# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Atsuhiro Osuka' _publ_contact_author_email OSUKA@KUCHEM.KYOTO-U.AC.JP _publ_section_title ; Synthesis of pyridine-fused porphyrinoid: oxopyridochlorin ; loop_ _publ_author_name 'Atsuhiro Osuka' 'Hideyuki Shinmori' 'Hiroshi Shinokubo' 'Yuji Takahashi' 'Sumito Tokuji' # Attachment '3H.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 707381' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H81 N5 O, C H4 O' _chemical_formula_sum 'C77 H85 N5 O2' _chemical_formula_weight 1112.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.251(5) _cell_length_b 20.011(6) _cell_length_c 18.977(7) _cell_angle_alpha 90.00 _cell_angle_beta 111.030(11) _cell_angle_gamma 90.00 _cell_volume 6824(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 30415 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.6 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2469 _exptl_absorpt_coefficient_mu 0.070 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9725 _exptl_absorpt_correction_T_max 0.9930 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48936 _diffrn_reflns_av_R_equivalents 0.1039 _diffrn_reflns_av_sigmaI/netI 0.0897 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11302 _reflns_number_gt 6672 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Though some electron density was properly assigned as a molecule of methanol, other electron density due to severely disordered solvents still remained. All attempts to model the disorder were unsatisfactory. The contributions to the scattering factors due to this solvent molecule were removed by use of the utility SQUEEZE in PLATON software packate, SQUEEZE-PLATON. ; _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^)+(0.1677P)^2^+3.8610P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11302 _refine_ls_number_parameters 777 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1436 _refine_ls_R_factor_gt 0.0952 _refine_ls_wR_factor_ref 0.3014 _refine_ls_wR_factor_gt 0.2721 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O2 O 0.41067(16) 0.38853(15) 0.29559(18) 0.0438(8) Uani 1 1 d . . . N1 N 0.51191(18) 0.71602(17) 0.4961(2) 0.0376(8) Uani 1 1 d . . . H26 H 0.5097 0.6760 0.4762 0.045 Uiso 1 1 calc R . . N2 N 0.39725(18) 0.63914(17) 0.3807(2) 0.0370(8) Uani 1 1 d . . . N3 N 0.61317(19) 0.60156(17) 0.5198(2) 0.0373(8) Uani 1 1 d . . . N4 N 0.65606(18) 0.37737(18) 0.4389(2) 0.0401(9) Uani 1 1 d . . . C6 C 0.5699(2) 0.7417(2) 0.5547(2) 0.0349(10) Uani 1 1 d . . . N5 N 0.49748(18) 0.52574(18) 0.4062(2) 0.0375(8) Uani 1 1 d . . . H27 H 0.4989 0.5646 0.4283 0.045 Uiso 1 1 calc R . . C8 C 0.4378(2) 0.5009(2) 0.3487(3) 0.0373(10) Uani 1 1 d . . . C9 C 0.3735(2) 0.5342(2) 0.3067(3) 0.0372(10) Uani 1 1 d . . . C10 C 0.6372(2) 0.7080(2) 0.5937(2) 0.0369(10) Uani 1 1 d . . . C11 C 0.5340(2) 0.4213(2) 0.3813(2) 0.0357(10) Uani 1 1 d . . . C12 C 0.5554(2) 0.4804(2) 0.4244(2) 0.0372(10) Uani 1 1 d . . . C13 C 0.3551(2) 0.6000(2) 0.3228(3) 0.0397(10) Uani 1 1 d . . . C14 C 0.4828(2) 0.8218(2) 0.5192(3) 0.0399(10) Uani 1 1 d . . . H1 H 0.4562 0.8625 0.5153 0.048 Uiso 1 1 calc R . . C15 C 0.4576(2) 0.7642(2) 0.4737(3) 0.0367(10) Uani 1 1 d . . . C16 C 0.4551(2) 0.4300(2) 0.3348(3) 0.0387(10) Uani 1 1 d . . . C17 C 0.8086(2) 0.8034(2) 0.7724(3) 0.0464(12) Uani 1 1 d . . . H2 H 0.8479 0.8236 0.8126 0.056 Uiso 1 1 calc R . . C18 C 0.3564(2) 0.4928(2) 0.1790(3) 0.0393(10) Uani 1 1 d . . . H3 H 0.4072 0.5041 0.1902 0.047 Uiso 1 1 calc R . . C19 C 0.2931(2) 0.6970(2) 0.3082(3) 0.0406(11) Uani 1 1 d . . . H4 H 0.2572 0.7316 0.2906 0.049 Uiso 1 1 calc R . . C20 C 0.2270(2) 0.8723(2) 0.3979(3) 0.0411(11) Uani 1 1 d . . . C21 C 0.5703(2) 0.3066(2) 0.3471(3) 0.0398(10) Uani 1 1 d . . . C22 C 0.3247(2) 0.5045(2) 0.2330(2) 0.0357(10) Uani 1 1 d . . . C23 C 0.3886(2) 0.7572(2) 0.4153(3) 0.0376(10) Uani 1 1 d . . . C24 C 0.3162(2) 0.4652(2) 0.1092(2) 0.0367(10) Uani 1 1 d . . . C25 C 0.2410(2) 0.4514(2) 0.0937(3) 0.0399(10) Uani 1 1 d . . . H5 H 0.2122 0.4330 0.0460 0.048 Uiso 1 1 calc R . . C26 C 0.6555(2) 0.6437(2) 0.5793(3) 0.0396(10) Uani 1 1 d . . . C27 C 0.3613(2) 0.7001(2) 0.3732(3) 0.0376(10) Uani 1 1 d . . . C28 C 0.2897(2) 0.6361(2) 0.2771(3) 0.0434(11) Uani 1 1 d . . . H6 H 0.2513 0.6199 0.2332 0.052 Uiso 1 1 calc R . . C29 C 0.5520(2) 0.8081(2) 0.5696(3) 0.0416(11) Uani 1 1 d . . . H7 H 0.5827 0.8373 0.6076 0.050 Uiso 1 1 calc R . . C30 C 0.3010(2) 0.9221(2) 0.3310(3) 0.0401(10) Uani 1 1 d . . . C31 C 0.7444(3) 0.7864(2) 0.7847(3) 0.0436(11) Uani 1 1 d . . . C32 C 0.3377(2) 0.8164(2) 0.3964(3) 0.0406(11) Uani 1 1 d . . . C33 C 0.7195(2) 0.6086(2) 0.6257(3) 0.0491(12) Uani 1 1 d . . . H8 H 0.7571 0.6253 0.6699 0.059 Uiso 1 1 calc R . . C34 C 0.6763(2) 0.4335(2) 0.4775(3) 0.0393(10) Uani 1 1 d . . . C35 C 0.3562(2) 0.4506(2) 0.0547(3) 0.0422(11) Uani 1 1 d . . . C36 C 0.6276(2) 0.4881(2) 0.4768(3) 0.0375(10) Uani 1 1 d . . . C37 C 0.6521(2) 0.5438(2) 0.5279(3) 0.0385(10) Uani 1 1 d . . . C38 C 0.2408(2) 0.9228(2) 0.3543(3) 0.0396(11) Uani 1 1 d . . . H9 H 0.2072 0.9595 0.3399 0.048 Uiso 1 1 calc R . . C39 C 0.5845(2) 0.3704(2) 0.3904(3) 0.0382(10) Uani 1 1 d . . . C40 C 0.2070(2) 0.4637(2) 0.1455(3) 0.0379(10) Uani 1 1 d . . . C41 C 0.6957(2) 0.7440(2) 0.6570(2) 0.0362(10) Uani 1 1 d . . . C42 C 0.7176(2) 0.5471(2) 0.5958(3) 0.0465(12) Uani 1 1 d . . . H10 H 0.7528 0.5124 0.6157 0.056 Uiso 1 1 calc R . . C43 C 0.6044(3) 0.2485(2) 0.3805(3) 0.0458(11) Uani 1 1 d . . . H11 H 0.6362 0.2492 0.4321 0.055 Uiso 1 1 calc R . . C44 C 0.3504(2) 0.8687(2) 0.3539(3) 0.0408(11) Uani 1 1 d . . . H12 H 0.3934 0.8679 0.3405 0.049 Uiso 1 1 calc R . . C45 C 0.2768(2) 0.8188(2) 0.4183(3) 0.0381(10) Uani 1 1 d . . . H13 H 0.2685 0.7835 0.4478 0.046 Uiso 1 1 calc R . . C46 C 0.4201(3) 0.4010(2) 0.0925(3) 0.0477(12) Uani 1 1 d . . . H28 H 0.4544 0.4203 0.1396 0.072 Uiso 1 1 calc R . . H29 H 0.4470 0.3920 0.0584 0.072 Uiso 1 1 calc R . . H30 H 0.3996 0.3592 0.1035 0.072 Uiso 1 1 calc R . . C47 C 0.7615(2) 0.7631(2) 0.6465(3) 0.0399(10) Uani 1 1 d . . . H14 H 0.7668 0.7556 0.5992 0.048 Uiso 1 1 calc R . . C48 C 0.2499(2) 0.4899(2) 0.2162(3) 0.0383(10) Uani 1 1 d . . . H15 H 0.2278 0.4978 0.2529 0.046 Uiso 1 1 calc R . . C49 C 0.6862(2) 0.7562(2) 0.7238(3) 0.0404(11) Uani 1 1 d . . . H16 H 0.6407 0.7446 0.7297 0.048 Uiso 1 1 calc R . . C50 C 0.5490(3) 0.1886(2) 0.2652(3) 0.0528(13) Uani 1 1 d . . . H17 H 0.5401 0.1477 0.2380 0.063 Uiso 1 1 calc R . . C51 C 0.7586(2) 0.4370(2) 0.5193(3) 0.0436(11) Uani 1 1 d . . . C52 C 0.5267(2) 0.3052(2) 0.2697(3) 0.0434(11) Uani 1 1 d . . . H18 H 0.5035 0.3451 0.2451 0.052 Uiso 1 1 calc R . . C53 C 0.3041(3) 0.4189(2) -0.0194(3) 0.0476(12) Uani 1 1 d . . . H31 H 0.2814 0.3785 -0.0079 0.071 Uiso 1 1 calc R . . H32 H 0.3327 0.4072 -0.0511 0.071 Uiso 1 1 calc R . . H33 H 0.2649 0.4509 -0.0463 0.071 Uiso 1 1 calc R . . C54 C 0.3882(3) 0.5151(2) 0.0357(3) 0.0474(12) Uani 1 1 d . . . H34 H 0.3475 0.5460 0.0100 0.071 Uiso 1 1 calc R . . H35 H 0.4158 0.5049 0.0025 0.071 Uiso 1 1 calc R . . H36 H 0.4218 0.5357 0.0823 0.071 Uiso 1 1 calc R . . C55 C 0.8188(2) 0.7928(2) 0.7050(3) 0.0412(11) Uani 1 1 d . . . C56 C 0.1243(2) 0.4507(2) 0.1288(3) 0.0455(11) Uani 1 1 d . . . C57 C 0.3160(3) 0.9781(2) 0.2822(3) 0.0501(12) Uani 1 1 d . . . C58 C 0.5174(3) 0.2465(2) 0.2291(3) 0.0486(12) Uani 1 1 d . . . H19 H 0.4892 0.2462 0.1765 0.058 Uiso 1 1 calc R . . C59 C 0.1611(2) 0.8728(2) 0.4244(3) 0.0515(13) Uani 1 1 d . . . C60 C 0.7935(3) 0.3903(3) 0.5734(3) 0.0622(15) Uani 1 1 d . . . H20 H 0.7659 0.3543 0.5828 0.075 Uiso 1 1 calc R . . C61 C 0.0854(3) 0.5171(3) 0.1329(3) 0.0576(14) Uani 1 1 d . . . H37 H 0.1072 0.5358 0.1839 0.086 Uiso 1 1 calc R . . H38 H 0.0322 0.5090 0.1210 0.086 Uiso 1 1 calc R . . H39 H 0.0920 0.5488 0.0964 0.086 Uiso 1 1 calc R . . C62 C 0.8932(3) 0.8122(2) 0.6958(3) 0.0529(13) Uani 1 1 d . . . C63 C 0.7332(3) 0.7964(2) 0.8603(3) 0.0522(13) Uani 1 1 d . . . C64 C 0.5937(3) 0.1891(2) 0.3409(3) 0.0513(13) Uani 1 1 d . . . H21 H 0.6166 0.1491 0.3653 0.062 Uiso 1 1 calc R . . C65 C 0.6650(3) 0.8399(3) 0.8507(3) 0.0700(16) Uani 1 1 d . . . H40 H 0.6542 0.8389 0.8973 0.105 Uiso 1 1 calc R . . H41 H 0.6221 0.8226 0.8089 0.105 Uiso 1 1 calc R . . H42 H 0.6751 0.8859 0.8397 0.105 Uiso 1 1 calc R . . C66 C 0.8012(3) 0.4875(3) 0.5035(3) 0.0594(14) Uani 1 1 d . . . H22 H 0.7776 0.5194 0.4653 0.071 Uiso 1 1 calc R . . C67 C 0.1148(3) 0.4013(3) 0.1875(3) 0.0599(14) Uani 1 1 d . . . H43 H 0.1449 0.3613 0.1899 0.090 Uiso 1 1 calc R . . H44 H 0.0623 0.3886 0.1726 0.090 Uiso 1 1 calc R . . H45 H 0.1311 0.4228 0.2373 0.090 Uiso 1 1 calc R . . C68 C 0.0855(3) 0.4203(3) 0.0502(3) 0.0621(15) Uani 1 1 d . . . H46 H 0.0887 0.4516 0.0117 0.093 Uiso 1 1 calc R . . H47 H 0.0332 0.4118 0.0422 0.093 Uiso 1 1 calc R . . H48 H 0.1100 0.3782 0.0463 0.093 Uiso 1 1 calc R . . C69 C 0.1882(3) 0.8669(3) 0.5104(4) 0.0664(16) Uani 1 1 d . . . H49 H 0.2181 0.8262 0.5264 0.100 Uiso 1 1 calc R . . H50 H 0.1453 0.8648 0.5265 0.100 Uiso 1 1 calc R . . H51 H 0.2187 0.9059 0.5333 0.100 Uiso 1 1 calc R . . C70 C 0.1152(3) 0.9368(3) 0.4009(4) 0.0705(17) Uani 1 1 d . . . H52 H 0.1467 0.9756 0.4228 0.106 Uiso 1 1 calc R . . H53 H 0.0736 0.9355 0.4192 0.106 Uiso 1 1 calc R . . H54 H 0.0958 0.9406 0.3458 0.106 Uiso 1 1 calc R . . C71 C 0.8016(3) 0.8302(3) 0.9200(3) 0.0757(17) Uani 1 1 d . . . H55 H 0.8445 0.8001 0.9328 0.113 Uiso 1 1 calc R . . H56 H 0.7905 0.8398 0.9655 0.113 Uiso 1 1 calc R . . H57 H 0.8130 0.8719 0.8994 0.113 Uiso 1 1 calc R . . C72 C 0.1105(3) 0.8130(3) 0.3878(4) 0.0763(19) Uani 1 1 d . . . H58 H 0.0891 0.8195 0.3330 0.114 Uiso 1 1 calc R . . H59 H 0.0704 0.8098 0.4081 0.114 Uiso 1 1 calc R . . H60 H 0.1399 0.7718 0.3991 0.114 Uiso 1 1 calc R . . C73 C 0.3918(3) 1.0105(3) 0.3233(3) 0.0652(15) Uani 1 1 d . . . H61 H 0.4313 0.9775 0.3301 0.098 Uiso 1 1 calc R . . H62 H 0.3940 1.0268 0.3727 0.098 Uiso 1 1 calc R . . H63 H 0.3988 1.0481 0.2933 0.098 Uiso 1 1 calc R . . C74 C 0.2559(3) 1.0320(3) 0.2646(4) 0.0687(16) Uani 1 1 d . . . H64 H 0.2634 1.0646 0.2294 0.103 Uiso 1 1 calc R . . H65 H 0.2590 1.0547 0.3114 0.103 Uiso 1 1 calc R . . H66 H 0.2067 1.0114 0.2417 0.103 Uiso 1 1 calc R . . C75 C 0.8690(3) 0.3957(3) 0.6142(4) 0.090(2) Uani 1 1 d . . . H23 H 0.8928 0.3645 0.6531 0.108 Uiso 1 1 calc R . . C76 C 0.7214(5) 0.7277(3) 0.8900(4) 0.095(2) Uani 1 1 d . . . H67 H 0.7667 0.7009 0.9014 0.143 Uiso 1 1 calc R . . H68 H 0.6799 0.7048 0.8516 0.143 Uiso 1 1 calc R . . H69 H 0.7100 0.7334 0.9360 0.143 Uiso 1 1 calc R . . C77 C 0.8757(3) 0.4917(3) 0.5420(4) 0.0798(19) Uani 1 1 d . . . H24 H 0.9041 0.5255 0.5297 0.096 Uiso 1 1 calc R . . C78 C 0.9068(3) 0.8884(3) 0.7106(5) 0.092(2) Uani 1 1 d . . . H70 H 0.9520 0.9015 0.7017 0.137 Uiso 1 1 calc R . . H71 H 0.9127 0.8984 0.7630 0.137 Uiso 1 1 calc R . . H72 H 0.8642 0.9134 0.6764 0.137 Uiso 1 1 calc R . . C79 C 0.8922(3) 0.8006(4) 0.6155(4) 0.095(2) Uani 1 1 d . . . H73 H 0.9414 0.8105 0.6139 0.143 Uiso 1 1 calc R . . H74 H 0.8551 0.8299 0.5803 0.143 Uiso 1 1 calc R . . H75 H 0.8795 0.7538 0.6012 0.143 Uiso 1 1 calc R . . C80 C 0.9099(3) 0.4468(4) 0.5985(5) 0.098(3) Uani 1 1 d . . . H25 H 0.9616 0.4508 0.6268 0.118 Uiso 1 1 calc R . . C81 C 0.9566(3) 0.7734(4) 0.7524(4) 0.087(2) Uani 1 1 d . . . H76 H 0.9463 0.7254 0.7455 0.131 Uiso 1 1 calc R . . H77 H 0.9613 0.7863 0.8038 0.131 Uiso 1 1 calc R . . H78 H 1.0031 0.7835 0.7446 0.131 Uiso 1 1 calc R . . C86 C 0.3175(4) 0.9478(3) 0.2095(3) 0.0702(16) Uani 1 1 d . . . H79 H 0.3573 0.9145 0.2212 0.105 Uiso 1 1 calc R . . H80 H 0.3265 0.9830 0.1779 0.105 Uiso 1 1 calc R . . H81 H 0.2695 0.9263 0.1823 0.105 Uiso 1 1 calc R . . O3 O 0.2187(3) 0.6954(3) 0.5733(4) 0.1155(19) Uani 1 1 d . . . H82 H 0.2564 0.6752 0.5719 0.173 Uiso 1 1 calc R . . C87 C 0.2340(5) 0.7219(4) 0.6450(5) 0.107(3) Uani 1 1 d . . . H83 H 0.2707 0.6938 0.6824 0.161 Uiso 1 1 calc R . . H84 H 0.1881 0.7234 0.6562 0.161 Uiso 1 1 calc R . . H85 H 0.2538 0.7673 0.6470 0.161 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 O2 0.0504(17) 0.0443(18) 0.038(2) -0.0049(14) 0.0171(14) -0.0044(13) N1 0.045(2) 0.038(2) 0.029(2) -0.0028(16) 0.0130(16) 0.0023(15) N2 0.048(2) 0.037(2) 0.028(2) -0.0016(15) 0.0156(16) 0.0015(14) N3 0.051(2) 0.037(2) 0.025(2) 0.0008(15) 0.0145(16) -0.0006(15) N4 0.045(2) 0.043(2) 0.031(2) 0.0034(16) 0.0126(16) 0.0003(15) C6 0.043(2) 0.039(2) 0.026(3) 0.0004(18) 0.0155(18) -0.0029(17) N5 0.045(2) 0.043(2) 0.026(2) -0.0053(16) 0.0141(16) 0.0048(15) C8 0.043(2) 0.043(2) 0.029(3) 0.0013(19) 0.0165(19) -0.0002(17) C9 0.042(2) 0.043(3) 0.028(3) -0.0012(19) 0.0149(19) -0.0011(17) C10 0.042(2) 0.045(3) 0.023(3) 0.0017(18) 0.0125(18) -0.0009(17) C11 0.046(2) 0.036(2) 0.028(3) 0.0005(18) 0.0170(19) 0.0005(17) C12 0.052(3) 0.039(2) 0.025(3) 0.0064(18) 0.019(2) 0.0014(18) C13 0.048(2) 0.046(3) 0.028(3) -0.002(2) 0.018(2) 0.0005(18) C14 0.048(2) 0.042(3) 0.035(3) 0.0000(19) 0.021(2) 0.0005(18) C15 0.046(2) 0.034(2) 0.033(3) 0.0014(18) 0.0181(19) -0.0001(17) C16 0.053(3) 0.040(2) 0.026(3) -0.0023(19) 0.018(2) -0.0048(19) C17 0.049(3) 0.038(3) 0.043(3) -0.003(2) 0.004(2) -0.0021(18) C18 0.046(2) 0.040(2) 0.034(3) 0.0005(19) 0.018(2) 0.0027(17) C19 0.041(2) 0.047(3) 0.031(3) -0.002(2) 0.0098(19) 0.0081(18) C20 0.041(2) 0.042(3) 0.038(3) -0.008(2) 0.011(2) -0.0018(18) C21 0.051(2) 0.041(3) 0.034(3) 0.0009(19) 0.022(2) -0.0007(18) C22 0.044(2) 0.036(2) 0.026(3) 0.0003(18) 0.0118(19) 0.0002(16) C23 0.043(2) 0.043(3) 0.032(3) 0.0045(19) 0.020(2) 0.0042(17) C24 0.047(2) 0.041(2) 0.023(3) 0.0033(18) 0.0131(19) 0.0012(17) C25 0.044(2) 0.041(2) 0.034(3) -0.0025(19) 0.013(2) -0.0024(17) C26 0.046(2) 0.041(3) 0.031(3) 0.0017(19) 0.0127(19) -0.0014(18) C27 0.046(2) 0.041(2) 0.029(3) -0.0007(19) 0.0171(19) 0.0031(17) C28 0.043(2) 0.044(3) 0.038(3) -0.004(2) 0.009(2) 0.0038(18) C29 0.053(3) 0.036(2) 0.035(3) -0.0004(19) 0.015(2) -0.0020(18) C30 0.051(3) 0.041(2) 0.028(3) -0.0024(19) 0.014(2) 0.0070(18) C31 0.064(3) 0.035(2) 0.029(3) -0.0005(19) 0.014(2) 0.0049(19) C32 0.043(2) 0.039(2) 0.040(3) -0.004(2) 0.015(2) 0.0015(17) C33 0.049(3) 0.050(3) 0.038(3) -0.003(2) 0.004(2) 0.001(2) C34 0.057(3) 0.036(2) 0.025(3) 0.0027(19) 0.015(2) -0.0019(18) C35 0.045(2) 0.052(3) 0.032(3) 0.002(2) 0.017(2) 0.0003(19) C36 0.047(2) 0.040(2) 0.027(3) 0.0026(18) 0.0143(19) 0.0031(17) C37 0.048(2) 0.041(3) 0.028(3) 0.0024(19) 0.0157(19) -0.0011(18) C38 0.043(2) 0.037(2) 0.034(3) -0.0035(19) 0.0092(19) 0.0034(17) C39 0.051(3) 0.038(2) 0.027(3) 0.0042(18) 0.016(2) 0.0001(18) C40 0.043(2) 0.041(2) 0.030(3) 0.0003(19) 0.0131(19) 0.0010(17) C41 0.047(2) 0.040(2) 0.021(3) 0.0006(17) 0.0109(18) 0.0001(17) C42 0.050(3) 0.048(3) 0.034(3) 0.003(2) 0.006(2) 0.0085(19) C43 0.059(3) 0.045(3) 0.035(3) 0.006(2) 0.020(2) 0.004(2) C44 0.045(2) 0.047(3) 0.032(3) 0.001(2) 0.016(2) 0.0048(18) C45 0.046(2) 0.038(2) 0.032(3) -0.0016(19) 0.0156(19) -0.0007(17) C46 0.056(3) 0.059(3) 0.030(3) 0.000(2) 0.018(2) 0.005(2) C47 0.047(2) 0.043(3) 0.029(3) -0.0002(19) 0.0127(19) 0.0043(18) C48 0.040(2) 0.049(3) 0.028(3) -0.0007(19) 0.0156(19) 0.0015(18) C49 0.054(3) 0.040(3) 0.027(3) 0.0006(18) 0.014(2) -0.0028(18) C50 0.062(3) 0.052(3) 0.058(4) -0.009(3) 0.038(3) -0.002(2) C51 0.045(2) 0.046(3) 0.037(3) 0.000(2) 0.012(2) 0.0061(19) C52 0.049(2) 0.048(3) 0.033(3) -0.001(2) 0.014(2) 0.0040(19) C53 0.058(3) 0.059(3) 0.028(3) -0.005(2) 0.018(2) 0.002(2) C54 0.055(3) 0.057(3) 0.034(3) -0.001(2) 0.020(2) -0.005(2) C55 0.045(2) 0.042(3) 0.033(3) 0.002(2) 0.009(2) 0.0002(18) C56 0.044(2) 0.055(3) 0.037(3) 0.002(2) 0.013(2) -0.0072(19) C57 0.073(3) 0.045(3) 0.039(3) 0.003(2) 0.028(2) 0.010(2) C58 0.055(3) 0.050(3) 0.042(3) -0.007(2) 0.020(2) 0.000(2) C59 0.049(3) 0.048(3) 0.065(4) -0.002(2) 0.029(2) 0.002(2) C60 0.061(3) 0.049(3) 0.058(4) 0.004(3) -0.001(3) 0.004(2) C61 0.048(3) 0.062(3) 0.062(4) 0.005(3) 0.020(2) 0.004(2) C62 0.049(3) 0.058(3) 0.048(4) -0.002(2) 0.012(2) -0.001(2) C63 0.087(3) 0.046(3) 0.025(3) -0.006(2) 0.021(2) -0.008(2) C64 0.066(3) 0.038(3) 0.057(4) 0.003(2) 0.030(3) 0.003(2) C65 0.077(4) 0.092(4) 0.047(4) -0.009(3) 0.029(3) -0.009(3) C66 0.060(3) 0.060(3) 0.049(4) 0.002(3) 0.009(3) -0.005(2) C67 0.054(3) 0.073(4) 0.052(4) 0.013(3) 0.018(2) -0.011(2) C68 0.044(3) 0.101(4) 0.037(3) -0.006(3) 0.010(2) -0.013(2) C69 0.075(4) 0.066(4) 0.080(5) 0.003(3) 0.054(3) 0.006(3) C70 0.059(3) 0.063(4) 0.103(5) 0.003(3) 0.046(3) 0.012(2) C71 0.106(4) 0.080(4) 0.036(4) -0.013(3) 0.020(3) 0.000(3) C72 0.050(3) 0.067(4) 0.118(6) -0.019(4) 0.037(3) -0.010(2) C73 0.086(4) 0.062(4) 0.056(4) 0.004(3) 0.036(3) -0.002(3) C74 0.094(4) 0.063(4) 0.059(4) 0.020(3) 0.040(3) 0.025(3) C75 0.076(4) 0.062(4) 0.092(5) 0.006(3) -0.019(4) 0.017(3) C76 0.188(7) 0.057(4) 0.049(4) 0.004(3) 0.052(5) -0.019(4) C77 0.059(4) 0.074(4) 0.096(5) 0.002(4) 0.015(3) -0.011(3) C78 0.070(4) 0.071(4) 0.137(7) 0.006(4) 0.042(4) -0.007(3) C79 0.058(4) 0.157(7) 0.071(5) 0.015(4) 0.024(3) -0.018(4) C80 0.058(4) 0.083(5) 0.119(7) -0.008(4) -0.010(4) 0.002(3) C81 0.057(3) 0.105(5) 0.090(6) 0.023(4) 0.015(3) 0.007(3) C86 0.116(5) 0.057(3) 0.052(4) 0.008(3) 0.048(3) 0.017(3) O3 0.109(4) 0.125(5) 0.114(5) -0.025(4) 0.043(3) 0.010(3) C87 0.138(7) 0.111(6) 0.077(6) -0.021(5) 0.043(5) -0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O2 C16 1.231(5) . ? N1 C6 1.363(5) . ? N1 C15 1.372(5) . ? N1 H26 0.8800 . ? N2 C13 1.356(5) . ? N2 C27 1.385(5) . ? N3 C37 1.357(5) . ? N3 C26 1.411(5) . ? N4 C34 1.322(6) . ? N4 C39 1.362(5) . ? C6 C10 1.413(6) . ? C6 C29 1.426(6) . ? N5 C8 1.363(5) . ? N5 C12 1.382(5) . ? N5 H27 0.8800 . ? C8 C9 1.379(6) . ? C8 C16 1.503(6) . ? C9 C13 1.425(6) . ? C9 C22 1.500(6) . ? C10 C26 1.385(6) . ? C10 C41 1.503(6) . ? C11 C39 1.376(6) . ? C11 C12 1.412(6) . ? C11 C16 1.468(6) . ? C12 C36 1.397(6) . ? C13 C28 1.441(6) . ? C14 C29 1.360(6) . ? C14 C15 1.418(6) . ? C14 H1 0.9500 . ? C15 C23 1.398(6) . ? C17 C31 1.380(7) . ? C17 C55 1.380(7) . ? C17 H2 0.9500 . ? C18 C24 1.387(6) . ? C18 C22 1.388(6) . ? C18 H3 0.9500 . ? C19 C28 1.345(6) . ? C19 C27 1.445(6) . ? C19 H4 0.9500 . ? C20 C38 1.389(6) . ? C20 C45 1.396(6) . ? C20 C59 1.524(6) . ? C21 C43 1.372(6) . ? C21 C52 1.406(7) . ? C21 C39 1.490(6) . ? C22 C48 1.388(6) . ? C23 C27 1.385(6) . ? C23 C32 1.498(6) . ? C24 C25 1.399(6) . ? C24 C35 1.522(6) . ? C25 C40 1.385(6) . ? C25 H5 0.9500 . ? C26 C33 1.419(6) . ? C28 H6 0.9500 . ? C29 H7 0.9500 . ? C30 C38 1.382(6) . ? C30 C44 1.392(6) . ? C30 C57 1.546(7) . ? C31 C49 1.423(6) . ? C31 C63 1.539(7) . ? C32 C45 1.378(6) . ? C32 C44 1.395(6) . ? C33 C42 1.349(7) . ? C33 H8 0.9500 . ? C34 C36 1.436(6) . ? C34 C51 1.497(6) . ? C35 C54 1.528(6) . ? C35 C46 1.543(6) . ? C35 C53 1.541(6) . ? C36 C37 1.441(6) . ? C37 C42 1.444(6) . ? C38 H9 0.9500 . ? C40 C48 1.402(6) . ? C40 C56 1.528(6) . ? C41 C49 1.367(6) . ? C41 C47 1.405(6) . ? C42 H10 0.9500 . ? C43 C64 1.382(7) . ? C43 H11 0.9500 . ? C44 H12 0.9500 . ? C45 H13 0.9500 . ? C46 H28 0.9800 . ? C46 H29 0.9800 . ? C46 H30 0.9800 . ? C47 C55 1.387(6) . ? C47 H14 0.9500 . ? C48 H15 0.9500 . ? C49 H16 0.9500 . ? C50 C58 1.373(7) . ? C50 C64 1.384(8) . ? C50 H17 0.9500 . ? C51 C60 1.372(7) . ? C51 C66 1.400(7) . ? C52 C58 1.381(6) . ? C52 H18 0.9500 . ? C53 H31 0.9800 . ? C53 H32 0.9800 . ? C53 H33 0.9800 . ? C54 H34 0.9800 . ? C54 H35 0.9800 . ? C54 H36 0.9800 . ? C55 C62 1.553(7) . ? C56 C68 1.535(7) . ? C56 C61 1.542(7) . ? C56 C67 1.549(7) . ? C57 C86 1.516(7) . ? C57 C73 1.531(7) . ? C57 C74 1.529(7) . ? C58 H19 0.9500 . ? C59 C70 1.530(7) . ? C59 C69 1.529(8) . ? C59 C72 1.541(7) . ? C60 C75 1.385(8) . ? C60 H20 0.9500 . ? C61 H37 0.9800 . ? C61 H38 0.9800 . ? C61 H39 0.9800 . ? C62 C81 1.518(8) . ? C62 C79 1.534(9) . ? C62 C78 1.556(8) . ? C63 C76 1.533(8) . ? C63 C65 1.530(8) . ? C63 C71 1.551(7) . ? C64 H21 0.9500 . ? C65 H40 0.9800 . ? C65 H41 0.9800 . ? C65 H42 0.9800 . ? C66 C77 1.359(7) . ? C66 H22 0.9500 . ? C67 H43 0.9800 . ? C67 H44 0.9800 . ? C67 H45 0.9800 . ? C68 H46 0.9800 . ? C68 H47 0.9800 . ? C68 H48 0.9800 . ? C69 H49 0.9800 . ? C69 H50 0.9800 . ? C69 H51 0.9800 . ? C70 H52 0.9800 . ? C70 H53 0.9800 . ? C70 H54 0.9800 . ? C71 H55 0.9800 . ? C71 H56 0.9800 . ? C71 H57 0.9800 . ? C72 H58 0.9800 . ? C72 H59 0.9800 . ? C72 H60 0.9800 . ? C73 H61 0.9800 . ? C73 H62 0.9800 . ? C73 H63 0.9800 . ? C74 H64 0.9800 . ? C74 H65 0.9800 . ? C74 H66 0.9800 . ? C75 C80 1.387(10) . ? C75 H23 0.9500 . ? C76 H67 0.9800 . ? C76 H68 0.9800 . ? C76 H69 0.9800 . ? C77 C80 1.371(10) . ? C77 H24 0.9500 . ? C78 H70 0.9800 . ? C78 H71 0.9800 . ? C78 H72 0.9800 . ? C79 H73 0.9800 . ? C79 H74 0.9800 . ? C79 H75 0.9800 . ? C80 H25 0.9500 . ? C81 H76 0.9800 . ? C81 H77 0.9800 . ? C81 H78 0.9800 . ? C86 H79 0.9800 . ? C86 H80 0.9800 . ? C86 H81 0.9800 . ? O3 C87 1.391(9) . ? O3 H82 0.8400 . ? C87 H83 0.9800 . ? C87 H84 0.9800 . ? C87 H85 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 N1 C15 107.3(3) . . ? C6 N1 H26 126.3 . . ? C15 N1 H26 126.3 . . ? C13 N2 C27 107.1(3) . . ? C37 N3 C26 106.4(3) . . ? C34 N4 C39 119.2(4) . . ? N1 C6 C10 125.2(4) . . ? N1 C6 C29 109.2(4) . . ? C10 C6 C29 125.6(4) . . ? C8 N5 C12 109.5(4) . . ? C8 N5 H27 125.2 . . ? C12 N5 H27 125.2 . . ? N5 C8 C9 127.7(4) . . ? N5 C8 C16 107.9(3) . . ? C9 C8 C16 124.3(4) . . ? C8 C9 C13 124.2(4) . . ? C8 C9 C22 118.7(4) . . ? C13 C9 C22 116.5(4) . . ? C26 C10 C6 126.2(4) . . ? C26 C10 C41 115.6(4) . . ? C6 C10 C41 118.2(4) . . ? C39 C11 C12 120.1(4) . . ? C39 C11 C16 134.0(4) . . ? C12 C11 C16 105.9(3) . . ? N5 C12 C36 127.8(4) . . ? N5 C12 C11 111.3(4) . . ? C36 C12 C11 120.9(4) . . ? N2 C13 C9 125.8(4) . . ? N2 C13 C28 109.7(4) . . ? C9 C13 C28 124.4(4) . . ? C29 C14 C15 107.4(4) . . ? C29 C14 H1 126.3 . . ? C15 C14 H1 126.3 . . ? N1 C15 C23 125.2(4) . . ? N1 C15 C14 109.0(4) . . ? C23 C15 C14 125.7(4) . . ? O2 C16 C11 128.9(4) . . ? O2 C16 C8 126.3(4) . . ? C11 C16 C8 104.6(3) . . ? C31 C17 C55 123.5(4) . . ? C31 C17 H2 118.2 . . ? C55 C17 H2 118.2 . . ? C24 C18 C22 121.9(4) . . ? C24 C18 H3 119.0 . . ? C22 C18 H3 119.0 . . ? C28 C19 C27 107.5(4) . . ? C28 C19 H4 126.3 . . ? C27 C19 H4 126.3 . . ? C38 C20 C45 117.7(4) . . ? C38 C20 C59 123.5(4) . . ? C45 C20 C59 118.8(4) . . ? C43 C21 C52 118.3(4) . . ? C43 C21 C39 120.5(4) . . ? C52 C21 C39 121.0(4) . . ? C48 C22 C18 119.4(4) . . ? C48 C22 C9 123.2(4) . . ? C18 C22 C9 117.4(4) . . ? C27 C23 C15 126.6(4) . . ? C27 C23 C32 115.7(4) . . ? C15 C23 C32 117.7(4) . . ? C18 C24 C25 117.4(4) . . ? C18 C24 C35 118.7(4) . . ? C25 C24 C35 123.9(4) . . ? C40 C25 C24 122.2(4) . . ? C40 C25 H5 118.9 . . ? C24 C25 H5 118.9 . . ? C10 C26 N3 126.8(4) . . ? C10 C26 C33 124.3(4) . . ? N3 C26 C33 108.9(4) . . ? C23 C27 N2 126.5(4) . . ? C23 C27 C19 124.7(4) . . ? N2 C27 C19 108.5(4) . . ? C19 C28 C13 107.2(4) . . ? C19 C28 H6 126.4 . . ? C13 C28 H6 126.4 . . ? C14 C29 C6 107.0(4) . . ? C14 C29 H7 126.5 . . ? C6 C29 H7 126.5 . . ? C38 C30 C44 117.8(4) . . ? C38 C30 C57 122.9(4) . . ? C44 C30 C57 119.3(4) . . ? C17 C31 C49 117.4(4) . . ? C17 C31 C63 124.0(4) . . ? C49 C31 C63 118.6(4) . . ? C45 C32 C44 119.6(4) . . ? C45 C32 C23 120.6(4) . . ? C44 C32 C23 119.7(4) . . ? C42 C33 C26 107.7(4) . . ? C42 C33 H8 126.2 . . ? C26 C33 H8 126.2 . . ? N4 C34 C36 125.4(4) . . ? N4 C34 C51 112.2(4) . . ? C36 C34 C51 122.2(4) . . ? C24 C35 C54 110.1(4) . . ? C24 C35 C46 108.7(4) . . ? C54 C35 C46 109.4(4) . . ? C24 C35 C53 112.1(4) . . ? C54 C35 C53 108.5(4) . . ? C46 C35 C53 108.0(4) . . ? C12 C36 C34 113.7(4) . . ? C12 C36 C37 124.5(4) . . ? C34 C36 C37 121.7(4) . . ? N3 C37 C36 123.3(4) . . ? N3 C37 C42 109.3(4) . . ? C36 C37 C42 127.3(4) . . ? C30 C38 C20 123.0(4) . . ? C30 C38 H9 118.5 . . ? C20 C38 H9 118.5 . . ? N4 C39 C11 120.4(4) . . ? N4 C39 C21 113.7(4) . . ? C11 C39 C21 125.8(4) . . ? C25 C40 C48 118.7(4) . . ? C25 C40 C56 123.0(4) . . ? C48 C40 C56 118.4(4) . . ? C49 C41 C47 120.7(4) . . ? C49 C41 C10 121.0(4) . . ? C47 C41 C10 118.2(4) . . ? C33 C42 C37 107.6(4) . . ? C33 C42 H10 126.2 . . ? C37 C42 H10 126.2 . . ? C21 C43 C64 121.6(5) . . ? C21 C43 H11 119.2 . . ? C64 C43 H11 119.2 . . ? C30 C44 C32 120.9(4) . . ? C30 C44 H12 119.6 . . ? C32 C44 H12 119.6 . . ? C32 C45 C20 121.1(4) . . ? C32 C45 H13 119.5 . . ? C20 C45 H13 119.5 . . ? C35 C46 H28 109.5 . . ? C35 C46 H29 109.5 . . ? H28 C46 H29 109.5 . . ? C35 C46 H30 109.5 . . ? H28 C46 H30 109.5 . . ? H29 C46 H30 109.5 . . ? C55 C47 C41 120.2(4) . . ? C55 C47 H14 119.9 . . ? C41 C47 H14 119.9 . . ? C22 C48 C40 120.3(4) . . ? C22 C48 H15 119.8 . . ? C40 C48 H15 119.8 . . ? C41 C49 C31 120.0(4) . . ? C41 C49 H16 120.0 . . ? C31 C49 H16 120.0 . . ? C58 C50 C64 120.7(5) . . ? C58 C50 H17 119.7 . . ? C64 C50 H17 119.7 . . ? C60 C51 C66 119.0(4) . . ? C60 C51 C34 120.3(4) . . ? C66 C51 C34 120.7(4) . . ? C58 C52 C21 120.5(4) . . ? C58 C52 H18 119.7 . . ? C21 C52 H18 119.7 . . ? C35 C53 H31 109.5 . . ? C35 C53 H32 109.5 . . ? H31 C53 H32 109.5 . . ? C35 C53 H33 109.5 . . ? H31 C53 H33 109.5 . . ? H32 C53 H33 109.5 . . ? C35 C54 H34 109.5 . . ? C35 C54 H35 109.5 . . ? H34 C54 H35 109.5 . . ? C35 C54 H36 109.5 . . ? H34 C54 H36 109.5 . . ? H35 C54 H36 109.5 . . ? C17 C55 C47 118.1(4) . . ? C17 C55 C62 120.6(4) . . ? C47 C55 C62 121.3(4) . . ? C40 C56 C68 112.1(4) . . ? C40 C56 C61 109.4(4) . . ? C68 C56 C61 108.3(4) . . ? C40 C56 C67 110.1(4) . . ? C68 C56 C67 107.8(4) . . ? C61 C56 C67 109.2(4) . . ? C86 C57 C73 107.9(5) . . ? C86 C57 C74 110.1(5) . . ? C73 C57 C74 108.7(4) . . ? C86 C57 C30 108.9(4) . . ? C73 C57 C30 110.6(4) . . ? C74 C57 C30 110.7(4) . . ? C50 C58 C52 119.7(5) . . ? C50 C58 H19 120.2 . . ? C52 C58 H19 120.2 . . ? C20 C59 C70 111.8(4) . . ? C20 C59 C69 110.2(4) . . ? C70 C59 C69 108.4(5) . . ? C20 C59 C72 108.3(4) . . ? C70 C59 C72 108.3(4) . . ? C69 C59 C72 109.8(5) . . ? C51 C60 C75 119.9(6) . . ? C51 C60 H20 120.0 . . ? C75 C60 H20 120.0 . . ? C56 C61 H37 109.5 . . ? C56 C61 H38 109.5 . . ? H37 C61 H38 109.5 . . ? C56 C61 H39 109.5 . . ? H37 C61 H39 109.5 . . ? H38 C61 H39 109.5 . . ? C81 C62 C79 110.3(5) . . ? C81 C62 C55 109.4(5) . . ? C79 C62 C55 112.9(4) . . ? C81 C62 C78 109.5(5) . . ? C79 C62 C78 105.6(6) . . ? C55 C62 C78 109.1(4) . . ? C76 C63 C65 108.7(5) . . ? C76 C63 C71 108.7(5) . . ? C65 C63 C71 107.8(4) . . ? C76 C63 C31 108.4(4) . . ? C65 C63 C31 111.4(4) . . ? C71 C63 C31 111.8(4) . . ? C50 C64 C43 119.1(5) . . ? C50 C64 H21 120.4 . . ? C43 C64 H21 120.4 . . ? C63 C65 H40 109.5 . . ? C63 C65 H41 109.5 . . ? H40 C65 H41 109.5 . . ? C63 C65 H42 109.5 . . ? H40 C65 H42 109.5 . . ? H41 C65 H42 109.5 . . ? C77 C66 C51 121.0(5) . . ? C77 C66 H22 119.5 . . ? C51 C66 H22 119.5 . . ? C56 C67 H43 109.5 . . ? C56 C67 H44 109.5 . . ? H43 C67 H44 109.5 . . ? C56 C67 H45 109.5 . . ? H43 C67 H45 109.5 . . ? H44 C67 H45 109.5 . . ? C56 C68 H46 109.5 . . ? C56 C68 H47 109.5 . . ? H46 C68 H47 109.5 . . ? C56 C68 H48 109.5 . . ? H46 C68 H48 109.5 . . ? H47 C68 H48 109.5 . . ? C59 C69 H49 109.5 . . ? C59 C69 H50 109.5 . . ? H49 C69 H50 109.5 . . ? C59 C69 H51 109.5 . . ? H49 C69 H51 109.5 . . ? H50 C69 H51 109.5 . . ? C59 C70 H52 109.5 . . ? C59 C70 H53 109.5 . . ? H52 C70 H53 109.5 . . ? C59 C70 H54 109.5 . . ? H52 C70 H54 109.5 . . ? H53 C70 H54 109.5 . . ? C63 C71 H55 109.5 . . ? C63 C71 H56 109.5 . . ? H55 C71 H56 109.5 . . ? C63 C71 H57 109.5 . . ? H55 C71 H57 109.5 . . ? H56 C71 H57 109.5 . . ? C59 C72 H58 109.5 . . ? C59 C72 H59 109.5 . . ? H58 C72 H59 109.5 . . ? C59 C72 H60 109.5 . . ? H58 C72 H60 109.5 . . ? H59 C72 H60 109.5 . . ? C57 C73 H61 109.5 . . ? C57 C73 H62 109.5 . . ? H61 C73 H62 109.5 . . ? C57 C73 H63 109.5 . . ? H61 C73 H63 109.5 . . ? H62 C73 H63 109.5 . . ? C57 C74 H64 109.5 . . ? C57 C74 H65 109.5 . . ? H64 C74 H65 109.5 . . ? C57 C74 H66 109.5 . . ? H64 C74 H66 109.5 . . ? H65 C74 H66 109.5 . . ? C80 C75 C60 120.0(6) . . ? C80 C75 H23 120.0 . . ? C60 C75 H23 120.0 . . ? C63 C76 H67 109.5 . . ? C63 C76 H68 109.5 . . ? H67 C76 H68 109.5 . . ? C63 C76 H69 109.5 . . ? H67 C76 H69 109.5 . . ? H68 C76 H69 109.5 . . ? C66 C77 C80 119.9(6) . . ? C66 C77 H24 120.1 . . ? C80 C77 H24 120.1 . . ? C62 C78 H70 109.5 . . ? C62 C78 H71 109.5 . . ? H70 C78 H71 109.5 . . ? C62 C78 H72 109.5 . . ? H70 C78 H72 109.5 . . ? H71 C78 H72 109.5 . . ? C62 C79 H73 109.5 . . ? C62 C79 H74 109.5 . . ? H73 C79 H74 109.5 . . ? C62 C79 H75 109.5 . . ? H73 C79 H75 109.5 . . ? H74 C79 H75 109.5 . . ? C77 C80 C75 120.1(6) . . ? C77 C80 H25 120.0 . . ? C75 C80 H25 120.0 . . ? C62 C81 H76 109.5 . . ? C62 C81 H77 109.5 . . ? H76 C81 H77 109.5 . . ? C62 C81 H78 109.5 . . ? H76 C81 H78 109.5 . . ? H77 C81 H78 109.5 . . ? C57 C86 H79 109.5 . . ? C57 C86 H80 109.5 . . ? H79 C86 H80 109.5 . . ? C57 C86 H81 109.5 . . ? H79 C86 H81 109.5 . . ? H80 C86 H81 109.5 . . ? C87 O3 H82 109.5 . . ? O3 C87 H83 109.5 . . ? O3 C87 H84 109.5 . . ? H83 C87 H84 109.5 . . ? O3 C87 H85 109.5 . . ? H83 C87 H85 109.5 . . ? H84 C87 H85 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 N1 C6 C10 -179.6(4) . . . . ? C15 N1 C6 C29 -0.3(5) . . . . ? C12 N5 C8 C9 -169.4(4) . . . . ? C12 N5 C8 C16 7.5(5) . . . . ? N5 C8 C9 C13 -7.5(7) . . . . ? C16 C8 C9 C13 176.0(4) . . . . ? N5 C8 C9 C22 162.9(4) . . . . ? C16 C8 C9 C22 -13.5(6) . . . . ? N1 C6 C10 C26 -0.2(7) . . . . ? C29 C6 C10 C26 -179.3(4) . . . . ? N1 C6 C10 C41 179.6(4) . . . . ? C29 C6 C10 C41 0.5(7) . . . . ? C8 N5 C12 C36 175.8(4) . . . . ? C8 N5 C12 C11 -3.3(5) . . . . ? C39 C11 C12 N5 179.0(4) . . . . ? C16 C11 C12 N5 -2.5(5) . . . . ? C39 C11 C12 C36 -0.2(7) . . . . ? C16 C11 C12 C36 178.3(4) . . . . ? C27 N2 C13 C9 176.7(4) . . . . ? C27 N2 C13 C28 -0.7(5) . . . . ? C8 C9 C13 N2 0.1(7) . . . . ? C22 C9 C13 N2 -170.6(4) . . . . ? C8 C9 C13 C28 177.0(4) . . . . ? C22 C9 C13 C28 6.4(6) . . . . ? C6 N1 C15 C23 -179.3(4) . . . . ? C6 N1 C15 C14 0.6(5) . . . . ? C29 C14 C15 N1 -0.6(5) . . . . ? C29 C14 C15 C23 179.3(4) . . . . ? C39 C11 C16 O2 8.2(9) . . . . ? C12 C11 C16 O2 -170.1(5) . . . . ? C39 C11 C16 C8 -175.1(5) . . . . ? C12 C11 C16 C8 6.6(5) . . . . ? N5 C8 C16 O2 168.0(4) . . . . ? C9 C8 C16 O2 -14.9(7) . . . . ? N5 C8 C16 C11 -8.7(5) . . . . ? C9 C8 C16 C11 168.3(4) . . . . ? C24 C18 C22 C48 -1.9(6) . . . . ? C24 C18 C22 C9 179.6(4) . . . . ? C8 C9 C22 C48 123.9(5) . . . . ? C13 C9 C22 C48 -64.9(6) . . . . ? C8 C9 C22 C18 -57.6(6) . . . . ? C13 C9 C22 C18 113.5(4) . . . . ? N1 C15 C23 C27 4.0(7) . . . . ? C14 C15 C23 C27 -175.9(5) . . . . ? N1 C15 C23 C32 -177.2(4) . . . . ? C14 C15 C23 C32 2.9(7) . . . . ? C22 C18 C24 C25 2.2(6) . . . . ? C22 C18 C24 C35 -176.8(4) . . . . ? C18 C24 C25 C40 -0.8(6) . . . . ? C35 C24 C25 C40 178.2(4) . . . . ? C6 C10 C26 N3 5.0(8) . . . . ? C41 C10 C26 N3 -174.8(4) . . . . ? C6 C10 C26 C33 -171.6(5) . . . . ? C41 C10 C26 C33 8.6(7) . . . . ? C37 N3 C26 C10 -179.8(4) . . . . ? C37 N3 C26 C33 -2.7(5) . . . . ? C15 C23 C27 N2 -0.4(8) . . . . ? C32 C23 C27 N2 -179.2(4) . . . . ? C15 C23 C27 C19 -173.0(4) . . . . ? C32 C23 C27 C19 8.1(7) . . . . ? C13 N2 C27 C23 -172.5(4) . . . . ? C13 N2 C27 C19 1.1(5) . . . . ? C28 C19 C27 C23 172.6(4) . . . . ? C28 C19 C27 N2 -1.2(5) . . . . ? C27 C19 C28 C13 0.7(5) . . . . ? N2 C13 C28 C19 -0.1(5) . . . . ? C9 C13 C28 C19 -177.4(4) . . . . ? C15 C14 C29 C6 0.4(5) . . . . ? N1 C6 C29 C14 0.0(5) . . . . ? C10 C6 C29 C14 179.2(4) . . . . ? C55 C17 C31 C49 0.0(7) . . . . ? C55 C17 C31 C63 178.4(4) . . . . ? C27 C23 C32 C45 74.5(6) . . . . ? C15 C23 C32 C45 -104.5(5) . . . . ? C27 C23 C32 C44 -103.2(5) . . . . ? C15 C23 C32 C44 77.8(6) . . . . ? C10 C26 C33 C42 177.8(5) . . . . ? N3 C26 C33 C42 0.6(6) . . . . ? C39 N4 C34 C36 4.1(7) . . . . ? C39 N4 C34 C51 -171.7(4) . . . . ? C18 C24 C35 C54 -60.1(5) . . . . ? C25 C24 C35 C54 120.9(4) . . . . ? C18 C24 C35 C46 59.7(5) . . . . ? C25 C24 C35 C46 -119.4(4) . . . . ? C18 C24 C35 C53 178.9(4) . . . . ? C25 C24 C35 C53 -0.1(6) . . . . ? N5 C12 C36 C34 -175.0(4) . . . . ? C11 C12 C36 C34 4.1(6) . . . . ? N5 C12 C36 C37 7.0(7) . . . . ? C11 C12 C36 C37 -173.9(4) . . . . ? N4 C34 C36 C12 -6.3(7) . . . . ? C51 C34 C36 C12 169.1(4) . . . . ? N4 C34 C36 C37 171.8(4) . . . . ? C51 C34 C36 C37 -12.8(7) . . . . ? C26 N3 C37 C36 -178.9(4) . . . . ? C26 N3 C37 C42 3.7(5) . . . . ? C12 C36 C37 N3 -15.1(7) . . . . ? C34 C36 C37 N3 167.1(4) . . . . ? C12 C36 C37 C42 161.9(5) . . . . ? C34 C36 C37 C42 -15.9(7) . . . . ? C44 C30 C38 C20 -1.3(7) . . . . ? C57 C30 C38 C20 179.7(4) . . . . ? C45 C20 C38 C30 -0.2(7) . . . . ? C59 C20 C38 C30 179.6(4) . . . . ? C34 N4 C39 C11 0.4(6) . . . . ? C34 N4 C39 C21 176.4(4) . . . . ? C12 C11 C39 N4 -2.3(7) . . . . ? C16 C11 C39 N4 179.6(5) . . . . ? C12 C11 C39 C21 -177.8(4) . . . . ? C16 C11 C39 C21 4.1(8) . . . . ? C43 C21 C39 N4 37.1(6) . . . . ? C52 C21 C39 N4 -137.7(4) . . . . ? C43 C21 C39 C11 -147.2(5) . . . . ? C52 C21 C39 C11 38.1(7) . . . . ? C24 C25 C40 C48 -1.0(6) . . . . ? C24 C25 C40 C56 178.4(4) . . . . ? C26 C10 C41 C49 -109.2(5) . . . . ? C6 C10 C41 C49 71.0(6) . . . . ? C26 C10 C41 C47 68.9(5) . . . . ? C6 C10 C41 C47 -111.0(5) . . . . ? C26 C33 C42 C37 1.6(6) . . . . ? N3 C37 C42 C33 -3.4(6) . . . . ? C36 C37 C42 C33 179.3(5) . . . . ? C52 C21 C43 C64 -3.4(7) . . . . ? C39 C21 C43 C64 -178.3(4) . . . . ? C38 C30 C44 C32 2.6(7) . . . . ? C57 C30 C44 C32 -178.4(4) . . . . ? C45 C32 C44 C30 -2.4(7) . . . . ? C23 C32 C44 C30 175.4(4) . . . . ? C44 C32 C45 C20 0.8(7) . . . . ? C23 C32 C45 C20 -176.9(4) . . . . ? C38 C20 C45 C32 0.4(7) . . . . ? C59 C20 C45 C32 -179.3(4) . . . . ? C49 C41 C47 C55 2.0(6) . . . . ? C10 C41 C47 C55 -176.0(4) . . . . ? C18 C22 C48 C40 0.0(6) . . . . ? C9 C22 C48 C40 178.4(4) . . . . ? C25 C40 C48 C22 1.4(6) . . . . ? C56 C40 C48 C22 -178.0(4) . . . . ? C47 C41 C49 C31 -2.3(6) . . . . ? C10 C41 C49 C31 175.7(4) . . . . ? C17 C31 C49 C41 1.2(6) . . . . ? C63 C31 C49 C41 -177.2(4) . . . . ? N4 C34 C51 C60 -61.0(6) . . . . ? C36 C34 C51 C60 123.1(5) . . . . ? N4 C34 C51 C66 118.6(5) . . . . ? C36 C34 C51 C66 -57.4(7) . . . . ? C43 C21 C52 C58 1.5(7) . . . . ? C39 C21 C52 C58 176.3(4) . . . . ? C31 C17 C55 C47 -0.3(7) . . . . ? C31 C17 C55 C62 -179.0(4) . . . . ? C41 C47 C55 C17 -0.7(6) . . . . ? C41 C47 C55 C62 178.0(4) . . . . ? C25 C40 C56 C68 2.2(6) . . . . ? C48 C40 C56 C68 -178.4(4) . . . . ? C25 C40 C56 C61 -117.9(5) . . . . ? C48 C40 C56 C61 61.4(5) . . . . ? C25 C40 C56 C67 122.1(5) . . . . ? C48 C40 C56 C67 -58.5(5) . . . . ? C38 C30 C57 C86 -121.2(5) . . . . ? C44 C30 C57 C86 59.8(6) . . . . ? C38 C30 C57 C73 120.4(5) . . . . ? C44 C30 C57 C73 -58.6(6) . . . . ? C38 C30 C57 C74 -0.1(7) . . . . ? C44 C30 C57 C74 -179.0(4) . . . . ? C64 C50 C58 C52 -3.7(7) . . . . ? C21 C52 C58 C50 2.0(7) . . . . ? C38 C20 C59 C70 -3.1(7) . . . . ? C45 C20 C59 C70 176.6(5) . . . . ? C38 C20 C59 C69 -123.8(5) . . . . ? C45 C20 C59 C69 55.9(6) . . . . ? C38 C20 C59 C72 116.0(5) . . . . ? C45 C20 C59 C72 -64.2(6) . . . . ? C66 C51 C60 C75 3.6(9) . . . . ? C34 C51 C60 C75 -176.9(5) . . . . ? C17 C55 C62 C81 60.4(6) . . . . ? C47 C55 C62 C81 -118.3(5) . . . . ? C17 C55 C62 C79 -176.5(5) . . . . ? C47 C55 C62 C79 4.9(7) . . . . ? C17 C55 C62 C78 -59.3(6) . . . . ? C47 C55 C62 C78 122.0(5) . . . . ? C17 C31 C63 C76 -117.8(6) . . . . ? C49 C31 C63 C76 60.6(6) . . . . ? C17 C31 C63 C65 122.7(5) . . . . ? C49 C31 C63 C65 -59.0(6) . . . . ? C17 C31 C63 C71 2.0(7) . . . . ? C49 C31 C63 C71 -179.6(4) . . . . ? C58 C50 C64 C43 1.9(7) . . . . ? C21 C43 C64 C50 1.8(7) . . . . ? C60 C51 C66 C77 -1.5(9) . . . . ? C34 C51 C66 C77 178.9(5) . . . . ? C51 C60 C75 C80 -2.5(11) . . . . ? C51 C66 C77 C80 -1.6(10) . . . . ? C66 C77 C80 C75 2.6(12) . . . . ? C60 C75 C80 C77 -0.6(12) . . . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.477 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.071 # SQUEEZE RESULTS (APPEND TO CIF) 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 _platon_squeeze_void_content 1 0.000 0.500 0.000 446 52 ' ' 2 0.500 0.000 0.000 446 52 ' ' _platon_squeeze_details ; ; # Attachment '3Ni.CIF' data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 707382' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H79 N5 Ni O, 3(C2 H4 Cl2)' _chemical_formula_sum 'C82 H91 Cl6 N5 Ni O' _chemical_formula_weight 1434.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.341(5) _cell_length_b 15.957(6) _cell_length_c 17.625(5) _cell_angle_alpha 73.134(11) _cell_angle_beta 82.737(12) _cell_angle_gamma 69.420(11) _cell_volume 3864(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 25328 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour greem _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 0.506 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_correction_T_max 0.953 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 5.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29611 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.1230 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13165 _reflns_number_gt 9486 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1381P)^2^+15.9713P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13165 _refine_ls_number_parameters 857 _refine_ls_number_restraints 216 _refine_ls_R_factor_all 0.1250 _refine_ls_R_factor_gt 0.0941 _refine_ls_wR_factor_ref 0.2782 _refine_ls_wR_factor_gt 0.2508 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.50665(5) 0.29788(4) 0.30532(4) 0.0175(2) Uani 1 1 d . . . Cl1 Cl 0.80347(15) 0.24349(18) 0.26376(12) 0.0635(6) Uani 1 1 d . . . Cl2 Cl 0.6773(2) 0.41267(17) 0.04307(15) 0.0808(8) Uani 1 1 d . . . Cl3 Cl 0.95180(17) 0.7251(2) 0.41963(16) 0.0769(7) Uani 1 1 d . . . Cl4 Cl 0.9282(3) 0.9701(2) 0.22759(19) 0.1014(10) Uani 1 1 d . . . Cl5 Cl 0.0877(3) 0.7228(2) 0.1558(3) 0.1406(17) Uani 1 1 d DU . . Cl6 Cl 0.1531(4) 0.9356(5) -0.0209(4) 0.244(4) Uani 1 1 d DU . . O1 O 0.7740(3) -0.0259(3) 0.3981(3) 0.0362(11) Uani 1 1 d . . . N1 N 0.6048(3) 0.1964(3) 0.3591(3) 0.0199(10) Uani 1 1 d . . . N2 N 0.4519(3) 0.2134(3) 0.2908(3) 0.0204(10) Uani 1 1 d . . . N3 N 0.4095(3) 0.3992(3) 0.2477(3) 0.0200(10) Uani 1 1 d . . . N4 N 0.5613(3) 0.3814(3) 0.3235(3) 0.0190(9) Uani 1 1 d . . . N5 N 0.7732(4) 0.1746(3) 0.5356(3) 0.0294(11) Uani 1 1 d . . . C1 C 0.6601(4) 0.1985(4) 0.4143(3) 0.0207(11) Uani 1 1 d . . . C2 C 0.7240(4) 0.1103(4) 0.4490(3) 0.0261(12) Uani 1 1 d . . . C3 C 0.7204(4) 0.0498(4) 0.4015(3) 0.0247(12) Uani 1 1 d . . . C4 C 0.6353(4) 0.1062(4) 0.3533(3) 0.0235(12) Uani 1 1 d . . . C5 C 0.5850(4) 0.0688(4) 0.3215(3) 0.0230(12) Uani 1 1 d . . . C6 C 0.4924(4) 0.1201(4) 0.3005(3) 0.0233(12) Uani 1 1 d . . . C7 C 0.4245(4) 0.0798(4) 0.2943(3) 0.0270(13) Uani 1 1 d . . . H2 H 0.4357 0.0176 0.2978 0.032 Uiso 1 1 calc R . . C8 C 0.3419(4) 0.1478(4) 0.2827(4) 0.0305(14) Uani 1 1 d . . . H3 H 0.2847 0.1413 0.2793 0.037 Uiso 1 1 calc R . . C9 C 0.3588(4) 0.2324(4) 0.2766(3) 0.0226(12) Uani 1 1 d . . . C10 C 0.2952(4) 0.3223(4) 0.2504(3) 0.0241(12) Uani 1 1 d . . . C11 C 0.3241(4) 0.4004(4) 0.2309(3) 0.0209(11) Uani 1 1 d . . . C12 C 0.2732(4) 0.4893(4) 0.1828(3) 0.0271(13) Uani 1 1 d . . . H4 H 0.2133 0.5072 0.1644 0.033 Uiso 1 1 calc R . . C13 C 0.3282(4) 0.5425(4) 0.1688(3) 0.0259(12) Uani 1 1 d . . . H5 H 0.3139 0.6036 0.1381 0.031 Uiso 1 1 calc R . . C14 C 0.4122(4) 0.4875(4) 0.2099(3) 0.0212(11) Uani 1 1 d . . . C15 C 0.4810(4) 0.5217(4) 0.2215(3) 0.0212(11) Uani 1 1 d . . . C16 C 0.5482(4) 0.4733(3) 0.2766(3) 0.0213(12) Uani 1 1 d . . . C17 C 0.6075(4) 0.5091(4) 0.3038(3) 0.0251(12) Uani 1 1 d . . . H6 H 0.6145 0.5669 0.2814 0.030 Uiso 1 1 calc R . . C18 C 0.6516(4) 0.4451(4) 0.3673(3) 0.0210(11) Uani 1 1 d . . . H7 H 0.6933 0.4510 0.3978 0.025 Uiso 1 1 calc R . . C19 C 0.6224(4) 0.3657(4) 0.3796(3) 0.0201(11) Uani 1 1 d . . . C20 C 0.6622(4) 0.2767(4) 0.4332(3) 0.0209(11) Uani 1 1 d . . . C21 C 0.6218(4) -0.0306(4) 0.3174(3) 0.0222(12) Uani 1 1 d . . . C22 C 0.6462(4) -0.0490(4) 0.2443(3) 0.0240(12) Uani 1 1 d . . . H8 H 0.6419 -0.0001 0.1991 0.029 Uiso 1 1 calc R . . C23 C 0.6774(4) -0.1399(4) 0.2370(3) 0.0260(13) Uani 1 1 d . . . C24 C 0.6841(4) -0.2111(4) 0.3062(3) 0.0266(13) Uani 1 1 d . . . H9 H 0.7066 -0.2721 0.3027 0.032 Uiso 1 1 calc R . . C25 C 0.6583(4) -0.1944(4) 0.3807(3) 0.0254(12) Uani 1 1 d . . . C26 C 0.6258(4) -0.1029(4) 0.3852(3) 0.0253(12) Uani 1 1 d . . . H10 H 0.6066 -0.0900 0.4340 0.030 Uiso 1 1 calc R . . C27 C 0.7074(5) -0.1618(4) 0.1565(3) 0.0301(14) Uani 1 1 d . . . C28 C 0.6872(6) -0.2483(5) 0.1531(4) 0.0445(18) Uani 1 1 d . . . H27 H 0.7403 -0.3024 0.1709 0.053 Uiso 1 1 calc R . . H28 H 0.6747 -0.2427 0.0995 0.053 Uiso 1 1 calc R . . H29 H 0.6341 -0.2538 0.1867 0.053 Uiso 1 1 calc R . . C29 C 0.6570(7) -0.0825(5) 0.0885(4) 0.058(2) Uani 1 1 d . . . H30 H 0.6009 -0.0910 0.0786 0.070 Uiso 1 1 calc R . . H31 H 0.6965 -0.0814 0.0417 0.070 Uiso 1 1 calc R . . H32 H 0.6415 -0.0248 0.1021 0.070 Uiso 1 1 calc R . . C30 C 0.8124(6) -0.1790(7) 0.1444(5) 0.065(3) Uani 1 1 d . . . H33 H 0.8229 -0.1215 0.1180 0.078 Uiso 1 1 calc R . . H34 H 0.8387 -0.2222 0.1127 0.078 Uiso 1 1 calc R . . H35 H 0.8414 -0.2042 0.1950 0.078 Uiso 1 1 calc R . . C31 C 0.6629(5) -0.2740(4) 0.4560(4) 0.0299(14) Uani 1 1 d . . . C32 C 0.7269(6) -0.3670(4) 0.4436(4) 0.051(2) Uani 1 1 d . . . H36 H 0.6914 -0.3957 0.4250 0.061 Uiso 1 1 calc R . . H37 H 0.7545 -0.4066 0.4930 0.061 Uiso 1 1 calc R . . H38 H 0.7750 -0.3573 0.4052 0.061 Uiso 1 1 calc R . . C33 C 0.7022(7) -0.2582(5) 0.5246(4) 0.052(2) Uani 1 1 d . . . H39 H 0.7688 -0.2858 0.5240 0.063 Uiso 1 1 calc R . . H40 H 0.6768 -0.2863 0.5740 0.063 Uiso 1 1 calc R . . H41 H 0.6855 -0.1928 0.5186 0.063 Uiso 1 1 calc R . . C34 C 0.5643(6) -0.2766(5) 0.4778(5) 0.057(2) Uani 1 1 d . . . H42 H 0.5344 -0.2363 0.5115 0.068 Uiso 1 1 calc R . . H43 H 0.5669 -0.3389 0.5052 0.068 Uiso 1 1 calc R . . H44 H 0.5295 -0.2563 0.4304 0.068 Uiso 1 1 calc R . . C35 C 0.1983(4) 0.3367(4) 0.2329(4) 0.0262(12) Uani 1 1 d . . . C36 C 0.1800(5) 0.3037(6) 0.1739(5) 0.0467(19) Uani 1 1 d . . . H11 H 0.2295 0.2693 0.1472 0.056 Uiso 1 1 calc R . . C37 C 0.0898(5) 0.3210(7) 0.1541(6) 0.065(3) Uani 1 1 d . . . C38 C 0.0169(5) 0.3721(6) 0.1960(5) 0.053(2) Uani 1 1 d . . . H12 H -0.0441 0.3830 0.1841 0.064 Uiso 1 1 calc R . . C39 C 0.0325(4) 0.4070(4) 0.2547(4) 0.0320(14) Uani 1 1 d . . . C40 C 0.1245(4) 0.3880(4) 0.2721(3) 0.0279(13) Uani 1 1 d . . . H13 H 0.1367 0.4105 0.3113 0.034 Uiso 1 1 calc R . . C41 C 0.0725(6) 0.2935(6) 0.0806(6) 0.076(2) Uani 1 1 d DU . . C42 C 0.1305(8) 0.1933(6) 0.0901(6) 0.080(3) Uani 1 1 d DU . . H45 H 0.1881 0.1894 0.0605 0.096 Uiso 1 1 calc R . . H46 H 0.0972 0.1631 0.0706 0.096 Uiso 1 1 calc R . . H47 H 0.1431 0.1632 0.1451 0.096 Uiso 1 1 calc R . . C43 C -0.0282(6) 0.3130(9) 0.0695(7) 0.091(3) Uani 1 1 d DU . . H48 H -0.0480 0.2647 0.1054 0.109 Uiso 1 1 calc R . . H49 H -0.0373 0.3155 0.0160 0.109 Uiso 1 1 calc R . . H50 H -0.0639 0.3715 0.0801 0.109 Uiso 1 1 calc R . . C44 C 0.1074(8) 0.3484(8) 0.0047(6) 0.086(3) Uani 1 1 d DU . . H51 H 0.0573 0.4033 -0.0183 0.103 Uiso 1 1 calc R . . H52 H 0.1298 0.3109 -0.0321 0.103 Uiso 1 1 calc R . . H53 H 0.1571 0.3656 0.0167 0.103 Uiso 1 1 calc R . . C45 C -0.0469(4) 0.4670(4) 0.2976(4) 0.0358(15) Uani 1 1 d . . . C46 C -0.1418(6) 0.4885(7) 0.2637(6) 0.064(2) Uani 1 1 d U . . H54 H -0.1558 0.5453 0.2222 0.077 Uiso 1 1 calc R . . H55 H -0.1890 0.4949 0.3051 0.077 Uiso 1 1 calc R . . H56 H -0.1403 0.4388 0.2427 0.077 Uiso 1 1 calc R . . C47 C -0.0486(7) 0.4202(7) 0.3831(5) 0.076(3) Uani 1 1 d U . . H57 H -0.0871 0.3818 0.3927 0.091 Uiso 1 1 calc R . . H58 H -0.0734 0.4659 0.4125 0.091 Uiso 1 1 calc R . . H59 H 0.0136 0.3824 0.3995 0.091 Uiso 1 1 calc R . . C48 C -0.0342(6) 0.5621(6) 0.2831(6) 0.063(2) Uani 1 1 d U . . H60 H 0.0043 0.5594 0.3233 0.076 Uiso 1 1 calc R . . H61 H -0.0939 0.6087 0.2851 0.076 Uiso 1 1 calc R . . H62 H -0.0051 0.5775 0.2319 0.076 Uiso 1 1 calc R . . C49 C 0.4688(4) 0.6211(4) 0.1774(3) 0.0217(11) Uani 1 1 d . . . C50 C 0.4952(4) 0.6426(4) 0.0974(3) 0.0244(12) Uani 1 1 d . . . H14 H 0.5250 0.5950 0.0731 0.029 Uiso 1 1 calc R . . C51 C 0.4773(4) 0.7347(4) 0.0533(3) 0.0274(13) Uani 1 1 d . . . C52 C 0.4326(4) 0.8035(4) 0.0925(3) 0.0248(12) Uani 1 1 d . . . H15 H 0.4198 0.8653 0.0638 0.030 Uiso 1 1 calc R . . C53 C 0.4061(4) 0.7847(4) 0.1724(4) 0.0263(13) Uani 1 1 d . . . C54 C 0.4256(4) 0.6915(4) 0.2145(3) 0.0238(12) Uani 1 1 d . . . H16 H 0.4094 0.6765 0.2682 0.029 Uiso 1 1 calc R . . C55 C 0.5006(5) 0.7602(4) -0.0355(3) 0.0319(14) Uani 1 1 d . . . C56 C 0.5580(6) 0.6750(5) -0.0651(4) 0.052(2) Uani 1 1 d . . . H63 H 0.6231 0.6636 -0.0607 0.062 Uiso 1 1 calc R . . H64 H 0.5445 0.6861 -0.1196 0.062 Uiso 1 1 calc R . . H65 H 0.5422 0.6219 -0.0336 0.062 Uiso 1 1 calc R . . C57 C 0.4091(6) 0.8053(5) -0.0792(4) 0.0431(17) Uani 1 1 d . . . H66 H 0.3918 0.7585 -0.0914 0.052 Uiso 1 1 calc R . . H67 H 0.4165 0.8497 -0.1275 0.052 Uiso 1 1 calc R . . H68 H 0.3613 0.8362 -0.0463 0.052 Uiso 1 1 calc R . . C58 C 0.5549(6) 0.8283(5) -0.0555(4) 0.0442(18) Uani 1 1 d . . . H69 H 0.5121 0.8907 -0.0673 0.053 Uiso 1 1 calc R . . H70 H 0.5955 0.8192 -0.1007 0.053 Uiso 1 1 calc R . . H71 H 0.5913 0.8176 -0.0110 0.053 Uiso 1 1 calc R . . C59 C 0.3549(5) 0.8607(4) 0.2156(4) 0.0332(14) Uani 1 1 d . . . C60 C 0.3487(6) 0.9576(4) 0.1634(4) 0.0452(18) Uani 1 1 d . . . H72 H 0.4012 0.9726 0.1724 0.054 Uiso 1 1 calc R . . H73 H 0.2923 1.0023 0.1765 0.054 Uiso 1 1 calc R . . H74 H 0.3486 0.9588 0.1087 0.054 Uiso 1 1 calc R . . C61 C 0.2559(5) 0.8566(5) 0.2393(5) 0.0476(18) Uani 1 1 d . . . H75 H 0.2144 0.8961 0.1970 0.057 Uiso 1 1 calc R . . H76 H 0.2349 0.8773 0.2865 0.057 Uiso 1 1 calc R . . H77 H 0.2567 0.7940 0.2490 0.057 Uiso 1 1 calc R . . C62 C 0.4055(5) 0.8421(5) 0.2910(4) 0.0406(17) Uani 1 1 d . . . H78 H 0.3823 0.8021 0.3341 0.049 Uiso 1 1 calc R . . H79 H 0.3951 0.8997 0.3033 0.049 Uiso 1 1 calc R . . H80 H 0.4711 0.8127 0.2831 0.049 Uiso 1 1 calc R . . C63 C 0.7814(4) 0.0995(4) 0.5088(4) 0.0281(13) Uani 1 1 d . . . C64 C 0.7173(4) 0.2582(4) 0.5000(3) 0.0225(12) Uani 1 1 d . . . C65 C 0.8470(5) 0.0108(4) 0.5521(4) 0.0406(16) Uani 1 1 d U . . C66 C 0.8317(5) -0.0726(4) 0.5650(4) 0.0423(16) Uani 1 1 d U . . H17 H 0.7793 -0.0737 0.5445 0.051 Uiso 1 1 calc R . . C67 C 0.8942(6) -0.1554(5) 0.6087(5) 0.0561(19) Uani 1 1 d U . . H18 H 0.8828 -0.2110 0.6177 0.067 Uiso 1 1 calc R . . C68 C 0.9717(7) -0.1540(5) 0.6378(7) 0.077(3) Uani 1 1 d U . . H19 H 1.0126 -0.2088 0.6677 0.093 Uiso 1 1 calc R . . C69 C 0.9901(8) -0.0708(6) 0.6232(7) 0.088(3) Uani 1 1 d U . . H20 H 1.0442 -0.0702 0.6414 0.106 Uiso 1 1 calc R . . C70 C 0.9268(7) 0.0108(5) 0.5812(6) 0.073(2) Uani 1 1 d U . . H21 H 0.9380 0.0665 0.5724 0.088 Uiso 1 1 calc R . . C71 C 0.7122(4) 0.3307(4) 0.5387(3) 0.0238(12) Uani 1 1 d U . . C72 C 0.7921(5) 0.3291(4) 0.5690(4) 0.0297(13) Uani 1 1 d U . . H22 H 0.8491 0.2853 0.5614 0.036 Uiso 1 1 calc R . . C73 C 0.7879(5) 0.3923(4) 0.6105(4) 0.0339(13) Uani 1 1 d U . . H23 H 0.8417 0.3908 0.6308 0.041 Uiso 1 1 calc R . . C74 C 0.7032(5) 0.4576(4) 0.6215(3) 0.0319(13) Uani 1 1 d U . . H24 H 0.7004 0.5000 0.6493 0.038 Uiso 1 1 calc R . . C75 C 0.6224(5) 0.4605(4) 0.5917(3) 0.0300(13) Uani 1 1 d U . . H25 H 0.5658 0.5048 0.5992 0.036 Uiso 1 1 calc R . . C76 C 0.6265(4) 0.3969(4) 0.5505(3) 0.0237(12) Uani 1 1 d U . . H26 H 0.5725 0.3982 0.5308 0.028 Uiso 1 1 calc R . . C77 C 0.7435(7) 0.2778(7) 0.1741(5) 0.068(2) Uani 1 1 d . . . H81 H 0.7812 0.2435 0.1374 0.082 Uiso 1 1 calc R . . H82 H 0.6854 0.2645 0.1848 0.082 Uiso 1 1 calc R . . C78 C 0.7240(7) 0.3797(6) 0.1383(5) 0.065(2) Uani 1 1 d . . . H83 H 0.7812 0.3940 0.1340 0.078 Uiso 1 1 calc R . . H84 H 0.6801 0.4142 0.1721 0.078 Uiso 1 1 calc R . . C79 C 0.9146(7) 0.8155(7) 0.3277(6) 0.074(3) Uani 1 1 d . . . H85 H 0.9293 0.7887 0.2829 0.088 Uiso 1 1 calc R . . H86 H 0.8479 0.8471 0.3299 0.088 Uiso 1 1 calc R . . C80 C 0.9638(8) 0.8801(9) 0.3193(7) 0.090(4) Uani 1 1 d . . . H87 H 1.0305 0.8484 0.3177 0.108 Uiso 1 1 calc R . . H88 H 0.9488 0.9072 0.3640 0.108 Uiso 1 1 calc R . . C81 C 0.0771(9) 0.8340(8) 0.0864(8) 0.130(6) Uani 1 1 d D . . H89 H 0.0263 0.8527 0.0508 0.156 Uiso 1 1 calc R . . H90 H 0.0664 0.8814 0.1139 0.156 Uiso 1 1 calc R . . C82 C 0.1662(8) 0.8183(7) 0.0433(8) 0.126(6) Uani 1 1 d D . . H91 H 0.1754 0.7744 0.0124 0.151 Uiso 1 1 calc R . . H92 H 0.2177 0.7963 0.0788 0.151 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 Ni1 0.0250(4) 0.0111(3) 0.0181(4) -0.0049(2) 0.0012(3) -0.0078(3) Cl1 0.0550(12) 0.0887(16) 0.0467(11) -0.0121(10) -0.0050(9) -0.0269(12) Cl2 0.116(2) 0.0598(14) 0.0617(15) -0.0064(11) -0.0275(14) -0.0228(14) Cl3 0.0612(14) 0.0944(18) 0.0769(16) -0.0219(14) -0.0038(12) -0.0278(13) Cl4 0.140(3) 0.0812(19) 0.086(2) -0.0177(15) 0.0041(19) -0.0468(19) Cl5 0.092(2) 0.0699(18) 0.206(4) 0.013(2) 0.040(2) -0.0177(17) Cl6 0.124(4) 0.212(5) 0.243(5) 0.130(4) 0.025(4) -0.035(3) O1 0.037(3) 0.018(2) 0.053(3) -0.0153(19) -0.009(2) -0.0006(19) N1 0.024(2) 0.014(2) 0.024(2) -0.0079(18) 0.0028(19) -0.0068(19) N2 0.028(3) 0.016(2) 0.020(2) -0.0098(18) 0.0029(19) -0.0092(19) N3 0.027(3) 0.017(2) 0.019(2) -0.0062(17) 0.0019(18) -0.0102(19) N4 0.025(2) 0.014(2) 0.018(2) -0.0052(17) 0.0031(18) -0.0069(19) N5 0.039(3) 0.020(2) 0.028(3) -0.006(2) -0.008(2) -0.005(2) C1 0.025(3) 0.016(3) 0.022(3) -0.006(2) 0.000(2) -0.008(2) C2 0.031(3) 0.019(3) 0.026(3) -0.003(2) -0.003(2) -0.007(2) C3 0.033(3) 0.014(3) 0.029(3) -0.006(2) -0.005(2) -0.010(2) C4 0.032(3) 0.012(2) 0.027(3) -0.006(2) 0.003(2) -0.009(2) C5 0.038(3) 0.014(3) 0.020(3) -0.007(2) 0.004(2) -0.011(2) C6 0.035(3) 0.019(3) 0.020(3) -0.008(2) 0.002(2) -0.013(2) C7 0.039(4) 0.018(3) 0.029(3) -0.009(2) 0.003(3) -0.016(3) C8 0.037(4) 0.031(3) 0.036(3) -0.018(3) 0.007(3) -0.022(3) C9 0.028(3) 0.021(3) 0.023(3) -0.010(2) 0.001(2) -0.010(2) C10 0.029(3) 0.028(3) 0.021(3) -0.011(2) 0.004(2) -0.015(3) C11 0.027(3) 0.019(3) 0.018(3) -0.010(2) 0.003(2) -0.007(2) C12 0.026(3) 0.027(3) 0.029(3) -0.009(2) -0.004(2) -0.007(3) C13 0.035(3) 0.018(3) 0.023(3) 0.000(2) -0.007(2) -0.008(2) C14 0.034(3) 0.016(3) 0.015(3) -0.004(2) 0.000(2) -0.011(2) C15 0.030(3) 0.016(3) 0.018(3) -0.005(2) 0.005(2) -0.009(2) C16 0.033(3) 0.015(2) 0.018(3) -0.005(2) 0.006(2) -0.012(2) C17 0.034(3) 0.017(3) 0.029(3) -0.007(2) 0.005(2) -0.014(2) C18 0.026(3) 0.019(3) 0.022(3) -0.007(2) 0.003(2) -0.011(2) C19 0.023(3) 0.019(3) 0.021(3) -0.009(2) 0.002(2) -0.008(2) C20 0.024(3) 0.014(2) 0.026(3) -0.009(2) 0.003(2) -0.007(2) C21 0.027(3) 0.015(3) 0.028(3) -0.009(2) 0.001(2) -0.009(2) C22 0.032(3) 0.016(3) 0.023(3) -0.003(2) 0.003(2) -0.010(2) C23 0.033(3) 0.023(3) 0.022(3) -0.011(2) 0.002(2) -0.006(2) C24 0.042(4) 0.013(3) 0.028(3) -0.008(2) 0.006(3) -0.013(2) C25 0.033(3) 0.020(3) 0.025(3) -0.007(2) 0.006(2) -0.013(2) C26 0.034(3) 0.021(3) 0.025(3) -0.011(2) 0.006(2) -0.013(2) C27 0.046(4) 0.022(3) 0.024(3) -0.010(2) 0.003(3) -0.010(3) C28 0.078(5) 0.030(3) 0.034(4) -0.017(3) 0.001(3) -0.021(4) C29 0.114(7) 0.028(4) 0.025(4) -0.009(3) -0.006(4) -0.011(4) C30 0.063(5) 0.105(7) 0.052(5) -0.050(5) 0.026(4) -0.042(5) C31 0.044(4) 0.019(3) 0.025(3) -0.005(2) 0.009(3) -0.011(3) C32 0.080(6) 0.021(3) 0.036(4) -0.001(3) 0.017(4) -0.010(3) C33 0.086(6) 0.034(4) 0.030(4) 0.001(3) -0.009(4) -0.017(4) C34 0.060(5) 0.047(4) 0.047(5) 0.014(4) 0.016(4) -0.026(4) C35 0.027(3) 0.028(3) 0.029(3) -0.014(2) 0.008(2) -0.014(3) C36 0.025(3) 0.074(5) 0.060(5) -0.049(4) 0.010(3) -0.018(4) C37 0.032(4) 0.106(7) 0.085(6) -0.074(6) 0.006(4) -0.020(4) C38 0.029(4) 0.086(6) 0.065(5) -0.051(5) 0.008(3) -0.022(4) C39 0.029(3) 0.035(3) 0.036(4) -0.014(3) 0.011(3) -0.015(3) C40 0.039(4) 0.025(3) 0.024(3) -0.010(2) 0.006(3) -0.014(3) C41 0.067(5) 0.101(5) 0.079(5) -0.057(4) -0.001(4) -0.024(4) C42 0.099(6) 0.077(5) 0.086(5) -0.050(4) -0.025(4) -0.027(4) C43 0.080(5) 0.117(6) 0.099(6) -0.058(5) -0.022(5) -0.032(5) C44 0.089(6) 0.103(6) 0.070(5) -0.041(5) -0.002(4) -0.023(5) C45 0.030(3) 0.032(3) 0.047(4) -0.016(3) 0.007(3) -0.010(3) C46 0.043(4) 0.074(5) 0.073(5) -0.040(4) 0.007(4) -0.005(4) C47 0.072(5) 0.065(5) 0.056(5) -0.016(4) 0.023(4) 0.011(4) C48 0.051(5) 0.046(4) 0.094(6) -0.027(4) 0.014(4) -0.018(4) C49 0.027(3) 0.017(3) 0.023(3) -0.002(2) -0.001(2) -0.011(2) C50 0.035(3) 0.016(3) 0.024(3) -0.006(2) -0.001(2) -0.008(2) C51 0.039(4) 0.023(3) 0.021(3) -0.002(2) 0.000(2) -0.015(3) C52 0.037(3) 0.013(2) 0.023(3) 0.000(2) -0.002(2) -0.009(2) C53 0.031(3) 0.017(3) 0.032(3) -0.007(2) 0.002(2) -0.010(2) C54 0.034(3) 0.021(3) 0.019(3) -0.004(2) 0.005(2) -0.015(2) C55 0.054(4) 0.022(3) 0.019(3) -0.002(2) 0.003(3) -0.017(3) C56 0.085(6) 0.032(4) 0.030(4) -0.007(3) 0.016(4) -0.017(4) C57 0.069(5) 0.040(4) 0.021(3) -0.001(3) -0.005(3) -0.023(4) C58 0.067(5) 0.042(4) 0.030(4) -0.008(3) 0.015(3) -0.033(4) C59 0.048(4) 0.022(3) 0.033(3) -0.011(3) 0.008(3) -0.016(3) C60 0.073(5) 0.018(3) 0.044(4) -0.012(3) 0.009(4) -0.015(3) C61 0.051(5) 0.040(4) 0.055(5) -0.027(3) 0.012(4) -0.012(3) C62 0.066(5) 0.029(3) 0.033(4) -0.018(3) 0.009(3) -0.019(3) C63 0.035(3) 0.017(3) 0.034(3) -0.008(2) -0.004(3) -0.009(3) C64 0.028(3) 0.016(3) 0.023(3) -0.004(2) -0.001(2) -0.007(2) C65 0.046(4) 0.017(3) 0.056(4) -0.009(3) -0.023(3) -0.002(3) C66 0.046(4) 0.023(3) 0.052(4) -0.004(3) -0.016(3) -0.004(3) C67 0.066(5) 0.024(3) 0.073(5) -0.002(3) -0.029(4) -0.007(3) C68 0.085(5) 0.028(3) 0.109(6) -0.004(4) -0.063(5) 0.003(4) C69 0.092(6) 0.040(4) 0.130(6) -0.010(4) -0.077(5) -0.005(4) C70 0.076(5) 0.028(3) 0.113(6) -0.011(4) -0.057(4) -0.001(3) C71 0.034(3) 0.016(2) 0.023(3) -0.005(2) -0.001(2) -0.010(2) C72 0.039(3) 0.023(3) 0.029(3) -0.008(2) -0.004(2) -0.011(2) C73 0.048(3) 0.032(3) 0.030(3) -0.009(2) -0.005(3) -0.021(3) C74 0.054(3) 0.023(3) 0.023(3) -0.006(2) 0.005(2) -0.019(2) C75 0.044(3) 0.019(2) 0.026(3) -0.005(2) 0.013(2) -0.014(2) C76 0.033(3) 0.020(2) 0.018(3) -0.005(2) 0.005(2) -0.010(2) C77 0.077(6) 0.085(7) 0.052(5) -0.014(5) -0.002(4) -0.042(6) C78 0.065(6) 0.070(6) 0.063(6) -0.037(5) 0.005(4) -0.012(5) C79 0.069(6) 0.078(7) 0.087(7) -0.050(6) -0.004(5) -0.016(5) C80 0.084(8) 0.113(9) 0.105(9) -0.062(8) 0.002(6) -0.046(7) C81 0.094(10) 0.183(17) 0.127(13) -0.066(12) 0.009(9) -0.045(11) C82 0.083(9) 0.126(12) 0.166(15) -0.078(11) -0.037(9) 0.011(8) _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 Ni1 N1 1.883(4) . ? Ni1 N3 1.898(4) . ? Ni1 N2 1.906(4) . ? Ni1 N4 1.919(4) . ? Cl1 C77 1.777(9) . ? Cl2 C78 1.771(9) . ? Cl3 C79 1.825(11) . ? Cl4 C80 1.817(13) . ? Cl5 C81 1.806(9) . ? Cl6 C82 1.840(9) . ? O1 C3 1.213(7) . ? N1 C4 1.378(7) . ? N1 C1 1.385(7) . ? N2 C6 1.364(7) . ? N2 C9 1.392(7) . ? N3 C11 1.372(7) . ? N3 C14 1.385(7) . ? N4 C19 1.359(7) . ? N4 C16 1.416(7) . ? N5 C64 1.325(7) . ? N5 C63 1.373(7) . ? C1 C20 1.392(7) . ? C1 C2 1.414(8) . ? C2 C63 1.392(8) . ? C2 C3 1.467(8) . ? C3 C4 1.500(8) . ? C4 C5 1.375(8) . ? C5 C6 1.402(9) . ? C5 C21 1.505(7) . ? C6 C7 1.433(8) . ? C7 C8 1.340(9) . ? C7 H2 0.9300 . ? C8 C9 1.434(8) . ? C8 H3 0.9300 . ? C9 C10 1.404(8) . ? C10 C11 1.401(8) . ? C10 C35 1.482(8) . ? C11 C12 1.426(8) . ? C12 C13 1.351(8) . ? C12 H4 0.9300 . ? C13 C14 1.423(8) . ? C13 H5 0.9300 . ? C14 C15 1.407(8) . ? C15 C16 1.364(8) . ? C15 C49 1.507(7) . ? C16 C17 1.421(8) . ? C17 C18 1.341(8) . ? C17 H6 0.9300 . ? C18 C19 1.438(7) . ? C18 H7 0.9300 . ? C19 C20 1.428(7) . ? C20 C64 1.436(8) . ? C21 C22 1.383(8) . ? C21 C26 1.390(8) . ? C22 C23 1.397(8) . ? C22 H8 0.9300 . ? C23 C24 1.391(8) . ? C23 C27 1.536(8) . ? C24 C25 1.396(8) . ? C24 H9 0.9300 . ? C25 C26 1.390(8) . ? C25 C31 1.536(8) . ? C26 H10 0.9300 . ? C27 C29 1.518(9) . ? C27 C30 1.534(10) . ? C27 C28 1.535(9) . ? C28 H27 0.9600 . ? C28 H28 0.9600 . ? C28 H29 0.9600 . ? C29 H30 0.9600 . ? C29 H31 0.9600 . ? C29 H32 0.9600 . ? C30 H33 0.9600 . ? C30 H34 0.9600 . ? C30 H35 0.9600 . ? C31 C32 1.524(8) . ? C31 C34 1.526(10) . ? C31 C33 1.535(10) . ? C32 H36 0.9600 . ? C32 H37 0.9600 . ? C32 H38 0.9600 . ? C33 H39 0.9600 . ? C33 H40 0.9600 . ? C33 H41 0.9600 . ? C34 H42 0.9600 . ? C34 H43 0.9600 . ? C34 H44 0.9600 . ? C35 C40 1.382(8) . ? C35 C36 1.391(9) . ? C36 C37 1.383(10) . ? C36 H11 0.9300 . ? C37 C38 1.400(10) . ? C37 C41 1.562(11) . ? C38 C39 1.388(10) . ? C38 H12 0.9300 . ? C39 C40 1.391(9) . ? C39 C45 1.530(8) . ? C40 H13 0.9300 . ? C41 C43 1.490(8) . ? C41 C42 1.503(8) . ? C41 C44 1.520(9) . ? C42 H45 0.9600 . ? C42 H46 0.9600 . ? C42 H47 0.9600 . ? C43 H48 0.9600 . ? C43 H49 0.9600 . ? C43 H50 0.9600 . ? C44 H51 0.9600 . ? C44 H52 0.9600 . ? C44 H53 0.9600 . ? C45 C47 1.476(11) . ? C45 C46 1.531(11) . ? C45 C48 1.541(10) . ? C46 H54 0.9600 . ? C46 H55 0.9600 . ? C46 H56 0.9600 . ? C47 H57 0.9600 . ? C47 H58 0.9600 . ? C47 H59 0.9600 . ? C48 H60 0.9600 . ? C48 H61 0.9600 . ? C48 H62 0.9600 . ? C49 C54 1.386(8) . ? C49 C50 1.394(8) . ? C50 C51 1.395(8) . ? C50 H14 0.9300 . ? C51 C52 1.396(8) . ? C51 C55 1.528(8) . ? C52 C53 1.390(8) . ? C52 H15 0.9300 . ? C53 C54 1.398(8) . ? C53 C59 1.543(8) . ? C54 H16 0.9300 . ? C55 C57 1.525(10) . ? C55 C58 1.528(9) . ? C55 C56 1.533(9) . ? C56 H63 0.9600 . ? C56 H64 0.9600 . ? C56 H65 0.9600 . ? C57 H66 0.9600 . ? C57 H67 0.9600 . ? C57 H68 0.9600 . ? C58 H69 0.9600 . ? C58 H70 0.9600 . ? C58 H71 0.9600 . ? C59 C62 1.526(10) . ? C59 C60 1.530(8) . ? C59 C61 1.542(10) . ? C60 H72 0.9600 . ? C60 H73 0.9600 . ? C60 H74 0.9600 . ? C61 H75 0.9600 . ? C61 H76 0.9600 . ? C61 H77 0.9600 . ? C62 H78 0.9600 . ? C62 H79 0.9600 . ? C62 H80 0.9600 . ? C63 C65 1.471(8) . ? C64 C71 1.481(7) . ? C65 C66 1.381(9) . ? C65 C70 1.385(11) . ? C66 C67 1.401(9) . ? C66 H17 0.9300 . ? C67 C68 1.363(12) . ? C67 H18 0.9300 . ? C68 C69 1.399(13) . ? C68 H19 0.9300 . ? C69 C70 1.385(11) . ? C69 H20 0.9300 . ? C70 H21 0.9300 . ? C71 C72 1.387(9) . ? C71 C76 1.403(8) . ? C72 C73 1.388(8) . ? C72 H22 0.9300 . ? C73 C74 1.383(9) . ? C73 H23 0.9300 . ? C74 C75 1.388(9) . ? C74 H24 0.9300 . ? C75 C76 1.390(8) . ? C75 H25 0.9300 . ? C76 H26 0.9300 . ? C77 C78 1.497(13) . ? C77 H81 0.9700 . ? C77 H82 0.9700 . ? C78 H83 0.9700 . ? C78 H84 0.9700 . ? C79 C80 1.444(14) . ? C79 H85 0.9700 . ? C79 H86 0.9700 . ? C80 H87 0.9700 . ? C80 H88 0.9700 . ? C81 C82 1.455(9) . ? C81 H89 0.9700 . ? C81 H90 0.9700 . ? C82 H91 0.9700 . ? C82 H92 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N3 177.96(19) . . ? N1 Ni1 N2 89.33(19) . . ? N3 Ni1 N2 90.09(19) . . ? N1 Ni1 N4 89.79(19) . . ? N3 Ni1 N4 90.85(19) . . ? N2 Ni1 N4 178.17(19) . . ? C4 N1 C1 106.3(4) . . ? C4 N1 Ni1 128.1(4) . . ? C1 N1 Ni1 125.6(3) . . ? C6 N2 C9 105.0(4) . . ? C6 N2 Ni1 127.8(4) . . ? C9 N2 Ni1 126.9(3) . . ? C11 N3 C14 105.1(4) . . ? C11 N3 Ni1 128.2(4) . . ? C14 N3 Ni1 126.7(4) . . ? C19 N4 C16 105.5(4) . . ? C19 N4 Ni1 128.9(3) . . ? C16 N4 Ni1 125.5(4) . . ? C64 N5 C63 120.1(5) . . ? N1 C1 C20 127.0(5) . . ? N1 C1 C2 113.0(5) . . ? C20 C1 C2 119.8(5) . . ? C63 C2 C1 120.3(5) . . ? C63 C2 C3 133.8(5) . . ? C1 C2 C3 105.4(5) . . ? O1 C3 C2 129.8(5) . . ? O1 C3 C4 126.9(5) . . ? C2 C3 C4 103.2(4) . . ? C5 C4 N1 124.5(5) . . ? C5 C4 C3 124.0(5) . . ? N1 C4 C3 110.3(5) . . ? C4 C5 C6 119.8(5) . . ? C4 C5 C21 122.1(5) . . ? C6 C5 C21 117.6(5) . . ? N2 C6 C5 125.1(5) . . ? N2 C6 C7 110.4(5) . . ? C5 C6 C7 124.1(5) . . ? C8 C7 C6 107.6(5) . . ? C8 C7 H2 126.2 . . ? C6 C7 H2 126.2 . . ? C7 C8 C9 106.7(5) . . ? C7 C8 H3 126.6 . . ? C9 C8 H3 126.6 . . ? N2 C9 C10 123.8(5) . . ? N2 C9 C8 110.0(5) . . ? C10 C9 C8 125.7(5) . . ? C11 C10 C9 121.1(5) . . ? C11 C10 C35 117.8(5) . . ? C9 C10 C35 120.6(5) . . ? N3 C11 C10 124.7(5) . . ? N3 C11 C12 110.5(5) . . ? C10 C11 C12 124.4(5) . . ? C13 C12 C11 107.1(5) . . ? C13 C12 H4 126.5 . . ? C11 C12 H4 126.5 . . ? C12 C13 C14 107.2(5) . . ? C12 C13 H5 126.4 . . ? C14 C13 H5 126.4 . . ? N3 C14 C15 124.3(5) . . ? N3 C14 C13 110.1(5) . . ? C15 C14 C13 124.8(5) . . ? C16 C15 C14 122.8(5) . . ? C16 C15 C49 120.7(5) . . ? C14 C15 C49 115.9(5) . . ? C15 C16 N4 124.4(5) . . ? C15 C16 C17 126.3(5) . . ? N4 C16 C17 108.8(5) . . ? C18 C17 C16 108.1(5) . . ? C18 C17 H6 126.0 . . ? C16 C17 H6 126.0 . . ? C17 C18 C19 107.3(5) . . ? C17 C18 H7 126.4 . . ? C19 C18 H7 126.4 . . ? N4 C19 C20 122.8(5) . . ? N4 C19 C18 110.3(5) . . ? C20 C19 C18 126.1(5) . . ? C1 C20 C19 118.6(5) . . ? C1 C20 C64 115.3(5) . . ? C19 C20 C64 125.4(5) . . ? C22 C21 C26 119.9(5) . . ? C22 C21 C5 119.0(5) . . ? C26 C21 C5 121.0(5) . . ? C21 C22 C23 121.2(5) . . ? C21 C22 H8 119.4 . . ? C23 C22 H8 119.4 . . ? C24 C23 C22 117.6(5) . . ? C24 C23 C27 120.5(5) . . ? C22 C23 C27 121.8(5) . . ? C23 C24 C25 122.5(5) . . ? C23 C24 H9 118.8 . . ? C25 C24 H9 118.8 . . ? C26 C25 C24 118.1(5) . . ? C26 C25 C31 120.3(5) . . ? C24 C25 C31 121.6(5) . . ? C25 C26 C21 120.6(5) . . ? C25 C26 H10 119.7 . . ? C21 C26 H10 119.7 . . ? C29 C27 C30 108.9(7) . . ? C29 C27 C28 107.2(6) . . ? C30 C27 C28 109.1(6) . . ? C29 C27 C23 112.0(5) . . ? C30 C27 C23 108.0(5) . . ? C28 C27 C23 111.6(5) . . ? C27 C28 H27 109.5 . . ? C27 C28 H28 109.5 . . ? H27 C28 H28 109.5 . . ? C27 C28 H29 109.5 . . ? H27 C28 H29 109.5 . . ? H28 C28 H29 109.5 . . ? C27 C29 H30 109.5 . . ? C27 C29 H31 109.5 . . ? H30 C29 H31 109.5 . . ? C27 C29 H32 109.5 . . ? H30 C29 H32 109.5 . . ? H31 C29 H32 109.5 . . ? C27 C30 H33 109.5 . . ? C27 C30 H34 109.5 . . ? H33 C30 H34 109.5 . . ? C27 C30 H35 109.5 . . ? H33 C30 H35 109.5 . . ? H34 C30 H35 109.5 . . ? C32 C31 C34 110.2(6) . . ? C32 C31 C33 106.8(6) . . ? C34 C31 C33 109.7(6) . . ? C32 C31 C25 111.6(5) . . ? C34 C31 C25 107.9(5) . . ? C33 C31 C25 110.6(5) . . ? C31 C32 H36 109.5 . . ? C31 C32 H37 109.5 . . ? H36 C32 H37 109.5 . . ? C31 C32 H38 109.5 . . ? H36 C32 H38 109.5 . . ? H37 C32 H38 109.5 . . ? C31 C33 H39 109.5 . . ? C31 C33 H40 109.5 . . ? H39 C33 H40 109.5 . . ? C31 C33 H41 109.5 . . ? H39 C33 H41 109.5 . . ? H40 C33 H41 109.5 . . ? C31 C34 H42 109.5 . . ? C31 C34 H43 109.5 . . ? H42 C34 H43 109.5 . . ? C31 C34 H44 109.5 . . ? H42 C34 H44 109.5 . . ? H43 C34 H44 109.5 . . ? C40 C35 C36 119.1(6) . . ? C40 C35 C10 120.0(5) . . ? C36 C35 C10 120.8(5) . . ? C37 C36 C35 121.2(6) . . ? C37 C36 H11 119.4 . . ? C35 C36 H11 119.4 . . ? C36 C37 C38 118.0(7) . . ? C36 C37 C41 119.5(7) . . ? C38 C37 C41 122.2(7) . . ? C39 C38 C37 122.4(7) . . ? C39 C38 H12 118.8 . . ? C37 C38 H12 118.8 . . ? C38 C39 C40 117.4(6) . . ? C38 C39 C45 122.5(6) . . ? C40 C39 C45 120.1(6) . . ? C35 C40 C39 121.9(6) . . ? C35 C40 H13 119.1 . . ? C39 C40 H13 119.1 . . ? C43 C41 C42 113.4(9) . . ? C43 C41 C44 106.2(9) . . ? C42 C41 C44 106.6(8) . . ? C43 C41 C37 112.8(7) . . ? C42 C41 C37 107.1(7) . . ? C44 C41 C37 110.7(8) . . ? C41 C42 H45 109.5 . . ? C41 C42 H46 109.5 . . ? H45 C42 H46 109.5 . . ? C41 C42 H47 109.5 . . ? H45 C42 H47 109.5 . . ? H46 C42 H47 109.5 . . ? C41 C43 H48 109.5 . . ? C41 C43 H49 109.5 . . ? H48 C43 H49 109.5 . . ? C41 C43 H50 109.5 . . ? H48 C43 H50 109.5 . . ? H49 C43 H50 109.5 . . ? C41 C44 H51 109.5 . . ? C41 C44 H52 109.5 . . ? H51 C44 H52 109.5 . . ? C41 C44 H53 109.5 . . ? H51 C44 H53 109.5 . . ? H52 C44 H53 109.5 . . ? C47 C45 C39 110.4(6) . . ? C47 C45 C46 108.9(7) . . ? C39 C45 C46 112.0(6) . . ? C47 C45 C48 111.4(7) . . ? C39 C45 C48 108.8(6) . . ? C46 C45 C48 105.3(6) . . ? C45 C46 H54 109.5 . . ? C45 C46 H55 109.5 . . ? H54 C46 H55 109.5 . . ? C45 C46 H56 109.5 . . ? H54 C46 H56 109.5 . . ? H55 C46 H56 109.5 . . ? C45 C47 H57 109.5 . . ? C45 C47 H58 109.5 . . ? H57 C47 H58 109.5 . . ? C45 C47 H59 109.5 . . ? H57 C47 H59 109.5 . . ? H58 C47 H59 109.5 . . ? C45 C48 H60 109.5 . . ? C45 C48 H61 109.5 . . ? H60 C48 H61 109.5 . . ? C45 C48 H62 109.5 . . ? H60 C48 H62 109.5 . . ? H61 C48 H62 109.5 . . ? C54 C49 C50 120.1(5) . . ? C54 C49 C15 120.2(5) . . ? C50 C49 C15 119.5(5) . . ? C49 C50 C51 120.7(5) . . ? C49 C50 H14 119.6 . . ? C51 C50 H14 119.6 . . ? C50 C51 C52 117.4(5) . . ? C50 C51 C55 121.8(5) . . ? C52 C51 C55 120.7(5) . . ? C53 C52 C51 123.4(5) . . ? C53 C52 H15 118.3 . . ? C51 C52 H15 118.3 . . ? C52 C53 C54 117.4(5) . . ? C52 C53 C59 123.5(5) . . ? C54 C53 C59 119.0(5) . . ? C49 C54 C53 120.9(5) . . ? C49 C54 H16 119.5 . . ? C53 C54 H16 119.5 . . ? C57 C55 C51 107.8(5) . . ? C57 C55 C58 109.5(5) . . ? C51 C55 C58 110.9(5) . . ? C57 C55 C56 107.8(6) . . ? C51 C55 C56 112.3(5) . . ? C58 C55 C56 108.5(6) . . ? C55 C56 H63 109.5 . . ? C55 C56 H64 109.5 . . ? H63 C56 H64 109.5 . . ? C55 C56 H65 109.5 . . ? H63 C56 H65 109.5 . . ? H64 C56 H65 109.5 . . ? C55 C57 H66 109.5 . . ? C55 C57 H67 109.5 . . ? H66 C57 H67 109.5 . . ? C55 C57 H68 109.5 . . ? H66 C57 H68 109.5 . . ? H67 C57 H68 109.5 . . ? C55 C58 H69 109.5 . . ? C55 C58 H70 109.5 . . ? H69 C58 H70 109.5 . . ? C55 C58 H71 109.5 . . ? H69 C58 H71 109.5 . . ? H70 C58 H71 109.5 . . ? C62 C59 C60 108.8(6) . . ? C62 C59 C61 108.3(6) . . ? C60 C59 C61 109.5(6) . . ? C62 C59 C53 109.9(5) . . ? C60 C59 C53 112.0(5) . . ? C61 C59 C53 108.3(5) . . ? C59 C60 H72 109.5 . . ? C59 C60 H73 109.5 . . ? H72 C60 H73 109.5 . . ? C59 C60 H74 109.5 . . ? H72 C60 H74 109.5 . . ? H73 C60 H74 109.5 . . ? C59 C61 H75 109.5 . . ? C59 C61 H76 109.5 . . ? H75 C61 H76 109.5 . . ? C59 C61 H77 109.5 . . ? H75 C61 H77 109.5 . . ? H76 C61 H77 109.5 . . ? C59 C62 H78 109.5 . . ? C59 C62 H79 109.5 . . ? H78 C62 H79 109.5 . . ? C59 C62 H80 109.5 . . ? H78 C62 H80 109.5 . . ? H79 C62 H80 109.5 . . ? N5 C63 C2 119.4(5) . . ? N5 C63 C65 115.1(5) . . ? C2 C63 C65 125.3(5) . . ? N5 C64 C20 123.8(5) . . ? N5 C64 C71 113.5(5) . . ? C20 C64 C71 122.6(5) . . ? C66 C65 C70 118.7(6) . . ? C66 C65 C63 122.2(6) . . ? C70 C65 C63 119.0(6) . . ? C65 C66 C67 120.8(7) . . ? C65 C66 H17 119.6 . . ? C67 C66 H17 119.6 . . ? C68 C67 C66 119.7(7) . . ? C68 C67 H18 120.1 . . ? C66 C67 H18 120.1 . . ? C67 C68 C69 120.4(7) . . ? C67 C68 H19 119.8 . . ? C69 C68 H19 119.8 . . ? C70 C69 C68 119.1(9) . . ? C70 C69 H20 120.4 . . ? C68 C69 H20 120.4 . . ? C65 C70 C69 121.2(8) . . ? C65 C70 H21 119.4 . . ? C69 C70 H21 119.4 . . ? C72 C71 C76 119.4(5) . . ? C72 C71 C64 119.5(5) . . ? C76 C71 C64 120.9(5) . . ? C71 C72 C73 120.5(6) . . ? C71 C72 H22 119.7 . . ? C73 C72 H22 119.7 . . ? C74 C73 C72 119.7(6) . . ? C74 C73 H23 120.2 . . ? C72 C73 H23 120.2 . . ? C73 C74 C75 120.8(6) . . ? C73 C74 H24 119.6 . . ? C75 C74 H24 119.6 . . ? C74 C75 C76 119.6(6) . . ? C74 C75 H25 120.2 . . ? C76 C75 H25 120.2 . . ? C75 C76 C71 120.0(6) . . ? C75 C76 H26 120.0 . . ? C71 C76 H26 120.0 . . ? C78 C77 Cl1 109.0(7) . . ? C78 C77 H81 109.9 . . ? Cl1 C77 H81 109.9 . . ? C78 C77 H82 109.9 . . ? Cl1 C77 H82 109.9 . . ? H81 C77 H82 108.3 . . ? C77 C78 Cl2 109.8(6) . . ? C77 C78 H83 109.7 . . ? Cl2 C78 H83 109.7 . . ? C77 C78 H84 109.7 . . ? Cl2 C78 H84 109.7 . . ? H83 C78 H84 108.2 . . ? C80 C79 Cl3 107.3(8) . . ? C80 C79 H85 110.3 . . ? Cl3 C79 H85 110.3 . . ? C80 C79 H86 110.3 . . ? Cl3 C79 H86 110.3 . . ? H85 C79 H86 108.5 . . ? C79 C80 Cl4 107.7(8) . . ? C79 C80 H87 110.2 . . ? Cl4 C80 H87 110.2 . . ? C79 C80 H88 110.2 . . ? Cl4 C80 H88 110.2 . . ? H87 C80 H88 108.5 . . ? C82 C81 Cl5 103.9(8) . . ? C82 C81 H89 111.0 . . ? Cl5 C81 H89 111.0 . . ? C82 C81 H90 111.0 . . ? Cl5 C81 H90 111.0 . . ? H89 C81 H90 109.0 . . ? C81 C82 Cl6 101.4(7) . . ? C81 C82 H91 111.5 . . ? Cl6 C82 H91 111.5 . . ? C81 C82 H92 111.5 . . ? Cl6 C82 H92 111.5 . . ? H91 C82 H92 109.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ni1 N1 C4 -50(6) . . . . ? N2 Ni1 N1 C4 23.4(5) . . . . ? N4 Ni1 N1 C4 -158.2(5) . . . . ? N3 Ni1 N1 C1 131(5) . . . . ? N2 Ni1 N1 C1 -155.4(4) . . . . ? N4 Ni1 N1 C1 23.0(4) . . . . ? N1 Ni1 N2 C6 -14.5(5) . . . . ? N3 Ni1 N2 C6 163.5(5) . . . . ? N4 Ni1 N2 C6 -76(6) . . . . ? N1 Ni1 N2 C9 157.8(4) . . . . ? N3 Ni1 N2 C9 -24.2(4) . . . . ? N4 Ni1 N2 C9 97(6) . . . . ? N1 Ni1 N3 C11 91(6) . . . . ? N2 Ni1 N3 C11 18.1(4) . . . . ? N4 Ni1 N3 C11 -160.3(4) . . . . ? N1 Ni1 N3 C14 -85(6) . . . . ? N2 Ni1 N3 C14 -158.5(4) . . . . ? N4 Ni1 N3 C14 23.1(4) . . . . ? N1 Ni1 N4 C19 -21.7(5) . . . . ? N3 Ni1 N4 C19 160.2(5) . . . . ? N2 Ni1 N4 C19 39(6) . . . . ? N1 Ni1 N4 C16 155.1(4) . . . . ? N3 Ni1 N4 C16 -23.0(4) . . . . ? N2 Ni1 N4 C16 -144(6) . . . . ? C4 N1 C1 C20 172.2(5) . . . . ? Ni1 N1 C1 C20 -8.8(8) . . . . ? C4 N1 C1 C2 -3.2(6) . . . . ? Ni1 N1 C1 C2 175.8(4) . . . . ? N1 C1 C2 C63 -176.6(5) . . . . ? C20 C1 C2 C63 7.7(9) . . . . ? N1 C1 C2 C3 10.8(6) . . . . ? C20 C1 C2 C3 -165.0(5) . . . . ? C63 C2 C3 O1 -7.0(12) . . . . ? C1 C2 C3 O1 164.3(6) . . . . ? C63 C2 C3 C4 175.8(7) . . . . ? C1 C2 C3 C4 -13.0(6) . . . . ? C1 N1 C4 C5 162.3(5) . . . . ? Ni1 N1 C4 C5 -16.7(8) . . . . ? C1 N1 C4 C3 -5.7(6) . . . . ? Ni1 N1 C4 C3 175.3(4) . . . . ? O1 C3 C4 C5 26.4(10) . . . . ? C2 C3 C4 C5 -156.2(6) . . . . ? O1 C3 C4 N1 -165.5(6) . . . . ? C2 C3 C4 N1 11.9(6) . . . . ? N1 C4 C5 C6 -7.3(9) . . . . ? C3 C4 C5 C6 159.1(5) . . . . ? N1 C4 C5 C21 -179.5(5) . . . . ? C3 C4 C5 C21 -13.1(9) . . . . ? C9 N2 C6 C5 -175.4(5) . . . . ? Ni1 N2 C6 C5 -1.7(8) . . . . ? C9 N2 C6 C7 -1.4(6) . . . . ? Ni1 N2 C6 C7 172.2(4) . . . . ? C4 C5 C6 N2 16.5(9) . . . . ? C21 C5 C6 N2 -171.0(5) . . . . ? C4 C5 C6 C7 -156.7(5) . . . . ? C21 C5 C6 C7 15.9(8) . . . . ? N2 C6 C7 C8 -1.4(7) . . . . ? C5 C6 C7 C8 172.6(5) . . . . ? C6 C7 C8 C9 3.6(7) . . . . ? C6 N2 C9 C10 -169.0(5) . . . . ? Ni1 N2 C9 C10 17.2(8) . . . . ? C6 N2 C9 C8 3.7(6) . . . . ? Ni1 N2 C9 C8 -170.1(4) . . . . ? C7 C8 C9 N2 -4.6(7) . . . . ? C7 C8 C9 C10 167.9(5) . . . . ? N2 C9 C10 C11 4.9(8) . . . . ? C8 C9 C10 C11 -166.6(6) . . . . ? N2 C9 C10 C35 177.0(5) . . . . ? C8 C9 C10 C35 5.5(9) . . . . ? C14 N3 C11 C10 173.0(5) . . . . ? Ni1 N3 C11 C10 -4.1(8) . . . . ? C14 N3 C11 C12 0.0(6) . . . . ? Ni1 N3 C11 C12 -177.2(4) . . . . ? C9 C10 C11 N3 -11.7(8) . . . . ? C35 C10 C11 N3 176.0(5) . . . . ? C9 C10 C11 C12 160.4(5) . . . . ? C35 C10 C11 C12 -11.9(8) . . . . ? N3 C11 C12 C13 1.0(6) . . . . ? C10 C11 C12 C13 -172.1(5) . . . . ? C11 C12 C13 C14 -1.5(6) . . . . ? C11 N3 C14 C15 169.5(5) . . . . ? Ni1 N3 C14 C15 -13.3(8) . . . . ? C11 N3 C14 C13 -0.9(6) . . . . ? Ni1 N3 C14 C13 176.3(4) . . . . ? C12 C13 C14 N3 1.5(6) . . . . ? C12 C13 C14 C15 -168.8(5) . . . . ? N3 C14 C15 C16 -5.7(8) . . . . ? C13 C14 C15 C16 163.3(5) . . . . ? N3 C14 C15 C49 -177.4(5) . . . . ? C13 C14 C15 C49 -8.4(8) . . . . ? C14 C15 C16 N4 5.4(8) . . . . ? C49 C15 C16 N4 176.7(5) . . . . ? C14 C15 C16 C17 -166.0(5) . . . . ? C49 C15 C16 C17 5.3(9) . . . . ? C19 N4 C16 C15 -169.1(5) . . . . ? Ni1 N4 C16 C15 13.4(7) . . . . ? C19 N4 C16 C17 3.5(6) . . . . ? Ni1 N4 C16 C17 -173.9(4) . . . . ? C15 C16 C17 C18 169.0(5) . . . . ? N4 C16 C17 C18 -3.4(6) . . . . ? C16 C17 C18 C19 1.9(6) . . . . ? C16 N4 C19 C20 -172.5(5) . . . . ? Ni1 N4 C19 C20 4.8(7) . . . . ? C16 N4 C19 C18 -2.4(6) . . . . ? Ni1 N4 C19 C18 174.9(4) . . . . ? C17 C18 C19 N4 0.3(6) . . . . ? C17 C18 C19 C20 170.0(5) . . . . ? N1 C1 C20 C19 -16.7(8) . . . . ? C2 C1 C20 C19 158.4(5) . . . . ? N1 C1 C20 C64 172.2(5) . . . . ? C2 C1 C20 C64 -12.7(8) . . . . ? N4 C19 C20 C1 18.5(8) . . . . ? C18 C19 C20 C1 -150.0(5) . . . . ? N4 C19 C20 C64 -171.4(5) . . . . ? C18 C19 C20 C64 20.1(9) . . . . ? C4 C5 C21 C22 -110.4(7) . . . . ? C6 C5 C21 C22 77.2(7) . . . . ? C4 C5 C21 C26 73.6(8) . . . . ? C6 C5 C21 C26 -98.8(7) . . . . ? C26 C21 C22 C23 -1.6(9) . . . . ? C5 C21 C22 C23 -177.6(6) . . . . ? C21 C22 C23 C24 -0.8(9) . . . . ? C21 C22 C23 C27 -178.3(6) . . . . ? C22 C23 C24 C25 2.0(10) . . . . ? C27 C23 C24 C25 179.5(6) . . . . ? C23 C24 C25 C26 -0.8(9) . . . . ? C23 C24 C25 C31 177.8(6) . . . . ? C24 C25 C26 C21 -1.8(9) . . . . ? C31 C25 C26 C21 179.7(6) . . . . ? C22 C21 C26 C25 2.9(9) . . . . ? C5 C21 C26 C25 178.8(6) . . . . ? C24 C23 C27 C29 154.0(7) . . . . ? C22 C23 C27 C29 -28.6(9) . . . . ? C24 C23 C27 C30 -86.1(8) . . . . ? C22 C23 C27 C30 91.3(8) . . . . ? C24 C23 C27 C28 33.9(8) . . . . ? C22 C23 C27 C28 -148.7(6) . . . . ? C26 C25 C31 C32 -162.1(6) . . . . ? C24 C25 C31 C32 19.4(9) . . . . ? C26 C25 C31 C34 76.6(8) . . . . ? C24 C25 C31 C34 -101.9(7) . . . . ? C26 C25 C31 C33 -43.4(8) . . . . ? C24 C25 C31 C33 138.1(6) . . . . ? C11 C10 C35 C40 -65.3(7) . . . . ? C9 C10 C35 C40 122.4(6) . . . . ? C11 C10 C35 C36 111.0(7) . . . . ? C9 C10 C35 C36 -61.3(8) . . . . ? C40 C35 C36 C37 -0.2(12) . . . . ? C10 C35 C36 C37 -176.5(8) . . . . ? C35 C36 C37 C38 -0.7(15) . . . . ? C35 C36 C37 C41 172.3(8) . . . . ? C36 C37 C38 C39 1.4(15) . . . . ? C41 C37 C38 C39 -171.5(9) . . . . ? C37 C38 C39 C40 -1.1(13) . . . . ? C37 C38 C39 C45 176.7(8) . . . . ? C36 C35 C40 C39 0.4(9) . . . . ? C10 C35 C40 C39 176.8(6) . . . . ? C38 C39 C40 C35 0.2(10) . . . . ? C45 C39 C40 C35 -177.7(6) . . . . ? C36 C37 C41 C43 177.5(10) . . . . ? C38 C37 C41 C43 -9.7(15) . . . . ? C36 C37 C41 C42 52.1(13) . . . . ? C38 C37 C41 C42 -135.1(10) . . . . ? C36 C37 C41 C44 -63.7(12) . . . . ? C38 C37 C41 C44 109.1(11) . . . . ? C38 C39 C45 C47 117.4(9) . . . . ? C40 C39 C45 C47 -64.7(9) . . . . ? C38 C39 C45 C46 -4.1(10) . . . . ? C40 C39 C45 C46 173.7(6) . . . . ? C38 C39 C45 C48 -120.0(8) . . . . ? C40 C39 C45 C48 57.8(8) . . . . ? C16 C15 C49 C54 -76.3(7) . . . . ? C14 C15 C49 C54 95.6(7) . . . . ? C16 C15 C49 C50 108.3(6) . . . . ? C14 C15 C49 C50 -79.8(7) . . . . ? C54 C49 C50 C51 -1.0(9) . . . . ? C15 C49 C50 C51 174.4(6) . . . . ? C49 C50 C51 C52 0.1(9) . . . . ? C49 C50 C51 C55 -176.6(6) . . . . ? C50 C51 C52 C53 0.5(9) . . . . ? C55 C51 C52 C53 177.2(6) . . . . ? C51 C52 C53 C54 -0.2(9) . . . . ? C51 C52 C53 C59 -178.8(6) . . . . ? C50 C49 C54 C53 1.3(9) . . . . ? C15 C49 C54 C53 -174.0(5) . . . . ? C52 C53 C54 C49 -0.7(9) . . . . ? C59 C53 C54 C49 177.9(6) . . . . ? C50 C51 C55 C57 109.6(7) . . . . ? C52 C51 C55 C57 -67.0(7) . . . . ? C50 C51 C55 C58 -130.6(7) . . . . ? C52 C51 C55 C58 52.8(8) . . . . ? C50 C51 C55 C56 -9.1(9) . . . . ? C52 C51 C55 C56 174.4(7) . . . . ? C52 C53 C59 C62 -128.7(6) . . . . ? C54 C53 C59 C62 52.8(8) . . . . ? C52 C53 C59 C60 -7.6(9) . . . . ? C54 C53 C59 C60 173.8(6) . . . . ? C52 C53 C59 C61 113.2(7) . . . . ? C54 C53 C59 C61 -65.4(8) . . . . ? C64 N5 C63 C2 -6.0(9) . . . . ? C64 N5 C63 C65 178.8(6) . . . . ? C1 C2 C63 N5 2.1(9) . . . . ? C3 C2 C63 N5 172.3(6) . . . . ? C1 C2 C63 C65 176.7(6) . . . . ? C3 C2 C63 C65 -13.0(11) . . . . ? C63 N5 C64 C20 0.2(9) . . . . ? C63 N5 C64 C71 176.7(5) . . . . ? C1 C20 C64 N5 9.2(8) . . . . ? C19 C20 C64 N5 -161.2(6) . . . . ? C1 C20 C64 C71 -167.0(5) . . . . ? C19 C20 C64 C71 22.6(9) . . . . ? N5 C63 C65 C66 145.1(7) . . . . ? C2 C63 C65 C66 -29.8(11) . . . . ? N5 C63 C65 C70 -34.7(11) . . . . ? C2 C63 C65 C70 150.4(8) . . . . ? C70 C65 C66 C67 1.8(13) . . . . ? C63 C65 C66 C67 -178.0(7) . . . . ? C65 C66 C67 C68 -0.9(14) . . . . ? C66 C67 C68 C69 -1.2(17) . . . . ? C67 C68 C69 C70 2.4(19) . . . . ? C66 C65 C70 C69 -0.6(16) . . . . ? C63 C65 C70 C69 179.2(10) . . . . ? C68 C69 C70 C65 -1.5(19) . . . . ? N5 C64 C71 C72 38.7(8) . . . . ? C20 C64 C71 C72 -144.7(6) . . . . ? N5 C64 C71 C76 -136.5(6) . . . . ? C20 C64 C71 C76 40.0(8) . . . . ? C76 C71 C72 C73 -0.1(9) . . . . ? C64 C71 C72 C73 -175.4(5) . . . . ? C71 C72 C73 C74 -0.2(9) . . . . ? C72 C73 C74 C75 0.1(9) . . . . ? C73 C74 C75 C76 0.2(9) . . . . ? C74 C75 C76 C71 -0.5(8) . . . . ? C72 C71 C76 C75 0.5(8) . . . . ? C64 C71 C76 C75 175.7(5) . . . . ? Cl1 C77 C78 Cl2 172.8(5) . . . . ? Cl3 C79 C80 Cl4 179.5(5) . . . . ? Cl5 C81 C82 Cl6 -176.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.553 _refine_diff_density_min -1.430 _refine_diff_density_rms 0.134 # Attachment '3Zn.CIF' data_shelxl3 _database_code_depnum_ccdc_archive 'CCDC 707383' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H87 N5 O3 Zn' _chemical_formula_weight 1207.90 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.549(15) _cell_length_b 16.88(3) _cell_length_c 20.16(3) _cell_angle_alpha 87.34(6) _cell_angle_beta 85.64(6) _cell_angle_gamma 74.93(6) _cell_volume 3455(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 3901 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 26.3 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.406 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7374 _exptl_absorpt_correction_T_max 0.9606 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32995 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.49 _reflns_number_total 14994 _reflns_number_gt 11672 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8' _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^)+(0.1066P)^2^+4.7451P] 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 14994 _refine_ls_number_parameters 822 _refine_ls_number_restraints 1470 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.2001 _refine_ls_wR_factor_gt 0.1852 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.53397(3) 0.111331(19) 0.115990(16) 0.01927(11) Uani 1 1 d U . . O1 O 0.5366(2) 0.19687(15) -0.14884(11) 0.0322(5) Uani 1 1 d U . . O2 O 0.6831(2) 0.17047(14) 0.12843(13) 0.0309(5) Uani 1 1 d U . . H1 H 0.752(4) 0.145(3) 0.140(2) 0.032(11) Uiso 1 1 d . . . O3 O 0.9098(2) 0.09984(17) 0.18119(14) 0.0397(6) Uani 1 1 d U . . H2 H 0.9829 0.0818 0.1602 0.060 Uiso 1 1 calc R . . N1 N 0.5576(2) 0.11155(14) 0.01420(12) 0.0185(5) Uani 1 1 d U . . N2 N 0.3805(2) 0.21580(14) 0.10808(12) 0.0199(5) Uani 1 1 d U . . N3 N 0.4718(3) 0.09912(16) 0.21422(13) 0.0268(6) Uani 1 1 d U . . N4 N 0.6429(2) -0.00958(14) 0.11846(12) 0.0200(5) Uani 1 1 d U . . N5 N 0.8449(3) -0.03652(16) -0.10905(13) 0.0248(5) Uani 1 1 d U A . C1 C 0.6534(3) 0.05581(17) -0.02114(14) 0.0181(5) Uani 1 1 d U . . C2 C 0.6668(3) 0.07941(18) -0.08882(15) 0.0217(6) Uani 1 1 d U A . C3 C 0.5659(3) 0.15711(18) -0.09803(15) 0.0230(6) Uani 1 1 d U . . C4 C 0.5046(3) 0.17508(17) -0.02869(14) 0.0189(5) Uani 1 1 d U . . C5 C 0.4117(3) 0.24687(17) -0.01221(14) 0.0187(5) Uani 1 1 d U . . C6 C 0.3511(3) 0.26423(17) 0.05304(15) 0.0187(5) Uani 1 1 d U . . C7 C 0.2515(3) 0.33797(17) 0.06956(16) 0.0224(6) Uani 1 1 d U . . H3 H 0.2144 0.3817 0.0398 0.027 Uiso 1 1 calc R . . C8 C 0.2211(3) 0.33312(18) 0.13542(16) 0.0246(6) Uani 1 1 d U . . H4 H 0.1573 0.3725 0.1608 0.030 Uiso 1 1 calc R . . C9 C 0.3030(3) 0.25726(17) 0.16011(15) 0.0218(6) Uani 1 1 d U . . C10 C 0.3069(3) 0.23190(19) 0.22613(16) 0.0274(7) Uani 1 1 d U . . C11 C 0.3887(4) 0.1592(2) 0.25136(16) 0.0309(7) Uani 1 1 d U . . C12 C 0.3900(4) 0.1340(2) 0.31963(18) 0.0395(9) Uani 1 1 d U . . H5 H 0.3431 0.1652 0.3559 0.047 Uiso 1 1 calc R . . C13 C 0.4707(4) 0.0571(2) 0.32326(17) 0.0393(9) Uani 1 1 d U . . H6 H 0.4901 0.0240 0.3624 0.047 Uiso 1 1 calc R . . C14 C 0.5207(3) 0.0355(2) 0.25703(16) 0.0295(7) Uani 1 1 d U . . C15 C 0.6013(3) -0.04162(19) 0.23783(15) 0.0269(6) Uani 1 1 d U . . C16 C 0.6522(3) -0.06259(18) 0.17402(15) 0.0228(6) Uani 1 1 d U . . C17 C 0.7331(3) -0.14178(19) 0.15589(16) 0.0266(6) Uani 1 1 d U . . H7 H 0.7550 -0.1892 0.1842 0.032 Uiso 1 1 calc R . . C18 C 0.7723(3) -0.13633(18) 0.09129(15) 0.0230(6) Uani 1 1 d U . . H8 H 0.8260 -0.1794 0.0652 0.028 Uiso 1 1 calc R . . C19 C 0.7176(3) -0.05276(17) 0.06877(14) 0.0188(5) Uani 1 1 d U . . C20 C 0.7355(3) -0.01893(17) 0.00270(14) 0.0182(5) Uani 1 1 d U . . C21 C 0.3752(3) 0.31512(17) -0.06306(15) 0.0203(6) Uani 1 1 d U . . C22 C 0.4632(3) 0.36126(19) -0.08276(16) 0.0229(6) Uani 1 1 d U . . H9 H 0.5476 0.3474 -0.0654 0.028 Uiso 1 1 calc R . . C23 C 0.4306(3) 0.42736(19) -0.12735(16) 0.0237(6) Uani 1 1 d U . . C24 C 0.3055(3) 0.44733(18) -0.15132(15) 0.0228(6) Uani 1 1 d U . . H10 H 0.2820 0.4925 -0.1819 0.027 Uiso 1 1 calc R . . C25 C 0.2141(3) 0.40317(17) -0.13191(15) 0.0199(6) Uani 1 1 d U . . C26 C 0.2509(3) 0.33705(17) -0.08717(15) 0.0210(6) Uani 1 1 d U . . H11 H 0.1895 0.3064 -0.0729 0.025 Uiso 1 1 calc R . . C27 C 0.5295(3) 0.4780(2) -0.14661(18) 0.0332(7) Uani 1 1 d U . . C28 C 0.5491(5) 0.5221(3) -0.0861(2) 0.0572(12) Uani 1 1 d U . . H12 H 0.5787 0.4819 -0.0502 0.069 Uiso 1 1 calc R . . H13 H 0.4658 0.5604 -0.0714 0.069 Uiso 1 1 calc R . . H14 H 0.6156 0.5525 -0.0974 0.069 Uiso 1 1 calc R . . C29 C 0.6627(4) 0.4210(3) -0.1708(2) 0.0460(10) Uani 1 1 d U . . H15 H 0.6944 0.3800 -0.1358 0.055 Uiso 1 1 calc R . . H16 H 0.7266 0.4535 -0.1812 0.055 Uiso 1 1 calc R . . H17 H 0.6516 0.3932 -0.2108 0.055 Uiso 1 1 calc R . . C30 C 0.4847(4) 0.5400(2) -0.20247(19) 0.0370(8) Uani 1 1 d U . . H18 H 0.5502 0.5715 -0.2127 0.044 Uiso 1 1 calc R . . H19 H 0.4000 0.5775 -0.1886 0.044 Uiso 1 1 calc R . . H20 H 0.4750 0.5112 -0.2421 0.044 Uiso 1 1 calc R . . C31 C 0.0737(3) 0.42676(18) -0.15487(15) 0.0226(6) Uani 1 1 d U . . C32 C 0.0530(3) 0.4960(2) -0.20756(16) 0.0273(7) Uani 1 1 d U . . H21 H -0.0379 0.5089 -0.2207 0.033 Uiso 1 1 calc R . . H22 H 0.1137 0.4787 -0.2465 0.033 Uiso 1 1 calc R . . H23 H 0.0698 0.5448 -0.1893 0.033 Uiso 1 1 calc R . . C33 C 0.0423(3) 0.3526(2) -0.18422(19) 0.0317(7) Uani 1 1 d U . . H24 H 0.0551 0.3072 -0.1512 0.038 Uiso 1 1 calc R . . H25 H 0.1009 0.3355 -0.2239 0.038 Uiso 1 1 calc R . . H26 H -0.0493 0.3675 -0.1964 0.038 Uiso 1 1 calc R . . C34 C -0.0210(3) 0.4552(2) -0.09395(17) 0.0285(7) Uani 1 1 d U . . H27 H -0.0087 0.4112 -0.0598 0.034 Uiso 1 1 calc R . . H28 H -0.1119 0.4689 -0.1071 0.034 Uiso 1 1 calc R . . H29 H -0.0027 0.5039 -0.0761 0.034 Uiso 1 1 calc R . . C35 C 0.2132(3) 0.2849(2) 0.27608(16) 0.0295(7) Uani 1 1 d U . . C36 C 0.2525(4) 0.3438(2) 0.30903(17) 0.0320(7) Uani 1 1 d U . . H30 H 0.3375 0.3521 0.2987 0.038 Uiso 1 1 calc R . . C37 C 0.1683(4) 0.3908(2) 0.35709(17) 0.0335(7) Uani 1 1 d U . . C38 C 0.0446(4) 0.3769(2) 0.37082(16) 0.0325(7) Uani 1 1 d U . . H31 H -0.0135 0.4089 0.4036 0.039 Uiso 1 1 calc R . . C39 C 0.0023(3) 0.3182(2) 0.33864(17) 0.0316(7) Uani 1 1 d U . . C40 C 0.0898(3) 0.2727(2) 0.29018(17) 0.0316(7) Uani 1 1 d U . . H32 H 0.0636 0.2328 0.2666 0.038 Uiso 1 1 calc R . . C41 C 0.2073(5) 0.4566(3) 0.3950(2) 0.0576(8) Uani 1 1 d DU . . C42 C 0.3450(5) 0.4614(4) 0.3776(3) 0.0682(10) Uani 1 1 d DU . . H33 H 0.3562 0.4731 0.3298 0.082 Uiso 1 1 calc R . . H34 H 0.4061 0.4089 0.3891 0.082 Uiso 1 1 calc R . . H35 H 0.3632 0.5052 0.4025 0.082 Uiso 1 1 calc R . . C43 C 0.1131(5) 0.5399(3) 0.3809(3) 0.0666(10) Uani 1 1 d DU . . H36 H 0.1215 0.5542 0.3334 0.080 Uiso 1 1 calc R . . H37 H 0.1346 0.5817 0.4069 0.080 Uiso 1 1 calc R . . H38 H 0.0225 0.5374 0.3933 0.080 Uiso 1 1 calc R . . C44 C 0.1926(5) 0.4388(3) 0.4687(2) 0.0582(9) Uani 1 1 d DU . . H39 H 0.1019 0.4366 0.4812 0.070 Uiso 1 1 calc R . . H40 H 0.2131 0.4823 0.4931 0.070 Uiso 1 1 calc R . . H41 H 0.2531 0.3860 0.4798 0.070 Uiso 1 1 calc R . . C45 C -0.1341(4) 0.3036(3) 0.3536(2) 0.0513(7) Uani 1 1 d U . . C46 C -0.2053(5) 0.3471(3) 0.4157(2) 0.0559(9) Uani 1 1 d U . . H42 H -0.1539 0.3266 0.4543 0.067 Uiso 1 1 calc R . . H43 H -0.2923 0.3364 0.4230 0.067 Uiso 1 1 calc R . . H44 H -0.2153 0.4063 0.4098 0.067 Uiso 1 1 calc R . . C47 C -0.2162(5) 0.3384(3) 0.2954(3) 0.0605(10) Uani 1 1 d U . . H45 H -0.1736 0.3112 0.2546 0.073 Uiso 1 1 calc R . . H46 H -0.2241 0.3974 0.2904 0.073 Uiso 1 1 calc R . . H47 H -0.3040 0.3289 0.3036 0.073 Uiso 1 1 calc R . . C48 C -0.1227(5) 0.2125(3) 0.3634(3) 0.0587(9) Uani 1 1 d U . . H48 H -0.0692 0.1911 0.4011 0.070 Uiso 1 1 calc R . . H49 H -0.0810 0.1839 0.3231 0.070 Uiso 1 1 calc R . . H50 H -0.2107 0.2037 0.3725 0.070 Uiso 1 1 calc R . . C49 C 0.6343(3) -0.1056(2) 0.29262(15) 0.0307(7) Uani 1 1 d U . . C50 C 0.7142(4) -0.0947(2) 0.34095(17) 0.0363(8) Uani 1 1 d U . . H51 H 0.7487 -0.0478 0.3384 0.044 Uiso 1 1 calc R . . C51 C 0.7447(4) -0.1521(3) 0.39356(19) 0.0448(9) Uani 1 1 d U . . C52 C 0.6921(4) -0.2191(3) 0.39496(18) 0.0439(9) Uani 1 1 d U . . H52 H 0.7114 -0.2582 0.4307 0.053 Uiso 1 1 calc R . . C53 C 0.6133(4) -0.2327(2) 0.34741(17) 0.0369(8) Uani 1 1 d U . . C54 C 0.5841(4) -0.1740(2) 0.29560(17) 0.0335(8) Uani 1 1 d U . . H53 H 0.5295 -0.1811 0.2622 0.040 Uiso 1 1 calc R . . C55 C 0.8349(5) -0.1436(4) 0.4470(3) 0.0736(9) Uani 1 1 d DU . . C56 C 0.8714(6) -0.0617(4) 0.4421(3) 0.0739(11) Uani 1 1 d DU . . H54 H 0.9118 -0.0544 0.3976 0.089 Uiso 1 1 calc R . . H55 H 0.9338 -0.0610 0.4756 0.089 Uiso 1 1 calc R . . H56 H 0.7919 -0.0169 0.4501 0.089 Uiso 1 1 calc R . . C57 C 0.7733(6) -0.1556(4) 0.5151(3) 0.0753(11) Uani 1 1 d DU . . H57 H 0.8328 -0.1504 0.5487 0.090 Uiso 1 1 calc R . . H58 H 0.7574 -0.2104 0.5190 0.090 Uiso 1 1 calc R . . H59 H 0.6897 -0.1139 0.5218 0.090 Uiso 1 1 calc R . . C58 C 0.9617(6) -0.2128(4) 0.4398(3) 0.0812(12) Uani 1 1 d DU . . H60 H 1.0068 -0.2076 0.3961 0.097 Uiso 1 1 calc R . . H61 H 0.9401 -0.2659 0.4439 0.097 Uiso 1 1 calc R . . H62 H 1.0193 -0.2090 0.4748 0.097 Uiso 1 1 calc R . . C59 C 0.5594(5) -0.3087(3) 0.3534(2) 0.0522(7) Uani 1 1 d U . . C60 C 0.4695(5) -0.3044(3) 0.4162(2) 0.0539(9) Uani 1 1 d U . . H63 H 0.4362 -0.3536 0.4207 0.065 Uiso 1 1 calc R . . H64 H 0.3955 -0.2555 0.4138 0.065 Uiso 1 1 calc R . . H65 H 0.5189 -0.3014 0.4549 0.065 Uiso 1 1 calc R . . C61 C 0.6735(5) -0.3863(3) 0.3569(2) 0.0597(10) Uani 1 1 d U . . H66 H 0.6385 -0.4348 0.3614 0.072 Uiso 1 1 calc R . . H67 H 0.7236 -0.3840 0.3955 0.072 Uiso 1 1 calc R . . H68 H 0.7313 -0.3896 0.3162 0.072 Uiso 1 1 calc R . . C62 C 0.4841(5) -0.3170(3) 0.2939(2) 0.0539(9) Uani 1 1 d U . . H69 H 0.4519 -0.3665 0.2998 0.065 Uiso 1 1 calc R . . H70 H 0.5426 -0.3211 0.2533 0.065 Uiso 1 1 calc R . . H71 H 0.4094 -0.2688 0.2901 0.065 Uiso 1 1 calc R . . C63 C 0.8345(3) -0.05979(17) -0.04513(15) 0.0201(6) Uani 1 1 d U . . C64 C 0.9427(3) -0.13292(17) -0.02883(15) 0.0209(6) Uani 1 1 d U . . C65 C 1.0339(3) -0.1300(2) 0.01656(17) 0.0283(7) Uani 1 1 d U . . H72 H 1.0275 -0.0805 0.0388 0.034 Uiso 1 1 calc R . . C66 C 1.1341(3) -0.1992(2) 0.0295(2) 0.0372(8) Uani 1 1 d U . . H73 H 1.1968 -0.1970 0.0603 0.045 Uiso 1 1 calc R . . C67 C 1.1431(3) -0.2714(2) -0.0024(2) 0.0385(8) Uani 1 1 d U . . H74 H 1.2107 -0.3190 0.0073 0.046 Uiso 1 1 calc R . . C68 C 1.0539(3) -0.2743(2) -0.04820(19) 0.0340(8) Uani 1 1 d U . . H75 H 1.0607 -0.3239 -0.0703 0.041 Uiso 1 1 calc R . . C69 C 0.9549(3) -0.20549(18) -0.06214(16) 0.0245(6) Uani 1 1 d U . . H76 H 0.8949 -0.2075 -0.0945 0.029 Uiso 1 1 calc R . . C70 C 0.7600(3) 0.0323(2) -0.13180(16) 0.0274(6) Uani 1 1 d U . . C71 C 0.6508(4) 0.2498(3) 0.1540(3) 0.0540(11) Uani 1 1 d U . . H77 H 0.5802 0.2855 0.1293 0.081 Uiso 1 1 calc R . . H78 H 0.7285 0.2717 0.1494 0.081 Uiso 1 1 calc R . . H79 H 0.6212 0.2474 0.2011 0.081 Uiso 1 1 calc R . . C72 C 0.8836(4) 0.0382(3) 0.2259(2) 0.0521(11) Uani 1 1 d U . . H80 H 0.9429 0.0296 0.2621 0.078 Uiso 1 1 calc R . . H81 H 0.8973 -0.0131 0.2022 0.078 Uiso 1 1 calc R . . H82 H 0.7922 0.0552 0.2442 0.078 Uiso 1 1 calc R . . C73 C 0.7722(7) 0.0447(4) -0.2059(2) 0.0312(14) Uani 0.478(13) 1 d PGU A 1 C74 C 0.7903(8) -0.0210(4) -0.2478(3) 0.0335(14) Uani 0.478(13) 1 d PGU A 1 H83 H 0.7883 -0.0737 -0.2297 0.040 Uiso 0.478(13) 1 calc PR A 1 C75 C 0.8112(7) -0.0096(6) -0.3160(3) 0.0416(16) Uani 0.478(13) 1 d PGU A 1 H84 H 0.8236 -0.0545 -0.3447 0.050 Uiso 0.478(13) 1 calc PR A 1 C76 C 0.8141(7) 0.0676(6) -0.3424(2) 0.0445(17) Uani 0.478(13) 1 d PGU A 1 H85 H 0.8284 0.0754 -0.3890 0.053 Uiso 0.478(13) 1 calc PR A 1 C77 C 0.7960(8) 0.1333(4) -0.3005(4) 0.0456(17) Uani 0.478(13) 1 d PGU A 1 H86 H 0.7980 0.1860 -0.3185 0.055 Uiso 0.478(13) 1 calc PR A 1 C78 C 0.7751(8) 0.1218(4) -0.2322(3) 0.0377(16) Uani 0.478(13) 1 d PGU A 1 H87 H 0.7627 0.1667 -0.2036 0.045 Uiso 0.478(13) 1 calc PR A 1 C79 C 0.7861(7) 0.0576(4) -0.2021(2) 0.0360(15) Uani 0.522(13) 1 d PGU A 2 C80 C 0.7800(7) 0.0041(5) -0.2515(3) 0.0380(14) Uani 0.522(13) 1 d PGU A 2 H88 H 0.7624 -0.0473 -0.2396 0.046 Uiso 0.522(13) 1 calc PR A 2 C81 C 0.7995(7) 0.0258(6) -0.3181(3) 0.0424(15) Uani 0.522(13) 1 d PGU A 2 H89 H 0.7953 -0.0107 -0.3517 0.051 Uiso 0.522(13) 1 calc PR A 2 C82 C 0.8253(6) 0.1011(5) -0.3353(2) 0.0460(16) Uani 0.522(13) 1 d PGU A 2 H90 H 0.8386 0.1160 -0.3808 0.055 Uiso 0.522(13) 1 calc PR A 2 C83 C 0.8314(8) 0.1546(4) -0.2860(3) 0.0486(17) Uani 0.522(13) 1 d PGU A 2 H91 H 0.8490 0.2060 -0.2978 0.058 Uiso 0.522(13) 1 calc PR A 2 C84 C 0.8118(8) 0.1329(4) -0.2194(3) 0.0444(16) Uani 0.522(13) 1 d PGU A 2 H92 H 0.8160 0.1694 -0.1857 0.053 Uiso 0.522(13) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02198(18) 0.01425(17) 0.01886(18) -0.00174(11) -0.00060(13) 0.00021(12) O1 0.0345(12) 0.0306(12) 0.0217(11) 0.0040(9) -0.0002(10) 0.0077(10) O2 0.0253(12) 0.0223(11) 0.0434(14) -0.0072(10) -0.0098(11) 0.0003(9) O3 0.0230(12) 0.0498(16) 0.0397(14) 0.0090(12) 0.0040(11) -0.0011(11) N1 0.0193(11) 0.0155(11) 0.0189(11) 0.0004(9) -0.0007(10) -0.0015(9) N2 0.0206(11) 0.0158(11) 0.0212(12) -0.0011(9) -0.0016(10) -0.0006(9) N3 0.0344(14) 0.0215(13) 0.0181(12) -0.0024(9) 0.0009(11) 0.0037(10) N4 0.0242(12) 0.0152(11) 0.0187(11) -0.0013(9) 0.0001(10) -0.0019(9) N5 0.0249(13) 0.0220(13) 0.0224(12) 0.0014(10) 0.0028(11) 0.0013(10) C1 0.0197(13) 0.0147(12) 0.0197(13) -0.0004(10) -0.0005(11) -0.0041(10) C2 0.0223(13) 0.0188(13) 0.0204(13) 0.0019(10) -0.0008(12) 0.0008(11) C3 0.0220(14) 0.0194(14) 0.0243(14) 0.0016(11) -0.0015(12) 0.0001(11) C4 0.0164(12) 0.0187(13) 0.0210(13) 0.0003(10) -0.0021(11) -0.0034(10) C5 0.0176(12) 0.0168(13) 0.0216(13) 0.0002(10) -0.0035(11) -0.0039(10) C6 0.0164(12) 0.0138(12) 0.0252(14) -0.0013(10) -0.0009(11) -0.0024(10) C7 0.0202(13) 0.0152(13) 0.0300(15) -0.0014(11) -0.0005(12) -0.0015(10) C8 0.0237(14) 0.0181(14) 0.0296(15) -0.0035(11) -0.0008(13) -0.0008(11) C9 0.0218(13) 0.0168(13) 0.0249(14) -0.0038(11) 0.0019(12) -0.0021(10) C10 0.0308(15) 0.0213(14) 0.0253(15) -0.0058(11) 0.0034(13) 0.0017(12) C11 0.0372(17) 0.0253(15) 0.0234(15) -0.0034(12) 0.0037(14) 0.0031(13) C12 0.051(2) 0.0331(18) 0.0244(16) -0.0025(13) 0.0054(16) 0.0062(16) C13 0.050(2) 0.0347(18) 0.0226(15) -0.0005(13) 0.0052(16) 0.0069(16) C14 0.0350(17) 0.0266(16) 0.0210(14) -0.0008(12) 0.0007(14) 0.0022(13) C15 0.0321(16) 0.0233(15) 0.0203(14) 0.0017(11) 0.0006(13) 0.0010(12) C16 0.0266(14) 0.0178(13) 0.0206(13) 0.0007(10) -0.0009(12) 0.0000(11) C17 0.0317(16) 0.0183(14) 0.0248(15) 0.0023(11) 0.0019(13) 0.0010(12) C18 0.0264(14) 0.0153(13) 0.0236(14) 0.0012(11) 0.0022(13) -0.0003(11) C19 0.0201(13) 0.0141(12) 0.0216(13) -0.0011(10) -0.0015(11) -0.0028(10) C20 0.0199(13) 0.0146(12) 0.0203(13) -0.0008(10) -0.0037(11) -0.0040(10) C21 0.0190(13) 0.0159(13) 0.0241(14) 0.0000(10) -0.0010(12) -0.0012(10) C22 0.0166(13) 0.0243(14) 0.0279(15) 0.0020(11) -0.0042(12) -0.0048(11) C23 0.0209(14) 0.0253(15) 0.0257(14) 0.0017(11) -0.0010(12) -0.0079(11) C24 0.0213(14) 0.0195(14) 0.0258(14) 0.0040(11) -0.0024(12) -0.0028(11) C25 0.0189(13) 0.0157(13) 0.0235(13) -0.0003(10) -0.0006(12) -0.0017(10) C26 0.0182(13) 0.0168(13) 0.0278(14) 0.0006(11) -0.0014(12) -0.0040(10) C27 0.0296(16) 0.0399(19) 0.0353(17) 0.0080(14) -0.0037(15) -0.0194(14) C28 0.080(3) 0.068(3) 0.043(2) 0.000(2) -0.003(2) -0.055(3) C29 0.0263(17) 0.059(3) 0.053(2) 0.0169(19) -0.0035(18) -0.0149(17) C30 0.0395(19) 0.0357(19) 0.0397(19) 0.0067(15) 0.0012(17) -0.0191(15) C31 0.0198(13) 0.0199(13) 0.0264(14) 0.0001(11) -0.0056(12) -0.0010(10) C32 0.0233(14) 0.0261(15) 0.0282(15) 0.0025(12) -0.0060(13) 0.0018(11) C33 0.0263(15) 0.0253(15) 0.0434(18) -0.0021(13) -0.0112(14) -0.0037(12) C34 0.0207(14) 0.0282(15) 0.0328(16) 0.0043(12) -0.0005(13) -0.0007(11) C35 0.0351(16) 0.0221(15) 0.0239(14) -0.0028(11) 0.0031(14) 0.0050(12) C36 0.0386(18) 0.0260(16) 0.0272(16) -0.0032(12) 0.0064(15) -0.0029(13) C37 0.0464(19) 0.0241(15) 0.0249(15) -0.0024(12) 0.0069(15) -0.0022(14) C38 0.0386(18) 0.0284(16) 0.0220(15) -0.0042(12) 0.0064(14) 0.0050(13) C39 0.0326(16) 0.0285(16) 0.0265(15) -0.0014(12) 0.0010(14) 0.0041(13) C40 0.0342(17) 0.0270(16) 0.0283(16) -0.0056(12) -0.0005(14) 0.0019(13) C41 0.0606(10) 0.0565(10) 0.0568(10) -0.0046(8) -0.0026(8) -0.0168(7) C42 0.0692(13) 0.0676(13) 0.0690(13) -0.0071(9) -0.0019(9) -0.0194(9) C43 0.0698(12) 0.0639(12) 0.0655(12) -0.0033(9) -0.0048(9) -0.0156(9) C44 0.0607(12) 0.0580(12) 0.0567(12) -0.0034(9) -0.0037(9) -0.0162(9) C45 0.0412(13) 0.0582(15) 0.0523(14) -0.0010(13) 0.0006(12) -0.0098(12) C46 0.0462(16) 0.0636(18) 0.0546(17) -0.0041(16) 0.0069(15) -0.0108(15) C47 0.0464(16) 0.0726(19) 0.0576(18) 0.0057(16) -0.0023(16) -0.0082(15) C48 0.0463(16) 0.0599(18) 0.0680(19) -0.0009(16) 0.0032(16) -0.0123(15) C49 0.0347(17) 0.0290(16) 0.0184(14) 0.0020(12) 0.0048(13) 0.0073(13) C50 0.0321(17) 0.048(2) 0.0237(16) 0.0075(14) 0.0031(15) -0.0033(15) C51 0.0353(18) 0.066(2) 0.0290(17) 0.0160(17) -0.0002(16) -0.0092(17) C52 0.041(2) 0.055(2) 0.0255(17) 0.0179(16) 0.0015(16) 0.0021(17) C53 0.0449(19) 0.0298(17) 0.0251(15) 0.0051(13) 0.0072(15) 0.0063(14) C54 0.0429(19) 0.0266(16) 0.0222(15) 0.0004(12) -0.0002(14) 0.0063(14) C55 0.0694(16) 0.0961(19) 0.0612(16) 0.0188(15) -0.0162(15) -0.0318(15) C56 0.0699(19) 0.098(2) 0.0617(19) 0.0145(18) -0.0177(18) -0.0343(18) C57 0.074(2) 0.099(2) 0.0605(19) 0.0146(18) -0.0145(18) -0.0350(18) C58 0.073(2) 0.100(2) 0.071(2) 0.0205(19) -0.0148(18) -0.0236(19) C59 0.0705(16) 0.0385(13) 0.0416(13) 0.0065(11) 0.0026(13) -0.0068(12) C60 0.0694(19) 0.0454(16) 0.0444(16) 0.0036(14) 0.0053(16) -0.0138(15) C61 0.075(2) 0.0434(17) 0.0499(17) 0.0084(14) 0.0032(16) -0.0001(16) C62 0.0758(19) 0.0384(16) 0.0453(16) 0.0043(14) -0.0013(16) -0.0125(15) C63 0.0214(13) 0.0158(13) 0.0221(13) 0.0005(10) -0.0008(12) -0.0033(10) C64 0.0176(13) 0.0168(13) 0.0259(14) 0.0014(10) 0.0033(12) -0.0019(10) C65 0.0253(15) 0.0237(15) 0.0374(17) 0.0036(12) -0.0062(14) -0.0087(12) C66 0.0249(15) 0.0340(18) 0.054(2) 0.0111(15) -0.0138(16) -0.0082(13) C67 0.0253(16) 0.0249(16) 0.060(2) 0.0089(15) -0.0030(17) 0.0003(13) C68 0.0301(16) 0.0198(15) 0.0469(19) -0.0003(13) 0.0051(16) 0.0008(12) C69 0.0231(14) 0.0194(14) 0.0285(15) -0.0025(11) 0.0032(13) -0.0021(11) C70 0.0269(15) 0.0248(15) 0.0248(14) 0.0032(12) 0.0023(13) 0.0018(12) C71 0.0397(19) 0.041(2) 0.084(3) -0.023(2) -0.002(2) -0.0122(16) C72 0.0316(18) 0.071(3) 0.052(2) 0.023(2) -0.0035(18) -0.0151(18) C73 0.025(2) 0.035(2) 0.030(2) 0.004(2) -0.001(2) -0.003(2) C74 0.029(2) 0.040(3) 0.030(2) -0.003(2) 0.000(2) -0.006(2) C75 0.038(2) 0.047(3) 0.037(2) -0.003(2) 0.000(2) -0.005(2) C76 0.042(3) 0.047(3) 0.041(3) 0.007(2) 0.002(2) -0.007(2) C77 0.045(3) 0.045(3) 0.041(3) 0.009(2) 0.002(2) -0.005(2) C78 0.035(3) 0.039(2) 0.034(2) 0.008(2) 0.002(2) -0.003(2) C79 0.033(2) 0.036(2) 0.029(2) 0.007(2) 0.004(2) 0.004(2) C80 0.034(2) 0.044(3) 0.031(2) 0.003(2) 0.000(2) -0.004(2) C81 0.041(2) 0.045(3) 0.037(2) 0.002(2) 0.000(2) -0.004(2) C82 0.048(3) 0.047(3) 0.039(2) 0.002(2) -0.001(2) -0.005(2) C83 0.051(3) 0.046(3) 0.044(3) 0.008(2) 0.003(2) -0.007(2) C84 0.046(3) 0.041(2) 0.039(2) 0.007(2) 0.007(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.049(4) . ? Zn1 N3 2.057(4) . ? Zn1 N4 2.066(4) . ? Zn1 N2 2.069(4) . ? Zn1 O2 2.106(3) . ? O1 C3 1.213(4) . ? O2 C71 1.405(5) . ? O2 H1 0.79(4) . ? O3 C72 1.413(5) . ? O3 H2 0.8400 . ? N1 C1 1.368(4) . ? N1 C4 1.373(4) . ? N2 C6 1.354(4) . ? N2 C9 1.378(4) . ? N3 C14 1.362(4) . ? N3 C11 1.366(4) . ? N4 C19 1.344(4) . ? N4 C16 1.394(4) . ? N5 C63 1.335(4) . ? N5 C70 1.355(4) . ? C1 C2 1.411(4) . ? C1 C20 1.418(4) . ? C2 C70 1.370(5) . ? C2 C3 1.473(4) . ? C3 C4 1.505(5) . ? C4 C5 1.382(4) . ? C5 C6 1.427(5) . ? C5 C21 1.499(4) . ? C6 C7 1.438(4) . ? C7 C8 1.346(5) . ? C7 H3 0.9500 . ? C8 C9 1.437(4) . ? C8 H4 0.9500 . ? C9 C10 1.380(5) . ? C10 C11 1.403(5) . ? C10 C35 1.504(5) . ? C11 C12 1.422(5) . ? C12 C13 1.356(5) . ? C12 H5 0.9500 . ? C13 C14 1.426(5) . ? C13 H6 0.9500 . ? C14 C15 1.411(5) . ? C15 C16 1.381(5) . ? C15 C49 1.504(5) . ? C16 C17 1.433(5) . ? C17 C18 1.343(5) . ? C17 H7 0.9500 . ? C18 C19 1.444(4) . ? C18 H8 0.9500 . ? C19 C20 1.443(4) . ? C20 C63 1.425(4) . ? C21 C22 1.385(4) . ? C21 C26 1.385(4) . ? C22 C23 1.388(5) . ? C22 H9 0.9500 . ? C23 C24 1.393(5) . ? C23 C27 1.530(5) . ? C24 C25 1.389(4) . ? C24 H10 0.9500 . ? C25 C26 1.394(4) . ? C25 C31 1.532(4) . ? C26 H11 0.9500 . ? C27 C28 1.512(6) . ? C27 C30 1.517(5) . ? C27 C29 1.541(6) . ? C28 H12 0.9800 . ? C28 H13 0.9800 . ? C28 H14 0.9800 . ? C29 H15 0.9800 . ? C29 H16 0.9800 . ? C29 H17 0.9800 . ? C30 H18 0.9800 . ? C30 H19 0.9800 . ? C30 H20 0.9800 . ? C31 C32 1.526(5) . ? C31 C33 1.530(5) . ? C31 C34 1.535(5) . ? C32 H21 0.9800 . ? C32 H22 0.9800 . ? C32 H23 0.9800 . ? C33 H24 0.9800 . ? C33 H25 0.9800 . ? C33 H26 0.9800 . ? C34 H27 0.9800 . ? C34 H28 0.9800 . ? C34 H29 0.9800 . ? C35 C40 1.377(5) . ? C35 C36 1.385(5) . ? C36 C37 1.390(5) . ? C36 H30 0.9500 . ? C37 C38 1.389(6) . ? C37 C41 1.534(6) . ? C38 C39 1.392(5) . ? C38 H31 0.9500 . ? C39 C40 1.400(5) . ? C39 C45 1.527(6) . ? C40 H32 0.9500 . ? C41 C42 1.490(6) . ? C41 C44 1.507(6) . ? C41 C43 1.525(6) . ? C42 H33 0.9800 . ? C42 H34 0.9800 . ? C42 H35 0.9800 . ? C43 H36 0.9800 . ? C43 H37 0.9800 . ? C43 H38 0.9800 . ? C44 H39 0.9800 . ? C44 H40 0.9800 . ? C44 H41 0.9800 . ? C45 C48 1.515(7) . ? C45 C47 1.516(7) . ? C45 C46 1.526(7) . ? C46 H42 0.9800 . ? C46 H43 0.9800 . ? C46 H44 0.9800 . ? C47 H45 0.9800 . ? C47 H46 0.9800 . ? C47 H47 0.9800 . ? C48 H48 0.9800 . ? C48 H49 0.9800 . ? C48 H50 0.9800 . ? C49 C50 1.385(5) . ? C49 C54 1.386(6) . ? C50 C51 1.401(5) . ? C50 H51 0.9500 . ? C51 C52 1.382(7) . ? C51 C55 1.525(7) . ? C52 C53 1.380(6) . ? C52 H52 0.9500 . ? C53 C54 1.400(5) . ? C53 C59 1.530(6) . ? C54 H53 0.9500 . ? C55 C57 1.502(6) . ? C55 C56 1.526(7) . ? C55 C58 1.532(7) . ? C56 H54 0.9800 . ? C56 H55 0.9800 . ? C56 H56 0.9800 . ? C57 H57 0.9800 . ? C57 H58 0.9800 . ? C57 H59 0.9800 . ? C58 H60 0.9800 . ? C58 H61 0.9800 . ? C58 H62 0.9800 . ? C59 C60 1.517(7) . ? C59 C62 1.519(7) . ? C59 C61 1.534(7) . ? C60 H63 0.9800 . ? C60 H64 0.9800 . ? C60 H65 0.9800 . ? C61 H66 0.9800 . ? C61 H67 0.9800 . ? C61 H68 0.9800 . ? C62 H69 0.9800 . ? C62 H70 0.9800 . ? C62 H71 0.9800 . ? C63 C64 1.490(4) . ? C64 C65 1.389(5) . ? C64 C69 1.396(5) . ? C65 C66 1.386(5) . ? C65 H72 0.9500 . ? C66 C67 1.382(6) . ? C66 H73 0.9500 . ? C67 C68 1.379(6) . ? C67 H74 0.9500 . ? C68 C69 1.379(5) . ? C68 H75 0.9500 . ? C69 H76 0.9500 . ? C70 C79 1.489(6) . ? C70 C73 1.499(6) . ? C71 H77 0.9800 . ? C71 H78 0.9800 . ? C71 H79 0.9800 . ? C72 H80 0.9800 . ? C72 H81 0.9800 . ? C72 H82 0.9800 . ? C73 C74 1.3900 . ? C73 C78 1.3900 . ? C74 C75 1.3900 . ? C74 H83 0.9500 . ? C75 C76 1.3900 . ? C75 H84 0.9500 . ? C76 C77 1.3900 . ? C76 H85 0.9500 . ? C77 C78 1.3900 . ? C77 H86 0.9500 . ? C78 H87 0.9500 . ? C79 C80 1.3900 . ? C79 C84 1.3900 . ? C80 C81 1.3900 . ? C80 H88 0.9500 . ? C81 C82 1.3900 . ? C81 H89 0.9500 . ? C82 C83 1.3900 . ? C82 H90 0.9500 . ? C83 C84 1.3900 . ? C83 H91 0.9500 . ? C84 H92 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N3 165.75(11) . . ? N1 Zn1 N4 89.16(12) . . ? N3 Zn1 N4 89.53(12) . . ? N1 Zn1 N2 88.32(12) . . ? N3 Zn1 N2 88.71(13) . . ? N4 Zn1 N2 162.67(10) . . ? N1 Zn1 O2 95.17(11) . . ? N3 Zn1 O2 99.04(13) . . ? N4 Zn1 O2 99.89(15) . . ? N2 Zn1 O2 97.42(16) . . ? C71 O2 Zn1 120.1(2) . . ? C71 O2 H1 110(3) . . ? Zn1 O2 H1 121(3) . . ? C72 O3 H2 109.5 . . ? C1 N1 C4 107.7(3) . . ? C1 N1 Zn1 124.1(2) . . ? C4 N1 Zn1 126.6(2) . . ? C6 N2 C9 106.2(3) . . ? C6 N2 Zn1 126.8(2) . . ? C9 N2 Zn1 126.2(2) . . ? C14 N3 C11 106.8(3) . . ? C14 N3 Zn1 126.8(2) . . ? C11 N3 Zn1 125.7(2) . . ? C19 N4 C16 106.5(3) . . ? C19 N4 Zn1 128.2(2) . . ? C16 N4 Zn1 125.3(2) . . ? C63 N5 C70 119.7(3) . . ? N1 C1 C2 112.7(3) . . ? N1 C1 C20 127.7(3) . . ? C2 C1 C20 119.6(3) . . ? C70 C2 C1 121.2(3) . . ? C70 C2 C3 132.5(3) . . ? C1 C2 C3 106.3(3) . . ? O1 C3 C2 129.1(3) . . ? O1 C3 C4 127.8(3) . . ? C2 C3 C4 103.1(3) . . ? N1 C4 C5 126.5(3) . . ? N1 C4 C3 110.0(3) . . ? C5 C4 C3 123.5(3) . . ? C4 C5 C6 124.2(3) . . ? C4 C5 C21 120.3(3) . . ? C6 C5 C21 115.4(3) . . ? N2 C6 C5 125.6(3) . . ? N2 C6 C7 110.4(3) . . ? C5 C6 C7 124.0(3) . . ? C8 C7 C6 106.7(3) . . ? C8 C7 H3 126.6 . . ? C6 C7 H3 126.6 . . ? C7 C8 C9 107.2(3) . . ? C7 C8 H4 126.4 . . ? C9 C8 H4 126.4 . . ? N2 C9 C10 125.5(3) . . ? N2 C9 C8 109.4(3) . . ? C10 C9 C8 125.0(3) . . ? C9 C10 C11 125.8(3) . . ? C9 C10 C35 118.0(3) . . ? C11 C10 C35 116.2(3) . . ? N3 C11 C10 125.6(3) . . ? N3 C11 C12 109.5(3) . . ? C10 C11 C12 124.7(3) . . ? C13 C12 C11 107.2(3) . . ? C13 C12 H5 126.4 . . ? C11 C12 H5 126.4 . . ? C12 C13 C14 106.8(3) . . ? C12 C13 H6 126.6 . . ? C14 C13 H6 126.6 . . ? N3 C14 C15 124.8(3) . . ? N3 C14 C13 109.6(3) . . ? C15 C14 C13 125.4(3) . . ? C16 C15 C14 125.8(3) . . ? C16 C15 C49 118.1(3) . . ? C14 C15 C49 116.1(3) . . ? C15 C16 N4 126.1(3) . . ? C15 C16 C17 124.6(3) . . ? N4 C16 C17 109.1(3) . . ? C18 C17 C16 107.1(3) . . ? C18 C17 H7 126.4 . . ? C16 C17 H7 126.4 . . ? C17 C18 C19 107.3(3) . . ? C17 C18 H8 126.4 . . ? C19 C18 H8 126.4 . . ? N4 C19 C20 123.6(3) . . ? N4 C19 C18 110.0(3) . . ? C20 C19 C18 126.4(3) . . ? C1 C20 C63 114.2(3) . . ? C1 C20 C19 123.2(3) . . ? C63 C20 C19 122.6(3) . . ? C22 C21 C26 119.0(3) . . ? C22 C21 C5 119.7(3) . . ? C26 C21 C5 121.1(3) . . ? C21 C22 C23 121.4(3) . . ? C21 C22 H9 119.3 . . ? C23 C22 H9 119.3 . . ? C22 C23 C24 118.3(3) . . ? C22 C23 C27 119.8(3) . . ? C24 C23 C27 121.9(3) . . ? C25 C24 C23 121.9(3) . . ? C25 C24 H10 119.0 . . ? C23 C24 H10 119.0 . . ? C24 C25 C26 118.0(3) . . ? C24 C25 C31 122.7(3) . . ? C26 C25 C31 119.2(3) . . ? C21 C26 C25 121.4(3) . . ? C21 C26 H11 119.3 . . ? C25 C26 H11 119.3 . . ? C28 C27 C30 109.6(4) . . ? C28 C27 C23 109.0(3) . . ? C30 C27 C23 112.3(3) . . ? C28 C27 C29 108.7(4) . . ? C30 C27 C29 107.4(3) . . ? C23 C27 C29 109.8(3) . . ? C27 C28 H12 109.5 . . ? C27 C28 H13 109.5 . . ? H12 C28 H13 109.5 . . ? C27 C28 H14 109.5 . . ? H12 C28 H14 109.5 . . ? H13 C28 H14 109.5 . . ? C27 C29 H15 109.5 . . ? C27 C29 H16 109.5 . . ? H15 C29 H16 109.5 . . ? C27 C29 H17 109.5 . . ? H15 C29 H17 109.5 . . ? H16 C29 H17 109.5 . . ? C27 C30 H18 109.5 . . ? C27 C30 H19 109.5 . . ? H18 C30 H19 109.5 . . ? C27 C30 H20 109.5 . . ? H18 C30 H20 109.5 . . ? H19 C30 H20 109.5 . . ? C32 C31 C33 108.1(3) . . ? C32 C31 C25 112.4(3) . . ? C33 C31 C25 110.2(3) . . ? C32 C31 C34 108.8(3) . . ? C33 C31 C34 109.5(3) . . ? C25 C31 C34 107.9(3) . . ? C31 C32 H21 109.5 . . ? C31 C32 H22 109.5 . . ? H21 C32 H22 109.5 . . ? C31 C32 H23 109.5 . . ? H21 C32 H23 109.5 . . ? H22 C32 H23 109.5 . . ? C31 C33 H24 109.5 . . ? C31 C33 H25 109.5 . . ? H24 C33 H25 109.5 . . ? C31 C33 H26 109.5 . . ? H24 C33 H26 109.5 . . ? H25 C33 H26 109.5 . . ? C31 C34 H27 109.5 . . ? C31 C34 H28 109.5 . . ? H27 C34 H28 109.5 . . ? C31 C34 H29 109.5 . . ? H27 C34 H29 109.5 . . ? H28 C34 H29 109.5 . . ? C40 C35 C36 120.3(3) . . ? C40 C35 C10 119.5(3) . . ? C36 C35 C10 120.1(3) . . ? C35 C36 C37 120.4(4) . . ? C35 C36 H30 119.8 . . ? C37 C36 H30 119.8 . . ? C38 C37 C36 118.2(3) . . ? C38 C37 C41 119.4(3) . . ? C36 C37 C41 122.4(4) . . ? C37 C38 C39 122.8(3) . . ? C37 C38 H31 118.6 . . ? C39 C38 H31 118.6 . . ? C38 C39 C40 117.2(3) . . ? C38 C39 C45 122.6(3) . . ? C40 C39 C45 120.2(4) . . ? C35 C40 C39 121.1(3) . . ? C35 C40 H32 119.4 . . ? C39 C40 H32 119.4 . . ? C42 C41 C44 108.4(4) . . ? C42 C41 C43 109.3(4) . . ? C44 C41 C43 107.2(4) . . ? C42 C41 C37 113.3(4) . . ? C44 C41 C37 109.3(4) . . ? C43 C41 C37 109.2(4) . . ? C41 C42 H33 109.5 . . ? C41 C42 H34 109.5 . . ? H33 C42 H34 109.5 . . ? C41 C42 H35 109.5 . . ? H33 C42 H35 109.5 . . ? H34 C42 H35 109.5 . . ? C41 C43 H36 109.5 . . ? C41 C43 H37 109.5 . . ? H36 C43 H37 109.5 . . ? C41 C43 H38 109.5 . . ? H36 C43 H38 109.5 . . ? H37 C43 H38 109.5 . . ? C41 C44 H39 109.5 . . ? C41 C44 H40 109.5 . . ? H39 C44 H40 109.5 . . ? C41 C44 H41 109.5 . . ? H39 C44 H41 109.5 . . ? H40 C44 H41 109.5 . . ? C48 C45 C47 110.6(4) . . ? C48 C45 C46 108.4(4) . . ? C47 C45 C46 107.3(4) . . ? C48 C45 C39 110.0(4) . . ? C47 C45 C39 108.0(4) . . ? C46 C45 C39 112.5(4) . . ? C45 C46 H42 109.5 . . ? C45 C46 H43 109.5 . . ? H42 C46 H43 109.5 . . ? C45 C46 H44 109.5 . . ? H42 C46 H44 109.5 . . ? H43 C46 H44 109.5 . . ? C45 C47 H45 109.5 . . ? C45 C47 H46 109.5 . . ? H45 C47 H46 109.5 . . ? C45 C47 H47 109.5 . . ? H45 C47 H47 109.5 . . ? H46 C47 H47 109.5 . . ? C45 C48 H48 109.5 . . ? C45 C48 H49 109.5 . . ? H48 C48 H49 109.5 . . ? C45 C48 H50 109.5 . . ? H48 C48 H50 109.5 . . ? H49 C48 H50 109.5 . . ? C50 C49 C54 120.2(3) . . ? C50 C49 C15 118.9(3) . . ? C54 C49 C15 120.8(3) . . ? C49 C50 C51 120.5(4) . . ? C49 C50 H51 119.7 . . ? C51 C50 H51 119.7 . . ? C52 C51 C50 117.5(4) . . ? C52 C51 C55 120.2(4) . . ? C50 C51 C55 122.3(4) . . ? C53 C52 C51 123.7(3) . . ? C53 C52 H52 118.1 . . ? C51 C52 H52 118.1 . . ? C52 C53 C54 117.5(4) . . ? C52 C53 C59 119.9(3) . . ? C54 C53 C59 122.6(4) . . ? C49 C54 C53 120.6(4) . . ? C49 C54 H53 119.7 . . ? C53 C54 H53 119.7 . . ? C57 C55 C51 110.5(4) . . ? C57 C55 C56 110.0(5) . . ? C51 C55 C56 113.0(4) . . ? C57 C55 C58 105.9(5) . . ? C51 C55 C58 108.7(5) . . ? C56 C55 C58 108.4(5) . . ? C55 C56 H54 109.5 . . ? C55 C56 H55 109.5 . . ? H54 C56 H55 109.5 . . ? C55 C56 H56 109.5 . . ? H54 C56 H56 109.5 . . ? H55 C56 H56 109.5 . . ? C55 C57 H57 109.5 . . ? C55 C57 H58 109.5 . . ? H57 C57 H58 109.5 . . ? C55 C57 H59 109.5 . . ? H57 C57 H59 109.5 . . ? H58 C57 H59 109.5 . . ? C55 C58 H60 109.5 . . ? C55 C58 H61 109.5 . . ? H60 C58 H61 109.5 . . ? C55 C58 H62 109.5 . . ? H60 C58 H62 109.5 . . ? H61 C58 H62 109.5 . . ? C60 C59 C62 109.3(4) . . ? C60 C59 C53 109.2(4) . . ? C62 C59 C53 112.5(4) . . ? C60 C59 C61 109.2(4) . . ? C62 C59 C61 106.8(4) . . ? C53 C59 C61 109.8(4) . . ? C59 C60 H63 109.5 . . ? C59 C60 H64 109.5 . . ? H63 C60 H64 109.5 . . ? C59 C60 H65 109.5 . . ? H63 C60 H65 109.5 . . ? H64 C60 H65 109.5 . . ? C59 C61 H66 109.5 . . ? C59 C61 H67 109.5 . . ? H66 C61 H67 109.5 . . ? C59 C61 H68 109.5 . . ? H66 C61 H68 109.5 . . ? H67 C61 H68 109.5 . . ? C59 C62 H69 109.5 . . ? C59 C62 H70 109.5 . . ? H69 C62 H70 109.5 . . ? C59 C62 H71 109.5 . . ? H69 C62 H71 109.5 . . ? H70 C62 H71 109.5 . . ? N5 C63 C20 124.9(3) . . ? N5 C63 C64 111.6(3) . . ? C20 C63 C64 123.5(3) . . ? C65 C64 C69 119.3(3) . . ? C65 C64 C63 122.0(3) . . ? C69 C64 C63 118.7(3) . . ? C66 C65 C64 120.0(3) . . ? C66 C65 H72 120.0 . . ? C64 C65 H72 120.0 . . ? C67 C66 C65 120.2(3) . . ? C67 C66 H73 119.9 . . ? C65 C66 H73 119.9 . . ? C68 C67 C66 120.1(3) . . ? C68 C67 H74 120.0 . . ? C66 C67 H74 120.0 . . ? C67 C68 C69 120.3(3) . . ? C67 C68 H75 119.9 . . ? C69 C68 H75 119.9 . . ? C68 C69 C64 120.1(3) . . ? C68 C69 H76 119.9 . . ? C64 C69 H76 119.9 . . ? N5 C70 C2 120.1(3) . . ? N5 C70 C79 116.0(4) . . ? C2 C70 C79 123.5(4) . . ? N5 C70 C73 113.6(4) . . ? C2 C70 C73 126.1(4) . . ? C79 C70 C73 11.8(4) . . ? O2 C71 H77 109.5 . . ? O2 C71 H78 109.5 . . ? H77 C71 H78 109.5 . . ? O2 C71 H79 109.5 . . ? H77 C71 H79 109.5 . . ? H78 C71 H79 109.5 . . ? O3 C72 H80 109.5 . . ? O3 C72 H81 109.5 . . ? H80 C72 H81 109.5 . . ? O3 C72 H82 109.5 . . ? H80 C72 H82 109.5 . . ? H81 C72 H82 109.5 . . ? C74 C73 C78 120.0 . . ? C74 C73 C70 120.8(4) . . ? C78 C73 C70 119.0(4) . . ? C73 C74 C75 120.0 . . ? C73 C74 H83 120.0 . . ? C75 C74 H83 120.0 . . ? C76 C75 C74 120.0 . . ? C76 C75 H84 120.0 . . ? C74 C75 H84 120.0 . . ? C77 C76 C75 120.0 . . ? C77 C76 H85 120.0 . . ? C75 C76 H85 120.0 . . ? C76 C77 C78 120.0 . . ? C76 C77 H86 120.0 . . ? C78 C77 H86 120.0 . . ? C77 C78 C73 120.0 . . ? C77 C78 H87 120.0 . . ? C73 C78 H87 120.0 . . ? C80 C79 C84 120.0 . . ? C80 C79 C70 117.7(4) . . ? C84 C79 C70 122.3(4) . . ? C79 C80 C81 120.0 . . ? C79 C80 H88 120.0 . . ? C81 C80 H88 120.0 . . ? C82 C81 C80 120.0 . . ? C82 C81 H89 120.0 . . ? C80 C81 H89 120.0 . . ? C83 C82 C81 120.0 . . ? C83 C82 H90 120.0 . . ? C81 C82 H90 120.0 . . ? C82 C83 C84 120.0 . . ? C82 C83 H91 120.0 . . ? C84 C83 H91 120.0 . . ? C83 C84 C79 120.0 . . ? C83 C84 H92 120.0 . . ? C79 C84 H92 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Zn1 O2 C71 113.4(3) . . . . ? N3 Zn1 O2 C71 -65.4(3) . . . . ? N4 Zn1 O2 C71 -156.5(3) . . . . ? N2 Zn1 O2 C71 24.5(3) . . . . ? N3 Zn1 N1 C1 -103.9(4) . . . . ? N4 Zn1 N1 C1 -19.2(2) . . . . ? N2 Zn1 N1 C1 178.0(2) . . . . ? O2 Zn1 N1 C1 80.7(3) . . . . ? N3 Zn1 N1 C4 92.3(5) . . . . ? N4 Zn1 N1 C4 177.1(2) . . . . ? N2 Zn1 N1 C4 14.3(2) . . . . ? O2 Zn1 N1 C4 -83.0(3) . . . . ? N1 Zn1 N2 C6 -13.7(2) . . . . ? N3 Zn1 N2 C6 -179.7(2) . . . . ? N4 Zn1 N2 C6 -95.4(4) . . . . ? O2 Zn1 N2 C6 81.3(2) . . . . ? N1 Zn1 N2 C9 178.3(2) . . . . ? N3 Zn1 N2 C9 12.3(2) . . . . ? N4 Zn1 N2 C9 96.6(4) . . . . ? O2 Zn1 N2 C9 -86.7(3) . . . . ? N1 Zn1 N3 C14 96.2(5) . . . . ? N4 Zn1 N3 C14 11.5(3) . . . . ? N2 Zn1 N3 C14 174.2(3) . . . . ? O2 Zn1 N3 C14 -88.5(3) . . . . ? N1 Zn1 N3 C11 -95.1(5) . . . . ? N4 Zn1 N3 C11 -179.8(3) . . . . ? N2 Zn1 N3 C11 -17.0(3) . . . . ? O2 Zn1 N3 C11 80.3(3) . . . . ? N1 Zn1 N4 C19 13.2(2) . . . . ? N3 Zn1 N4 C19 179.0(3) . . . . ? N2 Zn1 N4 C19 94.9(4) . . . . ? O2 Zn1 N4 C19 -81.9(3) . . . . ? N1 Zn1 N4 C16 -166.9(2) . . . . ? N3 Zn1 N4 C16 -1.1(2) . . . . ? N2 Zn1 N4 C16 -85.2(4) . . . . ? O2 Zn1 N4 C16 98.0(3) . . . . ? C4 N1 C1 C2 -0.7(3) . . . . ? Zn1 N1 C1 C2 -167.0(2) . . . . ? C4 N1 C1 C20 179.2(3) . . . . ? Zn1 N1 C1 C20 12.8(4) . . . . ? N1 C1 C2 C70 178.4(3) . . . . ? C20 C1 C2 C70 -1.5(4) . . . . ? N1 C1 C2 C3 -2.0(3) . . . . ? C20 C1 C2 C3 178.1(3) . . . . ? C70 C2 C3 O1 4.3(6) . . . . ? C1 C2 C3 O1 -175.2(3) . . . . ? C70 C2 C3 C4 -176.9(3) . . . . ? C1 C2 C3 C4 3.6(3) . . . . ? C1 N1 C4 C5 -175.0(3) . . . . ? Zn1 N1 C4 C5 -9.1(4) . . . . ? C1 N1 C4 C3 3.2(3) . . . . ? Zn1 N1 C4 C3 169.05(19) . . . . ? O1 C3 C4 N1 174.6(3) . . . . ? C2 C3 C4 N1 -4.2(3) . . . . ? O1 C3 C4 C5 -7.2(5) . . . . ? C2 C3 C4 C5 174.0(3) . . . . ? N1 C4 C5 C6 -3.2(5) . . . . ? C3 C4 C5 C6 178.9(3) . . . . ? N1 C4 C5 C21 172.5(3) . . . . ? C3 C4 C5 C21 -5.4(4) . . . . ? C9 N2 C6 C5 177.6(3) . . . . ? Zn1 N2 C6 C5 7.7(4) . . . . ? C9 N2 C6 C7 -0.7(3) . . . . ? Zn1 N2 C6 C7 -170.60(19) . . . . ? C4 C5 C6 N2 3.9(5) . . . . ? C21 C5 C6 N2 -172.0(3) . . . . ? C4 C5 C6 C7 -178.0(3) . . . . ? C21 C5 C6 C7 6.1(4) . . . . ? N2 C6 C7 C8 -0.2(3) . . . . ? C5 C6 C7 C8 -178.5(3) . . . . ? C6 C7 C8 C9 1.0(3) . . . . ? C6 N2 C9 C10 -176.2(3) . . . . ? Zn1 N2 C9 C10 -6.2(4) . . . . ? C6 N2 C9 C8 1.3(3) . . . . ? Zn1 N2 C9 C8 171.3(2) . . . . ? C7 C8 C9 N2 -1.4(3) . . . . ? C7 C8 C9 C10 176.0(3) . . . . ? N2 C9 C10 C11 -1.1(6) . . . . ? C8 C9 C10 C11 -178.2(3) . . . . ? N2 C9 C10 C35 -179.3(3) . . . . ? C8 C9 C10 C35 3.7(5) . . . . ? C14 N3 C11 C10 -172.9(4) . . . . ? Zn1 N3 C11 C10 16.5(5) . . . . ? C14 N3 C11 C12 2.6(4) . . . . ? Zn1 N3 C11 C12 -168.0(3) . . . . ? C9 C10 C11 N3 -4.4(6) . . . . ? C35 C10 C11 N3 173.8(3) . . . . ? C9 C10 C11 C12 -179.3(4) . . . . ? C35 C10 C11 C12 -1.2(6) . . . . ? N3 C11 C12 C13 -2.2(5) . . . . ? C10 C11 C12 C13 173.4(4) . . . . ? C11 C12 C13 C14 0.9(5) . . . . ? C11 N3 C14 C15 174.0(3) . . . . ? Zn1 N3 C14 C15 -15.5(5) . . . . ? C11 N3 C14 C13 -2.1(4) . . . . ? Zn1 N3 C14 C13 168.4(3) . . . . ? C12 C13 C14 N3 0.7(5) . . . . ? C12 C13 C14 C15 -175.4(4) . . . . ? N3 C14 C15 C16 5.7(6) . . . . ? C13 C14 C15 C16 -178.7(4) . . . . ? N3 C14 C15 C49 -174.7(3) . . . . ? C13 C14 C15 C49 0.9(6) . . . . ? C14 C15 C16 N4 6.1(6) . . . . ? C49 C15 C16 N4 -173.5(3) . . . . ? C14 C15 C16 C17 -179.5(3) . . . . ? C49 C15 C16 C17 0.9(5) . . . . ? C19 N4 C16 C15 173.3(3) . . . . ? Zn1 N4 C16 C15 -6.6(5) . . . . ? C19 N4 C16 C17 -1.8(3) . . . . ? Zn1 N4 C16 C17 178.2(2) . . . . ? C15 C16 C17 C18 -174.7(3) . . . . ? N4 C16 C17 C18 0.5(4) . . . . ? C16 C17 C18 C19 1.0(4) . . . . ? C16 N4 C19 C20 -179.0(3) . . . . ? Zn1 N4 C19 C20 0.9(4) . . . . ? C16 N4 C19 C18 2.5(3) . . . . ? Zn1 N4 C19 C18 -177.6(2) . . . . ? C17 C18 C19 N4 -2.2(4) . . . . ? C17 C18 C19 C20 179.3(3) . . . . ? N1 C1 C20 C63 -174.3(3) . . . . ? C2 C1 C20 C63 5.6(4) . . . . ? N1 C1 C20 C19 8.2(5) . . . . ? C2 C1 C20 C19 -172.0(3) . . . . ? N4 C19 C20 C1 -15.5(4) . . . . ? C18 C19 C20 C1 162.8(3) . . . . ? N4 C19 C20 C63 167.1(3) . . . . ? C18 C19 C20 C63 -14.6(5) . . . . ? C4 C5 C21 C22 -72.2(4) . . . . ? C6 C5 C21 C22 103.9(3) . . . . ? C4 C5 C21 C26 112.7(3) . . . . ? C6 C5 C21 C26 -71.2(4) . . . . ? C26 C21 C22 C23 -1.7(5) . . . . ? C5 C21 C22 C23 -176.9(3) . . . . ? C21 C22 C23 C24 1.0(5) . . . . ? C21 C22 C23 C27 178.6(3) . . . . ? C22 C23 C24 C25 0.0(5) . . . . ? C27 C23 C24 C25 -177.6(3) . . . . ? C23 C24 C25 C26 -0.1(5) . . . . ? C23 C24 C25 C31 176.8(3) . . . . ? C22 C21 C26 C25 1.5(5) . . . . ? C5 C21 C26 C25 176.7(3) . . . . ? C24 C25 C26 C21 -0.6(4) . . . . ? C31 C25 C26 C21 -177.6(3) . . . . ? C22 C23 C27 C28 -66.1(5) . . . . ? C24 C23 C27 C28 111.4(4) . . . . ? C22 C23 C27 C30 172.3(3) . . . . ? C24 C23 C27 C30 -10.3(5) . . . . ? C22 C23 C27 C29 52.9(4) . . . . ? C24 C23 C27 C29 -129.6(4) . . . . ? C24 C25 C31 C32 7.5(4) . . . . ? C26 C25 C31 C32 -175.7(3) . . . . ? C24 C25 C31 C33 128.0(3) . . . . ? C26 C25 C31 C33 -55.1(4) . . . . ? C24 C25 C31 C34 -112.4(3) . . . . ? C26 C25 C31 C34 64.4(4) . . . . ? C9 C10 C35 C40 88.7(4) . . . . ? C11 C10 C35 C40 -89.7(4) . . . . ? C9 C10 C35 C36 -93.2(4) . . . . ? C11 C10 C35 C36 88.4(4) . . . . ? C40 C35 C36 C37 0.6(5) . . . . ? C10 C35 C36 C37 -177.5(3) . . . . ? C35 C36 C37 C38 -0.1(5) . . . . ? C35 C36 C37 C41 179.9(3) . . . . ? C36 C37 C38 C39 0.1(5) . . . . ? C41 C37 C38 C39 -179.9(3) . . . . ? C37 C38 C39 C40 -0.6(5) . . . . ? C37 C38 C39 C45 -179.6(4) . . . . ? C36 C35 C40 C39 -1.1(5) . . . . ? C10 C35 C40 C39 177.0(3) . . . . ? C38 C39 C40 C35 1.1(5) . . . . ? C45 C39 C40 C35 -179.9(3) . . . . ? C38 C37 C41 C42 176.9(4) . . . . ? C36 C37 C41 C42 -3.1(6) . . . . ? C38 C37 C41 C44 55.9(5) . . . . ? C36 C37 C41 C44 -124.1(4) . . . . ? C38 C37 C41 C43 -61.1(5) . . . . ? C36 C37 C41 C43 119.0(4) . . . . ? C38 C39 C45 C48 -132.4(4) . . . . ? C40 C39 C45 C48 48.7(5) . . . . ? C38 C39 C45 C47 106.9(5) . . . . ? C40 C39 C45 C47 -72.1(5) . . . . ? C38 C39 C45 C46 -11.4(6) . . . . ? C40 C39 C45 C46 169.6(4) . . . . ? C16 C15 C49 C50 112.0(4) . . . . ? C14 C15 C49 C50 -67.6(4) . . . . ? C16 C15 C49 C54 -69.0(5) . . . . ? C14 C15 C49 C54 111.4(4) . . . . ? C54 C49 C50 C51 -0.4(5) . . . . ? C15 C49 C50 C51 178.6(3) . . . . ? C49 C50 C51 C52 0.0(6) . . . . ? C49 C50 C51 C55 178.5(4) . . . . ? C50 C51 C52 C53 0.7(6) . . . . ? C55 C51 C52 C53 -177.8(4) . . . . ? C51 C52 C53 C54 -1.0(6) . . . . ? C51 C52 C53 C59 -179.9(4) . . . . ? C50 C49 C54 C53 0.1(5) . . . . ? C15 C49 C54 C53 -178.9(3) . . . . ? C52 C53 C54 C49 0.5(5) . . . . ? C59 C53 C54 C49 179.4(4) . . . . ? C52 C51 C55 C57 -49.9(7) . . . . ? C50 C51 C55 C57 131.7(5) . . . . ? C52 C51 C55 C56 -173.6(5) . . . . ? C50 C51 C55 C56 7.9(7) . . . . ? C52 C51 C55 C58 65.9(6) . . . . ? C50 C51 C55 C58 -112.5(5) . . . . ? C52 C53 C59 C60 63.1(5) . . . . ? C54 C53 C59 C60 -115.7(4) . . . . ? C52 C53 C59 C62 -175.3(4) . . . . ? C54 C53 C59 C62 5.8(6) . . . . ? C52 C53 C59 C61 -56.6(5) . . . . ? C54 C53 C59 C61 124.6(4) . . . . ? C70 N5 C63 C20 2.4(5) . . . . ? C70 N5 C63 C64 -175.6(3) . . . . ? C1 C20 C63 N5 -6.3(4) . . . . ? C19 C20 C63 N5 171.3(3) . . . . ? C1 C20 C63 C64 171.5(3) . . . . ? C19 C20 C63 C64 -10.9(4) . . . . ? N5 C63 C64 C65 117.1(3) . . . . ? C20 C63 C64 C65 -60.9(4) . . . . ? N5 C63 C64 C69 -60.5(4) . . . . ? C20 C63 C64 C69 121.4(3) . . . . ? C69 C64 C65 C66 -1.4(5) . . . . ? C63 C64 C65 C66 -179.0(3) . . . . ? C64 C65 C66 C67 -0.5(6) . . . . ? C65 C66 C67 C68 1.4(6) . . . . ? C66 C67 C68 C69 -0.5(6) . . . . ? C67 C68 C69 C64 -1.4(5) . . . . ? C65 C64 C69 C68 2.3(5) . . . . ? C63 C64 C69 C68 -180.0(3) . . . . ? C63 N5 C70 C2 2.3(5) . . . . ? C63 N5 C70 C79 174.8(4) . . . . ? C63 N5 C70 C73 -172.4(4) . . . . ? C1 C2 C70 N5 -2.8(5) . . . . ? C3 C2 C70 N5 177.8(3) . . . . ? C1 C2 C70 C79 -174.7(5) . . . . ? C3 C2 C70 C79 5.9(7) . . . . ? C1 C2 C70 C73 171.3(4) . . . . ? C3 C2 C70 C73 -8.1(7) . . . . ? N5 C70 C73 C74 41.3(6) . . . . ? C2 C70 C73 C74 -133.1(4) . . . . ? C79 C70 C73 C74 145(3) . . . . ? N5 C70 C73 C78 -134.0(4) . . . . ? C2 C70 C73 C78 51.6(6) . . . . ? C79 C70 C73 C78 -30(2) . . . . ? C78 C73 C74 C75 0.0 . . . . ? C70 C73 C74 C75 -175.2(6) . . . . ? C73 C74 C75 C76 0.0 . . . . ? C74 C75 C76 C77 0.0 . . . . ? C75 C76 C77 C78 0.0 . . . . ? C76 C77 C78 C73 0.0 . . . . ? C74 C73 C78 C77 0.0 . . . . ? C70 C73 C78 C77 175.3(6) . . . . ? N5 C70 C79 C80 62.5(6) . . . . ? C2 C70 C79 C80 -125.3(4) . . . . ? C73 C70 C79 C80 -19(2) . . . . ? N5 C70 C79 C84 -119.6(5) . . . . ? C2 C70 C79 C84 52.6(6) . . . . ? C73 C70 C79 C84 159(3) . . . . ? C84 C79 C80 C81 0.0 . . . . ? C70 C79 C80 C81 178.0(6) . . . . ? C79 C80 C81 C82 0.0 . . . . ? C80 C81 C82 C83 0.0 . . . . ? C81 C82 C83 C84 0.0 . . . . ? C82 C83 C84 C79 0.0 . . . . ? C80 C79 C84 C83 0.0 . . . . ? C70 C79 C84 C83 -177.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 1.658 _refine_diff_density_min -0.921 _refine_diff_density_rms 0.087