# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C114 H115 N14 O18 Zn3' _chemical_formula_weight 2165.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 '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 16.0621(4) _cell_length_b 20.7199(5) _cell_length_c 21.2873(5) _cell_angle_alpha 62.257(2) _cell_angle_beta 83.386(2) _cell_angle_gamma 82.529(2) _cell_volume 6204.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16557 _cell_measurement_theta_min 2.7777 _cell_measurement_theta_max 62.5227 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2260 _exptl_absorpt_coefficient_mu 1.195 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 40380 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 62.61 _reflns_number_total 19396 _reflns_number_gt 15345 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0813P)^2^+4.5371P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19396 _refine_ls_number_parameters 1346 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1535 _refine_ls_wR_factor_gt 0.1431 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.005 _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 0.44258(2) 1.01867(2) -0.19724(2) 0.01995(11) Uani 1 1 d . . . Zn2 Zn 0.22738(2) 1.062314(19) -0.19877(2) 0.02014(11) Uani 1 1 d . . . Zn3 Zn 0.03310(2) 1.11315(2) -0.20695(2) 0.02217(11) Uani 1 1 d . . . C8 C 0.2954(2) 1.80138(17) -0.41019(17) 0.0281(7) Uani 1 1 d . . . C38 C 0.3299(2) 1.95872(16) -0.25165(16) 0.0250(7) Uani 1 1 d . . . C42 C 0.1270(2) 0.16445(16) -0.14058(17) 0.0267(7) Uani 1 1 d . . . C43 C 0.2600(2) 1.85434(17) -0.88048(16) 0.0277(7) Uani 1 1 d . . . H43A H 0.2149 1.8261 -0.8583 0.033 Uiso 1 1 calc R . . C46 C 0.58917(19) 0.91216(17) -0.17583(17) 0.0279(7) Uani 1 1 d . . . C52 C 0.3381(2) 1.97761(16) -1.06777(16) 0.0247(7) Uani 1 1 d . . . C54 C 0.2856(2) 1.72858(16) -0.49252(16) 0.0266(7) Uani 1 1 d . . . C55 C 0.1644(2) 0.51445(16) 0.09200(16) 0.0286(7) Uani 1 1 d . . . C56 C 0.2658(2) 1.89473(17) -0.95363(16) 0.0270(7) Uani 1 1 d . . . H56A H 0.2237 1.8942 -0.9800 0.032 Uiso 1 1 calc R . . C57 C 0.3216(2) 1.91795(17) -0.29257(17) 0.0263(7) Uani 1 1 d . . . C59 C 0.2170(2) 0.22597(17) -0.09902(17) 0.0294(7) Uani 1 1 d . . . H59A H 0.2627 0.2162 -0.1254 0.035 Uiso 1 1 calc R . . C60 C 0.31378(19) 1.81305(16) -0.76105(16) 0.0237(6) Uani 1 1 d . . . C61 C 0.1112(2) 0.77026(17) -0.11799(17) 0.0315(8) Uani 1 1 d . . . H61A H 0.1075 0.7364 -0.1345 0.038 Uiso 1 1 calc R . . C62 C -0.12399(19) 1.04489(17) -0.17066(18) 0.0283(7) Uani 1 1 d . . . C65 C 0.10326(19) 0.89552(16) -0.13974(16) 0.0229(6) Uani 1 1 d . . . C69 C 0.2278(2) 0.26186(17) -0.06045(18) 0.0308(7) Uani 1 1 d . . . H69A H 0.2801 0.2773 -0.0620 0.037 Uiso 1 1 calc R . . C71 C 0.2939(2) 1.61603(16) -0.50412(16) 0.0254(7) Uani 1 1 d . . . C72 C 0.1603(2) 0.27527(17) -0.01874(18) 0.0304(7) Uani 1 1 d . . . C73 C 0.08165(19) 0.97455(16) -0.18723(17) 0.0252(7) Uani 1 1 d . . . C77 C 0.12499(19) 0.87193(16) -0.07087(17) 0.0258(7) Uani 1 1 d . . . H77A H 0.1304 0.9061 -0.0551 0.031 Uiso 1 1 calc R . . C78 C 0.34338(19) 1.83725(16) -0.71743(16) 0.0247(7) Uani 1 1 d . . . H78A H 0.3698 1.8805 -0.7380 0.030 Uiso 1 1 calc R . . C79 C 0.1387(2) 0.79803(16) -0.02518(17) 0.0274(7) Uani 1 1 d . . . H79A H 0.1532 0.7832 0.0209 0.033 Uiso 1 1 calc R . . C81 C 0.2941(2) 1.73458(16) -0.61151(16) 0.0262(7) Uani 1 1 d . . . C85 C 0.3039(2) 1.84097(18) -0.36900(17) 0.0288(7) Uani 1 1 d . . . C86 C 0.33282(19) 1.93584(16) -0.98828(16) 0.0247(7) Uani 1 1 d . . . C87 C 0.3211(2) 1.85548(16) -0.83943(16) 0.0252(7) Uani 1 1 d . . . C89 C 0.3344(2) 1.79850(16) -0.64420(16) 0.0258(7) Uani 1 1 d . . . H89A H 0.3557 1.8156 -0.6164 0.031 Uiso 1 1 calc R . . C92 C 0.2394(2) 1.57547(17) -0.44825(17) 0.0289(7) Uani 1 1 d . . . H92A H 0.1937 1.5990 -0.4338 0.035 Uiso 1 1 calc R . . C96 C 0.1419(2) 0.66585(16) 0.00162(16) 0.0270(7) Uani 1 1 d . . . C98 C 0.2527(2) 1.50013(17) -0.41378(17) 0.0286(7) Uani 1 1 d . . . H98A H 0.2152 1.4735 -0.3766 0.034 Uiso 1 1 calc R . . C99 C 0.3209(2) 1.46301(17) -0.43335(18) 0.0293(7) Uani 1 1 d . . . C102 C 0.1313(2) 0.74567(17) -0.04721(17) 0.0260(7) Uani 1 1 d . . . C105 C 0.2648(2) 1.70875(17) -0.65404(17) 0.0299(7) Uani 1 1 d . . . H10A H 0.2384 1.6655 -0.6330 0.036 Uiso 1 1 calc R . . C106 C 0.2358(2) 1.88342(18) -0.35568(17) 0.0309(7) Uani 1 1 d . . . H10B H 0.1839 1.8863 -0.3725 0.037 Uiso 1 1 calc R . . C107 C 0.1787(2) 0.39273(16) 0.09974(17) 0.0294(7) Uani 1 1 d . . . C109 C 0.3947(2) 1.93740(18) -0.94829(17) 0.0291(7) Uani 1 1 d . . . H10C H 0.4405 1.9646 -0.9709 0.035 Uiso 1 1 calc R . . C111 C 0.1698(2) 0.31345(17) 0.02410(17) 0.0299(7) Uani 1 1 d . . . C115 C 0.2439(2) 1.83109(17) -0.46812(17) 0.0302(7) Uani 1 1 d . . . H11A H 0.2130 1.8759 -0.4799 0.036 Uiso 1 1 calc R . . C118 C 0.0970(2) 0.84379(17) -0.16273(17) 0.0292(7) Uani 1 1 d . . . H11B H 0.0830 0.8591 -0.2091 0.035 Uiso 1 1 calc R . . C119 C 0.3897(2) 1.87554(18) -0.30539(18) 0.0316(7) Uani 1 1 d . . . H11C H 0.4417 1.8728 -0.2886 0.038 Uiso 1 1 calc R . . C121 C 0.1249(2) 0.43853(17) 0.24570(17) 0.0297(7) Uani 1 1 d . . . H12A H 0.0949 0.4835 0.2207 0.036 Uiso 1 1 calc R . . C123 C 0.1392(2) 0.20414(16) -0.09918(17) 0.0271(7) Uani 1 1 d . . . C125 C 0.3389(2) 1.73337(19) -0.39383(19) 0.0346(8) Uani 1 1 d . . . H12B H 0.3719 1.7115 -0.3548 0.042 Uiso 1 1 calc R . . C126 C 0.2236(2) 0.36890(17) -0.00003(18) 0.0300(7) Uani 1 1 d . . . H12C H 0.2574 0.3797 -0.0417 0.036 Uiso 1 1 calc R . . C129 C 0.0715(2) 0.21878(18) -0.05927(19) 0.0343(8) Uani 1 1 d . . . H12D H 0.0186 0.2055 -0.0600 0.041 Uiso 1 1 calc R . . C130 C 0.1229(2) 0.17268(17) 0.66541(17) 0.0283(7) Uani 1 1 d . . . C133 C 0.2443(2) 1.92092(18) -0.31823(17) 0.0283(7) Uani 1 1 d . . . H13A H 0.1981 1.9486 -0.3099 0.034 Uiso 1 1 calc R . . C135 C 0.0998(2) 0.61643(17) -0.00734(18) 0.0307(7) Uani 1 1 d . . . H13B H 0.0637 0.6339 -0.0440 0.037 Uiso 1 1 calc R . . C140 C 0.1941(2) 0.63693(17) 0.05833(18) 0.0331(8) Uani 1 1 d . . . H14A H 0.2225 0.6686 0.0662 0.040 Uiso 1 1 calc R . . C143 C 0.1749(2) 0.40530(17) 0.20925(16) 0.0278(7) Uani 1 1 d . . . C144 C 0.1634(2) 0.33642(18) 0.35868(17) 0.0315(7) Uani 1 1 d . . . C145 C 0.1276(2) 0.33508(17) 0.12602(18) 0.0331(8) Uani 1 1 d . . . H14B H 0.0962 0.3226 0.1690 0.040 Uiso 1 1 calc R . . C147 C 0.3879(2) 1.89827(18) -0.87468(17) 0.0291(7) Uani 1 1 d . . . H14C H 0.4287 1.9006 -0.8484 0.035 Uiso 1 1 calc R . . C149 C 0.3385(2) 1.38262(17) -0.39275(18) 0.0313(7) Uani 1 1 d . . . C153 C 0.2386(2) 1.79528(17) -0.50750(17) 0.0299(7) Uani 1 1 d . . . H15A H 0.2030 1.8156 -0.5448 0.036 Uiso 1 1 calc R . . C154 C 0.0689(2) 0.26645(19) 0.54769(18) 0.0369(8) Uani 1 1 d . . . H15B H 0.0181 0.2721 0.5712 0.044 Uiso 1 1 calc R . . C155 C 0.1342(2) 0.21830(18) 0.58623(17) 0.0322(8) Uani 1 1 d . . . C160 C 0.2747(2) 1.74732(17) -0.72756(17) 0.0287(7) Uani 1 1 d . . . H16A H 0.2552 1.7293 -0.7552 0.034 Uiso 1 1 calc R . . C161 C 0.4154(3) 0.1608(3) 0.4434(3) 0.0614(14) Uani 1 1 d . . . C162 C 0.3763(2) 1.23099(17) -0.31116(18) 0.0302(7) Uani 1 1 d . . . C163 C 0.2215(2) 0.33942(18) 0.24799(18) 0.0350(8) Uani 1 1 d . . . H16B H 0.2572 0.3178 0.2242 0.042 Uiso 1 1 calc R . . C167 C 0.3344(2) 1.69697(18) -0.43436(18) 0.0314(7) Uani 1 1 d . . . H16C H 0.3642 1.6516 -0.4222 0.038 Uiso 1 1 calc R . . C169 C 0.2049(2) 0.56275(17) 0.10306(17) 0.0322(8) Uani 1 1 d . . . H16D H 0.2396 0.5453 0.1408 0.039 Uiso 1 1 calc R . . C173 C 0.1103(2) 0.54245(17) 0.03660(18) 0.0327(8) Uani 1 1 d . . . H17A H 0.0811 0.5108 0.0294 0.039 Uiso 1 1 calc R . . C174 C 0.1198(2) 0.40439(18) 0.31941(17) 0.0323(8) Uani 1 1 d . . . H17B H 0.0866 0.4273 0.3433 0.039 Uiso 1 1 calc R . . C177 C 0.39563(19) 1.15126(16) -0.26872(16) 0.0248(7) Uani 1 1 d . . . C180 C 0.2199(2) 0.2513(2) 0.47754(19) 0.0440(10) Uani 1 1 d . . . H18A H 0.2712 0.2463 0.4544 0.053 Uiso 1 1 calc R . . C181 C 0.4378(3) 1.2770(2) -0.3469(4) 0.097(2) Uani 1 1 d . . . H18B H 0.4938 1.2579 -0.3434 0.117 Uiso 1 1 calc R . . C182 C 0.1541(2) 0.29815(18) 0.43776(17) 0.0330(8) Uani 1 1 d . . . C183 C 0.3599(2) 1.58041(18) -0.52619(19) 0.0363(8) Uani 1 1 d . . . H18C H 0.3959 1.6073 -0.5646 0.044 Uiso 1 1 calc R . . C185 C 0.2276(2) 0.40819(17) 0.03730(17) 0.0305(7) Uani 1 1 d . . . H18D H 0.2636 0.4453 0.0202 0.037 Uiso 1 1 calc R . . C186 C 0.3806(2) 1.83768(18) -0.34268(19) 0.0324(8) Uani 1 1 d . . . H18E H 0.4266 1.8094 -0.3504 0.039 Uiso 1 1 calc R . . C188 C 0.2101(2) 0.2122(2) 0.55068(19) 0.0423(9) Uani 1 1 d . . . H18F H 0.2549 0.1817 0.5762 0.051 Uiso 1 1 calc R . . C190 C 0.0791(2) 0.30604(19) 0.47442(18) 0.0362(8) Uani 1 1 d . . . H19A H 0.0351 0.3384 0.4493 0.043 Uiso 1 1 calc R . . C193 C 0.2152(2) 0.30582(19) 0.32131(18) 0.0366(8) Uani 1 1 d . . . H19B H 0.2466 0.2615 0.3462 0.044 Uiso 1 1 calc R . . C194 C 0.5768(2) 0.8760(2) -0.04847(19) 0.0394(8) Uani 1 1 d . . . H19C H 0.5580 0.9269 -0.0660 0.059 Uiso 1 1 calc R . . H19D H 0.6274 0.8655 -0.0241 0.059 Uiso 1 1 calc R . . H19E H 0.5340 0.8469 -0.0162 0.059 Uiso 1 1 calc R . . C196 C 0.0820(2) 0.25260(19) -0.0190(2) 0.0350(8) Uani 1 1 d . . . H19F H 0.0365 0.2606 0.0085 0.042 Uiso 1 1 calc R . . C200 C 0.0935(4) 0.6922(3) 0.2000(3) 0.0870(18) Uani 1 1 d . . . H20A H 0.1426 0.6795 0.1763 0.130 Uiso 1 1 calc R . . H20B H 0.0980 0.7391 0.1975 0.130 Uiso 1 1 calc R . . H20C H 0.0443 0.6943 0.1772 0.130 Uiso 1 1 calc R . . C204 C -0.1881(3) 0.9337(2) -0.0876(3) 0.0639(13) Uani 1 1 d . . . H20D H -0.1703 0.8906 -0.0450 0.077 Uiso 1 1 calc R . . H20E H -0.2460 0.9490 -0.0785 0.077 Uiso 1 1 calc R . . C208 C 0.3879(3) 0.0313(3) 0.5046(3) 0.0705(14) Uani 1 1 d . . . H20F H 0.3766 0.0421 0.4572 0.106 Uiso 1 1 calc R . . H20G H 0.3367 0.0209 0.5343 0.106 Uiso 1 1 calc R . . H20H H 0.4283 -0.0104 0.5232 0.106 Uiso 1 1 calc R . . C210 C -0.1833(4) 0.9157(3) -0.1457(3) 0.0732(15) Uani 1 1 d . . . H21A H -0.2246 0.8814 -0.1359 0.088 Uiso 1 1 calc R . . H21B H -0.1281 0.8913 -0.1483 0.088 Uiso 1 1 calc R . . C211 C 0.4411(3) 0.0848(3) 0.5716(2) 0.0574(11) Uani 1 1 d . . . H21C H 0.4676 0.0358 0.5986 0.069 Uiso 1 1 calc R . . H21D H 0.3898 0.0906 0.5981 0.069 Uiso 1 1 calc R . . C212 C 0.9081(3) 0.4457(3) 0.2809(3) 0.0603(12) Uani 1 1 d . . . C214 C 0.6449(3) 0.8227(2) -0.2202(3) 0.0616(13) Uani 1 1 d . . . C215 C 0.4194(3) 1.3504(2) -0.3875(4) 0.097(2) Uani 1 1 d . . . H21G H 0.4632 1.3795 -0.4125 0.117 Uiso 1 1 calc R . . C219 C -0.1976(3) 0.9787(2) -0.2147(2) 0.0541(11) Uani 1 1 d . . . H21H H -0.2576 0.9917 -0.2191 0.065 Uiso 1 1 calc R . . H21I H -0.1761 0.9655 -0.2520 0.065 Uiso 1 1 calc R . . C220 C 0.6233(3) 0.7819(2) -0.0894(2) 0.0483(10) Uani 1 1 d . . . C223 C 0.3730(2) 1.50434(18) -0.4915(2) 0.0391(9) Uani 1 1 d . . . H22C H 0.4173 1.4809 -0.5075 0.047 Uiso 1 1 calc R . . C228 C 0.1546(3) 0.5880(2) 0.2998(2) 0.0511(11) Uani 1 1 d . . . C236 C -0.0964(3) 0.9923(2) -0.0450(2) 0.0503(10) Uani 1 1 d . . . H23A H -0.0632 1.0333 -0.0630 0.075 Uiso 1 1 calc R . . H23B H -0.0610 0.9477 -0.0221 0.075 Uiso 1 1 calc R . . H23C H -0.1396 0.9959 -0.0113 0.075 Uiso 1 1 calc R . . C237 C -0.1382(2) 1.0973(2) -0.29647(19) 0.0436(9) Uani 1 1 d . . . H23D H -0.1113 1.1355 -0.2954 0.065 Uiso 1 1 calc R . . H23E H -0.1895 1.1176 -0.3203 0.065 Uiso 1 1 calc R . . H23F H -0.1014 1.0754 -0.3215 0.065 Uiso 1 1 calc R . . C241 C 0.2762(2) 1.33657(18) -0.3566(2) 0.0399(9) Uani 1 1 d . . . H24A H 0.2204 1.3559 -0.3596 0.048 Uiso 1 1 calc R . . C246 C 0.2945(2) 1.26285(18) -0.3164(2) 0.0379(9) Uani 1 1 d . . . H24B H 0.2508 1.2335 -0.2920 0.046 Uiso 1 1 calc R . . C247 C 0.1233(2) 0.29622(17) 0.08841(18) 0.0323(8) Uani 1 1 d . . . H24C H 0.0888 0.2580 0.1065 0.039 Uiso 1 1 calc R . . C300 C 0.2169(6) 0.4911(4) 0.4013(5) 0.177(5) Uani 1 1 d . . . H30A H 0.2569 0.4901 0.3645 0.265 Uiso 1 1 calc R . . H30B H 0.1989 0.4430 0.4306 0.265 Uiso 1 1 calc R . . H30C H 0.2427 0.5067 0.4298 0.265 Uiso 1 1 calc R . . C301 C 0.0148(5) 0.6503(4) 0.3158(5) 0.133(3) Uani 1 1 d . . . H30D H -0.0342 0.6683 0.2878 0.160 Uiso 1 1 calc R . . H30E H 0.0257 0.6870 0.3293 0.160 Uiso 1 1 calc R . . C303 C 0.8894(5) 0.3760(5) 0.2170(4) 0.125(3) Uani 1 1 d . . . H30F H 0.8320 0.3654 0.2182 0.150 Uiso 1 1 calc R . . H30G H 0.9268 0.3362 0.2150 0.150 Uiso 1 1 calc R . . C304 C 0.9076(6) 0.5770(4) 0.2180(5) 0.141(3) Uani 1 1 d . . . H30H H 0.9169 0.5685 0.2651 0.211 Uiso 1 1 calc R . . H30I H 0.8550 0.6059 0.2036 0.211 Uiso 1 1 calc R . . H30J H 0.9524 0.6027 0.1856 0.211 Uiso 1 1 calc R . . C306 C 0.0051(5) 0.0775(5) 0.5570(4) 0.132(3) Uani 1 1 d . . . H30K H -0.0534 0.0796 0.5503 0.197 Uiso 1 1 calc R . . H30L H 0.0143 0.1164 0.5673 0.197 Uiso 1 1 calc R . . H30M H 0.0218 0.0312 0.5959 0.197 Uiso 1 1 calc R . . C307 C 0.0165(5) 0.1225(5) 0.3135(4) 0.142(4) Uani 1 1 d . . . H30N H -0.0427 0.1200 0.3264 0.213 Uiso 1 1 calc R . . H30O H 0.0364 0.0863 0.2979 0.213 Uiso 1 1 calc R . . H30P H 0.0263 0.1703 0.2758 0.213 Uiso 1 1 calc R . . C308 C 0.6101(4) 0.7642(3) -0.1485(4) 0.0324(16) Uani 0.50 1 d P . . C309 C 0.4305(4) 0.2890(3) 0.3816(4) 0.143(4) Uani 1 1 d . . . H30R H 0.4166 0.2825 0.3423 0.215 Uiso 1 1 calc R . . H30S H 0.4820 0.3122 0.3695 0.215 Uiso 1 1 calc R . . H30T H 0.3861 0.3192 0.3918 0.215 Uiso 1 1 calc R . . C310 C 0.0128(4) 0.0978(4) 0.4359(4) 0.0882(18) Uani 1 1 d . . . C312 C 0.9092(4) 0.3124(3) 0.3498(3) 0.094(2) Uani 1 1 d . . . H31A H 0.9176 0.3239 0.3873 0.141 Uiso 1 1 calc R . . H31B H 0.9563 0.2809 0.3451 0.141 Uiso 1 1 calc R . . H31C H 0.8587 0.2881 0.3609 0.141 Uiso 1 1 calc R . . C313 C 0.4628(4) 0.2154(3) 0.5099(4) 0.098(2) Uani 1 1 d . . . H31D H 0.4128 0.2290 0.5327 0.117 Uiso 1 1 calc R . . H31E H 0.5028 0.2512 0.4982 0.117 Uiso 1 1 calc R . . C315 C 0.5002(3) 0.1413(3) 0.5609(3) 0.0730(14) Uani 1 1 d . . . H31F H 0.5072 0.1404 0.6060 0.088 Uiso 1 1 calc R . . H31G H 0.5550 0.1304 0.5418 0.088 Uiso 1 1 calc R . . C320 C 0.8936(5) 0.5077(5) 0.1526(4) 0.122(3) Uani 1 1 d . . . H32A H 0.8771 0.5505 0.1128 0.147 Uiso 1 1 calc R . . C321 C 0.9066(10) 0.4468(5) 0.1511(5) 0.206(7) Uani 1 1 d . . . H32B H 0.9271 0.4456 0.1089 0.247 Uiso 1 1 calc R . . C322 C 0.1472(5) 0.1094(5) 0.3667(5) 0.137(3) Uani 1 1 d . . . H32C H 0.1760 0.1250 0.3223 0.165 Uiso 1 1 calc R . . C323 C 0.1421(5) 0.0853(6) 0.4889(5) 0.143(3) Uani 1 1 d . . . H32D H 0.1636 0.0418 0.5295 0.172 Uiso 1 1 calc R . . H32E H 0.1551 0.1273 0.4934 0.172 Uiso 1 1 calc R . . C324 C 0.1875(5) 0.0870(7) 0.4252(6) 0.174(5) Uani 1 1 d . . . H32F H 0.2447 0.0724 0.4254 0.208 Uiso 1 1 calc R . . C325 C 0.0780(8) 0.5490(5) 0.4195(4) 0.145(4) Uani 1 1 d . . . H32G H 0.0933 0.5808 0.4374 0.174 Uiso 1 1 calc R . . H32H H 0.0680 0.5019 0.4597 0.174 Uiso 1 1 calc R . . C326 C -0.0010(7) 0.5818(5) 0.3796(5) 0.151(4) Uani 1 1 d . . . H32I H -0.0195 0.5475 0.3661 0.182 Uiso 1 1 calc R . . H32J H -0.0453 0.5911 0.4101 0.182 Uiso 1 1 calc R . . C328 C 0.6096(3) 0.9536(2) -0.3022(2) 0.0487(10) Uani 1 1 d . . . H32K H 0.5890 0.9991 -0.3021 0.073 Uiso 1 1 calc R . . H32L H 0.5722 0.9417 -0.3266 0.073 Uiso 1 1 calc R . . H32M H 0.6646 0.9580 -0.3261 0.073 Uiso 1 1 calc R . . O1 O 0.40407(13) 1.96148(12) -0.23788(12) 0.0308(5) Uani 1 1 d . . . O2 O 0.33931(15) 1.11046(12) -0.23725(14) 0.0415(6) Uani 1 1 d . . . O3 O 0.56330(13) 0.97697(11) -0.18820(12) 0.0284(5) Uani 1 1 d . . . O4 O 0.41078(14) 1.99343(12) -1.09793(11) 0.0293(5) Uani 1 1 d . . . O5 O 0.47046(15) 1.12380(13) -0.26276(16) 0.0518(8) Uani 1 1 d . . . O6 O 0.04119(15) 0.99531(12) -0.23938(13) 0.0361(6) Uani 1 1 d . . . O7 O 0.10471(13) 1.02023(11) -0.16649(11) 0.0241(5) Uani 1 1 d . . . O8 O 0.05210(14) 0.15693(12) -0.14649(12) 0.0321(5) Uani 1 1 d . . . O9 O -0.08485(13) 1.09950(12) -0.18305(13) 0.0346(6) Uani 1 1 d . . . O10 O 0.05091(15) 0.18081(12) 0.69407(12) 0.0343(5) Uani 1 1 d . . . O11 O 0.27056(14) 1.99358(12) -1.09909(11) 0.0284(5) Uani 1 1 d . . . O12 O 0.18386(15) 0.13099(13) 0.69780(12) 0.0369(6) Uani 1 1 d . . . O13 O 0.19143(14) 0.14119(12) -0.16586(12) 0.0315(5) Uani 1 1 d . . . O14 O 0.26349(13) 1.98719(12) -0.23457(12) 0.0283(5) Uani 1 1 d . . . O15 O 0.3905(2) 0.1661(2) 0.38836(18) 0.0842(12) Uani 1 1 d . . . O16 O 0.9171(2) 0.44763(17) 0.33542(17) 0.0631(8) Uani 1 1 d . . . O17 O 0.2145(2) 0.58549(18) 0.2609(2) 0.0672(9) Uani 1 1 d . . . O18 O -0.0629(3) 0.0972(5) 0.4388(4) 0.180(3) Uani 1 1 d . . . N1 N 0.28246(18) 1.69419(14) -0.53644(13) 0.0290(6) Uani 1 1 d . . . N2 N 0.1792(2) 0.43732(14) 0.13383(14) 0.0326(7) Uani 1 1 d . . . N3 N 0.61426(18) 0.89608(16) -0.22962(16) 0.0359(7) Uani 1 1 d . . . N4 N -0.15680(17) 1.04218(15) -0.22427(16) 0.0345(7) Uani 1 1 d . . . N5 N 0.59366(18) 0.85853(14) -0.10812(15) 0.0329(6) Uani 1 1 d . . . N6 N -0.13496(19) 0.99220(16) -0.10360(15) 0.0387(7) Uani 1 1 d . . . N7 N 0.4214(2) 0.0945(2) 0.50317(19) 0.0560(9) Uani 1 1 d . . . N8 N 0.9052(3) 0.5080(3) 0.2176(2) 0.0849(15) Uani 1 1 d . . . N9 N 0.1481(4) 0.5395(2) 0.3708(2) 0.0933(18) Uani 1 1 d . . . N10 N 0.4408(3) 0.2172(2) 0.4445(3) 0.0789(14) Uani 1 1 d . . . N11 N 0.9018(3) 0.3811(3) 0.2818(3) 0.0803(13) Uani 1 1 d . . . N12 N 0.0871(3) 0.6370(2) 0.2743(2) 0.0706(12) Uani 1 1 d . . . N13 N 0.0607(3) 0.1088(3) 0.3744(3) 0.0867(14) Uani 1 1 d . . . N14 N 0.0545(3) 0.0854(3) 0.4929(3) 0.0890(14) Uani 1 1 d . . . C500 C 0.6610(10) 0.7755(8) -0.1541(8) 0.093(4) Uiso 0.50 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 Zn1 0.0213(2) 0.0185(2) 0.0183(2) -0.00716(17) -0.00027(16) -0.00184(15) Zn2 0.0218(2) 0.0178(2) 0.0183(2) -0.00665(17) 0.00058(16) -0.00111(15) Zn3 0.0223(2) 0.0203(2) 0.0209(2) -0.00729(17) 0.00045(16) -0.00206(16) C8 0.0272(17) 0.0288(17) 0.0297(18) -0.0147(15) 0.0039(14) -0.0070(13) C38 0.0285(17) 0.0244(16) 0.0238(16) -0.0128(14) 0.0020(13) -0.0037(13) C42 0.0345(18) 0.0167(15) 0.0257(17) -0.0065(13) -0.0056(14) -0.0016(13) C43 0.0271(16) 0.0318(17) 0.0223(16) -0.0100(14) 0.0027(13) -0.0092(13) C46 0.0192(15) 0.0315(18) 0.0326(18) -0.0144(15) -0.0043(13) -0.0001(13) C52 0.0281(17) 0.0243(16) 0.0207(16) -0.0084(13) -0.0009(13) -0.0066(13) C54 0.0374(18) 0.0226(16) 0.0207(16) -0.0102(13) 0.0008(14) -0.0067(13) C55 0.0432(19) 0.0184(15) 0.0202(16) -0.0067(13) 0.0022(14) -0.0010(14) C56 0.0251(16) 0.0333(17) 0.0230(16) -0.0122(14) -0.0033(13) -0.0051(13) C57 0.0265(16) 0.0291(17) 0.0272(17) -0.0164(14) 0.0023(13) -0.0052(13) C59 0.0325(18) 0.0254(16) 0.0307(18) -0.0140(14) -0.0018(14) 0.0010(14) C60 0.0261(16) 0.0250(16) 0.0188(15) -0.0097(13) 0.0003(13) -0.0012(13) C61 0.046(2) 0.0223(16) 0.0273(17) -0.0125(14) -0.0002(15) -0.0046(14) C62 0.0199(15) 0.0240(16) 0.0359(19) -0.0093(15) -0.0035(14) -0.0008(13) C65 0.0237(15) 0.0204(15) 0.0241(16) -0.0099(13) 0.0004(13) -0.0034(12) C69 0.0330(18) 0.0277(17) 0.0340(19) -0.0157(15) -0.0014(15) -0.0043(14) C71 0.0376(18) 0.0179(15) 0.0203(16) -0.0074(13) -0.0062(14) -0.0026(13) C72 0.0376(19) 0.0238(16) 0.0314(18) -0.0145(14) -0.0069(15) 0.0038(14) C73 0.0223(16) 0.0248(16) 0.0269(17) -0.0101(14) -0.0007(13) -0.0044(13) C77 0.0258(16) 0.0233(16) 0.0290(17) -0.0123(14) -0.0004(13) -0.0042(13) C78 0.0272(16) 0.0201(15) 0.0227(16) -0.0069(13) -0.0012(13) -0.0008(12) C79 0.0303(17) 0.0229(16) 0.0253(17) -0.0076(14) -0.0034(14) -0.0024(13) C81 0.0368(18) 0.0209(16) 0.0178(15) -0.0070(13) -0.0020(13) 0.0006(13) C85 0.0328(18) 0.0311(17) 0.0271(17) -0.0171(15) 0.0022(14) -0.0071(14) C86 0.0266(16) 0.0249(16) 0.0210(16) -0.0097(13) 0.0018(13) -0.0032(13) C87 0.0299(17) 0.0226(16) 0.0212(16) -0.0087(13) -0.0017(13) -0.0016(13) C89 0.0313(17) 0.0258(16) 0.0232(16) -0.0135(14) -0.0014(13) -0.0032(13) C92 0.0359(18) 0.0241(16) 0.0240(17) -0.0103(14) -0.0004(14) 0.0027(14) C96 0.0369(18) 0.0203(15) 0.0211(16) -0.0080(13) 0.0015(14) -0.0017(13) C98 0.0325(18) 0.0223(16) 0.0248(17) -0.0059(14) 0.0033(14) -0.0051(13) C99 0.0317(18) 0.0222(16) 0.0294(18) -0.0083(14) 0.0006(14) -0.0035(13) C102 0.0283(16) 0.0239(16) 0.0253(16) -0.0115(14) 0.0018(13) -0.0027(13) C105 0.0421(19) 0.0232(16) 0.0243(17) -0.0097(14) -0.0010(15) -0.0084(14) C106 0.0265(17) 0.0397(19) 0.0300(18) -0.0188(16) -0.0012(14) -0.0039(14) C107 0.045(2) 0.0187(15) 0.0228(16) -0.0088(13) -0.0042(15) 0.0019(14) C109 0.0239(16) 0.0349(18) 0.0262(17) -0.0110(15) 0.0004(13) -0.0087(14) C111 0.0368(18) 0.0245(16) 0.0291(18) -0.0136(14) -0.0049(15) 0.0023(14) C115 0.0397(19) 0.0248(16) 0.0241(17) -0.0102(14) -0.0014(14) -0.0006(14) C118 0.0388(19) 0.0252(17) 0.0207(16) -0.0083(14) -0.0009(14) -0.0031(14) C119 0.0240(16) 0.0394(19) 0.040(2) -0.0250(17) -0.0015(14) -0.0035(14) C121 0.0357(18) 0.0221(16) 0.0241(17) -0.0062(14) -0.0023(14) 0.0042(14) C123 0.0316(17) 0.0200(15) 0.0281(17) -0.0102(14) -0.0052(14) 0.0029(13) C125 0.042(2) 0.0341(19) 0.0320(19) -0.0175(16) -0.0080(16) -0.0029(15) C126 0.0361(18) 0.0245(16) 0.0280(17) -0.0121(14) -0.0019(14) 0.0025(14) C129 0.0317(18) 0.0314(18) 0.043(2) -0.0199(16) -0.0064(16) 0.0027(14) C130 0.0320(18) 0.0228(16) 0.0224(17) -0.0050(14) 0.0013(14) 0.0001(14) C133 0.0262(16) 0.0357(18) 0.0286(17) -0.0207(15) 0.0015(14) -0.0004(14) C135 0.0389(19) 0.0240(17) 0.0271(17) -0.0089(14) -0.0059(15) -0.0031(14) C140 0.046(2) 0.0220(16) 0.0315(18) -0.0116(15) -0.0055(16) -0.0052(15) C143 0.0387(18) 0.0233(16) 0.0169(15) -0.0053(13) 0.0001(13) -0.0048(14) C144 0.0345(18) 0.0310(18) 0.0204(17) -0.0060(14) 0.0014(14) 0.0002(14) C145 0.043(2) 0.0247(17) 0.0273(18) -0.0096(14) 0.0025(15) -0.0024(15) C147 0.0301(17) 0.0351(18) 0.0224(17) -0.0123(15) -0.0031(14) -0.0058(14) C149 0.0289(17) 0.0231(16) 0.0346(19) -0.0081(15) 0.0025(14) -0.0020(13) C153 0.0377(19) 0.0277(17) 0.0220(16) -0.0105(14) -0.0024(14) 0.0012(14) C154 0.0349(19) 0.041(2) 0.0247(18) -0.0102(16) 0.0057(15) 0.0046(16) C155 0.0356(19) 0.0313(18) 0.0222(17) -0.0078(14) 0.0014(14) 0.0005(14) C160 0.0421(19) 0.0249(16) 0.0215(16) -0.0117(14) -0.0026(14) -0.0063(14) C161 0.034(2) 0.059(3) 0.051(3) 0.004(2) 0.002(2) 0.009(2) C162 0.0245(16) 0.0229(16) 0.0383(19) -0.0101(15) 0.0001(14) -0.0028(13) C163 0.047(2) 0.0281(18) 0.0253(18) -0.0123(15) 0.0026(15) 0.0068(15) C167 0.0404(19) 0.0255(17) 0.0310(18) -0.0152(15) -0.0045(15) -0.0011(14) C169 0.047(2) 0.0239(17) 0.0233(17) -0.0074(14) -0.0083(15) -0.0014(15) C173 0.041(2) 0.0243(17) 0.0332(19) -0.0126(15) -0.0049(15) -0.0034(14) C174 0.0370(19) 0.0319(18) 0.0242(17) -0.0121(15) 0.0044(14) 0.0011(15) C177 0.0246(16) 0.0238(16) 0.0232(16) -0.0085(13) 0.0005(13) -0.0041(13) C180 0.0315(19) 0.053(2) 0.0260(19) -0.0044(17) 0.0047(15) 0.0078(17) C181 0.029(2) 0.033(2) 0.157(6) 0.011(3) 0.016(3) 0.0043(18) C182 0.0383(19) 0.0305(18) 0.0208(17) -0.0058(14) 0.0010(14) 0.0019(15) C183 0.041(2) 0.0235(17) 0.0320(19) -0.0033(15) 0.0083(16) -0.0092(15) C185 0.0411(19) 0.0224(16) 0.0264(17) -0.0098(14) -0.0028(15) -0.0028(14) C186 0.0321(18) 0.0340(18) 0.040(2) -0.0259(16) 0.0039(15) -0.0034(14) C188 0.0341(19) 0.048(2) 0.0249(18) -0.0034(16) 0.0004(15) 0.0089(17) C190 0.0377(19) 0.0331(19) 0.0250(18) -0.0055(15) -0.0012(15) 0.0076(15) C193 0.043(2) 0.0278(18) 0.0268(18) -0.0051(15) -0.0040(15) 0.0111(15) C194 0.041(2) 0.040(2) 0.0296(19) -0.0099(16) -0.0068(16) 0.0033(16) C196 0.0300(18) 0.0379(19) 0.045(2) -0.0269(17) -0.0008(16) 0.0022(15) C200 0.073(4) 0.056(3) 0.089(4) 0.002(3) -0.012(3) 0.002(3) C204 0.088(4) 0.038(2) 0.056(3) -0.008(2) 0.000(3) -0.031(2) C208 0.064(3) 0.073(3) 0.066(3) -0.024(3) -0.009(3) -0.002(3) C210 0.088(4) 0.053(3) 0.078(4) -0.021(3) -0.014(3) -0.032(3) C211 0.052(3) 0.066(3) 0.042(2) -0.014(2) -0.009(2) -0.002(2) C212 0.047(3) 0.081(3) 0.057(3) -0.039(3) 0.013(2) -0.005(2) C214 0.091(4) 0.037(2) 0.056(3) -0.026(2) 0.006(3) 0.006(2) C215 0.033(2) 0.024(2) 0.164(6) 0.010(3) 0.026(3) -0.0036(18) C219 0.059(3) 0.045(2) 0.061(3) -0.022(2) -0.024(2) -0.009(2) C220 0.053(2) 0.0289(19) 0.049(2) -0.0098(18) -0.0022(19) 0.0114(17) C223 0.0363(19) 0.0240(17) 0.047(2) -0.0116(16) 0.0116(17) -0.0007(15) C228 0.079(3) 0.034(2) 0.045(2) -0.0183(19) -0.015(2) -0.010(2) C236 0.058(3) 0.051(2) 0.042(2) -0.019(2) -0.018(2) 0.001(2) C237 0.034(2) 0.049(2) 0.034(2) -0.0095(18) -0.0049(16) 0.0048(17) C241 0.0249(17) 0.0278(18) 0.055(2) -0.0100(17) 0.0015(16) -0.0023(14) C246 0.0266(18) 0.0223(17) 0.052(2) -0.0063(16) 0.0035(16) -0.0055(14) C247 0.0392(19) 0.0218(16) 0.0339(19) -0.0112(15) -0.0021(15) -0.0026(14) C300 0.237(11) 0.106(6) 0.143(7) 0.025(5) -0.143(8) -0.078(6) C301 0.150(7) 0.093(5) 0.157(7) -0.074(5) 0.088(6) -0.035(5) C303 0.111(6) 0.184(9) 0.136(7) -0.123(7) -0.024(5) 0.016(6) C304 0.169(9) 0.076(5) 0.128(7) -0.010(5) 0.018(6) -0.018(5) C306 0.114(6) 0.212(9) 0.120(6) -0.119(7) 0.023(5) -0.040(6) C307 0.108(6) 0.234(10) 0.118(6) -0.116(7) -0.056(5) 0.054(6) C308 0.026(4) 0.018(3) 0.054(5) -0.020(3) 0.011(3) -0.002(3) C309 0.061(4) 0.079(4) 0.178(8) 0.038(5) -0.011(4) -0.018(3) C310 0.053(3) 0.136(5) 0.104(5) -0.079(4) -0.022(3) 0.007(3) C312 0.101(5) 0.079(4) 0.104(5) -0.044(4) 0.035(4) -0.039(3) C313 0.056(3) 0.067(4) 0.160(7) -0.048(4) 0.032(4) -0.023(3) C315 0.044(3) 0.090(4) 0.085(4) -0.038(3) -0.003(3) -0.012(3) C320 0.124(6) 0.149(7) 0.063(4) -0.028(5) -0.028(4) 0.030(6) C321 0.46(2) 0.097(6) 0.071(5) -0.034(5) -0.093(9) -0.006(9) C322 0.118(6) 0.163(8) 0.137(7) -0.055(6) -0.054(6) -0.047(6) C323 0.089(6) 0.192(9) 0.167(9) -0.086(7) -0.062(6) -0.014(6) C324 0.066(5) 0.297(14) 0.131(8) -0.078(9) 0.005(5) -0.013(7) C325 0.240(12) 0.152(8) 0.050(4) -0.037(5) 0.025(6) -0.103(8) C326 0.197(11) 0.161(9) 0.110(7) -0.082(7) 0.080(7) -0.063(8) C328 0.053(2) 0.055(2) 0.036(2) -0.0197(19) 0.0015(18) -0.0056(19) O1 0.0243(12) 0.0347(12) 0.0402(13) -0.0231(11) -0.0028(10) -0.0011(9) O2 0.0292(13) 0.0193(11) 0.0566(16) -0.0025(11) 0.0063(12) -0.0045(10) O3 0.0256(11) 0.0246(12) 0.0323(12) -0.0106(10) -0.0039(9) -0.0011(9) O4 0.0278(12) 0.0352(12) 0.0222(11) -0.0104(10) 0.0012(9) -0.0071(10) O5 0.0212(13) 0.0261(13) 0.083(2) -0.0055(13) 0.0013(13) 0.0006(10) O6 0.0423(14) 0.0267(12) 0.0361(14) -0.0096(11) -0.0158(11) 0.0001(10) O7 0.0269(11) 0.0195(10) 0.0245(11) -0.0086(9) 0.0002(9) -0.0047(8) O8 0.0292(12) 0.0325(12) 0.0387(13) -0.0201(11) -0.0041(10) 0.0004(10) O9 0.0210(11) 0.0283(12) 0.0501(15) -0.0151(11) 0.0014(10) -0.0021(9) O10 0.0379(14) 0.0313(12) 0.0243(12) -0.0075(10) 0.0069(10) -0.0001(10) O11 0.0296(12) 0.0304(12) 0.0199(11) -0.0065(9) -0.0004(9) -0.0056(9) O12 0.0396(14) 0.0359(13) 0.0232(12) -0.0053(10) 0.0025(11) -0.0005(11) O13 0.0331(13) 0.0282(12) 0.0397(13) -0.0217(11) 0.0034(10) -0.0047(10) O14 0.0243(11) 0.0331(12) 0.0339(12) -0.0215(10) 0.0013(9) -0.0023(9) O15 0.052(2) 0.106(3) 0.045(2) 0.0017(19) -0.0025(16) 0.0129(19) O16 0.0571(19) 0.068(2) 0.058(2) -0.0264(17) 0.0158(16) -0.0113(15) O17 0.058(2) 0.069(2) 0.084(2) -0.0410(19) -0.0174(19) -0.0004(16) O18 0.055(3) 0.385(11) 0.180(6) -0.201(7) -0.017(3) 0.012(4) N1 0.0472(17) 0.0202(13) 0.0166(13) -0.0061(11) -0.0020(12) -0.0021(12) N2 0.0561(19) 0.0179(13) 0.0204(14) -0.0064(11) -0.0011(13) -0.0026(12) N3 0.0332(16) 0.0410(17) 0.0362(17) -0.0215(14) -0.0022(13) 0.0030(13) N4 0.0267(15) 0.0348(16) 0.0376(17) -0.0120(13) -0.0074(13) -0.0013(12) N5 0.0351(16) 0.0263(14) 0.0333(16) -0.0122(13) -0.0046(13) 0.0069(12) N6 0.0436(18) 0.0354(16) 0.0311(16) -0.0075(14) -0.0054(14) -0.0110(13) N7 0.054(2) 0.055(2) 0.044(2) -0.0115(18) -0.0028(17) 0.0007(17) N8 0.068(3) 0.103(4) 0.059(3) -0.023(3) -0.008(2) 0.023(3) N9 0.167(5) 0.059(3) 0.050(3) -0.008(2) -0.032(3) -0.042(3) N10 0.046(2) 0.053(3) 0.093(4) 0.001(2) 0.006(2) -0.0008(19) N11 0.062(3) 0.106(4) 0.079(3) -0.048(3) 0.002(2) -0.008(3) N12 0.088(3) 0.041(2) 0.070(3) -0.021(2) 0.019(2) 0.002(2) N13 0.064(3) 0.128(4) 0.081(3) -0.060(3) -0.014(3) 0.006(3) N14 0.073(3) 0.123(4) 0.089(4) -0.062(3) -0.012(3) -0.008(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 O4 1.948(2) 1_546 ? Zn1 O1 1.950(2) 1_545 ? Zn1 O3 2.010(2) . ? Zn1 O5 2.042(2) . ? Zn1 O2 2.256(2) . ? Zn1 C177 2.503(3) . ? Zn2 O14 2.027(2) 1_545 ? Zn2 O13 2.055(2) 1_565 ? Zn2 O2 2.065(2) . ? Zn2 O11 2.069(2) 1_546 ? Zn2 O12 2.131(2) 1_564 ? Zn2 O7 2.166(2) . ? Zn2 Zn3 3.1586(5) . ? Zn3 O10 1.924(2) 1_564 ? Zn3 O9 1.926(2) . ? Zn3 O8 1.955(2) 1_565 ? Zn3 O7 1.970(2) . ? C8 C125 1.392(5) . ? C8 C115 1.407(5) . ? C8 C85 1.478(4) . ? C38 O14 1.251(4) . ? C38 O1 1.274(4) . ? C38 C57 1.494(4) . ? C42 O13 1.256(4) . ? C42 O8 1.261(4) . ? C42 C123 1.499(4) . ? C43 C56 1.381(4) . ? C43 C87 1.397(4) . ? C43 H43A 0.9300 . ? C46 O3 1.263(4) . ? C46 N3 1.341(4) . ? C46 N5 1.353(4) . ? C52 O11 1.265(4) . ? C52 O4 1.270(4) . ? C52 C86 1.497(4) . ? C54 C167 1.382(5) . ? C54 C153 1.399(4) . ? C54 N1 1.423(4) . ? C55 C169 1.380(5) . ? C55 C173 1.396(5) . ? C55 N2 1.424(4) . ? C56 C86 1.378(4) . ? C56 H56A 0.9300 . ? C57 C133 1.395(5) . ? C57 C119 1.396(5) . ? C59 C69 1.375(5) . ? C59 C123 1.384(5) . ? C59 H59A 0.9300 . ? C60 C78 1.392(4) . ? C60 C160 1.404(4) . ? C60 C87 1.479(4) . ? C61 C118 1.375(4) . ? C61 C102 1.410(5) . ? C61 H61A 0.9300 . ? C62 O9 1.271(4) . ? C62 N4 1.338(4) . ? C62 N6 1.342(4) . ? C65 C77 1.384(4) . ? C65 C118 1.388(4) . ? C65 C73 1.488(4) . ? C69 C72 1.403(5) . ? C69 H69A 0.9300 . ? C71 C183 1.375(5) . ? C71 C92 1.381(5) . ? C71 N1 1.430(4) . ? C72 C196 1.401(5) . ? C72 C111 1.488(4) . ? C73 O6 1.220(4) . ? C73 O7 1.321(4) . ? C77 C79 1.384(4) . ? C77 H77A 0.9300 . ? C78 C89 1.382(4) . ? C78 H78A 0.9300 . ? C79 C102 1.390(4) . ? C79 H79A 0.9300 . ? C81 C89 1.385(4) . ? C81 C105 1.394(4) . ? C81 N1 1.420(4) . ? C85 C186 1.393(5) . ? C85 C106 1.400(5) . ? C86 C109 1.393(4) . ? C87 C147 1.393(4) . ? C89 H89A 0.9300 . ? C92 C98 1.380(4) . ? C92 H92A 0.9300 . ? C96 C135 1.390(5) . ? C96 C140 1.396(5) . ? C96 C102 1.487(4) . ? C98 C99 1.393(5) . ? C98 H98A 0.9300 . ? C99 C223 1.388(5) . ? C99 C149 1.482(4) . ? C105 C160 1.387(4) . ? C105 H10A 0.9300 . ? C106 C133 1.374(5) . ? C106 H10B 0.9300 . ? C107 C185 1.384(5) . ? C107 C145 1.393(5) . ? C107 N2 1.417(4) . ? C109 C147 1.388(4) . ? C109 H10C 0.9300 . ? C111 C247 1.392(5) . ? C111 C126 1.392(5) . ? C115 C153 1.369(5) . ? C115 H11A 0.9300 . ? C118 H11B 0.9300 . ? C119 C186 1.380(5) . ? C119 H11C 0.9300 . ? C121 C174 1.386(5) . ? C121 C143 1.390(5) . ? C121 H12A 0.9300 . ? C123 C129 1.392(5) . ? C125 C167 1.397(5) . ? C125 H12B 0.9300 . ? C126 C185 1.388(5) . ? C126 H12C 0.9300 . ? C129 C196 1.370(5) . ? C129 H12D 0.9300 . ? C130 O12 1.249(4) . ? C130 O10 1.273(4) . ? C130 C155 1.503(4) . ? C133 H13A 0.9300 . ? C135 C173 1.374(4) . ? C135 H13B 0.9300 . ? C140 C169 1.380(4) . ? C140 H14A 0.9300 . ? C143 C163 1.390(5) . ? C143 N2 1.420(4) . ? C144 C193 1.381(5) . ? C144 C174 1.398(5) . ? C144 C182 1.488(4) . ? C145 C247 1.386(5) . ? C145 H14B 0.9300 . ? C147 H14C 0.9300 . ? C149 C215 1.373(5) . ? C149 C241 1.375(5) . ? C153 H15A 0.9300 . ? C154 C190 1.385(5) . ? C154 C155 1.391(5) . ? C154 H15B 0.9300 . ? C155 C188 1.383(5) . ? C160 H16A 0.9300 . ? C161 O15 1.234(6) . ? C161 N10 1.297(7) . ? C161 N7 1.372(6) . ? C162 C181 1.365(5) . ? C162 C246 1.383(5) . ? C162 C177 1.478(4) . ? C163 C193 1.379(5) . ? C163 H16B 0.9300 . ? C167 H16C 0.9300 . ? C169 H16D 0.9300 . ? C173 H17A 0.9300 . ? C174 H17B 0.9300 . ? C177 O2 1.230(4) . ? C177 O5 1.255(4) . ? C180 C188 1.381(5) . ? C180 C182 1.396(5) . ? C180 H18A 0.9300 . ? C181 C215 1.365(6) . ? C181 H18B 0.9300 . ? C182 C190 1.393(5) . ? C183 C223 1.393(5) . ? C183 H18C 0.9300 . ? C185 H18D 0.9300 . ? C186 H18E 0.9300 . ? C188 H18F 0.9300 . ? C190 H19A 0.9300 . ? C193 H19B 0.9300 . ? C194 N5 1.463(4) . ? C194 H19C 0.9600 . ? C194 H19D 0.9600 . ? C194 H19E 0.9600 . ? C196 H19F 0.9300 . ? C200 N12 1.460(6) . ? C200 H20A 0.9600 . ? C200 H20B 0.9600 . ? C200 H20C 0.9600 . ? C204 C210 1.441(7) . ? C204 N6 1.460(5) . ? C204 H20D 0.9700 . ? C204 H20E 0.9700 . ? C208 N7 1.465(6) . ? C208 H20F 0.9600 . ? C208 H20G 0.9600 . ? C208 H20H 0.9600 . ? C210 C219 1.458(6) . ? C210 H21A 0.9700 . ? C210 H21B 0.9700 . ? C211 N7 1.442(6) . ? C211 C315 1.522(7) . ? C211 H21C 0.9700 . ? C211 H21D 0.9700 . ? C212 O16 1.206(6) . ? C212 N11 1.346(7) . ? C212 N8 1.365(7) . ? C214 C500 1.319(14) . ? C214 N3 1.463(5) . ? C214 C308 1.540(8) . ? C215 H21G 0.9300 . ? C219 N4 1.464(5) . ? C219 H21H 0.9700 . ? C219 H21I 0.9700 . ? C220 N5 1.472(4) . ? C220 C500 1.497(15) . ? C220 C308 1.506(9) . ? C223 H22C 0.9300 . ? C228 O17 1.208(6) . ? C228 N12 1.355(6) . ? C228 N9 1.372(6) . ? C236 N6 1.456(5) . ? C236 H23A 0.9600 . ? C236 H23B 0.9600 . ? C236 H23C 0.9600 . ? C237 N4 1.451(5) . ? C237 H23D 0.9600 . ? C237 H23E 0.9600 . ? C237 H23F 0.9600 . ? C241 C246 1.370(5) . ? C241 H24A 0.9300 . ? C246 H24B 0.9300 . ? C247 H24C 0.9300 . ? C300 N9 1.384(10) . ? C300 H30A 0.9600 . ? C300 H30B 0.9600 . ? C300 H30C 0.9600 . ? C301 N12 1.454(7) . ? C301 C326 1.463(10) . ? C301 H30D 0.9700 . ? C301 H30E 0.9700 . ? C303 N11 1.469(8) . ? C303 C321 1.516(12) . ? C303 H30F 0.9700 . ? C303 H30G 0.9700 . ? C304 N8 1.440(9) . ? C304 H30H 0.9600 . ? C304 H30I 0.9600 . ? C304 H30J 0.9600 . ? C306 N14 1.447(8) . ? C306 H30K 0.9600 . ? C306 H30L 0.9600 . ? C306 H30M 0.9600 . ? C307 N13 1.443(7) . ? C307 H30N 0.9600 . ? C307 H30O 0.9600 . ? C307 H30P 0.9600 . ? C308 C500 0.859(14) . ? C309 N10 1.472(7) . ? C309 H30R 0.9600 . ? C309 H30S 0.9600 . ? C309 H30T 0.9600 . ? C310 O18 1.212(7) . ? C310 N14 1.356(7) . ? C310 N13 1.376(8) . ? C312 N11 1.487(7) . ? C312 H31A 0.9600 . ? C312 H31B 0.9600 . ? C312 H31C 0.9600 . ? C313 N10 1.457(8) . ? C313 C315 1.502(8) . ? C313 H31D 0.9700 . ? C313 H31E 0.9700 . ? C315 H31F 0.9700 . ? C315 H31G 0.9700 . ? C320 C321 1.267(11) . ? C320 N8 1.420(9) . ? C320 H32A 0.9300 . ? C321 H32B 0.9300 . ? C322 C324 1.323(11) . ? C322 N13 1.381(9) . ? C322 H32C 0.9300 . ? C323 N14 1.400(9) . ? C323 C324 1.451(12) . ? C323 H32D 0.9700 . ? C323 H32E 0.9700 . ? C324 H32F 0.9300 . ? C325 N9 1.498(11) . ? C325 C326 1.509(13) . ? C325 H32G 0.9700 . ? C325 H32H 0.9700 . ? C326 H32I 0.9700 . ? C326 H32J 0.9700 . ? C328 N3 1.450(5) . ? C328 H32K 0.9600 . ? C328 H32L 0.9600 . ? C328 H32M 0.9600 . ? O1 Zn1 1.950(2) 1_565 ? O4 Zn1 1.948(2) 1_564 ? O8 Zn3 1.955(2) 1_545 ? O10 Zn3 1.924(2) 1_546 ? O11 Zn2 2.069(2) 1_564 ? O12 Zn2 2.131(2) 1_546 ? O13 Zn2 2.055(2) 1_545 ? O14 Zn2 2.027(2) 1_565 ? 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 O4 Zn1 O1 118.75(9) 1_546 1_545 ? O4 Zn1 O3 99.45(9) 1_546 . ? O1 Zn1 O3 97.86(9) 1_545 . ? O4 Zn1 O5 117.18(11) 1_546 . ? O1 Zn1 O5 119.29(12) 1_545 . ? O3 Zn1 O5 94.60(9) . . ? O4 Zn1 O2 93.08(10) 1_546 . ? O1 Zn1 O2 95.98(10) 1_545 . ? O3 Zn1 O2 153.89(8) . . ? O5 Zn1 O2 59.30(9) . . ? O4 Zn1 C177 106.93(10) 1_546 . ? O1 Zn1 C177 109.89(10) 1_545 . ? O3 Zn1 C177 124.51(9) . . ? O5 Zn1 C177 29.92(10) . . ? O2 Zn1 C177 29.38(9) . . ? O14 Zn2 O13 178.10(9) 1_545 1_565 ? O14 Zn2 O2 92.02(9) 1_545 . ? O13 Zn2 O2 86.93(10) 1_565 . ? O14 Zn2 O11 92.69(9) 1_545 1_546 ? O13 Zn2 O11 88.95(9) 1_565 1_546 ? O2 Zn2 O11 93.39(9) . 1_546 ? O14 Zn2 O12 85.87(9) 1_545 1_564 ? O13 Zn2 O12 92.49(9) 1_565 1_564 ? O2 Zn2 O12 86.70(10) . 1_564 ? O11 Zn2 O12 178.56(9) 1_546 1_564 ? O14 Zn2 O7 89.29(8) 1_545 . ? O13 Zn2 O7 91.62(8) 1_565 . ? O2 Zn2 O7 174.79(9) . . ? O11 Zn2 O7 91.58(8) 1_546 . ? O12 Zn2 O7 88.37(9) 1_564 . ? O14 Zn2 Zn3 113.87(6) 1_545 . ? O13 Zn2 Zn3 66.10(6) 1_565 . ? O2 Zn2 Zn3 137.37(6) . . ? O11 Zn2 Zn3 117.15(6) 1_546 . ? O12 Zn2 Zn3 63.52(6) 1_564 . ? O7 Zn2 Zn3 37.96(5) . . ? O10 Zn3 O9 110.21(10) 1_564 . ? O10 Zn3 O8 110.95(10) 1_564 1_565 ? O9 Zn3 O8 99.66(10) . 1_565 ? O10 Zn3 O7 119.16(9) 1_564 . ? O9 Zn3 O7 112.54(9) . . ? O8 Zn3 O7 102.24(9) 1_565 . ? O10 Zn3 Zn2 90.24(7) 1_564 . ? O9 Zn3 Zn2 154.85(7) . . ? O8 Zn3 Zn2 85.74(7) 1_565 . ? O7 Zn3 Zn2 42.56(6) . . ? C125 C8 C115 117.0(3) . . ? C125 C8 C85 121.4(3) . . ? C115 C8 C85 121.5(3) . . ? O14 C38 O1 126.3(3) . . ? O14 C38 C57 116.9(3) . . ? O1 C38 C57 116.8(3) . . ? O13 C42 O8 125.6(3) . . ? O13 C42 C123 117.9(3) . . ? O8 C42 C123 116.6(3) . . ? C56 C43 C87 120.7(3) . . ? C56 C43 H43A 119.6 . . ? C87 C43 H43A 119.6 . . ? O3 C46 N3 120.4(3) . . ? O3 C46 N5 120.3(3) . . ? N3 C46 N5 119.3(3) . . ? O11 C52 O4 125.7(3) . . ? O11 C52 C86 117.7(3) . . ? O4 C52 C86 116.7(3) . . ? C167 C54 C153 118.7(3) . . ? C167 C54 N1 121.1(3) . . ? C153 C54 N1 120.2(3) . . ? C169 C55 C173 118.7(3) . . ? C169 C55 N2 121.5(3) . . ? C173 C55 N2 119.8(3) . . ? C86 C56 C43 121.1(3) . . ? C86 C56 H56A 119.5 . . ? C43 C56 H56A 119.5 . . ? C133 C57 C119 118.4(3) . . ? C133 C57 C38 120.2(3) . . ? C119 C57 C38 121.4(3) . . ? C69 C59 C123 120.9(3) . . ? C69 C59 H59A 119.5 . . ? C123 C59 H59A 119.5 . . ? C78 C60 C160 117.2(3) . . ? C78 C60 C87 121.6(3) . . ? C160 C60 C87 121.1(3) . . ? C118 C61 C102 120.6(3) . . ? C118 C61 H61A 119.7 . . ? C102 C61 H61A 119.7 . . ? O9 C62 N4 119.5(3) . . ? O9 C62 N6 119.6(3) . . ? N4 C62 N6 120.8(3) . . ? C77 C65 C118 118.9(3) . . ? C77 C65 C73 120.9(3) . . ? C118 C65 C73 120.1(3) . . ? C59 C69 C72 120.5(3) . . ? C59 C69 H69A 119.8 . . ? C72 C69 H69A 119.8 . . ? C183 C71 C92 119.3(3) . . ? C183 C71 N1 121.2(3) . . ? C92 C71 N1 119.5(3) . . ? C196 C72 C69 118.1(3) . . ? C196 C72 C111 119.9(3) . . ? C69 C72 C111 122.0(3) . . ? O6 C73 O7 122.4(3) . . ? O6 C73 C65 122.1(3) . . ? O7 C73 C65 115.3(3) . . ? C79 C77 C65 120.7(3) . . ? C79 C77 H77A 119.6 . . ? C65 C77 H77A 119.6 . . ? C89 C78 C60 121.5(3) . . ? C89 C78 H78A 119.3 . . ? C60 C78 H78A 119.3 . . ? C77 C79 C102 121.0(3) . . ? C77 C79 H79A 119.5 . . ? C102 C79 H79A 119.5 . . ? C89 C81 C105 118.6(3) . . ? C89 C81 N1 122.4(3) . . ? C105 C81 N1 119.0(3) . . ? C186 C85 C106 117.7(3) . . ? C186 C85 C8 120.7(3) . . ? C106 C85 C8 121.5(3) . . ? C56 C86 C109 119.0(3) . . ? C56 C86 C52 119.7(3) . . ? C109 C86 C52 121.3(3) . . ? C147 C87 C43 117.9(3) . . ? C147 C87 C60 121.7(3) . . ? C43 C87 C60 120.4(3) . . ? C78 C89 C81 121.0(3) . . ? C78 C89 H89A 119.5 . . ? C81 C89 H89A 119.5 . . ? C98 C92 C71 120.1(3) . . ? C98 C92 H92A 119.9 . . ? C71 C92 H92A 119.9 . . ? C135 C96 C140 116.9(3) . . ? C135 C96 C102 121.1(3) . . ? C140 C96 C102 122.0(3) . . ? C92 C98 C99 121.6(3) . . ? C92 C98 H98A 119.2 . . ? C99 C98 H98A 119.2 . . ? C223 C99 C98 117.5(3) . . ? C223 C99 C149 121.1(3) . . ? C98 C99 C149 121.4(3) . . ? C79 C102 C61 117.9(3) . . ? C79 C102 C96 122.2(3) . . ? C61 C102 C96 119.9(3) . . ? C160 C105 C81 120.3(3) . . ? C160 C105 H10A 119.9 . . ? C81 C105 H10A 119.9 . . ? C133 C106 C85 121.3(3) . . ? C133 C106 H10B 119.4 . . ? C85 C106 H10B 119.4 . . ? C185 C107 C145 118.8(3) . . ? C185 C107 N2 119.5(3) . . ? C145 C107 N2 121.6(3) . . ? C147 C109 C86 119.9(3) . . ? C147 C109 H10C 120.0 . . ? C86 C109 H10C 120.0 . . ? C247 C111 C126 118.1(3) . . ? C247 C111 C72 121.0(3) . . ? C126 C111 C72 120.9(3) . . ? C153 C115 C8 121.3(3) . . ? C153 C115 H11A 119.4 . . ? C8 C115 H11A 119.4 . . ? C61 C118 C65 120.9(3) . . ? C61 C118 H11B 119.5 . . ? C65 C118 H11B 119.5 . . ? C186 C119 C57 120.6(3) . . ? C186 C119 H11C 119.7 . . ? C57 C119 H11C 119.7 . . ? C174 C121 C143 119.8(3) . . ? C174 C121 H12A 120.1 . . ? C143 C121 H12A 120.1 . . ? C59 C123 C129 118.9(3) . . ? C59 C123 C42 121.3(3) . . ? C129 C123 C42 119.7(3) . . ? C8 C125 C167 121.9(3) . . ? C8 C125 H12B 119.0 . . ? C167 C125 H12B 119.0 . . ? C185 C126 C111 120.8(3) . . ? C185 C126 H12C 119.6 . . ? C111 C126 H12C 119.6 . . ? C196 C129 C123 120.7(3) . . ? C196 C129 H12D 119.7 . . ? C123 C129 H12D 119.7 . . ? O12 C130 O10 125.3(3) . . ? O12 C130 C155 118.5(3) . . ? O10 C130 C155 116.1(3) . . ? C106 C133 C57 120.7(3) . . ? C106 C133 H13A 119.7 . . ? C57 C133 H13A 119.7 . . ? C173 C135 C96 121.7(3) . . ? C173 C135 H13B 119.1 . . ? C96 C135 H13B 119.1 . . ? C169 C140 C96 122.0(3) . . ? C169 C140 H14A 119.0 . . ? C96 C140 H14A 119.0 . . ? C121 C143 C163 118.8(3) . . ? C121 C143 N2 121.4(3) . . ? C163 C143 N2 119.9(3) . . ? C193 C144 C174 117.5(3) . . ? C193 C144 C182 121.1(3) . . ? C174 C144 C182 121.4(3) . . ? C247 C145 C107 120.3(3) . . ? C247 C145 H14B 119.9 . . ? C107 C145 H14B 119.9 . . ? C109 C147 C87 121.3(3) . . ? C109 C147 H14C 119.3 . . ? C87 C147 H14C 119.3 . . ? C215 C149 C241 116.3(3) . . ? C215 C149 C99 121.0(3) . . ? C241 C149 C99 122.6(3) . . ? C115 C153 C54 121.1(3) . . ? C115 C153 H15A 119.5 . . ? C54 C153 H15A 119.5 . . ? C190 C154 C155 120.3(3) . . ? C190 C154 H15B 119.9 . . ? C155 C154 H15B 119.9 . . ? C188 C155 C154 119.1(3) . . ? C188 C155 C130 120.0(3) . . ? C154 C155 C130 120.9(3) . . ? C105 C160 C60 121.4(3) . . ? C105 C160 H16A 119.3 . . ? C60 C160 H16A 119.3 . . ? O15 C161 N10 120.4(5) . . ? O15 C161 N7 120.7(5) . . ? N10 C161 N7 118.8(5) . . ? C181 C162 C246 116.5(3) . . ? C181 C162 C177 121.9(3) . . ? C246 C162 C177 121.5(3) . . ? C193 C163 C143 120.7(3) . . ? C193 C163 H16B 119.7 . . ? C143 C163 H16B 119.7 . . ? C54 C167 C125 119.8(3) . . ? C54 C167 H16C 120.1 . . ? C125 C167 H16C 120.1 . . ? C140 C169 C55 120.2(3) . . ? C140 C169 H16D 119.9 . . ? C55 C169 H16D 119.9 . . ? C135 C173 C55 120.5(3) . . ? C135 C173 H17A 119.7 . . ? C55 C173 H17A 119.7 . . ? C121 C174 C144 121.6(3) . . ? C121 C174 H17B 119.2 . . ? C144 C174 H17B 119.2 . . ? O2 C177 O5 118.4(3) . . ? O2 C177 C162 121.1(3) . . ? O5 C177 C162 120.5(3) . . ? O2 C177 Zn1 64.13(16) . . ? O5 C177 Zn1 54.28(16) . . ? C162 C177 Zn1 174.6(2) . . ? C188 C180 C182 121.2(3) . . ? C188 C180 H18A 119.4 . . ? C182 C180 H18A 119.4 . . ? C162 C181 C215 121.7(4) . . ? C162 C181 H18B 119.1 . . ? C215 C181 H18B 119.1 . . ? C190 C182 C180 117.8(3) . . ? C190 C182 C144 121.3(3) . . ? C180 C182 C144 120.9(3) . . ? C71 C183 C223 120.5(3) . . ? C71 C183 H18C 119.8 . . ? C223 C183 H18C 119.8 . . ? C107 C185 C126 120.8(3) . . ? C107 C185 H18D 119.6 . . ? C126 C185 H18D 119.6 . . ? C119 C186 C85 121.3(3) . . ? C119 C186 H18E 119.4 . . ? C85 C186 H18E 119.4 . . ? C180 C188 C155 120.4(3) . . ? C180 C188 H18F 119.8 . . ? C155 C188 H18F 119.8 . . ? C154 C190 C182 121.0(3) . . ? C154 C190 H19A 119.5 . . ? C182 C190 H19A 119.5 . . ? C163 C193 C144 121.5(3) . . ? C163 C193 H19B 119.3 . . ? C144 C193 H19B 119.3 . . ? N5 C194 H19C 109.5 . . ? N5 C194 H19D 109.5 . . ? H19C C194 H19D 109.5 . . ? N5 C194 H19E 109.5 . . ? H19C C194 H19E 109.5 . . ? H19D C194 H19E 109.5 . . ? C129 C196 C72 120.9(3) . . ? C129 C196 H19F 119.6 . . ? C72 C196 H19F 119.6 . . ? N12 C200 H20A 109.5 . . ? N12 C200 H20B 109.5 . . ? H20A C200 H20B 109.5 . . ? N12 C200 H20C 109.5 . . ? H20A C200 H20C 109.5 . . ? H20B C200 H20C 109.5 . . ? C210 C204 N6 111.1(4) . . ? C210 C204 H20D 109.4 . . ? N6 C204 H20D 109.4 . . ? C210 C204 H20E 109.4 . . ? N6 C204 H20E 109.4 . . ? H20D C204 H20E 108.0 . . ? N7 C208 H20F 109.5 . . ? N7 C208 H20G 109.5 . . ? H20F C208 H20G 109.5 . . ? N7 C208 H20H 109.5 . . ? H20F C208 H20H 109.5 . . ? H20G C208 H20H 109.5 . . ? C204 C210 C219 114.1(4) . . ? C204 C210 H21A 108.7 . . ? C219 C210 H21A 108.7 . . ? C204 C210 H21B 108.7 . . ? C219 C210 H21B 108.7 . . ? H21A C210 H21B 107.6 . . ? N7 C211 C315 109.2(4) . . ? N7 C211 H21C 109.8 . . ? C315 C211 H21C 109.8 . . ? N7 C211 H21D 109.8 . . ? C315 C211 H21D 109.8 . . ? H21C C211 H21D 108.3 . . ? O16 C212 N11 119.9(5) . . ? O16 C212 N8 121.0(5) . . ? N11 C212 N8 119.1(5) . . ? C500 C214 N3 113.9(7) . . ? C500 C214 C308 33.9(6) . . ? N3 C214 C308 110.4(4) . . ? C181 C215 C149 122.2(4) . . ? C181 C215 H21G 118.9 . . ? C149 C215 H21G 118.9 . . ? C210 C219 N4 112.3(3) . . ? C210 C219 H21H 109.1 . . ? N4 C219 H21H 109.1 . . ? C210 C219 H21I 109.1 . . ? N4 C219 H21I 109.1 . . ? H21H C219 H21I 107.9 . . ? N5 C220 C500 110.2(6) . . ? N5 C220 C308 110.7(4) . . ? C500 C220 C308 33.2(6) . . ? C99 C223 C183 120.9(3) . . ? C99 C223 H22C 119.6 . . ? C183 C223 H22C 119.6 . . ? O17 C228 N12 121.1(4) . . ? O17 C228 N9 122.7(5) . . ? N12 C228 N9 116.1(5) . . ? N6 C236 H23A 109.5 . . ? N6 C236 H23B 109.5 . . ? H23A C236 H23B 109.5 . . ? N6 C236 H23C 109.5 . . ? H23A C236 H23C 109.5 . . ? H23B C236 H23C 109.5 . . ? N4 C237 H23D 109.5 . . ? N4 C237 H23E 109.5 . . ? H23D C237 H23E 109.5 . . ? N4 C237 H23F 109.5 . . ? H23D C237 H23F 109.5 . . ? H23E C237 H23F 109.5 . . ? C246 C241 C149 121.5(3) . . ? C246 C241 H24A 119.2 . . ? C149 C241 H24A 119.2 . . ? C241 C246 C162 121.6(3) . . ? C241 C246 H24B 119.2 . . ? C162 C246 H24B 119.2 . . ? C145 C247 C111 121.2(3) . . ? C145 C247 H24C 119.4 . . ? C111 C247 H24C 119.4 . . ? N9 C300 H30A 109.5 . . ? N9 C300 H30B 109.5 . . ? H30A C300 H30B 109.5 . . ? N9 C300 H30C 109.5 . . ? H30A C300 H30C 109.5 . . ? H30B C300 H30C 109.5 . . ? N12 C301 C326 108.9(6) . . ? N12 C301 H30D 109.9 . . ? C326 C301 H30D 109.9 . . ? N12 C301 H30E 109.9 . . ? C326 C301 H30E 109.9 . . ? H30D C301 H30E 108.3 . . ? N11 C303 C321 111.0(7) . . ? N11 C303 H30F 109.4 . . ? C321 C303 H30F 109.4 . . ? N11 C303 H30G 109.4 . . ? C321 C303 H30G 109.4 . . ? H30F C303 H30G 108.0 . . ? N8 C304 H30H 109.5 . . ? N8 C304 H30I 109.5 . . ? H30H C304 H30I 109.5 . . ? N8 C304 H30J 109.5 . . ? H30H C304 H30J 109.5 . . ? H30I C304 H30J 109.5 . . ? N14 C306 H30K 109.5 . . ? N14 C306 H30L 109.5 . . ? H30K C306 H30L 109.5 . . ? N14 C306 H30M 109.5 . . ? H30K C306 H30M 109.5 . . ? H30L C306 H30M 109.5 . . ? N13 C307 H30N 109.5 . . ? N13 C307 H30O 109.5 . . ? H30N C307 H30O 109.5 . . ? N13 C307 H30P 109.5 . . ? H30N C307 H30P 109.5 . . ? H30O C307 H30P 109.5 . . ? C500 C308 C220 72.8(12) . . ? C500 C308 C214 58.8(11) . . ? C220 C308 C214 110.3(5) . . ? N10 C309 H30R 109.5 . . ? N10 C309 H30S 109.5 . . ? H30R C309 H30S 109.5 . . ? N10 C309 H30T 109.5 . . ? H30R C309 H30T 109.5 . . ? H30S C309 H30T 109.5 . . ? O18 C310 N14 122.2(7) . . ? O18 C310 N13 120.9(6) . . ? N14 C310 N13 116.9(5) . . ? N11 C312 H31A 109.5 . . ? N11 C312 H31B 109.5 . . ? H31A C312 H31B 109.5 . . ? N11 C312 H31C 109.5 . . ? H31A C312 H31C 109.5 . . ? H31B C312 H31C 109.5 . . ? N10 C313 C315 112.4(5) . . ? N10 C313 H31D 109.1 . . ? C315 C313 H31D 109.1 . . ? N10 C313 H31E 109.1 . . ? C315 C313 H31E 109.1 . . ? H31D C313 H31E 107.9 . . ? C313 C315 C211 108.2(4) . . ? C313 C315 H31F 110.1 . . ? C211 C315 H31F 110.1 . . ? C313 C315 H31G 110.1 . . ? C211 C315 H31G 110.1 . . ? H31F C315 H31G 108.4 . . ? C321 C320 N8 117.3(7) . . ? C321 C320 H32A 121.4 . . ? N8 C320 H32A 121.4 . . ? C320 C321 C303 120.9(9) . . ? C320 C321 H32B 119.6 . . ? C303 C321 H32B 119.6 . . ? C324 C322 N13 117.2(9) . . ? C324 C322 H32C 121.4 . . ? N13 C322 H32C 121.4 . . ? N14 C323 C324 116.9(7) . . ? N14 C323 H32D 108.1 . . ? C324 C323 H32D 108.1 . . ? N14 C323 H32E 108.1 . . ? C324 C323 H32E 108.1 . . ? H32D C323 H32E 107.3 . . ? C322 C324 C323 119.9(9) . . ? C322 C324 H32F 120.0 . . ? C323 C324 H32F 120.0 . . ? N9 C325 C326 109.6(6) . . ? N9 C325 H32G 109.7 . . ? C326 C325 H32G 109.7 . . ? N9 C325 H32H 109.7 . . ? C326 C325 H32H 109.7 . . ? H32G C325 H32H 108.2 . . ? C301 C326 C325 110.4(9) . . ? C301 C326 H32I 109.6 . . ? C325 C326 H32I 109.6 . . ? C301 C326 H32J 109.6 . . ? C325 C326 H32J 109.6 . . ? H32I C326 H32J 108.1 . . ? N3 C328 H32K 109.5 . . ? N3 C328 H32L 109.5 . . ? H32K C328 H32L 109.5 . . ? N3 C328 H32M 109.5 . . ? H32K C328 H32M 109.5 . . ? H32L C328 H32M 109.5 . . ? C38 O1 Zn1 129.2(2) . 1_565 ? C177 O2 Zn2 167.0(2) . . ? C177 O2 Zn1 86.49(19) . . ? Zn2 O2 Zn1 106.18(9) . . ? C46 O3 Zn1 125.47(19) . . ? C52 O4 Zn1 125.2(2) . 1_564 ? C177 O5 Zn1 95.81(19) . . ? C73 O7 Zn3 109.95(18) . . ? C73 O7 Zn2 121.23(18) . . ? Zn3 O7 Zn2 99.48(8) . . ? C42 O8 Zn3 117.8(2) . 1_545 ? C62 O9 Zn3 129.3(2) . . ? C130 O10 Zn3 115.4(2) . 1_546 ? C52 O11 Zn2 138.4(2) . 1_564 ? C130 O12 Zn2 143.3(2) . 1_546 ? C42 O13 Zn2 139.2(2) . 1_545 ? C38 O14 Zn2 138.8(2) . 1_565 ? C81 N1 C54 120.3(2) . . ? C81 N1 C71 119.1(3) . . ? C54 N1 C71 117.8(2) . . ? C107 N2 C143 120.0(3) . . ? C107 N2 C55 117.7(3) . . ? C143 N2 C55 120.8(3) . . ? C46 N3 C328 119.3(3) . . ? C46 N3 C214 124.1(3) . . ? C328 N3 C214 116.6(3) . . ? C62 N4 C237 118.9(3) . . ? C62 N4 C219 122.4(3) . . ? C237 N4 C219 117.7(3) . . ? C46 N5 C194 120.5(3) . . ? C46 N5 C220 123.6(3) . . ? C194 N5 C220 115.7(3) . . ? C62 N6 C236 121.6(3) . . ? C62 N6 C204 120.1(3) . . ? C236 N6 C204 118.2(3) . . ? C161 N7 C211 124.2(4) . . ? C161 N7 C208 119.6(4) . . ? C211 N7 C208 114.7(4) . . ? C212 N8 C320 122.5(6) . . ? C212 N8 C304 118.4(6) . . ? C320 N8 C304 118.9(6) . . ? C228 N9 C300 118.9(7) . . ? C228 N9 C325 121.5(6) . . ? C300 N9 C325 117.9(7) . . ? C161 N10 C313 122.2(4) . . ? C161 N10 C309 118.7(6) . . ? C313 N10 C309 117.9(6) . . ? C212 N11 C303 121.8(6) . . ? C212 N11 C312 119.6(5) . . ? C303 N11 C312 118.6(6) . . ? C228 N12 C301 126.6(5) . . ? C228 N12 C200 117.6(4) . . ? C301 N12 C200 114.6(5) . . ? C310 N13 C322 124.6(6) . . ? C310 N13 C307 117.0(5) . . ? C322 N13 C307 118.3(6) . . ? C310 N14 C323 121.5(6) . . ? C310 N14 C306 117.9(6) . . ? C323 N14 C306 120.4(6) . . ? C308 C500 C214 87.3(13) . . ? C308 C500 C220 74.0(12) . . ? C214 C500 C220 125.2(11) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 62.61 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.635 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.069 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.214 0.957 0.385 9.9 -0.3 2 0.500 0.500 1.000 1232.6 30.9 3 0.786 0.042 0.615 9.9 -0.2 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 948625' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C97 H67 N6 O13 Zn3' _chemical_formula_weight 1720.74 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.9124(2) _cell_length_b 36.7010(3) _cell_length_c 38.7102(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.5990(10) _cell_angle_gamma 90.00 _cell_volume 30599.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 31901 _cell_measurement_theta_min 3.0474 _cell_measurement_theta_max 74.2377 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 0.7470(1) _exptl_crystal_density_diffrn 0.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7127 _exptl_absorpt_coefficient_mu 0.504 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 32294 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 20.00 _reflns_number_total 14260 _reflns_number_gt 11791 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1754P)^2^+30.6576P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14260 _refine_ls_number_parameters 1046 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0910 _refine_ls_R_factor_gt 0.0835 _refine_ls_wR_factor_ref 0.2567 _refine_ls_wR_factor_gt 0.2478 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _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 1.36950(3) 0.039682(18) 0.031600(18) 0.0628(3) Uani 1 1 d . . . Zn3 Zn 0.37437(14) 0.08812(6) 0.11523(9) 0.0605(6) Uani 0.75 1 d P . . Zn3' Zn 0.3856(4) 0.0755(3) 0.1182(2) 0.099(3) Uani 0.25 1 d P . . Zn4 Zn 0.84229(3) -0.41383(2) 0.211531(19) 0.0716(3) Uani 1 1 d . . . N1 N 0.3298(2) -0.24979(18) 0.16977(16) 0.0879(18) Uani 1 1 d . . . N2 N 0.8763(2) 0.20115(12) 0.05644(16) 0.0716(15) Uani 1 1 d . . . N3 N 1.3863(2) 0.03916(12) -0.01926(13) 0.0592(12) Uani 1 1 d . . . N4 N 1.3677(2) -0.06382(13) -0.23899(12) 0.0596(12) Uani 1 1 d . . . O1 O 0.7918(4) -0.3594(3) 0.2301(2) 0.221(6) Uani 1 1 d . . . O2 O 0.3425(3) 0.13382(13) 0.08699(14) 0.122(2) Uani 1 1 d . . . O3 O 0.7968(3) 0.48676(12) 0.02735(14) 0.0920(14) Uani 1 1 d . . . O4 O 0.7554(2) -0.4003(2) 0.19456(16) 0.1063(18) Uani 1 1 d . . . O5 O 0.3412(3) 0.03857(14) 0.18788(14) 0.0967(15) Uani 1 1 d . . . O6 O 0.8976(2) 0.49129(11) 0.04908(11) 0.0758(12) Uani 1 1 d . . . O7 O -0.07664(19) -0.38962(11) 0.21186(12) 0.0706(11) Uani 1 1 d . . . O8 O 0.3903(2) 0.03807(13) 0.14426(13) 0.0859(13) Uani 1 1 d . . . O9 O -0.11300(18) -0.38044(12) 0.15558(12) 0.0726(11) Uani 1 1 d . . . O10 O 1.31038(18) 0.06235(11) 0.08314(14) 0.0761(12) Uani 1 1 d . . . O11 O 0.44746(19) 0.06799(11) 0.04830(12) 0.0666(10) Uani 1 1 d . . . O12 O 0.45986(19) 0.08332(13) 0.10437(12) 0.0802(13) Uani 1 1 d . . . O13 O 1.29644(18) 0.07195(10) 0.02585(13) 0.0721(11) Uani 1 1 d . . . C1 C 0.303(2) 0.2305(14) 0.1142(13) 0.48(2) Uiso 1 1 d . . . C2 C 0.3841(11) 0.2402(7) 0.1131(6) 0.258(9) Uiso 1 1 d . . . C3 C 0.2664(10) 0.1750(6) 0.1266(6) 0.268(10) Uiso 1 1 d . . . H3B H 0.2637 0.1489 0.1248 0.403 Uiso 1 1 calc R . . H3C H 0.2261 0.1854 0.1186 0.403 Uiso 1 1 calc R . . H3D H 0.2812 0.1818 0.1506 0.403 Uiso 1 1 calc R . . C4 C 0.4137(11) 0.2256(7) 0.0762(6) 0.267(10) Uiso 1 1 d . . . C5 C 0.4168(6) 0.1647(4) 0.0517(3) 0.164(4) Uiso 1 1 d . . . H5A H 0.4028 0.1399 0.0503 0.247 Uiso 1 1 calc R . . H5B H 0.4610 0.1653 0.0596 0.247 Uiso 1 1 calc R . . H5C H 0.4067 0.1759 0.0290 0.247 Uiso 1 1 calc R . . C6 C 0.3424(6) 0.1672(4) 0.0908(3) 0.136(3) Uiso 1 1 d . . . C7 C 0.6782(4) -0.3220(4) 0.2181(3) 0.146(4) Uani 1 1 d . . . H7A H 0.7137 -0.3106 0.2302 0.176 Uiso 1 1 calc R . . N5 N 0.3056(6) 0.1873(3) 0.1067(4) 0.198(6) Uani 1 1 d . . . N6 N 0.3857(4) 0.1852(2) 0.0773(2) 0.126(2) Uiso 1 1 d . . . C10 C 1.3926(5) 0.0689(2) -0.0732(2) 0.116(3) Uani 1 1 d . . . H10A H 1.3783 0.0876 -0.0889 0.139 Uiso 1 1 calc R . . C11 C 0.5804(4) -0.3509(3) 0.1787(3) 0.130(4) Uani 1 1 d . . . H11A H 0.5491 -0.3604 0.1616 0.156 Uiso 1 1 calc R . . C12 C 0.3054(4) -0.1895(2) 0.1894(2) 0.104(3) Uani 1 1 d . . . H12A H 0.2830 -0.2002 0.2049 0.125 Uiso 1 1 calc R . . C13 C 1.4340(4) 0.0275(2) -0.14336(19) 0.101(2) Uani 1 1 d . . . H13A H 1.4148 0.0383 -0.1643 0.121 Uiso 1 1 calc R . . C14 C 1.4631(5) 0.0497(3) -0.1133(2) 0.125(4) Uani 1 1 d . . . H14A H 1.4597 0.0752 -0.1201 0.150 Uiso 1 1 calc R . . H14B H 1.5069 0.0438 -0.1076 0.150 Uiso 1 1 calc R . . C15 C 1.4349(4) 0.0448(2) -0.0803(2) 0.084(2) Uani 1 1 d . . . C16 C 1.4361(4) -0.0118(2) -0.13965(19) 0.097(2) Uani 1 1 d . . . H16A H 1.4118 -0.0189 -0.1222 0.116 Uiso 1 1 calc R . . H16B H 1.4787 -0.0192 -0.1311 0.116 Uiso 1 1 calc R . . C17 C 1.4478(4) -0.0384(2) -0.1968(2) 0.105(3) Uani 1 1 d . . . H17A H 1.4898 -0.0327 -0.1910 0.126 Uiso 1 1 calc R . . C18 C 0.3419(5) -0.0726(2) 0.1950(2) 0.113(3) Uani 1 1 d . . . H18A H 0.3317 -0.0839 0.2146 0.135 Uiso 1 1 calc R . . C19 C 0.3740(6) -0.1568(2) 0.1463(3) 0.137(4) Uani 1 1 d . . . H19A H 0.3995 -0.1464 0.1323 0.164 Uiso 1 1 calc R . . C20 C 1.4520(3) 0.0181(2) -0.0571(2) 0.090(2) Uani 1 1 d . . . H20A H 1.4811 0.0009 -0.0611 0.108 Uiso 1 1 calc R . . C21 C 0.3463(5) -0.0356(2) 0.1949(2) 0.107(3) Uani 1 1 d . . . H21A H 0.3392 -0.0223 0.2142 0.128 Uiso 1 1 calc R . . C22 C 0.6840(4) -0.3564(3) 0.20435(18) 0.099(3) Uani 1 1 d . . . C23 C 0.6368(4) -0.3682(3) 0.1839(3) 0.132(4) Uani 1 1 d . . . H23A H 0.6403 -0.3897 0.1717 0.159 Uiso 1 1 calc R . . C24 C 0.9231(3) 0.26064(16) 0.0696(2) 0.0777(19) Uani 1 1 d . . . H24A H 0.9595 0.2497 0.0810 0.093 Uiso 1 1 calc R . . C25 C 0.4952(4) -0.2721(3) 0.2045(3) 0.133(4) Uani 1 1 d . . . H25A H 0.5274 -0.2615 0.2203 0.159 Uiso 1 1 calc R . . C26 C 1.4253(3) -0.0533(2) -0.2288(2) 0.100(3) Uani 1 1 d . . . H26A H 1.4526 -0.0562 -0.2444 0.120 Uiso 1 1 calc R . . C27 C 0.3984(3) -0.3017(3) 0.1626(2) 0.106(3) Uani 1 1 d . . . H27A H 0.3652 -0.3123 0.1475 0.127 Uiso 1 1 calc R . . C28 C 0.3894(3) -0.2691(2) 0.1778(2) 0.085(2) Uani 1 1 d . . . C29 C 0.3655(5) -0.1947(2) 0.1456(3) 0.129(4) Uani 1 1 d . . . H29A H 0.3825 -0.2089 0.1298 0.155 Uiso 1 1 calc R . . C30 C 0.3451(3) -0.1345(2) 0.16751(17) 0.0801(19) Uani 1 1 d . . . C31 C 1.3706(4) 0.06524(19) -0.0412(2) 0.101(3) Uani 1 1 d . . . H31A H 1.3431 0.0827 -0.0358 0.121 Uiso 1 1 calc R . . C32 C 0.8479(4) 0.47312(17) 0.04004(17) 0.0703(17) Uani 1 1 d . . . C33 C 0.5670(3) -0.3220(3) 0.19583(17) 0.093(2) Uani 1 1 d . . . C34 C 0.0372(3) -0.35688(19) 0.20788(17) 0.0789(19) Uani 1 1 d . . . H34A H 0.0333 -0.3692 0.2283 0.095 Uiso 1 1 calc R . . C35 C 0.0916(3) -0.33981(18) 0.20605(18) 0.0795(18) Uani 1 1 d . . . H35A H 0.1245 -0.3414 0.2250 0.095 Uiso 1 1 calc R . . C36 C 0.6225(4) -0.3037(4) 0.2146(3) 0.150(5) Uani 1 1 d . . . H36A H 0.6203 -0.2805 0.2240 0.180 Uiso 1 1 calc R . . C37 C 0.7469(4) -0.3735(3) 0.2099(2) 0.112(3) Uani 1 1 d . . . C38 C 1.3528(4) -0.0441(3) -0.1834(2) 0.131(4) Uani 1 1 d . . . H38A H 1.3251 -0.0414 -0.1681 0.157 Uiso 1 1 calc R . . C39 C 0.4389(4) -0.2543(3) 0.1981(3) 0.131(3) Uani 1 1 d . . . H39A H 0.4353 -0.2315 0.2081 0.157 Uiso 1 1 calc R . . C40 C 1.4115(4) -0.03196(17) -0.17393(17) 0.0790(19) Uani 1 1 d . . . C41 C 0.1629(3) -0.27016(16) 0.15489(18) 0.0702(16) Uani 1 1 d . . . H41A H 0.1262 -0.2602 0.1427 0.084 Uiso 1 1 calc R . . C42 C 0.2147(3) -0.3166(2) 0.1922(2) 0.087(2) Uani 1 1 d . . . H42A H 0.2141 -0.3384 0.2044 0.104 Uiso 1 1 calc R . . C43 C 1.3334(4) -0.0604(3) -0.2151(3) 0.134(4) Uani 1 1 d . . . H43A H 1.2932 -0.0696 -0.2199 0.160 Uiso 1 1 calc R . . C44 C 0.2710(3) -0.2982(2) 0.1917(2) 0.091(2) Uani 1 1 d . . . H44A H 0.3072 -0.3069 0.2056 0.109 Uiso 1 1 calc R . . C45 C 0.5062(3) -0.3034(2) 0.18967(18) 0.083(2) Uani 1 1 d . . . C46 C 0.4525(4) -0.3188(3) 0.1684(2) 0.112(3) Uani 1 1 d . . . H46A H 0.4556 -0.3416 0.1582 0.134 Uiso 1 1 calc R . . C47 C 0.3521(3) -0.09450(19) 0.16709(18) 0.0756(18) Uani 1 1 d . . . C48 C 0.2172(3) -0.25353(17) 0.15300(19) 0.0784(19) Uani 1 1 d . . . H48A H 0.2174 -0.2325 0.1397 0.094 Uiso 1 1 calc R . . C49 C 0.8673(3) 0.31553(16) 0.05112(17) 0.0651(16) Uani 1 1 d . . . C50 C 0.0484(3) -0.31850(16) 0.14912(18) 0.0705(17) Uani 1 1 d . . . H50A H 0.0510 -0.3045 0.1294 0.085 Uiso 1 1 calc R . . C51 C 0.8015(3) 0.41103(16) 0.04363(18) 0.0729(18) Uani 1 1 d . . . H51A H 0.7628 0.4222 0.0409 0.088 Uiso 1 1 calc R . . C52 C 0.9203(3) 0.29843(17) 0.0674(2) 0.0764(19) Uani 1 1 d . . . H52A H 0.9548 0.3122 0.0772 0.092 Uiso 1 1 calc R . . C53 C 0.2742(3) -0.26818(17) 0.17133(18) 0.0738(17) Uani 1 1 d . . . C54 C 1.1376(3) 0.11088(17) 0.08512(18) 0.0733(17) Uani 1 1 d . . . H54A H 1.1204 0.1108 0.1054 0.088 Uiso 1 1 calc R . . C55 C -0.0058(3) -0.33711(17) 0.15037(17) 0.0695(17) Uani 1 1 d . . . H55A H -0.0381 -0.3367 0.1311 0.083 Uiso 1 1 calc R . . C56 C 1.4272(3) 0.0160(2) -0.02777(17) 0.0772(18) Uani 1 1 d . . . H56A H 1.4399 -0.0031 -0.0124 0.093 Uiso 1 1 calc R . . C57 C 0.8180(3) 0.29483(15) 0.03686(18) 0.0688(16) Uani 1 1 d . . . H57A H 0.7815 0.3061 0.0261 0.083 Uiso 1 1 calc R . . C58 C 0.3708(3) -0.0755(2) 0.13951(19) 0.0793(19) Uani 1 1 d . . . H58A H 0.3798 -0.0885 0.1204 0.095 Uiso 1 1 calc R . . C59 C 0.3106(4) -0.1518(2) 0.1886(2) 0.095(2) Uani 1 1 d . . . H59A H 0.2899 -0.1379 0.2029 0.114 Uiso 1 1 calc R . . C60 C 0.9162(3) 0.37787(16) 0.05180(17) 0.0664(16) Uani 1 1 d . . . H60A H 0.9554 0.3673 0.0546 0.080 Uiso 1 1 calc R . . C61 C 0.8637(3) 0.35590(16) 0.05009(17) 0.0679(16) Uani 1 1 d . . . C62 C 0.9714(3) 0.19324(17) 0.0334(2) 0.085(2) Uani 1 1 d . . . H62A H 0.9603 0.2128 0.0183 0.102 Uiso 1 1 calc R . . C63 C 0.8527(3) 0.43126(16) 0.04486(16) 0.0679(16) Uani 1 1 d . . . C64 C 0.7549(2) 0.13032(15) 0.04542(18) 0.0665(16) Uani 1 1 d . . . H64A H 0.7450 0.1091 0.0326 0.080 Uiso 1 1 calc R . . C65 C 0.8229(2) 0.18181(15) 0.06058(19) 0.0690(17) Uani 1 1 d . . . C66 C 0.3612(3) -0.01784(19) 0.16639(15) 0.0702(17) Uani 1 1 d . . . C67 C 0.0993(3) -0.31997(15) 0.17626(16) 0.0656(16) Uani 1 1 d . . . C68 C 0.3320(3) -0.21085(18) 0.1682(2) 0.0765(18) Uani 1 1 d . . . C69 C 0.8069(3) 0.14980(16) 0.04144(19) 0.0711(18) Uani 1 1 d . . . H69A H 0.8315 0.1416 0.0259 0.085 Uiso 1 1 calc R . . C70 C 1.0049(3) 0.13476(16) 0.07804(17) 0.0655(16) Uani 1 1 d . . . H70A H 1.0151 0.1148 0.0928 0.079 Uiso 1 1 calc R . . C71 C 0.1599(3) -0.30120(17) 0.17417(16) 0.0702(17) Uani 1 1 d . . . C72 C 0.6370(3) 0.12079(17) 0.10284(17) 0.0664(16) Uani 1 1 d . . . H72A H 0.6620 0.1290 0.1234 0.080 Uiso 1 1 calc R . . C73 C 1.1836(3) 0.10657(16) 0.02490(16) 0.0634(15) Uani 1 1 d . . . H73A H 1.1975 0.1040 0.0037 0.076 Uiso 1 1 calc R . . C74 C 0.7330(2) 0.17341(15) 0.08739(16) 0.0617(15) Uani 1 1 d . . . H74A H 0.7086 0.1813 0.1032 0.074 Uiso 1 1 calc R . . C75 C 0.3763(3) -0.03817(17) 0.13978(18) 0.0711(17) Uani 1 1 d . . . H75A H 0.3906 -0.0266 0.1214 0.085 Uiso 1 1 calc R . . C76 C 0.6213(3) 0.10785(18) 0.04100(17) 0.0691(17) Uani 1 1 d . . . H76A H 0.6350 0.1081 0.0196 0.083 Uiso 1 1 calc R . . C77 C 0.8062(3) 0.37382(16) 0.04633(18) 0.0706(17) Uani 1 1 d . . . H77A H 0.7704 0.3601 0.0457 0.085 Uiso 1 1 calc R . . C78 C 0.9101(3) 0.41527(16) 0.04927(16) 0.0663(17) Uani 1 1 d . . . H78A H 0.9453 0.4297 0.0506 0.080 Uiso 1 1 calc R . . C79 C -0.0124(3) -0.35634(15) 0.18015(15) 0.0611(15) Uani 1 1 d . . . C80 C 0.8740(2) 0.23913(15) 0.05532(19) 0.0690(17) Uani 1 1 d . . . C81 C 0.9329(3) 0.18193(16) 0.0556(2) 0.0747(19) Uani 1 1 d . . . C82 C 0.8209(3) 0.25646(15) 0.03805(19) 0.0731(18) Uani 1 1 d . . . H82A H 0.7870 0.2428 0.0272 0.088 Uiso 1 1 calc R . . C83 C 1.0269(3) 0.17505(18) 0.0339(2) 0.0789(19) Uani 1 1 d . . . H83A H 1.0527 0.1829 0.0189 0.095 Uiso 1 1 calc R . . C84 C 0.7848(3) 0.19356(16) 0.08338(18) 0.0676(16) Uani 1 1 d . . . H84A H 0.7941 0.2150 0.0960 0.081 Uiso 1 1 calc R . . C85 C 0.6580(2) 0.12338(15) 0.07103(16) 0.0593(15) Uani 1 1 d . . . C86 C 0.4781(3) 0.07942(15) 0.07566(18) 0.0588(15) Uani 1 1 d . . . C87 C 1.1948(3) 0.09468(17) 0.08659(18) 0.0707(17) Uani 1 1 d . . . H87A H 1.2171 0.0857 0.1076 0.085 Uiso 1 1 calc R . . C88 C 1.0458(3) 0.14551(15) 0.05584(17) 0.0626(15) Uani 1 1 d . . . C89 C 0.9510(3) 0.15279(16) 0.07849(19) 0.0705(17) Uani 1 1 d . . . H89A H 0.9258 0.1457 0.0942 0.085 Uiso 1 1 calc R . . C90 C 0.5426(2) 0.09239(15) 0.07465(16) 0.0580(14) Uani 1 1 d . . . C91 C -0.0707(3) -0.37707(16) 0.18250(19) 0.0658(16) Uani 1 1 d . . . C92 C 1.1042(2) 0.12715(15) 0.05541(15) 0.0568(14) Uani 1 1 d . . . C93 C 0.3651(3) 0.02270(18) 0.16604(16) 0.0626(16) Uani 1 1 d . . . C94 C 1.2182(3) 0.09227(14) 0.05525(16) 0.0572(14) Uani 1 1 d . . . C95 C 0.7169(2) 0.14204(16) 0.06850(16) 0.0612(15) Uani 1 1 d . . . C96 C 0.5643(3) 0.09211(17) 0.04338(17) 0.0651(16) Uani 1 1 d . . . H96A H 0.5407 0.0813 0.0236 0.078 Uiso 1 1 calc R . . C97 C 0.5798(2) 0.10633(15) 0.10414(16) 0.0603(15) Uani 1 1 d . . . H97A H 0.5658 0.1059 0.1254 0.072 Uiso 1 1 calc R . . C98 C 1.2799(3) 0.07463(16) 0.0548(2) 0.0644(16) Uani 1 1 d . . . C99 C 1.1290(3) 0.12447(16) 0.02553(16) 0.0630(15) Uani 1 1 d . . . H99A H 1.1080 0.1352 0.0050 0.076 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 0.0505(5) 0.0562(5) 0.0859(5) -0.0136(3) 0.0241(3) 0.0016(3) Zn3 0.0543(9) 0.0520(8) 0.0784(10) 0.0048(6) 0.0204(6) 0.0007(6) Zn3' 0.079(5) 0.163(8) 0.061(3) -0.033(5) 0.026(3) -0.054(5) Zn4 0.0658(5) 0.0801(6) 0.0713(5) 0.0060(4) 0.0192(4) 0.0120(4) N1 0.046(3) 0.106(5) 0.115(4) 0.025(3) 0.023(3) 0.014(3) N2 0.034(3) 0.036(3) 0.150(5) -0.002(3) 0.032(3) 0.006(2) N3 0.060(3) 0.038(3) 0.084(3) -0.008(3) 0.026(2) 0.011(2) N4 0.058(3) 0.061(3) 0.063(3) -0.004(2) 0.018(2) 0.004(2) O1 0.137(6) 0.303(12) 0.185(7) -0.104(8) -0.070(6) 0.148(8) O2 0.201(6) 0.045(3) 0.104(4) -0.008(2) -0.010(4) -0.003(3) O3 0.109(4) 0.048(3) 0.122(4) -0.004(2) 0.028(3) 0.018(3) O4 0.062(3) 0.162(6) 0.098(4) 0.018(4) 0.024(3) 0.034(3) O5 0.126(4) 0.081(3) 0.096(3) -0.010(3) 0.052(3) -0.021(3) O6 0.103(4) 0.042(2) 0.085(3) -0.007(2) 0.025(2) 0.000(2) O7 0.073(3) 0.063(2) 0.079(3) 0.014(2) 0.023(2) -0.001(2) O8 0.088(3) 0.095(4) 0.086(3) 0.001(3) 0.044(3) -0.013(3) O9 0.048(2) 0.084(3) 0.086(3) 0.017(2) 0.014(2) 0.010(2) O10 0.036(2) 0.053(2) 0.135(4) 0.000(2) 0.005(2) 0.0071(18) O11 0.058(2) 0.062(2) 0.088(3) -0.014(2) 0.034(2) -0.015(2) O12 0.058(3) 0.118(4) 0.070(3) -0.006(2) 0.028(2) -0.025(2) O13 0.060(2) 0.056(2) 0.108(3) -0.015(2) 0.036(2) 0.0096(19) C7 0.083(7) 0.236(15) 0.112(7) 0.021(8) -0.004(5) 0.046(8) N5 0.207(11) 0.097(6) 0.335(16) 0.064(8) 0.168(12) 0.034(6) C10 0.195(10) 0.063(5) 0.103(6) 0.015(4) 0.062(6) 0.031(6) C11 0.075(6) 0.166(9) 0.137(7) -0.040(7) -0.014(5) 0.054(6) C12 0.118(6) 0.085(6) 0.130(6) 0.005(5) 0.074(6) -0.017(5) C13 0.157(8) 0.078(5) 0.074(4) -0.003(4) 0.037(4) -0.018(5) C14 0.170(9) 0.114(7) 0.114(6) -0.054(6) 0.085(6) -0.052(6) C15 0.097(5) 0.063(4) 0.101(5) -0.026(4) 0.040(4) -0.022(4) C16 0.133(7) 0.086(6) 0.076(5) -0.013(4) 0.034(4) -0.004(5) C17 0.076(5) 0.117(7) 0.122(6) -0.066(5) 0.022(5) -0.008(4) C18 0.175(9) 0.086(6) 0.090(5) 0.008(5) 0.059(5) -0.002(6) C19 0.197(11) 0.072(6) 0.170(9) 0.036(6) 0.108(9) 0.017(6) C20 0.083(5) 0.090(6) 0.103(6) -0.025(5) 0.033(4) 0.018(4) C21 0.164(8) 0.092(6) 0.077(5) 0.009(4) 0.056(5) 0.011(5) C22 0.076(6) 0.163(8) 0.056(4) -0.003(4) 0.006(4) 0.063(6) C23 0.073(6) 0.212(12) 0.107(6) -0.023(7) 0.004(5) 0.054(7) C24 0.047(4) 0.047(4) 0.144(6) 0.002(4) 0.029(4) 0.008(3) C25 0.046(5) 0.137(8) 0.207(11) -0.023(8) 0.004(5) 0.004(5) C26 0.059(5) 0.133(7) 0.112(6) -0.074(5) 0.026(4) -0.024(4) C27 0.064(5) 0.110(6) 0.134(7) -0.018(5) -0.009(4) 0.023(5) C28 0.055(5) 0.099(6) 0.109(5) 0.021(4) 0.034(4) 0.024(4) C29 0.185(10) 0.082(6) 0.147(8) 0.016(5) 0.105(8) 0.014(6) C30 0.080(4) 0.096(6) 0.073(4) 0.005(4) 0.035(3) 0.014(4) C31 0.156(8) 0.051(4) 0.112(6) -0.002(4) 0.067(5) 0.037(4) C32 0.092(5) 0.046(4) 0.081(4) -0.006(3) 0.036(4) 0.003(4) C33 0.077(5) 0.139(7) 0.063(4) 0.015(4) 0.015(4) 0.049(5) C34 0.084(5) 0.081(5) 0.070(4) 0.031(3) 0.010(4) -0.016(4) C35 0.090(5) 0.069(4) 0.077(4) 0.010(3) 0.007(3) -0.009(4) C36 0.073(6) 0.241(13) 0.124(7) -0.012(8) -0.015(5) 0.082(7) C37 0.088(7) 0.172(9) 0.069(5) -0.001(5) -0.001(5) 0.048(7) C38 0.096(6) 0.205(11) 0.109(6) -0.074(7) 0.067(5) -0.043(6) C39 0.070(6) 0.118(7) 0.207(11) -0.026(7) 0.031(6) 0.010(5) C40 0.112(6) 0.055(4) 0.073(4) 0.002(3) 0.023(4) 0.015(4) C41 0.054(4) 0.056(4) 0.102(4) 0.010(3) 0.019(3) 0.006(3) C42 0.074(5) 0.078(5) 0.108(5) 0.031(4) 0.018(4) 0.026(4) C43 0.087(6) 0.194(10) 0.137(8) -0.072(8) 0.066(6) -0.049(6) C44 0.055(4) 0.085(5) 0.132(6) 0.033(5) 0.016(4) 0.025(4) C45 0.076(5) 0.106(6) 0.074(4) 0.009(4) 0.034(4) 0.038(4) C46 0.069(5) 0.140(7) 0.115(6) -0.024(5) -0.010(4) 0.050(5) C47 0.071(4) 0.074(5) 0.085(5) 0.008(4) 0.023(3) 0.008(3) C48 0.073(5) 0.054(4) 0.116(5) 0.027(3) 0.038(4) 0.002(3) C49 0.050(4) 0.049(4) 0.100(4) 0.002(3) 0.025(3) 0.008(3) C50 0.068(4) 0.060(4) 0.091(4) 0.022(3) 0.038(4) 0.010(3) C51 0.076(5) 0.047(4) 0.104(5) -0.009(3) 0.038(4) 0.009(3) C52 0.038(3) 0.052(4) 0.142(6) -0.009(4) 0.021(3) 0.003(3) C53 0.063(5) 0.062(4) 0.099(5) 0.019(4) 0.021(3) 0.016(3) C54 0.066(4) 0.076(4) 0.085(4) -0.004(3) 0.034(3) 0.021(3) C55 0.060(4) 0.070(4) 0.080(4) 0.005(3) 0.018(3) 0.022(3) C56 0.068(4) 0.092(5) 0.072(4) -0.018(3) 0.014(3) 0.024(4) C57 0.051(4) 0.041(4) 0.112(5) 0.001(3) 0.008(3) -0.002(3) C58 0.059(4) 0.094(6) 0.094(5) -0.007(4) 0.041(3) 0.000(3) C59 0.090(5) 0.088(6) 0.117(6) -0.018(4) 0.045(5) -0.004(4) C60 0.059(4) 0.050(4) 0.096(4) -0.008(3) 0.030(3) -0.005(3) C61 0.066(4) 0.048(4) 0.094(4) -0.015(3) 0.027(3) 0.007(3) C62 0.051(4) 0.051(4) 0.164(7) 0.019(4) 0.049(4) 0.015(3) C63 0.088(5) 0.043(4) 0.079(4) -0.015(3) 0.032(3) 0.008(4) C64 0.044(3) 0.048(3) 0.116(5) -0.010(3) 0.037(3) -0.001(3) C65 0.034(3) 0.042(4) 0.135(5) -0.006(3) 0.025(3) 0.004(3) C66 0.068(4) 0.082(5) 0.062(4) -0.008(4) 0.017(3) 0.005(3) C67 0.070(4) 0.047(3) 0.079(4) 0.011(3) 0.010(3) 0.011(3) C68 0.059(4) 0.056(4) 0.115(5) 0.019(4) 0.018(4) 0.007(3) C69 0.050(4) 0.051(4) 0.124(5) -0.003(4) 0.047(3) 0.006(3) C70 0.049(4) 0.056(3) 0.096(4) 0.001(3) 0.025(3) 0.007(3) C71 0.072(4) 0.062(4) 0.082(4) 0.001(3) 0.028(3) 0.002(3) C72 0.044(4) 0.074(4) 0.081(4) -0.010(3) 0.011(3) -0.005(3) C73 0.053(4) 0.069(4) 0.071(4) -0.010(3) 0.019(3) 0.014(3) C74 0.041(3) 0.055(4) 0.096(4) -0.017(3) 0.028(3) 0.003(3) C75 0.071(4) 0.064(5) 0.091(4) -0.002(3) 0.047(3) -0.011(3) C76 0.044(3) 0.086(4) 0.085(4) -0.015(3) 0.032(3) -0.015(3) C77 0.058(4) 0.050(4) 0.106(5) -0.014(3) 0.019(3) -0.002(3) C78 0.072(4) 0.049(4) 0.081(4) -0.015(3) 0.023(3) -0.021(3) C79 0.060(4) 0.053(3) 0.071(4) 0.019(3) 0.015(3) 0.007(3) C80 0.039(3) 0.037(4) 0.136(5) -0.008(3) 0.032(3) 0.000(3) C81 0.045(4) 0.053(4) 0.136(6) 0.001(4) 0.045(4) 0.010(3) C82 0.053(4) 0.037(4) 0.129(5) -0.004(3) 0.016(3) 0.005(3) C83 0.051(4) 0.069(4) 0.128(5) 0.006(4) 0.046(4) 0.002(3) C84 0.044(3) 0.050(3) 0.109(5) -0.011(3) 0.015(3) 0.007(3) C85 0.038(3) 0.051(3) 0.095(4) -0.003(3) 0.027(3) -0.003(3) C86 0.058(4) 0.051(3) 0.074(4) -0.006(3) 0.028(4) -0.014(3) C87 0.052(4) 0.073(4) 0.084(4) 0.011(3) 0.006(3) 0.012(3) C88 0.049(3) 0.047(3) 0.096(4) 0.002(3) 0.021(3) 0.010(3) C89 0.053(4) 0.048(4) 0.122(5) 0.005(4) 0.045(3) 0.007(3) C90 0.041(3) 0.056(3) 0.081(4) -0.003(3) 0.022(3) -0.006(3) C91 0.071(4) 0.050(4) 0.080(5) 0.019(3) 0.025(4) 0.014(3) C92 0.041(3) 0.050(3) 0.080(4) -0.005(3) 0.014(3) 0.017(3) C93 0.047(3) 0.084(5) 0.059(4) -0.017(4) 0.017(3) -0.014(3) C94 0.049(3) 0.050(3) 0.079(4) -0.003(3) 0.028(3) 0.007(3) C95 0.035(3) 0.064(4) 0.086(4) -0.001(3) 0.014(3) 0.000(3) C96 0.045(3) 0.073(4) 0.081(4) -0.013(3) 0.023(3) -0.007(3) C97 0.048(4) 0.063(4) 0.076(4) 0.006(3) 0.028(3) -0.003(3) C98 0.040(3) 0.047(3) 0.110(5) -0.007(4) 0.022(4) 0.001(3) C99 0.055(4) 0.062(4) 0.074(4) 0.005(3) 0.018(3) 0.015(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 O6 1.959(4) 3_545 ? Zn1 O13 1.971(4) . ? Zn1 O11 2.002(4) 1_655 ? Zn1 N3 2.068(5) . ? Zn1 O3 2.498(5) 3_545 ? Zn1 C32 2.521(6) 3_545 ? Zn3 Zn3' 0.527(10) . ? Zn3 O9 1.921(6) 3 ? Zn3 O10 1.940(6) 1_455 ? Zn3 O12 2.002(5) . ? Zn3 O2 2.053(5) . ? Zn3 O8 2.148(5) . ? Zn3' O8 1.696(11) . ? Zn3' O12 1.828(11) . ? Zn3' O10 1.992(9) 1_455 ? Zn3' O9 2.166(10) 3 ? Zn3' O2 2.552(11) . ? Zn4 O4 1.960(5) . ? Zn4 O5 1.971(5) 3_545 ? Zn4 O7 1.984(4) 1_655 ? Zn4 N4 2.064(5) 8_446 ? Zn4 O1 2.453(7) . ? Zn4 C37 2.552(10) . ? N1 C53 1.405(9) . ? N1 C68 1.431(9) . ? N1 C28 1.467(9) . ? N2 C80 1.395(8) . ? N2 C65 1.403(7) . ? N2 C81 1.431(7) . ? N3 C31 1.285(9) . ? N3 C56 1.320(8) . ? N4 C43 1.303(9) . ? N4 C26 1.309(8) . ? N4 Zn4 2.064(5) 8_545 ? O1 C37 1.249(13) . ? O2 C6 1.234(13) . ? O3 C32 1.242(8) . ? O3 Zn1 2.498(5) 3_455 ? O4 C37 1.182(11) . ? O5 C93 1.221(7) . ? O5 Zn4 1.971(5) 3_455 ? O6 C32 1.270(8) . ? O6 Zn1 1.959(4) 3_455 ? O7 C91 1.255(7) . ? O7 Zn4 1.984(4) 1_455 ? O8 C93 1.226(7) . ? O9 C91 1.267(8) . ? O9 Zn3 1.921(6) 3_445 ? O9 Zn3' 2.166(10) 3_445 ? O10 C98 1.257(8) . ? O10 Zn3 1.940(6) 1_655 ? O10 Zn3' 1.992(9) 1_655 ? O11 C86 1.219(7) . ? O11 Zn1 2.002(4) 1_455 ? O12 C86 1.257(7) . ? O13 C98 1.245(8) . ? C1 N5 1.62(5) . ? C1 C2 1.83(4) . ? C2 C4 1.76(3) . ? C3 N5 1.33(2) . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C3 H3D 0.9600 . ? C4 N6 1.61(2) . ? C5 N6 1.503(14) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 N5 1.324(14) . ? C6 N6 1.340(13) . ? C7 C36 1.379(13) . ? C7 C22 1.386(15) . ? C7 H7A 0.9300 . ? C10 C15 1.348(11) . ? C10 C31 1.415(11) . ? C10 H10A 0.9300 . ? C11 C33 1.311(12) . ? C11 C23 1.371(12) . ? C11 H11A 0.9300 . ? C12 C68 1.343(10) . ? C12 C59 1.388(11) . ? C12 H12A 0.9300 . ? C13 C16 1.449(11) . ? C13 C14 1.469(11) . ? C13 H13A 0.9300 . ? C14 C15 1.525(11) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C20 1.336(11) . ? C16 C40 1.528(10) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C40 1.318(10) . ? C17 C26 1.359(10) . ? C17 H17A 0.9300 . ? C18 C21 1.361(11) . ? C18 C47 1.396(11) . ? C18 H18A 0.9300 . ? C19 C30 1.391(11) . ? C19 C29 1.403(13) . ? C19 H19A 0.9300 . ? C20 C56 1.347(10) . ? C20 H20A 0.9300 . ? C21 C66 1.372(10) . ? C21 H21A 0.9300 . ? C22 C23 1.258(13) . ? C22 C37 1.493(12) . ? C23 H23A 0.9300 . ? C24 C80 1.367(9) . ? C24 C52 1.390(9) . ? C24 H24A 0.9300 . ? C25 C45 1.327(12) . ? C25 C39 1.378(13) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C46 1.325(11) . ? C27 C28 1.363(11) . ? C27 H27A 0.9300 . ? C28 C39 1.333(12) . ? C29 C68 1.374(11) . ? C29 H29A 0.9300 . ? C30 C59 1.368(10) . ? C30 C47 1.477(10) . ? C31 H31A 0.9300 . ? C32 C63 1.549(9) . ? C32 Zn1 2.521(6) 3_455 ? C33 C36 1.462(14) . ? C33 C45 1.478(10) . ? C34 C35 1.361(9) . ? C34 C79 1.380(9) . ? C34 H34A 0.9300 . ? C35 C67 1.400(9) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C38 C40 1.347(11) . ? C38 C43 1.358(12) . ? C38 H38A 0.9300 . ? C39 H39A 0.9300 . ? C41 C48 1.351(9) . ? C41 C71 1.370(9) . ? C41 H41A 0.9300 . ? C42 C71 1.392(9) . ? C42 C44 1.408(10) . ? C42 H42A 0.9300 . ? C43 H43A 0.9300 . ? C44 C53 1.365(10) . ? C44 H44A 0.9300 . ? C45 C46 1.423(12) . ? C46 H46A 0.9300 . ? C47 C58 1.398(10) . ? C48 C53 1.423(9) . ? C48 H48A 0.9300 . ? C49 C57 1.353(8) . ? C49 C52 1.368(9) . ? C49 C61 1.484(9) . ? C50 C55 1.380(9) . ? C50 C67 1.384(9) . ? C50 H50A 0.9300 . ? C51 C63 1.338(9) . ? C51 C77 1.372(9) . ? C51 H51A 0.9300 . ? C52 H52A 0.9300 . ? C54 C92 1.380(9) . ? C54 C87 1.380(9) . ? C54 H54A 0.9300 . ? C55 C79 1.381(8) . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? C57 C82 1.410(8) . ? C57 H57A 0.9300 . ? C58 C75 1.376(9) . ? C58 H58A 0.9300 . ? C59 H59A 0.9300 . ? C60 C78 1.381(8) . ? C60 C61 1.398(8) . ? C60 H60A 0.9300 . ? C61 C77 1.404(8) . ? C62 C81 1.376(9) . ? C62 C83 1.383(9) . ? C62 H62A 0.9300 . ? C63 C78 1.370(9) . ? C64 C69 1.377(8) . ? C64 C95 1.396(8) . ? C64 H64A 0.9300 . ? C65 C84 1.390(9) . ? C65 C69 1.399(9) . ? C66 C75 1.361(9) . ? C66 C93 1.491(9) . ? C67 C71 1.513(9) . ? C69 H69A 0.9300 . ? C70 C89 1.357(8) . ? C70 C88 1.408(8) . ? C70 H70A 0.9300 . ? C72 C97 1.370(8) . ? C72 C85 1.396(8) . ? C72 H72A 0.9300 . ? C73 C99 1.369(8) . ? C73 C94 1.380(8) . ? C73 H73A 0.9300 . ? C74 C95 1.375(8) . ? C74 C84 1.388(8) . ? C74 H74A 0.9300 . ? C75 H75A 0.9300 . ? C76 C96 1.394(8) . ? C76 C85 1.407(9) . ? C76 H76A 0.9300 . ? C77 H77A 0.9300 . ? C78 H78A 0.9300 . ? C79 C91 1.505(9) . ? C80 C82 1.385(9) . ? C81 C89 1.398(9) . ? C82 H82A 0.9300 . ? C83 C88 1.392(9) . ? C83 H83A 0.9300 . ? C84 H84A 0.9300 . ? C85 C95 1.480(8) . ? C86 C90 1.498(8) . ? C87 C94 1.404(9) . ? C87 H87A 0.9300 . ? C88 C92 1.449(8) . ? C89 H89A 0.9300 . ? C90 C97 1.373(8) . ? C90 C96 1.380(8) . ? C92 C99 1.368(8) . ? C94 C98 1.502(8) . ? C96 H96A 0.9300 . ? C97 H97A 0.9300 . ? C99 H99A 0.9300 . ? 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 O6 Zn1 O13 141.3(2) 3_545 . ? O6 Zn1 O11 99.42(19) 3_545 1_655 ? O13 Zn1 O11 110.60(17) . 1_655 ? O6 Zn1 N3 102.76(17) 3_545 . ? O13 Zn1 N3 100.43(19) . . ? O11 Zn1 N3 91.24(18) 1_655 . ? O6 Zn1 O3 58.26(18) 3_545 3_545 ? O13 Zn1 O3 87.97(17) . 3_545 ? O11 Zn1 O3 157.00(18) 1_655 3_545 ? N3 Zn1 O3 98.80(17) . 3_545 ? O6 Zn1 C32 29.7(2) 3_545 3_545 ? O13 Zn1 C32 115.4(2) . 3_545 ? O11 Zn1 C32 129.1(2) 1_655 3_545 ? N3 Zn1 C32 100.66(18) . 3_545 ? O3 Zn1 C32 28.65(19) 3_545 3_545 ? Zn3' Zn3 O9 111.0(13) . 3 ? Zn3' Zn3 O10 88.0(12) . 1_455 ? O9 Zn3 O10 142.4(2) 3 1_455 ? Zn3' Zn3 O12 63.4(14) . . ? O9 Zn3 O12 102.9(2) 3 . ? O10 Zn3 O12 114.6(2) 1_455 . ? Zn3' Zn3 O2 159.1(14) . . ? O9 Zn3 O2 85.8(2) 3 . ? O10 Zn3 O2 85.5(2) 1_455 . ? O12 Zn3 O2 101.5(3) . . ? Zn3' Zn3 O8 27.1(13) . . ? O9 Zn3 O8 95.9(2) 3 . ? O10 Zn3 O8 86.9(2) 1_455 . ? O12 Zn3 O8 88.1(2) . . ? O2 Zn3 O8 169.6(3) . . ? Zn3 Zn3' O8 144.8(17) . . ? Zn3 Zn3' O12 101.6(15) . . ? O8 Zn3' O12 110.0(6) . . ? Zn3 Zn3' O10 76.7(12) . 1_455 ? O8 Zn3' O10 99.3(5) . 1_455 ? O12 Zn3' O10 120.5(5) . 1_455 ? Zn3 Zn3' O9 55.9(11) . 3 ? O8 Zn3' O9 102.5(5) . 3 ? O12 Zn3' O9 100.1(4) . 3 ? O10 Zn3' O9 123.0(5) 1_455 3 ? Zn3 Zn3' O2 16.7(12) . . ? O8 Zn3' O2 159.7(6) . . ? O12 Zn3' O2 90.0(4) . . ? O10 Zn3' O2 72.1(3) 1_455 . ? O9 Zn3' O2 69.4(3) 3 . ? O4 Zn4 O5 98.1(3) . 3_545 ? O4 Zn4 O7 134.6(2) . 1_655 ? O5 Zn4 O7 109.5(2) 3_545 1_655 ? O4 Zn4 N4 119.4(2) . 8_446 ? O5 Zn4 N4 93.2(2) 3_545 8_446 ? O7 Zn4 N4 94.78(18) 1_655 8_446 ? O4 Zn4 O1 55.2(3) . . ? O5 Zn4 O1 152.9(3) 3_545 . ? O7 Zn4 O1 94.9(3) 1_655 . ? N4 Zn4 O1 96.4(3) 8_446 . ? O4 Zn4 C37 26.4(3) . . ? O5 Zn4 C37 124.3(3) 3_545 . ? O7 Zn4 C37 117.9(3) 1_655 . ? N4 Zn4 C37 109.5(2) 8_446 . ? O1 Zn4 C37 28.8(3) . . ? C53 N1 C68 121.2(5) . . ? C53 N1 C28 120.3(6) . . ? C68 N1 C28 117.1(6) . . ? C80 N2 C65 118.8(4) . . ? C80 N2 C81 121.3(4) . . ? C65 N2 C81 119.8(5) . . ? C31 N3 C56 115.2(6) . . ? C31 N3 Zn1 123.4(4) . . ? C56 N3 Zn1 119.4(4) . . ? C43 N4 C26 114.1(6) . . ? C43 N4 Zn4 127.3(5) . 8_545 ? C26 N4 Zn4 118.5(4) . 8_545 ? C37 O1 Zn4 80.0(6) . . ? C6 O2 Zn3 139.0(7) . . ? C6 O2 Zn3' 141.6(7) . . ? Zn3 O2 Zn3' 4.2(3) . . ? C32 O3 Zn1 76.7(4) . 3_455 ? C37 O4 Zn4 105.9(6) . . ? C93 O5 Zn4 140.8(4) . 3_455 ? C32 O6 Zn1 100.5(4) . 3_455 ? C91 O7 Zn4 113.6(4) . 1_455 ? C93 O8 Zn3' 142.7(6) . . ? C93 O8 Zn3 134.6(4) . . ? Zn3' O8 Zn3 8.1(4) . . ? C91 O9 Zn3 134.6(4) . 3_445 ? C91 O9 Zn3' 122.7(4) . 3_445 ? Zn3 O9 Zn3' 13.1(3) 3_445 3_445 ? C98 O10 Zn3 126.1(4) . 1_655 ? C98 O10 Zn3' 138.4(5) . 1_655 ? Zn3 O10 Zn3' 15.3(3) 1_655 1_655 ? C86 O11 Zn1 139.5(4) . 1_455 ? C86 O12 Zn3' 133.4(5) . . ? C86 O12 Zn3 131.2(4) . . ? Zn3' O12 Zn3 15.0(3) . . ? C98 O13 Zn1 108.1(4) . . ? N5 C1 C2 97(3) . . ? C4 C2 C1 118(2) . . ? N5 C3 H3B 109.5 . . ? N5 C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N5 C3 H3D 109.5 . . ? H3B C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? N6 C4 C2 93.5(15) . . ? N6 C5 H5A 109.5 . . ? N6 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N6 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O2 C6 N5 128.5(11) . . ? O2 C6 N6 115.2(11) . . ? N5 C6 N6 116.3(11) . . ? C36 C7 C22 123.4(11) . . ? C36 C7 H7A 118.3 . . ? C22 C7 H7A 118.3 . . ? C6 N5 C3 126.4(14) . . ? C6 N5 C1 132.5(19) . . ? C3 N5 C1 100(2) . . ? C6 N6 C5 116.8(10) . . ? C6 N6 C4 139.9(13) . . ? C5 N6 C4 103.0(12) . . ? C15 C10 C31 118.4(7) . . ? C15 C10 H10A 120.8 . . ? C31 C10 H10A 120.8 . . ? C33 C11 C23 125.4(9) . . ? C33 C11 H11A 117.3 . . ? C23 C11 H11A 117.3 . . ? C68 C12 C59 121.5(7) . . ? C68 C12 H12A 119.2 . . ? C59 C12 H12A 119.2 . . ? C16 C13 C14 118.3(8) . . ? C16 C13 H13A 120.9 . . ? C14 C13 H13A 120.9 . . ? C13 C14 C15 114.4(7) . . ? C13 C14 H14A 108.7 . . ? C15 C14 H14A 108.7 . . ? C13 C14 H14B 108.7 . . ? C15 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C20 C15 C10 117.5(7) . . ? C20 C15 C14 123.0(8) . . ? C10 C15 C14 119.5(8) . . ? C13 C16 C40 113.3(7) . . ? C13 C16 H16A 108.9 . . ? C40 C16 H16A 108.9 . . ? C13 C16 H16B 108.9 . . ? C40 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C40 C17 C26 121.5(7) . . ? C40 C17 H17A 119.3 . . ? C26 C17 H17A 119.3 . . ? C21 C18 C47 123.5(7) . . ? C21 C18 H18A 118.3 . . ? C47 C18 H18A 118.3 . . ? C30 C19 C29 121.4(8) . . ? C30 C19 H19A 119.3 . . ? C29 C19 H19A 119.3 . . ? C15 C20 C56 120.2(7) . . ? C15 C20 H20A 119.9 . . ? C56 C20 H20A 119.9 . . ? C18 C21 C66 120.2(7) . . ? C18 C21 H21A 119.9 . . ? C66 C21 H21A 119.9 . . ? C23 C22 C7 115.6(8) . . ? C23 C22 C37 125.2(10) . . ? C7 C22 C37 118.4(10) . . ? C22 C23 C11 123.2(10) . . ? C22 C23 H23A 118.4 . . ? C11 C23 H23A 118.4 . . ? C80 C24 C52 122.0(6) . . ? C80 C24 H24A 119.0 . . ? C52 C24 H24A 119.0 . . ? C45 C25 C39 124.1(9) . . ? C45 C25 H25A 117.9 . . ? C39 C25 H25A 117.9 . . ? N4 C26 C17 124.1(7) . . ? N4 C26 H26A 117.9 . . ? C17 C26 H26A 117.9 . . ? C46 C27 C28 122.7(8) . . ? C46 C27 H27A 118.7 . . ? C28 C27 H27A 118.7 . . ? C39 C28 C27 116.5(7) . . ? C39 C28 N1 121.5(8) . . ? C27 C28 N1 121.8(8) . . ? C68 C29 C19 120.0(8) . . ? C68 C29 H29A 120.0 . . ? C19 C29 H29A 120.0 . . ? C59 C30 C19 116.2(7) . . ? C59 C30 C47 122.5(6) . . ? C19 C30 C47 121.3(6) . . ? N3 C31 C10 123.8(7) . . ? N3 C31 H31A 118.1 . . ? C10 C31 H31A 118.1 . . ? O3 C32 O6 124.2(6) . . ? O3 C32 C63 118.9(6) . . ? O6 C32 C63 116.8(6) . . ? O3 C32 Zn1 74.7(4) . 3_455 ? O6 C32 Zn1 49.8(3) . 3_455 ? C63 C32 Zn1 165.1(5) . 3_455 ? C11 C33 C36 112.4(7) . . ? C11 C33 C45 124.8(8) . . ? C36 C33 C45 120.7(8) . . ? C35 C34 C79 121.7(6) . . ? C35 C34 H34A 119.2 . . ? C79 C34 H34A 119.2 . . ? C34 C35 C67 121.4(6) . . ? C34 C35 H35A 119.3 . . ? C67 C35 H35A 119.3 . . ? C7 C36 C33 117.6(12) . . ? C7 C36 H36A 121.2 . . ? C33 C36 H36A 121.2 . . ? O4 C37 O1 118.7(9) . . ? O4 C37 C22 120.2(9) . . ? O1 C37 C22 121.0(10) . . ? O4 C37 Zn4 47.6(4) . . ? O1 C37 Zn4 71.2(5) . . ? C22 C37 Zn4 167.7(9) . . ? C40 C38 C43 121.1(7) . . ? C40 C38 H38A 119.5 . . ? C43 C38 H38A 119.5 . . ? C28 C39 C25 121.1(9) . . ? C28 C39 H39A 119.4 . . ? C25 C39 H39A 119.4 . . ? C17 C40 C38 114.9(7) . . ? C17 C40 C16 120.7(7) . . ? C38 C40 C16 124.3(7) . . ? C48 C41 C71 122.4(6) . . ? C48 C41 H41A 118.8 . . ? C71 C41 H41A 118.8 . . ? C71 C42 C44 118.3(6) . . ? C71 C42 H42A 120.8 . . ? C44 C42 H42A 120.8 . . ? N4 C43 C38 123.9(8) . . ? N4 C43 H43A 118.0 . . ? C38 C43 H43A 118.0 . . ? C53 C44 C42 122.2(6) . . ? C53 C44 H44A 118.9 . . ? C42 C44 H44A 118.9 . . ? C25 C45 C46 113.5(7) . . ? C25 C45 C33 124.1(8) . . ? C46 C45 C33 122.3(8) . . ? C27 C46 C45 121.8(8) . . ? C27 C46 H46A 119.1 . . ? C45 C46 H46A 119.1 . . ? C18 C47 C58 114.5(7) . . ? C18 C47 C30 122.2(6) . . ? C58 C47 C30 123.3(6) . . ? C41 C48 C53 120.2(6) . . ? C41 C48 H48A 119.9 . . ? C53 C48 H48A 119.9 . . ? C57 C49 C52 118.5(6) . . ? C57 C49 C61 121.0(5) . . ? C52 C49 C61 120.5(6) . . ? C55 C50 C67 122.2(6) . . ? C55 C50 H50A 118.9 . . ? C67 C50 H50A 118.9 . . ? C63 C51 C77 119.9(6) . . ? C63 C51 H51A 120.1 . . ? C77 C51 H51A 120.1 . . ? C49 C52 C24 120.6(6) . . ? C49 C52 H52A 119.7 . . ? C24 C52 H52A 119.7 . . ? C44 C53 N1 123.4(6) . . ? C44 C53 C48 117.3(6) . . ? N1 C53 C48 119.1(5) . . ? C92 C54 C87 124.0(6) . . ? C92 C54 H54A 118.0 . . ? C87 C54 H54A 118.0 . . ? C50 C55 C79 120.3(6) . . ? C50 C55 H55A 119.8 . . ? C79 C55 H55A 119.8 . . ? N3 C56 C20 124.9(7) . . ? N3 C56 H56A 117.6 . . ? C20 C56 H56A 117.6 . . ? C49 C57 C82 121.3(6) . . ? C49 C57 H57A 119.3 . . ? C82 C57 H57A 119.3 . . ? C75 C58 C47 121.9(6) . . ? C75 C58 H58A 119.0 . . ? C47 C58 H58A 119.0 . . ? C30 C59 C12 122.1(7) . . ? C30 C59 H59A 119.0 . . ? C12 C59 H59A 119.0 . . ? C78 C60 C61 120.1(6) . . ? C78 C60 H60A 119.9 . . ? C61 C60 H60A 119.9 . . ? C60 C61 C77 116.7(5) . . ? C60 C61 C49 122.3(5) . . ? C77 C61 C49 120.9(5) . . ? C81 C62 C83 118.9(6) . . ? C81 C62 H62A 120.5 . . ? C83 C62 H62A 120.5 . . ? C51 C63 C78 120.7(6) . . ? C51 C63 C32 120.5(6) . . ? C78 C63 C32 118.7(6) . . ? C69 C64 C95 120.9(6) . . ? C69 C64 H64A 119.5 . . ? C95 C64 H64A 119.5 . . ? C84 C65 C69 118.4(5) . . ? C84 C65 N2 121.8(5) . . ? C69 C65 N2 119.9(5) . . ? C75 C66 C21 118.4(7) . . ? C75 C66 C93 121.2(6) . . ? C21 C66 C93 120.2(6) . . ? C50 C67 C35 116.4(6) . . ? C50 C67 C71 122.3(5) . . ? C35 C67 C71 121.3(6) . . ? C12 C68 C29 118.6(7) . . ? C12 C68 N1 122.3(6) . . ? C29 C68 N1 118.9(7) . . ? C64 C69 C65 120.6(5) . . ? C64 C69 H69A 119.7 . . ? C65 C69 H69A 119.7 . . ? C89 C70 C88 121.7(6) . . ? C89 C70 H70A 119.2 . . ? C88 C70 H70A 119.2 . . ? C41 C71 C42 119.2(6) . . ? C41 C71 C67 122.6(6) . . ? C42 C71 C67 118.2(6) . . ? C97 C72 C85 120.8(5) . . ? C97 C72 H72A 119.6 . . ? C85 C72 H72A 119.6 . . ? C99 C73 C94 120.9(5) . . ? C99 C73 H73A 119.6 . . ? C94 C73 H73A 119.6 . . ? C95 C74 C84 121.4(5) . . ? C95 C74 H74A 119.3 . . ? C84 C74 H74A 119.3 . . ? C66 C75 C58 121.2(6) . . ? C66 C75 H75A 119.4 . . ? C58 C75 H75A 119.4 . . ? C96 C76 C85 119.7(5) . . ? C96 C76 H76A 120.1 . . ? C85 C76 H76A 120.1 . . ? C51 C77 C61 121.9(6) . . ? C51 C77 H77A 119.1 . . ? C61 C77 H77A 119.1 . . ? C63 C78 C60 120.6(5) . . ? C63 C78 H78A 119.7 . . ? C60 C78 H78A 119.7 . . ? C34 C79 C55 117.9(6) . . ? C34 C79 C91 120.1(5) . . ? C55 C79 C91 121.9(6) . . ? C24 C80 C82 117.3(5) . . ? C24 C80 N2 122.9(5) . . ? C82 C80 N2 119.8(5) . . ? C62 C81 C89 119.4(5) . . ? C62 C81 N2 119.9(6) . . ? C89 C81 N2 120.6(5) . . ? C80 C82 C57 120.2(6) . . ? C80 C82 H82A 119.9 . . ? C57 C82 H82A 119.9 . . ? C62 C83 C88 123.2(6) . . ? C62 C83 H83A 118.4 . . ? C88 C83 H83A 118.4 . . ? C74 C84 C65 120.3(5) . . ? C74 C84 H84A 119.8 . . ? C65 C84 H84A 119.8 . . ? C72 C85 C76 118.0(5) . . ? C72 C85 C95 121.6(5) . . ? C76 C85 C95 120.4(5) . . ? O11 C86 O12 126.4(5) . . ? O11 C86 C90 117.3(5) . . ? O12 C86 C90 116.2(6) . . ? C54 C87 C94 117.7(6) . . ? C54 C87 H87A 121.1 . . ? C94 C87 H87A 121.1 . . ? C83 C88 C70 116.0(5) . . ? C83 C88 C92 121.3(5) . . ? C70 C88 C92 122.7(5) . . ? C70 C89 C81 120.7(5) . . ? C70 C89 H89A 119.6 . . ? C81 C89 H89A 119.6 . . ? C97 C90 C96 118.9(5) . . ? C97 C90 C86 121.0(5) . . ? C96 C90 C86 120.0(5) . . ? O7 C91 O9 121.8(6) . . ? O7 C91 C79 118.1(6) . . ? O9 C91 C79 120.0(5) . . ? C99 C92 C54 116.2(5) . . ? C99 C92 C88 122.1(5) . . ? C54 C92 C88 121.6(5) . . ? O5 C93 O8 124.1(6) . . ? O5 C93 C66 116.0(6) . . ? O8 C93 C66 119.9(6) . . ? C73 C94 C87 118.7(5) . . ? C73 C94 C98 120.7(5) . . ? C87 C94 C98 120.6(6) . . ? C74 C95 C64 118.3(5) . . ? C74 C95 C85 119.5(5) . . ? C64 C95 C85 122.0(5) . . ? C90 C96 C76 120.9(6) . . ? C90 C96 H96A 119.6 . . ? C76 C96 H96A 119.6 . . ? C72 C97 C90 121.4(5) . . ? C72 C97 H97A 119.3 . . ? C90 C97 H97A 119.3 . . ? O13 C98 O10 124.2(5) . . ? O13 C98 C94 117.1(6) . . ? O10 C98 C94 118.7(6) . . ? C92 C99 C73 122.2(5) . . ? C92 C99 H99A 118.9 . . ? C73 C99 H99A 118.9 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.615 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.075 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.006 -0.005 -0.006 17919.2 218.6 _platon_squeeze_details ; ; #end _database_code_depnum_ccdc_archive 'CCDC 948626'