.4(5) 2_657 . . . ? C48 C49 C50 C41 174.3(3) . . . . ? N42 C49 C50 C51 -175.3(3) 2_657 . . . ? C48 C49 C50 C51 -2.4(4) . . . . ? C41 C50 C51 C56 98.8(4) . . . . ? C49 C50 C51 C56 -84.3(4) . . . . ? C41 C50 C51 C52 -89.0(4) . . . . ? C49 C50 C51 C52 88.0(4) . . . . ? C56 C51 C52 C53 4.4(5) . . . . ? C50 C51 C52 C53 -168.1(3) . . . . ? C51 C52 C53 C54 -1.0(5) . . . . ? C52 C53 C54 C55 -2.5(5) . . . . ? C53 C54 C55 C56 2.4(5) . . . . ? C54 C55 C56 C51 1.1(5) . . . . ? C54 C55 C56 N43 -178.6(3) . . . . ? C52 C51 C56 C55 -4.4(4) . . . . ? C50 C51 C56 C55 168.0(3) . . . . ? C52 C51 C56 N43 175.3(3) . . . . ? C50 C51 C56 N43 -12.3(4) . . . . ? C57 N43 C56 C55 -63.0(4) . . . . ? C57 N43 C56 C51 117.3(3) . . . . ? C58 N44 C57 O41 -8.1(5) . . . . ? C63 N44 C57 O41 173.7(3) 2_657 . . . ? C58 N44 C57 N43 172.9(3) . . . . ? C63 N44 C57 N43 -5.3(4) 2_657 . . . ? C56 N43 C57 O41 12.7(5) . . . . ? C56 N43 C57 N44 -168.3(3) . . . . ? C57 N44 C58 C59 -72.2(4) . . . . ? C63 N44 C58 C59 106.1(3) 2_657 . . . ? C60 O42 C59 C58 172.5(3) . . . . ? N44 C58 C59 O42 -61.7(3) . . . . ? C59 O42 C60 C61 -168.4(3) . . . . ? C62 O43 C61 C60 166.2(3) . . . . ? O42 C60 C61 O43 -59.6(3) . . . . ? C61 O43 C62 C63 159.8(3) . . . . ? O43 C62 C63 N44 160.7(3) . . . 2_657 ? C44 C45 C64 C65 -106.2(3) . . . . ? C46 C45 C64 C65 74.8(4) . . . . ? C44 C45 C64 C69 73.8(4) . . . . ? C46 C45 C64 C69 -105.3(3) . . . . ? C69 C64 C65 C66 0.1(5) . . . . ? C45 C64 C65 C66 -180.0(3) . . . . ? C70 O45 C66 C67 3.4(5) . . . . ? C70 O45 C66 C65 -176.9(3) . . . . ? C64 C65 C66 O45 -178.6(3) . . . . ? C64 C65 C66 C67 1.1(5) . . . . ? O45 C66 C67 C68 178.4(3) . . . . ? C65 C66 C67 C68 -1.3(5) . . . . ? C71 O46 C68 C69 -176.7(3) . . . . ? C71 O46 C68 C67 3.7(5) . . . . ? C66 C67 C68 O46 179.9(3) . . . . ? C66 C67 C68 C69 0.4(5) . . . . ? O46 C68 C69 C64 -178.8(3) . . . . ? C67 C68 C69 C64 0.7(5) . . . . ? C65 C64 C69 C68 -1.0(5) . . . . ? C45 C64 C69 C68 179.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.388 _refine_diff_density_min -0.670 _refine_diff_density_rms 0.068 data_1Pb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H64 Cl6 N8 O11 Pb' _chemical_formula_weight 1541.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.2553(4) _cell_length_b 20.8685(5) _cell_length_c 18.5943(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.284(2) _cell_angle_gamma 90.00 _cell_volume 6566.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 2.879 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.527 _exptl_absorpt_correction_T_max 0.852 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD Saphire 3 Xcalibur' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 19.64 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60218 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_sigmaI/netI 0.1124 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 32.22 _reflns_number_total 20640 _reflns_number_gt 12452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,Version 1.171.26' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26' _computing_structure_solution 'SIR-97_(Altomare & al., 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON_(Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0743P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20640 _refine_ls_number_parameters 820 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1413 _refine_ls_wR_factor_gt 0.1348 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 2.925 _refine_ls_shift/su_mean 0.038 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 O20 O 0.2387(11) 0.4653(8) 0.1292(10) 0.159(8) Uani 0.50 1 d P . . H20B H 0.2795 0.4409 0.1697 0.239 Uiso 0.50 1 d P . . H20A H 0.1921 0.4740 0.1349 0.239 Uiso 0.50 1 d P . . O21 O 0.8098(9) 0.4579(5) 0.7905(6) 0.078(4) Uani 0.50 1 d P . . H21A H 0.8605 0.4568 0.8091 0.117 Uiso 0.50 1 d P . . H21B H 0.7840 0.4328 0.7910 0.117 Uiso 0.50 1 d P . . C63 C 0.4174(4) 0.3515(3) 0.2048(4) 0.0426(16) Uani 1 1 d . . . H63 H 0.3701 0.3250 0.2029 0.051 Uiso 1 1 calc R . . Cl1 Cl 0.41969(11) 0.37842(10) 0.11643(9) 0.0525(5) Uani 1 1 d . . . Cl2 Cl 0.50175(13) 0.30393(14) 0.23718(16) 0.0870(8) Uani 1 1 d . . . Cl3 Cl 0.41406(18) 0.41424(11) 0.26416(12) 0.0793(7) Uani 1 1 d . . . C64 C 0.2975(5) 0.2187(5) 0.3807(5) 0.068(2) Uani 1 1 d . . . H64 H 0.2948 0.2575 0.4099 0.082 Uiso 1 1 calc R . . Cl4 Cl 0.37127(13) 0.23122(13) 0.32971(13) 0.0742(7) Uani 1 1 d . . . Cl5 Cl 0.20555(13) 0.20906(13) 0.32389(13) 0.0768(7) Uani 1 1 d . . . Cl6 Cl 0.31888(16) 0.15489(15) 0.44203(14) 0.0908(9) Uani 1 1 d . . . Pb1 Pb 0.111943(10) 0.457217(9) 0.553027(10) 0.01516(5) Uani 1 1 d . . . O1 O 0.0393(2) 0.19372(18) 0.2303(2) 0.0281(9) Uani 1 1 d . . . O2 O 0.0431(2) 0.25812(17) 0.4600(2) 0.0277(9) Uani 1 1 d . . . O3 O 0.2018(2) 0.24888(18) 0.6254(2) 0.0299(9) Uani 1 1 d . . . O4 O 0.0625(2) 0.06661(19) 0.4475(2) 0.0307(9) Uani 1 1 d . . . O5 O 0.1700(2) 0.05518(19) 0.6252(2) 0.0329(10) Uani 1 1 d . . . O6 O 0.1909(2) 0.17046(18) 0.8485(2) 0.0245(8) Uani 1 1 d . . . O7 O -0.3427(2) 0.4409(2) 0.6146(3) 0.0378(11) Uani 1 1 d . . . O8 O -0.2534(2) 0.21966(19) 0.6385(2) 0.0291(9) Uani 1 1 d . . . O9 O 0.5087(2) 0.23645(19) 0.4966(3) 0.0369(11) Uani 1 1 d . . . O10 O 0.5301(2) 0.45819(18) 0.4237(2) 0.0256(8) Uani 1 1 d . . . N1 N -0.0017(2) 0.40338(19) 0.4832(2) 0.0129(8) Uani 1 1 d . . . N2 N 0.0612(2) 0.3964(2) 0.6422(2) 0.0150(8) Uani 1 1 d . . . N3 N 0.2227(2) 0.39579(19) 0.6140(2) 0.0149(8) Uani 1 1 d . . . N4 N 0.1618(2) 0.4059(2) 0.4560(2) 0.0152(8) Uani 1 1 d . . . N5 N 0.0087(2) 0.2766(2) 0.3015(2) 0.0198(9) Uani 1 1 d . . . H5 H 0.0089 0.2861 0.3466 0.024 Uiso 1 1 calc R . . N6 N -0.0045(2) 0.1707(2) 0.3365(2) 0.0192(9) Uani 1 1 d . . . N7 N 0.2370(2) 0.1509(2) 0.7434(2) 0.0191(9) Uani 1 1 d . . . N8 N 0.2270(3) 0.2558(2) 0.7844(2) 0.0203(9) Uani 1 1 d . . . H8 H 0.2323 0.2673 0.7412 0.024 Uiso 1 1 calc R . . C1 C -0.0168(3) 0.3972(2) 0.4087(3) 0.0154(9) Uani 1 1 d . . . C2 C -0.0987(3) 0.3791(2) 0.3838(3) 0.0178(10) Uani 1 1 d . . . H2 H -0.1248 0.3727 0.3357 0.021 Uiso 1 1 calc R . . C3 C -0.1290(3) 0.3736(2) 0.4445(2) 0.0099(9) Uani 1 1 d . . . H3 H -0.1808 0.3617 0.4454 0.012 Uiso 1 1 calc R . . C4 C -0.0699(3) 0.3886(2) 0.5078(3) 0.0151(10) Uani 1 1 d . . . C5 C -0.0792(3) 0.3842(2) 0.5801(3) 0.0170(10) Uani 1 1 d . . . C6 C -0.0179(3) 0.3874(2) 0.6430(3) 0.0166(10) Uani 1 1 d . . . C7 C -0.0280(3) 0.3750(3) 0.7160(3) 0.0231(11) Uani 1 1 d . . . H7 H -0.0757 0.3684 0.7311 0.028 Uiso 1 1 calc R . . C8 C 0.0454(3) 0.3747(3) 0.7595(3) 0.0198(10) Uani 1 1 d . . . H8A H 0.0574 0.3680 0.8099 0.024 Uiso 1 1 calc R . . C9 C 0.1013(3) 0.3869(2) 0.7123(3) 0.0154(9) Uani 1 1 d . . . C10 C 0.1840(3) 0.3831(2) 0.7340(3) 0.0149(9) Uani 1 1 d . . . C11 C 0.2390(3) 0.3849(2) 0.6884(3) 0.0155(9) Uani 1 1 d . . . C12 C 0.3220(3) 0.3698(2) 0.7112(3) 0.0190(10) Uani 1 1 d . . . H12 H 0.3481 0.3613 0.7589 0.023 Uiso 1 1 calc R . . C13 C 0.3548(3) 0.3704(2) 0.6511(3) 0.0193(10) Uani 1 1 d . . . H13 H 0.4074 0.3622 0.6496 0.023 Uiso 1 1 calc R . . C14 C 0.2924(3) 0.3863(2) 0.5893(3) 0.0154(10) Uani 1 1 d . . . C15 C 0.3016(3) 0.3886(2) 0.5168(3) 0.0153(9) Uani 1 1 d . . . C16 C 0.2401(3) 0.3974(2) 0.4547(3) 0.0161(10) Uani 1 1 d . . . C17 C 0.2494(3) 0.3912(3) 0.3797(3) 0.0205(11) Uani 1 1 d . . . H17 H 0.2966 0.3853 0.3636 0.025 Uiso 1 1 calc R . . C18 C 0.1759(3) 0.3956(3) 0.3370(3) 0.0218(11) Uani 1 1 d . . . H18 H 0.1635 0.3939 0.2860 0.026 Uiso 1 1 calc R . . C19 C 0.1212(3) 0.4034(2) 0.3853(3) 0.0165(10) Uani 1 1 d . . . C20 C 0.0379(3) 0.4003(2) 0.3628(3) 0.0157(9) Uani 1 1 d . . . C21 C 0.0084(3) 0.3902(2) 0.2815(3) 0.0177(10) Uani 1 1 d . . . C22 C -0.0077(3) 0.4425(3) 0.2339(3) 0.0269(13) Uani 1 1 d . . . H22 H -0.0057 0.4838 0.2529 0.032 Uiso 1 1 calc R . . C23 C -0.0268(4) 0.4333(3) 0.1586(3) 0.0317(13) Uani 1 1 d . . . H23 H -0.0365 0.4685 0.1274 0.038 Uiso 1 1 calc R . . C24 C -0.0313(3) 0.3727(3) 0.1301(3) 0.0262(12) Uani 1 1 d . . . H24 H -0.0435 0.3670 0.0796 0.031 Uiso 1 1 calc R . . C25 C -0.0180(3) 0.3195(3) 0.1758(3) 0.0191(10) Uani 1 1 d . . . H25 H -0.0217 0.2785 0.1558 0.023 Uiso 1 1 calc R . . C26 C 0.0011(3) 0.3278(2) 0.2529(3) 0.0162(10) Uani 1 1 d . . . C27 C 0.0159(3) 0.2122(3) 0.2862(3) 0.0204(11) Uani 1 1 d . . . C28 C -0.0539(3) 0.1900(3) 0.3885(3) 0.0223(11) Uani 1 1 d . . . H28A H -0.0909 0.1558 0.3923 0.027 Uiso 1 1 calc R . . H28B H -0.0843 0.2275 0.3692 0.027 Uiso 1 1 calc R . . C29 C -0.0087(3) 0.2052(3) 0.4633(3) 0.0273(12) Uani 1 1 d . . . H29A H -0.0450 0.2157 0.4952 0.033 Uiso 1 1 calc R . . H29B H 0.0219 0.1681 0.4834 0.033 Uiso 1 1 calc R . . C30 C 0.1226(3) 0.2513(3) 0.5025(3) 0.0273(12) Uani 1 1 d . . . H30A H 0.1546 0.2871 0.4922 0.033 Uiso 1 1 calc R . . H30B H 0.1460 0.2122 0.4880 0.033 Uiso 1 1 calc R . . C31 C 0.1227(3) 0.2490(3) 0.5837(3) 0.0288(13) Uani 1 1 d . . . H31A H 0.0945 0.2858 0.5973 0.035 Uiso 1 1 calc R . . H31B H 0.0955 0.2106 0.5948 0.035 Uiso 1 1 calc R . . C32 C 0.2456(3) 0.1926(3) 0.6188(3) 0.0264(12) Uani 1 1 d . . . H32A H 0.2835 0.2008 0.5876 0.032 Uiso 1 1 calc R . . H32B H 0.2104 0.1588 0.5967 0.032 Uiso 1 1 calc R . . C33 C 0.2888(3) 0.1720(3) 0.6947(3) 0.0230(11) Uani 1 1 d . . . H33A H 0.3246 0.1373 0.6892 0.028 Uiso 1 1 calc R . . H33B H 0.3205 0.2076 0.7176 0.028 Uiso 1 1 calc R . . C34 C 0.0085(3) 0.1024(3) 0.3270(3) 0.0264(12) Uani 1 1 d . . . H34A H 0.0133 0.0953 0.2765 0.032 Uiso 1 1 calc R . . H34B H -0.0383 0.0796 0.3345 0.032 Uiso 1 1 calc R . . C35 C 0.0782(3) 0.0731(3) 0.3753(3) 0.0279(12) Uani 1 1 d . . . H35A H 0.0888 0.0313 0.3564 0.033 Uiso 1 1 calc R . . H35B H 0.1243 0.0999 0.3764 0.033 Uiso 1 1 calc R . . C36 C 0.1294(4) 0.0437(4) 0.4972(4) 0.0447(17) Uani 1 1 d . . . H36A H 0.1731 0.0735 0.5002 0.054 Uiso 1 1 calc R . . H36B H 0.1456 0.0024 0.4812 0.054 Uiso 1 1 calc R . . C37 C 0.1055(4) 0.0375(4) 0.5717(4) 0.051(2) Uani 1 1 d . . . H37A H 0.0609 0.0651 0.5739 0.061 Uiso 1 1 calc R . . H37B H 0.0905 -0.0064 0.5796 0.061 Uiso 1 1 calc R . . C38 C 0.1539(3) 0.0549(3) 0.6985(3) 0.0298(13) Uani 1 1 d . . . H38A H 0.1431 0.0115 0.7125 0.036 Uiso 1 1 calc R . . H38B H 0.1078 0.0810 0.7002 0.036 Uiso 1 1 calc R . . C39 C 0.2255(3) 0.0815(3) 0.7517(3) 0.0255(12) Uani 1 1 d . . . H39A H 0.2193 0.0729 0.8015 0.031 Uiso 1 1 calc R . . H39B H 0.2725 0.0591 0.7440 0.031 Uiso 1 1 calc R . . C40 C 0.2159(3) 0.1905(3) 0.7963(3) 0.0189(10) Uani 1 1 d . . . C41 C 0.2301(3) 0.3039(2) 0.8374(3) 0.0170(10) Uani 1 1 d . . . C42 C 0.2524(3) 0.2911(3) 0.9130(3) 0.0206(11) Uani 1 1 d . . . H42 H 0.2634 0.2492 0.9288 0.025 Uiso 1 1 calc R . . C43 C 0.2583(3) 0.3397(3) 0.9635(3) 0.0227(11) Uani 1 1 d . . . H43 H 0.2734 0.3306 1.0133 0.027 Uiso 1 1 calc R . . C44 C 0.2415(3) 0.4031(3) 0.9405(3) 0.0283(13) Uani 1 1 d . . . H44 H 0.2454 0.4359 0.9749 0.034 Uiso 1 1 calc R . . C45 C 0.2190(3) 0.4168(3) 0.8663(3) 0.0239(11) Uani 1 1 d . . . H45 H 0.2077 0.4589 0.8513 0.029 Uiso 1 1 calc R . . C46 C 0.2133(3) 0.3678(2) 0.8137(3) 0.0171(10) Uani 1 1 d . . . C47 C -0.1587(3) 0.3663(2) 0.5939(3) 0.0173(10) Uani 1 1 d . . . C48 C -0.2173(3) 0.4122(3) 0.5951(3) 0.0243(11) Uani 1 1 d . . . H48 H -0.2088 0.4549 0.5845 0.029 Uiso 1 1 calc R . . C49 C -0.2894(3) 0.3929(3) 0.6127(3) 0.0241(12) Uani 1 1 d . . . C50 C -0.3041(3) 0.3294(3) 0.6278(3) 0.0229(11) Uani 1 1 d . . . H50 H -0.3520 0.3174 0.6395 0.027 Uiso 1 1 calc R . . C51 C -0.2459(3) 0.2843(3) 0.6250(3) 0.0196(10) Uani 1 1 d . . . C52 C -0.1738(3) 0.3022(3) 0.6079(3) 0.0207(11) Uani 1 1 d . . . H52 H -0.1354 0.2713 0.6059 0.025 Uiso 1 1 calc R . . C53 C -0.4108(3) 0.4263(3) 0.6432(4) 0.0368(15) Uani 1 1 d . . . H53A H -0.4432 0.4638 0.6415 0.055 Uiso 1 1 calc R . . H53B H -0.3952 0.4121 0.6930 0.055 Uiso 1 1 calc R . . H53C H -0.4401 0.3929 0.6143 0.055 Uiso 1 1 calc R . . C54 C -0.3274(3) 0.1976(3) 0.6539(3) 0.0349(14) Uani 1 1 d . . . H54A H -0.3248 0.1522 0.6625 0.052 Uiso 1 1 calc R . . H54B H -0.3691 0.2068 0.6128 0.052 Uiso 1 1 calc R . . H54C H -0.3379 0.2191 0.6966 0.052 Uiso 1 1 calc R . . C55 C 0.3824(3) 0.3744(2) 0.4998(3) 0.0173(10) Uani 1 1 d . . . C56 C 0.4125(3) 0.3128(3) 0.5097(3) 0.0236(11) Uani 1 1 d . . . H56 H 0.3859 0.2812 0.5306 0.028 Uiso 1 1 calc R . . C57 C 0.4840(3) 0.2988(3) 0.4875(3) 0.0254(12) Uani 1 1 d . . . C58 C 0.5259(3) 0.3459(3) 0.4586(3) 0.0215(11) Uani 1 1 d . . . H58 H 0.5733 0.3365 0.4443 0.026 Uiso 1 1 calc R . . C59 C 0.4946(3) 0.4079(3) 0.4517(3) 0.0206(11) Uani 1 1 d . . . C60 C 0.4226(3) 0.4219(2) 0.4707(3) 0.0173(10) Uani 1 1 d . . . H60 H 0.4016 0.4630 0.4638 0.021 Uiso 1 1 calc R . . C61 C 0.5717(4) 0.2181(3) 0.4620(4) 0.0389(15) Uani 1 1 d . . . H61A H 0.5838 0.1736 0.4718 0.058 Uiso 1 1 calc R . . H61B H 0.6174 0.2436 0.4808 0.058 Uiso 1 1 calc R . . H61C H 0.5563 0.2246 0.4100 0.058 Uiso 1 1 calc R . . C62 C 0.6068(3) 0.4482(3) 0.4066(4) 0.0353(15) Uani 1 1 d . . . H62A H 0.6245 0.4872 0.3876 0.053 Uiso 1 1 calc R . . H62B H 0.6037 0.4150 0.3704 0.053 Uiso 1 1 calc R . . H62C H 0.6433 0.4358 0.4501 0.053 Uiso 1 1 calc 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 O20 0.214(16) 0.124(14) 0.201(17) -0.065(12) 0.193(15) -0.101(12) O21 0.141(12) 0.061(8) 0.036(6) -0.011(5) 0.025(7) -0.001(8) C63 0.040(4) 0.048(4) 0.043(4) 0.001(3) 0.015(3) -0.008(3) Cl1 0.0531(10) 0.0750(14) 0.0305(9) -0.0113(8) 0.0104(7) -0.0161(10) Cl2 0.0487(12) 0.0974(19) 0.116(2) 0.0504(17) 0.0191(13) 0.0109(12) Cl3 0.140(2) 0.0623(14) 0.0437(12) -0.0155(10) 0.0372(13) -0.0135(15) C64 0.075(6) 0.080(7) 0.054(5) 0.004(5) 0.024(4) -0.008(5) Cl4 0.0611(13) 0.0999(19) 0.0647(14) 0.0001(13) 0.0197(11) -0.0136(13) Cl5 0.0566(13) 0.1001(19) 0.0700(15) 0.0091(14) 0.0031(11) -0.0147(13) Cl6 0.0865(18) 0.107(2) 0.0700(16) 0.0229(15) -0.0065(13) -0.0186(16) Pb1 0.01394(8) 0.01475(8) 0.01645(9) 0.00025(8) 0.00215(5) -0.00015(8) O1 0.035(2) 0.024(2) 0.029(2) -0.0031(17) 0.0140(17) 0.0034(17) O2 0.037(2) 0.0175(19) 0.024(2) 0.0037(15) -0.0060(16) 0.0017(16) O3 0.043(2) 0.022(2) 0.0189(19) 0.0019(16) -0.0066(17) 0.0022(18) O4 0.029(2) 0.026(2) 0.035(2) 0.0061(18) 0.0015(18) 0.0094(17) O5 0.034(2) 0.031(2) 0.029(2) -0.0071(17) -0.0032(17) -0.0073(17) O6 0.0224(18) 0.030(2) 0.0230(19) 0.0046(16) 0.0083(15) -0.0073(16) O7 0.027(2) 0.030(2) 0.064(3) 0.021(2) 0.028(2) 0.0119(17) O8 0.024(2) 0.026(2) 0.040(2) 0.0032(18) 0.0123(17) -0.0061(16) O9 0.034(2) 0.024(2) 0.061(3) 0.010(2) 0.028(2) 0.0155(18) O10 0.0205(17) 0.0225(19) 0.038(2) -0.0014(18) 0.0171(16) -0.0023(16) N1 0.0121(18) 0.0136(19) 0.0134(19) 0.0000(15) 0.0037(14) -0.0002(15) N2 0.0117(18) 0.019(2) 0.0141(19) 0.0029(16) 0.0015(15) -0.0005(15) N3 0.0129(18) 0.016(2) 0.016(2) 0.0046(16) 0.0037(15) 0.0004(15) N4 0.0135(19) 0.019(2) 0.0143(19) 0.0023(16) 0.0048(15) 0.0016(16) N5 0.025(2) 0.017(2) 0.017(2) -0.0031(17) 0.0031(17) 0.0026(17) N6 0.016(2) 0.020(2) 0.021(2) -0.0021(17) 0.0026(16) 0.0006(17) N7 0.021(2) 0.017(2) 0.019(2) 0.0025(17) 0.0031(17) -0.0011(17) N8 0.026(2) 0.018(2) 0.016(2) 0.0018(17) 0.0026(17) 0.0012(18) C1 0.014(2) 0.015(2) 0.016(2) 0.0006(18) 0.0017(18) 0.0013(18) C2 0.018(2) 0.015(2) 0.017(2) -0.0035(19) -0.0035(19) 0.0020(19) C3 0.019(2) 0.0031(19) 0.0071(19) -0.0013(16) 0.0011(17) -0.0056(15) C4 0.009(2) 0.019(2) 0.017(2) -0.0023(19) 0.0007(17) -0.0008(18) C5 0.013(2) 0.016(2) 0.021(2) 0.0000(19) 0.0011(18) 0.0018(18) C6 0.014(2) 0.018(2) 0.018(2) 0.0016(19) 0.0028(18) 0.0001(18) C7 0.014(2) 0.034(3) 0.021(3) 0.001(2) 0.0029(19) -0.002(2) C8 0.019(2) 0.025(3) 0.016(2) 0.003(2) 0.0021(19) 0.001(2) C9 0.018(2) 0.015(2) 0.014(2) 0.0002(18) 0.0037(18) -0.0022(18) C10 0.017(2) 0.014(2) 0.013(2) 0.0012(18) 0.0016(17) -0.0025(18) C11 0.016(2) 0.013(2) 0.017(2) 0.0004(18) 0.0012(18) -0.0013(18) C12 0.013(2) 0.022(3) 0.019(2) 0.003(2) -0.0025(18) -0.002(2) C13 0.017(2) 0.021(3) 0.020(3) 0.004(2) 0.0057(19) 0.002(2) C14 0.008(2) 0.013(2) 0.024(3) 0.0011(19) 0.0018(18) 0.0015(17) C15 0.013(2) 0.014(2) 0.019(2) 0.0010(18) 0.0054(18) 0.0012(17) C16 0.014(2) 0.016(2) 0.020(2) -0.0029(19) 0.0066(18) -0.0018(18) C17 0.016(2) 0.029(3) 0.019(3) -0.003(2) 0.0086(19) 0.000(2) C18 0.022(3) 0.030(3) 0.014(2) -0.003(2) 0.0050(19) 0.002(2) C19 0.013(2) 0.020(2) 0.017(2) 0.0027(19) 0.0035(18) -0.0015(18) C20 0.017(2) 0.013(2) 0.017(2) 0.0007(18) 0.0024(18) -0.0005(18) C21 0.015(2) 0.024(3) 0.015(2) -0.0004(19) 0.0053(18) -0.0014(19) C22 0.033(3) 0.027(3) 0.018(3) -0.002(2) -0.002(2) -0.004(2) C23 0.047(4) 0.030(3) 0.016(3) 0.008(2) 0.001(2) 0.000(3) C24 0.027(3) 0.039(3) 0.013(2) -0.001(2) 0.004(2) -0.001(2) C25 0.015(2) 0.026(3) 0.017(2) -0.004(2) 0.0043(19) 0.002(2) C26 0.011(2) 0.020(3) 0.017(2) -0.0003(19) 0.0011(18) 0.0023(18) C27 0.018(2) 0.020(3) 0.022(3) -0.003(2) 0.002(2) 0.003(2) C28 0.019(2) 0.024(3) 0.024(3) 0.000(2) 0.005(2) 0.001(2) C29 0.035(3) 0.024(3) 0.022(3) 0.003(2) 0.004(2) 0.004(2) C30 0.033(3) 0.024(3) 0.022(3) 0.003(2) -0.001(2) -0.005(2) C31 0.033(3) 0.025(3) 0.025(3) -0.002(2) -0.002(2) 0.002(2) C32 0.036(3) 0.022(3) 0.022(3) 0.001(2) 0.008(2) 0.000(2) C33 0.019(2) 0.024(3) 0.027(3) -0.002(2) 0.006(2) -0.001(2) C34 0.029(3) 0.019(3) 0.031(3) 0.001(2) 0.006(2) 0.000(2) C35 0.028(3) 0.022(3) 0.034(3) 0.001(2) 0.009(2) 0.006(2) C36 0.027(3) 0.066(5) 0.034(3) -0.003(3) -0.010(3) 0.011(3) C37 0.023(3) 0.076(6) 0.052(4) -0.004(4) 0.004(3) -0.008(3) C38 0.029(3) 0.027(3) 0.033(3) 0.002(2) 0.005(2) -0.005(2) C39 0.028(3) 0.022(3) 0.026(3) 0.001(2) 0.004(2) 0.000(2) C40 0.012(2) 0.025(3) 0.018(2) 0.003(2) -0.0002(18) 0.0004(19) C41 0.015(2) 0.021(3) 0.015(2) 0.0005(19) 0.0033(18) -0.0007(19) C42 0.017(2) 0.027(3) 0.018(2) 0.005(2) 0.0032(19) 0.000(2) C43 0.019(2) 0.035(3) 0.013(2) 0.001(2) 0.0007(19) -0.008(2) C44 0.037(3) 0.025(3) 0.021(3) -0.005(2) 0.002(2) -0.010(2) C45 0.028(3) 0.023(3) 0.020(3) -0.003(2) 0.005(2) -0.010(2) C46 0.015(2) 0.023(3) 0.013(2) 0.0026(19) 0.0017(18) -0.0027(19) C47 0.012(2) 0.025(3) 0.015(2) 0.002(2) 0.0020(17) -0.0028(19) C48 0.020(3) 0.025(3) 0.030(3) 0.009(2) 0.009(2) 0.001(2) C49 0.014(2) 0.030(3) 0.031(3) 0.013(2) 0.009(2) 0.007(2) C50 0.012(2) 0.033(3) 0.022(3) 0.006(2) 0.0017(19) -0.004(2) C51 0.022(3) 0.021(3) 0.017(2) 0.000(2) 0.008(2) -0.005(2) C52 0.015(2) 0.024(3) 0.023(3) 0.000(2) 0.0021(19) 0.002(2) C53 0.025(3) 0.040(4) 0.051(4) 0.013(3) 0.022(3) 0.009(3) C54 0.032(3) 0.036(3) 0.039(3) 0.003(3) 0.011(3) -0.009(3) C55 0.013(2) 0.022(3) 0.017(2) -0.001(2) 0.0041(18) 0.0007(19) C56 0.019(2) 0.021(3) 0.033(3) 0.003(2) 0.009(2) 0.002(2) C57 0.020(3) 0.020(3) 0.037(3) 0.002(2) 0.008(2) 0.004(2) C58 0.018(2) 0.025(3) 0.022(3) 0.001(2) 0.006(2) 0.004(2) C59 0.022(3) 0.022(3) 0.019(3) -0.005(2) 0.007(2) -0.006(2) C60 0.015(2) 0.018(2) 0.018(2) -0.0024(19) 0.0022(19) 0.0026(18) C61 0.036(3) 0.034(4) 0.051(4) 0.002(3) 0.020(3) 0.015(3) C62 0.026(3) 0.038(4) 0.049(4) 0.001(3) 0.025(3) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O20 H20B 1.0567 . ? O20 H20A 0.8504 . ? O21 H21A 0.8760 . ? O21 H21B 0.6883 . ? C63 Cl3 1.721(7) . ? C63 Cl1 1.745(7) . ? C63 Cl2 1.767(7) . ? C63 H63 0.9800 . ? C64 Cl5 1.737(9) . ? C64 Cl6 1.745(9) . ? C64 Cl4 1.750(9) . ? C64 H64 0.9800 . ? Pb1 N2 2.386(4) . ? Pb1 N3 2.394(4) . ? Pb1 N4 2.398(4) . ? Pb1 N1 2.408(4) . ? O1 C27 1.248(6) . ? O2 C29 1.428(7) . ? O2 C30 1.450(6) . ? O3 C32 1.415(7) . ? O3 C31 1.432(6) . ? O4 C36 1.414(7) . ? O4 C35 1.428(7) . ? O5 C37 1.390(7) . ? O5 C38 1.443(7) . ? O6 C40 1.213(6) . ? O7 C49 1.366(6) . ? O7 C53 1.413(7) . ? O8 C51 1.382(6) . ? O8 C54 1.439(7) . ? O9 C57 1.369(6) . ? O9 C61 1.419(7) . ? O10 C59 1.369(6) . ? O10 C62 1.436(6) . ? N1 C1 1.365(6) . ? N1 C4 1.377(6) . ? N2 C9 1.365(6) . ? N2 C6 1.381(6) . ? N3 C11 1.376(6) . ? N3 C14 1.384(6) . ? N4 C19 1.364(6) . ? N4 C16 1.368(6) . ? N5 C26 1.388(6) . ? N5 C27 1.386(6) . ? N5 H5 0.8600 . ? N6 C27 1.369(7) . ? N6 C34 1.460(7) . ? N6 C28 1.465(7) . ? N7 C40 1.387(7) . ? N7 C33 1.459(7) . ? N7 C39 1.474(7) . ? N8 C40 1.399(7) . ? N8 C41 1.402(6) . ? N8 H8 0.8600 . ? C1 C20 1.392(7) . ? C1 C2 1.449(6) . ? C2 C3 1.338(7) . ? C2 H2 0.9300 . ? C3 C4 1.434(6) . ? C3 H3 0.9300 . ? C4 C5 1.387(7) . ? C5 C6 1.417(6) . ? C5 C47 1.493(7) . ? C6 C7 1.425(7) . ? C7 C8 1.363(7) . ? C7 H7 0.9300 . ? C8 C9 1.448(7) . ? C8 H8A 0.9300 . ? C9 C10 1.408(6) . ? C10 C11 1.390(7) . ? C10 C46 1.503(6) . ? C11 C12 1.446(6) . ? C12 C13 1.348(7) . ? C12 H12 0.9300 . ? C13 C14 1.451(6) . ? C13 H13 0.9300 . ? C14 C15 1.389(7) . ? C15 C16 1.419(6) . ? C15 C55 1.518(6) . ? C16 C17 1.440(7) . ? C17 C18 1.362(7) . ? C17 H17 0.9300 . ? C18 C19 1.434(7) . ? C18 H18 0.9300 . ? C19 C20 1.417(6) . ? C20 C21 1.513(7) . ? C21 C22 1.398(7) . ? C21 C26 1.404(7) . ? C22 C23 1.388(7) . ? C22 H22 0.9300 . ? C23 C24 1.367(8) . ? C23 H23 0.9300 . ? C24 C25 1.391(8) . ? C24 H24 0.9300 . ? C25 C26 1.418(7) . ? C25 H25 0.9300 . ? C28 C29 1.489(7) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.511(8) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.523(7) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.485(7) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.527(10) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.528(7) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C41 C42 1.408(7) . ? C41 C46 1.416(7) . ? C42 C43 1.373(7) . ? C42 H42 0.9300 . ? C43 C44 1.402(8) . ? C43 H43 0.9300 . ? C44 C45 1.388(7) . ? C44 H44 0.9300 . ? C45 C46 1.406(7) . ? C45 H45 0.9300 . ? C47 C48 1.397(7) . ? C47 C52 1.397(7) . ? C48 C49 1.406(7) . ? C48 H48 0.9300 . ? C49 C50 1.388(7) . ? C50 C51 1.384(7) . ? C50 H50 0.9300 . ? C51 C52 1.395(7) . ? C52 H52 0.9300 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C60 1.378(7) . ? C55 C56 1.387(7) . ? C56 C57 1.406(7) . ? C56 H56 0.9300 . ? C57 C58 1.390(7) . ? C58 C59 1.396(7) . ? C58 H58 0.9300 . ? C59 C60 1.387(7) . ? C60 H60 0.9300 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag H20B O20 H20A 121.9 . . ? H21A O21 H21B 125.0 . . ? Cl3 C63 Cl1 111.6(4) . . ? Cl3 C63 Cl2 109.8(4) . . ? Cl1 C63 Cl2 109.4(4) . . ? Cl3 C63 H63 108.7 . . ? Cl1 C63 H63 108.6 . . ? Cl2 C63 H63 108.7 . . ? Cl5 C64 Cl6 111.1(5) . . ? Cl5 C64 Cl4 111.2(5) . . ? Cl6 C64 Cl4 112.6(5) . . ? Cl5 C64 H64 107.2 . . ? Cl6 C64 H64 107.2 . . ? Cl4 C64 H64 107.2 . . ? N2 Pb1 N3 75.74(13) . . ? N2 Pb1 N4 121.33(14) . . ? N3 Pb1 N4 75.33(13) . . ? N2 Pb1 N1 75.84(13) . . ? N3 Pb1 N1 119.73(13) . . ? N4 Pb1 N1 76.14(13) . . ? C29 O2 C30 115.7(4) . . ? C32 O3 C31 115.1(4) . . ? C36 O4 C35 111.5(5) . . ? C37 O5 C38 113.5(5) . . ? C49 O7 C53 117.6(4) . . ? C51 O8 C54 117.8(4) . . ? C57 O9 C61 116.7(5) . . ? C59 O10 C62 118.3(4) . . ? C1 N1 C4 108.1(4) . . ? C1 N1 Pb1 124.4(3) . . ? C4 N1 Pb1 125.7(3) . . ? C9 N2 C6 106.7(4) . . ? C9 N2 Pb1 123.6(3) . . ? C6 N2 Pb1 125.3(3) . . ? C11 N3 C14 106.9(4) . . ? C11 N3 Pb1 123.5(3) . . ? C14 N3 Pb1 125.8(3) . . ? C19 N4 C16 107.5(4) . . ? C19 N4 Pb1 123.4(3) . . ? C16 N4 Pb1 124.9(3) . . ? C26 N5 C27 127.9(4) . . ? C26 N5 H5 116.1 . . ? C27 N5 H5 116.1 . . ? C27 N6 C34 118.0(4) . . ? C27 N6 C28 122.5(4) . . ? C34 N6 C28 118.1(4) . . ? C40 N7 C33 122.5(4) . . ? C40 N7 C39 116.9(4) . . ? C33 N7 C39 118.2(4) . . ? C40 N8 C41 125.0(4) . . ? C40 N8 H8 117.5 . . ? C41 N8 H8 117.5 . . ? N1 C1 C20 126.9(4) . . ? N1 C1 C2 109.2(4) . . ? C20 C1 C2 123.6(4) . . ? C3 C2 C1 105.8(4) . . ? C3 C2 H2 127.1 . . ? C1 C2 H2 127.1 . . ? C2 C3 C4 109.9(4) . . ? C2 C3 H3 125.1 . . ? C4 C3 H3 125.1 . . ? N1 C4 C5 127.2(4) . . ? N1 C4 C3 107.1(4) . . ? C5 C4 C3 125.6(4) . . ? C4 C5 C6 126.1(4) . . ? C4 C5 C47 117.9(4) . . ? C6 C5 C47 115.6(4) . . ? N2 C6 C5 125.2(4) . . ? N2 C6 C7 109.9(4) . . ? C5 C6 C7 124.6(4) . . ? C8 C7 C6 107.0(4) . . ? C8 C7 H7 126.5 . . ? C6 C7 H7 126.5 . . ? C7 C8 C9 106.9(4) . . ? C7 C8 H8A 126.5 . . ? C9 C8 H8A 126.6 . . ? N2 C9 C10 125.3(4) . . ? N2 C9 C8 109.4(4) . . ? C10 C9 C8 125.0(4) . . ? C11 C10 C9 126.7(4) . . ? C11 C10 C46 118.0(4) . . ? C9 C10 C46 114.9(4) . . ? N3 C11 C10 126.0(4) . . ? N3 C11 C12 109.1(4) . . ? C10 C11 C12 124.7(4) . . ? C13 C12 C11 107.9(4) . . ? C13 C12 H12 126.0 . . ? C11 C12 H12 126.1 . . ? C12 C13 C14 107.0(4) . . ? C12 C13 H13 126.5 . . ? C14 C13 H13 126.5 . . ? N3 C14 C15 126.1(4) . . ? N3 C14 C13 109.1(4) . . ? C15 C14 C13 124.7(4) . . ? C14 C15 C16 125.8(4) . . ? C14 C15 C55 118.7(4) . . ? C16 C15 C55 115.2(4) . . ? N4 C16 C15 125.9(4) . . ? N4 C16 C17 109.0(4) . . ? C15 C16 C17 124.7(4) . . ? C18 C17 C16 107.0(4) . . ? C18 C17 H17 126.5 . . ? C16 C17 H17 126.5 . . ? C17 C18 C19 107.1(4) . . ? C17 C18 H18 126.4 . . ? C19 C18 H18 126.5 . . ? N4 C19 C20 125.8(4) . . ? N4 C19 C18 109.4(4) . . ? C20 C19 C18 124.4(4) . . ? C1 C20 C19 126.3(4) . . ? C1 C20 C21 118.0(4) . . ? C19 C20 C21 115.1(4) . . ? C22 C21 C26 119.5(5) . . ? C22 C21 C20 120.7(5) . . ? C26 C21 C20 119.7(4) . . ? C23 C22 C21 120.7(5) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.6 . . ? C24 C23 C22 120.2(5) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.8(5) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C24 C25 C26 119.9(5) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? N5 C26 C21 118.5(4) . . ? N5 C26 C25 122.5(5) . . ? C21 C26 C25 118.9(5) . . ? O1 C27 N6 122.8(5) . . ? O1 C27 N5 121.8(5) . . ? N6 C27 N5 115.3(5) . . ? N6 C28 C29 114.2(4) . . ? N6 C28 H28A 108.7 . . ? C29 C28 H28A 108.7 . . ? N6 C28 H28B 108.7 . . ? C29 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? O2 C29 C28 110.0(4) . . ? O2 C29 H29A 109.6 . . ? C28 C29 H29A 109.6 . . ? O2 C29 H29B 109.7 . . ? C28 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? O2 C30 C31 111.3(5) . . ? O2 C30 H30A 109.4 . . ? C31 C30 H30A 109.4 . . ? O2 C30 H30B 109.4 . . ? C31 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? O3 C31 C30 110.8(5) . . ? O3 C31 H31A 109.5 . . ? C30 C31 H31A 109.5 . . ? O3 C31 H31B 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? O3 C32 C33 109.1(4) . . ? O3 C32 H32A 109.9 . . ? C33 C32 H32A 109.9 . . ? O3 C32 H32B 109.8 . . ? C33 C32 H32B 109.8 . . ? H32A C32 H32B 108.3 . . ? N7 C33 C32 114.3(4) . . ? N7 C33 H33A 108.7 . . ? C32 C33 H33A 108.7 . . ? N7 C33 H33B 108.7 . . ? C32 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? N6 C34 C35 117.0(5) . . ? N6 C34 H34A 108.0 . . ? C35 C34 H34A 108.0 . . ? N6 C34 H34B 108.0 . . ? C35 C34 H34B 108.0 . . ? H34A C34 H34B 107.3 . . ? O4 C35 C34 109.1(5) . . ? O4 C35 H35A 109.9 . . ? C34 C35 H35A 109.9 . . ? O4 C35 H35B 109.9 . . ? C34 C35 H35B 109.9 . . ? H35A C35 H35B 108.3 . . ? O4 C36 C37 106.9(5) . . ? O4 C36 H36A 110.3 . . ? C37 C36 H36A 110.3 . . ? O4 C36 H36B 110.4 . . ? C37 C36 H36B 110.4 . . ? H36A C36 H36B 108.6 . . ? O5 C37 C36 107.8(5) . . ? O5 C37 H37A 110.2 . . ? C36 C37 H37A 110.2 . . ? O5 C37 H37B 110.1 . . ? C36 C37 H37B 110.1 . . ? H37A C37 H37B 108.5 . . ? O5 C38 C39 109.2(5) . . ? O5 C38 H38A 109.8 . . ? C39 C38 H38A 109.8 . . ? O5 C38 H38B 109.8 . . ? C39 C38 H38B 109.8 . . ? H38A C38 H38B 108.3 . . ? N7 C39 C38 113.4(4) . . ? N7 C39 H39A 108.9 . . ? C38 C39 H39A 108.9 . . ? N7 C39 H39B 108.9 . . ? C38 C39 H39B 108.9 . . ? H39A C39 H39B 107.7 . . ? O6 C40 N7 123.1(5) . . ? O6 C40 N8 123.0(5) . . ? N7 C40 N8 113.9(4) . . ? N8 C41 C42 122.1(5) . . ? N8 C41 C46 118.6(4) . . ? C42 C41 C46 119.3(5) . . ? C43 C42 C41 120.7(5) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C42 C43 C44 120.3(5) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C45 C44 C43 119.9(5) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C46 120.7(5) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C45 C46 C41 119.0(4) . . ? C45 C46 C10 119.8(5) . . ? C41 C46 C10 121.0(4) . . ? C48 C47 C52 119.5(5) . . ? C48 C47 C5 121.6(5) . . ? C52 C47 C5 118.9(4) . . ? C47 C48 C49 118.9(5) . . ? C47 C48 H48 120.6 . . ? C49 C48 H48 120.6 . . ? O7 C49 C50 123.1(5) . . ? O7 C49 C48 115.2(5) . . ? C50 C49 C48 121.7(5) . . ? C51 C50 C49 118.7(5) . . ? C51 C50 H50 120.7 . . ? C49 C50 H50 120.7 . . ? O8 C51 C50 124.3(5) . . ? O8 C51 C52 114.9(5) . . ? C50 C51 C52 120.8(5) . . ? C51 C52 C47 120.4(5) . . ? C51 C52 H52 119.8 . . ? C47 C52 H52 119.8 . . ? O7 C53 H53A 109.5 . . ? O7 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? O7 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O8 C54 H54A 109.5 . . ? O8 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O8 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C60 C55 C56 121.0(5) . . ? C60 C55 C15 119.7(4) . . ? C56 C55 C15 119.2(5) . . ? C55 C56 C57 118.7(5) . . ? C55 C56 H56 120.6 . . ? C57 C56 H56 120.6 . . ? O9 C57 C58 123.2(5) . . ? O9 C57 C56 115.6(5) . . ? C58 C57 C56 121.3(5) . . ? C57 C58 C59 118.0(5) . . ? C57 C58 H58 121.0 . . ? C59 C58 H58 121.0 . . ? O10 C59 C60 115.1(5) . . ? O10 C59 C58 123.5(5) . . ? C60 C59 C58 121.4(5) . . ? C55 C60 C59 119.6(5) . . ? C55 C60 H60 120.2 . . ? C59 C60 H60 120.2 . . ? O9 C61 H61A 109.5 . . ? O9 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? O9 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O10 C62 H62A 109.5 . . ? O10 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? O10 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Pb1 N1 C1 -164.2(4) . . . . ? N3 Pb1 N1 C1 -100.1(4) . . . . ? N4 Pb1 N1 C1 -36.3(4) . . . . ? N2 Pb1 N1 C4 33.0(4) . . . . ? N3 Pb1 N1 C4 97.1(4) . . . . ? N4 Pb1 N1 C4 160.9(4) . . . . ? N3 Pb1 N2 C9 41.7(4) . . . . ? N4 Pb1 N2 C9 104.3(4) . . . . ? N1 Pb1 N2 C9 168.0(4) . . . . ? N3 Pb1 N2 C6 -164.9(4) . . . . ? N4 Pb1 N2 C6 -102.3(4) . . . . ? N1 Pb1 N2 C6 -38.6(4) . . . . ? N2 Pb1 N3 C11 -39.9(3) . . . . ? N4 Pb1 N3 C11 -168.3(4) . . . . ? N1 Pb1 N3 C11 -104.0(4) . . . . ? N2 Pb1 N3 C14 165.2(4) . . . . ? N4 Pb1 N3 C14 36.8(4) . . . . ? N1 Pb1 N3 C14 101.0(4) . . . . ? N2 Pb1 N4 C19 104.1(4) . . . . ? N3 Pb1 N4 C19 166.9(4) . . . . ? N1 Pb1 N4 C19 40.5(4) . . . . ? N2 Pb1 N4 C16 -101.9(4) . . . . ? N3 Pb1 N4 C16 -39.1(4) . . . . ? N1 Pb1 N4 C16 -165.5(4) . . . . ? C4 N1 C1 C20 -172.0(5) . . . . ? Pb1 N1 C1 C20 22.7(7) . . . . ? C4 N1 C1 C2 1.4(5) . . . . ? Pb1 N1 C1 C2 -163.9(3) . . . . ? N1 C1 C2 C3 -1.5(5) . . . . ? C20 C1 C2 C3 172.1(5) . . . . ? C1 C2 C3 C4 1.1(5) . . . . ? C1 N1 C4 C5 174.9(5) . . . . ? Pb1 N1 C4 C5 -20.0(7) . . . . ? C1 N1 C4 C3 -0.7(5) . . . . ? Pb1 N1 C4 C3 164.4(3) . . . . ? C2 C3 C4 N1 -0.3(5) . . . . ? C2 C3 C4 C5 -176.0(5) . . . . ? N1 C4 C5 C6 -7.3(8) . . . . ? C3 C4 C5 C6 167.6(5) . . . . ? N1 C4 C5 C47 -178.9(5) . . . . ? C3 C4 C5 C47 -4.0(7) . . . . ? C9 N2 C6 C5 -171.0(5) . . . . ? Pb1 N2 C6 C5 31.9(7) . . . . ? C9 N2 C6 C7 2.8(6) . . . . ? Pb1 N2 C6 C7 -154.3(3) . . . . ? C4 C5 C6 N2 1.0(8) . . . . ? C47 C5 C6 N2 172.8(5) . . . . ? C4 C5 C6 C7 -171.9(5) . . . . ? C47 C5 C6 C7 -0.1(7) . . . . ? N2 C6 C7 C8 -1.6(6) . . . . ? C5 C6 C7 C8 172.3(5) . . . . ? C6 C7 C8 C9 -0.3(6) . . . . ? C6 N2 C9 C10 171.2(5) . . . . ? Pb1 N2 C9 C10 -31.2(6) . . . . ? C6 N2 C9 C8 -3.0(5) . . . . ? Pb1 N2 C9 C8 154.6(3) . . . . ? C7 C8 C9 N2 2.1(6) . . . . ? C7 C8 C9 C10 -172.2(5) . . . . ? N2 C9 C10 C11 -3.7(8) . . . . ? C8 C9 C10 C11 169.6(5) . . . . ? N2 C9 C10 C46 -176.0(4) . . . . ? C8 C9 C10 C46 -2.7(7) . . . . ? C14 N3 C11 C10 -173.4(5) . . . . ? Pb1 N3 C11 C10 27.6(6) . . . . ? C14 N3 C11 C12 1.6(5) . . . . ? Pb1 N3 C11 C12 -157.4(3) . . . . ? C9 C10 C11 N3 5.5(8) . . . . ? C46 C10 C11 N3 177.6(4) . . . . ? C9 C10 C11 C12 -168.7(5) . . . . ? C46 C10 C11 C12 3.4(7) . . . . ? N3 C11 C12 C13 -1.2(6) . . . . ? C10 C11 C12 C13 173.9(5) . . . . ? C11 C12 C13 C14 0.3(6) . . . . ? C11 N3 C14 C15 175.9(5) . . . . ? Pb1 N3 C14 C15 -25.8(7) . . . . ? C11 N3 C14 C13 -1.4(5) . . . . ? Pb1 N3 C14 C13 157.0(3) . . . . ? C12 C13 C14 N3 0.6(6) . . . . ? C12 C13 C14 C15 -176.7(5) . . . . ? N3 C14 C15 C16 -3.8(8) . . . . ? C13 C14 C15 C16 173.0(5) . . . . ? N3 C14 C15 C55 -177.7(4) . . . . ? C13 C14 C15 C55 -0.8(7) . . . . ? C19 N4 C16 C15 -171.4(5) . . . . ? Pb1 N4 C16 C15 31.1(7) . . . . ? C19 N4 C16 C17 1.8(6) . . . . ? Pb1 N4 C16 C17 -155.7(3) . . . . ? C14 C15 C16 N4 0.8(8) . . . . ? C55 C15 C16 N4 174.9(5) . . . . ? C14 C15 C16 C17 -171.4(5) . . . . ? C55 C15 C16 C17 2.7(7) . . . . ? N4 C16 C17 C18 -0.4(6) . . . . ? C15 C16 C17 C18 172.9(5) . . . . ? C16 C17 C18 C19 -1.0(6) . . . . ? C16 N4 C19 C20 169.9(5) . . . . ? Pb1 N4 C19 C20 -32.2(7) . . . . ? C16 N4 C19 C18 -2.4(6) . . . . ? Pb1 N4 C19 C18 155.4(3) . . . . ? C17 C18 C19 N4 2.2(6) . . . . ? C17 C18 C19 C20 -170.3(5) . . . . ? N1 C1 C20 C19 7.6(8) . . . . ? C2 C1 C20 C19 -164.8(5) . . . . ? N1 C1 C20 C21 178.3(5) . . . . ? C2 C1 C20 C21 5.9(7) . . . . ? N4 C19 C20 C1 -2.4(8) . . . . ? C18 C19 C20 C1 168.9(5) . . . . ? N4 C19 C20 C21 -173.3(5) . . . . ? C18 C19 C20 C21 -2.0(7) . . . . ? C1 C20 C21 C22 98.4(6) . . . . ? C19 C20 C21 C22 -89.9(6) . . . . ? C1 C20 C21 C26 -85.1(6) . . . . ? C19 C20 C21 C26 86.6(6) . . . . ? C26 C21 C22 C23 -3.3(8) . . . . ? C20 C21 C22 C23 173.2(5) . . . . ? C21 C22 C23 C24 1.1(9) . . . . ? C22 C23 C24 C25 0.8(9) . . . . ? C23 C24 C25 C26 -0.5(8) . . . . ? C27 N5 C26 C21 -169.1(5) . . . . ? C27 N5 C26 C25 14.6(8) . . . . ? C22 C21 C26 N5 -172.9(5) . . . . ? C20 C21 C26 N5 10.6(7) . . . . ? C22 C21 C26 C25 3.6(7) . . . . ? C20 C21 C26 C25 -172.9(4) . . . . ? C24 C25 C26 N5 174.6(5) . . . . ? C24 C25 C26 C21 -1.7(7) . . . . ? C34 N6 C27 O1 5.4(7) . . . . ? C28 N6 C27 O1 -160.7(5) . . . . ? C34 N6 C27 N5 -174.6(4) . . . . ? C28 N6 C27 N5 19.2(6) . . . . ? C26 N5 C27 O1 21.5(8) . . . . ? C26 N5 C27 N6 -158.5(5) . . . . ? C27 N6 C28 C29 -99.4(6) . . . . ? C34 N6 C28 C29 94.5(5) . . . . ? C30 O2 C29 C28 -135.7(5) . . . . ? N6 C28 C29 O2 61.9(6) . . . . ? C29 O2 C30 C31 -65.7(6) . . . . ? C32 O3 C31 C30 -68.2(6) . . . . ? O2 C30 C31 O3 -174.0(4) . . . . ? C31 O3 C32 C33 -135.0(5) . . . . ? C40 N7 C33 C32 -98.8(5) . . . . ? C39 N7 C33 C32 99.3(5) . . . . ? O3 C32 C33 N7 66.6(6) . . . . ? C27 N6 C34 C35 102.8(6) . . . . ? C28 N6 C34 C35 -90.5(6) . . . . ? C36 O4 C35 C34 -175.2(5) . . . . ? N6 C34 C35 O4 74.0(6) . . . . ? C35 O4 C36 C37 -178.9(5) . . . . ? C38 O5 C37 C36 176.7(5) . . . . ? O4 C36 C37 O5 -142.9(6) . . . . ? C37 O5 C38 C39 -174.3(5) . . . . ? C40 N7 C39 C38 104.5(5) . . . . ? C33 N7 C39 C38 -92.6(6) . . . . ? O5 C38 C39 N7 70.6(6) . . . . ? C33 N7 C40 O6 -160.3(5) . . . . ? C39 N7 C40 O6 1.8(7) . . . . ? C33 N7 C40 N8 19.0(6) . . . . ? C39 N7 C40 N8 -179.0(4) . . . . ? C41 N8 C40 O6 16.6(7) . . . . ? C41 N8 C40 N7 -162.7(4) . . . . ? C40 N8 C41 C42 25.0(7) . . . . ? C40 N8 C41 C46 -157.7(5) . . . . ? N8 C41 C42 C43 177.1(5) . . . . ? C46 C41 C42 C43 -0.1(7) . . . . ? C41 C42 C43 C44 0.3(8) . . . . ? C42 C43 C44 C45 -0.1(8) . . . . ? C43 C44 C45 C46 -0.3(8) . . . . ? C44 C45 C46 C41 0.5(8) . . . . ? C44 C45 C46 C10 176.2(5) . . . . ? N8 C41 C46 C45 -177.7(4) . . . . ? C42 C41 C46 C45 -0.3(7) . . . . ? N8 C41 C46 C10 6.7(7) . . . . ? C42 C41 C46 C10 -175.9(4) . . . . ? C11 C10 C46 C45 105.8(6) . . . . ? C9 C10 C46 C45 -81.2(6) . . . . ? C11 C10 C46 C41 -78.6(6) . . . . ? C9 C10 C46 C41 94.4(6) . . . . ? C4 C5 C47 C48 -86.0(6) . . . . ? C6 C5 C47 C48 101.5(6) . . . . ? C4 C5 C47 C52 95.9(6) . . . . ? C6 C5 C47 C52 -76.7(6) . . . . ? C52 C47 C48 C49 1.9(8) . . . . ? C5 C47 C48 C49 -176.3(5) . . . . ? C53 O7 C49 C50 9.1(9) . . . . ? C53 O7 C49 C48 -170.2(5) . . . . ? C47 C48 C49 O7 178.3(5) . . . . ? C47 C48 C49 C50 -0.9(8) . . . . ? O7 C49 C50 C51 -179.5(5) . . . . ? C48 C49 C50 C51 -0.3(8) . . . . ? C54 O8 C51 C50 2.4(8) . . . . ? C54 O8 C51 C52 -177.9(5) . . . . ? C49 C50 C51 O8 -179.7(5) . . . . ? C49 C50 C51 C52 0.5(8) . . . . ? O8 C51 C52 C47 -179.3(4) . . . . ? C50 C51 C52 C47 0.4(8) . . . . ? C48 C47 C52 C51 -1.7(7) . . . . ? C5 C47 C52 C51 176.5(5) . . . . ? C14 C15 C55 C60 -115.6(5) . . . . ? C16 C15 C55 C60 69.9(6) . . . . ? C14 C15 C55 C56 68.2(6) . . . . ? C16 C15 C55 C56 -106.3(5) . . . . ? C60 C55 C56 C57 -1.8(8) . . . . ? C15 C55 C56 C57 174.3(5) . . . . ? C61 O9 C57 C58 -12.1(8) . . . . ? C61 O9 C57 C56 168.1(5) . . . . ? C55 C56 C57 O9 -177.8(5) . . . . ? C55 C56 C57 C58 2.4(8) . . . . ? O9 C57 C58 C59 179.7(5) . . . . ? C56 C57 C58 C59 -0.4(8) . . . . ? C62 O10 C59 C60 176.7(5) . . . . ? C62 O10 C59 C58 -5.6(7) . . . . ? C57 C58 C59 O10 -179.7(5) . . . . ? C57 C58 C59 C60 -2.1(8) . . . . ? C56 C55 C60 C59 -0.6(7) . . . . ? C15 C55 C60 C59 -176.7(4) . . . . ? O10 C59 C60 C55 -179.6(4) . . . . ? C58 C59 C60 C55 2.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 32.22 _diffrn_measured_fraction_theta_full 0.889 _refine_diff_density_max 2.699 _refine_diff_density_min -1.982 _refine_diff_density_rms 0.165