# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 _publ_contact_author_name 'Olivia Reinaud' _publ_contact_author_email OLIVIA.REINAUD@UNIV-PARIS5.FR _publ_section_title ; Spectacular Induced-Fit Process for Guest Binding by a Calix[6]arene Zn(II) Funnel Complex ; loop_ _publ_author_name 'Olivia Reinaud' 'David Coquiere' 'Jerome Marrot' # Attachment 'datazn.cif' data_3aqua _database_code_depnum_ccdc_archive 'CCDC 690395' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H129 Cl2 N9 O19 Zn' _chemical_formula_weight 1753.27 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(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.4885(3) _cell_length_b 26.3581(6) _cell_length_c 23.3178(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.2790(10) _cell_angle_gamma 90.00 _cell_volume 9565.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6981 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 30.01 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3744 _exptl_absorpt_coefficient_mu 0.381 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8626 _exptl_absorpt_correction_T_max 0.9451 _exptl_absorpt_process_details 'SADABS (Sheldrick, V2.10)' _exptl_special_details ; 'Blessing, Acta Cryst. (1995) A51, 33-38' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 512x512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 117512 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 30.08 _reflns_number_total 28046 _reflns_number_gt 19361 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1120P)^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 28046 _refine_ls_number_parameters 995 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0874 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1922 _refine_ls_wR_factor_gt 0.1782 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _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 Zn1 Zn 0.096585(14) 0.901806(9) 0.449703(11) 0.01436(7) Uani 1 1 d . . . N1 N 0.20963(11) 0.93188(7) 0.49831(8) 0.0167(3) Uani 1 1 d . . . C2 C 0.24936(14) 0.92212(9) 0.55920(10) 0.0216(4) Uani 1 1 d . . . H2 H 0.2248 0.9043 0.5848 0.026 Uiso 1 1 calc R . . C3 C 0.32968(14) 0.94236(10) 0.57643(11) 0.0250(5) Uani 1 1 d . . . H3 H 0.3713 0.9413 0.6159 0.030 Uiso 1 1 calc R . . N4 N 0.33907(11) 0.96437(8) 0.52643(9) 0.0220(4) Uani 1 1 d . . . C5 C 0.26542(13) 0.95780(8) 0.47958(10) 0.0183(4) Uani 1 1 d . . . C6 C 0.25013(13) 0.97623(9) 0.41650(10) 0.0202(4) Uani 1 1 d . . . H6A H 0.1878 0.9803 0.3950 0.024 Uiso 1 1 calc R . . H6B H 0.2784 1.0095 0.4173 0.024 Uiso 1 1 calc R . . O7 O 0.28541(9) 0.93917(6) 0.38597(7) 0.0195(3) Uani 1 1 d . . . C8 C 0.33238(13) 0.95661(8) 0.35010(10) 0.0170(4) Uani 1 1 d . . . C9 C 0.41439(13) 0.93638(8) 0.36269(10) 0.0176(4) Uani 1 1 d . . . C10 C 0.46296(13) 0.95078(9) 0.32627(10) 0.0189(4) Uani 1 1 d . . . H10 H 0.5190 0.9371 0.3346 0.023 Uiso 1 1 calc R . . C11 C 0.43150(13) 0.98465(9) 0.27807(10) 0.0190(4) Uani 1 1 d . . . C12 C 0.34809(13) 1.00312(9) 0.26635(10) 0.0207(4) Uani 1 1 d . . . H12 H 0.3253 1.0261 0.2335 0.025 Uiso 1 1 calc R . . C13 C 0.29698(13) 0.98909(8) 0.30103(10) 0.0184(4) Uani 1 1 d . . . C14 C 0.20511(12) 1.00715(9) 0.28209(11) 0.0198(4) Uani 1 1 d . . . H14A H 0.1952 1.0310 0.2476 0.024 Uiso 1 1 calc R . . H14B H 0.1968 1.0263 0.3163 0.024 Uiso 1 1 calc R . . C15 C 0.13765(13) 0.96508(8) 0.26332(9) 0.0176(4) Uani 1 1 d . . . C16 C 0.15742(13) 0.91548(9) 0.25210(10) 0.0192(4) Uani 1 1 d . . . H16 H 0.2150 0.9068 0.2563 0.023 Uiso 1 1 calc R . . C17 C 0.09323(13) 0.87829(9) 0.23465(9) 0.0185(4) Uani 1 1 d . . . C18 C 0.00855(13) 0.89251(8) 0.22698(10) 0.0179(4) Uani 1 1 d . . . H18 H -0.0357 0.8678 0.2139 0.021 Uiso 1 1 calc R . . C19 C -0.01248(13) 0.94146(8) 0.23792(10) 0.0174(4) Uani 1 1 d . . . C20 C 0.05273(13) 0.97799(8) 0.25679(10) 0.0170(4) Uani 1 1 d . . . C21 C -0.10382(12) 0.95751(8) 0.23141(10) 0.0187(4) Uani 1 1 d . . . H21A H -0.1029 0.9752 0.2691 0.022 Uiso 1 1 calc R . . H21B H -0.1235 0.9823 0.1977 0.022 Uiso 1 1 calc R . . C22 C -0.16841(12) 0.91498(8) 0.21946(10) 0.0166(4) Uani 1 1 d . . . C23 C -0.16401(12) 0.87799(8) 0.26314(9) 0.0153(4) Uani 1 1 d . . . C24 C -0.22318(12) 0.83821(8) 0.25204(9) 0.0156(4) Uani 1 1 d . . . C25 C -0.28879(12) 0.83675(8) 0.19625(10) 0.0182(4) Uani 1 1 d . . . H25 H -0.3296 0.8100 0.1884 0.022 Uiso 1 1 calc R . . C26 C -0.29673(13) 0.87315(9) 0.15147(10) 0.0188(4) Uani 1 1 d . . . C27 C -0.23549(13) 0.91187(8) 0.16427(10) 0.0178(4) Uani 1 1 d . . . H27 H -0.2397 0.9370 0.1343 0.021 Uiso 1 1 calc R . . C28 C -0.21217(12) 0.79682(8) 0.29860(10) 0.0177(4) Uani 1 1 d . . . H28A H -0.2610 0.7729 0.2842 0.021 Uiso 1 1 calc R . . H28B H -0.2137 0.8121 0.3370 0.021 Uiso 1 1 calc R . . C29 C -0.12843(13) 0.76748(8) 0.31104(10) 0.0168(4) Uani 1 1 d . . . C30 C -0.08320(13) 0.75077(8) 0.36935(9) 0.0163(4) Uani 1 1 d . . . C31 C -0.00799(13) 0.72190(8) 0.38088(10) 0.0180(4) Uani 1 1 d . . . C32 C 0.02268(13) 0.71184(9) 0.33314(10) 0.0210(4) Uani 1 1 d . . . H32 H 0.0738 0.6926 0.3405 0.025 Uiso 1 1 calc R . . C33 C -0.02088(14) 0.72970(9) 0.27450(10) 0.0199(4) Uani 1 1 d . . . C34 C -0.09659(13) 0.75647(9) 0.26417(10) 0.0198(4) Uani 1 1 d . . . H34 H -0.1275 0.7676 0.2241 0.024 Uiso 1 1 calc R . . C35 C 0.03547(13) 0.70142(9) 0.44459(10) 0.0211(4) Uani 1 1 d . . . H35A H 0.0351 0.7282 0.4743 0.025 Uiso 1 1 calc R . . H35B H 0.0014 0.6725 0.4514 0.025 Uiso 1 1 calc R . . C36 C 0.12692(13) 0.68410(9) 0.45678(10) 0.0189(4) Uani 1 1 d . . . C37 C 0.19352(13) 0.71891(8) 0.46995(10) 0.0174(4) Uani 1 1 d . . . C38 C 0.27872(13) 0.70366(8) 0.48126(9) 0.0173(4) Uani 1 1 d . . . C39 C 0.29477(13) 0.65226(8) 0.47795(10) 0.0189(4) Uani 1 1 d . . . H39 H 0.3524 0.6415 0.4858 0.023 Uiso 1 1 calc R . . C40 C 0.22926(14) 0.61538(9) 0.46349(10) 0.0200(4) Uani 1 1 d . . . C41 C 0.14588(14) 0.63256(9) 0.45337(10) 0.0212(4) Uani 1 1 d . . . H41 H 0.1003 0.6086 0.4439 0.025 Uiso 1 1 calc R . . C42 C 0.35088(13) 0.74149(8) 0.49467(10) 0.0184(4) Uani 1 1 d . . . H42A H 0.4061 0.7231 0.5108 0.022 Uiso 1 1 calc R . . H42B H 0.3466 0.7648 0.5269 0.022 Uiso 1 1 calc R . . C43 C 0.35229(13) 0.77286(8) 0.44044(10) 0.0170(4) Uani 1 1 d . . . C44 C 0.31587(13) 0.75518(8) 0.38109(10) 0.0191(4) Uani 1 1 d . . . H44 H 0.2859 0.7238 0.3740 0.023 Uiso 1 1 calc R . . C45 C 0.32279(13) 0.78285(9) 0.33195(10) 0.0194(4) Uani 1 1 d . . . C46 C 0.36594(13) 0.82931(9) 0.34264(10) 0.0198(4) Uani 1 1 d . . . H46 H 0.3705 0.8485 0.3093 0.024 Uiso 1 1 calc R . . C47 C 0.40239(13) 0.84792(8) 0.40161(10) 0.0172(4) Uani 1 1 d . . . C48 C 0.39510(13) 0.81953(8) 0.44987(10) 0.0173(4) Uani 1 1 d . . . C49 C 0.44933(13) 0.89858(8) 0.41348(10) 0.0192(4) Uani 1 1 d . . . H49A H 0.4452 0.9132 0.4515 0.023 Uiso 1 1 calc R . . H49B H 0.5109 0.8927 0.4195 0.023 Uiso 1 1 calc R . . N50 N 0.00480(10) 0.95334(7) 0.42210(8) 0.0156(3) Uani 1 1 d . . . C51 C 0.01371(13) 1.00561(8) 0.42601(10) 0.0185(4) Uani 1 1 d . . . H51 H 0.0655 1.0234 0.4458 0.022 Uiso 1 1 calc R . . C52 C -0.06394(14) 1.02722(8) 0.39681(10) 0.0191(4) Uani 1 1 d . . . H52 H -0.0764 1.0625 0.3925 0.023 Uiso 1 1 calc R . . N53 N -0.12065(11) 0.98831(7) 0.37484(8) 0.0166(4) Uani 1 1 d . . . C54 C -0.07794(12) 0.94416(8) 0.39079(9) 0.0156(4) Uani 1 1 d . . . C55 C -0.11517(13) 0.89301(8) 0.37103(9) 0.0168(4) Uani 1 1 d . . . H55A H -0.0905 0.8680 0.4038 0.020 Uiso 1 1 calc R . . H55B H -0.1782 0.8938 0.3619 0.020 Uiso 1 1 calc R . . O56 O -0.09513(9) 0.87880(6) 0.31735(6) 0.0165(3) Uani 1 1 d . . . N57 N 0.06965(11) 0.85384(7) 0.50723(8) 0.0158(3) Uani 1 1 d . . . C58 C -0.00080(13) 0.85573(8) 0.52688(10) 0.0180(4) Uani 1 1 d . . . H58 H -0.0466 0.8794 0.5138 0.022 Uiso 1 1 calc R . . C59 C 0.00639(14) 0.81834(9) 0.56779(11) 0.0230(5) Uani 1 1 d . . . H59 H -0.0328 0.8111 0.5888 0.028 Uiso 1 1 calc R . . N60 N 0.08111(12) 0.79285(7) 0.57330(9) 0.0221(4) Uani 1 1 d . . . C61 C 0.11760(13) 0.81493(8) 0.53580(10) 0.0176(4) Uani 1 1 d . . . C62 C 0.19707(13) 0.79664(9) 0.52536(10) 0.0195(4) Uani 1 1 d . . . H62A H 0.2349 0.8257 0.5250 0.023 Uiso 1 1 calc R . . H62B H 0.2288 0.7734 0.5585 0.023 Uiso 1 1 calc R . . O63 O 0.17342(9) 0.77036(6) 0.46760(7) 0.0192(3) Uani 1 1 d . . . C64 C 0.41609(14) 0.99121(10) 0.52507(12) 0.0294(6) Uani 1 1 d . . . H64A H 0.4109 0.9990 0.4829 0.044 Uiso 1 1 calc R . . H64B H 0.4667 0.9698 0.5432 0.044 Uiso 1 1 calc R . . H64C H 0.4223 1.0228 0.5482 0.044 Uiso 1 1 calc R . . O65 O 0.42817(10) 0.83851(6) 0.50895(7) 0.0234(3) Uani 1 1 d . . . C66 C 0.51715(17) 0.82699(12) 0.53856(12) 0.0368(6) Uani 1 1 d . . . H66A H 0.5258 0.7902 0.5380 0.055 Uiso 1 1 calc R . . H66B H 0.5348 0.8389 0.5807 0.055 Uiso 1 1 calc R . . H66C H 0.5517 0.8440 0.5172 0.055 Uiso 1 1 calc R . . C67 C 0.48344(13) 1.00116(9) 0.23766(10) 0.0225(5) Uani 1 1 d . . . C68 C 0.49573(17) 1.05938(10) 0.24225(14) 0.0339(6) Uani 1 1 d . . . H68A H 0.4396 1.0761 0.2264 0.051 Uiso 1 1 calc R . . H68B H 0.5319 1.0700 0.2184 0.051 Uiso 1 1 calc R . . H68C H 0.5235 1.0690 0.2849 0.051 Uiso 1 1 calc R . . C69 C 0.57193(15) 0.97632(12) 0.25608(12) 0.0328(6) Uani 1 1 d . . . H69A H 0.6028 0.9833 0.2991 0.049 Uiso 1 1 calc R . . H69B H 0.6045 0.9901 0.2313 0.049 Uiso 1 1 calc R . . H69C H 0.5653 0.9396 0.2497 0.049 Uiso 1 1 calc R . . C70 C 0.43465(16) 0.98699(12) 0.17143(11) 0.0350(6) Uani 1 1 d . . . H70A H 0.4279 0.9501 0.1679 0.053 Uiso 1 1 calc R . . H70B H 0.4670 0.9988 0.1455 0.053 Uiso 1 1 calc R . . H70C H 0.3779 1.0031 0.1586 0.053 Uiso 1 1 calc R . . N71 N 0.28320(12) 0.76581(8) 0.27210(9) 0.0240(4) Uani 1 1 d . . . H71A H 0.2536 0.7374 0.2653 0.029 Uiso 1 1 calc R . . H71B H 0.2880 0.7836 0.2414 0.029 Uiso 1 1 calc R . . N72 N 0.11245(12) 0.82852(8) 0.22365(9) 0.0238(4) Uani 1 1 d . . . H72A H 0.0712 0.8058 0.2118 0.029 Uiso 1 1 calc R . . H72B H 0.1659 0.8198 0.2286 0.029 Uiso 1 1 calc R . . N73 N 0.01309(13) 0.72308(8) 0.22752(9) 0.0253(4) Uani 1 1 d . . . H73A H -0.0136 0.7359 0.1914 0.030 Uiso 1 1 calc R . . H73B H 0.0612 0.7061 0.2341 0.030 Uiso 1 1 calc R . . O74 O 0.03439(9) 1.02601(6) 0.27325(8) 0.0221(3) Uani 1 1 d . . . C75 C 0.01327(16) 1.06297(10) 0.22572(13) 0.0333(6) Uani 1 1 d . . . H75A H 0.0631 1.0687 0.2125 0.050 Uiso 1 1 calc R . . H75B H -0.0028 1.0949 0.2407 0.050 Uiso 1 1 calc R . . H75C H -0.0350 1.0507 0.1913 0.050 Uiso 1 1 calc R . . C76 C -0.37047(14) 0.87259(9) 0.09046(10) 0.0233(5) Uani 1 1 d . . . C77 C -0.33826(18) 0.88598(13) 0.03772(12) 0.0389(7) Uani 1 1 d . . . H77A H -0.2937 0.8618 0.0366 0.058 Uiso 1 1 calc R . . H77B H -0.3142 0.9203 0.0435 0.058 Uiso 1 1 calc R . . H77C H -0.3862 0.8844 -0.0006 0.058 Uiso 1 1 calc R . . C78 C -0.43667(18) 0.91178(14) 0.09277(15) 0.0489(8) Uani 1 1 d . . . H78A H -0.4812 0.9143 0.0528 0.073 Uiso 1 1 calc R . . H78B H -0.4087 0.9448 0.1040 0.073 Uiso 1 1 calc R . . H78C H -0.4630 0.9016 0.1230 0.073 Uiso 1 1 calc R . . C79 C -0.41273(18) 0.82036(12) 0.07625(12) 0.0389(7) Uani 1 1 d . . . H79A H -0.4390 0.8116 0.1070 0.058 Uiso 1 1 calc R . . H79B H -0.3692 0.7950 0.0765 0.058 Uiso 1 1 calc R . . H79C H -0.4571 0.8211 0.0361 0.058 Uiso 1 1 calc R . . C80 C -0.21247(13) 0.99280(9) 0.34043(10) 0.0216(5) Uani 1 1 d . . . H80A H -0.2261 0.9724 0.3033 0.032 Uiso 1 1 calc R . . H80B H -0.2266 1.0284 0.3296 0.032 Uiso 1 1 calc R . . H80C H -0.2461 0.9806 0.3653 0.032 Uiso 1 1 calc R . . O81 O -0.10887(9) 0.76541(6) 0.41800(7) 0.0213(3) Uani 1 1 d . . . C82 C -0.17402(16) 0.73492(11) 0.42773(12) 0.0305(6) Uani 1 1 d . . . H82A H -0.2211 0.7306 0.3893 0.046 Uiso 1 1 calc R . . H82B H -0.1958 0.7515 0.4574 0.046 Uiso 1 1 calc R . . H82C H -0.1502 0.7017 0.4433 0.046 Uiso 1 1 calc R . . C83 C 0.11644(18) 0.75040(10) 0.61513(12) 0.0327(6) Uani 1 1 d . . . H83A H 0.1067 0.7185 0.5923 0.049 Uiso 1 1 calc R . . H83B H 0.0879 0.7490 0.6459 0.049 Uiso 1 1 calc R . . H83C H 0.1783 0.7555 0.6351 0.049 Uiso 1 1 calc R . . C84 C 0.25193(15) 0.55979(9) 0.45831(11) 0.0236(5) Uani 1 1 d . . . C85 C 0.2953(2) 0.55467(12) 0.41015(16) 0.0490(8) Uani 1 1 d . . . H85A H 0.3100 0.5190 0.4068 0.074 Uiso 1 1 calc R . . H85B H 0.3477 0.5753 0.4217 0.074 Uiso 1 1 calc R . . H85C H 0.2560 0.5664 0.3709 0.074 Uiso 1 1 calc R . . C86 C 0.31298(18) 0.54168(10) 0.52031(13) 0.0386(7) Uani 1 1 d . . . H86A H 0.3308 0.5067 0.5167 0.058 Uiso 1 1 calc R . . H86B H 0.2833 0.5432 0.5504 0.058 Uiso 1 1 calc R . . H86C H 0.3637 0.5637 0.5333 0.058 Uiso 1 1 calc R . . C87 C 0.17285(17) 0.52549(10) 0.44187(13) 0.0324(6) Uani 1 1 d . . . H87A H 0.1316 0.5364 0.4030 0.049 Uiso 1 1 calc R . . H87B H 0.1461 0.5278 0.4736 0.049 Uiso 1 1 calc R . . H87C H 0.1901 0.4903 0.4385 0.049 Uiso 1 1 calc R . . O88 O 0.10909(14) 0.86031(8) 0.37920(9) 0.0417(5) Uani 1 1 d . . . Cl1A Cl 0.20677(4) 0.62211(2) 0.23323(3) 0.02733(13) Uani 1 1 d . . . Cl1B Cl 0.26225(3) 0.40332(2) 0.03049(3) 0.02416(12) Uani 1 1 d . . . O1A O 0.29720(15) 0.61430(12) 0.25734(14) 0.0766(9) Uani 1 1 d . . . O2A O 0.18661(16) 0.66509(8) 0.26341(12) 0.0538(6) Uani 1 1 d . . . O3A O 0.18545(18) 0.63117(9) 0.16975(10) 0.0578(7) Uani 1 1 d . . . O4A O 0.16577(18) 0.57808(9) 0.24474(12) 0.0602(7) Uani 1 1 d . . . O1B O 0.32102(12) 0.41861(8) 0.08848(9) 0.0389(5) Uani 1 1 d . . . O2B O 0.18927(12) 0.43699(8) 0.01446(10) 0.0467(6) Uani 1 1 d . . . O3B O 0.30449(15) 0.40669(9) -0.01402(10) 0.0493(6) Uani 1 1 d . . . O4B O 0.23338(14) 0.35273(8) 0.03405(11) 0.0461(5) Uani 1 1 d . . . C1C C 0.8987(2) 0.80772(13) 0.08420(15) 0.0464(7) Uiso 1 1 d . . . H1C1 H 0.9415 0.8116 0.1247 0.070 Uiso 1 1 calc R . . H1C2 H 0.8783 0.8413 0.0675 0.070 Uiso 1 1 calc R . . H1C3 H 0.9248 0.7904 0.0574 0.070 Uiso 1 1 calc R . . C2C C 0.82534(18) 0.77737(12) 0.08862(14) 0.0384(6) Uiso 1 1 d . . . H2C1 H 0.7991 0.7946 0.1159 0.046 Uiso 1 1 calc R . . H2C2 H 0.7811 0.7744 0.0480 0.046 Uiso 1 1 calc R . . O3C O 0.85391(11) 0.72840(7) 0.11158(8) 0.0327(4) Uiso 1 1 d . . . C4C C 0.78542(19) 0.69571(12) 0.11202(14) 0.0420(7) Uiso 1 1 d . . . H4C1 H 0.7469 0.6898 0.0699 0.050 Uiso 1 1 calc R . . H4C2 H 0.7514 0.7117 0.1350 0.050 Uiso 1 1 calc R . . C5C C 0.8214(2) 0.64662(14) 0.14080(16) 0.0533(8) Uiso 1 1 d . . . H5C1 H 0.8540 0.6306 0.1173 0.080 Uiso 1 1 calc R . . H5C2 H 0.7744 0.6242 0.1416 0.080 Uiso 1 1 calc R . . H5C3 H 0.8595 0.6527 0.1824 0.080 Uiso 1 1 calc R . . C1D C 0.3976(2) 0.68873(12) 0.16626(15) 0.0448(7) Uiso 1 1 d . . . H1D1 H 0.3528 0.6815 0.1842 0.067 Uiso 1 1 calc R . . H1D2 H 0.4490 0.6688 0.1873 0.067 Uiso 1 1 calc R . . H1D3 H 0.3768 0.6796 0.1231 0.067 Uiso 1 1 calc R . . C2D C 0.41927(18) 0.74442(11) 0.17271(14) 0.0381(6) Uiso 1 1 d . . . H2D1 H 0.4502 0.7526 0.2159 0.046 Uiso 1 1 calc R . . H2D2 H 0.4571 0.7530 0.1488 0.046 Uiso 1 1 calc R . . O3D O 0.34193(11) 0.77321(7) 0.15141(8) 0.0313(4) Uiso 1 1 d . . . C4D C 0.35731(18) 0.82623(11) 0.15208(13) 0.0357(6) Uiso 1 1 d . . . H4D1 H 0.3888 0.8344 0.1237 0.043 Uiso 1 1 calc R . . H4D2 H 0.3932 0.8369 0.1934 0.043 Uiso 1 1 calc R . . C5D C 0.27363(17) 0.85441(11) 0.13365(13) 0.0361(6) Uiso 1 1 d . . . H5D1 H 0.2397 0.8454 0.0918 0.054 Uiso 1 1 calc R . . H5D2 H 0.2848 0.8910 0.1362 0.054 Uiso 1 1 calc R . . H5D3 H 0.2416 0.8453 0.1609 0.054 Uiso 1 1 calc R . . C1E C 0.4912(3) 0.67094(18) 0.3591(2) 0.0760(12) Uiso 1 1 d . . . H1E1 H 0.4388 0.6798 0.3257 0.114 Uiso 1 1 calc R . . H1E2 H 0.4758 0.6528 0.3907 0.114 Uiso 1 1 calc R . . H1E3 H 0.5276 0.6493 0.3436 0.114 Uiso 1 1 calc R . . C2E C 0.5393(2) 0.71877(14) 0.38554(17) 0.0533(8) Uiso 1 1 d . . . H2E1 H 0.5098 0.7366 0.4104 0.064 Uiso 1 1 calc R . . H2E2 H 0.5983 0.7102 0.4120 0.064 Uiso 1 1 calc R . . O3E O 0.54265(14) 0.75074(9) 0.33697(10) 0.0506(6) Uiso 1 1 d . . . C4E C 0.58918(19) 0.79540(12) 0.35805(14) 0.0415(7) Uiso 1 1 d . . . H4E1 H 0.6505 0.7872 0.3790 0.050 Uiso 1 1 calc R . . H4E2 H 0.5667 0.8126 0.3874 0.050 Uiso 1 1 calc R . . C5E C 0.5807(2) 0.82923(13) 0.30543(15) 0.0470(7) Uiso 1 1 d . . . H5E1 H 0.5996 0.8111 0.2754 0.071 Uiso 1 1 calc R . . H5E2 H 0.6164 0.8595 0.3193 0.071 Uiso 1 1 calc R . . H5E3 H 0.5205 0.8394 0.2869 0.071 Uiso 1 1 calc R . . C1F C 0.6554(3) 0.67153(18) 0.2325(2) 0.0734(12) Uiso 1 1 d . . . H1F1 H 0.6135 0.6450 0.2136 0.110 Uiso 1 1 calc R . . H1F2 H 0.6686 0.6909 0.2008 0.110 Uiso 1 1 calc R . . H1F3 H 0.6313 0.6943 0.2560 0.110 Uiso 1 1 calc R . . C2F C 0.7333(2) 0.64846(15) 0.27251(17) 0.0568(9) Uiso 1 1 d . . . H2F1 H 0.7520 0.6209 0.2509 0.068 Uiso 1 1 calc R . . H2F2 H 0.7797 0.6741 0.2851 0.068 Uiso 1 1 calc R . . O3F O 0.71746(19) 0.62851(12) 0.32478(14) 0.0752(8) Uiso 1 1 d . . . C4F C 0.7882(3) 0.60564(18) 0.3656(2) 0.0763(12) Uiso 1 1 d . . . H4F1 H 0.8382 0.6288 0.3763 0.092 Uiso 1 1 calc R . . H4F2 H 0.8031 0.5742 0.3480 0.092 Uiso 1 1 calc R . . C5F C 0.7634(4) 0.5932(2) 0.4224(3) 0.115(2) Uiso 1 1 d . . . H5F1 H 0.7514 0.6248 0.4403 0.173 Uiso 1 1 calc R . . H5F2 H 0.8110 0.5753 0.4522 0.173 Uiso 1 1 calc R . . H5F3 H 0.7121 0.5716 0.4107 0.173 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 Zn1 0.01344(11) 0.01334(13) 0.01615(12) 0.00086(9) 0.00471(9) -0.00003(8) N1 0.0149(8) 0.0170(9) 0.0189(8) -0.0033(7) 0.0068(7) -0.0009(6) C2 0.0229(10) 0.0227(12) 0.0188(10) -0.0042(9) 0.0063(8) -0.0002(9) C3 0.0201(10) 0.0305(13) 0.0217(11) -0.0076(10) 0.0034(8) 0.0001(9) N4 0.0158(8) 0.0231(10) 0.0274(10) -0.0091(8) 0.0073(7) -0.0033(7) C5 0.0144(9) 0.0162(10) 0.0250(11) -0.0052(8) 0.0076(8) -0.0013(7) C6 0.0171(9) 0.0191(11) 0.0267(11) 0.0006(9) 0.0105(8) -0.0005(8) O7 0.0221(7) 0.0168(8) 0.0230(8) -0.0007(6) 0.0121(6) -0.0036(6) C8 0.0170(9) 0.0155(10) 0.0192(10) 0.0001(8) 0.0071(8) -0.0038(7) C9 0.0172(9) 0.0145(10) 0.0198(10) -0.0001(8) 0.0043(8) -0.0028(7) C10 0.0131(9) 0.0196(11) 0.0225(10) -0.0016(8) 0.0037(8) -0.0020(8) C11 0.0151(9) 0.0207(11) 0.0196(10) 0.0001(8) 0.0035(8) -0.0042(8) C12 0.0163(9) 0.0211(11) 0.0240(11) 0.0039(9) 0.0057(8) -0.0029(8) C13 0.0146(9) 0.0172(11) 0.0234(10) 0.0008(8) 0.0062(8) -0.0019(8) C14 0.0118(9) 0.0192(11) 0.0279(11) 0.0046(9) 0.0058(8) -0.0024(7) C15 0.0144(9) 0.0188(11) 0.0189(10) 0.0000(8) 0.0047(8) -0.0030(8) C16 0.0144(9) 0.0208(11) 0.0239(11) -0.0013(9) 0.0083(8) -0.0014(8) C17 0.0202(10) 0.0207(11) 0.0162(9) -0.0028(8) 0.0082(8) 0.0002(8) C18 0.0153(9) 0.0191(11) 0.0188(10) -0.0029(8) 0.0051(8) -0.0044(8) C19 0.0157(9) 0.0187(11) 0.0178(9) 0.0000(8) 0.0053(8) -0.0040(8) C20 0.0143(9) 0.0161(10) 0.0201(10) 0.0009(8) 0.0049(7) -0.0011(7) C21 0.0138(9) 0.0164(11) 0.0252(11) 0.0025(8) 0.0055(8) -0.0016(7) C22 0.0145(9) 0.0150(10) 0.0203(10) 0.0003(8) 0.0058(8) -0.0008(7) C23 0.0125(8) 0.0163(10) 0.0163(9) -0.0031(8) 0.0037(7) 0.0000(7) C24 0.0126(8) 0.0152(10) 0.0192(10) -0.0010(8) 0.0055(7) 0.0001(7) C25 0.0135(9) 0.0183(11) 0.0217(10) -0.0029(8) 0.0044(8) -0.0041(8) C26 0.0150(9) 0.0208(11) 0.0187(10) -0.0006(8) 0.0032(8) -0.0007(8) C27 0.0139(9) 0.0192(11) 0.0198(10) 0.0024(8) 0.0049(8) -0.0004(7) C28 0.0141(9) 0.0155(10) 0.0216(10) 0.0009(8) 0.0032(8) -0.0020(7) C29 0.0168(9) 0.0120(10) 0.0202(10) -0.0005(8) 0.0042(8) -0.0006(7) C30 0.0166(9) 0.0145(10) 0.0174(9) -0.0023(8) 0.0053(8) -0.0012(7) C31 0.0161(9) 0.0178(11) 0.0192(10) -0.0008(8) 0.0047(8) -0.0026(8) C32 0.0177(9) 0.0205(12) 0.0237(11) 0.0004(9) 0.0052(8) 0.0030(8) C33 0.0228(10) 0.0166(11) 0.0215(10) -0.0012(8) 0.0090(8) -0.0015(8) C34 0.0206(10) 0.0184(11) 0.0191(10) 0.0008(8) 0.0051(8) -0.0021(8) C35 0.0178(9) 0.0231(12) 0.0229(11) 0.0057(9) 0.0074(8) 0.0039(8) C36 0.0170(9) 0.0223(12) 0.0176(10) 0.0039(8) 0.0060(8) 0.0024(8) C37 0.0193(9) 0.0159(10) 0.0178(10) 0.0037(8) 0.0072(8) 0.0040(8) C38 0.0177(9) 0.0173(11) 0.0179(10) 0.0038(8) 0.0070(8) 0.0015(8) C39 0.0183(9) 0.0181(11) 0.0212(10) 0.0020(8) 0.0074(8) 0.0048(8) C40 0.0237(10) 0.0166(11) 0.0179(10) 0.0015(8) 0.0043(8) 0.0032(8) C41 0.0201(10) 0.0201(11) 0.0220(10) 0.0033(9) 0.0051(8) -0.0016(8) C42 0.0154(9) 0.0187(11) 0.0208(10) 0.0035(8) 0.0058(8) 0.0014(8) C43 0.0163(9) 0.0156(10) 0.0203(10) 0.0006(8) 0.0075(8) 0.0028(7) C44 0.0184(9) 0.0156(11) 0.0235(10) -0.0008(8) 0.0072(8) -0.0010(8) C45 0.0184(9) 0.0167(11) 0.0228(11) -0.0021(8) 0.0063(8) 0.0002(8) C46 0.0195(10) 0.0210(11) 0.0193(10) 0.0009(8) 0.0069(8) -0.0021(8) C47 0.0157(9) 0.0150(10) 0.0200(10) 0.0000(8) 0.0048(8) 0.0002(7) C48 0.0169(9) 0.0159(10) 0.0176(10) -0.0004(8) 0.0036(8) 0.0030(8) C49 0.0176(9) 0.0153(11) 0.0221(10) 0.0014(8) 0.0030(8) -0.0029(8) N50 0.0145(8) 0.0150(9) 0.0158(8) -0.0012(7) 0.0029(6) -0.0006(6) C51 0.0192(9) 0.0141(10) 0.0199(10) -0.0038(8) 0.0033(8) -0.0015(8) C52 0.0220(10) 0.0126(10) 0.0209(10) -0.0029(8) 0.0047(8) -0.0006(8) N53 0.0157(8) 0.0149(9) 0.0176(8) -0.0020(7) 0.0031(6) -0.0002(6) C54 0.0152(9) 0.0148(10) 0.0160(9) 0.0000(8) 0.0040(7) 0.0012(7) C55 0.0172(9) 0.0150(10) 0.0174(9) -0.0023(8) 0.0047(8) -0.0028(7) O56 0.0129(6) 0.0183(8) 0.0163(7) -0.0025(6) 0.0021(5) 0.0006(5) N57 0.0168(8) 0.0117(8) 0.0188(8) 0.0012(7) 0.0060(7) -0.0006(6) C58 0.0167(9) 0.0175(11) 0.0211(10) -0.0021(8) 0.0080(8) -0.0009(8) C59 0.0244(11) 0.0230(12) 0.0266(11) 0.0031(9) 0.0153(9) 0.0033(9) N60 0.0261(9) 0.0197(10) 0.0237(9) 0.0059(8) 0.0124(8) 0.0043(7) C61 0.0201(10) 0.0166(11) 0.0174(9) 0.0013(8) 0.0078(8) 0.0010(8) C62 0.0208(10) 0.0169(11) 0.0209(10) -0.0003(8) 0.0071(8) 0.0035(8) O63 0.0237(7) 0.0156(8) 0.0192(7) 0.0038(6) 0.0082(6) 0.0067(6) C64 0.0162(10) 0.0339(15) 0.0388(14) -0.0120(11) 0.0098(10) -0.0085(9) O65 0.0269(8) 0.0224(9) 0.0182(7) -0.0023(6) 0.0038(6) -0.0031(6) C66 0.0305(13) 0.0394(16) 0.0285(13) 0.0065(12) -0.0064(10) -0.0032(11) C67 0.0160(9) 0.0292(13) 0.0227(11) 0.0060(9) 0.0070(8) -0.0009(8) C68 0.0326(13) 0.0308(15) 0.0434(15) 0.0080(12) 0.0192(12) -0.0049(11) C69 0.0203(11) 0.0484(17) 0.0322(13) 0.0111(12) 0.0120(10) 0.0043(11) C70 0.0277(12) 0.0537(19) 0.0238(12) -0.0020(12) 0.0088(10) 0.0013(12) N71 0.0297(10) 0.0214(10) 0.0199(9) -0.0026(8) 0.0068(8) -0.0054(8) N72 0.0194(9) 0.0201(10) 0.0323(11) -0.0097(8) 0.0090(8) -0.0003(7) N73 0.0258(9) 0.0307(12) 0.0215(9) 0.0020(8) 0.0106(8) 0.0063(8) O74 0.0177(7) 0.0140(8) 0.0327(9) -0.0007(7) 0.0056(6) -0.0009(6) C75 0.0249(12) 0.0221(13) 0.0488(16) 0.0079(12) 0.0067(11) 0.0022(9) C76 0.0165(9) 0.0277(13) 0.0206(10) 0.0002(9) -0.0006(8) -0.0030(8) C77 0.0343(14) 0.0524(19) 0.0225(12) 0.0073(12) -0.0007(10) -0.0140(13) C78 0.0263(13) 0.065(2) 0.0435(17) -0.0065(16) -0.0046(12) 0.0155(14) C79 0.0340(14) 0.0450(18) 0.0283(13) 0.0016(12) -0.0023(11) -0.0177(12) C80 0.0156(9) 0.0242(12) 0.0227(11) 0.0003(9) 0.0033(8) 0.0056(8) O81 0.0204(7) 0.0257(9) 0.0192(7) -0.0005(6) 0.0082(6) 0.0024(6) C82 0.0310(12) 0.0375(15) 0.0290(12) 0.0115(11) 0.0179(10) 0.0075(11) C83 0.0409(14) 0.0283(14) 0.0345(14) 0.0177(11) 0.0203(12) 0.0119(11) C84 0.0292(11) 0.0151(11) 0.0249(11) -0.0002(9) 0.0068(9) 0.0038(9) C85 0.078(2) 0.0236(15) 0.065(2) -0.0045(14) 0.0495(19) 0.0033(14) C86 0.0421(15) 0.0197(13) 0.0401(15) 0.0025(11) -0.0050(12) 0.0053(11) C87 0.0346(13) 0.0209(13) 0.0372(14) -0.0056(11) 0.0054(11) -0.0029(10) O88 0.0540(12) 0.0407(12) 0.0318(10) -0.0033(9) 0.0160(9) 0.0077(10) Cl1A 0.0297(3) 0.0212(3) 0.0325(3) -0.0048(2) 0.0122(2) -0.0031(2) Cl1B 0.0197(2) 0.0237(3) 0.0279(3) 0.0033(2) 0.0064(2) 0.0023(2) O1A 0.0331(12) 0.102(2) 0.097(2) 0.0237(18) 0.0237(13) 0.0118(13) O2A 0.0665(15) 0.0322(12) 0.0713(16) -0.0198(11) 0.0342(13) -0.0037(10) O3A 0.0862(18) 0.0499(15) 0.0342(12) -0.0018(10) 0.0157(12) -0.0189(13) O4A 0.101(2) 0.0328(13) 0.0660(16) -0.0143(11) 0.0535(15) -0.0303(13) O1B 0.0293(9) 0.0491(13) 0.0301(10) -0.0009(9) -0.0012(8) 0.0009(9) O2B 0.0304(10) 0.0403(13) 0.0558(13) 0.0039(10) -0.0042(9) 0.0140(9) O3B 0.0582(14) 0.0565(15) 0.0446(12) -0.0117(10) 0.0326(11) -0.0182(11) O4B 0.0530(13) 0.0249(11) 0.0629(14) 0.0048(10) 0.0225(11) -0.0080(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N50 1.9766(17) . ? Zn1 N57 1.9972(18) . ? Zn1 N1 1.9980(17) . ? Zn1 O88 2.041(2) . ? N1 C5 1.330(3) . ? N1 C2 1.377(3) . ? C2 C3 1.360(3) . ? C2 H2 0.9500 . ? C3 N4 1.356(3) . ? C3 H3 0.9500 . ? N4 C5 1.350(3) . ? N4 C64 1.463(3) . ? C5 C6 1.489(3) . ? C6 O7 1.440(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O7 C8 1.392(2) . ? C8 C9 1.392(3) . ? C8 C13 1.394(3) . ? C9 C10 1.399(3) . ? C9 C49 1.509(3) . ? C10 C11 1.394(3) . ? C10 H10 0.9500 . ? C11 C12 1.398(3) . ? C11 C67 1.531(3) . ? C12 C13 1.397(3) . ? C12 H12 0.9500 . ? C13 C14 1.508(3) . ? C14 C15 1.529(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.393(3) . ? C15 C20 1.400(3) . ? C16 C17 1.401(3) . ? C16 H16 0.9500 . ? C17 N72 1.393(3) . ? C17 C18 1.399(3) . ? C18 C19 1.382(3) . ? C18 H18 0.9500 . ? C19 C20 1.402(3) . ? C19 C21 1.523(3) . ? C20 O74 1.385(3) . ? C21 C22 1.507(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.395(3) . ? C22 C27 1.395(3) . ? C23 O56 1.393(2) . ? C23 C24 1.397(3) . ? C24 C25 1.391(3) . ? C24 C28 1.507(3) . ? C25 C26 1.392(3) . ? C25 H25 0.9500 . ? C26 C27 1.397(3) . ? C26 C76 1.536(3) . ? C27 H27 0.9500 . ? C28 C29 1.525(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.389(3) . ? C29 C34 1.390(3) . ? C30 O81 1.390(2) . ? C30 C31 1.403(3) . ? C31 C32 1.392(3) . ? C31 C35 1.519(3) . ? C32 C33 1.400(3) . ? C32 H32 0.9500 . ? C33 C34 1.384(3) . ? C33 N73 1.396(3) . ? C34 H34 0.9500 . ? C35 C36 1.510(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.385(3) . ? C36 C41 1.402(3) . ? C37 O63 1.393(3) . ? C37 C38 1.400(3) . ? C38 C39 1.387(3) . ? C38 C42 1.504(3) . ? C39 C40 1.409(3) . ? C39 H39 0.9500 . ? C40 C41 1.392(3) . ? C40 C84 1.527(3) . ? C41 H41 0.9500 . ? C42 C43 1.518(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.394(3) . ? C43 C48 1.399(3) . ? C44 C45 1.394(3) . ? C44 H44 0.9500 . ? C45 C46 1.397(3) . ? C45 N71 1.405(3) . ? C46 C47 1.395(3) . ? C46 H46 0.9500 . ? C47 C48 1.389(3) . ? C47 C49 1.522(3) . ? C48 O65 1.396(3) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? N50 C54 1.340(2) . ? N50 C51 1.385(3) . ? C51 C52 1.361(3) . ? C51 H51 0.9500 . ? C52 N53 1.368(3) . ? C52 H52 0.9500 . ? N53 C54 1.347(3) . ? N53 C80 1.466(3) . ? C54 C55 1.490(3) . ? C55 O56 1.445(2) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? N57 C61 1.331(3) . ? N57 C58 1.383(3) . ? C58 C59 1.349(3) . ? C58 H58 0.9500 . ? C59 N60 1.372(3) . ? C59 H59 0.9500 . ? N60 C61 1.346(3) . ? N60 C83 1.472(3) . ? C61 C62 1.490(3) . ? C62 O63 1.449(3) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? O65 C66 1.433(3) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C69 1.526(3) . ? C67 C70 1.533(3) . ? C67 C68 1.547(4) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? N71 H71A 0.8800 . ? N71 H71B 0.8800 . ? N72 H72A 0.8800 . ? N72 H72B 0.8800 . ? N73 H73A 0.8800 . ? N73 H73B 0.8800 . ? O74 C75 1.429(3) . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 C78 1.517(4) . ? C76 C79 1.529(4) . ? C76 C77 1.533(4) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? O81 C82 1.418(3) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 C85 1.523(4) . ? C84 C87 1.528(3) . ? C84 C86 1.540(3) . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? Cl1A O4A 1.412(2) . ? Cl1A O3A 1.424(2) . ? Cl1A O1A 1.424(2) . ? Cl1A O2A 1.430(2) . ? Cl1B O4B 1.427(2) . ? Cl1B O3B 1.431(2) . ? Cl1B O1B 1.4369(19) . ? Cl1B O2B 1.4417(19) . ? C1C C2C 1.482(4) . ? C1C H1C1 0.9800 . ? C1C H1C2 0.9800 . ? C1C H1C3 0.9800 . ? C2C O3C 1.417(3) . ? C2C H2C1 0.9900 . ? C2C H2C2 0.9900 . ? O3C C4C 1.423(3) . ? C4C C5C 1.488(5) . ? C4C H4C1 0.9900 . ? C4C H4C2 0.9900 . ? C5C H5C1 0.9800 . ? C5C H5C2 0.9800 . ? C5C H5C3 0.9800 . ? C1D C2D 1.507(4) . ? C1D H1D1 0.9800 . ? C1D H1D2 0.9800 . ? C1D H1D3 0.9800 . ? C2D O3D 1.425(3) . ? C2D H2D1 0.9900 . ? C2D H2D2 0.9900 . ? O3D C4D 1.420(3) . ? C4D C5D 1.500(4) . ? C4D H4D1 0.9900 . ? C4D H4D2 0.9900 . ? C5D H5D1 0.9800 . ? C5D H5D2 0.9800 . ? C5D H5D3 0.9800 . ? C1E C2E 1.509(6) . ? C1E H1E1 0.9800 . ? C1E H1E2 0.9800 . ? C1E H1E3 0.9800 . ? C2E O3E 1.427(4) . ? C2E H2E1 0.9900 . ? C2E H2E2 0.9900 . ? O3E C4E 1.402(4) . ? C4E C5E 1.486(4) . ? C4E H4E1 0.9900 . ? C4E H4E2 0.9900 . ? C5E H5E1 0.9800 . ? C5E H5E2 0.9800 . ? C5E H5E3 0.9800 . ? C1F C2F 1.449(5) . ? C1F H1F1 0.9800 . ? C1F H1F2 0.9800 . ? C1F H1F3 0.9800 . ? C2F O3F 1.428(5) . ? C2F H2F1 0.9900 . ? C2F H2F2 0.9900 . ? O3F C4F 1.377(5) . ? C4F C5F 1.544(8) . ? C4F H4F1 0.9900 . ? C4F H4F2 0.9900 . ? C5F H5F1 0.9800 . ? C5F H5F2 0.9800 . ? C5F H5F3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N50 Zn1 N57 109.74(7) . . ? N50 Zn1 N1 112.50(7) . . ? N57 Zn1 N1 104.05(7) . . ? N50 Zn1 O88 112.09(8) . . ? N57 Zn1 O88 107.81(8) . . ? N1 Zn1 O88 110.25(8) . . ? C5 N1 C2 106.82(18) . . ? C5 N1 Zn1 129.36(15) . . ? C2 N1 Zn1 123.22(15) . . ? C3 C2 N1 108.5(2) . . ? C3 C2 H2 125.8 . . ? N1 C2 H2 125.8 . . ? N4 C3 C2 106.9(2) . . ? N4 C3 H3 126.6 . . ? C2 C3 H3 126.6 . . ? C5 N4 C3 108.27(19) . . ? C5 N4 C64 126.9(2) . . ? C3 N4 C64 124.9(2) . . ? N1 C5 N4 109.6(2) . . ? N1 C5 C6 125.59(19) . . ? N4 C5 C6 124.84(19) . . ? O7 C6 C5 107.62(18) . . ? O7 C6 H6A 110.2 . . ? C5 C6 H6A 110.2 . . ? O7 C6 H6B 110.2 . . ? C5 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? C8 O7 C6 117.96(17) . . ? C9 C8 O7 116.18(18) . . ? C9 C8 C13 121.53(19) . . ? O7 C8 C13 122.06(18) . . ? C8 C9 C10 118.63(19) . . ? C8 C9 C49 120.74(19) . . ? C10 C9 C49 120.61(19) . . ? C11 C10 C9 121.87(19) . . ? C11 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C10 C11 C12 117.4(2) . . ? C10 C11 C67 122.90(19) . . ? C12 C11 C67 119.7(2) . . ? C13 C12 C11 122.5(2) . . ? C13 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C8 C13 C12 117.96(19) . . ? C8 C13 C14 122.84(19) . . ? C12 C13 C14 119.12(19) . . ? C13 C14 C15 114.86(19) . . ? C13 C14 H14A 108.6 . . ? C15 C14 H14A 108.6 . . ? C13 C14 H14B 108.6 . . ? C15 C14 H14B 108.6 . . ? H14A C14 H14B 107.5 . . ? C16 C15 C20 119.70(19) . . ? C16 C15 C14 122.77(18) . . ? C20 C15 C14 117.52(19) . . ? C15 C16 C17 120.68(19) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? N72 C17 C18 120.5(2) . . ? N72 C17 C16 121.10(19) . . ? C18 C17 C16 118.4(2) . . ? C19 C18 C17 121.8(2) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C18 C19 C20 119.09(19) . . ? C18 C19 C21 122.77(18) . . ? C20 C19 C21 118.13(19) . . ? O74 C20 C15 119.62(18) . . ? O74 C20 C19 119.99(18) . . ? C15 C20 C19 120.2(2) . . ? C22 C21 C19 115.27(18) . . ? C22 C21 H21A 108.5 . . ? C19 C21 H21A 108.5 . . ? C22 C21 H21B 108.5 . . ? C19 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C23 C22 C27 117.82(19) . . ? C23 C22 C21 121.45(18) . . ? C27 C22 C21 120.72(19) . . ? O56 C23 C22 118.84(18) . . ? O56 C23 C24 119.34(18) . . ? C22 C23 C24 121.65(18) . . ? C25 C24 C23 118.30(19) . . ? C25 C24 C28 121.68(18) . . ? C23 C24 C28 119.94(18) . . ? C24 C25 C26 122.28(19) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C25 C26 C27 117.45(19) . . ? C25 C26 C76 122.53(19) . . ? C27 C26 C76 120.0(2) . . ? C22 C27 C26 122.5(2) . . ? C22 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? C24 C28 C29 112.98(17) . . ? C24 C28 H28A 109.0 . . ? C29 C28 H28A 109.0 . . ? C24 C28 H28B 109.0 . . ? C29 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C30 C29 C34 118.90(19) . . ? C30 C29 C28 120.46(19) . . ? C34 C29 C28 120.63(19) . . ? C29 C30 O81 120.08(18) . . ? C29 C30 C31 120.96(19) . . ? O81 C30 C31 118.83(18) . . ? C32 C31 C30 118.79(19) . . ? C32 C31 C35 122.39(19) . . ? C30 C31 C35 118.79(19) . . ? C31 C32 C33 120.8(2) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C34 C33 N73 120.0(2) . . ? C34 C33 C32 119.0(2) . . ? N73 C33 C32 121.0(2) . . ? C33 C34 C29 121.5(2) . . ? C33 C34 H34 119.3 . . ? C29 C34 H34 119.3 . . ? C36 C35 C31 114.25(18) . . ? C36 C35 H35A 108.7 . . ? C31 C35 H35A 108.7 . . ? C36 C35 H35B 108.7 . . ? C31 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? C37 C36 C41 118.63(19) . . ? C37 C36 C35 120.7(2) . . ? C41 C36 C35 120.6(2) . . ? C36 C37 O63 118.38(18) . . ? C36 C37 C38 121.6(2) . . ? O63 C37 C38 119.86(19) . . ? C39 C38 C37 117.9(2) . . ? C39 C38 C42 120.44(18) . . ? C37 C38 C42 121.6(2) . . ? C38 C39 C40 122.81(19) . . ? C38 C39 H39 118.6 . . ? C40 C39 H39 118.6 . . ? C41 C40 C39 116.9(2) . . ? C41 C40 C84 123.6(2) . . ? C39 C40 C84 119.52(19) . . ? C40 C41 C36 122.1(2) . . ? C40 C41 H41 118.9 . . ? C36 C41 H41 118.9 . . ? C38 C42 C43 114.63(17) . . ? C38 C42 H42A 108.6 . . ? C43 C42 H42A 108.6 . . ? C38 C42 H42B 108.6 . . ? C43 C42 H42B 108.6 . . ? H42A C42 H42B 107.6 . . ? C44 C43 C48 118.7(2) . . ? C44 C43 C42 121.7(2) . . ? C48 C43 C42 119.60(19) . . ? C43 C44 C45 121.0(2) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C44 C45 C46 119.1(2) . . ? C44 C45 N71 120.8(2) . . ? C46 C45 N71 120.0(2) . . ? C47 C46 C45 120.8(2) . . ? C47 C46 H46 119.6 . . ? C45 C46 H46 119.6 . . ? C48 C47 C46 119.0(2) . . ? C48 C47 C49 119.99(19) . . ? C46 C47 C49 121.02(19) . . ? C47 C48 O65 119.75(19) . . ? C47 C48 C43 121.36(19) . . ? O65 C48 C43 118.85(19) . . ? C9 C49 C47 113.39(17) . . ? C9 C49 H49A 108.9 . . ? C47 C49 H49A 108.9 . . ? C9 C49 H49B 108.9 . . ? C47 C49 H49B 108.9 . . ? H49A C49 H49B 107.7 . . ? C54 N50 C51 106.40(17) . . ? C54 N50 Zn1 125.86(15) . . ? C51 N50 Zn1 127.50(13) . . ? C52 C51 N50 108.75(18) . . ? C52 C51 H51 125.6 . . ? N50 C51 H51 125.6 . . ? C51 C52 N53 106.70(19) . . ? C51 C52 H52 126.6 . . ? N53 C52 H52 126.6 . . ? C54 N53 C52 108.28(17) . . ? C54 N53 C80 124.90(18) . . ? C52 N53 C80 126.82(19) . . ? N50 C54 N53 109.86(18) . . ? N50 C54 C55 124.98(18) . . ? N53 C54 C55 124.87(18) . . ? O56 C55 C54 108.28(17) . . ? O56 C55 H55A 110.0 . . ? C54 C55 H55A 110.0 . . ? O56 C55 H55B 110.0 . . ? C54 C55 H55B 110.0 . . ? H55A C55 H55B 108.4 . . ? C23 O56 C55 116.03(15) . . ? C61 N57 C58 106.68(18) . . ? C61 N57 Zn1 126.63(14) . . ? C58 N57 Zn1 126.65(14) . . ? C59 C58 N57 108.68(19) . . ? C59 C58 H58 125.7 . . ? N57 C58 H58 125.7 . . ? C58 C59 N60 106.89(19) . . ? C58 C59 H59 126.6 . . ? N60 C59 H59 126.6 . . ? C61 N60 C59 107.92(18) . . ? C61 N60 C83 126.5(2) . . ? C59 N60 C83 125.5(2) . . ? N57 C61 N60 109.82(18) . . ? N57 C61 C62 125.21(19) . . ? N60 C61 C62 124.89(19) . . ? O63 C62 C61 108.99(17) . . ? O63 C62 H62A 109.9 . . ? C61 C62 H62A 109.9 . . ? O63 C62 H62B 109.9 . . ? C61 C62 H62B 109.9 . . ? H62A C62 H62B 108.3 . . ? C37 O63 C62 116.18(16) . . ? N4 C64 H64A 109.5 . . ? N4 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? N4 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C48 O65 C66 113.82(19) . . ? O65 C66 H66A 109.5 . . ? O65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? O65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C69 C67 C11 112.46(19) . . ? C69 C67 C70 108.3(2) . . ? C11 C67 C70 109.67(19) . . ? C69 C67 C68 108.4(2) . . ? C11 C67 C68 109.1(2) . . ? C70 C67 C68 108.9(2) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C67 C70 H70A 109.5 . . ? C67 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C67 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C45 N71 H71A 120.0 . . ? C45 N71 H71B 120.0 . . ? H71A N71 H71B 120.0 . . ? C17 N72 H72A 120.0 . . ? C17 N72 H72B 120.0 . . ? H72A N72 H72B 120.0 . . ? C33 N73 H73A 120.0 . . ? C33 N73 H73B 120.0 . . ? H73A N73 H73B 120.0 . . ? C20 O74 C75 115.32(19) . . ? O74 C75 H75A 109.5 . . ? O74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? O74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C78 C76 C79 109.8(2) . . ? C78 C76 C77 108.4(2) . . ? C79 C76 C77 106.7(2) . . ? C78 C76 C26 108.6(2) . . ? C79 C76 C26 112.0(2) . . ? C77 C76 C26 111.27(19) . . ? C76 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C76 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C76 C78 H78A 109.5 . . ? C76 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C76 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C76 C79 H79A 109.5 . . ? C76 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C76 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? N53 C80 H80A 109.5 . . ? N53 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? N53 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C30 O81 C82 115.09(18) . . ? O81 C82 H82A 109.5 . . ? O81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? O81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N60 C83 H83A 109.5 . . ? N60 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? N60 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C85 C84 C40 109.3(2) . . ? C85 C84 C87 109.4(2) . . ? C40 C84 C87 112.1(2) . . ? C85 C84 C86 110.1(2) . . ? C40 C84 C86 108.93(19) . . ? C87 C84 C86 106.9(2) . . ? C84 C85 H85A 109.5 . . ? C84 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C84 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C84 C86 H86A 109.5 . . ? C84 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C84 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C84 C87 H87A 109.5 . . ? C84 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C84 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? O4A Cl1A O3A 111.46(15) . . ? O4A Cl1A O1A 108.10(18) . . ? O3A Cl1A O1A 107.56(17) . . ? O4A Cl1A O2A 110.72(15) . . ? O3A Cl1A O2A 111.16(16) . . ? O1A Cl1A O2A 107.66(17) . . ? O4B Cl1B O3B 110.59(14) . . ? O4B Cl1B O1B 109.98(13) . . ? O3B Cl1B O1B 109.07(13) . . ? O4B Cl1B O2B 108.92(13) . . ? O3B Cl1B O2B 109.76(15) . . ? O1B Cl1B O2B 108.49(13) . . ? C2C C1C H1C1 109.5 . . ? C2C C1C H1C2 109.5 . . ? H1C1 C1C H1C2 109.5 . . ? C2C C1C H1C3 109.5 . . ? H1C1 C1C H1C3 109.5 . . ? H1C2 C1C H1C3 109.5 . . ? O3C C2C C1C 109.9(2) . . ? O3C C2C H2C1 109.7 . . ? C1C C2C H2C1 109.7 . . ? O3C C2C H2C2 109.7 . . ? C1C C2C H2C2 109.7 . . ? H2C1 C2C H2C2 108.2 . . ? C2C O3C C4C 112.9(2) . . ? O3C C4C C5C 109.3(3) . . ? O3C C4C H4C1 109.8 . . ? C5C C4C H4C1 109.8 . . ? O3C C4C H4C2 109.8 . . ? C5C C4C H4C2 109.8 . . ? H4C1 C4C H4C2 108.3 . . ? C4C C5C H5C1 109.5 . . ? C4C C5C H5C2 109.5 . . ? H5C1 C5C H5C2 109.5 . . ? C4C C5C H5C3 109.5 . . ? H5C1 C5C H5C3 109.5 . . ? H5C2 C5C H5C3 109.5 . . ? C2D C1D H1D1 109.5 . . ? C2D C1D H1D2 109.5 . . ? H1D1 C1D H1D2 109.5 . . ? C2D C1D H1D3 109.5 . . ? H1D1 C1D H1D3 109.5 . . ? H1D2 C1D H1D3 109.5 . . ? O3D C2D C1D 109.2(2) . . ? O3D C2D H2D1 109.8 . . ? C1D C2D H2D1 109.8 . . ? O3D C2D H2D2 109.8 . . ? C1D C2D H2D2 109.8 . . ? H2D1 C2D H2D2 108.3 . . ? C4D O3D C2D 112.6(2) . . ? O3D C4D C5D 109.9(2) . . ? O3D C4D H4D1 109.7 . . ? C5D C4D H4D1 109.7 . . ? O3D C4D H4D2 109.7 . . ? C5D C4D H4D2 109.7 . . ? H4D1 C4D H4D2 108.2 . . ? C4D C5D H5D1 109.5 . . ? C4D C5D H5D2 109.5 . . ? H5D1 C5D H5D2 109.5 . . ? C4D C5D H5D3 109.5 . . ? H5D1 C5D H5D3 109.5 . . ? H5D2 C5D H5D3 109.5 . . ? C2E C1E H1E1 109.5 . . ? C2E C1E H1E2 109.5 . . ? H1E1 C1E H1E2 109.5 . . ? C2E C1E H1E3 109.5 . . ? H1E1 C1E H1E3 109.5 . . ? H1E2 C1E H1E3 109.5 . . ? O3E C2E C1E 108.8(3) . . ? O3E C2E H2E1 109.9 . . ? C1E C2E H2E1 109.9 . . ? O3E C2E H2E2 109.9 . . ? C1E C2E H2E2 109.9 . . ? H2E1 C2E H2E2 108.3 . . ? C4E O3E C2E 112.2(2) . . ? O3E C4E C5E 108.8(3) . . ? O3E C4E H4E1 109.9 . . ? C5E C4E H4E1 109.9 . . ? O3E C4E H4E2 109.9 . . ? C5E C4E H4E2 109.9 . . ? H4E1 C4E H4E2 108.3 . . ? C4E C5E H5E1 109.5 . . ? C4E C5E H5E2 109.5 . . ? H5E1 C5E H5E2 109.5 . . ? C4E C5E H5E3 109.5 . . ? H5E1 C5E H5E3 109.5 . . ? H5E2 C5E H5E3 109.5 . . ? C2F C1F H1F1 109.5 . . ? C2F C1F H1F2 109.5 . . ? H1F1 C1F H1F2 109.5 . . ? C2F C1F H1F3 109.5 . . ? H1F1 C1F H1F3 109.5 . . ? H1F2 C1F H1F3 109.5 . . ? O3F C2F C1F 109.3(3) . . ? O3F C2F H2F1 109.8 . . ? C1F C2F H2F1 109.8 . . ? O3F C2F H2F2 109.8 . . ? C1F C2F H2F2 109.8 . . ? H2F1 C2F H2F2 108.3 . . ? C4F O3F C2F 113.5(3) . . ? O3F C4F C5F 106.4(4) . . ? O3F C4F H4F1 110.4 . . ? C5F C4F H4F1 110.4 . . ? O3F C4F H4F2 110.4 . . ? C5F C4F H4F2 110.4 . . ? H4F1 C4F H4F2 108.6 . . ? C4F C5F H5F1 109.5 . . ? C4F C5F H5F2 109.5 . . ? H5F1 C5F H5F2 109.5 . . ? C4F C5F H5F3 109.5 . . ? H5F1 C5F H5F3 109.5 . . ? H5F2 C5F H5F3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.285 _refine_diff_density_min -1.031 _refine_diff_density_rms 0.116 #===END data_3dopa _database_code_depnum_ccdc_archive 'CCDC 690396' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H102 Cl2 N10 O16 Zn' _chemical_formula_weight 1620.01 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.0388(6) _cell_length_b 16.3548(7) _cell_length_c 20.0055(9) _cell_angle_alpha 75.968(2) _cell_angle_beta 78.527(2) _cell_angle_gamma 88.231(2) _cell_volume 4988.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8625 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 22.71 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.079 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 0.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8699 _exptl_absorpt_correction_T_max 0.9650 _exptl_absorpt_process_details 'SADABS (Sheldrick, V2.10)' _exptl_special_details ; 'Blessing, Acta Cryst. (1995) A51, 33-38' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 512x512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 76509 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.1398 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 30.16 _reflns_number_total 29217 _reflns_number_gt 12362 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The following distance restraints were applied: DFIX 1.5 C65 C67 DFIX -1.5 C72 C75 DFIX 1.5 C72 C74 DFIX -2.5 C66 C67 DFIX 1.5 C65 C66 DFIX -1.42 O97 C98 DFIX 1.42 O99 C100 ; _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^)+(0.1173P)^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 29217 _refine_ls_number_parameters 1017 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1435 _refine_ls_R_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.2158 _refine_ls_wR_factor_gt 0.1927 _refine_ls_goodness_of_fit_ref 0.869 _refine_ls_restrained_S_all 0.871 _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 Zn Zn 0.35914(2) 0.11102(2) 0.616058(18) 0.02762(10) Uani 1 1 d . . . N1 N 0.40927(16) -0.00228(16) 0.61408(13) 0.0334(6) Uani 1 1 d . . . C2 C 0.4952(2) -0.0197(2) 0.60008(17) 0.0411(8) Uani 1 1 d . . . H2 H 0.5406 0.0204 0.5887 0.049 Uiso 1 1 calc R . . C3 C 0.5035(2) -0.1031(2) 0.60530(18) 0.0509(10) Uani 1 1 d . . . H3 H 0.5555 -0.1320 0.5977 0.061 Uiso 1 1 calc R . . N4 N 0.42396(19) -0.13870(17) 0.62336(15) 0.0453(8) Uani 1 1 d . . . C5 C 0.3678(2) -0.07529(19) 0.62837(16) 0.0328(7) Uani 1 1 d . . . C6 C 0.2736(2) -0.0873(2) 0.64858(17) 0.0361(7) Uani 1 1 d . . . H6A H 0.2460 -0.0461 0.6150 0.043 Uiso 1 1 calc R . . H6B H 0.2577 -0.1447 0.6471 0.043 Uiso 1 1 calc R . . O7 O 0.24484(13) -0.07528(12) 0.71887(10) 0.0302(5) Uani 1 1 d . . . C8 C 0.21253(18) -0.14721(17) 0.77051(15) 0.0277(6) Uani 1 1 d . . . C9 C 0.26247(19) -0.18825(18) 0.81697(16) 0.0311(7) Uani 1 1 d . . . C10 C 0.2273(2) -0.25855(19) 0.86902(18) 0.0388(8) Uani 1 1 d . . . H10 H 0.2611 -0.2876 0.9009 0.047 Uiso 1 1 calc R . . C11 C 0.1455(2) -0.2873(2) 0.8759(2) 0.0500(10) Uani 1 1 d . . . C12 C 0.0973(2) -0.2433(2) 0.8282(2) 0.0464(9) Uani 1 1 d . . . H12 H 0.0404 -0.2617 0.8324 0.056 Uiso 1 1 calc R . . C13 C 0.1293(2) -0.17390(19) 0.77489(18) 0.0365(8) Uani 1 1 d . . . C14 C 0.0759(2) -0.1304(2) 0.7220(2) 0.0439(9) Uani 1 1 d . . . H14A H 0.1094 -0.1266 0.6741 0.053 Uiso 1 1 calc R . . H14B H 0.0249 -0.1660 0.7280 0.053 Uiso 1 1 calc R . . C15 C 0.04735(19) -0.04298(19) 0.72786(18) 0.0345(7) Uani 1 1 d . . . C16 C 0.00375(19) -0.0295(2) 0.79153(19) 0.0384(8) Uani 1 1 d . . . H16 H -0.0040 -0.0750 0.8322 0.046 Uiso 1 1 calc R . . C17 C -0.02875(19) 0.0485(2) 0.79718(18) 0.0370(8) Uani 1 1 d . . . C18 C -0.01701(18) 0.1152(2) 0.73599(18) 0.0348(7) Uani 1 1 d . . . H18 H -0.0384 0.1693 0.7391 0.042 Uiso 1 1 calc R . . C19 C 0.02451(19) 0.1036(2) 0.67237(18) 0.0352(7) Uani 1 1 d . . . C20 C 0.05843(19) 0.0243(2) 0.66863(18) 0.0355(7) Uani 1 1 d . . . C21 C 0.0301(2) 0.1727(2) 0.60435(19) 0.0423(8) Uani 1 1 d . . . H21A H 0.0833 0.1654 0.5717 0.051 Uiso 1 1 calc R . . H21B H -0.0179 0.1644 0.5822 0.051 Uiso 1 1 calc R . . C22 C 0.02849(19) 0.2611(2) 0.61210(18) 0.0381(8) Uani 1 1 d . . . C23 C -0.0462(2) 0.3076(2) 0.61460(19) 0.0436(9) Uani 1 1 d . . . H23 H -0.0974 0.2803 0.6139 0.052 Uiso 1 1 calc R . . C24 C -0.0501(2) 0.3901(2) 0.6179(2) 0.0464(9) Uani 1 1 d . . . C25 C 0.02580(19) 0.4286(2) 0.62155(19) 0.0425(9) Uani 1 1 d . . . H25 H 0.0248 0.4854 0.6255 0.051 Uiso 1 1 calc R . . C26 C 0.10251(18) 0.3853(2) 0.61954(17) 0.0352(8) Uani 1 1 d . . . C27 C 0.10195(19) 0.30309(19) 0.61471(17) 0.0339(7) Uani 1 1 d . . . C28 C 0.18287(19) 0.4302(2) 0.62241(17) 0.0359(8) Uani 1 1 d . . . H28A H 0.1708 0.4909 0.6175 0.043 Uiso 1 1 calc R . . H28B H 0.2274 0.4251 0.5816 0.043 Uiso 1 1 calc R . . C29 C 0.21778(18) 0.39778(18) 0.68872(16) 0.0314(7) Uani 1 1 d . . . C30 C 0.1642(2) 0.38610(19) 0.75530(17) 0.0365(8) Uani 1 1 d . . . H30 H 0.1047 0.3941 0.7584 0.044 Uiso 1 1 calc R . . C31 C 0.1965(2) 0.36316(19) 0.81634(17) 0.0353(7) Uani 1 1 d . . . C32 C 0.2837(2) 0.35177(18) 0.81204(17) 0.0344(7) Uani 1 1 d . . . H32 H 0.3061 0.3363 0.8538 0.041 Uiso 1 1 calc R . . C33 C 0.33860(19) 0.36308(18) 0.74636(16) 0.0308(7) Uani 1 1 d . . . C34 C 0.30424(18) 0.38441(17) 0.68542(15) 0.0277(6) Uani 1 1 d . . . C35 C 0.43450(19) 0.35404(19) 0.73965(18) 0.0372(8) Uani 1 1 d . . . H35A H 0.4571 0.3334 0.6971 0.045 Uiso 1 1 calc R . . H35B H 0.4600 0.4106 0.7324 0.045 Uiso 1 1 calc R . . C36 C 0.46372(19) 0.2958(2) 0.80134(18) 0.0360(8) Uani 1 1 d . . . C37 C 0.4806(2) 0.3259(2) 0.85723(19) 0.0412(8) Uani 1 1 d . . . H37 H 0.4724 0.3839 0.8562 0.049 Uiso 1 1 calc R . . C38 C 0.5089(2) 0.2741(2) 0.91429(18) 0.0397(8) Uani 1 1 d . . . C39 C 0.5232(2) 0.1899(2) 0.91292(18) 0.0390(8) Uani 1 1 d . . . H39 H 0.5442 0.1538 0.9506 0.047 Uiso 1 1 calc R . . C40 C 0.50814(19) 0.15683(19) 0.85904(18) 0.0351(7) Uani 1 1 d . . . C41 C 0.47752(18) 0.21077(19) 0.80381(17) 0.0324(7) Uani 1 1 d . . . O42 O 0.45362(13) 0.17818(14) 0.75164(11) 0.0364(5) Uani 1 1 d . . . C43 C 0.52013(19) 0.1623(2) 0.69690(18) 0.0371(8) Uani 1 1 d . . . H43A H 0.5193 0.1017 0.6970 0.045 Uiso 1 1 calc R . . H43B H 0.5760 0.1760 0.7058 0.045 Uiso 1 1 calc R . . C44 C 0.50886(18) 0.21370(19) 0.62756(17) 0.0332(7) Uani 1 1 d . . . N45 N 0.55330(16) 0.28426(17) 0.59037(16) 0.0420(7) Uani 1 1 d . . . C46 C 0.5263(2) 0.3118(2) 0.5281(2) 0.0459(9) Uani 1 1 d . . . H46 H 0.5470 0.3599 0.4916 0.055 Uiso 1 1 calc R . . C47 C 0.4647(2) 0.2572(2) 0.52860(17) 0.0374(8) Uani 1 1 d . . . H47 H 0.4341 0.2604 0.4920 0.045 Uiso 1 1 calc R . . N48 N 0.45328(15) 0.19626(15) 0.59066(13) 0.0292(6) Uani 1 1 d . . . C49 C 0.5264(2) 0.06506(19) 0.85959(19) 0.0375(8) Uani 1 1 d . . . H49A H 0.5647 0.0436 0.8928 0.045 Uiso 1 1 calc R . . H49B H 0.5569 0.0618 0.8122 0.045 Uiso 1 1 calc R . . C50 C 0.4476(2) 0.00782(19) 0.88012(18) 0.0357(7) Uani 1 1 d . . . C51 C 0.3898(2) 0.00506(19) 0.94245(18) 0.0365(8) Uani 1 1 d . . . H51 H 0.3995 0.0397 0.9721 0.044 Uiso 1 1 calc R . . C52 C 0.3186(2) -0.0470(2) 0.96212(17) 0.0352(7) Uani 1 1 d . . . C53 C 0.30567(19) -0.09994(19) 0.92007(17) 0.0340(7) Uani 1 1 d . . . H53 H 0.2574 -0.1368 0.9341 0.041 Uiso 1 1 calc R . . C54 C 0.36332(18) -0.09957(18) 0.85697(16) 0.0309(7) Uani 1 1 d . . . C55 C 0.43385(19) -0.04469(19) 0.83730(16) 0.0311(7) Uani 1 1 d . . . C56 C 0.35269(19) -0.15984(19) 0.81168(17) 0.0340(7) Uani 1 1 d . . . H56A H 0.3763 -0.1320 0.7620 0.041 Uiso 1 1 calc R . . H56B H 0.3870 -0.2104 0.8250 0.041 Uiso 1 1 calc R . . N57 N 0.29832(16) 0.13862(16) 0.53387(14) 0.0339(6) Uani 1 1 d . . . C58 C 0.2914(2) 0.0866(2) 0.49020(17) 0.0397(8) Uani 1 1 d . . . H58 H 0.3181 0.0338 0.4913 0.048 Uiso 1 1 calc R . . C59 C 0.2401(2) 0.1235(2) 0.44541(19) 0.0453(9) Uani 1 1 d . . . H59 H 0.2239 0.1012 0.4101 0.054 Uiso 1 1 calc R . . N60 N 0.21684(18) 0.19731(19) 0.46059(15) 0.0431(7) Uani 1 1 d . . . C61 C 0.25129(19) 0.2071(2) 0.51409(17) 0.0340(7) Uani 1 1 d . . . C62 C 0.23973(19) 0.2788(2) 0.54817(17) 0.0351(7) Uani 1 1 d . . . H62A H 0.2948 0.2938 0.5576 0.042 Uiso 1 1 calc R . . H62B H 0.2202 0.3285 0.5162 0.042 Uiso 1 1 calc R . . O63 O 0.17809(12) 0.25705(13) 0.61332(11) 0.0337(5) Uani 1 1 d . . . C64 C 0.4033(3) -0.2287(2) 0.6356(2) 0.0698(14) Uani 1 1 d . . . H64A H 0.3589 -0.2458 0.6779 0.105 Uiso 1 1 calc R . . H64B H 0.4544 -0.2619 0.6420 0.105 Uiso 1 1 calc R . . H64C H 0.3830 -0.2386 0.5951 0.105 Uiso 1 1 calc R . . C65 C 0.1075(3) -0.3665(3) 0.9316(3) 0.0761(15) Uani 1 1 d D . . C66 C 0.1684(6) -0.4098(7) 0.9715(6) 0.292(9) Uani 1 1 d D . . H66A H 0.1526 -0.4697 0.9885 0.437 Uiso 1 1 calc R . . H66B H 0.1686 -0.3855 1.0117 0.437 Uiso 1 1 calc R . . H66C H 0.2252 -0.4035 0.9415 0.437 Uiso 1 1 calc R . . C67 C 0.0909(8) -0.4307(5) 0.8870(5) 0.249(7) Uani 1 1 d D . . H67A H 0.0359 -0.4596 0.9079 0.373 Uiso 1 1 calc R . . H67B H 0.1362 -0.4723 0.8870 0.373 Uiso 1 1 calc R . . H67C H 0.0904 -0.3997 0.8386 0.373 Uiso 1 1 calc R . . C68 C 0.0183(4) -0.3566(4) 0.9639(4) 0.159(4) Uani 1 1 d . . . H68A H -0.0096 -0.4122 0.9826 0.238 Uiso 1 1 calc R . . H68B H -0.0110 -0.3225 0.9285 0.238 Uiso 1 1 calc R . . H68C H 0.0161 -0.3284 1.0022 0.238 Uiso 1 1 calc R . . N69 N -0.07094(17) 0.06160(18) 0.86115(15) 0.0466(8) Uani 1 1 d . . . H69A H -0.0775 0.0199 0.8991 0.056 Uiso 1 1 calc R . . H69B H -0.0912 0.1116 0.8638 0.056 Uiso 1 1 calc R . . O70 O 0.10531(14) 0.01363(15) 0.60510(12) 0.0419(6) Uani 1 1 d . . . C71 C 0.0545(2) -0.0095(3) 0.5616(2) 0.0553(10) Uani 1 1 d . . . H71A H 0.0272 -0.0646 0.5849 0.083 Uiso 1 1 calc R . . H71B H 0.0906 -0.0126 0.5166 0.083 Uiso 1 1 calc R . . H71C H 0.0107 0.0328 0.5532 0.083 Uiso 1 1 calc R . . C72 C -0.1327(2) 0.4392(2) 0.6136(3) 0.0698(15) Uani 1 1 d D . . C73 C -0.2007(3) 0.3980(3) 0.6684(4) 0.114(3) Uani 1 1 d . . . H73A H -0.1905 0.4033 0.7139 0.171 Uiso 1 1 calc R . . H73B H -0.2032 0.3382 0.6684 0.171 Uiso 1 1 calc R . . H73C H -0.2547 0.4243 0.6604 0.171 Uiso 1 1 calc R . . C74 C -0.1669(3) 0.4228(4) 0.5455(3) 0.117(2) Uani 1 1 d D . . H74A H -0.2218 0.4501 0.5428 0.176 Uiso 1 1 calc R . . H74B H -0.1738 0.3621 0.5509 0.176 Uiso 1 1 calc R . . H74C H -0.1256 0.4465 0.5024 0.176 Uiso 1 1 calc R . . C75 C -0.1191(3) 0.5273(3) 0.5846(5) 0.176(5) Uani 1 1 d D . . H75A H -0.1724 0.5530 0.5739 0.264 Uiso 1 1 calc R . . H75B H -0.0757 0.5366 0.5413 0.264 Uiso 1 1 calc R . . H75C H -0.0998 0.5529 0.6185 0.264 Uiso 1 1 calc R . . N76 N 0.14251(19) 0.35315(18) 0.88274(15) 0.0501(8) Uani 1 1 d . . . H76A H 0.0876 0.3615 0.8858 0.060 Uiso 1 1 calc R . . H76B H 0.1637 0.3386 0.9212 0.060 Uiso 1 1 calc R . . C77 C 0.6190(2) 0.3267(2) 0.6122(2) 0.0606(12) Uani 1 1 d . . . H77A H 0.5942 0.3748 0.6297 0.091 Uiso 1 1 calc R . . H77B H 0.6655 0.3465 0.5719 0.091 Uiso 1 1 calc R . . H77C H 0.6411 0.2870 0.6495 0.091 Uiso 1 1 calc R . . C78 C 0.5264(3) 0.3078(2) 0.9754(2) 0.0531(10) Uani 1 1 d . . . C79 C 0.4847(3) 0.2494(3) 1.0469(2) 0.0730(13) Uani 1 1 d . . . H79A H 0.4948 0.2730 1.0852 0.110 Uiso 1 1 calc R . . H79B H 0.5095 0.1933 1.0513 0.110 Uiso 1 1 calc R . . H79C H 0.4233 0.2450 1.0494 0.110 Uiso 1 1 calc R . . C80 C 0.4928(4) 0.3950(3) 0.9738(3) 0.106(2) Uani 1 1 d . . . H80A H 0.5028 0.4125 1.0151 0.159 Uiso 1 1 calc R . . H80B H 0.4315 0.3948 0.9743 0.159 Uiso 1 1 calc R . . H80C H 0.5220 0.4344 0.9310 0.159 Uiso 1 1 calc R . . C81 C 0.6231(3) 0.3071(3) 0.9720(3) 0.0768(14) Uani 1 1 d . . . H81A H 0.6513 0.3464 0.9288 0.115 Uiso 1 1 calc R . . H81B H 0.6441 0.2502 0.9725 0.115 Uiso 1 1 calc R . . H81C H 0.6353 0.3244 1.0128 0.115 Uiso 1 1 calc R . . N82 N 0.2609(2) -0.04997(18) 1.02558(15) 0.0504(8) Uani 1 1 d . . . H82A H 0.2700 -0.0183 1.0534 0.060 Uiso 1 1 calc R . . H82B H 0.2157 -0.0835 1.0375 0.060 Uiso 1 1 calc R . . O83 O 0.35722(12) 0.38922(12) 0.62055(11) 0.0304(5) Uani 1 1 d . . . C84 C 0.3933(2) 0.47154(19) 0.58654(18) 0.0404(8) Uani 1 1 d . . . H84A H 0.3479 0.5130 0.5847 0.061 Uiso 1 1 calc R . . H84B H 0.4231 0.4720 0.5387 0.061 Uiso 1 1 calc R . . H84C H 0.4337 0.4859 0.6130 0.061 Uiso 1 1 calc R . . O85 O 0.48834(13) -0.03956(13) 0.77267(12) 0.0374(5) Uani 1 1 d . . . C86 C 0.5573(2) -0.0972(2) 0.7756(2) 0.0490(9) Uani 1 1 d . . . H86A H 0.5857 -0.0926 0.8136 0.074 Uiso 1 1 calc R . . H86B H 0.5980 -0.0836 0.7307 0.074 Uiso 1 1 calc R . . H86C H 0.5352 -0.1549 0.7844 0.074 Uiso 1 1 calc R . . C87 C 0.1629(3) 0.2610(3) 0.4213(2) 0.0653(12) Uani 1 1 d . . . H87A H 0.1977 0.3111 0.3951 0.098 Uiso 1 1 calc R . . H87B H 0.1157 0.2770 0.4547 0.098 Uiso 1 1 calc R . . H87C H 0.1403 0.2363 0.3884 0.098 Uiso 1 1 calc R . . N88 N 0.25899(14) 0.10864(15) 0.69720(13) 0.0288(6) Uani 1 1 d . . . H88A H 0.2206 0.1464 0.6794 0.035 Uiso 1 1 calc R . . H88B H 0.2338 0.0561 0.7073 0.035 Uiso 1 1 calc R . . C89 C 0.26504(17) 0.12516(19) 0.76572(15) 0.0282(6) Uani 1 1 d . . . H89A H 0.2855 0.1838 0.7583 0.034 Uiso 1 1 calc R . . H89B H 0.3068 0.0867 0.7869 0.034 Uiso 1 1 calc R . . C90 C 0.17945(19) 0.1123(2) 0.81546(16) 0.0367(8) Uani 1 1 d . . . H90A H 0.1609 0.0529 0.8235 0.044 Uiso 1 1 calc R . . H90B H 0.1377 0.1482 0.7921 0.044 Uiso 1 1 calc R . . C91 C 0.17650(18) 0.13166(18) 0.88675(16) 0.0295(7) Uani 1 1 d . . . C92 C 0.2462(2) 0.15548(19) 0.90770(17) 0.0345(7) Uani 1 1 d . . . H92 H 0.3007 0.1579 0.8779 0.041 Uiso 1 1 calc R . . C93 C 0.2384(2) 0.1764(2) 0.97282(19) 0.0448(9) Uani 1 1 d . . . H93 H 0.2873 0.1941 0.9861 0.054 Uiso 1 1 calc R . . C94 C 0.1602(2) 0.1715(2) 1.01756(19) 0.0472(9) Uani 1 1 d . . . C95 C 0.0896(2) 0.1441(2) 0.99744(17) 0.0377(8) Uani 1 1 d . . . C96 C 0.09699(18) 0.12597(18) 0.93309(16) 0.0299(7) Uani 1 1 d . . . H96 H 0.0478 0.1094 0.9195 0.036 Uiso 1 1 calc R . . O97 O 0.01438(15) 0.14124(16) 1.04553(12) 0.0503(6) Uani 1 1 d D . . C98 C -0.0593(2) 0.1119(2) 1.03058(19) 0.0456(9) Uani 1 1 d D . . H98A H -0.0705 0.1476 0.9864 0.068 Uiso 1 1 calc R . . H98B H -0.1077 0.1140 1.0687 0.068 Uiso 1 1 calc R . . H98C H -0.0513 0.0537 1.0261 0.068 Uiso 1 1 calc R . . O99 O 0.14461(19) 0.1917(2) 1.08145(16) 0.0849(11) Uani 1 1 d D . . C100 C 0.2111(4) 0.2376(6) 1.0951(4) 0.184(5) Uani 1 1 d D . . H10A H 0.2588 0.2001 1.1034 0.276 Uiso 1 1 calc R . . H10B H 0.1898 0.2594 1.1367 0.276 Uiso 1 1 calc R . . H10C H 0.2304 0.2847 1.0545 0.276 Uiso 1 1 calc R . . Cl1A Cl 0.39848(6) 0.40964(6) 0.37319(5) 0.0483(2) Uani 1 1 d . . . O1A O 0.3649(3) 0.3268(3) 0.3850(2) 0.1286(18) Uani 1 1 d . . . O2A O 0.3817(3) 0.4645(3) 0.31087(19) 0.1189(16) Uani 1 1 d . . . O3A O 0.48489(19) 0.3996(2) 0.3674(2) 0.0928(12) Uani 1 1 d . . . O4A O 0.3688(3) 0.4463(3) 0.43160(18) 0.1107(14) Uani 1 1 d . . . Cl2B Cl 0.26210(8) 0.88332(7) 0.43269(7) 0.0772(4) Uani 1 1 d . . . O1B O 0.2899(3) 0.8693(3) 0.4922(2) 0.1363(19) Uani 1 1 d . . . O2B O 0.2514(4) 0.8087(3) 0.4156(3) 0.175(3) Uani 1 1 d . . . O3B O 0.1858(2) 0.9266(3) 0.4351(3) 0.150(2) Uani 1 1 d . . . O4B O 0.3248(2) 0.9285(4) 0.3794(2) 0.158(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.02177(17) 0.03153(19) 0.0246(2) -0.00209(14) 0.00106(13) 0.00132(13) N1 0.0320(14) 0.0384(15) 0.0254(14) -0.0039(11) -0.0005(11) 0.0044(11) C2 0.0283(16) 0.053(2) 0.0290(18) 0.0020(15) 0.0081(13) 0.0118(15) C3 0.043(2) 0.056(2) 0.037(2) 0.0006(17) 0.0146(16) 0.0209(17) N4 0.0496(18) 0.0395(16) 0.0326(16) -0.0013(12) 0.0142(13) 0.0130(13) C5 0.0398(18) 0.0321(16) 0.0220(16) -0.0039(13) 0.0003(13) 0.0068(13) C6 0.0447(19) 0.0364(17) 0.0247(17) -0.0090(13) 0.0007(14) -0.0011(14) O7 0.0336(11) 0.0277(10) 0.0242(11) -0.0050(8) 0.0055(9) -0.0013(8) C8 0.0310(15) 0.0251(14) 0.0226(16) -0.0041(12) 0.0036(12) -0.0018(12) C9 0.0309(16) 0.0315(16) 0.0273(17) -0.0059(13) 0.0010(13) 0.0000(12) C10 0.0392(18) 0.0309(16) 0.039(2) -0.0015(14) 0.0008(15) 0.0023(14) C11 0.050(2) 0.0336(18) 0.053(2) 0.0029(16) 0.0077(18) -0.0065(16) C12 0.0395(19) 0.0383(19) 0.055(2) -0.0079(17) 0.0022(17) -0.0110(15) C13 0.0343(17) 0.0266(15) 0.048(2) -0.0101(14) -0.0044(15) -0.0014(13) C14 0.0403(19) 0.0408(19) 0.056(2) -0.0136(17) -0.0187(17) 0.0008(15) C15 0.0258(15) 0.0350(17) 0.044(2) -0.0077(15) -0.0126(14) -0.0010(13) C16 0.0287(16) 0.0364(17) 0.044(2) 0.0026(15) -0.0063(15) -0.0053(13) C17 0.0230(15) 0.0374(17) 0.045(2) -0.0034(15) -0.0020(14) -0.0027(13) C18 0.0215(14) 0.0356(17) 0.045(2) -0.0060(15) -0.0055(14) 0.0015(12) C19 0.0247(15) 0.0390(17) 0.045(2) -0.0117(15) -0.0125(14) 0.0026(13) C20 0.0262(15) 0.0461(19) 0.0365(19) -0.0125(15) -0.0085(14) -0.0005(14) C21 0.0355(18) 0.047(2) 0.044(2) -0.0095(16) -0.0087(16) 0.0037(15) C22 0.0269(16) 0.0418(18) 0.037(2) 0.0059(15) -0.0061(14) 0.0000(13) C23 0.0264(16) 0.0440(19) 0.050(2) 0.0090(16) -0.0086(15) 0.0031(14) C24 0.0245(16) 0.0372(18) 0.064(3) 0.0111(17) -0.0055(16) 0.0037(13) C25 0.0263(16) 0.0329(17) 0.056(2) 0.0071(15) -0.0011(15) 0.0070(13) C26 0.0244(15) 0.0384(17) 0.0337(18) 0.0078(14) -0.0054(13) 0.0041(13) C27 0.0275(15) 0.0361(17) 0.0326(18) 0.0028(14) -0.0075(13) 0.0073(13) C28 0.0287(16) 0.0355(17) 0.0354(19) 0.0055(14) -0.0056(14) 0.0050(13) C29 0.0277(15) 0.0283(15) 0.0326(18) 0.0020(13) -0.0049(13) 0.0042(12) C30 0.0275(16) 0.0373(17) 0.0363(19) -0.0003(14) 0.0016(14) 0.0063(13) C31 0.0407(18) 0.0296(16) 0.0274(18) -0.0008(13) 0.0049(14) 0.0024(13) C32 0.0397(18) 0.0306(16) 0.0297(18) -0.0004(13) -0.0068(14) -0.0026(13) C33 0.0322(16) 0.0262(15) 0.0310(18) -0.0023(13) -0.0049(13) 0.0032(12) C34 0.0245(14) 0.0256(14) 0.0250(16) 0.0031(12) 0.0023(12) -0.0002(11) C35 0.0291(16) 0.0335(17) 0.043(2) 0.0031(14) -0.0083(15) -0.0032(13) C36 0.0266(15) 0.0419(18) 0.0354(19) 0.0026(15) -0.0098(14) -0.0072(13) C37 0.0410(19) 0.0352(18) 0.045(2) 0.0007(15) -0.0156(16) -0.0012(14) C38 0.0427(19) 0.0407(18) 0.035(2) -0.0023(15) -0.0158(16) 0.0001(15) C39 0.0381(18) 0.0356(17) 0.040(2) 0.0041(15) -0.0163(16) 0.0022(14) C40 0.0281(16) 0.0361(17) 0.0382(19) -0.0003(14) -0.0097(14) -0.0021(13) C41 0.0248(15) 0.0348(17) 0.0371(19) -0.0042(14) -0.0093(13) -0.0042(12) O42 0.0258(11) 0.0488(13) 0.0341(13) -0.0077(10) -0.0071(10) -0.0050(9) C43 0.0273(16) 0.0381(17) 0.043(2) -0.0062(15) -0.0053(15) -0.0025(13) C44 0.0234(15) 0.0317(16) 0.0380(19) -0.0044(14) 0.0045(13) -0.0010(12) N45 0.0289(14) 0.0383(15) 0.0499(19) -0.0079(14) 0.0111(13) -0.0095(12) C46 0.0365(18) 0.0350(18) 0.046(2) 0.0059(15) 0.0202(16) 0.0020(14) C47 0.0314(16) 0.0388(17) 0.0297(18) 0.0050(14) 0.0057(13) 0.0060(14) N48 0.0238(12) 0.0337(13) 0.0242(14) -0.0013(11) 0.0022(10) 0.0022(10) C49 0.0346(17) 0.0351(17) 0.040(2) -0.0015(14) -0.0114(15) -0.0007(13) C50 0.0328(17) 0.0341(17) 0.038(2) -0.0013(14) -0.0121(15) 0.0031(13) C51 0.0408(18) 0.0307(16) 0.0356(19) -0.0012(14) -0.0100(15) -0.0011(14) C52 0.0402(18) 0.0359(17) 0.0249(17) -0.0012(13) -0.0032(14) 0.0018(14) C53 0.0301(16) 0.0355(17) 0.0319(18) -0.0035(14) -0.0012(14) -0.0014(13) C54 0.0272(15) 0.0291(15) 0.0320(18) -0.0007(13) -0.0040(13) 0.0048(12) C55 0.0287(15) 0.0319(16) 0.0271(17) 0.0019(13) -0.0036(13) 0.0013(12) C56 0.0310(16) 0.0314(16) 0.0352(19) -0.0035(14) -0.0020(14) 0.0025(13) N57 0.0308(14) 0.0349(14) 0.0303(15) -0.0022(12) 0.0005(11) -0.0005(11) C58 0.047(2) 0.0427(19) 0.0263(18) -0.0101(15) 0.0019(15) 0.0006(15) C59 0.050(2) 0.055(2) 0.033(2) -0.0100(17) -0.0131(17) 0.0002(17) N60 0.0408(16) 0.0537(18) 0.0364(17) -0.0087(14) -0.0158(13) 0.0106(13) C61 0.0257(15) 0.0428(18) 0.0297(18) -0.0034(14) -0.0036(13) 0.0019(13) C62 0.0276(15) 0.0403(17) 0.0326(18) -0.0049(14) -0.0005(13) 0.0057(13) O63 0.0247(10) 0.0431(12) 0.0273(12) 0.0010(9) -0.0036(9) 0.0089(9) C64 0.091(3) 0.0325(19) 0.061(3) -0.0010(18) 0.030(2) 0.010(2) C65 0.079(3) 0.039(2) 0.079(3) 0.023(2) 0.015(3) -0.010(2) C66 0.196(10) 0.257(12) 0.277(14) 0.229(12) -0.055(9) -0.085(9) C67 0.338(15) 0.068(5) 0.251(13) -0.021(6) 0.139(12) -0.047(7) C68 0.098(5) 0.135(6) 0.149(7) 0.068(5) 0.069(4) 0.014(4) N69 0.0383(16) 0.0474(17) 0.0402(18) 0.0023(14) 0.0094(13) -0.0008(13) O70 0.0390(13) 0.0551(14) 0.0377(14) -0.0185(11) -0.0137(11) 0.0037(11) C71 0.052(2) 0.075(3) 0.049(2) -0.024(2) -0.024(2) 0.008(2) C72 0.0196(16) 0.051(2) 0.106(4) 0.034(2) -0.003(2) 0.0077(15) C73 0.039(2) 0.068(3) 0.193(7) 0.012(4) 0.021(3) 0.020(2) C74 0.064(3) 0.122(5) 0.135(6) 0.031(4) -0.025(4) 0.014(3) C75 0.043(3) 0.080(4) 0.317(11) 0.095(5) -0.008(4) 0.018(3) N76 0.0495(18) 0.0542(18) 0.0346(17) -0.0037(14) 0.0098(14) 0.0105(14) C77 0.0325(19) 0.054(2) 0.089(3) -0.023(2) 0.013(2) -0.0135(17) C78 0.065(3) 0.052(2) 0.050(2) -0.0127(19) -0.029(2) 0.0075(19) C79 0.090(4) 0.071(3) 0.064(3) -0.022(2) -0.022(3) -0.001(3) C80 0.185(6) 0.068(3) 0.102(4) -0.042(3) -0.097(5) 0.042(4) C81 0.081(3) 0.079(3) 0.076(3) -0.011(3) -0.036(3) -0.012(3) N82 0.063(2) 0.0474(17) 0.0365(18) -0.0155(14) 0.0093(15) -0.0126(15) O83 0.0232(10) 0.0317(11) 0.0287(12) 0.0013(9) 0.0021(9) -0.0005(8) C84 0.0344(17) 0.0361(17) 0.039(2) 0.0064(15) 0.0026(15) -0.0075(14) O85 0.0302(11) 0.0372(12) 0.0363(13) -0.0014(10) 0.0036(10) 0.0015(9) C86 0.0318(18) 0.049(2) 0.057(3) -0.0069(18) 0.0060(17) 0.0037(15) C87 0.061(3) 0.084(3) 0.053(3) -0.009(2) -0.031(2) 0.020(2) N88 0.0232(12) 0.0286(13) 0.0288(14) -0.0009(10) 0.0010(10) 0.0010(10) C89 0.0218(14) 0.0345(16) 0.0248(16) -0.0023(13) -0.0021(12) 0.0008(12) C90 0.0253(15) 0.057(2) 0.0254(17) -0.0102(15) 0.0024(13) -0.0034(14) C91 0.0275(15) 0.0299(15) 0.0242(16) 0.0007(12) 0.0029(12) -0.0026(12) C92 0.0298(16) 0.0371(17) 0.0302(18) -0.0024(14) 0.0019(13) 0.0002(13) C93 0.042(2) 0.053(2) 0.035(2) -0.0075(16) 0.0002(16) -0.0127(16) C94 0.047(2) 0.064(2) 0.032(2) -0.0192(17) 0.0007(16) -0.0060(18) C95 0.0425(19) 0.0348(17) 0.0268(18) -0.0049(14) 0.0118(14) -0.0051(14) C96 0.0264(15) 0.0285(15) 0.0290(17) -0.0019(12) 0.0023(13) -0.0016(12) O97 0.0388(13) 0.0684(17) 0.0354(14) -0.0152(12) 0.0176(11) -0.0138(12) C98 0.0363(19) 0.052(2) 0.040(2) -0.0078(17) 0.0072(16) -0.0006(16) O99 0.0633(19) 0.150(3) 0.0491(19) -0.053(2) 0.0125(15) -0.038(2) C100 0.119(5) 0.358(12) 0.114(6) -0.170(7) 0.042(4) -0.111(7) Cl1A 0.0425(5) 0.0589(6) 0.0366(5) 0.0003(4) -0.0070(4) 0.0031(4) O1A 0.167(4) 0.140(3) 0.073(3) -0.009(2) -0.012(3) -0.107(3) O2A 0.171(4) 0.116(3) 0.070(3) -0.007(2) -0.055(3) 0.080(3) O3A 0.0469(18) 0.086(2) 0.153(4) -0.052(2) -0.012(2) 0.0154(16) O4A 0.159(4) 0.119(3) 0.047(2) -0.021(2) -0.008(2) 0.045(3) Cl2B 0.0791(8) 0.0637(7) 0.0842(10) -0.0297(7) 0.0105(7) -0.0046(6) O1B 0.204(5) 0.115(3) 0.074(3) 0.042(2) -0.068(3) -0.011(3) O2B 0.271(7) 0.098(3) 0.214(6) -0.100(4) -0.112(5) 0.054(4) O3B 0.064(2) 0.127(3) 0.245(6) -0.096(4) 0.061(3) 0.002(2) O4B 0.044(2) 0.309(7) 0.107(4) -0.044(4) 0.013(2) -0.021(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 Zn N48 1.991(2) . ? Zn N1 2.003(3) . ? Zn N57 2.027(3) . ? Zn N88 2.038(2) . ? N1 C5 1.326(4) . ? N1 C2 1.386(4) . ? C2 C3 1.348(5) . ? C2 H2 0.9500 . ? C3 N4 1.363(5) . ? C3 H3 0.9500 . ? N4 C5 1.361(4) . ? N4 C64 1.470(5) . ? C5 C6 1.491(4) . ? C6 O7 1.448(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O7 C8 1.398(3) . ? C8 C9 1.384(4) . ? C8 C13 1.397(4) . ? C9 C10 1.396(4) . ? C9 C56 1.509(4) . ? C10 C11 1.378(5) . ? C10 H10 0.9500 . ? C11 C12 1.397(5) . ? C11 C65 1.540(5) . ? C12 C13 1.386(4) . ? C12 H12 0.9500 . ? C13 C14 1.521(5) . ? C14 C15 1.513(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.390(5) . ? C15 C20 1.393(4) . ? C16 C17 1.385(5) . ? C16 H16 0.9500 . ? C17 N69 1.386(4) . ? C17 C18 1.414(4) . ? C18 C19 1.368(5) . ? C18 H18 0.9500 . ? C19 C20 1.404(4) . ? C19 C21 1.533(5) . ? C20 O70 1.389(4) . ? C21 C22 1.489(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.398(4) . ? C22 C23 1.399(4) . ? C23 C24 1.366(5) . ? C23 H23 0.9500 . ? C24 C25 1.409(5) . ? C24 C72 1.535(4) . ? C25 C26 1.399(4) . ? C25 H25 0.9500 . ? C26 C27 1.372(5) . ? C26 C28 1.521(4) . ? C27 O63 1.414(3) . ? C28 C29 1.514(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C34 1.388(4) . ? C29 C30 1.407(4) . ? C30 C31 1.385(5) . ? C30 H30 0.9500 . ? C31 C32 1.394(4) . ? C31 N76 1.410(4) . ? C32 C33 1.403(4) . ? C32 H32 0.9500 . ? C33 C34 1.400(4) . ? C33 C35 1.523(4) . ? C34 O83 1.389(3) . ? C35 C36 1.511(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C41 1.392(4) . ? C36 C37 1.401(5) . ? C37 C38 1.393(4) . ? C37 H37 0.9500 . ? C38 C39 1.394(5) . ? C38 C78 1.534(5) . ? C39 C40 1.381(5) . ? C39 H39 0.9500 . ? C40 C41 1.399(4) . ? C40 C49 1.518(4) . ? C41 O42 1.401(4) . ? O42 C43 1.436(4) . ? C43 C44 1.480(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 N48 1.342(4) . ? C44 N45 1.348(4) . ? N45 C46 1.369(5) . ? N45 C77 1.468(5) . ? C46 C47 1.349(5) . ? C46 H46 0.9500 . ? C47 N48 1.374(4) . ? C47 H47 0.9500 . ? C49 C50 1.523(4) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.390(5) . ? C50 C55 1.401(5) . ? C51 C52 1.380(4) . ? C51 H51 0.9500 . ? C52 C53 1.390(5) . ? C52 N82 1.406(4) . ? C53 C54 1.407(4) . ? C53 H53 0.9500 . ? C54 C55 1.398(4) . ? C54 C56 1.525(4) . ? C55 O85 1.395(4) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? N57 C61 1.353(4) . ? N57 C58 1.380(4) . ? C58 C59 1.357(5) . ? C58 H58 0.9500 . ? C59 N60 1.340(5) . ? C59 H59 0.9500 . ? N60 C61 1.342(4) . ? N60 C87 1.506(4) . ? C61 C62 1.483(5) . ? C62 O63 1.445(4) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.443(9) . ? C65 C68 1.469(7) . ? C65 C67 1.593(10) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? N69 H69A 0.8800 . ? N69 H69B 0.8800 . ? O70 C71 1.423(4) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C75 1.422(6) . ? C72 C73 1.434(6) . ? C72 C74 1.648(8) . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? N76 H76A 0.8800 . ? N76 H76B 0.8800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 C80 1.504(6) . ? C78 C81 1.538(6) . ? C78 C79 1.550(6) . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? N82 H82A 0.8800 . ? N82 H82B 0.8800 . ? O83 C84 1.435(3) . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? O85 C86 1.432(4) . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? N88 C89 1.482(4) . ? N88 H88A 0.9200 . ? N88 H88B 0.9200 . ? C89 C90 1.514(4) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C90 C91 1.526(4) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 C92 1.368(4) . ? C91 C96 1.411(4) . ? C92 C93 1.407(5) . ? C92 H92 0.9500 . ? C93 C94 1.381(5) . ? C93 H93 0.9500 . ? C94 O99 1.370(4) . ? C94 C95 1.394(5) . ? C95 C96 1.372(4) . ? C95 O97 1.380(4) . ? C96 H96 0.9500 . ? O97 C98 1.401(4) . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? O99 C100 1.428(6) . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? Cl1A O3A 1.375(3) . ? Cl1A O2A 1.417(3) . ? Cl1A O1A 1.422(4) . ? Cl1A O4A 1.432(4) . ? Cl2B O1B 1.319(4) . ? Cl2B O2B 1.369(4) . ? Cl2B O4B 1.389(4) . ? Cl2B O3B 1.394(4) . ? 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 N48 Zn N1 108.71(10) . . ? N48 Zn N57 104.87(10) . . ? N1 Zn N57 104.40(11) . . ? N48 Zn N88 122.38(10) . . ? N1 Zn N88 113.83(10) . . ? N57 Zn N88 100.28(10) . . ? C5 N1 C2 106.6(3) . . ? C5 N1 Zn 127.3(2) . . ? C2 N1 Zn 126.1(2) . . ? C3 C2 N1 108.4(3) . . ? C3 C2 H2 125.8 . . ? N1 C2 H2 125.8 . . ? C2 C3 N4 107.8(3) . . ? C2 C3 H3 126.1 . . ? N4 C3 H3 126.1 . . ? C5 N4 C3 107.0(3) . . ? C5 N4 C64 126.8(3) . . ? C3 N4 C64 126.2(3) . . ? N1 C5 N4 110.1(3) . . ? N1 C5 C6 125.4(3) . . ? N4 C5 C6 124.5(3) . . ? O7 C6 C5 109.3(3) . . ? O7 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? O7 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? C8 O7 C6 115.9(2) . . ? C9 C8 C13 122.0(3) . . ? C9 C8 O7 119.5(3) . . ? C13 C8 O7 118.6(3) . . ? C8 C9 C10 117.9(3) . . ? C8 C9 C56 121.9(3) . . ? C10 C9 C56 120.2(3) . . ? C11 C10 C9 122.5(3) . . ? C11 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? C10 C11 C12 117.5(3) . . ? C10 C11 C65 122.7(4) . . ? C12 C11 C65 119.8(4) . . ? C13 C12 C11 122.5(3) . . ? C13 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C12 C13 C8 117.7(3) . . ? C12 C13 C14 120.7(3) . . ? C8 C13 C14 121.6(3) . . ? C15 C14 C13 114.9(3) . . ? C15 C14 H14A 108.5 . . ? C13 C14 H14A 108.5 . . ? C15 C14 H14B 108.5 . . ? C13 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? C16 C15 C20 118.6(3) . . ? C16 C15 C14 120.4(3) . . ? C20 C15 C14 120.8(3) . . ? C17 C16 C15 121.7(3) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 N69 121.2(3) . . ? C16 C17 C18 118.3(3) . . ? N69 C17 C18 120.5(3) . . ? C19 C18 C17 121.4(3) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C18 C19 C20 119.0(3) . . ? C18 C19 C21 121.9(3) . . ? C20 C19 C21 119.0(3) . . ? O70 C20 C15 119.8(3) . . ? O70 C20 C19 119.2(3) . . ? C15 C20 C19 121.0(3) . . ? C22 C21 C19 116.0(3) . . ? C22 C21 H21A 108.3 . . ? C19 C21 H21A 108.3 . . ? C22 C21 H21B 108.3 . . ? C19 C21 H21B 108.3 . . ? H21A C21 H21B 107.4 . . ? C27 C22 C23 116.3(3) . . ? C27 C22 C21 122.0(3) . . ? C23 C22 C21 121.7(3) . . ? C24 C23 C22 123.9(3) . . ? C24 C23 H23 118.1 . . ? C22 C23 H23 118.1 . . ? C23 C24 C25 117.2(3) . . ? C23 C24 C72 120.7(3) . . ? C25 C24 C72 122.1(3) . . ? C26 C25 C24 121.7(3) . . ? C26 C25 H25 119.2 . . ? C24 C25 H25 119.2 . . ? C27 C26 C25 118.0(3) . . ? C27 C26 C28 122.5(3) . . ? C25 C26 C28 119.6(3) . . ? C26 C27 C22 123.0(3) . . ? C26 C27 O63 119.6(3) . . ? C22 C27 O63 117.4(3) . . ? C26 C28 C29 115.1(2) . . ? C26 C28 H28A 108.5 . . ? C29 C28 H28A 108.5 . . ? C26 C28 H28B 108.5 . . ? C29 C28 H28B 108.5 . . ? H28A C28 H28B 107.5 . . ? C34 C29 C30 118.4(3) . . ? C34 C29 C28 120.8(3) . . ? C30 C29 C28 120.7(3) . . ? C31 C30 C29 121.2(3) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C30 C31 C32 119.6(3) . . ? C30 C31 N76 120.8(3) . . ? C32 C31 N76 119.6(3) . . ? C31 C32 C33 120.3(3) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C34 C33 C32 119.0(3) . . ? C34 C33 C35 119.3(3) . . ? C32 C33 C35 121.7(3) . . ? C29 C34 O83 119.3(3) . . ? C29 C34 C33 121.3(3) . . ? O83 C34 C33 119.3(3) . . ? C36 C35 C33 115.8(3) . . ? C36 C35 H35A 108.3 . . ? C33 C35 H35A 108.3 . . ? C36 C35 H35B 108.3 . . ? C33 C35 H35B 108.3 . . ? H35A C35 H35B 107.4 . . ? C41 C36 C37 117.4(3) . . ? C41 C36 C35 121.4(3) . . ? C37 C36 C35 121.2(3) . . ? C36 C37 C38 122.6(3) . . ? C36 C37 H37 118.7 . . ? C38 C37 H37 118.7 . . ? C39 C38 C37 117.2(3) . . ? C39 C38 C78 120.8(3) . . ? C37 C38 C78 122.0(3) . . ? C40 C39 C38 122.7(3) . . ? C40 C39 H39 118.7 . . ? C38 C39 H39 118.7 . . ? C39 C40 C41 118.0(3) . . ? C39 C40 C49 120.5(3) . . ? C41 C40 C49 121.5(3) . . ? C36 C41 C40 122.1(3) . . ? C36 C41 O42 117.9(3) . . ? C40 C41 O42 119.8(3) . . ? C41 O42 C43 117.5(2) . . ? O42 C43 C44 110.5(2) . . ? O42 C43 H43A 109.5 . . ? C44 C43 H43A 109.5 . . ? O42 C43 H43B 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 108.1 . . ? N48 C44 N45 108.7(3) . . ? N48 C44 C43 125.1(3) . . ? N45 C44 C43 126.1(3) . . ? C44 N45 C46 108.6(3) . . ? C44 N45 C77 126.7(3) . . ? C46 N45 C77 124.7(3) . . ? C47 C46 N45 106.6(3) . . ? C47 C46 H46 126.7 . . ? N45 C46 H46 126.7 . . ? C46 C47 N48 109.0(3) . . ? C46 C47 H47 125.5 . . ? N48 C47 H47 125.5 . . ? C44 N48 C47 107.1(3) . . ? C44 N48 Zn 131.4(2) . . ? C47 N48 Zn 121.2(2) . . ? C40 C49 C50 114.5(3) . . ? C40 C49 H49A 108.6 . . ? C50 C49 H49A 108.6 . . ? C40 C49 H49B 108.6 . . ? C50 C49 H49B 108.6 . . ? H49A C49 H49B 107.6 . . ? C51 C50 C55 119.1(3) . . ? C51 C50 C49 120.6(3) . . ? C55 C50 C49 120.3(3) . . ? C52 C51 C50 121.3(3) . . ? C52 C51 H51 119.3 . . ? C50 C51 H51 119.3 . . ? C51 C52 C53 119.5(3) . . ? C51 C52 N82 120.9(3) . . ? C53 C52 N82 119.5(3) . . ? C52 C53 C54 120.8(3) . . ? C52 C53 H53 119.6 . . ? C54 C53 H53 119.6 . . ? C55 C54 C53 118.6(3) . . ? C55 C54 C56 119.6(3) . . ? C53 C54 C56 121.7(3) . . ? O85 C55 C54 119.2(3) . . ? O85 C55 C50 120.0(3) . . ? C54 C55 C50 120.7(3) . . ? C9 C56 C54 115.5(3) . . ? C9 C56 H56A 108.4 . . ? C54 C56 H56A 108.4 . . ? C9 C56 H56B 108.4 . . ? C54 C56 H56B 108.4 . . ? H56A C56 H56B 107.5 . . ? C61 N57 C58 106.3(3) . . ? C61 N57 Zn 127.8(2) . . ? C58 N57 Zn 125.8(2) . . ? C59 C58 N57 108.7(3) . . ? C59 C58 H58 125.6 . . ? N57 C58 H58 125.6 . . ? N60 C59 C58 106.7(3) . . ? N60 C59 H59 126.6 . . ? C58 C59 H59 126.6 . . ? C61 N60 C59 109.8(3) . . ? C61 N60 C87 125.4(3) . . ? C59 N60 C87 124.7(3) . . ? N60 C61 N57 108.4(3) . . ? N60 C61 C62 127.1(3) . . ? N57 C61 C62 124.4(3) . . ? O63 C62 C61 110.5(3) . . ? O63 C62 H62A 109.6 . . ? C61 C62 H62A 109.6 . . ? O63 C62 H62B 109.6 . . ? C61 C62 H62B 109.6 . . ? H62A C62 H62B 108.1 . . ? C27 O63 C62 115.5(2) . . ? N4 C64 H64A 109.5 . . ? N4 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? N4 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 C68 122.5(6) . . ? C66 C65 C11 112.9(5) . . ? C68 C65 C11 112.9(4) . . ? C66 C65 C67 103.1(7) . . ? C68 C65 C67 97.4(6) . . ? C11 C65 C67 104.2(4) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C17 N69 H69A 120.0 . . ? C17 N69 H69B 120.0 . . ? H69A N69 H69B 120.0 . . ? C20 O70 C71 113.4(3) . . ? O70 C71 H71A 109.5 . . ? O70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? O70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C75 C72 C73 127.7(5) . . ? C75 C72 C24 113.5(3) . . ? C73 C72 C24 110.4(3) . . ? C75 C72 C74 94.2(5) . . ? C73 C72 C74 98.9(4) . . ? C24 C72 C74 106.9(4) . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C72 C74 H74A 109.5 . . ? C72 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C72 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C72 C75 H75A 109.5 . . ? C72 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C72 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C31 N76 H76A 120.0 . . ? C31 N76 H76B 120.0 . . ? H76A N76 H76B 120.0 . . ? N45 C77 H77A 109.5 . . ? N45 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? N45 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C80 C78 C38 112.5(3) . . ? C80 C78 C81 110.4(4) . . ? C38 C78 C81 108.1(4) . . ? C80 C78 C79 107.7(4) . . ? C38 C78 C79 110.7(3) . . ? C81 C78 C79 107.3(3) . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C78 C80 H80A 109.5 . . ? C78 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C78 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C78 C81 H81A 109.5 . . ? C78 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C78 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C52 N82 H82A 120.0 . . ? C52 N82 H82B 120.0 . . ? H82A N82 H82B 120.0 . . ? C34 O83 C84 114.2(2) . . ? O83 C84 H84A 109.5 . . ? O83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? O83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C55 O85 C86 114.0(2) . . ? O85 C86 H86A 109.5 . . ? O85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? O85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N60 C87 H87A 109.5 . . ? N60 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? N60 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C89 N88 Zn 125.01(18) . . ? C89 N88 H88A 106.1 . . ? Zn N88 H88A 106.1 . . ? C89 N88 H88B 106.1 . . ? Zn N88 H88B 106.1 . . ? H88A N88 H88B 106.3 . . ? N88 C89 C90 110.9(2) . . ? N88 C89 H89A 109.4 . . ? C90 C89 H89A 109.4 . . ? N88 C89 H89B 109.4 . . ? C90 C89 H89B 109.4 . . ? H89A C89 H89B 108.0 . . ? C89 C90 C91 115.9(3) . . ? C89 C90 H90A 108.3 . . ? C91 C90 H90A 108.3 . . ? C89 C90 H90B 108.3 . . ? C91 C90 H90B 108.3 . . ? H90A C90 H90B 107.4 . . ? C92 C91 C96 118.3(3) . . ? C92 C91 C90 123.7(3) . . ? C96 C91 C90 118.0(3) . . ? C91 C92 C93 120.8(3) . . ? C91 C92 H92 119.6 . . ? C93 C92 H92 119.6 . . ? C94 C93 C92 120.5(3) . . ? C94 C93 H93 119.8 . . ? C92 C93 H93 119.8 . . ? O99 C94 C93 125.6(3) . . ? O99 C94 C95 115.6(3) . . ? C93 C94 C95 118.7(3) . . ? C96 C95 O97 124.8(3) . . ? C96 C95 C94 120.7(3) . . ? O97 C95 C94 114.5(3) . . ? C95 C96 C91 120.9(3) . . ? C95 C96 H96 119.5 . . ? C91 C96 H96 119.5 . . ? C95 O97 C98 118.3(3) . . ? O97 C98 H98A 109.5 . . ? O97 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? O97 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C94 O99 C100 115.6(3) . . ? O99 C100 H10A 109.5 . . ? O99 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? O99 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? O3A Cl1A O2A 109.4(3) . . ? O3A Cl1A O1A 104.9(3) . . ? O2A Cl1A O1A 113.0(3) . . ? O3A Cl1A O4A 107.6(2) . . ? O2A Cl1A O4A 109.6(2) . . ? O1A Cl1A O4A 112.1(3) . . ? O1B Cl2B O2B 110.2(3) . . ? O1B Cl2B O4B 108.1(3) . . ? O2B Cl2B O4B 106.2(4) . . ? O1B Cl2B O3B 113.0(4) . . ? O2B Cl2B O3B 108.9(4) . . ? O4B Cl2B O3B 110.2(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.16 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.474 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.107 #===END data_3benzyl _database_code_depnum_ccdc_archive 'CCDC 690397' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H96 Cl2 N10 O14 Zn' _chemical_formula_weight 1545.93 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(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 19.874(3) _cell_length_b 25.382(4) _cell_length_c 23.188(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.988(6) _cell_angle_gamma 90.00 _cell_volume 10602(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9886 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 21.74 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.968 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 0.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9674 _exptl_absorpt_correction_T_max 0.9868 _exptl_absorpt_process_details 'SADABS (Sheldrick, V2.10)' _exptl_special_details ; 'Blessing, Acta Cryst. (1995) A51, 33-38' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 512x512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 284267 _diffrn_reflns_av_R_equivalents 0.1614 _diffrn_reflns_av_sigmaI/netI 0.1105 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 25.20 _reflns_number_total 18776 _reflns_number_gt 9992 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The following distance restraints were applied: DFIX -1.5 N89 C90 DFIX 1.4 CL1A O1A DFIX -2.4 O1A O4A DFIX 2.3 O1A O2A DFIX 2.3 O1A O3A DFIX -3.5 O1A C64_$1 ; _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^)+(0.1900P)^2^+58.0000P] 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 18776 _refine_ls_number_parameters 915 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1910 _refine_ls_R_factor_gt 0.1406 _refine_ls_wR_factor_ref 0.3715 _refine_ls_wR_factor_gt 0.3437 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.679085(19) 0.030097(13) 0.124687(15) 0.02519(10) Uani 1 1 d . . . N1 N 0.62238(14) 0.05629(9) 0.17228(10) 0.0264(7) Uani 1 1 d . . . C2 C 0.55352(14) 0.07868(11) 0.14303(12) 0.0219(8) Uani 1 1 d . . . H2 H 0.5275 0.0851 0.0987 0.026 Uiso 1 1 calc R . . C3 C 0.52836(17) 0.09028(12) 0.18787(14) 0.0300(10) Uani 1 1 d . . . H3 H 0.4828 0.1070 0.1810 0.036 Uiso 1 1 calc R . . N4 N 0.58179(14) 0.07305(10) 0.24494(11) 0.0291(8) Uani 1 1 d . . . C5 C 0.63631(15) 0.05425(11) 0.23306(11) 0.0204(8) Uani 1 1 d . . . C6 C 0.70784(15) 0.03067(12) 0.28370(12) 0.0224(8) Uani 1 1 d . . . H6A H 0.6997 0.0207 0.3215 0.027 Uiso 1 1 calc R . . H6B H 0.7209 -0.0016 0.2667 0.027 Uiso 1 1 calc R . . O7 O 0.76763(10) 0.06743(8) 0.30189(8) 0.0271(6) Uani 1 1 d . . . C8 C 0.79165(15) 0.09072(11) 0.36225(11) 0.0200(8) Uani 1 1 d . . . C9 C 0.83672(15) 0.06018(11) 0.41557(11) 0.0212(8) Uani 1 1 d . . . C10 C 0.86180(15) 0.08479(12) 0.47535(12) 0.0230(8) Uani 1 1 d . . . H10 H 0.8933 0.0657 0.5121 0.028 Uiso 1 1 calc R . . C11 C 0.84206(16) 0.13641(12) 0.48280(12) 0.0257(9) Uani 1 1 d . . . C12 C 0.79817(16) 0.16502(11) 0.42758(12) 0.0238(8) Uani 1 1 d . . . H12 H 0.7855 0.2005 0.4315 0.029 Uiso 1 1 calc R . . C13 C 0.77278(15) 0.14220(11) 0.36707(12) 0.0213(8) Uani 1 1 d . . . C14 C 0.72136(15) 0.17334(12) 0.30971(13) 0.0241(9) Uani 1 1 d . . . H14A H 0.6946 0.1993 0.3241 0.029 Uiso 1 1 calc R . . H14B H 0.6838 0.1488 0.2802 0.029 Uiso 1 1 calc R . . C15 C 0.75693(15) 0.20264(11) 0.27250(11) 0.0229(8) Uani 1 1 d . . . C16 C 0.82760(15) 0.22149(11) 0.30019(12) 0.0236(8) Uani 1 1 d . . . H16 H 0.8573 0.2142 0.3438 0.028 Uiso 1 1 calc R . . C17 C 0.85766(15) 0.25133(12) 0.26604(13) 0.0238(8) Uani 1 1 d . . . C18 C 0.81179(15) 0.26178(12) 0.19979(12) 0.0247(8) Uani 1 1 d . . . H18 H 0.8309 0.2820 0.1756 0.030 Uiso 1 1 calc R . . C19 C 0.74066(17) 0.24262(11) 0.17148(12) 0.0264(9) Uani 1 1 d . . . C20 C 0.71260(17) 0.21309(11) 0.20682(12) 0.0269(9) Uani 1 1 d . . . C21 C 0.69161(16) 0.25641(12) 0.10195(12) 0.0264(9) Uani 1 1 d . . . H21A H 0.6451 0.2358 0.0880 0.032 Uiso 1 1 calc R . . H21B H 0.6782 0.2941 0.0997 0.032 Uiso 1 1 calc R . . C22 C 0.72557(17) 0.24645(11) 0.05519(12) 0.0259(9) Uani 1 1 d . . . C23 C 0.75048(18) 0.28918(13) 0.03107(14) 0.0328(10) Uani 1 1 d . . . H23 H 0.7475 0.3238 0.0453 0.039 Uiso 1 1 calc R . . C24 C 0.77910(19) 0.28166(13) -0.01285(15) 0.0386(11) Uani 1 1 d . . . C25 C 0.7837(2) 0.23173(13) -0.03275(14) 0.0395(11) Uani 1 1 d . . . H25 H 0.8048 0.2267 -0.0622 0.047 Uiso 1 1 calc R . . C26 C 0.75814(19) 0.18719(13) -0.01104(14) 0.0360(10) Uani 1 1 d . . . C27 C 0.73049(18) 0.19633(11) 0.03323(13) 0.0276(9) Uani 1 1 d . . . O28 O 0.70936(12) 0.15212(8) 0.05867(9) 0.0312(7) Uani 1 1 d . . . C29 C 0.62964(19) 0.14352(12) 0.03530(15) 0.0370(11) Uani 1 1 d . . . H29A H 0.6024 0.1721 0.0055 0.044 Uiso 1 1 calc R . . H29B H 0.6154 0.1440 0.0714 0.044 Uiso 1 1 calc R . . C30 C 0.60980(19) 0.09197(12) 0.00225(14) 0.0353(10) Uani 1 1 d . . . N31 N 0.57370(16) 0.08448(11) -0.06074(12) 0.0419(9) Uani 1 1 d . . . C32 C 0.55813(18) 0.03155(12) -0.07276(13) 0.0332(10) Uani 1 1 d . . . H32 H 0.5326 0.0151 -0.1130 0.040 Uiso 1 1 calc R . . C33 C 0.58737(16) 0.00764(13) -0.01416(13) 0.0272(9) Uani 1 1 d . . . H33 H 0.5863 -0.0291 -0.0069 0.033 Uiso 1 1 calc R . . N34 N 0.61879(13) 0.04571(10) 0.03295(11) 0.0283(7) Uani 1 1 d . . . N35 N 0.68714(12) -0.04803(9) 0.13691(9) 0.0212(7) Uani 1 1 d . . . C36 C 0.65571(15) -0.07543(11) 0.17113(12) 0.0226(8) Uani 1 1 d . . . H36 H 0.6226 -0.0611 0.1869 0.027 Uiso 1 1 calc R . . C37 C 0.67989(16) -0.12578(12) 0.17832(13) 0.0280(9) Uani 1 1 d . . . H37 H 0.6659 -0.1533 0.1988 0.034 Uiso 1 1 calc R . . N38 N 0.72767(13) -0.12973(9) 0.15104(10) 0.0240(7) Uani 1 1 d . . . C39 C 0.73185(16) -0.08195(12) 0.12597(12) 0.0262(9) Uani 1 1 d . . . C40 C 0.77593(16) -0.06912(11) 0.08950(12) 0.0254(8) Uani 1 1 d . . . H40A H 0.7887 -0.1019 0.0732 0.030 Uiso 1 1 calc R . . H40B H 0.7464 -0.0465 0.0527 0.030 Uiso 1 1 calc R . . O41 O 0.84358(11) -0.04179(8) 0.13104(9) 0.0294(6) Uani 1 1 d . . . C42 C 0.91226(15) -0.06609(12) 0.14415(12) 0.0284(8) Uani 1 1 d . . . C43 C 0.95063(16) -0.08794(12) 0.20184(13) 0.0286(9) Uani 1 1 d . . . C44 C 1.02107(16) -0.10950(14) 0.21513(13) 0.0344(10) Uani 1 1 d . . . H44 H 1.0485 -0.1257 0.2552 0.041 Uiso 1 1 calc R . . C45 C 1.05163(18) -0.10753(15) 0.17037(14) 0.0409(11) Uani 1 1 d . . . C46 C 1.00663(17) -0.08708(15) 0.11041(14) 0.0381(10) Uani 1 1 d . . . H46 H 1.0240 -0.0885 0.0780 0.046 Uiso 1 1 calc R . . C47 C 0.93805(18) -0.06487(14) 0.09627(14) 0.0365(10) Uani 1 1 d . . . C48 C 0.89199(19) -0.04192(13) 0.03090(14) 0.0356(10) Uani 1 1 d . . . H48A H 0.8395 -0.0523 0.0171 0.043 Uiso 1 1 calc R . . H48B H 0.9094 -0.0567 0.0001 0.043 Uiso 1 1 calc R . . C49 C 0.89712(15) 0.01764(13) 0.03050(14) 0.0332(9) Uani 1 1 d . . . C50 C 0.96346(18) 0.04418(13) 0.04963(14) 0.0333(7) Uani 1 1 d . . . H50 H 1.0084 0.0247 0.0680 0.040 Uiso 1 1 calc R . . C51 C 0.96716(17) 0.10045(16) 0.04286(17) 0.0505(11) Uani 1 1 d . . . C52 C 0.90378(18) 0.12706(14) 0.01966(15) 0.0452(10) Uani 1 1 d . . . H52 H 0.9055 0.1644 0.0182 0.054 Uiso 1 1 calc R . . C53 C 0.83234(18) 0.10160(13) -0.00350(12) 0.0315(9) Uani 1 1 d . . . C54 C 0.82947(16) 0.04800(13) 0.00103(12) 0.0290(9) Uani 1 1 d . . . C55 C 0.7595(2) 0.13220(12) -0.03598(13) 0.0379(11) Uani 1 1 d . . . H55A H 0.7474 0.1349 -0.0819 0.046 Uiso 1 1 calc R . . H55B H 0.7195 0.1114 -0.0320 0.046 Uiso 1 1 calc R . . C56 C 0.92053(17) -0.09360(13) 0.25154(12) 0.0299(9) Uani 1 1 d . . . H56A H 0.8658 -0.0956 0.2289 0.036 Uiso 1 1 calc R . . H56B H 0.9379 -0.1279 0.2730 0.036 Uiso 1 1 calc R . . C57 C 0.93909(17) -0.05208(15) 0.30260(13) 0.0360(10) Uani 1 1 d . . . C58 C 1.00954(15) -0.02831(12) 0.32793(13) 0.0272(8) Uani 1 1 d . . . H58 H 1.0432 -0.0353 0.3095 0.033 Uiso 1 1 calc R . . C59 C 1.03025(15) 0.00561(12) 0.38022(13) 0.0264(9) Uani 1 1 d . . . C60 C 0.97841(17) 0.01685(13) 0.40563(14) 0.0326(10) Uani 1 1 d . . . H60 H 0.9917 0.0403 0.4407 0.039 Uiso 1 1 calc R . . C61 C 0.90831(17) -0.00600(11) 0.37996(12) 0.0272(9) Uani 1 1 d . . . C62 C 0.88950(17) -0.04128(13) 0.32910(14) 0.0333(7) Uani 1 1 d . . . C63 C 0.57760(18) 0.07719(14) 0.30664(13) 0.0376(10) Uani 1 1 d . . . H63A H 0.5476 0.1079 0.3063 0.056 Uiso 1 1 calc R . . H63B H 0.6277 0.0812 0.3406 0.056 Uiso 1 1 calc R . . H63C H 0.5547 0.0453 0.3141 0.056 Uiso 1 1 calc R . . C64 C 0.5513(2) 0.12408(16) -0.11162(16) 0.0687(17) Uani 1 1 d . . . H64A H 0.5019 0.1376 -0.1197 0.103 Uiso 1 1 calc R . . H64B H 0.5498 0.1079 -0.1505 0.103 Uiso 1 1 calc R . . H64C H 0.5871 0.1531 -0.0986 0.103 Uiso 1 1 calc R . . C65 C 0.85639(17) 0.00406(12) 0.41067(13) 0.0280(9) Uani 1 1 d . . . H65A H 0.8098 -0.0155 0.3864 0.034 Uiso 1 1 calc R . . H65B H 0.8790 -0.0110 0.4541 0.034 Uiso 1 1 calc R . . C66 C 0.8672(2) 0.15818(13) 0.55041(13) 0.0387(11) Uani 1 1 d . . . C67 C 0.8358(3) 0.21386(15) 0.54968(16) 0.0723(16) Uani 1 1 d . . . H67A H 0.8597 0.2389 0.5319 0.108 Uiso 1 1 calc R . . H67B H 0.8458 0.2244 0.5932 0.108 Uiso 1 1 calc R . . H67C H 0.7821 0.2138 0.5234 0.108 Uiso 1 1 calc R . . C68 C 0.8349(2) 0.12171(14) 0.58595(13) 0.0424(11) Uani 1 1 d . . . H68A H 0.7810 0.1268 0.5689 0.064 Uiso 1 1 calc R . . H68B H 0.8576 0.1303 0.6314 0.064 Uiso 1 1 calc R . . H68C H 0.8455 0.0849 0.5801 0.064 Uiso 1 1 calc R . . C69 C 0.9522(2) 0.15997(17) 0.58525(15) 0.0577(14) Uani 1 1 d . . . H69A H 0.9723 0.1246 0.5864 0.087 Uiso 1 1 calc R . . H69B H 0.9668 0.1726 0.6288 0.087 Uiso 1 1 calc R . . H69C H 0.9717 0.1839 0.5628 0.087 Uiso 1 1 calc R . . N70 N 1.10140(15) 0.02652(12) 0.40867(14) 0.0451(9) Uani 1 1 d . . . H70A H 1.1342 0.0185 0.3938 0.054 Uiso 1 1 calc R . . H70B H 1.1137 0.0478 0.4415 0.054 Uiso 1 1 calc R . . C71 C 0.8006(2) 0.33039(14) -0.04200(16) 0.0541(13) Uani 1 1 d . . . C72 C 0.8536(3) 0.3661(2) 0.0124(3) 0.121(2) Uani 1 1 d . . . H72A H 0.8726 0.3465 0.0526 0.181 Uiso 1 1 calc R . . H72B H 0.8266 0.3973 0.0160 0.181 Uiso 1 1 calc R . . H72C H 0.8953 0.3770 0.0030 0.181 Uiso 1 1 calc R . . C73 C 0.8378(3) 0.3154(2) -0.0831(2) 0.0959(18) Uani 1 1 d . . . H73A H 0.8032 0.2952 -0.1197 0.144 Uiso 1 1 calc R . . H73B H 0.8814 0.2937 -0.0587 0.144 Uiso 1 1 calc R . . H73C H 0.8533 0.3472 -0.0981 0.144 Uiso 1 1 calc R . . C74 C 0.7291(3) 0.3621(2) -0.0807(3) 0.108(2) Uani 1 1 d . . . H74A H 0.7395 0.3888 -0.1064 0.162 Uiso 1 1 calc R . . H74B H 0.7120 0.3794 -0.0515 0.162 Uiso 1 1 calc R . . H74C H 0.6904 0.3382 -0.1087 0.162 Uiso 1 1 calc R . . C75 C 1.1282(2) -0.13162(19) 0.18268(15) 0.0545(13) Uani 1 1 d . . . C76 C 1.1160(2) -0.18052(16) 0.14256(18) 0.0649(14) Uani 1 1 d . . . H76A H 1.1618 -0.2014 0.1583 0.097 Uiso 1 1 calc R . . H76B H 1.1024 -0.1704 0.0982 0.097 Uiso 1 1 calc R . . H76C H 1.0760 -0.2015 0.1451 0.097 Uiso 1 1 calc R . . C77 C 1.1715(2) -0.1438(2) 0.25265(17) 0.0650(15) Uani 1 1 d . . . H77A H 1.1527 -0.1764 0.2631 0.097 Uiso 1 1 calc R . . H77B H 1.1658 -0.1147 0.2781 0.097 Uiso 1 1 calc R . . H77C H 1.2242 -0.1481 0.2621 0.097 Uiso 1 1 calc R . . C78 C 1.1719(2) -0.09129(18) 0.1675(2) 0.0602(15) Uani 1 1 d . . . H78A H 1.2220 -0.1047 0.1784 0.090 Uiso 1 1 calc R . . H78B H 1.1749 -0.0593 0.1921 0.090 Uiso 1 1 calc R . . H78C H 1.1477 -0.0831 0.1220 0.090 Uiso 1 1 calc R . . O79 O 0.82032(10) -0.06398(7) 0.30289(8) 0.0236(6) Uani 1 1 d . . . C80 C 0.81710(16) -0.11349(12) 0.33301(13) 0.0280(9) Uani 1 1 d . . . H80A H 0.8433 -0.1408 0.3206 0.042 Uiso 1 1 calc R . . H80B H 0.7651 -0.1239 0.3194 0.042 Uiso 1 1 calc R . . H80C H 0.8407 -0.1092 0.3793 0.042 Uiso 1 1 calc R . . C81 C 0.76838(18) -0.17754(13) 0.14785(15) 0.0369(11) Uani 1 1 d . . . H81A H 0.7567 -0.2065 0.1701 0.055 Uiso 1 1 calc R . . H81B H 0.8219 -0.1706 0.1681 0.055 Uiso 1 1 calc R . . H81C H 0.7536 -0.1873 0.1032 0.055 Uiso 1 1 calc R . . O82 O 0.64066(11) 0.19411(8) 0.17840(9) 0.0292(6) Uani 1 1 d . . . C83 C 0.58753(16) 0.22933(14) 0.18307(15) 0.0348(10) Uani 1 1 d . . . H83A H 0.5969 0.2335 0.2278 0.052 Uiso 1 1 calc R . . H83B H 0.5375 0.2151 0.1591 0.052 Uiso 1 1 calc R . . H83C H 0.5916 0.2637 0.1655 0.052 Uiso 1 1 calc R . . N84 N 0.93078(14) 0.27100(11) 0.29480(12) 0.0334(8) Uani 1 1 d . . . H84A H 0.9588 0.2646 0.3352 0.040 Uiso 1 1 calc R . . H84B H 0.9484 0.2897 0.2723 0.040 Uiso 1 1 calc R . . N86 N 1.03145(17) 0.12500(14) 0.05854(17) 0.0664(12) Uani 1 1 d . . . H86A H 1.0324 0.1593 0.0536 0.080 Uiso 1 1 calc R . . H86B H 1.0732 0.1070 0.0739 0.080 Uiso 1 1 calc R . . O87 O 0.76087(11) 0.02272(8) -0.01864(9) 0.0290(6) Uani 1 1 d . . . C88 C 0.7313(2) 0.00649(14) -0.08433(14) 0.0410(11) Uani 1 1 d . . . H88A H 0.7291 0.0369 -0.1111 0.061 Uiso 1 1 calc R . . H88B H 0.6812 -0.0078 -0.0971 0.061 Uiso 1 1 calc R . . H88C H 0.7634 -0.0207 -0.0895 0.061 Uiso 1 1 calc R . . N89 N 0.7785(2) 0.06070(14) 0.13820(14) 0.0620(13) Uani 1 1 d D . . H89A H 0.8006 0.0388 0.1197 0.074 Uiso 1 1 calc R . . H89B H 0.7710 0.0928 0.1180 0.074 Uiso 1 1 calc R . . C90 C 0.8274(3) 0.0676(3) 0.2036(3) 0.106(2) Uiso 1 1 d D . . H90A H 0.8425 0.0324 0.2230 0.128 Uiso 1 1 calc R . . H90B H 0.7994 0.0848 0.2250 0.128 Uiso 1 1 calc R . . C91 C 0.89800(15) 0.10008(11) 0.21774(14) 0.0831(11) Uiso 1 1 d GD . . C92 C 0.93979(18) 0.11185(16) 0.28159(14) 0.1227(17) Uiso 1 1 d G . . H92 H 0.9216 0.1029 0.3122 0.147 Uiso 1 1 calc R . . C93 C 1.00818(19) 0.13667(19) 0.30063(19) 0.104(2) Uiso 1 1 d G . . H93 H 1.0367 0.1447 0.3443 0.125 Uiso 1 1 calc R . . C94 C 1.03477(18) 0.14972(18) 0.2558(3) 0.133(3) Uiso 1 1 d G . . H94 H 1.0815 0.1667 0.2689 0.160 Uiso 1 1 calc R . . C95 C 0.9930(2) 0.13795(17) 0.1920(2) 0.0831(11) Uiso 1 1 d G . . H95 H 1.0112 0.1469 0.1614 0.100 Uiso 1 1 calc R . . C96 C 0.9246(2) 0.11313(15) 0.17294(16) 0.1227(17) Uiso 1 1 d G . . H96 H 0.8960 0.1051 0.1293 0.147 Uiso 1 1 calc R . . Cl1A Cl 0.56502(9) 0.82698(5) 1.01350(6) 0.1736(6) Uani 1 1 d D . . O1A O 0.5581(3) 0.79970(17) 1.06414(14) 0.627(11) Uani 1 1 d D . . O2A O 0.55008(16) 0.87923(10) 1.01426(12) 0.0603(10) Uani 1 1 d D . . O3A O 0.51452(19) 0.80211(14) 0.95613(15) 0.1134(14) Uani 1 1 d D . . O4A O 0.6472(4) 0.8168(3) 1.0294(3) 0.428(6) Uani 1 1 d D . . Cl1B Cl 0.42762(5) 0.08097(3) 0.70098(4) 0.0461(3) Uani 1 1 d . . . O1B O 0.45576(16) 0.04611(11) 0.75573(11) 0.0597(9) Uani 1 1 d . . . O2B O 0.4424(5) 0.13007(15) 0.7198(2) 0.215(4) Uani 1 1 d . . . O3B O 0.4532(3) 0.0640(2) 0.65813(18) 0.169(2) Uani 1 1 d . . . O4B O 0.3517(3) 0.0767(3) 0.6698(3) 0.200(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.03600(16) 0.01975(16) 0.01661(13) 0.00084(13) 0.00798(11) 0.00050(15) N1 0.0510(13) 0.0155(12) 0.0108(9) -0.0037(9) 0.0112(9) -0.0040(11) C2 0.0187(12) 0.0282(15) 0.0117(11) 0.0007(11) -0.0004(10) 0.0067(12) C3 0.0254(14) 0.0244(16) 0.0301(15) 0.0006(13) 0.0021(12) 0.0042(13) N4 0.0405(13) 0.0222(13) 0.0139(10) 0.0023(10) 0.0010(10) 0.0015(11) C5 0.0324(13) 0.0163(13) 0.0092(10) -0.0066(10) 0.0055(9) -0.0046(12) C6 0.0224(12) 0.0265(15) 0.0118(11) 0.0003(11) 0.0008(10) -0.0019(12) O7 0.0359(9) 0.0409(12) 0.0020(7) -0.0028(8) 0.0057(6) -0.0106(9) C8 0.0255(12) 0.0279(15) 0.0050(10) -0.0059(10) 0.0049(9) -0.0058(12) C9 0.0309(13) 0.0224(14) 0.0048(10) 0.0030(10) 0.0022(9) -0.0020(12) C10 0.0232(13) 0.0283(15) 0.0088(11) 0.0042(11) -0.0016(10) 0.0000(12) C11 0.0365(14) 0.0294(16) 0.0043(10) -0.0039(11) 0.0019(10) -0.0077(13) C12 0.0450(14) 0.0161(14) 0.0131(10) -0.0012(10) 0.0150(10) 0.0012(12) C13 0.0222(13) 0.0285(15) 0.0068(10) 0.0029(11) -0.0001(9) -0.0043(12) C14 0.0174(12) 0.0249(15) 0.0238(13) 0.0018(12) 0.0027(10) 0.0031(12) C15 0.0370(14) 0.0238(15) 0.0080(10) 0.0030(10) 0.0096(9) 0.0084(12) C16 0.0279(14) 0.0248(15) 0.0068(11) 0.0005(11) -0.0037(10) 0.0098(12) C17 0.0178(12) 0.0314(16) 0.0172(12) 0.0017(12) 0.0024(10) 0.0020(12) C18 0.0280(13) 0.0296(16) 0.0140(11) 0.0026(11) 0.0064(10) 0.0013(12) C19 0.0460(16) 0.0144(13) 0.0106(11) 0.0012(11) 0.0040(11) 0.0057(13) C20 0.0394(16) 0.0197(14) 0.0060(11) -0.0077(11) -0.0056(11) 0.0064(13) C21 0.0340(15) 0.0242(15) 0.0102(11) 0.0025(11) -0.0013(11) -0.0036(13) C22 0.0435(16) 0.0167(14) 0.0076(11) 0.0065(10) 0.0013(11) 0.0023(13) C23 0.0443(16) 0.0236(16) 0.0236(13) 0.0052(12) 0.0075(12) 0.0010(14) C24 0.0611(18) 0.0261(17) 0.0282(14) 0.0013(13) 0.0186(13) 0.0004(15) C25 0.0706(19) 0.0260(17) 0.0241(13) 0.0051(12) 0.0221(12) -0.0030(15) C26 0.0563(19) 0.0280(17) 0.0126(12) -0.0027(12) 0.0039(13) 0.0022(15) C27 0.0478(16) 0.0117(14) 0.0125(12) 0.0021(11) 0.0022(11) -0.0047(13) O28 0.0445(11) 0.0162(10) 0.0172(9) 0.0103(8) -0.0024(8) -0.0043(9) C29 0.0457(18) 0.0214(16) 0.0261(15) 0.0016(13) -0.0022(14) 0.0013(15) C30 0.0583(18) 0.0227(15) 0.0139(12) -0.0037(12) 0.0047(12) -0.0181(14) N31 0.0592(16) 0.0296(14) 0.0189(12) 0.0114(11) -0.0011(12) -0.0130(13) C32 0.0533(18) 0.0247(16) 0.0111(12) -0.0011(12) 0.0033(12) -0.0067(15) C33 0.0317(13) 0.0273(15) 0.0227(12) -0.0106(12) 0.0117(10) -0.0068(13) N34 0.0430(12) 0.0202(12) 0.0257(10) -0.0019(10) 0.0184(9) 0.0019(10) N35 0.0309(11) 0.0214(12) 0.0047(9) -0.0004(8) 0.0012(8) 0.0001(10) C36 0.0280(12) 0.0262(15) 0.0177(11) -0.0077(11) 0.0135(9) -0.0037(12) C37 0.0393(15) 0.0271(16) 0.0131(11) 0.0053(11) 0.0066(10) -0.0058(13) N38 0.0330(12) 0.0168(12) 0.0132(10) 0.0105(9) 0.0009(9) 0.0010(10) C39 0.0411(15) 0.0259(15) 0.0068(10) -0.0083(11) 0.0055(10) -0.0001(13) C40 0.0453(15) 0.0143(14) 0.0176(11) -0.0055(10) 0.0144(10) -0.0002(12) O41 0.0380(10) 0.0276(11) 0.0243(8) -0.0095(8) 0.0147(7) 0.0012(9) C42 0.0394(12) 0.0319(16) 0.0280(11) -0.0063(11) 0.0281(9) -0.0053(12) C43 0.0438(14) 0.0254(15) 0.0218(11) -0.0103(11) 0.0187(10) -0.0025(13) C44 0.0343(14) 0.055(2) 0.0148(12) -0.0015(13) 0.0112(10) -0.0027(15) C45 0.0525(17) 0.052(2) 0.0228(13) -0.0048(14) 0.0200(11) 0.0075(16) C46 0.0401(14) 0.061(2) 0.0177(12) 0.0031(13) 0.0165(10) 0.0192(15) C47 0.0470(17) 0.0416(19) 0.0176(12) -0.0105(13) 0.0104(11) -0.0027(15) C48 0.0548(17) 0.0325(17) 0.0196(12) 0.0016(12) 0.0159(11) 0.0128(14) C49 0.0446(13) 0.0292(17) 0.0461(13) -0.0001(12) 0.0389(9) 0.0029(12) C50 0.0461(11) 0.0317(12) 0.0257(9) 0.0044(9) 0.0187(8) 0.0069(10) C51 0.0440(14) 0.055(2) 0.0744(17) -0.0302(16) 0.0463(11) -0.0184(15) C52 0.0770(17) 0.0284(17) 0.0554(14) -0.0127(13) 0.0524(11) -0.0076(15) C53 0.0524(17) 0.0333(17) 0.0048(10) 0.0037(11) 0.0084(11) 0.0047(14) C54 0.0399(14) 0.0405(18) 0.0093(10) -0.0015(11) 0.0131(9) 0.0000(14) C55 0.069(2) 0.0232(15) 0.0042(11) -0.0044(11) -0.0020(13) 0.0162(15) C56 0.0425(15) 0.0367(17) 0.0114(11) -0.0009(12) 0.0124(10) 0.0028(14) C57 0.0298(14) 0.061(2) 0.0153(12) 0.0034(14) 0.0074(11) -0.0029(15) C58 0.0233(12) 0.0350(17) 0.0263(12) -0.0082(12) 0.0134(9) -0.0002(13) C59 0.0264(12) 0.0304(16) 0.0244(12) 0.0010(12) 0.0128(10) 0.0043(12) C60 0.0379(16) 0.0327(17) 0.0194(13) -0.0045(13) 0.0045(12) -0.0048(14) C61 0.0458(15) 0.0202(14) 0.0125(11) 0.0039(11) 0.0094(10) 0.0140(13) C62 0.0461(11) 0.0317(12) 0.0257(9) 0.0044(9) 0.0187(8) 0.0069(10) C63 0.0585(17) 0.0419(19) 0.0186(12) -0.0056(12) 0.0223(11) 0.0009(15) C64 0.100(3) 0.051(2) 0.0162(16) 0.0103(16) -0.013(2) -0.020(2) C65 0.0427(15) 0.0233(15) 0.0148(12) 0.0039(11) 0.0090(11) 0.0106(13) C66 0.072(2) 0.0255(16) 0.0138(12) -0.0041(12) 0.0132(13) -0.0010(16) C67 0.162(4) 0.031(2) 0.0258(14) -0.0078(14) 0.0419(17) 0.007(2) C68 0.081(2) 0.0359(18) 0.0116(11) -0.0105(12) 0.0202(12) -0.0067(17) C69 0.087(2) 0.067(2) 0.0093(13) -0.0097(15) 0.0115(15) -0.028(2) N70 0.0368(13) 0.0593(19) 0.0376(13) -0.0173(13) 0.0140(10) -0.0152(14) C71 0.101(3) 0.0282(18) 0.0360(16) 0.0045(14) 0.0318(16) 0.0053(19) C72 0.216(4) 0.067(3) 0.096(3) -0.021(2) 0.082(3) -0.086(3) C73 0.168(3) 0.052(3) 0.114(3) 0.010(2) 0.105(2) -0.007(3) C74 0.149(4) 0.080(3) 0.114(3) 0.065(2) 0.073(3) 0.030(3) C75 0.0514(17) 0.096(3) 0.0196(13) 0.0102(17) 0.0188(12) 0.023(2) C76 0.100(2) 0.060(2) 0.0451(17) 0.0259(17) 0.0399(16) 0.043(2) C77 0.0459(18) 0.113(3) 0.0300(17) 0.021(2) 0.0107(14) 0.038(2) C78 0.0414(19) 0.076(3) 0.054(2) -0.001(2) 0.0106(17) 0.017(2) O79 0.0353(9) 0.0194(10) 0.0177(8) 0.0052(7) 0.0127(7) 0.0027(8) C80 0.0394(14) 0.0222(15) 0.0259(12) 0.0013(11) 0.0174(10) -0.0034(13) C81 0.0383(17) 0.0311(17) 0.0221(15) 0.0120(13) -0.0060(13) 0.0092(15) O82 0.0349(10) 0.0245(11) 0.0130(9) -0.0006(8) -0.0048(8) -0.0075(9) C83 0.0205(14) 0.052(2) 0.0220(14) -0.0006(14) -0.0006(11) -0.0087(14) N84 0.0296(12) 0.0386(15) 0.0226(12) 0.0039(11) 0.0020(10) -0.0010(12) N86 0.0626(15) 0.051(2) 0.103(2) -0.0228(17) 0.0525(13) -0.0126(16) O87 0.0365(10) 0.0262(11) 0.0181(9) 0.0047(8) 0.0054(8) 0.0024(9) C88 0.0609(19) 0.0378(19) 0.0230(13) -0.0075(13) 0.0165(13) -0.0086(16) N89 0.076(2) 0.0498(19) 0.0306(16) 0.0065(15) -0.0064(16) 0.0070(18) Cl1A 0.1601(10) 0.1098(7) 0.0909(7) -0.0803(5) -0.1025(8) 0.1040(6) O1A 0.438(9) 0.042(2) 0.066(3) -0.0046(19) 0.010(4) 0.042(4) O2A 0.0758(17) 0.0482(15) 0.0358(13) -0.0009(12) 0.0031(13) 0.0076(14) O3A 0.086(2) 0.102(2) 0.0661(19) -0.0529(16) -0.0521(18) 0.0439(18) O4A 0.470(13) 0.389(7) 0.167(4) -0.205(4) -0.117(7) 0.181(8) Cl1B 0.0732(4) 0.0368(5) 0.0404(3) -0.0073(3) 0.0360(3) -0.0082(4) O1B 0.0994(16) 0.0490(15) 0.0375(11) 0.0045(11) 0.0355(10) -0.0021(14) O2B 0.438(9) 0.042(2) 0.066(3) -0.0046(19) 0.010(4) 0.042(4) O3B 0.241(3) 0.223(5) 0.0878(18) 0.053(3) 0.1117(17) 0.099(3) O4B 0.110(3) 0.289(5) 0.186(3) 0.146(3) 0.048(2) -0.025(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N34 1.991(2) . ? Zn1 N1 1.995(3) . ? Zn1 N35 2.000(2) . ? Zn1 N89 2.020(4) . ? N1 C5 1.317(4) . ? N1 C2 1.368(4) . ? C2 C3 1.363(5) . ? C2 H2 0.9500 . ? C3 N4 1.372(3) . ? C3 H3 0.9500 . ? N4 C5 1.315(4) . ? N4 C63 1.472(4) . ? C5 C6 1.532(3) . ? C6 O7 1.427(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O7 C8 1.404(3) . ? C8 C13 1.377(4) . ? C8 C9 1.413(3) . ? C9 C10 1.406(4) . ? C9 C65 1.494(4) . ? C10 C11 1.399(4) . ? C10 H10 0.9500 . ? C11 C12 1.409(4) . ? C11 C66 1.533(4) . ? C12 C13 1.400(4) . ? C12 H12 0.9500 . ? C13 C14 1.513(4) . ? C14 C15 1.521(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.361(4) . ? C15 C20 1.426(3) . ? C16 C17 1.399(5) . ? C16 H16 0.9500 . ? C17 N84 1.410(4) . ? C17 C18 1.442(4) . ? C18 C19 1.372(4) . ? C18 H18 0.9500 . ? C19 C20 1.389(5) . ? C19 C21 1.531(3) . ? C20 O82 1.384(4) . ? C21 C22 1.521(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.389(4) . ? C22 C23 1.403(5) . ? C23 C24 1.373(6) . ? C23 H23 0.9500 . ? C24 C25 1.365(5) . ? C24 C71 1.554(5) . ? C25 C26 1.416(5) . ? C25 H25 0.9500 . ? C26 C27 1.374(5) . ? C26 C55 1.515(4) . ? C27 O28 1.412(4) . ? O28 C29 1.458(4) . ? C29 C30 1.483(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 N34 1.345(4) . ? C30 N31 1.341(4) . ? N31 C32 1.380(4) . ? N31 C64 1.469(5) . ? C32 C33 1.373(4) . ? C32 H32 0.9500 . ? C33 N34 1.393(4) . ? C33 H33 0.9500 . ? N35 C39 1.336(4) . ? N35 C36 1.386(4) . ? C36 C37 1.351(4) . ? C36 H36 0.9500 . ? C37 N38 1.349(5) . ? C37 H37 0.9500 . ? N38 C39 1.362(4) . ? N38 C81 1.478(4) . ? C39 C40 1.488(5) . ? C40 O41 1.457(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? O41 C42 1.409(4) . ? C42 C43 1.348(4) . ? C42 C47 1.406(5) . ? C43 C44 1.411(5) . ? C43 C56 1.513(5) . ? C44 C45 1.407(5) . ? C44 H44 0.9500 . ? C45 C46 1.397(4) . ? C45 C75 1.551(5) . ? C46 C47 1.380(5) . ? C46 H46 0.9500 . ? C47 C48 1.517(4) . ? C48 C49 1.515(5) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.376(4) . ? C49 C54 1.446(4) . ? C50 C51 1.442(5) . ? C50 H50 0.9500 . ? C51 C52 1.326(5) . ? C51 N86 1.327(5) . ? C52 C53 1.441(5) . ? C52 H52 0.9500 . ? C53 C54 1.367(5) . ? C53 C55 1.532(5) . ? C54 O87 1.398(4) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.510(5) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C62 1.391(5) . ? C57 C58 1.405(4) . ? C58 C59 1.400(4) . ? C58 H58 0.9500 . ? C59 N70 1.389(4) . ? C59 C60 1.415(5) . ? C60 C61 1.389(4) . ? C60 H60 0.9500 . ? C61 C62 1.400(4) . ? C61 C65 1.503(5) . ? C62 O79 1.373(4) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C69 1.535(5) . ? C66 C67 1.542(5) . ? C66 C68 1.548(5) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? N70 H70A 0.8800 . ? N70 H70B 0.8800 . ? C71 C73 1.481(8) . ? C71 C72 1.548(6) . ? C71 C74 1.548(7) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C78 1.478(7) . ? C75 C77 1.513(5) . ? C75 C76 1.508(6) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? O79 C80 1.452(4) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? O82 C83 1.422(4) . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? N84 H84A 0.8800 . ? N84 H84B 0.8800 . ? N86 H86A 0.8800 . ? N86 H86B 0.8800 . ? O87 C88 1.442(4) . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? N89 C90 1.425(6) . ? N89 H89A 0.9200 . ? N89 H89B 0.9200 . ? C90 C91 1.538(7) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 C92 1.3900 . ? C91 C96 1.3900 . ? C92 C93 1.3900 . ? C92 H92 0.9500 . ? C93 C94 1.3900 . ? C93 H93 0.9500 . ? C94 C95 1.3900 . ? C94 H94 0.9500 . ? C95 C96 1.3900 . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? Cl1A O2A 1.361(3) . ? Cl1A O3A 1.431(3) . ? Cl1A O1A 1.420(5) . ? Cl1A O4A 1.536(8) . ? Cl1B O2B 1.312(4) . ? Cl1B O3B 1.364(5) . ? Cl1B O4B 1.374(5) . ? Cl1B O1B 1.452(3) . ? 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 N34 Zn1 N1 107.40(10) . . ? N34 Zn1 N35 108.95(9) . . ? N1 Zn1 N35 106.38(10) . . ? N34 Zn1 N89 101.36(12) . . ? N1 Zn1 N89 122.00(12) . . ? N35 Zn1 N89 110.17(12) . . ? C5 N1 C2 105.1(3) . . ? C5 N1 Zn1 131.8(2) . . ? C2 N1 Zn1 123.00(19) . . ? C3 C2 N1 108.9(2) . . ? C3 C2 H2 125.5 . . ? N1 C2 H2 125.5 . . ? C2 C3 N4 106.4(3) . . ? C2 C3 H3 126.8 . . ? N4 C3 H3 126.8 . . ? C5 N4 C3 106.5(3) . . ? C5 N4 C63 128.3(2) . . ? C3 N4 C63 125.2(3) . . ? N4 C5 N1 113.0(2) . . ? N4 C5 C6 124.1(3) . . ? N1 C5 C6 122.9(3) . . ? O7 C6 C5 111.0(2) . . ? O7 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? O7 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C8 O7 C6 117.4(2) . . ? C13 C8 O7 119.4(2) . . ? C13 C8 C9 122.9(2) . . ? O7 C8 C9 117.7(2) . . ? C10 C9 C8 116.7(3) . . ? C10 C9 C65 120.2(2) . . ? C8 C9 C65 123.1(2) . . ? C11 C10 C9 122.5(2) . . ? C11 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C10 C11 C12 118.0(2) . . ? C10 C11 C66 118.5(2) . . ? C12 C11 C66 123.6(3) . . ? C13 C12 C11 121.3(3) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C8 C13 C12 118.6(2) . . ? C8 C13 C14 122.0(2) . . ? C12 C13 C14 119.2(3) . . ? C13 C14 C15 116.8(2) . . ? C13 C14 H14A 108.1 . . ? C15 C14 H14A 108.1 . . ? C13 C14 H14B 108.1 . . ? C15 C14 H14B 108.1 . . ? H14A C14 H14B 107.3 . . ? C16 C15 C20 119.2(3) . . ? C16 C15 C14 122.6(2) . . ? C20 C15 C14 118.1(2) . . ? C15 C16 C17 121.7(2) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C16 C17 N84 121.7(2) . . ? C16 C17 C18 118.3(2) . . ? N84 C17 C18 120.0(3) . . ? C19 C18 C17 120.3(3) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 119.9(2) . . ? C18 C19 C21 119.5(3) . . ? C20 C19 C21 120.6(3) . . ? O82 C20 C19 119.9(2) . . ? O82 C20 C15 119.5(3) . . ? C19 C20 C15 120.6(3) . . ? C22 C21 C19 115.8(3) . . ? C22 C21 H21A 108.3 . . ? C19 C21 H21A 108.3 . . ? C22 C21 H21B 108.3 . . ? C19 C21 H21B 108.3 . . ? H21A C21 H21B 107.4 . . ? C27 C22 C23 118.1(3) . . ? C27 C22 C21 122.3(3) . . ? C23 C22 C21 119.6(3) . . ? C24 C23 C22 121.0(3) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C25 C24 C23 119.2(3) . . ? C25 C24 C71 121.5(4) . . ? C23 C24 C71 119.2(3) . . ? C24 C25 C26 122.4(4) . . ? C24 C25 H25 118.8 . . ? C26 C25 H25 118.8 . . ? C27 C26 C25 116.6(3) . . ? C27 C26 C55 121.2(3) . . ? C25 C26 C55 122.2(3) . . ? C26 C27 C22 122.8(3) . . ? C26 C27 O28 117.5(3) . . ? C22 C27 O28 119.7(3) . . ? C27 O28 C29 115.6(2) . . ? O28 C29 C30 109.5(3) . . ? O28 C29 H29A 109.8 . . ? C30 C29 H29A 109.8 . . ? O28 C29 H29B 109.8 . . ? C30 C29 H29B 109.8 . . ? H29A C29 H29B 108.2 . . ? N34 C30 N31 110.1(3) . . ? N34 C30 C29 123.3(3) . . ? N31 C30 C29 126.2(3) . . ? C30 N31 C32 109.2(3) . . ? C30 N31 C64 128.2(3) . . ? C32 N31 C64 122.5(3) . . ? C33 C32 N31 105.4(2) . . ? C33 C32 H32 127.3 . . ? N31 C32 H32 127.3 . . ? C32 C33 N34 109.4(3) . . ? C32 C33 H33 125.3 . . ? N34 C33 H33 125.3 . . ? C30 N34 C33 106.0(2) . . ? C30 N34 Zn1 128.64(19) . . ? C33 N34 Zn1 124.61(19) . . ? C39 N35 C36 106.4(2) . . ? C39 N35 Zn1 129.2(2) . . ? C36 N35 Zn1 123.4(2) . . ? C37 C36 N35 108.8(3) . . ? C37 C36 H36 125.6 . . ? N35 C36 H36 125.6 . . ? N38 C37 C36 107.3(3) . . ? N38 C37 H37 126.4 . . ? C36 C37 H37 126.4 . . ? C37 N38 C39 108.4(3) . . ? C37 N38 C81 126.4(3) . . ? C39 N38 C81 125.2(3) . . ? N35 C39 N38 109.1(3) . . ? N35 C39 C40 124.4(3) . . ? N38 C39 C40 126.4(3) . . ? O41 C40 C39 109.2(2) . . ? O41 C40 H40A 109.8 . . ? C39 C40 H40A 109.8 . . ? O41 C40 H40B 109.8 . . ? C39 C40 H40B 109.8 . . ? H40A C40 H40B 108.3 . . ? C42 O41 C40 118.3(2) . . ? C43 C42 C47 123.4(3) . . ? C43 C42 O41 119.0(3) . . ? C47 C42 O41 117.6(2) . . ? C42 C43 C44 118.0(3) . . ? C42 C43 C56 123.7(3) . . ? C44 C43 C56 118.2(2) . . ? C45 C44 C43 121.5(3) . . ? C45 C44 H44 119.2 . . ? C43 C44 H44 119.2 . . ? C46 C45 C44 116.9(3) . . ? C46 C45 C75 119.7(3) . . ? C44 C45 C75 123.1(3) . . ? C47 C46 C45 122.7(3) . . ? C47 C46 H46 118.6 . . ? C45 C46 H46 118.6 . . ? C46 C47 C42 117.1(3) . . ? C46 C47 C48 120.8(3) . . ? C42 C47 C48 122.0(3) . . ? C47 C48 C49 112.0(2) . . ? C47 C48 H48A 109.2 . . ? C49 C48 H48A 109.2 . . ? C47 C48 H48B 109.2 . . ? C49 C48 H48B 109.2 . . ? H48A C48 H48B 107.9 . . ? C50 C49 C54 117.6(3) . . ? C50 C49 C48 123.0(3) . . ? C54 C49 C48 118.9(3) . . ? C49 C50 C51 122.4(3) . . ? C49 C50 H50 118.8 . . ? C51 C50 H50 118.8 . . ? C52 C51 N86 120.8(4) . . ? C52 C51 C50 117.7(3) . . ? N86 C51 C50 121.5(3) . . ? C51 C52 C53 122.7(3) . . ? C51 C52 H52 118.7 . . ? C53 C52 H52 118.7 . . ? C54 C53 C52 118.9(3) . . ? C54 C53 C55 118.7(3) . . ? C52 C53 C55 122.3(3) . . ? C53 C54 O87 119.9(3) . . ? C53 C54 C49 120.4(3) . . ? O87 C54 C49 119.6(3) . . ? C26 C55 C53 116.4(2) . . ? C26 C55 H55A 108.2 . . ? C53 C55 H55A 108.2 . . ? C26 C55 H55B 108.2 . . ? C53 C55 H55B 108.2 . . ? H55A C55 H55B 107.3 . . ? C57 C56 C43 119.1(3) . . ? C57 C56 H56A 107.5 . . ? C43 C56 H56A 107.5 . . ? C57 C56 H56B 107.5 . . ? C43 C56 H56B 107.5 . . ? H56A C56 H56B 107.0 . . ? C62 C57 C58 119.8(3) . . ? C62 C57 C56 120.0(3) . . ? C58 C57 C56 119.8(3) . . ? C59 C58 C57 120.2(3) . . ? C59 C58 H58 119.9 . . ? C57 C58 H58 119.9 . . ? N70 C59 C58 121.0(3) . . ? N70 C59 C60 120.0(3) . . ? C58 C59 C60 119.0(3) . . ? C61 C60 C59 120.8(3) . . ? C61 C60 H60 119.6 . . ? C59 C60 H60 119.6 . . ? C60 C61 C62 119.4(3) . . ? C60 C61 C65 119.4(3) . . ? C62 C61 C65 121.0(3) . . ? O79 C62 C57 119.0(3) . . ? O79 C62 C61 120.1(3) . . ? C57 C62 C61 120.7(3) . . ? N4 C63 H63A 109.5 . . ? N4 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N4 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N31 C64 H64A 109.5 . . ? N31 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? N31 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C9 C65 C61 116.9(3) . . ? C9 C65 H65A 108.1 . . ? C61 C65 H65A 108.1 . . ? C9 C65 H65B 108.1 . . ? C61 C65 H65B 108.1 . . ? H65A C65 H65B 107.3 . . ? C11 C66 C69 111.1(3) . . ? C11 C66 C67 111.3(2) . . ? C69 C66 C67 109.2(3) . . ? C11 C66 C68 107.4(3) . . ? C69 C66 C68 110.5(3) . . ? C67 C66 C68 107.3(3) . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C66 C68 H68A 109.5 . . ? C66 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C66 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C66 C69 H69A 109.5 . . ? C66 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C66 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C59 N70 H70A 120.0 . . ? C59 N70 H70B 120.0 . . ? H70A N70 H70B 120.0 . . ? C73 C71 C72 108.8(4) . . ? C73 C71 C74 110.3(4) . . ? C72 C71 C74 108.1(4) . . ? C73 C71 C24 112.2(3) . . ? C72 C71 C24 109.2(3) . . ? C74 C71 C24 108.2(4) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C71 C73 H73A 109.5 . . ? C71 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C71 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C71 C74 H74A 109.5 . . ? C71 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C71 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C78 C75 C77 105.7(3) . . ? C78 C75 C76 112.4(4) . . ? C77 C75 C76 111.3(4) . . ? C78 C75 C45 108.2(4) . . ? C77 C75 C45 110.3(3) . . ? C76 C75 C45 108.8(3) . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C75 C77 H77A 109.5 . . ? C75 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C75 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C75 C78 H78A 109.5 . . ? C75 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C75 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C62 O79 C80 112.9(2) . . ? O79 C80 H80A 109.5 . . ? O79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? O79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? N38 C81 H81A 109.5 . . ? N38 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? N38 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C20 O82 C83 113.3(2) . . ? O82 C83 H83A 109.5 . . ? O82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? O82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C17 N84 H84A 120.0 . . ? C17 N84 H84B 120.0 . . ? H84A N84 H84B 120.0 . . ? C51 N86 H86A 120.0 . . ? C51 N86 H86B 120.0 . . ? H86A N86 H86B 120.0 . . ? C54 O87 C88 112.5(3) . . ? O87 C88 H88A 109.5 . . ? O87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? O87 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C90 N89 Zn1 113.3(4) . . ? C90 N89 H89A 108.9 . . ? Zn1 N89 H89A 108.9 . . ? C90 N89 H89B 108.9 . . ? Zn1 N89 H89B 108.9 . . ? H89A N89 H89B 107.7 . . ? N89 C90 C91 116.4(5) . . ? N89 C90 H90A 108.2 . . ? C91 C90 H90A 108.2 . . ? N89 C90 H90B 108.2 . . ? C91 C90 H90B 108.2 . . ? H90A C90 H90B 107.3 . . ? C92 C91 C96 120.0 . . ? C92 C91 C90 115.0(3) . . ? C96 C91 C90 124.7(3) . . ? C91 C92 C93 120.0 . . ? C91 C92 H92 120.0 . . ? C93 C92 H92 120.0 . . ? C94 C93 C92 120.0 . . ? C94 C93 H93 120.0 . . ? C92 C93 H93 120.0 . . ? C93 C94 C95 120.0 . . ? C93 C94 H94 120.0 . . ? C95 C94 H94 120.0 . . ? C96 C95 C94 120.0 . . ? C96 C95 H95 120.0 . . ? C94 C95 H95 120.0 . . ? C95 C96 C91 120.0 . . ? C95 C96 H96 120.0 . . ? C91 C96 H96 120.0 . . ? O2A Cl1A O3A 111.77(19) . . ? O2A Cl1A O1A 111.5(3) . . ? O3A Cl1A O1A 106.2(3) . . ? O2A Cl1A O4A 112.2(4) . . ? O3A Cl1A O4A 113.9(3) . . ? O1A Cl1A O4A 100.6(4) . . ? O2B Cl1B O3B 116.3(5) . . ? O2B Cl1B O4B 106.9(5) . . ? O3B Cl1B O4B 104.9(3) . . ? O2B Cl1B O1B 109.8(2) . . ? O3B Cl1B O1B 108.6(3) . . ? O4B Cl1B O1B 110.1(3) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.701 _refine_diff_density_min -1.064 _refine_diff_density_rms 0.173 #===END