# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dolphin, David' _publ_contact_author_email david.dolphin@ubc.ca _publ_section_title ; Self-assembly of [2x2] grids and a hexagon using bis(dipyrrin)s ; loop_ _publ_author_name L.Ma B.Patrick D.Dolphin # Attachment '- grid 9 & hexagon 11 revised.cif' data_grid_9 _database_code_depnum_ccdc_archive 'CCDC 791800' #TrackingRef '- grid 9 & hexagon 11 revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C206 H254 N16 Zn4' _chemical_formula_weight 3215.73 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' 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 'P 2/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 24.936(3) _cell_length_b 12.9012(17) _cell_length_c 28.201(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.206(6) _cell_angle_gamma 90.00 _cell_volume 9035(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9851 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.45 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3444 _exptl_absorpt_coefficient_mu 0.582 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.682 _exptl_absorpt_correction_T_max 0.792 _exptl_absorpt_process_details 'SADABS (Bruker-AXS, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21591 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.93 _reflns_number_total 21591 _reflns_number_gt 12724 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SAINT (Bruker-AXS, 2008)' _computing_cell_refinement 'SAINT (Bruker-AXS, 2008)' _computing_data_reduction 'APEX2 (Bruker-AXS, 2008)' _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WINGX (Farrugia, 1999)' _refine_special_details ; The material crystallizes with one half-molecule related to another by rotation about a two-fold axis. Additionally, the material crystallizes with 2.5 molecules of n-hexane in the asymmetric unit. Two of these hexane molecules were successfully modeled (albeit, with some disorder in one molecule), a third, however, residing in a channel produced by adjacent Zn4 complexes, could not be modeled properly. The PLATON/SQUEEZE program was used to produce a solvent-free data set (at least solvent-free at the site mentioned above). DFIX and SADI constraints were used to maintain reasonable geometries for the remaining disordered solvent fragments. The final formula includes the missing hexane molecule. Finally, one ethyl substituent was also disordered and was modeled in two orientations. All non-hydrogen atoms except some of those in the disordered n-hexane were refined anisotropically. All hydrogen atoms were placed in calculated positions but were not refined. 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^ > 2\s(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^)+(0.0985P)^2^+0.5944P] 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 21591 _refine_ls_number_parameters 1020 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.1061 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1849 _refine_ls_wR_factor_gt 0.1615 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.059 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.17161(11) 0.2328(2) 0.56954(10) 0.0393(7) Uani 1 1 d . . . C2 C 0.15642(13) 0.3286(3) 0.58992(11) 0.0481(8) Uani 1 1 d . . . C3 C 0.17170(12) 0.4049(2) 0.56075(11) 0.0457(7) Uani 1 1 d . . . C4 C 0.19805(12) 0.3557(2) 0.52380(10) 0.0386(7) Uani 1 1 d . . . C5 C 0.22475(12) 0.4056(2) 0.48874(10) 0.0418(7) Uani 1 1 d . . . H5 H 0.2197 0.4785 0.4869 0.050 Uiso 1 1 calc R . . C6 C 0.25767(12) 0.3644(2) 0.45618(10) 0.0382(7) Uani 1 1 d . . . C7 C 0.28487(12) 0.4198(2) 0.42188(10) 0.0427(7) Uani 1 1 d . . . C8 C 0.31409(12) 0.3469(2) 0.39914(10) 0.0373(7) Uani 1 1 d . . . C9 C 0.30375(11) 0.2499(2) 0.42010(9) 0.0319(6) Uani 1 1 d . . . C10 C 0.32837(12) 0.1508(2) 0.40595(10) 0.0368(6) Uani 1 1 d . . . H10A H 0.3045 0.0923 0.4127 0.044 Uiso 1 1 calc R . . H10B H 0.3633 0.1406 0.4250 0.044 Uiso 1 1 calc R . . C11 C 0.33714(12) 0.15126(19) 0.35269(10) 0.0350(6) Uani 1 1 d . . . H11A H 0.3617 0.0939 0.3458 0.042 Uiso 1 1 calc R . . H11B H 0.3023 0.1399 0.3336 0.042 Uiso 1 1 calc R . . C12 C 0.36064(10) 0.25158(19) 0.33882(9) 0.0296(6) Uani 1 1 d . . . C13 C 0.34919(12) 0.3490(2) 0.36008(10) 0.0376(7) Uani 1 1 d . . . C14 C 0.37772(13) 0.4220(2) 0.33726(11) 0.0507(9) Uani 1 1 d . . . C15 C 0.40464(12) 0.3685(2) 0.30192(10) 0.0399(7) Uani 1 1 d . . . C16 C 0.43725(12) 0.4109(2) 0.27009(10) 0.0456(8) Uani 1 1 d . . . H16 H 0.4390 0.4845 0.2702 0.055 Uiso 1 1 calc R . . C17 C 0.46816(12) 0.3625(2) 0.23767(10) 0.0384(7) Uani 1 1 d . . . C18 C 0.49692(12) 0.4126(2) 0.20277(10) 0.0433(7) Uani 1 1 d . . . C19 C 0.51952(12) 0.3340(2) 0.17745(10) 0.0413(7) Uani 1 1 d . . . C20 C 0.50405(11) 0.2398(2) 0.19717(9) 0.0340(6) Uani 1 1 d . . . C21 C 0.16421(12) 0.1267(2) 0.58686(10) 0.0423(7) Uani 1 1 d . . . C22 C 0.14473(12) 0.0479(2) 0.55621(11) 0.0463(8) Uani 1 1 d . . . H22 H 0.1339 0.0641 0.5239 0.056 Uiso 1 1 calc R . . C23 C 0.14072(14) -0.0544(3) 0.57181(12) 0.0542(9) Uani 1 1 d . . . C24 C 0.15704(13) -0.0759(3) 0.61905(12) 0.0595(9) Uani 1 1 d . . . H24 H 0.1547 -0.1450 0.6303 0.071 Uiso 1 1 calc R . . C25 C 0.17660(14) 0.0003(3) 0.65023(12) 0.0563(9) Uani 1 1 d . . . C26 C 0.17956(12) 0.1014(3) 0.63446(11) 0.0482(8) Uani 1 1 d . . . H26 H 0.1921 0.1542 0.6561 0.058 Uiso 1 1 calc R . . C27 C 0.11919(17) -0.1397(3) 0.53925(14) 0.0722(11) Uani 1 1 d . . . H27A H 0.1436 -0.1993 0.5425 0.108 Uiso 1 1 calc R . . H27B H 0.1164 -0.1150 0.5063 0.108 Uiso 1 1 calc R . . H27C H 0.0835 -0.1605 0.5478 0.108 Uiso 1 1 calc R . . C28 C 0.19520(19) -0.0274(4) 0.70147(13) 0.0931(15) Uani 1 1 d . . . H28A H 0.2094 0.0347 0.7183 0.140 Uiso 1 1 calc R . . H28B H 0.2235 -0.0802 0.7019 0.140 Uiso 1 1 calc R . . H28C H 0.1647 -0.0546 0.7172 0.140 Uiso 1 1 calc R . . C29 C 0.12705(16) 0.3410(3) 0.63420(12) 0.0631(10) Uani 1 1 d . . . H29A H 0.1532 0.3525 0.6618 0.095 Uiso 1 1 calc R . . H29B H 0.1063 0.2781 0.6392 0.095 Uiso 1 1 calc R . . H29C H 0.1026 0.4005 0.6303 0.095 Uiso 1 1 calc R . . C30 C 0.16461(15) 0.5200(2) 0.56719(13) 0.0614(10) Uani 1 1 d . . . H30A H 0.1277 0.5335 0.5760 0.074 Uiso 1 1 calc R . . H30B H 0.1685 0.5552 0.5365 0.074 Uiso 1 1 calc R . . C31 C 0.20503(19) 0.5661(3) 0.60523(17) 0.0962(15) Uani 1 1 d . . . H31A H 0.2021 0.5304 0.6356 0.144 Uiso 1 1 calc R . . H31B H 0.1975 0.6400 0.6089 0.144 Uiso 1 1 calc R . . H31C H 0.2416 0.5574 0.5956 0.144 Uiso 1 1 calc R . . C32 C 0.27868(16) 0.5352(2) 0.41336(13) 0.0681(11) Uani 1 1 d . . . H32A H 0.3097 0.5716 0.4294 0.102 Uiso 1 1 calc R . . H32B H 0.2456 0.5595 0.4261 0.102 Uiso 1 1 calc R . . H32C H 0.2767 0.5492 0.3791 0.102 Uiso 1 1 calc R . . C33 C 0.3837(2) 0.5365(3) 0.34737(17) 0.0994(18) Uani 1 1 d . . . H33A H 0.3538 0.5741 0.3303 0.149 Uiso 1 1 calc R . . H33B H 0.4179 0.5611 0.3368 0.149 Uiso 1 1 calc R . . H33C H 0.3834 0.5486 0.3817 0.149 Uiso 1 1 calc R . . C34 C 0.50298(16) 0.5280(2) 0.19626(13) 0.0625(10) Uani 1 1 d . . . H34A H 0.5094 0.5417 0.1627 0.075 Uiso 1 1 calc R . . H34B H 0.4687 0.5620 0.2023 0.075 Uiso 1 1 calc R . . C35 C 0.5469(2) 0.5757(3) 0.22741(14) 0.0991(17) Uani 1 1 d . . . H35A H 0.5383 0.5719 0.2606 0.149 Uiso 1 1 calc R . . H35B H 0.5509 0.6484 0.2184 0.149 Uiso 1 1 calc R . . H35C H 0.5806 0.5385 0.2240 0.149 Uiso 1 1 calc R . . C36 C 0.55553(14) 0.3475(2) 0.13761(12) 0.0530(9) Uani 1 1 d . . . H36A H 0.5334 0.3515 0.1071 0.080 Uiso 1 1 calc R . . H36B H 0.5801 0.2882 0.1372 0.080 Uiso 1 1 calc R . . H36C H 0.5765 0.4114 0.1427 0.080 Uiso 1 1 calc R . . C37 C 0.51681(11) 0.1345(2) 0.18198(10) 0.0355(6) Uani 1 1 d . . . C38 C 0.54008(12) 0.0613(2) 0.21298(10) 0.0430(7) Uani 1 1 d . . . H38 H 0.5499 0.0807 0.2451 0.052 Uiso 1 1 calc R . . C39 C 0.54970(14) -0.0396(2) 0.19899(12) 0.0529(8) Uani 1 1 d . . . C40 C 0.53327(14) -0.0665(3) 0.15185(13) 0.0563(9) Uani 1 1 d . . . H40 H 0.5386 -0.1356 0.1417 0.068 Uiso 1 1 calc R . . C41 C 0.50961(13) 0.0037(3) 0.11959(11) 0.0530(8) Uani 1 1 d . . . C42 C 0.50211(11) 0.1039(3) 0.13469(10) 0.0437(7) Uani 1 1 d . . . H42 H 0.4866 0.1535 0.1126 0.052 Uiso 1 1 calc R . . C43 C 0.57570(19) -0.1190(3) 0.23301(14) 0.0826(13) Uani 1 1 d . . . H43A H 0.5885 -0.0851 0.2630 0.124 Uiso 1 1 calc R . . H43B H 0.6062 -0.1510 0.2190 0.124 Uiso 1 1 calc R . . H43C H 0.5493 -0.1726 0.2391 0.124 Uiso 1 1 calc R . . C44 C 0.49126(18) -0.0291(3) 0.06943(13) 0.0817(13) Uani 1 1 d . . . H44A H 0.4610 -0.0774 0.0699 0.123 Uiso 1 1 calc R . . H44B H 0.5210 -0.0633 0.0552 0.123 Uiso 1 1 calc R . . H44C H 0.4798 0.0320 0.0505 0.123 Uiso 1 1 calc R . . C45 C 0.49039(12) 0.0730(2) 0.36556(10) 0.0410(7) Uani 1 1 d . A . C46 C 0.50425(15) -0.0221(3) 0.38843(11) 0.0582(9) Uani 1 1 d . A . C47 C 0.48905(17) -0.0994(3) 0.35600(12) 0.0656(10) Uani 1 1 d D . . C48 C 0.46671(13) -0.0499(2) 0.31369(10) 0.0462(8) Uani 1 1 d . A . C49 C 0.44359(13) -0.0985(2) 0.27287(10) 0.0461(8) Uani 1 1 d . . . H49 H 0.4482 -0.1716 0.2723 0.055 Uiso 1 1 calc R A . C50 C 0.41494(11) -0.05745(19) 0.23301(9) 0.0347(6) Uani 1 1 d . A . C51 C 0.39403(12) -0.1119(2) 0.19163(10) 0.0397(7) Uani 1 1 d . . . C52 C 0.36664(11) -0.04115(19) 0.16243(9) 0.0328(6) Uani 1 1 d . A . C53 C 0.37298(10) 0.05735(18) 0.18658(9) 0.0274(5) Uani 1 1 d . . . C54 C 0.34989(12) 0.15611(19) 0.16685(9) 0.0339(6) Uani 1 1 d . A . H54A H 0.3725 0.2148 0.1795 0.041 Uiso 1 1 calc R . . H54B H 0.3133 0.1656 0.1772 0.041 Uiso 1 1 calc R . . C55 C 0.34693(12) 0.15648(19) 0.11229(9) 0.0348(6) Uani 1 1 d . . . H55A H 0.3235 0.2140 0.0997 0.042 Uiso 1 1 calc R A . H55B H 0.3833 0.1679 0.1019 0.042 Uiso 1 1 calc R . . C56 C 0.17488(10) 0.05634(19) 0.40712(9) 0.0288(5) Uani 1 1 d . . . C57 C 0.33537(10) -0.04096(19) 0.11581(9) 0.0314(6) Uani 1 1 d . . . C58 C 0.30820(12) -0.1137(2) 0.08707(10) 0.0391(7) Uani 1 1 d . . . C59 C 0.21758(11) -0.0597(2) 0.45252(10) 0.0354(6) Uani 1 1 d . . . C60 C 0.25100(12) -0.1011(2) 0.48972(10) 0.0440(7) Uani 1 1 d . . . H60 H 0.2545 -0.1744 0.4890 0.053 Uiso 1 1 calc R . . C61 C 0.28020(12) -0.0529(2) 0.52783(10) 0.0440(7) Uani 1 1 d . . . C62 C 0.31046(13) -0.1039(3) 0.56644(12) 0.0560(9) Uani 1 1 d . . . C63 C 0.32858(13) -0.0284(3) 0.59818(11) 0.0570(9) Uani 1 1 d . . . C64 C 0.31020(12) 0.0683(3) 0.57803(10) 0.0457(7) Uani 1 1 d . . . C65 C 0.49679(12) 0.1783(2) 0.38514(10) 0.0434(7) Uani 1 1 d . . . C66 C 0.51961(14) 0.2561(3) 0.35951(11) 0.0602(10) Uani 1 1 d . . . H66 H 0.5321 0.2404 0.3295 0.072 Uiso 1 1 calc R . . C67 C 0.52441(19) 0.3568(3) 0.37729(14) 0.0781(13) Uani 1 1 d . . . C68 C 0.50520(18) 0.3782(3) 0.42028(14) 0.0762(12) Uani 1 1 d . . . H68 H 0.5075 0.4472 0.4320 0.091 Uiso 1 1 calc R . . C69 C 0.48286(16) 0.3038(3) 0.44681(13) 0.0657(10) Uani 1 1 d . . . C70 C 0.47917(13) 0.2036(3) 0.42946(11) 0.0535(8) Uani 1 1 d . . . H70 H 0.4644 0.1509 0.4479 0.064 Uiso 1 1 calc R . . C71 C 0.5490(3) 0.4413(4) 0.34953(17) 0.151(3) Uani 1 1 d . . . H71A H 0.5219 0.4948 0.3410 0.227 Uiso 1 1 calc R . . H71B H 0.5617 0.4121 0.3205 0.227 Uiso 1 1 calc R . . H71C H 0.5794 0.4722 0.3690 0.227 Uiso 1 1 calc R . . C72 C 0.4598(3) 0.3297(4) 0.49326(17) 0.119(2) Uani 1 1 d . . . H72A H 0.4351 0.2745 0.5012 0.179 Uiso 1 1 calc R . . H72B H 0.4402 0.3955 0.4899 0.179 Uiso 1 1 calc R . . H72C H 0.4892 0.3357 0.5187 0.179 Uiso 1 1 calc R . . C73 C 0.53220(19) -0.0354(3) 0.43783(12) 0.0831(14) Uani 1 1 d . . . H73A H 0.5065 -0.0623 0.4591 0.125 Uiso 1 1 calc R A . H73B H 0.5461 0.0317 0.4497 0.125 Uiso 1 1 calc R . . H73C H 0.5622 -0.0843 0.4367 0.125 Uiso 1 1 calc R . . C74A C 0.4844(3) -0.2187(6) 0.3642(4) 0.048(3) Uani 0.462(11) 1 d PD A 1 H74A H 0.4760 -0.2329 0.3972 0.058 Uiso 0.462(11) 1 calc PR A 1 H74B H 0.4554 -0.2483 0.3420 0.058 Uiso 0.462(11) 1 calc PR A 1 C76 C 0.40495(17) -0.2252(2) 0.18253(13) 0.0718(12) Uani 1 1 d . A . H76A H 0.3749 -0.2671 0.1919 0.108 Uiso 1 1 calc R . . H76B H 0.4383 -0.2463 0.2012 0.108 Uiso 1 1 calc R . . H76C H 0.4088 -0.2357 0.1486 0.108 Uiso 1 1 calc R . . C77 C 0.30358(16) -0.2285(2) 0.09528(13) 0.0651(11) Uani 1 1 d . . . H77A H 0.3359 -0.2634 0.0858 0.098 Uiso 1 1 calc R A . H77B H 0.2718 -0.2554 0.0763 0.098 Uiso 1 1 calc R . . H77C H 0.3001 -0.2416 0.1291 0.098 Uiso 1 1 calc R . . C78 C 0.32167(18) -0.2185(3) 0.56901(15) 0.0816(13) Uani 1 1 d . . . H78A H 0.2880 -0.2569 0.5596 0.098 Uiso 1 1 calc R . . H78B H 0.3338 -0.2376 0.6023 0.098 Uiso 1 1 calc R . . C79 C 0.3658(2) -0.2514(4) 0.5358(2) 0.129(2) Uani 1 1 d . . . H79A H 0.3514 -0.2445 0.5024 0.193 Uiso 1 1 calc R . . H79B H 0.3762 -0.3236 0.5423 0.193 Uiso 1 1 calc R . . H79C H 0.3974 -0.2066 0.5419 0.193 Uiso 1 1 calc R . . C80 C 0.36320(16) -0.0426(3) 0.64451(12) 0.0773(13) Uani 1 1 d . . . H80A H 0.3401 -0.0497 0.6706 0.116 Uiso 1 1 calc R . . H80B H 0.3867 0.0179 0.6503 0.116 Uiso 1 1 calc R . . H80C H 0.3853 -0.1050 0.6427 0.116 Uiso 1 1 calc R . . C81 C 0.31892(12) 0.1725(3) 0.59792(11) 0.0489(8) Uani 1 1 d . . . C82 C 0.31372(12) 0.1919(3) 0.64627(12) 0.0561(9) Uani 1 1 d . . . H82 H 0.3063 0.1357 0.6665 0.067 Uiso 1 1 calc R . . C83 C 0.31900(14) 0.2894(4) 0.66496(13) 0.0662(11) Uani 1 1 d . . . C84 C 0.33003(16) 0.3705(3) 0.63596(14) 0.0718(11) Uani 1 1 d . . . H84 H 0.3334 0.4383 0.6491 0.086 Uiso 1 1 calc R . . C85 C 0.33646(15) 0.3562(3) 0.58724(14) 0.0640(10) Uani 1 1 d . . . C86 C 0.33071(12) 0.2561(3) 0.56969(12) 0.0555(9) Uani 1 1 d . . . H86 H 0.3350 0.2442 0.5370 0.067 Uiso 1 1 calc R . . C87 C 0.31177(19) 0.3093(4) 0.71702(14) 0.0927(14) Uani 1 1 d . . . H87A H 0.2959 0.2480 0.7308 0.139 Uiso 1 1 calc R . . H87B H 0.2879 0.3690 0.7197 0.139 Uiso 1 1 calc R . . H87C H 0.3469 0.3239 0.7343 0.139 Uiso 1 1 calc R . . C88 C 0.34877(18) 0.4462(3) 0.55581(15) 0.0867(13) Uani 1 1 d . . . H88A H 0.3425 0.4255 0.5223 0.130 Uiso 1 1 calc R . . H88B H 0.3865 0.4668 0.5628 0.130 Uiso 1 1 calc R . . H88C H 0.3253 0.5047 0.5619 0.130 Uiso 1 1 calc R . . N1 N 0.19598(9) 0.24917(17) 0.52960(7) 0.0345(5) Uani 1 1 d . . . N2 N 0.27069(9) 0.25865(16) 0.45404(7) 0.0322(5) Uani 1 1 d . . . N3 N 0.39315(8) 0.26189(15) 0.30445(7) 0.0296(5) Uani 1 1 d . . . N4 N 0.47400(8) 0.25527(16) 0.23397(7) 0.0306(5) Uani 1 1 d . . . N5 N 0.46843(9) 0.05710(17) 0.32030(7) 0.0339(5) Uani 1 1 d . . . N6 N 0.40100(8) 0.04784(15) 0.22829(7) 0.0284(5) Uani 1 1 d . A . N7 N 0.20586(9) 0.04631(16) 0.44778(7) 0.0310(5) Uani 1 1 d . . . N8 N 0.28153(9) 0.05399(18) 0.53572(8) 0.0378(5) Uani 1 1 d . . . Zn1 Zn 0.434710(12) 0.15530(2) 0.272119(10) 0.02759(10) Uani 1 1 d . A . Zn2 Zn 0.238096(12) 0.15139(2) 0.493711(10) 0.03123(10) Uani 1 1 d . . . C75A C 0.5388(3) -0.2668(8) 0.3552(3) 0.078(3) Uani 0.462(11) 1 d PD A 1 H75A H 0.5374 -0.3419 0.3600 0.118 Uiso 0.462(11) 1 calc PR A 1 H75B H 0.5672 -0.2370 0.3774 0.118 Uiso 0.462(11) 1 calc PR A 1 H75C H 0.5467 -0.2521 0.3224 0.118 Uiso 0.462(11) 1 calc PR A 1 C74B C 0.5104(5) -0.2117(6) 0.3614(5) 0.094(5) Uani 0.538(11) 1 d PD A 2 H74C H 0.5098 -0.2479 0.3304 0.112 Uiso 0.538(11) 1 calc PR A 2 H74D H 0.5471 -0.2145 0.3779 0.112 Uiso 0.538(11) 1 calc PR A 2 C75B C 0.4681(6) -0.2545(8) 0.3923(5) 0.186(8) Uani 0.538(11) 1 d PD A 2 H75D H 0.4757 -0.3276 0.3994 0.279 Uiso 0.538(11) 1 calc PR A 2 H75E H 0.4323 -0.2481 0.3751 0.279 Uiso 0.538(11) 1 calc PR A 2 H75F H 0.4692 -0.2151 0.4220 0.279 Uiso 0.538(11) 1 calc PR A 2 C90 C 0.8656(3) 0.2850(8) 0.2311(4) 0.229(5) Uani 1 1 d D . . H90A H 0.9028 0.2998 0.2436 0.343 Uiso 1 1 calc R . . H90B H 0.8618 0.2957 0.1965 0.343 Uiso 1 1 calc R . . H90C H 0.8568 0.2129 0.2382 0.343 Uiso 1 1 calc R . . C91 C 0.82778(16) 0.3566(7) 0.2541(3) 0.235(5) Uani 1 1 d D . . H91A H 0.8399 0.4291 0.2509 0.282 Uiso 1 1 calc R . . H91B H 0.8287 0.3403 0.2885 0.282 Uiso 1 1 calc R . . C92 C 0.77015(16) 0.3458(9) 0.23127(17) 0.386(14) Uani 1 1 d D . . H92A H 0.7620 0.4039 0.2089 0.463 Uiso 1 1 calc R . . H92B H 0.7667 0.2804 0.2129 0.463 Uiso 1 1 calc R . . C93 C 0.0476(6) 0.2702(10) 0.4851(4) 0.082(4) Uani 0.452(5) 1 d PD B 1 H93A H 0.0852 0.2492 0.4929 0.122 Uiso 0.452(5) 1 calc PR B 1 H93B H 0.0454 0.3167 0.4575 0.122 Uiso 0.452(5) 1 calc PR B 1 H93C H 0.0254 0.2087 0.4776 0.122 Uiso 0.452(5) 1 calc PR B 1 C94 C 0.0273(4) 0.3266(8) 0.5278(4) 0.067(3) Uiso 0.452(5) 1 d PD B 1 H94A H 0.0324 0.2798 0.5556 0.081 Uiso 0.452(5) 1 calc PR B 1 H94B H 0.0507 0.3877 0.5348 0.081 Uiso 0.452(5) 1 calc PR B 1 C95 C -0.0299(4) 0.3630(8) 0.5236(4) 0.076(3) Uani 0.452(5) 1 d P B 1 H95A H -0.0542 0.3023 0.5193 0.092 Uiso 0.452(5) 1 calc PR B 1 H95B H -0.0364 0.4076 0.4951 0.092 Uiso 0.452(5) 1 calc PR B 1 C96 C -0.0434(3) 0.4240(7) 0.5676(3) 0.071(3) Uiso 0.452(5) 1 d P B 1 H96A H -0.0405 0.3767 0.5954 0.086 Uiso 0.452(5) 1 calc PR B 1 H96B H -0.0161 0.4793 0.5740 0.086 Uiso 0.452(5) 1 calc PR B 1 C97 C -0.0993(4) 0.4736(8) 0.5636(4) 0.081(3) Uiso 0.452(5) 1 d P B 1 H97A H -0.1262 0.4197 0.5536 0.097 Uiso 0.452(5) 1 calc PR B 1 H97B H -0.1007 0.5267 0.5381 0.097 Uiso 0.452(5) 1 calc PR B 1 C98 C -0.1168(6) 0.5285(9) 0.6126(5) 0.088(4) Uiso 0.452(5) 1 d P B 1 H98A H -0.1526 0.5595 0.6064 0.132 Uiso 0.452(5) 1 calc PR B 1 H98B H -0.0907 0.5826 0.6228 0.132 Uiso 0.452(5) 1 calc PR B 1 H98C H -0.1175 0.4761 0.6377 0.132 Uiso 0.452(5) 1 calc PR B 1 C102 C -0.1080(6) 0.5189(11) 0.5924(6) 0.101(5) Uiso 0.410(6) 1 d PD C 2 H10C H -0.1312 0.4794 0.5684 0.121 Uiso 0.410(6) 1 calc PR C 2 H10D H -0.0776 0.4727 0.6032 0.121 Uiso 0.410(6) 1 calc PR C 2 C103 C -0.0834(6) 0.6120(11) 0.5651(5) 0.134(6) Uiso 0.410(6) 1 d PD C 2 H10E H -0.1142 0.6573 0.5544 0.161 Uiso 0.410(6) 1 calc PR C 2 H10F H -0.0610 0.6516 0.5896 0.161 Uiso 0.410(6) 1 calc PR C 2 C101 C -0.1408(6) 0.5352(11) 0.6351(5) 0.106(5) Uiso 0.410(6) 1 d PD C 2 H10G H -0.1527 0.4679 0.6463 0.159 Uiso 0.410(6) 1 calc PR C 2 H10H H -0.1722 0.5784 0.6256 0.159 Uiso 0.410(6) 1 calc PR C 2 H10I H -0.1183 0.5696 0.6608 0.159 Uiso 0.410(6) 1 calc PR C 2 C106 C 0.0010(9) 0.6825(15) 0.4609(6) 0.163(8) Uiso 0.410(6) 1 d PD C 2 H10J H 0.0268 0.7391 0.4582 0.245 Uiso 0.410(6) 1 calc PR C 2 H10K H -0.0220 0.6760 0.4309 0.245 Uiso 0.410(6) 1 calc PR C 2 H10L H 0.0206 0.6175 0.4675 0.245 Uiso 0.410(6) 1 calc PR C 2 C104 C -0.0505(6) 0.6033(10) 0.5237(5) 0.117(5) Uiso 0.410(6) 1 d PD C 2 H10M H -0.0711 0.5621 0.4986 0.140 Uiso 0.410(6) 1 calc PR C 2 H10N H -0.0174 0.5640 0.5339 0.140 Uiso 0.410(6) 1 calc PR C 2 C105 C -0.0340(9) 0.7059(12) 0.5015(7) 0.127(8) Uiso 0.410(6) 1 d PD C 2 H10O H -0.0665 0.7448 0.4891 0.152 Uiso 0.410(6) 1 calc PR C 2 H10P H -0.0135 0.7490 0.5259 0.152 Uiso 0.410(6) 1 calc PR C 2 C108 C -0.023(3) 0.647(3) 0.4956(17) 0.153(15) Uiso 0.138(6) 1 d PD D 3 H10Q H -0.0504 0.6464 0.4682 0.184 Uiso 0.138(6) 1 calc PR D 3 H10R H 0.0117 0.6691 0.4835 0.184 Uiso 0.138(6) 1 calc PR D 3 C107 C -0.039(3) 0.729(3) 0.531(2) 0.153(15) Uiso 0.138(6) 1 d PD D 3 H10S H -0.0367 0.7982 0.5168 0.230 Uiso 0.138(6) 1 calc PR D 3 H10T H -0.0138 0.7259 0.5601 0.230 Uiso 0.138(6) 1 calc PR D 3 H10U H -0.0753 0.7159 0.5391 0.230 Uiso 0.138(6) 1 calc PR D 3 C109 C -0.0157(19) 0.537(3) 0.5149(15) 0.153(15) Uiso 0.138(6) 1 d PD . 3 H10V H -0.0518 0.5071 0.5176 0.184 Uiso 0.138(6) 1 calc PR D 3 H10W H 0.0030 0.5404 0.5473 0.184 Uiso 0.138(6) 1 calc PR D 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0324(16) 0.0502(18) 0.0373(15) -0.0050(13) 0.0136(12) -0.0026(12) C2 0.0479(19) 0.059(2) 0.0410(16) -0.0095(15) 0.0242(14) -0.0049(15) C3 0.0467(18) 0.0455(19) 0.0484(17) -0.0100(14) 0.0241(14) 0.0011(14) C4 0.0379(16) 0.0420(18) 0.0386(15) -0.0100(13) 0.0182(13) 0.0006(12) C5 0.0523(18) 0.0293(16) 0.0475(16) -0.0103(13) 0.0240(14) 0.0000(12) C6 0.0436(17) 0.0349(16) 0.0390(15) -0.0073(12) 0.0194(13) -0.0044(12) C7 0.0539(19) 0.0288(15) 0.0500(17) -0.0111(13) 0.0291(15) -0.0058(12) C8 0.0407(16) 0.0317(15) 0.0428(15) -0.0147(12) 0.0220(13) -0.0089(11) C9 0.0324(15) 0.0311(15) 0.0336(13) -0.0064(11) 0.0103(11) -0.0063(11) C10 0.0371(16) 0.0353(16) 0.0404(15) -0.0029(12) 0.0169(13) 0.0026(11) C11 0.0415(16) 0.0250(14) 0.0416(15) -0.0053(12) 0.0204(13) -0.0025(11) C12 0.0293(14) 0.0251(14) 0.0364(13) -0.0057(11) 0.0135(11) -0.0039(10) C13 0.0452(17) 0.0281(15) 0.0432(15) -0.0116(12) 0.0240(13) -0.0102(11) C14 0.067(2) 0.0285(16) 0.064(2) -0.0177(14) 0.0442(17) -0.0119(14) C15 0.0472(18) 0.0289(15) 0.0477(16) -0.0105(12) 0.0269(14) -0.0101(12) C16 0.058(2) 0.0309(16) 0.0521(18) -0.0145(13) 0.0299(15) -0.0137(13) C17 0.0457(17) 0.0303(16) 0.0422(15) -0.0055(12) 0.0212(13) -0.0082(12) C18 0.0508(18) 0.0334(16) 0.0499(17) -0.0017(13) 0.0270(14) -0.0065(13) C19 0.0427(17) 0.0430(18) 0.0416(15) 0.0005(13) 0.0217(13) -0.0028(13) C20 0.0327(15) 0.0390(16) 0.0319(13) -0.0039(12) 0.0112(12) 0.0006(11) C21 0.0334(16) 0.0542(19) 0.0413(16) 0.0028(14) 0.0146(13) -0.0011(13) C22 0.0440(19) 0.057(2) 0.0395(16) 0.0003(15) 0.0130(14) -0.0048(14) C23 0.058(2) 0.047(2) 0.061(2) 0.0067(17) 0.0214(17) -0.0052(15) C24 0.056(2) 0.057(2) 0.067(2) 0.0191(19) 0.0136(19) -0.0009(16) C25 0.047(2) 0.071(3) 0.0517(19) 0.0143(18) 0.0099(16) -0.0002(17) C26 0.0349(17) 0.070(2) 0.0400(16) 0.0024(16) 0.0073(13) -0.0044(15) C27 0.086(3) 0.059(2) 0.076(3) -0.003(2) 0.027(2) -0.024(2) C28 0.086(3) 0.126(4) 0.063(2) 0.039(3) -0.014(2) -0.007(3) C29 0.081(3) 0.060(2) 0.054(2) -0.0050(17) 0.0425(19) 0.0011(18) C30 0.073(2) 0.051(2) 0.068(2) -0.0181(17) 0.045(2) 0.0023(17) C31 0.103(4) 0.077(3) 0.111(4) -0.039(3) 0.020(3) -0.010(3) C32 0.097(3) 0.0351(19) 0.082(3) -0.0059(17) 0.060(2) -0.0006(17) C33 0.147(4) 0.036(2) 0.133(4) -0.036(2) 0.114(3) -0.037(2) C34 0.087(3) 0.0359(18) 0.073(2) 0.0020(17) 0.053(2) -0.0087(17) C35 0.163(5) 0.074(3) 0.065(3) -0.014(2) 0.037(3) -0.064(3) C36 0.055(2) 0.053(2) 0.0563(19) -0.0025(16) 0.0351(17) -0.0074(15) C37 0.0306(15) 0.0429(17) 0.0352(14) -0.0033(12) 0.0150(12) 0.0038(11) C38 0.0459(18) 0.0461(18) 0.0382(15) -0.0059(14) 0.0111(14) 0.0085(14) C39 0.058(2) 0.0451(19) 0.059(2) -0.0040(16) 0.0221(17) 0.0113(15) C40 0.057(2) 0.047(2) 0.068(2) -0.0200(18) 0.0200(18) 0.0041(16) C41 0.049(2) 0.063(2) 0.0484(18) -0.0205(17) 0.0115(15) 0.0015(16) C42 0.0369(17) 0.058(2) 0.0372(15) -0.0103(14) 0.0093(13) 0.0051(14) C43 0.114(4) 0.065(3) 0.072(3) 0.006(2) 0.028(2) 0.033(2) C44 0.092(3) 0.091(3) 0.060(2) -0.038(2) 0.003(2) 0.007(2) C45 0.0413(17) 0.0481(18) 0.0341(14) -0.0027(13) 0.0054(13) -0.0003(13) C46 0.072(3) 0.062(2) 0.0378(17) -0.0002(16) -0.0096(16) 0.0149(18) C47 0.095(3) 0.048(2) 0.0497(19) 0.0015(17) -0.0146(19) 0.0214(19) C48 0.060(2) 0.0411(18) 0.0358(15) -0.0007(13) -0.0047(14) 0.0155(14) C49 0.067(2) 0.0240(16) 0.0460(17) 0.0011(13) -0.0005(15) 0.0136(13) C50 0.0426(16) 0.0220(14) 0.0385(14) 0.0010(11) -0.0010(12) 0.0046(11) C51 0.0499(18) 0.0237(14) 0.0441(16) -0.0030(13) -0.0038(14) 0.0035(12) C52 0.0375(16) 0.0210(13) 0.0396(15) -0.0045(11) 0.0010(12) 0.0012(11) C53 0.0293(14) 0.0197(13) 0.0338(13) -0.0010(10) 0.0060(11) -0.0014(10) C54 0.0412(16) 0.0243(14) 0.0348(14) -0.0039(11) -0.0034(12) 0.0045(11) C55 0.0452(17) 0.0237(14) 0.0342(14) 0.0023(11) -0.0036(12) -0.0008(11) C56 0.0293(14) 0.0243(14) 0.0333(13) 0.0030(11) 0.0049(11) 0.0010(10) C57 0.0312(15) 0.0254(14) 0.0372(14) -0.0054(11) 0.0009(12) 0.0007(10) C58 0.0486(18) 0.0243(14) 0.0433(16) -0.0039(12) -0.0022(13) -0.0011(12) C59 0.0389(16) 0.0283(15) 0.0392(15) 0.0051(12) 0.0039(12) 0.0011(11) C60 0.0511(19) 0.0331(17) 0.0463(17) 0.0058(14) -0.0045(14) 0.0052(13) C61 0.0430(18) 0.0477(19) 0.0400(16) 0.0071(14) -0.0034(14) 0.0066(13) C62 0.051(2) 0.066(2) 0.0497(19) 0.0108(18) -0.0079(16) 0.0144(17) C63 0.042(2) 0.082(3) 0.0453(18) 0.0054(18) -0.0025(15) 0.0140(17) C64 0.0359(17) 0.065(2) 0.0357(15) -0.0008(15) -0.0008(13) 0.0012(14) C65 0.0375(17) 0.057(2) 0.0339(15) -0.0047(14) -0.0054(13) 0.0013(13) C66 0.065(2) 0.075(3) 0.0397(17) -0.0042(17) -0.0015(16) -0.0270(19) C67 0.104(3) 0.071(3) 0.055(2) 0.001(2) -0.024(2) -0.039(2) C68 0.107(3) 0.057(2) 0.060(2) -0.018(2) -0.023(2) -0.006(2) C69 0.075(3) 0.069(3) 0.052(2) -0.019(2) 0.0028(19) 0.006(2) C70 0.052(2) 0.068(2) 0.0403(16) -0.0074(16) 0.0036(15) 0.0040(16) C71 0.216(7) 0.150(5) 0.080(3) 0.011(3) -0.024(4) -0.139(5) C72 0.163(6) 0.113(4) 0.088(3) -0.037(3) 0.044(4) 0.020(4) C73 0.123(4) 0.077(3) 0.0442(19) 0.0025(19) -0.025(2) 0.034(3) C74A 0.040(6) 0.061(6) 0.042(4) 0.029(4) -0.006(5) 0.017(4) C76 0.110(3) 0.0319(18) 0.067(2) -0.0150(17) -0.030(2) 0.0223(18) C77 0.091(3) 0.0279(17) 0.071(2) 0.0014(16) -0.025(2) -0.0125(17) C78 0.088(3) 0.073(3) 0.077(3) 0.013(2) -0.032(2) 0.024(2) C79 0.109(4) 0.100(4) 0.168(6) -0.031(4) -0.038(4) 0.040(3) C80 0.071(3) 0.102(3) 0.053(2) 0.004(2) -0.022(2) 0.028(2) C81 0.0254(16) 0.080(2) 0.0411(16) -0.0063(16) 0.0008(13) -0.0050(14) C82 0.0352(18) 0.087(3) 0.0457(18) -0.0131(18) 0.0038(14) -0.0018(16) C83 0.043(2) 0.103(3) 0.054(2) -0.020(2) 0.0109(17) -0.0092(19) C84 0.061(2) 0.084(3) 0.071(3) -0.035(2) 0.010(2) -0.016(2) C85 0.050(2) 0.076(3) 0.065(2) -0.014(2) 0.0051(18) -0.0185(18) C86 0.0365(18) 0.081(3) 0.0487(18) -0.0160(18) 0.0014(15) -0.0129(16) C87 0.093(3) 0.124(4) 0.065(3) -0.039(3) 0.029(2) -0.008(3) C88 0.084(3) 0.085(3) 0.091(3) -0.015(3) 0.008(2) -0.037(2) N1 0.0317(13) 0.0415(14) 0.0321(11) -0.0044(10) 0.0122(10) -0.0032(10) N2 0.0357(13) 0.0335(13) 0.0291(11) -0.0065(9) 0.0122(10) -0.0011(9) N3 0.0323(12) 0.0243(11) 0.0341(11) -0.0069(9) 0.0136(9) -0.0061(9) N4 0.0323(12) 0.0306(12) 0.0304(11) -0.0066(9) 0.0117(9) -0.0027(9) N5 0.0323(13) 0.0379(14) 0.0318(11) -0.0002(10) 0.0040(10) 0.0010(9) N6 0.0344(12) 0.0186(11) 0.0329(11) -0.0035(9) 0.0062(9) 0.0011(8) N7 0.0318(12) 0.0279(12) 0.0333(11) 0.0053(9) 0.0038(10) 0.0022(9) N8 0.0325(13) 0.0467(15) 0.0338(12) 0.0006(11) 0.0011(10) 0.0008(10) Zn1 0.03082(18) 0.02604(17) 0.02703(16) -0.00411(12) 0.00867(12) -0.00099(12) Zn2 0.03165(19) 0.03454(19) 0.02843(16) -0.00149(13) 0.00788(13) -0.00028(12) C75A 0.075(7) 0.051(6) 0.105(7) 0.002(5) -0.019(5) 0.021(5) C74B 0.118(12) 0.065(7) 0.086(8) 0.001(6) -0.052(9) 0.053(8) C75B 0.32(2) 0.069(7) 0.151(13) 0.009(8) -0.096(13) -0.054(10) C90 0.209(10) 0.258(12) 0.216(10) -0.061(9) 0.002(8) 0.090(9) C91 0.254(13) 0.241(12) 0.192(10) -0.036(8) -0.071(9) -0.042(9) C92 0.63(4) 0.312(14) 0.177(14) 0.046(9) -0.16(2) -0.08(2) C93 0.091(9) 0.090(8) 0.061(7) -0.021(6) -0.011(6) 0.013(6) C95 0.054(6) 0.079(7) 0.091(7) -0.005(5) -0.023(5) -0.012(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.344(3) . ? C1 C2 1.428(4) . ? C1 C21 1.471(4) . ? C2 C3 1.360(4) . ? C2 C29 1.512(4) . ? C3 C4 1.430(4) . ? C3 C30 1.507(4) . ? C4 N1 1.386(3) . ? C4 C5 1.398(4) . ? C5 C6 1.392(4) . ? C5 H5 0.9500 . ? C6 N2 1.405(3) . ? C6 C7 1.423(4) . ? C7 C8 1.382(3) . ? C7 C32 1.513(4) . ? C8 C9 1.418(4) . ? C8 C13 1.468(4) . ? C9 N2 1.323(3) . ? C9 C10 1.488(3) . ? C10 C11 1.538(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.487(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N3 1.325(3) . ? C12 C13 1.433(3) . ? C13 C14 1.374(4) . ? C14 C15 1.429(4) . ? C14 C33 1.509(4) . ? C15 C16 1.378(4) . ? C15 N3 1.408(3) . ? C16 C17 1.395(4) . ? C16 H16 0.9500 . ? C17 N4 1.396(3) . ? C17 C18 1.424(4) . ? C18 C19 1.388(4) . ? C18 C34 1.509(4) . ? C19 C20 1.405(4) . ? C19 C36 1.511(4) . ? C20 N4 1.349(3) . ? C20 C37 1.468(4) . ? C21 C22 1.393(4) . ? C21 C26 1.401(4) . ? C22 C23 1.398(4) . ? C22 H22 0.9500 . ? C23 C24 1.385(4) . ? C23 C27 1.501(5) . ? C24 C25 1.378(5) . ? C24 H24 0.9500 . ? C25 C26 1.381(5) . ? C25 C28 1.520(5) . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.525(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.474(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.379(4) . ? C37 C42 1.407(4) . ? C38 C39 1.388(4) . ? C38 H38 0.9500 . ? C39 C40 1.399(5) . ? C39 C43 1.509(5) . ? C40 C41 1.378(5) . ? C40 H40 0.9500 . ? C41 C42 1.379(4) . ? C41 C44 1.507(4) . ? C42 H42 0.9500 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 N5 1.358(3) . ? C45 C46 1.414(4) . ? C45 C65 1.470(4) . ? C46 C47 1.383(5) . ? C46 C73 1.510(4) . ? C47 C48 1.422(4) . ? C47 C74B 1.547(7) . ? C47 C74A 1.562(8) . ? C48 C49 1.390(4) . ? C48 N5 1.393(4) . ? C49 C50 1.382(4) . ? C49 H49 0.9500 . ? C50 N6 1.405(3) . ? C50 C51 1.420(4) . ? C51 C52 1.369(4) . ? C51 C76 1.514(4) . ? C52 C53 1.444(3) . ? C52 C57 1.466(4) . ? C53 N6 1.318(3) . ? C53 C54 1.486(3) . ? C54 C55 1.534(4) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.487(3) 2 ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 N7 1.329(3) . ? C56 C57 1.425(3) 2 ? C56 C55 1.487(3) 2 ? C57 C58 1.378(4) . ? C57 C56 1.425(3) 2 ? C58 C59 1.419(4) 2 ? C58 C77 1.505(4) . ? C59 C60 1.386(4) . ? C59 N7 1.403(3) . ? C59 C58 1.419(4) 2 ? C60 C61 1.389(4) . ? C60 H60 0.9500 . ? C61 N8 1.397(4) . ? C61 C62 1.428(4) . ? C62 C63 1.372(5) . ? C62 C78 1.505(5) . ? C63 C64 1.429(5) . ? C63 C80 1.510(4) . ? C64 N8 1.347(3) . ? C64 C81 1.464(4) . ? C65 C66 1.388(4) . ? C65 C70 1.400(4) . ? C66 C67 1.395(5) . ? C66 H66 0.9500 . ? C67 C68 1.371(6) . ? C67 C71 1.505(5) . ? C68 C69 1.367(5) . ? C68 H68 0.9500 . ? C69 C70 1.383(5) . ? C69 C72 1.515(5) . ? C70 H70 0.9500 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74A C75A 1.534(7) . ? C74A H74A 0.9900 . ? C74A H74B 0.9900 . ? 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 C79 1.567(7) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? 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 C86 1.388(5) . ? C81 C82 1.404(4) . ? C82 C83 1.366(5) . ? C82 H82 0.9500 . ? C83 C84 1.372(5) . ? C83 C87 1.517(5) . ? C84 C85 1.410(5) . ? C84 H84 0.9500 . ? C85 C86 1.386(5) . ? C85 C88 1.509(5) . ? C86 H86 0.9500 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? N1 Zn2 1.978(2) . ? N2 Zn2 1.998(2) . ? N3 Zn1 1.992(2) . ? N4 Zn1 1.993(2) . ? N5 Zn1 1.988(2) . ? N6 Zn1 1.992(2) . ? N7 Zn2 1.993(2) . ? N8 Zn2 1.981(2) . ? C75A H75A 0.9800 . ? C75A H75B 0.9800 . ? C75A H75C 0.9800 . ? C74B C75B 1.529(11) . ? C74B H74C 0.9900 . ? C74B H74D 0.9900 . ? C75B H75D 0.9800 . ? C75B H75E 0.9800 . ? C75B H75F 0.9800 . ? C90 C91 1.509(5) . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C91 C92 1.527(5) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 C92 1.522(5) 2_655 ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 C94 1.530(13) . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 C95 1.498(14) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 C96 1.533(12) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 C97 1.529(12) . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? C97 C98 1.647(15) . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? C102 C101 1.531(13) . ? C102 C103 1.580(13) . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.491(11) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C101 H10G 0.9800 . ? C101 H10H 0.9800 . ? C101 H10I 0.9800 . ? C106 C105 1.531(15) . ? C106 H10J 0.9800 . ? C106 H10K 0.9800 . ? C106 H10L 0.9800 . ? C104 C105 1.537(12) . ? C104 H10M 0.9900 . ? C104 H10N 0.9900 . ? C105 H10O 0.9900 . ? C105 H10P 0.9900 . ? C108 C109 1.53(2) . ? C108 C107 1.53(2) . ? C108 H10Q 0.9900 . ? C108 H10R 0.9900 . ? C107 H10S 0.9800 . ? C107 H10T 0.9800 . ? C107 H10U 0.9800 . ? C109 C109 1.53(2) 3_566 ? C109 H10V 0.9900 . ? C109 H10W 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.0(3) . . ? N1 C1 C21 120.3(2) . . ? C2 C1 C21 128.7(3) . . ? C3 C2 C1 106.5(2) . . ? C3 C2 C29 127.3(3) . . ? C1 C2 C29 126.1(3) . . ? C2 C3 C4 106.9(3) . . ? C2 C3 C30 126.7(3) . . ? C4 C3 C30 126.3(3) . . ? N1 C4 C5 124.4(2) . . ? N1 C4 C3 109.3(2) . . ? C5 C4 C3 126.2(3) . . ? C6 C5 C4 129.7(3) . . ? C6 C5 H5 115.2 . . ? C4 C5 H5 115.2 . . ? C5 C6 N2 123.5(2) . . ? C5 C6 C7 127.1(3) . . ? N2 C6 C7 109.4(2) . . ? C8 C7 C6 106.1(2) . . ? C8 C7 C32 130.2(3) . . ? C6 C7 C32 123.6(2) . . ? C7 C8 C9 106.5(2) . . ? C7 C8 C13 135.3(3) . . ? C9 C8 C13 118.2(2) . . ? N2 C9 C8 112.0(2) . . ? N2 C9 C10 124.5(2) . . ? C8 C9 C10 123.5(2) . . ? C9 C10 C11 110.9(2) . . ? C9 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 110.8(2) . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N3 C12 C13 112.1(2) . . ? N3 C12 C11 124.1(2) . . ? C13 C12 C11 123.7(2) . . ? C14 C13 C12 105.9(2) . . ? C14 C13 C8 137.2(2) . . ? C12 C13 C8 116.9(2) . . ? C13 C14 C15 107.0(2) . . ? C13 C14 C33 128.9(3) . . ? C15 C14 C33 124.0(3) . . ? C16 C15 N3 123.8(2) . . ? C16 C15 C14 127.3(3) . . ? N3 C15 C14 109.0(2) . . ? C15 C16 C17 130.0(3) . . ? C15 C16 H16 115.0 . . ? C17 C16 H16 115.0 . . ? C16 C17 N4 124.1(2) . . ? C16 C17 C18 126.3(3) . . ? N4 C17 C18 109.6(2) . . ? C19 C18 C17 106.1(2) . . ? C19 C18 C34 127.4(3) . . ? C17 C18 C34 126.4(3) . . ? C18 C19 C20 106.8(2) . . ? C18 C19 C36 126.5(3) . . ? C20 C19 C36 126.6(3) . . ? N4 C20 C19 111.6(2) . . ? N4 C20 C37 120.7(2) . . ? C19 C20 C37 127.6(2) . . ? C22 C21 C26 118.3(3) . . ? C22 C21 C1 121.4(3) . . ? C26 C21 C1 120.3(3) . . ? C21 C22 C23 121.6(3) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C24 C23 C22 117.9(3) . . ? C24 C23 C27 120.0(3) . . ? C22 C23 C27 122.1(3) . . ? C25 C24 C23 121.8(3) . . ? C25 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C24 C25 C26 119.6(3) . . ? C24 C25 C28 119.9(4) . . ? C26 C25 C28 120.5(4) . . ? C25 C26 C21 120.7(3) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C2 C29 H29A 109.5 . . ? C2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C3 C30 C31 113.1(3) . . ? C3 C30 H30A 109.0 . . ? C31 C30 H30A 109.0 . . ? C3 C30 H30B 109.0 . . ? C31 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C7 C32 H32A 109.5 . . ? C7 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C7 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C14 C33 H33A 109.5 . . ? C14 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C14 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C18 114.6(3) . . ? C35 C34 H34A 108.6 . . ? C18 C34 H34A 108.6 . . ? C35 C34 H34B 108.6 . . ? C18 C34 H34B 108.6 . . ? H34A C34 H34B 107.6 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C19 C36 H36A 109.5 . . ? C19 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C19 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C42 117.9(3) . . ? C38 C37 C20 122.6(2) . . ? C42 C37 C20 119.4(3) . . ? C37 C38 C39 122.4(3) . . ? C37 C38 H38 118.8 . . ? C39 C38 H38 118.8 . . ? C38 C39 C40 117.3(3) . . ? C38 C39 C43 122.1(3) . . ? C40 C39 C43 120.5(3) . . ? C41 C40 C39 122.4(3) . . ? C41 C40 H40 118.8 . . ? C39 C40 H40 118.8 . . ? C40 C41 C42 118.3(3) . . ? C40 C41 C44 120.7(3) . . ? C42 C41 C44 121.0(3) . . ? C41 C42 C37 121.7(3) . . ? C41 C42 H42 119.2 . . ? C37 C42 H42 119.2 . . ? C39 C43 H43A 109.5 . . ? C39 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C39 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N5 C45 C46 111.0(3) . . ? N5 C45 C65 120.9(3) . . ? C46 C45 C65 128.1(3) . . ? C47 C46 C45 106.4(3) . . ? C47 C46 C73 127.1(3) . . ? C45 C46 C73 126.4(3) . . ? C46 C47 C48 107.1(3) . . ? C46 C47 C74B 122.6(6) . . ? C48 C47 C74B 127.5(6) . . ? C46 C47 C74A 129.2(5) . . ? C48 C47 C74A 122.5(5) . . ? C74B C47 C74A 24.7(5) . . ? C49 C48 N5 124.3(2) . . ? C49 C48 C47 126.5(3) . . ? N5 C48 C47 109.1(3) . . ? C50 C49 C48 130.2(3) . . ? C50 C49 H49 114.9 . . ? C48 C49 H49 114.9 . . ? C49 C50 N6 123.6(2) . . ? C49 C50 C51 127.1(2) . . ? N6 C50 C51 109.3(2) . . ? C52 C51 C50 106.9(2) . . ? C52 C51 C76 129.0(3) . . ? C50 C51 C76 124.0(2) . . ? C51 C52 C53 106.0(2) . . ? C51 C52 C57 137.4(2) . . ? C53 C52 C57 116.6(2) . . ? N6 C53 C52 111.4(2) . . ? N6 C53 C54 124.8(2) . . ? C52 C53 C54 123.8(2) . . ? C53 C54 C55 111.1(2) . . ? C53 C54 H54A 109.4 . . ? C55 C54 H54A 109.4 . . ? C53 C54 H54B 109.4 . . ? C55 C54 H54B 109.4 . . ? H54A C54 H54B 108.0 . . ? C56 C55 C54 110.4(2) 2 . ? C56 C55 H55A 109.6 2 . ? C54 C55 H55A 109.6 . . ? C56 C55 H55B 109.6 2 . ? C54 C55 H55B 109.6 . . ? H55A C55 H55B 108.1 . . ? N7 C56 C57 111.8(2) . 2 ? N7 C56 C55 124.5(2) . 2 ? C57 C56 C55 123.6(2) 2 2 ? C58 C57 C56 106.0(2) . 2 ? C58 C57 C52 136.0(2) . . ? C56 C57 C52 117.9(2) 2 . ? C57 C58 C59 107.0(2) . 2 ? C57 C58 C77 128.4(3) . . ? C59 C58 C77 124.6(2) 2 . ? C60 C59 N7 123.6(2) . . ? C60 C59 C58 127.2(3) . 2 ? N7 C59 C58 109.2(2) . 2 ? C59 C60 C61 130.6(3) . . ? C59 C60 H60 114.7 . . ? C61 C60 H60 114.7 . . ? C60 C61 N8 124.6(3) . . ? C60 C61 C62 126.0(3) . . ? N8 C61 C62 109.3(3) . . ? C63 C62 C61 106.9(3) . . ? C63 C62 C78 128.1(3) . . ? C61 C62 C78 124.9(3) . . ? C62 C63 C64 106.6(3) . . ? C62 C63 C80 127.4(3) . . ? C64 C63 C80 125.9(3) . . ? N8 C64 C63 110.9(3) . . ? N8 C64 C81 120.9(3) . . ? C63 C64 C81 128.1(3) . . ? C66 C65 C70 118.3(3) . . ? C66 C65 C45 120.5(3) . . ? C70 C65 C45 121.2(3) . . ? C65 C66 C67 120.8(3) . . ? C65 C66 H66 119.6 . . ? C67 C66 H66 119.6 . . ? C68 C67 C66 118.7(4) . . ? C68 C67 C71 120.4(4) . . ? C66 C67 C71 120.9(4) . . ? C69 C68 C67 122.4(4) . . ? C69 C68 H68 118.8 . . ? C67 C68 H68 118.8 . . ? C68 C69 C70 118.7(3) . . ? C68 C69 C72 121.6(4) . . ? C70 C69 C72 119.6(4) . . ? C69 C70 C65 121.2(3) . . ? C69 C70 H70 119.4 . . ? C65 C70 H70 119.4 . . ? C67 C71 H71A 109.5 . . ? C67 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C67 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C69 C72 H72A 109.5 . . ? C69 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C69 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C46 C73 H73A 109.5 . . ? C46 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C46 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C75A C74A C47 107.2(6) . . ? C75A C74A H74A 110.3 . . ? C47 C74A H74A 110.3 . . ? C75A C74A H74B 110.3 . . ? C47 C74A H74B 110.3 . . ? H74A C74A H74B 108.5 . . ? C51 C76 H76A 109.5 . . ? C51 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C51 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C58 C77 H77A 109.5 . . ? C58 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C58 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C62 C78 C79 112.0(4) . . ? C62 C78 H78A 109.2 . . ? C79 C78 H78A 109.2 . . ? C62 C78 H78B 109.2 . . ? C79 C78 H78B 109.2 . . ? H78A C78 H78B 107.9 . . ? 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 . . ? C63 C80 H80A 109.5 . . ? C63 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C63 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C86 C81 C82 117.5(3) . . ? C86 C81 C64 121.7(3) . . ? C82 C81 C64 120.8(3) . . ? C83 C82 C81 121.7(4) . . ? C83 C82 H82 119.2 . . ? C81 C82 H82 119.2 . . ? C82 C83 C84 119.4(3) . . ? C82 C83 C87 120.9(4) . . ? C84 C83 C87 119.7(4) . . ? C83 C84 C85 121.8(4) . . ? C83 C84 H84 119.1 . . ? C85 C84 H84 119.1 . . ? C86 C85 C84 116.9(4) . . ? C86 C85 C88 121.8(3) . . ? C84 C85 C88 121.3(4) . . ? C85 C86 C81 122.7(3) . . ? C85 C86 H86 118.7 . . ? C81 C86 H86 118.7 . . ? C83 C87 H87A 109.5 . . ? C83 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C83 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C85 C88 H88A 109.5 . . ? C85 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C85 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C1 N1 C4 106.2(2) . . ? C1 N1 Zn2 129.1(2) . . ? C4 N1 Zn2 123.02(17) . . ? C9 N2 C6 106.0(2) . . ? C9 N2 Zn2 131.10(18) . . ? C6 N2 Zn2 122.76(17) . . ? C12 N3 C15 106.0(2) . . ? C12 N3 Zn1 130.06(17) . . ? C15 N3 Zn1 122.30(16) . . ? C20 N4 C17 105.8(2) . . ? C20 N4 Zn1 130.88(18) . . ? C17 N4 Zn1 122.77(17) . . ? C45 N5 C48 106.3(2) . . ? C45 N5 Zn1 131.0(2) . . ? C48 N5 Zn1 122.29(18) . . ? C53 N6 C50 106.3(2) . . ? C53 N6 Zn1 130.44(17) . . ? C50 N6 Zn1 121.80(17) . . ? C56 N7 C59 106.1(2) . . ? C56 N7 Zn2 131.51(17) . . ? C59 N7 Zn2 122.22(17) . . ? C64 N8 C61 106.3(2) . . ? C64 N8 Zn2 131.3(2) . . ? C61 N8 Zn2 121.82(18) . . ? N5 Zn1 N3 109.42(9) . . ? N5 Zn1 N6 96.26(9) . . ? N3 Zn1 N6 123.83(8) . . ? N5 Zn1 N4 125.68(9) . . ? N3 Zn1 N4 95.86(8) . . ? N6 Zn1 N4 108.42(8) . . ? N1 Zn2 N8 112.67(9) . . ? N1 Zn2 N7 124.39(9) . . ? N8 Zn2 N7 97.10(9) . . ? N1 Zn2 N2 96.13(9) . . ? N8 Zn2 N2 123.10(9) . . ? N7 Zn2 N2 105.53(8) . . ? C74A C75A H75A 109.5 . . ? C74A C75A H75B 109.5 . . ? H75A C75A H75B 109.5 . . ? C74A C75A H75C 109.5 . . ? H75A C75A H75C 109.5 . . ? H75B C75A H75C 109.5 . . ? C75B C74B C47 98.4(8) . . ? C75B C74B H74C 112.1 . . ? C47 C74B H74C 112.1 . . ? C75B C74B H74D 112.1 . . ? C47 C74B H74D 112.1 . . ? H74C C74B H74D 109.7 . . ? C74B C75B H75D 109.5 . . ? C74B C75B H75E 109.5 . . ? H75D C75B H75E 109.5 . . ? C74B C75B H75F 109.5 . . ? H75D C75B H75F 109.5 . . ? H75E C75B H75F 109.5 . . ? C91 C90 H90A 109.5 . . ? C91 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C91 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C90 C91 C92 111.4(4) . . ? C90 C91 H91A 109.4 . . ? C92 C91 H91A 109.4 . . ? C90 C91 H91B 109.4 . . ? C92 C91 H91B 109.4 . . ? H91A C91 H91B 108.0 . . ? C92 C92 C91 111.3(5) 2_655 . ? C92 C92 H92A 109.4 2_655 . ? C91 C92 H92A 109.4 . . ? C92 C92 H92B 109.4 2_655 . ? C91 C92 H92B 109.4 . . ? H92A C92 H92B 108.0 . . ? C94 C93 H93A 109.5 . . ? C94 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C94 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C95 C94 C93 118.0(9) . . ? C95 C94 H94A 107.8 . . ? C93 C94 H94A 107.8 . . ? C95 C94 H94B 107.8 . . ? C93 C94 H94B 107.8 . . ? H94A C94 H94B 107.2 . . ? C94 C95 C96 112.0(7) . . ? C94 C95 H95A 109.2 . . ? C96 C95 H95A 109.2 . . ? C94 C95 H95B 109.2 . . ? C96 C95 H95B 109.2 . . ? H95A C95 H95B 107.9 . . ? C97 C96 C95 114.8(8) . . ? C97 C96 H96A 108.6 . . ? C95 C96 H96A 108.6 . . ? C97 C96 H96B 108.6 . . ? C95 C96 H96B 108.6 . . ? H96A C96 H96B 107.6 . . ? C96 C97 C98 115.2(8) . . ? C96 C97 H97A 108.5 . . ? C98 C97 H97A 108.5 . . ? C96 C97 H97B 108.5 . . ? C98 C97 H97B 108.5 . . ? H97A C97 H97B 107.5 . . ? C97 C98 H98A 109.5 . . ? C97 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C97 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C101 C102 C103 122.5(12) . . ? C101 C102 H10C 106.7 . . ? C103 C102 H10C 106.7 . . ? C101 C102 H10D 106.7 . . ? C103 C102 H10D 106.7 . . ? H10C C102 H10D 106.6 . . ? C104 C103 C102 126.1(12) . . ? C104 C103 H10E 105.8 . . ? C102 C103 H10E 105.8 . . ? C104 C103 H10F 105.8 . . ? C102 C103 H10F 105.8 . . ? H10E C103 H10F 106.2 . . ? C102 C101 H10G 109.5 . . ? C102 C101 H10H 109.5 . . ? H10G C101 H10H 109.5 . . ? C102 C101 H10I 109.5 . . ? H10G C101 H10I 109.5 . . ? H10H C101 H10I 109.5 . . ? C105 C106 H10J 109.5 . . ? C105 C106 H10K 109.5 . . ? H10J C106 H10K 109.5 . . ? C105 C106 H10L 109.5 . . ? H10J C106 H10L 109.5 . . ? H10K C106 H10L 109.5 . . ? C103 C104 C105 116.2(11) . . ? C103 C104 H10M 108.2 . . ? C105 C104 H10M 108.2 . . ? C103 C104 H10N 108.2 . . ? C105 C104 H10N 108.2 . . ? H10M C104 H10N 107.4 . . ? C106 C105 C104 109.1(11) . . ? C106 C105 H10O 109.9 . . ? C104 C105 H10O 109.9 . . ? C106 C105 H10P 109.9 . . ? C104 C105 H10P 109.9 . . ? H10O C105 H10P 108.3 . . ? C109 C108 C107 116(2) . . ? C109 C108 H10Q 108.3 . . ? C107 C108 H10Q 108.3 . . ? C109 C108 H10R 108.3 . . ? C107 C108 H10R 108.3 . . ? H10Q C108 H10R 107.4 . . ? C108 C107 H10S 109.5 . . ? C108 C107 H10T 109.4 . . ? H10S C107 H10T 109.5 . . ? C108 C107 H10U 109.5 . . ? H10S C107 H10U 109.5 . . ? H10T C107 H10U 109.5 . . ? C108 C109 C109 116(5) . 3_566 ? C108 C109 H10V 108.3 . . ? C109 C109 H10V 108.3 3_566 . ? C108 C109 H10W 108.4 . . ? C109 C109 H10W 108.4 3_566 . ? H10V C109 H10W 107.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.8(4) . . . . ? C21 C1 C2 C3 -179.8(3) . . . . ? N1 C1 C2 C29 178.5(3) . . . . ? C21 C1 C2 C29 -2.1(5) . . . . ? C1 C2 C3 C4 -2.3(4) . . . . ? C29 C2 C3 C4 -180.0(3) . . . . ? C1 C2 C3 C30 -179.7(3) . . . . ? C29 C2 C3 C30 2.6(6) . . . . ? C2 C3 C4 N1 3.1(4) . . . . ? C30 C3 C4 N1 -179.4(3) . . . . ? C2 C3 C4 C5 -173.3(3) . . . . ? C30 C3 C4 C5 4.1(5) . . . . ? N1 C4 C5 C6 -6.3(5) . . . . ? C3 C4 C5 C6 169.6(3) . . . . ? C4 C5 C6 N2 -1.2(5) . . . . ? C4 C5 C6 C7 -178.4(3) . . . . ? C5 C6 C7 C8 177.7(3) . . . . ? N2 C6 C7 C8 0.1(3) . . . . ? C5 C6 C7 C32 -4.4(5) . . . . ? N2 C6 C7 C32 178.0(3) . . . . ? C6 C7 C8 C9 0.1(3) . . . . ? C32 C7 C8 C9 -177.6(3) . . . . ? C6 C7 C8 C13 177.9(4) . . . . ? C32 C7 C8 C13 0.2(6) . . . . ? C7 C8 C9 N2 -0.4(3) . . . . ? C13 C8 C9 N2 -178.6(3) . . . . ? C7 C8 C9 C10 -179.2(3) . . . . ? C13 C8 C9 C10 2.6(4) . . . . ? N2 C9 C10 C11 148.6(3) . . . . ? C8 C9 C10 C11 -32.7(4) . . . . ? C9 C10 C11 C12 44.6(3) . . . . ? C10 C11 C12 N3 149.4(3) . . . . ? C10 C11 C12 C13 -32.8(4) . . . . ? N3 C12 C13 C14 -1.1(4) . . . . ? C11 C12 C13 C14 -179.1(3) . . . . ? N3 C12 C13 C8 -179.2(3) . . . . ? C11 C12 C13 C8 2.9(4) . . . . ? C7 C8 C13 C14 18.9(7) . . . . ? C9 C8 C13 C14 -163.5(4) . . . . ? C7 C8 C13 C12 -163.9(3) . . . . ? C9 C8 C13 C12 13.7(4) . . . . ? C12 C13 C14 C15 1.5(4) . . . . ? C8 C13 C14 C15 178.9(4) . . . . ? C12 C13 C14 C33 -175.4(4) . . . . ? C8 C13 C14 C33 2.0(7) . . . . ? C13 C14 C15 C16 179.0(3) . . . . ? C33 C14 C15 C16 -3.8(6) . . . . ? C13 C14 C15 N3 -1.5(4) . . . . ? C33 C14 C15 N3 175.6(4) . . . . ? N3 C15 C16 C17 -5.5(6) . . . . ? C14 C15 C16 C17 173.9(3) . . . . ? C15 C16 C17 N4 -4.3(5) . . . . ? C15 C16 C17 C18 173.7(3) . . . . ? C16 C17 C18 C19 -177.3(3) . . . . ? N4 C17 C18 C19 0.9(4) . . . . ? C16 C17 C18 C34 4.7(5) . . . . ? N4 C17 C18 C34 -177.0(3) . . . . ? C17 C18 C19 C20 0.2(3) . . . . ? C34 C18 C19 C20 178.1(3) . . . . ? C17 C18 C19 C36 -177.7(3) . . . . ? C34 C18 C19 C36 0.2(6) . . . . ? C18 C19 C20 N4 -1.3(4) . . . . ? C36 C19 C20 N4 176.7(3) . . . . ? C18 C19 C20 C37 178.5(3) . . . . ? C36 C19 C20 C37 -3.6(5) . . . . ? N1 C1 C21 C22 -46.3(4) . . . . ? C2 C1 C21 C22 134.3(3) . . . . ? N1 C1 C21 C26 130.1(3) . . . . ? C2 C1 C21 C26 -49.3(5) . . . . ? C26 C21 C22 C23 -0.5(4) . . . . ? C1 C21 C22 C23 176.0(3) . . . . ? C21 C22 C23 C24 -0.3(5) . . . . ? C21 C22 C23 C27 179.3(3) . . . . ? C22 C23 C24 C25 0.2(5) . . . . ? C27 C23 C24 C25 -179.4(3) . . . . ? C23 C24 C25 C26 0.8(5) . . . . ? C23 C24 C25 C28 -178.6(3) . . . . ? C24 C25 C26 C21 -1.7(5) . . . . ? C28 C25 C26 C21 177.8(3) . . . . ? C22 C21 C26 C25 1.5(4) . . . . ? C1 C21 C26 C25 -175.0(3) . . . . ? C2 C3 C30 C31 76.4(4) . . . . ? C4 C3 C30 C31 -100.6(4) . . . . ? C19 C18 C34 C35 -93.5(4) . . . . ? C17 C18 C34 C35 84.0(4) . . . . ? N4 C20 C37 C38 -53.5(4) . . . . ? C19 C20 C37 C38 126.8(3) . . . . ? N4 C20 C37 C42 122.7(3) . . . . ? C19 C20 C37 C42 -57.1(4) . . . . ? C42 C37 C38 C39 0.6(4) . . . . ? C20 C37 C38 C39 176.8(3) . . . . ? C37 C38 C39 C40 -1.9(5) . . . . ? C37 C38 C39 C43 179.4(3) . . . . ? C38 C39 C40 C41 1.6(5) . . . . ? C43 C39 C40 C41 -179.7(3) . . . . ? C39 C40 C41 C42 0.1(5) . . . . ? C39 C40 C41 C44 -178.5(3) . . . . ? C40 C41 C42 C37 -1.5(5) . . . . ? C44 C41 C42 C37 177.1(3) . . . . ? C38 C37 C42 C41 1.2(4) . . . . ? C20 C37 C42 C41 -175.2(3) . . . . ? N5 C45 C46 C47 -1.3(4) . . . . ? C65 C45 C46 C47 178.2(3) . . . . ? N5 C45 C46 C73 176.5(3) . . . . ? C65 C45 C46 C73 -4.0(6) . . . . ? C45 C46 C47 C48 0.6(4) . . . . ? C73 C46 C47 C48 -177.1(4) . . . . ? C45 C46 C47 C74B 163.1(7) . . . . ? C73 C46 C47 C74B -14.6(9) . . . . ? C45 C46 C47 C74A -167.3(5) . . . . ? C73 C46 C47 C74A 15.0(8) . . . . ? C46 C47 C48 C49 -176.2(3) . . . . ? C74B C47 C48 C49 22.4(9) . . . . ? C74A C47 C48 C49 -7.3(7) . . . . ? C46 C47 C48 N5 0.1(4) . . . . ? C74B C47 C48 N5 -161.2(7) . . . . ? C74A C47 C48 N5 169.1(5) . . . . ? N5 C48 C49 C50 -5.3(6) . . . . ? C47 C48 C49 C50 170.5(4) . . . . ? C48 C49 C50 N6 -4.0(5) . . . . ? C48 C49 C50 C51 177.5(3) . . . . ? C49 C50 C51 C52 177.4(3) . . . . ? N6 C50 C51 C52 -1.3(3) . . . . ? C49 C50 C51 C76 -6.4(5) . . . . ? N6 C50 C51 C76 174.9(3) . . . . ? C50 C51 C52 C53 1.7(3) . . . . ? C76 C51 C52 C53 -174.3(3) . . . . ? C50 C51 C52 C57 -179.2(3) . . . . ? C76 C51 C52 C57 4.8(6) . . . . ? C51 C52 C53 N6 -1.6(3) . . . . ? C57 C52 C53 N6 179.1(2) . . . . ? C51 C52 C53 C54 179.3(3) . . . . ? C57 C52 C53 C54 0.0(4) . . . . ? N6 C53 C54 C55 150.0(2) . . . . ? C52 C53 C54 C55 -31.1(4) . . . . ? C53 C54 C55 C56 45.1(3) . . . 2 ? C51 C52 C57 C58 21.4(6) . . . . ? C53 C52 C57 C58 -159.6(3) . . . . ? C51 C52 C57 C56 -164.0(3) . . . 2 ? C53 C52 C57 C56 15.0(4) . . . 2 ? C56 C57 C58 C59 0.3(3) 2 . . 2 ? C52 C57 C58 C59 175.3(3) . . . 2 ? C56 C57 C58 C77 -177.5(3) 2 . . . ? C52 C57 C58 C77 -2.5(6) . . . . ? N7 C59 C60 C61 -1.9(5) . . . . ? C58 C59 C60 C61 175.4(3) 2 . . . ? C59 C60 C61 N8 -0.7(5) . . . . ? C59 C60 C61 C62 175.0(3) . . . . ? C60 C61 C62 C63 -174.4(3) . . . . ? N8 C61 C62 C63 1.8(4) . . . . ? C60 C61 C62 C78 8.4(6) . . . . ? N8 C61 C62 C78 -175.4(3) . . . . ? C61 C62 C63 C64 -1.3(4) . . . . ? C78 C62 C63 C64 175.7(4) . . . . ? C61 C62 C63 C80 -179.0(3) . . . . ? C78 C62 C63 C80 -1.9(6) . . . . ? C62 C63 C64 N8 0.4(4) . . . . ? C80 C63 C64 N8 178.1(3) . . . . ? C62 C63 C64 C81 -179.9(3) . . . . ? C80 C63 C64 C81 -2.2(6) . . . . ? N5 C45 C65 C66 -48.3(4) . . . . ? C46 C45 C65 C66 132.3(4) . . . . ? N5 C45 C65 C70 130.4(3) . . . . ? C46 C45 C65 C70 -49.0(5) . . . . ? C70 C65 C66 C67 -0.6(5) . . . . ? C45 C65 C66 C67 178.2(3) . . . . ? C65 C66 C67 C68 -1.2(6) . . . . ? C65 C66 C67 C71 -179.8(4) . . . . ? C66 C67 C68 C69 1.7(6) . . . . ? C71 C67 C68 C69 -179.6(4) . . . . ? C67 C68 C69 C70 -0.5(6) . . . . ? C67 C68 C69 C72 -177.5(4) . . . . ? C68 C69 C70 C65 -1.4(5) . . . . ? C72 C69 C70 C65 175.7(4) . . . . ? C66 C65 C70 C69 1.9(5) . . . . ? C45 C65 C70 C69 -176.9(3) . . . . ? C46 C47 C74A C75A -91.6(9) . . . . ? C48 C47 C74A C75A 102.1(8) . . . . ? C74B C47 C74A C75A -7.8(16) . . . . ? C63 C62 C78 C79 -101.3(5) . . . . ? C61 C62 C78 C79 75.2(5) . . . . ? N8 C64 C81 C86 -41.3(4) . . . . ? C63 C64 C81 C86 139.0(3) . . . . ? N8 C64 C81 C82 136.4(3) . . . . ? C63 C64 C81 C82 -43.3(5) . . . . ? C86 C81 C82 C83 1.2(5) . . . . ? C64 C81 C82 C83 -176.6(3) . . . . ? C81 C82 C83 C84 -0.4(5) . . . . ? C81 C82 C83 C87 178.3(3) . . . . ? C82 C83 C84 C85 -0.4(6) . . . . ? C87 C83 C84 C85 -179.2(4) . . . . ? C83 C84 C85 C86 0.5(6) . . . . ? C83 C84 C85 C88 -179.8(4) . . . . ? C84 C85 C86 C81 0.3(5) . . . . ? C88 C85 C86 C81 -179.4(3) . . . . ? C82 C81 C86 C85 -1.1(5) . . . . ? C64 C81 C86 C85 176.7(3) . . . . ? C2 C1 N1 C4 1.2(3) . . . . ? C21 C1 N1 C4 -178.3(3) . . . . ? C2 C1 N1 Zn2 166.4(2) . . . . ? C21 C1 N1 Zn2 -13.1(4) . . . . ? C5 C4 N1 C1 173.9(3) . . . . ? C3 C4 N1 C1 -2.6(3) . . . . ? C5 C4 N1 Zn2 7.6(4) . . . . ? C3 C4 N1 Zn2 -168.92(19) . . . . ? C8 C9 N2 C6 0.5(3) . . . . ? C10 C9 N2 C6 179.2(3) . . . . ? C8 C9 N2 Zn2 176.20(19) . . . . ? C10 C9 N2 Zn2 -5.0(4) . . . . ? C5 C6 N2 C9 -178.0(3) . . . . ? C7 C6 N2 C9 -0.4(3) . . . . ? C5 C6 N2 Zn2 5.8(4) . . . . ? C7 C6 N2 Zn2 -176.56(19) . . . . ? C13 C12 N3 C15 0.2(3) . . . . ? C11 C12 N3 C15 178.2(3) . . . . ? C13 C12 N3 Zn1 165.62(19) . . . . ? C11 C12 N3 Zn1 -16.4(4) . . . . ? C16 C15 N3 C12 -179.7(3) . . . . ? C14 C15 N3 C12 0.8(3) . . . . ? C16 C15 N3 Zn1 13.5(4) . . . . ? C14 C15 N3 Zn1 -166.0(2) . . . . ? C19 C20 N4 C17 1.8(3) . . . . ? C37 C20 N4 C17 -178.0(2) . . . . ? C19 C20 N4 Zn1 173.5(2) . . . . ? C37 C20 N4 Zn1 -6.3(4) . . . . ? C16 C17 N4 C20 176.6(3) . . . . ? C18 C17 N4 C20 -1.7(3) . . . . ? C16 C17 N4 Zn1 4.1(4) . . . . ? C18 C17 N4 Zn1 -174.17(19) . . . . ? C46 C45 N5 C48 1.3(3) . . . . ? C65 C45 N5 C48 -178.2(3) . . . . ? C46 C45 N5 Zn1 173.5(2) . . . . ? C65 C45 N5 Zn1 -6.1(4) . . . . ? C49 C48 N5 C45 175.5(3) . . . . ? C47 C48 N5 C45 -0.9(4) . . . . ? C49 C48 N5 Zn1 2.5(4) . . . . ? C47 C48 N5 Zn1 -173.9(2) . . . . ? C52 C53 N6 C50 0.8(3) . . . . ? C54 C53 N6 C50 179.9(2) . . . . ? C52 C53 N6 Zn1 166.98(17) . . . . ? C54 C53 N6 Zn1 -13.9(4) . . . . ? C49 C50 N6 C53 -178.4(3) . . . . ? C51 C50 N6 C53 0.3(3) . . . . ? C49 C50 N6 Zn1 13.9(4) . . . . ? C51 C50 N6 Zn1 -167.36(18) . . . . ? C57 C56 N7 C59 0.7(3) 2 . . . ? C55 C56 N7 C59 -179.6(2) 2 . . . ? C57 C56 N7 Zn2 175.54(17) 2 . . . ? C55 C56 N7 Zn2 -4.8(4) 2 . . . ? C60 C59 N7 C56 177.2(3) . . . . ? C58 C59 N7 C56 -0.5(3) 2 . . . ? C60 C59 N7 Zn2 1.8(4) . . . . ? C58 C59 N7 Zn2 -175.94(18) 2 . . . ? C63 C64 N8 C61 0.7(3) . . . . ? C81 C64 N8 C61 -179.0(3) . . . . ? C63 C64 N8 Zn2 171.6(2) . . . . ? C81 C64 N8 Zn2 -8.1(4) . . . . ? C60 C61 N8 C64 174.8(3) . . . . ? C62 C61 N8 C64 -1.5(3) . . . . ? C60 C61 N8 Zn2 2.8(4) . . . . ? C62 C61 N8 Zn2 -173.5(2) . . . . ? C45 N5 Zn1 N3 -36.8(3) . . . . ? C48 N5 Zn1 N3 134.3(2) . . . . ? C45 N5 Zn1 N6 -166.0(2) . . . . ? C48 N5 Zn1 N6 5.0(2) . . . . ? C45 N5 Zn1 N4 76.0(3) . . . . ? C48 N5 Zn1 N4 -113.0(2) . . . . ? C12 N3 Zn1 N5 -42.9(2) . . . . ? C15 N3 Zn1 N5 120.5(2) . . . . ? C12 N3 Zn1 N6 69.2(3) . . . . ? C15 N3 Zn1 N6 -127.5(2) . . . . ? C12 N3 Zn1 N4 -174.0(2) . . . . ? C15 N3 Zn1 N4 -10.7(2) . . . . ? C53 N6 Zn1 N5 -177.1(2) . . . . ? C50 N6 Zn1 N5 -12.8(2) . . . . ? C53 N6 Zn1 N3 64.5(2) . . . . ? C50 N6 Zn1 N3 -131.19(19) . . . . ? C53 N6 Zn1 N4 -46.2(2) . . . . ? C50 N6 Zn1 N4 118.2(2) . . . . ? C20 N4 Zn1 N5 73.0(3) . . . . ? C17 N4 Zn1 N5 -116.6(2) . . . . ? C20 N4 Zn1 N3 -168.0(2) . . . . ? C17 N4 Zn1 N3 2.4(2) . . . . ? C20 N4 Zn1 N6 -39.4(3) . . . . ? C17 N4 Zn1 N6 131.1(2) . . . . ? C1 N1 Zn2 N8 -36.0(3) . . . . ? C4 N1 Zn2 N8 127.0(2) . . . . ? C1 N1 Zn2 N7 80.6(3) . . . . ? C4 N1 Zn2 N7 -116.4(2) . . . . ? C1 N1 Zn2 N2 -165.8(2) . . . . ? C4 N1 Zn2 N2 -2.8(2) . . . . ? C64 N8 Zn2 N1 -39.9(3) . . . . ? C61 N8 Zn2 N1 129.8(2) . . . . ? C64 N8 Zn2 N7 -171.9(3) . . . . ? C61 N8 Zn2 N7 -2.2(2) . . . . ? C64 N8 Zn2 N2 74.3(3) . . . . ? C61 N8 Zn2 N2 -116.0(2) . . . . ? C56 N7 Zn2 N1 62.1(3) . . . . ? C59 N7 Zn2 N1 -123.7(2) . . . . ? C56 N7 Zn2 N8 -174.1(2) . . . . ? C59 N7 Zn2 N8 0.0(2) . . . . ? C56 N7 Zn2 N2 -46.8(2) . . . . ? C59 N7 Zn2 N2 127.3(2) . . . . ? C9 N2 Zn2 N1 -178.6(2) . . . . ? C6 N2 Zn2 N1 -3.5(2) . . . . ? C9 N2 Zn2 N8 59.2(3) . . . . ? C6 N2 Zn2 N8 -125.7(2) . . . . ? C9 N2 Zn2 N7 -50.4(3) . . . . ? C6 N2 Zn2 N7 124.8(2) . . . . ? C46 C47 C74B C75B 87.8(9) . . . . ? C48 C47 C74B C75B -113.5(8) . . . . ? C74A C47 C74B C75B -26.1(17) . . . . ? C90 C91 C92 C92 137.9(7) . . . 2_655 ? C93 C94 C95 C96 -176.3(9) . . . . ? C94 C95 C96 C97 173.6(9) . . . . ? C95 C96 C97 C98 173.6(8) . . . . ? C101 C102 C103 C104 179.2(14) . . . . ? C102 C103 C104 C105 176.5(16) . . . . ? C103 C104 C105 C106 178.0(17) . . . . ? C107 C108 C109 C109 -163(6) . . . 3_566 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.93 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.821 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.073 #===End data_hexagon_11 _database_code_depnum_ccdc_archive 'CCDC 791801' #TrackingRef '- grid 9 & hexagon 11 revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C243.24 H219.24 Cl9.72 F12 N24 Zn6' _chemical_formula_weight 4443.34 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 24.2358(14) _cell_length_b 24.2358(14) _cell_length_c 11.8480(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6026.8(6) _cell_formula_units_Z 1 _cell_measurement_temperature 103.0(1) _cell_measurement_reflns_used 9995 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 25.01 _exptl_crystal_description tablet _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2286 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.799 _exptl_absorpt_correction_T_max 0.920 _exptl_absorpt_process_details 'SADABS (Bruker-AXS, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 103.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50775 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.06 _reflns_number_total 7126 _reflns_number_gt 5647 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'APEX2 (Bruker-AXS, 2009)' _computing_data_reduction 'APEX2 (Bruker-AXS, 2009)' _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WINGX (Farrugia, 1999)' _refine_special_details ; The material crystallizes with one partially occupied site containing chloroform. Refining this molecules population gave a value of 0.54. 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^)+(0.0896P)^2^+13.1370P] 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 7126 _refine_ls_number_parameters 467 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1862 _refine_ls_wR_factor_gt 0.1711 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.38300(19) -0.04713(18) 0.4564(4) 0.0327(9) Uani 1 1 d . . . C2 C 0.3777(2) -0.08541(19) 0.3619(4) 0.0366(10) Uani 1 1 d . . . C3 C 0.3630(2) -0.0606(2) 0.2700(4) 0.0371(10) Uani 1 1 d . . . C4 C 0.3582(2) -0.00769(19) 0.3109(4) 0.0339(9) Uani 1 1 d . . . C5 C 0.3391(2) 0.0292(2) 0.2502(4) 0.0363(9) Uani 1 1 d . . . H5 H 0.3318 0.0193 0.1720 0.044 Uiso 1 1 calc R . . C6 C 0.3291(2) 0.07771(19) 0.2857(3) 0.0344(9) Uani 1 1 d . . . C7 C 0.3108(2) 0.1154(2) 0.2195(4) 0.0375(10) Uani 1 1 d . . . C8 C 0.3109(2) 0.1601(2) 0.2922(3) 0.0344(9) Uani 1 1 d . . . C9 C 0.32633(19) 0.14651(19) 0.4012(3) 0.0310(9) Uani 1 1 d . . . C10 C 0.3309(2) 0.1833(2) 0.5049(3) 0.0367(10) Uani 1 1 d . . . H10A H 0.3753 0.2186 0.5140 0.044 Uiso 1 1 calc R . . H10B H 0.3200 0.1551 0.5716 0.044 Uiso 1 1 calc R . . C11 C 0.2860(2) 0.2104(2) 0.4989(4) 0.0418(11) Uani 1 1 d . . . H11A H 0.2416 0.1759 0.5117 0.050 Uiso 1 1 calc R . . H11B H 0.2973 0.2429 0.5586 0.050 Uiso 1 1 calc R . . C12 C 0.2910(2) 0.2396(2) 0.3869(3) 0.0340(9) Uani 1 1 d . . . C13 C 0.2996(2) 0.2137(2) 0.2833(3) 0.0346(9) Uani 1 1 d . . . C14 C 0.3015(2) 0.2536(2) 0.1985(4) 0.0367(10) Uani 1 1 d . . . C15 C 0.29469(19) 0.3027(2) 0.2520(3) 0.0326(9) Uani 1 1 d . . . C16 C 0.2989(2) 0.3563(2) 0.2025(4) 0.0365(10) Uani 1 1 d . . . H16 H 0.2998 0.3565 0.1223 0.044 Uiso 1 1 calc R . . C17 C 0.30210(18) 0.4098(2) 0.2515(3) 0.0322(9) Uani 1 1 d . . . C18 C 0.30549(19) 0.4630(2) 0.1932(4) 0.0385(10) Uani 1 1 d . . . C19 C 0.30898(19) 0.5051(2) 0.2732(4) 0.0388(10) Uani 1 1 d . . . C20 C 0.30780(18) 0.4781(2) 0.3798(4) 0.0357(10) Uani 1 1 d . . . C21 C 0.3954(2) -0.05478(19) 0.5745(4) 0.0339(9) Uani 1 1 d . . . C22 C 0.4489(2) -0.0084(2) 0.6298(4) 0.0411(10) Uani 1 1 d . . . H22 H 0.4795 0.0277 0.5887 0.049 Uiso 1 1 calc R . . C23 C 0.4589(3) -0.0132(2) 0.7431(4) 0.0486(12) Uani 1 1 d . . . H23 H 0.4958 0.0187 0.7804 0.058 Uiso 1 1 calc R . . C24 C 0.4137(3) -0.0656(3) 0.8000(4) 0.0520(13) Uani 1 1 d . . . C25 C 0.3616(3) -0.1127(3) 0.7498(5) 0.0577(14) Uani 1 1 d . . . H25 H 0.3316 -0.1487 0.7918 0.069 Uiso 1 1 calc R . . C26 C 0.3523(2) -0.1075(2) 0.6349(4) 0.0477(12) Uani 1 1 d . . . H26 H 0.3161 -0.1407 0.5980 0.057 Uiso 1 1 calc R . . C27 C 0.3915(2) -0.1396(2) 0.3618(4) 0.0443(11) Uani 1 1 d . . . H27A H 0.3557 -0.1772 0.3271 0.066 Uiso 1 1 calc R . . H27B H 0.3972 -0.1495 0.4396 0.066 Uiso 1 1 calc R . . H27C H 0.4304 -0.1272 0.3186 0.066 Uiso 1 1 calc R . . C28 C 0.3511(3) -0.0863(2) 0.1520(4) 0.0480(12) Uani 1 1 d . . . H28A H 0.3823 -0.0999 0.1329 0.058 Uiso 1 1 calc R . . H28B H 0.3573 -0.0523 0.0987 0.058 Uiso 1 1 calc R . . C29 C 0.2843(3) -0.1423(2) 0.1390(5) 0.0726(19) Uani 1 1 d . . . H29A H 0.2777 -0.1757 0.1929 0.109 Uiso 1 1 calc R . . H29B H 0.2785 -0.1591 0.0620 0.109 Uiso 1 1 calc R . . H29C H 0.2533 -0.1284 0.1536 0.109 Uiso 1 1 calc R . . C30 C 0.2926(3) 0.1035(3) 0.0972(4) 0.0538(13) Uani 1 1 d . . . H30A H 0.2579 0.1121 0.0824 0.081 Uiso 1 1 calc R . . H30B H 0.2786 0.0590 0.0788 0.081 Uiso 1 1 calc R . . H30C H 0.3295 0.1317 0.0506 0.081 Uiso 1 1 calc R . . C31 C 0.3139(3) 0.2515(3) 0.0755(4) 0.0557(14) Uani 1 1 d . . . H31A H 0.3452 0.2375 0.0655 0.084 Uiso 1 1 calc R . . H31B H 0.3306 0.2940 0.0428 0.084 Uiso 1 1 calc R . . H31C H 0.2741 0.2215 0.0375 0.084 Uiso 1 1 calc R . . C32 C 0.3084(2) 0.4711(3) 0.0671(4) 0.0496(12) Uani 1 1 d . . . H32A H 0.2930 0.5006 0.0466 0.060 Uiso 1 1 calc R . . H32B H 0.2797 0.4294 0.0314 0.060 Uiso 1 1 calc R . . C33 C 0.3751(3) 0.4967(4) 0.0217(5) 0.089(2) Uani 1 1 d . . . H33A H 0.4037 0.5380 0.0569 0.134 Uiso 1 1 calc R . . H33B H 0.3749 0.5021 -0.0603 0.134 Uiso 1 1 calc R . . H33C H 0.3899 0.4667 0.0390 0.134 Uiso 1 1 calc R . . C34 C 0.3163(2) 0.5697(2) 0.2511(5) 0.0501(12) Uani 1 1 d . . . H34A H 0.3442 0.5892 0.1857 0.075 Uiso 1 1 calc R . . H34B H 0.3351 0.5969 0.3175 0.075 Uiso 1 1 calc R . . H34C H 0.2744 0.5650 0.2358 0.075 Uiso 1 1 calc R . . C35 C 0.31146(19) 0.5045(2) 0.4923(4) 0.0391(10) Uani 1 1 d . . . C36 C 0.2775(2) 0.5351(2) 0.5195(5) 0.0539(13) Uani 1 1 d . . . H36 H 0.2524 0.5400 0.4631 0.065 Uiso 1 1 calc R . . C37 C 0.2797(3) 0.5585(3) 0.6269(6) 0.0656(16) Uani 1 1 d . . . H37 H 0.2566 0.5797 0.6441 0.079 Uiso 1 1 calc R . . C38 C 0.3154(3) 0.5507(3) 0.7078(5) 0.0625(15) Uani 1 1 d . . . C39 C 0.3502(2) 0.5224(2) 0.6855(5) 0.0524(12) Uani 1 1 d . . . H39 H 0.3755 0.5184 0.7426 0.063 Uiso 1 1 calc R . . C40 C 0.3481(2) 0.4993(2) 0.5775(4) 0.0422(11) Uani 1 1 d . . . H40 H 0.3725 0.4794 0.5613 0.051 Uiso 1 1 calc R . . C41 C 0.1322(7) 0.1873(8) 0.2317(13) 0.106(5) Uani 0.546(6) 1 d P . . H41 H 0.1789 0.2189 0.2362 0.127 Uiso 0.546(6) 1 calc PR . . N1 N 0.37169(16) -0.00046(15) 0.4249(3) 0.0320(7) Uani 1 1 d . . . N2 N 0.33703(16) 0.09838(16) 0.3973(3) 0.0328(8) Uani 1 1 d . . . N3 N 0.28807(16) 0.29161(16) 0.3677(3) 0.0330(8) Uani 1 1 d . . . N4 N 0.30395(15) 0.42095(16) 0.3663(3) 0.0325(8) Uani 1 1 d . . . F1 F 0.42225(19) -0.06915(19) 0.9130(3) 0.0788(11) Uani 1 1 d . . . F2 F 0.3161(2) 0.57228(19) 0.8140(3) 0.0929(12) Uani 1 1 d . . . Zn1 Zn 0.35860(2) 0.05864(2) 0.52238(4) 0.02991(17) Uani 1 1 d . . . Cl1 Cl 0.0974(3) 0.2288(3) 0.2085(4) 0.154(3) Uani 0.546(6) 1 d P . . Cl2 Cl 0.1236(4) 0.1376(4) 0.1228(7) 0.209(4) Uani 0.546(6) 1 d P . . Cl3 Cl 0.1135(4) 0.1440(5) 0.3549(8) 0.247(5) Uani 0.546(6) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.035(2) 0.026(2) 0.038(2) 0.0012(17) -0.0036(17) 0.0156(18) C2 0.040(2) 0.026(2) 0.043(3) -0.0059(18) -0.0040(19) 0.0157(18) C3 0.038(2) 0.032(2) 0.041(3) -0.0058(18) -0.0028(19) 0.0177(19) C4 0.039(2) 0.028(2) 0.035(2) -0.0065(17) -0.0058(18) 0.0165(18) C5 0.044(2) 0.035(2) 0.030(2) -0.0042(17) -0.0053(18) 0.020(2) C6 0.043(2) 0.032(2) 0.029(2) -0.0014(17) -0.0066(18) 0.0207(19) C7 0.045(2) 0.042(2) 0.030(2) -0.0010(18) -0.0039(18) 0.026(2) C8 0.042(2) 0.036(2) 0.029(2) 0.0025(17) 0.0007(18) 0.0219(19) C9 0.036(2) 0.030(2) 0.028(2) 0.0020(16) -0.0014(16) 0.0172(18) C10 0.049(3) 0.036(2) 0.031(2) 0.0060(18) 0.0008(19) 0.026(2) C11 0.062(3) 0.044(3) 0.032(2) 0.0069(19) 0.007(2) 0.035(2) C12 0.039(2) 0.036(2) 0.032(2) 0.0054(18) 0.0019(18) 0.0236(19) C13 0.040(2) 0.040(2) 0.033(2) 0.0064(18) 0.0018(18) 0.027(2) C14 0.043(2) 0.047(2) 0.029(2) 0.0064(18) 0.0027(18) 0.029(2) C15 0.035(2) 0.043(2) 0.027(2) 0.0073(17) 0.0046(17) 0.0249(19) C16 0.038(2) 0.049(3) 0.030(2) 0.0110(19) 0.0038(17) 0.027(2) C17 0.029(2) 0.039(2) 0.032(2) 0.0122(17) 0.0053(16) 0.0201(18) C18 0.027(2) 0.042(2) 0.046(3) 0.014(2) -0.0001(18) 0.0170(19) C19 0.026(2) 0.037(2) 0.054(3) 0.011(2) -0.0035(19) 0.0157(18) C20 0.0214(19) 0.035(2) 0.052(3) 0.0091(19) 0.0007(18) 0.0147(17) C21 0.043(2) 0.030(2) 0.036(2) -0.0017(17) 0.0010(18) 0.0237(19) C22 0.049(3) 0.036(2) 0.036(3) 0.0015(19) -0.003(2) 0.021(2) C23 0.060(3) 0.051(3) 0.040(3) -0.001(2) -0.008(2) 0.031(3) C24 0.072(4) 0.068(3) 0.036(3) 0.010(2) 0.001(2) 0.050(3) C25 0.058(3) 0.061(3) 0.058(3) 0.028(3) 0.014(3) 0.033(3) C26 0.049(3) 0.042(3) 0.055(3) 0.008(2) -0.002(2) 0.024(2) C27 0.053(3) 0.035(2) 0.051(3) -0.004(2) -0.001(2) 0.027(2) C28 0.067(3) 0.044(3) 0.042(3) -0.011(2) -0.010(2) 0.034(3) C29 0.107(5) 0.037(3) 0.056(4) -0.010(2) -0.039(3) 0.023(3) C30 0.086(4) 0.061(3) 0.035(3) -0.008(2) -0.016(2) 0.052(3) C31 0.093(4) 0.070(3) 0.029(3) 0.010(2) 0.007(2) 0.059(3) C32 0.048(3) 0.055(3) 0.049(3) 0.022(2) 0.000(2) 0.028(2) C33 0.066(4) 0.156(7) 0.046(4) 0.043(4) 0.017(3) 0.054(5) C34 0.039(3) 0.037(2) 0.074(4) 0.015(2) -0.008(2) 0.018(2) C35 0.026(2) 0.030(2) 0.056(3) 0.0042(19) 0.0019(19) 0.0097(17) C36 0.045(3) 0.048(3) 0.075(4) -0.009(3) -0.007(2) 0.027(2) C37 0.061(3) 0.052(3) 0.091(5) -0.020(3) 0.001(3) 0.034(3) C38 0.062(3) 0.051(3) 0.065(4) -0.014(3) 0.001(3) 0.021(3) C39 0.053(3) 0.045(3) 0.057(3) 0.000(2) 0.000(2) 0.022(2) C40 0.043(3) 0.041(2) 0.047(3) 0.009(2) 0.006(2) 0.024(2) C41 0.073(9) 0.111(12) 0.100(11) -0.006(9) -0.014(8) 0.021(9) N1 0.0383(19) 0.0249(16) 0.0331(19) -0.0047(14) -0.0055(15) 0.0162(15) N2 0.0395(19) 0.0310(18) 0.0311(19) 0.0009(14) -0.0051(15) 0.0200(16) N3 0.0385(19) 0.0381(19) 0.0285(19) 0.0077(14) 0.0066(14) 0.0238(16) N4 0.0288(17) 0.0356(18) 0.039(2) 0.0110(15) 0.0050(14) 0.0208(15) F1 0.107(3) 0.111(3) 0.0411(18) 0.0195(18) 0.0016(17) 0.072(3) F2 0.111(3) 0.091(3) 0.082(3) -0.038(2) -0.008(2) 0.054(3) Zn1 0.0367(3) 0.0223(2) 0.0303(3) -0.00320(18) -0.00828(19) 0.0144(2) Cl1 0.198(6) 0.190(6) 0.088(3) -0.017(3) -0.011(3) 0.107(5) Cl2 0.197(8) 0.185(7) 0.226(8) -0.044(6) -0.031(6) 0.081(6) Cl3 0.135(6) 0.313(12) 0.237(9) 0.101(8) 0.013(6) 0.071(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.343(5) . ? C1 C2 1.418(6) . ? C1 C21 1.463(6) . ? C2 C3 1.373(6) . ? C2 C27 1.508(6) . ? C3 C4 1.429(6) . ? C3 C28 1.499(6) . ? C4 N1 1.380(5) . ? C4 C5 1.395(6) . ? C5 C6 1.380(6) . ? C5 H5 0.9500 . ? C6 N2 1.393(5) . ? C6 C7 1.433(6) . ? C7 C8 1.383(6) . ? C7 C30 1.499(6) . ? C8 C9 1.429(6) . ? C8 C13 1.460(6) . ? C9 N2 1.316(5) . ? C9 C10 1.488(6) . ? C10 C11 1.528(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.481(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N3 1.317(5) . ? C12 C13 1.439(6) . ? C13 C14 1.379(6) . ? C14 C15 1.429(6) . ? C14 C31 1.494(6) . ? C15 C16 1.381(6) . ? C15 N3 1.390(5) . ? C16 C17 1.388(6) . ? C16 H16 0.9500 . ? C17 N4 1.383(5) . ? C17 C18 1.428(6) . ? C18 C19 1.364(7) . ? C18 C32 1.503(7) . ? C19 C20 1.416(6) . ? C19 C34 1.508(6) . ? C20 N4 1.349(5) . ? C20 C35 1.463(7) . ? C21 C26 1.379(6) . ? C21 C22 1.385(6) . ? C22 C23 1.379(6) . ? C22 H22 0.9500 . ? C23 C24 1.370(7) . ? C23 H23 0.9500 . ? C24 C25 1.346(8) . ? C24 F1 1.363(6) . ? C25 C26 1.396(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.513(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.512(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.392(6) . ? C35 C40 1.393(6) . ? C36 C37 1.384(8) . ? C36 H36 0.9500 . ? C37 C38 1.366(9) . ? C37 H37 0.9500 . ? C38 C39 1.354(8) . ? C38 F2 1.359(6) . ? C39 C40 1.387(7) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 Cl1 1.629(19) . ? C41 Cl2 1.705(18) . ? C41 Cl3 1.721(17) . ? C41 H41 1.0000 . ? N1 Zn1 1.985(3) . ? N2 Zn1 1.975(3) . ? N3 Zn1 1.987(3) 6_556 ? N4 Zn1 1.971(3) 6_556 ? Zn1 N4 1.971(3) 5_556 ? Zn1 N3 1.987(3) 5_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 110.0(4) . . ? N1 C1 C21 120.9(4) . . ? C2 C1 C21 129.0(4) . . ? C3 C2 C1 107.4(4) . . ? C3 C2 C27 126.8(4) . . ? C1 C2 C27 125.6(4) . . ? C2 C3 C4 106.2(4) . . ? C2 C3 C28 126.6(4) . . ? C4 C3 C28 127.2(4) . . ? N1 C4 C5 123.8(4) . . ? N1 C4 C3 109.0(4) . . ? C5 C4 C3 127.0(4) . . ? C6 C5 C4 130.1(4) . . ? C6 C5 H5 114.9 . . ? C4 C5 H5 114.9 . . ? C5 C6 N2 123.0(4) . . ? C5 C6 C7 128.2(4) . . ? N2 C6 C7 108.8(3) . . ? C8 C7 C6 106.2(4) . . ? C8 C7 C30 129.6(4) . . ? C6 C7 C30 124.2(4) . . ? C7 C8 C9 106.3(4) . . ? C7 C8 C13 136.5(4) . . ? C9 C8 C13 117.2(4) . . ? N2 C9 C8 111.3(4) . . ? N2 C9 C10 124.8(4) . . ? C8 C9 C10 123.9(4) . . ? C9 C10 C11 111.3(4) . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 110.0(4) . . ? C12 C11 H11A 109.7 . . ? C10 C11 H11A 109.7 . . ? C12 C11 H11B 109.7 . . ? C10 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? N3 C12 C13 111.0(4) . . ? N3 C12 C11 125.6(4) . . ? C13 C12 C11 123.4(4) . . ? C14 C13 C12 106.1(4) . . ? C14 C13 C8 136.1(4) . . ? C12 C13 C8 117.3(4) . . ? C13 C14 C15 106.4(4) . . ? C13 C14 C31 128.6(4) . . ? C15 C14 C31 124.8(4) . . ? C16 C15 N3 123.2(4) . . ? C16 C15 C14 127.5(4) . . ? N3 C15 C14 109.1(3) . . ? C15 C16 C17 130.1(4) . . ? C15 C16 H16 114.9 . . ? C17 C16 H16 114.9 . . ? N4 C17 C16 125.1(4) . . ? N4 C17 C18 108.5(4) . . ? C16 C17 C18 126.3(4) . . ? C19 C18 C17 107.0(4) . . ? C19 C18 C32 127.7(4) . . ? C17 C18 C32 125.2(4) . . ? C18 C19 C20 107.1(4) . . ? C18 C19 C34 125.9(4) . . ? C20 C19 C34 126.8(4) . . ? N4 C20 C19 110.1(4) . . ? N4 C20 C35 121.0(4) . . ? C19 C20 C35 128.8(4) . . ? C26 C21 C22 118.4(4) . . ? C26 C21 C1 120.4(4) . . ? C22 C21 C1 121.2(4) . . ? C23 C22 C21 121.6(4) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C24 C23 C22 117.7(5) . . ? C24 C23 H23 121.1 . . ? C22 C23 H23 121.1 . . ? C25 C24 F1 119.2(5) . . ? C25 C24 C23 123.0(5) . . ? F1 C24 C23 117.8(5) . . ? C24 C25 C26 118.7(5) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? C21 C26 C25 120.5(5) . . ? C21 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C2 C27 H27A 109.5 . . ? C2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C3 C28 C29 111.4(4) . . ? C3 C28 H28A 109.3 . . ? C29 C28 H28A 109.3 . . ? C3 C28 H28B 109.3 . . ? C29 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C7 C30 H30A 109.5 . . ? C7 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C7 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C14 C31 H31A 109.5 . . ? C14 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C14 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C18 C32 C33 112.2(4) . . ? C18 C32 H32A 109.2 . . ? C33 C32 H32A 109.2 . . ? C18 C32 H32B 109.2 . . ? C33 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C19 C34 H34A 109.5 . . ? C19 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C19 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 117.0(5) . . ? C36 C35 C20 121.5(4) . . ? C40 C35 C20 121.5(4) . . ? C37 C36 C35 121.4(5) . . ? C37 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C38 C37 C36 119.0(5) . . ? C38 C37 H37 120.5 . . ? C36 C37 H37 120.5 . . ? C39 C38 F2 119.0(6) . . ? C39 C38 C37 122.1(5) . . ? F2 C38 C37 118.9(5) . . ? C38 C39 C40 118.6(5) . . ? C38 C39 H39 120.7 . . ? C40 C39 H39 120.7 . . ? C39 C40 C35 121.9(4) . . ? C39 C40 H40 119.1 . . ? C35 C40 H40 119.1 . . ? Cl1 C41 Cl2 113.0(10) . . ? Cl1 C41 Cl3 117.4(11) . . ? Cl2 C41 Cl3 108.0(11) . . ? Cl1 C41 H41 105.9 . . ? Cl2 C41 H41 105.9 . . ? Cl3 C41 H41 105.9 . . ? C1 N1 C4 107.4(3) . . ? C1 N1 Zn1 128.3(3) . . ? C4 N1 Zn1 123.3(3) . . ? C9 N2 C6 107.4(3) . . ? C9 N2 Zn1 128.6(3) . . ? C6 N2 Zn1 124.0(3) . . ? C12 N3 C15 107.4(3) . . ? C12 N3 Zn1 127.8(3) . 6_556 ? C15 N3 Zn1 122.2(3) . 6_556 ? C20 N4 C17 107.2(3) . . ? C20 N4 Zn1 131.2(3) . 6_556 ? C17 N4 Zn1 121.6(3) . 6_556 ? N4 Zn1 N2 116.54(14) 5_556 . ? N4 Zn1 N1 124.42(14) 5_556 . ? N2 Zn1 N1 95.30(14) . . ? N4 Zn1 N3 96.85(14) 5_556 5_556 ? N2 Zn1 N3 119.54(14) . 5_556 ? N1 Zn1 N3 105.55(14) . 5_556 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.4(5) . . . . ? C21 C1 C2 C3 177.3(4) . . . . ? N1 C1 C2 C27 175.5(4) . . . . ? C21 C1 C2 C27 -7.5(7) . . . . ? C1 C2 C3 C4 -1.2(5) . . . . ? C27 C2 C3 C4 -176.2(4) . . . . ? C1 C2 C3 C28 -178.3(4) . . . . ? C27 C2 C3 C28 6.6(8) . . . . ? C2 C3 C4 N1 1.6(5) . . . . ? C28 C3 C4 N1 178.7(4) . . . . ? C2 C3 C4 C5 -174.4(4) . . . . ? C28 C3 C4 C5 2.8(8) . . . . ? N1 C4 C5 C6 -0.6(8) . . . . ? C3 C4 C5 C6 174.8(5) . . . . ? C4 C5 C6 N2 -0.4(8) . . . . ? C4 C5 C6 C7 178.4(5) . . . . ? C5 C6 C7 C8 -176.3(4) . . . . ? N2 C6 C7 C8 2.7(5) . . . . ? C5 C6 C7 C30 6.4(8) . . . . ? N2 C6 C7 C30 -174.6(4) . . . . ? C6 C7 C8 C9 -2.6(5) . . . . ? C30 C7 C8 C9 174.5(5) . . . . ? C6 C7 C8 C13 177.5(5) . . . . ? C30 C7 C8 C13 -5.4(9) . . . . ? C7 C8 C9 N2 1.8(5) . . . . ? C13 C8 C9 N2 -178.3(4) . . . . ? C7 C8 C9 C10 -179.4(4) . . . . ? C13 C8 C9 C10 0.5(6) . . . . ? N2 C9 C10 C11 -151.2(4) . . . . ? C8 C9 C10 C11 30.1(6) . . . . ? C9 C10 C11 C12 -45.5(5) . . . . ? C10 C11 C12 N3 -143.2(4) . . . . ? C10 C11 C12 C13 37.3(6) . . . . ? N3 C12 C13 C14 -0.1(5) . . . . ? C11 C12 C13 C14 179.5(4) . . . . ? N3 C12 C13 C8 173.3(4) . . . . ? C11 C12 C13 C8 -7.1(6) . . . . ? C7 C8 C13 C14 -22.5(9) . . . . ? C9 C8 C13 C14 157.5(5) . . . . ? C7 C8 C13 C12 166.7(5) . . . . ? C9 C8 C13 C12 -13.3(6) . . . . ? C12 C13 C14 C15 0.4(5) . . . . ? C8 C13 C14 C15 -171.1(5) . . . . ? C12 C13 C14 C31 175.5(5) . . . . ? C8 C13 C14 C31 3.9(9) . . . . ? C13 C14 C15 C16 174.3(4) . . . . ? C31 C14 C15 C16 -0.9(8) . . . . ? C13 C14 C15 N3 -0.6(5) . . . . ? C31 C14 C15 N3 -175.9(4) . . . . ? N3 C15 C16 C17 4.9(7) . . . . ? C14 C15 C16 C17 -169.3(4) . . . . ? C15 C16 C17 N4 2.5(7) . . . . ? C15 C16 C17 C18 -179.0(4) . . . . ? N4 C17 C18 C19 -0.3(4) . . . . ? C16 C17 C18 C19 -179.0(4) . . . . ? N4 C17 C18 C32 176.5(4) . . . . ? C16 C17 C18 C32 -2.2(7) . . . . ? C17 C18 C19 C20 0.0(4) . . . . ? C32 C18 C19 C20 -176.7(4) . . . . ? C17 C18 C19 C34 177.0(4) . . . . ? C32 C18 C19 C34 0.3(7) . . . . ? C18 C19 C20 N4 0.2(5) . . . . ? C34 C19 C20 N4 -176.7(4) . . . . ? C18 C19 C20 C35 178.9(4) . . . . ? C34 C19 C20 C35 1.9(7) . . . . ? N1 C1 C21 C26 112.8(5) . . . . ? C2 C1 C21 C26 -63.9(6) . . . . ? N1 C1 C21 C22 -64.5(6) . . . . ? C2 C1 C21 C22 118.8(5) . . . . ? C26 C21 C22 C23 -1.6(7) . . . . ? C1 C21 C22 C23 175.7(4) . . . . ? C21 C22 C23 C24 -0.3(7) . . . . ? C22 C23 C24 C25 1.7(8) . . . . ? C22 C23 C24 F1 -177.4(4) . . . . ? F1 C24 C25 C26 178.0(5) . . . . ? C23 C24 C25 C26 -1.1(8) . . . . ? C22 C21 C26 C25 2.2(7) . . . . ? C1 C21 C26 C25 -175.1(4) . . . . ? C24 C25 C26 C21 -0.9(8) . . . . ? C2 C3 C28 C29 79.7(6) . . . . ? C4 C3 C28 C29 -96.9(6) . . . . ? C19 C18 C32 C33 94.3(6) . . . . ? C17 C18 C32 C33 -81.8(7) . . . . ? N4 C20 C35 C36 -138.5(4) . . . . ? C19 C20 C35 C36 43.0(7) . . . . ? N4 C20 C35 C40 40.3(6) . . . . ? C19 C20 C35 C40 -138.2(5) . . . . ? C40 C35 C36 C37 -0.8(7) . . . . ? C20 C35 C36 C37 178.2(5) . . . . ? C35 C36 C37 C38 -0.7(8) . . . . ? C36 C37 C38 C39 1.9(9) . . . . ? C36 C37 C38 F2 -178.3(5) . . . . ? F2 C38 C39 C40 178.6(5) . . . . ? C37 C38 C39 C40 -1.5(8) . . . . ? C38 C39 C40 C35 0.0(7) . . . . ? C36 C35 C40 C39 1.1(7) . . . . ? C20 C35 C40 C39 -177.8(4) . . . . ? C2 C1 N1 C4 0.6(5) . . . . ? C21 C1 N1 C4 -176.6(4) . . . . ? C2 C1 N1 Zn1 169.2(3) . . . . ? C21 C1 N1 Zn1 -8.1(6) . . . . ? C5 C4 N1 C1 174.8(4) . . . . ? C3 C4 N1 C1 -1.3(5) . . . . ? C5 C4 N1 Zn1 5.5(6) . . . . ? C3 C4 N1 Zn1 -170.6(3) . . . . ? C8 C9 N2 C6 -0.1(5) . . . . ? C10 C9 N2 C6 -178.9(4) . . . . ? C8 C9 N2 Zn1 -178.8(3) . . . . ? C10 C9 N2 Zn1 2.4(6) . . . . ? C5 C6 N2 C9 177.5(4) . . . . ? C7 C6 N2 C9 -1.6(5) . . . . ? C5 C6 N2 Zn1 -3.7(6) . . . . ? C7 C6 N2 Zn1 177.2(3) . . . . ? C13 C12 N3 C15 -0.3(5) . . . . ? C11 C12 N3 C15 -179.9(4) . . . . ? C13 C12 N3 Zn1 -162.1(3) . . . 6_556 ? C11 C12 N3 Zn1 18.3(6) . . . 6_556 ? C16 C15 N3 C12 -174.7(4) . . . . ? C14 C15 N3 C12 0.5(5) . . . . ? C16 C15 N3 Zn1 -11.6(5) . . . 6_556 ? C14 C15 N3 Zn1 163.6(3) . . . 6_556 ? C19 C20 N4 C17 -0.4(4) . . . . ? C35 C20 N4 C17 -179.2(3) . . . . ? C19 C20 N4 Zn1 -179.6(3) . . . 6_556 ? C35 C20 N4 Zn1 1.7(6) . . . 6_556 ? C16 C17 N4 C20 179.1(4) . . . . ? C18 C17 N4 C20 0.5(4) . . . . ? C16 C17 N4 Zn1 -1.6(5) . . . 6_556 ? C18 C17 N4 Zn1 179.7(3) . . . 6_556 ? C9 N2 Zn1 N4 -42.2(4) . . . 5_556 ? C6 N2 Zn1 N4 139.2(3) . . . 5_556 ? C9 N2 Zn1 N1 -175.1(4) . . . . ? C6 N2 Zn1 N1 6.3(3) . . . . ? C9 N2 Zn1 N3 73.6(4) . . . 5_556 ? C6 N2 Zn1 N3 -104.9(3) . . . 5_556 ? C1 N1 Zn1 N4 58.5(4) . . . 5_556 ? C4 N1 Zn1 N4 -134.5(3) . . . 5_556 ? C1 N1 Zn1 N2 -174.0(3) . . . . ? C4 N1 Zn1 N2 -7.1(3) . . . . ? C1 N1 Zn1 N3 -51.4(4) . . . 5_556 ? C4 N1 Zn1 N3 115.6(3) . . . 5_556 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.831 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.091