# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Lindoy, Leonard' _publ_contact_author_name 'Dr Leonard Lindoy' _publ_contact_author_email lindoy@gmail.com _publ_section_title ; Nickel(II) and iron(II) triple helicates assembled from expanded quaterpyridines incorporating flexible linkages ; # Attachment '- combined lindoy.CIF' data_lj189sad _database_code_depnum_ccdc_archive 'CCDC 824369' #TrackingRef '- combined lindoy.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C90 H72 N12 Ni2 O6), (C4 H8 O), 4(P F6), 3.2(H2 O)' _chemical_formula_sum 'C94 H86.4 F24 N12 Ni2 O10.20 P4' _chemical_formula_weight 2244.61 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _Intl_tables_symmetry_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.0800(16) _cell_length_b 15.0530(11) _cell_length_c 32.656(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.778(4) _cell_angle_gamma 90.00 _cell_volume 10918.0(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8912 _cell_measurement_theta_min 2.343 _cell_measurement_theta_max 32.582 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4568 _exptl_absorpt_coefficient_mu 0.502 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.813 _exptl_absorpt_correction_T_max 0.951 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; The crystal was coated in Exxon Paratone N hydrocarbon oil and mounted on a thin mohair fibre attached to a copper pin. Upon mounting on the diffractometer, the crystal was quenched to 150(K) under a cold nitrogen gas stream supplied by an Oxford Cryosystems Cryostream. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type APEXII-FR591 _diffrn_measurement_method \w+\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 111989 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0123 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9594 _reflns_number_gt 8211 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX (Bruker-Nonius, 2003)' _computing_cell_refinement 'SAINT (Bruker-Nonius, 2003)' _computing_data_reduction 'SAINT (Bruker-Nonius, 2003), XPREP (Bruker-Nonius, 2003)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.1 (CCDC, 2005)' _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^)+(0.1529P)^2^+26.7618P] 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 9594 _refine_ls_number_parameters 798 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0735 _refine_ls_wR_factor_ref 0.2345 _refine_ls_wR_factor_gt 0.2180 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.093 _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 C1 C -0.0725(2) 0.2138(3) 0.44028(14) 0.0636(12) Uani 1 1 d . . . H1A H -0.0782 0.1712 0.4168 0.095 Uiso 1 1 calc R . . H1B H -0.0405 0.2558 0.4392 0.095 Uiso 1 1 calc R . . H1C H -0.1101 0.2463 0.4377 0.095 Uiso 1 1 calc R . . C2 C -0.05526(17) 0.1647(3) 0.48199(12) 0.0461(9) Uani 1 1 d . . . C3 C -0.07535(17) 0.0801(3) 0.48709(13) 0.0499(9) Uani 1 1 d . . . H3 H -0.1017 0.0507 0.4636 0.060 Uiso 1 1 calc R . . C4 C -0.05741(17) 0.0380(3) 0.52614(14) 0.0485(9) Uani 1 1 d . . . H4 H -0.0715 -0.0202 0.5295 0.058 Uiso 1 1 calc R . . C5 C -0.01845(15) 0.0814(2) 0.56076(11) 0.0381(7) Uani 1 1 d . . . C6 C -0.01632(17) 0.2037(3) 0.51820(12) 0.0414(8) Uani 1 1 d . . . H6 H -0.0018 0.2619 0.5155 0.050 Uiso 1 1 calc R . . C7 C 0.00363(16) 0.0431(2) 0.60378(12) 0.0399(8) Uani 1 1 d . . . C8 C -0.0111(2) -0.0433(3) 0.61408(14) 0.0515(10) Uani 1 1 d . . . H8 H -0.0359 -0.0806 0.5930 0.062 Uiso 1 1 calc R . . C9 C 0.0109(2) -0.0723(3) 0.65480(16) 0.0586(11) Uani 1 1 d . . . H9 H 0.0003 -0.1299 0.6623 0.070 Uiso 1 1 calc R . . C10 C 0.0487(2) -0.0195(3) 0.68577(13) 0.0488(9) Uani 1 1 d . . . C11 C 0.06151(17) 0.0650(2) 0.67316(12) 0.0416(8) Uani 1 1 d . . . H11 H 0.0868 0.1027 0.6938 0.050 Uiso 1 1 calc R . . C12 C 0.0752(3) -0.0551(3) 0.72961(14) 0.0610(12) Uani 1 1 d . . . H12A H 0.0457 -0.0943 0.7377 0.073 Uiso 1 1 calc R . . H12B H 0.1116 -0.0906 0.7303 0.073 Uiso 1 1 calc R . . C13 C 0.1165(2) -0.0044(3) 0.80094(13) 0.0552(11) Uani 1 1 d . . . C14 C 0.13445(19) 0.0674(3) 0.82821(13) 0.0573(11) Uani 1 1 d . . . C15 C 0.1595(2) 0.0542(5) 0.87192(15) 0.0782(17) Uani 1 1 d . . . H15 H 0.1708 0.1027 0.8910 0.094 Uiso 1 1 calc R . . C16 C 0.1671(3) -0.0372(5) 0.88656(18) 0.095(2) Uani 1 1 d . . . H16 H 0.1847 -0.0489 0.9159 0.114 Uiso 1 1 calc R . . C17 C 0.1501(3) -0.1054(5) 0.85969(19) 0.095(2) Uani 1 1 d . . . H17 H 0.1558 -0.1645 0.8702 0.113 Uiso 1 1 calc R . . C18 C 0.1243(3) -0.0906(4) 0.81705(17) 0.0798(17) Uani 1 1 d . . . H18 H 0.1116 -0.1396 0.7984 0.096 Uiso 1 1 calc R . . C19 C 0.1536(2) 0.2252(3) 0.83203(15) 0.0607(12) Uani 1 1 d . . . H19A H 0.1639 0.2680 0.8121 0.073 Uiso 1 1 calc R . . H19B H 0.1916 0.2065 0.8526 0.073 Uiso 1 1 calc R . . C20 C 0.11426(19) 0.2719(3) 0.85607(12) 0.0490(9) Uani 1 1 d . . . C21 C 0.1313(2) 0.3532(3) 0.87610(14) 0.0578(11) Uani 1 1 d . . . H21 H 0.1689 0.3788 0.8760 0.069 Uiso 1 1 calc R . . C22 C 0.09391(19) 0.3965(3) 0.89600(13) 0.0525(10) Uani 1 1 d . . . H22 H 0.1053 0.4520 0.9096 0.063 Uiso 1 1 calc R . . C23 C 0.03895(17) 0.3572(2) 0.89586(11) 0.0424(8) Uani 1 1 d . . . C24 C 0.06009(18) 0.2364(3) 0.85782(11) 0.0420(8) Uani 1 1 d . . . H24 H 0.0481 0.1807 0.8445 0.050 Uiso 1 1 calc R . . C25 C -0.00603(17) 0.3996(2) 0.91457(12) 0.0430(8) Uani 1 1 d . . . C26 C 0.0006(2) 0.4861(3) 0.93107(15) 0.0598(11) Uani 1 1 d . . . H26 H 0.0355 0.5202 0.9318 0.072 Uiso 1 1 calc R . . C27 C -0.0455(3) 0.5207(3) 0.94640(16) 0.0655(12) Uani 1 1 d . . . H27 H -0.0421 0.5793 0.9576 0.079 Uiso 1 1 calc R . . C28 C -0.0957(2) 0.4710(3) 0.94550(14) 0.0544(10) Uani 1 1 d . . . C29 C -0.09785(18) 0.3852(3) 0.92954(12) 0.0443(8) Uani 1 1 d . . . H29 H -0.1319 0.3496 0.9293 0.053 Uiso 1 1 calc R . . C30 C -0.1472(3) 0.5056(3) 0.96186(18) 0.0738(14) Uani 1 1 d . . . H30A H -0.1330 0.5556 0.9812 0.111 Uiso 1 1 calc R . . H30B H -0.1616 0.4581 0.9771 0.111 Uiso 1 1 calc R . . H30C H -0.1801 0.5255 0.9378 0.111 Uiso 1 1 calc R . . C31 C 0.2143(2) 0.0790(4) 0.52773(18) 0.0720(14) Uani 1 1 d . . . H31A H 0.2263 0.0172 0.5350 0.108 Uiso 1 1 calc R . . H31B H 0.2458 0.1094 0.5182 0.108 Uiso 1 1 calc R . . H31C H 0.1765 0.0801 0.5049 0.108 Uiso 1 1 calc R . . C32 C 0.20534(19) 0.1254(3) 0.56633(15) 0.0559(10) Uani 1 1 d . . . C33 C 0.2536(2) 0.1495(4) 0.60036(19) 0.0757(15) Uani 1 1 d . . . C34 C 0.2441(2) 0.1929(5) 0.6348(2) 0.0799(16) Uani 1 1 d . . . C35 C 0.18549(19) 0.2146(3) 0.63481(14) 0.0536(10) Uani 1 1 d . A . C36 C 0.14803(16) 0.1454(2) 0.56949(12) 0.0421(8) Uani 1 1 d . A . C37 C 0.1710(2) 0.2672(3) 0.66899(14) 0.0627(12) Uani 1 1 d . . . C38 C 0.2052(6) 0.3128(14) 0.7045(5) 0.081(5) Uani 0.50 1 d P A 1 H38 H 0.2477 0.3089 0.7098 0.097 Uiso 0.50 1 calc PR A 1 C39 C 0.1843(9) 0.3631(14) 0.7330(5) 0.084(6) Uani 0.50 1 d P A 1 H39 H 0.2118 0.3964 0.7544 0.101 Uiso 0.50 1 calc PR A 1 C40 C 0.1237(7) 0.3651(10) 0.7303(4) 0.061(5) Uani 0.50 1 d P A 1 C41 C 0.0862(6) 0.3201(12) 0.6985(5) 0.033(3) Uani 0.50 1 d P A 1 H41 H 0.0441 0.3196 0.6953 0.040 Uiso 0.50 1 calc PR A 1 C42 C 0.1017(6) 0.4258(11) 0.7605(4) 0.053(3) Uani 0.50 1 d P A 1 H42A H 0.1196 0.4059 0.7901 0.064 Uiso 0.50 1 calc PR A 1 H42B H 0.1160 0.4871 0.7579 0.064 Uiso 0.50 1 calc PR A 1 O3 O 0.0384(4) 0.4267(4) 0.75211(18) 0.0474(15) Uani 0.50 1 d P . 1 C43 C 0.0059(4) 0.4856(5) 0.7219(2) 0.0433(16) Uani 0.50 1 d P . 1 C45 C -0.0091(5) 0.5960(6) 0.6669(3) 0.059(2) Uani 0.50 1 d P . . H45 H 0.0053 0.6289 0.6468 0.071 Uiso 0.50 1 calc PR . . C44 C 0.0288(4) 0.5352(5) 0.6945(2) 0.0501(18) Uani 0.50 1 d P . . H44 H 0.0696 0.5284 0.6942 0.060 Uiso 0.50 1 calc PR . 1 C38A C 0.2230(6) 0.3210(10) 0.6927(4) 0.059(3) Uani 0.50 1 d P A 2 H38A H 0.2619 0.3180 0.6883 0.071 Uiso 0.50 1 calc PR A 2 C39A C 0.2078(7) 0.3763(8) 0.7219(4) 0.063(3) Uani 0.50 1 d P A 2 H39A H 0.2375 0.4126 0.7402 0.075 Uiso 0.50 1 calc PR A 2 C40A C 0.1473(8) 0.3782(7) 0.7244(3) 0.047(3) Uani 0.50 1 d P A 2 C41A C 0.1061(7) 0.3208(15) 0.6959(7) 0.045(4) Uani 0.50 1 d P A 2 H41A H 0.0664 0.3218 0.6992 0.054 Uiso 0.50 1 calc PR A 2 C42A C 0.1340(6) 0.4418(7) 0.7560(3) 0.057(2) Uani 0.50 1 d P A 2 H42C H 0.1560 0.4240 0.7852 0.068 Uiso 0.50 1 calc PR A 2 H42D H 0.1468 0.5025 0.7507 0.068 Uiso 0.50 1 calc PR A 2 O3A O 0.0743(5) 0.4401(7) 0.7514(3) 0.054(2) Uani 0.50 1 d P A 2 C43A C 0.0544(4) 0.4938(5) 0.7794(2) 0.0477(18) Uani 0.50 1 d P A 2 C44A C 0.0900(4) 0.5548(7) 0.8076(3) 0.059(2) Uani 0.50 1 d P . . H44A H 0.1319 0.5582 0.8100 0.070 Uiso 0.50 1 calc PR A 2 C45A C 0.0665(4) 0.6068(6) 0.8305(3) 0.060(2) Uani 0.50 1 d P . . H45A H 0.0901 0.6538 0.8459 0.072 Uiso 0.50 1 calc PR . . O1W O 0.0000 0.1855(4) 0.7500 0.0909(17) Uani 1 2 d S . . N1 N 0.00154(12) 0.16434(19) 0.55605(9) 0.0365(6) Uani 1 1 d . . . N2 N 0.04023(13) 0.09581(18) 0.63374(9) 0.0367(6) Uani 1 1 d . . . N3 N 0.02319(15) 0.27726(19) 0.87769(10) 0.0407(7) Uani 1 1 d . . . N4 N -0.05452(14) 0.34992(19) 0.91439(9) 0.0388(7) Uani 1 1 d . . . N5 N 0.13775(13) 0.1885(2) 0.60289(9) 0.0400(7) Uani 1 1 d . . . N6 N 0.11257(17) 0.2710(2) 0.66821(10) 0.0483(8) Uani 1 1 d . A . O1 O 0.09086(14) 0.01683(18) 0.75917(9) 0.0531(7) Uani 1 1 d . . . O2 O 0.12589(13) 0.15003(19) 0.80892(8) 0.0515(7) Uani 1 1 d . . . O1T O 0.1902(7) 0.6500(12) 0.7481(4) 0.091(2) Uiso 0.35 1 d PD B 1 C4T C 0.1521(8) 0.6919(13) 0.7123(4) 0.091(2) Uiso 0.35 1 d PD B 1 H4T1 H 0.1634 0.7552 0.7115 0.110 Uiso 0.35 1 calc PR B 1 H4T2 H 0.1098 0.6888 0.7136 0.110 Uiso 0.35 1 calc PR B 1 C1T C 0.2359(8) 0.6224(14) 0.7287(5) 0.091(2) Uiso 0.35 1 d PD B 1 H1T1 H 0.2597 0.5743 0.7461 0.110 Uiso 0.35 1 calc PR B 1 H1T2 H 0.2634 0.6730 0.7291 0.110 Uiso 0.35 1 calc PR B 1 C2T C 0.2135(8) 0.5903(13) 0.6842(5) 0.091(2) Uiso 0.35 1 d PD B 1 H2T1 H 0.2412 0.6050 0.6668 0.110 Uiso 0.35 1 calc PR B 1 H2T2 H 0.2047 0.5258 0.6826 0.110 Uiso 0.35 1 calc PR B 1 C3T C 0.1585(9) 0.6452(13) 0.6734(5) 0.091(2) Uiso 0.35 1 d PD B 1 H3T1 H 0.1229 0.6070 0.6617 0.110 Uiso 0.35 1 calc PR B 1 H3T2 H 0.1608 0.6893 0.6514 0.110 Uiso 0.35 1 calc PR B 1 O3W O 0.0381(11) 0.6936(17) 0.7902(8) 0.069(6) Uiso 0.15 1 d P C 3 O4W O 0.2201(11) 0.2208(16) 0.9482(8) 0.056(6) Uiso 0.15 1 d P D 3 O5W O 0.2998(15) 0.263(2) 1.0097(11) 0.057(7) Uiso 0.10 1 d P E 4 O6W O 0.2719(9) 0.2645(14) 0.9716(7) 0.057(5) Uiso 0.15 1 d P F 5 O7W O 0.3102(15) 0.306(2) 1.0234(10) 0.051(7) Uiso 0.10 1 d P G 6 O8W O 0.2388(11) 0.1974(17) 0.9534(7) 0.058(6) Uiso 0.15 1 d P H 7 O10W O 0.2789(18) 0.312(2) 1.0148(11) 0.064(8) Uiso 0.10 1 d P I 8 O2W O 0.0252(7) 0.7512(12) 0.7750(5) 0.064(4) Uiso 0.20 1 d P . 8 O2T O 0.1837(15) 0.653(3) 0.7362(9) 0.091(2) Uiso 0.15 1 d PD J 9 C5T C 0.1268(15) 0.693(3) 0.7170(11) 0.091(2) Uiso 0.15 1 d PD J 9 H5T1 H 0.1290 0.7581 0.7131 0.110 Uiso 0.15 1 calc PR J 9 H5T2 H 0.0955 0.6782 0.7315 0.110 Uiso 0.15 1 calc PR J 9 C6T C 0.1217(18) 0.642(3) 0.6777(12) 0.091(2) Uiso 0.15 1 d PD J 9 H6T1 H 0.0969 0.6761 0.6533 0.110 Uiso 0.15 1 calc PR J 9 H6T2 H 0.0999 0.5858 0.6794 0.110 Uiso 0.15 1 calc PR J 9 C7T C 0.1801(16) 0.619(4) 0.6688(12) 0.091(2) Uiso 0.15 1 d PD J 9 H7T1 H 0.1802 0.5571 0.6587 0.110 Uiso 0.15 1 calc PR J 9 H7T2 H 0.1888 0.6599 0.6474 0.110 Uiso 0.15 1 calc PR J 9 C8T C 0.2235(15) 0.631(3) 0.7110(11) 0.091(2) Uiso 0.15 1 d PD J 9 H8T1 H 0.2462 0.5763 0.7211 0.110 Uiso 0.15 1 calc PR J 9 H8T2 H 0.2520 0.6804 0.7107 0.110 Uiso 0.15 1 calc PR J 9 F1 F 0.06048(18) 0.2679(2) 0.40987(10) 0.0892(11) Uani 1 1 d . . . F2 F 0.15542(13) 0.29635(18) 0.49985(9) 0.0663(7) Uani 1 1 d . . . F3 F 0.05752(12) 0.33188(17) 0.47265(9) 0.0607(6) Uani 1 1 d . . . F4 F 0.08820(14) 0.18864(16) 0.47023(8) 0.0652(7) Uani 1 1 d . . . F5 F 0.15920(17) 0.2353(2) 0.43832(11) 0.0844(10) Uani 1 1 d . . . F6 F 0.12590(13) 0.37825(17) 0.43909(9) 0.0656(7) Uani 1 1 d . . . F7 F 0.15446(19) 0.9773(4) 0.62122(15) 0.0863(15) Uani 0.70 1 d P K 1 F8 F 0.2450(2) 0.8456(3) 0.68345(19) 0.0987(17) Uani 0.70 1 d P K 1 F9 F 0.1953(2) 0.9682(4) 0.69362(15) 0.0839(13) Uani 0.70 1 d P K 1 F10 F 0.2576(2) 0.9732(4) 0.6516(2) 0.0941(16) Uani 0.70 1 d P K 1 F11 F 0.2059(2) 0.8508(5) 0.6153(2) 0.114(2) Uani 0.70 1 d P K 1 F12 F 0.14333(18) 0.8565(3) 0.65543(14) 0.0744(11) Uani 0.70 1 d P K 1 F7A F 0.2128(5) 0.9409(9) 0.6037(4) 0.090(3) Uiso 0.30 1 d P K 2 F8A F 0.1925(5) 0.9091(9) 0.6932(4) 0.079(3) Uiso 0.30 1 d P K 2 F9A F 0.2735(6) 0.9314(9) 0.6691(4) 0.088(3) Uiso 0.30 1 d P K 2 F10A F 0.1324(8) 0.9210(13) 0.6273(6) 0.127(5) Uiso 0.30 1 d P K 2 F11A F 0.2212(9) 0.8295(13) 0.6483(7) 0.133(6) Uiso 0.30 1 d P K 2 F12A F 0.1924(7) 1.0300(11) 0.6557(5) 0.117(4) Uiso 0.30 1 d P K 2 P1 P 0.10784(6) 0.28276(7) 0.45478(4) 0.0534(3) Uani 1 1 d . . . P2 P 0.20130(5) 0.91847(10) 0.65165(4) 0.0670(4) Uani 1 1 d . . . Ni1 Ni 0.054832(19) 0.22219(3) 0.611960(13) 0.03443(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.066(3) 0.070(3) 0.044(2) -0.006(2) -0.003(2) -0.015(2) C2 0.0413(18) 0.051(2) 0.044(2) -0.0100(17) 0.0081(15) -0.0071(16) C3 0.0428(19) 0.054(2) 0.047(2) -0.0146(18) 0.0025(16) -0.0113(17) C4 0.048(2) 0.0375(19) 0.061(2) -0.0117(17) 0.0157(18) -0.0128(16) C5 0.0371(16) 0.0367(17) 0.0447(19) -0.0094(15) 0.0183(15) -0.0064(14) C6 0.0448(19) 0.0416(18) 0.0371(19) -0.0034(15) 0.0101(15) -0.0111(15) C7 0.0457(18) 0.0308(17) 0.050(2) -0.0073(15) 0.0242(16) -0.0031(14) C8 0.066(2) 0.039(2) 0.055(2) -0.0061(17) 0.026(2) -0.0116(18) C9 0.085(3) 0.0307(19) 0.071(3) 0.0003(18) 0.040(2) -0.0058(19) C10 0.068(2) 0.041(2) 0.048(2) 0.0024(16) 0.0337(19) 0.0062(18) C11 0.056(2) 0.0333(17) 0.0409(19) -0.0014(14) 0.0228(16) 0.0028(15) C12 0.101(3) 0.039(2) 0.055(2) 0.0078(18) 0.041(2) 0.010(2) C13 0.070(3) 0.060(3) 0.044(2) 0.0149(19) 0.0307(19) 0.022(2) C14 0.054(2) 0.082(3) 0.042(2) 0.024(2) 0.0243(18) 0.025(2) C15 0.076(3) 0.124(5) 0.039(2) 0.020(3) 0.023(2) 0.038(3) C16 0.099(4) 0.143(6) 0.051(3) 0.052(4) 0.036(3) 0.062(4) C17 0.141(6) 0.099(4) 0.060(3) 0.037(3) 0.055(4) 0.062(4) C18 0.116(4) 0.074(3) 0.062(3) 0.032(3) 0.046(3) 0.038(3) C19 0.053(2) 0.085(3) 0.050(2) -0.005(2) 0.024(2) -0.003(2) C20 0.052(2) 0.064(3) 0.0326(19) 0.0019(17) 0.0135(16) -0.0009(18) C21 0.051(2) 0.076(3) 0.047(2) -0.007(2) 0.0157(18) -0.014(2) C22 0.056(2) 0.055(2) 0.047(2) -0.0064(18) 0.0138(18) -0.0119(19) C23 0.053(2) 0.0418(19) 0.0331(17) 0.0045(15) 0.0120(15) -0.0007(16) C24 0.053(2) 0.0428(19) 0.0337(18) 0.0028(15) 0.0175(16) 0.0037(16) C25 0.053(2) 0.0377(18) 0.0374(18) 0.0022(15) 0.0112(16) 0.0001(16) C26 0.077(3) 0.042(2) 0.066(3) -0.007(2) 0.028(2) -0.009(2) C27 0.094(3) 0.039(2) 0.068(3) -0.009(2) 0.030(3) 0.005(2) C28 0.074(3) 0.040(2) 0.053(2) -0.0003(17) 0.025(2) 0.0090(19) C29 0.055(2) 0.0401(19) 0.0400(19) 0.0071(15) 0.0161(16) 0.0128(16) C30 0.098(4) 0.051(3) 0.086(4) -0.005(2) 0.047(3) 0.019(3) C31 0.057(3) 0.085(3) 0.086(3) -0.009(3) 0.039(3) 0.004(2) C32 0.048(2) 0.057(2) 0.066(3) 0.002(2) 0.023(2) -0.0052(19) C33 0.043(2) 0.095(4) 0.087(4) -0.002(3) 0.014(2) -0.008(2) C34 0.046(2) 0.101(4) 0.086(4) -0.009(3) 0.004(2) -0.016(3) C35 0.045(2) 0.055(2) 0.054(2) -0.0027(19) 0.0005(18) -0.0116(17) C36 0.0409(18) 0.0421(19) 0.045(2) 0.0022(16) 0.0149(15) -0.0028(15) C37 0.071(3) 0.058(3) 0.043(2) -0.0057(19) -0.013(2) -0.006(2) C38 0.043(7) 0.143(14) 0.058(9) -0.028(9) 0.016(5) -0.027(7) C39 0.074(11) 0.143(15) 0.032(7) -0.033(8) 0.010(6) -0.057(10) C40 0.066(8) 0.088(9) 0.033(6) 0.000(5) 0.022(5) -0.037(6) C41 0.048(7) 0.036(4) 0.018(4) -0.004(3) 0.013(5) 0.007(6) C42 0.034(7) 0.096(10) 0.031(5) -0.016(5) 0.011(5) -0.025(7) O3 0.068(5) 0.045(3) 0.032(3) 0.006(2) 0.019(3) 0.000(3) C43 0.066(5) 0.038(4) 0.024(3) -0.003(3) 0.010(3) -0.006(3) C45 0.089(7) 0.042(4) 0.042(4) 0.020(3) 0.009(4) -0.004(4) C44 0.075(5) 0.043(4) 0.035(4) 0.004(3) 0.018(4) -0.007(4) C38A 0.046(7) 0.081(7) 0.048(7) -0.021(5) 0.007(5) -0.005(6) C39A 0.074(8) 0.061(6) 0.041(6) -0.016(5) -0.005(5) -0.011(6) C40A 0.069(9) 0.040(5) 0.020(5) -0.002(4) -0.009(6) -0.001(6) C41A 0.048(8) 0.056(6) 0.036(6) 0.006(4) 0.020(6) 0.019(7) C42A 0.071(7) 0.057(5) 0.038(5) -0.009(4) 0.006(5) 0.002(5) O3A 0.049(7) 0.072(5) 0.042(4) -0.027(4) 0.013(5) -0.008(5) C43A 0.065(5) 0.044(4) 0.032(4) -0.009(3) 0.008(3) -0.001(4) C44A 0.058(5) 0.075(6) 0.038(4) -0.009(4) 0.005(4) 0.005(4) C45A 0.075(6) 0.042(4) 0.056(5) -0.033(4) 0.004(4) 0.013(4) O1W 0.085(4) 0.078(4) 0.098(4) 0.000 0.004(3) 0.000 N1 0.0358(14) 0.0368(15) 0.0393(15) -0.0071(12) 0.0141(12) -0.0079(11) N2 0.0477(16) 0.0309(14) 0.0369(15) -0.0046(11) 0.0207(13) -0.0012(12) N3 0.0543(18) 0.0376(16) 0.0334(15) 0.0062(12) 0.0176(13) 0.0040(13) N4 0.0498(16) 0.0354(15) 0.0299(14) 0.0058(11) 0.0089(12) 0.0078(13) N5 0.0409(15) 0.0403(16) 0.0360(15) -0.0004(12) 0.0060(12) -0.0075(13) N6 0.071(2) 0.0391(17) 0.0288(16) 0.0004(13) 0.0038(15) 0.0006(15) O1 0.0783(19) 0.0431(15) 0.0420(14) 0.0116(12) 0.0233(13) 0.0149(14) O2 0.0632(17) 0.0580(17) 0.0365(13) 0.0037(12) 0.0192(12) 0.0076(13) F1 0.126(3) 0.085(2) 0.0512(16) 0.0044(14) 0.0157(17) -0.038(2) F2 0.0752(17) 0.0553(14) 0.0677(17) -0.0055(12) 0.0185(14) -0.0062(13) F3 0.0668(15) 0.0536(14) 0.0704(16) 0.0027(12) 0.0332(13) -0.0018(11) F4 0.098(2) 0.0414(13) 0.0603(15) -0.0041(11) 0.0290(14) -0.0147(13) F5 0.121(3) 0.0612(17) 0.092(2) -0.0138(15) 0.066(2) 0.0016(17) F6 0.0807(17) 0.0503(14) 0.0780(18) 0.0026(13) 0.0426(15) -0.0085(12) F7 0.059(2) 0.122(4) 0.078(3) 0.053(3) 0.019(2) 0.034(3) F8 0.065(3) 0.080(3) 0.118(4) 0.000(3) -0.030(3) 0.023(2) F9 0.076(3) 0.102(4) 0.070(3) -0.035(3) 0.013(2) -0.007(3) F10 0.059(2) 0.079(3) 0.147(5) 0.014(3) 0.033(3) 0.008(2) F11 0.055(2) 0.177(6) 0.105(4) -0.081(4) 0.013(2) 0.007(3) F12 0.058(2) 0.083(3) 0.074(3) -0.010(2) 0.0060(19) -0.002(2) P1 0.0751(8) 0.0407(6) 0.0521(6) -0.0059(4) 0.0305(6) -0.0092(5) P2 0.0537(7) 0.0827(9) 0.0537(7) -0.0110(6) -0.0041(5) 0.0205(6) Ni1 0.0435(3) 0.0313(3) 0.0298(3) -0.00380(15) 0.0122(2) -0.00618(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.505(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.380(6) . ? C2 C6 1.404(5) . ? C3 C4 1.383(6) . ? C3 H3 0.9500 . ? C4 C5 1.400(5) . ? C4 H4 0.9500 . ? C5 N1 1.354(5) . ? C5 C7 1.475(5) . ? C6 N1 1.331(5) . ? C6 H6 0.9500 . ? C7 N2 1.361(5) . ? C7 C8 1.407(5) . ? C8 C9 1.360(6) . ? C8 H8 0.9500 . ? C9 C10 1.391(6) . ? C9 H9 0.9500 . ? C10 C11 1.393(5) . ? C10 C12 1.494(6) . ? C11 N2 1.330(5) . ? C11 H11 0.9500 . ? C12 O1 1.430(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O1 1.369(5) . ? C13 C14 1.390(7) . ? C13 C18 1.393(7) . ? C14 O2 1.385(5) . ? C14 C15 1.401(6) . ? C15 C16 1.451(9) . ? C15 H15 0.9500 . ? C16 C17 1.338(10) . ? C16 H16 0.9500 . ? C17 C18 1.376(8) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 O2 1.413(6) . ? C19 C20 1.523(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C24 1.375(6) . ? C20 C21 1.393(6) . ? C21 C22 1.378(6) . ? C21 H21 0.9500 . ? C22 C23 1.398(6) . ? C22 H22 0.9500 . ? C23 N3 1.348(5) . ? C23 C25 1.484(5) . ? C24 N3 1.351(5) . ? C24 H24 0.9500 . ? C25 N4 1.344(5) . ? C25 C26 1.402(6) . ? C26 C27 1.393(7) . ? C26 H26 0.9500 . ? C27 C28 1.374(7) . ? C27 H27 0.9500 . ? C28 C29 1.388(6) . ? C28 C30 1.521(6) . ? C29 N4 1.340(5) . ? C29 H29 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.503(7) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C36 1.388(6) . ? C32 C33 1.390(7) . ? C33 C34 1.370(8) . ? C34 C35 1.392(7) . ? C35 N5 1.353(5) . ? C35 C37 1.479(7) . ? C36 N5 1.344(5) . ? C37 N6 1.343(7) . ? C37 C38 1.394(17) . ? C37 C38A 1.479(14) . ? C38 C39 1.38(2) . ? C38 H38 0.9500 . ? C39 C40 1.38(2) . ? C39 H39 0.9500 . ? C40 C41 1.34(2) . ? C40 C42 1.53(2) . ? C41 N6 1.491(15) . ? C41 H41 0.9500 . ? C42 O3 1.412(13) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? O3 C43 1.385(9) . ? O3 C43 1.738(10) 2_556 ? O3 O3 1.741(17) 2_556 ? C43 C44 1.378(11) . ? C43 O3 1.738(10) 2_556 ? C45 C45A 1.360(14) 2_556 ? C45 C44 1.410(12) . ? C45 H45 0.9500 . ? C44 H44 0.9500 . ? C38A C39A 1.382(19) . ? C38A H38A 0.9500 . ? C39A C40A 1.42(2) . ? C39A H39A 0.9500 . ? C40A C41A 1.43(3) . ? C40A C42A 1.500(15) . ? C41A N6 1.22(2) . ? C41A H41A 0.9500 . ? C42A O3A 1.345(13) . ? C42A H42C 0.9900 . ? C42A H42D 0.9900 . ? O3A C43A 1.387(11) . ? C43A C44A 1.397(12) . ? C44A C45A 1.300(12) . ? C44A H44A 0.9500 . ? C45A C45 1.360(14) 2_556 ? C45A H45A 0.9500 . ? N1 Ni1 2.094(3) . ? N2 Ni1 2.090(3) . ? N3 Ni1 2.092(3) 2_556 ? N4 Ni1 2.106(3) 2_556 ? N5 Ni1 2.077(3) . ? N6 Ni1 2.088(3) . ? O1T C4T 1.408(10) . ? O1T C1T 1.431(10) . ? C4T C3T 1.493(10) . ? C4T H4T1 0.9900 . ? C4T H4T2 0.9900 . ? C1T C2T 1.483(10) . ? C1T H1T1 0.9900 . ? C1T H1T2 0.9900 . ? C2T C3T 1.476(10) . ? C2T H2T1 0.9900 . ? C2T H2T2 0.9900 . ? C3T H3T1 0.9900 . ? C3T H3T2 0.9900 . ? O2W O2W 1.73(3) 2_556 ? O2T C5T 1.423(10) . ? O2T C8T 1.428(10) . ? C5T C6T 1.477(10) . ? C5T H5T1 0.9900 . ? C5T H5T2 0.9900 . ? C6T C7T 1.493(10) . ? C6T H6T1 0.9900 . ? C6T H6T2 0.9900 . ? C7T C8T 1.479(10) . ? C7T H7T1 0.9900 . ? C7T H7T2 0.9900 . ? C8T H8T1 0.9900 . ? C8T H8T2 0.9900 . ? F1 P1 1.589(3) . ? F2 P1 1.592(3) . ? F3 P1 1.614(3) . ? F4 P1 1.610(3) . ? F5 P1 1.597(3) . ? F6 P1 1.618(3) . ? F7 P2 1.535(4) . ? F8 P2 1.652(4) . ? F9 P2 1.601(4) . ? F10 P2 1.539(5) . ? F11 P2 1.590(5) . ? F12 P2 1.663(5) . ? F7A P2 1.693(13) . ? F8A P2 1.433(12) . ? F9A P2 1.620(13) . ? F10A P2 1.572(17) . ? F11A P2 1.43(2) . ? F12A P2 1.701(16) . ? Ni1 N3 2.092(3) 2_556 ? Ni1 N4 2.106(3) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C6 116.3(4) . . ? C3 C2 C1 123.2(4) . . ? C6 C2 C1 120.5(4) . . ? C2 C3 C4 120.5(3) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 119.7(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 120.1(3) . . ? N1 C5 C7 115.4(3) . . ? C4 C5 C7 124.5(3) . . ? N1 C6 C2 124.1(3) . . ? N1 C6 H6 117.9 . . ? C2 C6 H6 117.9 . . ? N2 C7 C8 120.7(4) . . ? N2 C7 C5 116.3(3) . . ? C8 C7 C5 123.0(3) . . ? C9 C8 C7 118.7(4) . . ? C9 C8 H8 120.7 . . ? C7 C8 H8 120.7 . . ? C8 C9 C10 121.4(4) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C9 C10 C11 116.6(4) . . ? C9 C10 C12 120.3(4) . . ? C11 C10 C12 123.1(4) . . ? N2 C11 C10 123.5(4) . . ? N2 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? O1 C12 C10 109.8(3) . . ? O1 C12 H12A 109.7 . . ? C10 C12 H12A 109.7 . . ? O1 C12 H12B 109.7 . . ? C10 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? O1 C13 C14 115.4(4) . . ? O1 C13 C18 124.8(5) . . ? C14 C13 C18 119.8(4) . . ? O2 C14 C13 115.2(3) . . ? O2 C14 C15 124.0(5) . . ? C13 C14 C15 120.8(5) . . ? C14 C15 C16 116.7(6) . . ? C14 C15 H15 121.6 . . ? C16 C15 H15 121.6 . . ? C17 C16 C15 121.5(5) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 C18 120.6(6) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C13 120.6(6) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? O2 C19 C20 113.5(4) . . ? O2 C19 H19A 108.9 . . ? C20 C19 H19A 108.9 . . ? O2 C19 H19B 108.9 . . ? C20 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? C24 C20 C21 117.8(4) . . ? C24 C20 C19 121.2(4) . . ? C21 C20 C19 121.0(4) . . ? C22 C21 C20 120.2(4) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 118.9(4) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? N3 C23 C22 121.0(4) . . ? N3 C23 C25 115.4(3) . . ? C22 C23 C25 123.6(4) . . ? N3 C24 C20 122.8(4) . . ? N3 C24 H24 118.6 . . ? C20 C24 H24 118.6 . . ? N4 C25 C26 121.4(4) . . ? N4 C25 C23 115.7(3) . . ? C26 C25 C23 122.8(4) . . ? C27 C26 C25 118.2(4) . . ? C27 C26 H26 120.9 . . ? C25 C26 H26 120.9 . . ? C28 C27 C26 120.7(4) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 117.3(4) . . ? C27 C28 C30 122.7(4) . . ? C29 C28 C30 120.0(4) . . ? N4 C29 C28 123.6(4) . . ? N4 C29 H29 118.2 . . ? C28 C29 H29 118.2 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C36 C32 C33 117.2(4) . . ? C36 C32 C31 120.9(4) . . ? C33 C32 C31 121.9(4) . . ? C34 C33 C32 120.6(5) . . ? C33 C34 C35 119.0(5) . . ? N5 C35 C34 121.3(4) . . ? N5 C35 C37 115.7(4) . . ? C34 C35 C37 123.0(4) . . ? N5 C36 C32 123.2(4) . . ? N6 C37 C38 109.5(7) . . ? N6 C37 C35 116.1(4) . . ? C38 C37 C35 134.3(8) . . ? C39 C38 C37 127.3(12) . . ? C39 C38 H38 116.3 . . ? C37 C38 H38 116.3 . . ? C40 C39 C38 120.3(13) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C41 C40 C39 117.8(14) . . ? C41 C40 C42 123.1(12) . . ? C39 C40 C42 118.8(14) . . ? C40 C41 N6 118.1(11) . . ? C40 C41 H41 120.9 . . ? N6 C41 H41 120.9 . . ? O3 C42 C40 112.8(10) . . ? O3 C42 H42A 109.0 . . ? C40 C42 H42A 109.0 . . ? O3 C42 H42B 109.0 . . ? C40 C42 H42B 109.0 . . ? H42A C42 H42B 107.8 . . ? C43 O3 C42 118.4(8) . . ? C43 O3 C43 75.2(6) . 2_556 ? C42 O3 C43 128.7(8) . 2_556 ? C43 O3 O3 66.4(5) . 2_556 ? C42 O3 O3 173.6(8) . 2_556 ? C43 O3 O3 46.9(4) 2_556 2_556 ? C44 C43 O3 125.4(8) . . ? C44 C43 O3 167.1(7) . 2_556 ? O3 C43 O3 66.6(6) . 2_556 ? C45A C45 C44 118.8(8) 2_556 . ? C45A C45 H45 120.6 2_556 . ? C44 C45 H45 120.6 . . ? C43 C44 C45 119.1(9) . . ? C43 C44 H44 120.4 . . ? C45 C44 H44 120.4 . . ? C39A C38A C37 111.7(11) . . ? C39A C38A H38A 124.2 . . ? C37 C38A H38A 124.2 . . ? C38A C39A C40A 119.2(11) . . ? C38A C39A H39A 120.4 . . ? C40A C39A H39A 120.4 . . ? C39A C40A C41A 116.4(11) . . ? C39A C40A C42A 116.1(12) . . ? C41A C40A C42A 127.5(15) . . ? N6 C41A C40A 131.5(12) . . ? N6 C41A H41A 114.3 . . ? C40A C41A H41A 114.3 . . ? O3A C42A C40A 107.9(10) . . ? O3A C42A H42C 110.1 . . ? C40A C42A H42C 110.1 . . ? O3A C42A H42D 110.1 . . ? C40A C42A H42D 110.1 . . ? H42C C42A H42D 108.4 . . ? C42A O3A C43A 115.4(9) . . ? O3A C43A C44A 125.2(9) . . ? C45A C44A C43A 120.9(9) . . ? C45A C44A H44A 119.6 . . ? C43A C44A H44A 119.6 . . ? C44A C45A C45 122.1(8) . 2_556 ? C44A C45A H45A 119.0 . . ? C45 C45A H45A 119.0 2_556 . ? C6 N1 C5 119.1(3) . . ? C6 N1 Ni1 125.8(2) . . ? C5 N1 Ni1 115.0(2) . . ? C11 N2 C7 119.1(3) . . ? C11 N2 Ni1 126.5(2) . . ? C7 N2 Ni1 114.3(2) . . ? C23 N3 C24 119.3(3) . . ? C23 N3 Ni1 115.1(2) . 2_556 ? C24 N3 Ni1 125.4(3) . 2_556 ? C29 N4 C25 118.8(3) . . ? C29 N4 Ni1 126.4(3) . 2_556 ? C25 N4 Ni1 114.8(2) . 2_556 ? C36 N5 C35 118.6(3) . . ? C36 N5 Ni1 127.3(2) . . ? C35 N5 Ni1 114.1(3) . . ? C41A N6 C37 109.8(8) . . ? C37 N6 C41 126.7(7) . . ? C41A N6 Ni1 133.9(8) . . ? C37 N6 Ni1 113.5(3) . . ? C41 N6 Ni1 118.7(7) . . ? C13 O1 C12 117.2(3) . . ? C14 O2 C19 119.3(3) . . ? C4T O1T C1T 97.5(14) . . ? O1T C4T C3T 108.1(14) . . ? O1T C4T H4T1 110.1 . . ? C3T C4T H4T1 110.1 . . ? O1T C4T H4T2 110.1 . . ? C3T C4T H4T2 110.1 . . ? H4T1 C4T H4T2 108.4 . . ? O1T C1T C2T 115.2(15) . . ? O1T C1T H1T1 108.5 . . ? C2T C1T H1T1 108.5 . . ? O1T C1T H1T2 108.5 . . ? C2T C1T H1T2 108.5 . . ? H1T1 C1T H1T2 107.5 . . ? C3T C2T C1T 95.8(14) . . ? C3T C2T H2T1 112.6 . . ? C1T C2T H2T1 112.6 . . ? C3T C2T H2T2 112.6 . . ? C1T C2T H2T2 112.6 . . ? H2T1 C2T H2T2 110.1 . . ? C2T C3T C4T 109.7(14) . . ? C2T C3T H3T1 109.7 . . ? C4T C3T H3T1 109.7 . . ? C2T C3T H3T2 109.7 . . ? C4T C3T H3T2 109.7 . . ? H3T1 C3T H3T2 108.2 . . ? C5T O2T C8T 120.4(17) . . ? O2T C5T C6T 90(3) . . ? O2T C5T H5T1 113.6 . . ? C6T C5T H5T1 113.6 . . ? O2T C5T H5T2 113.6 . . ? C6T C5T H5T2 113.6 . . ? H5T1 C5T H5T2 110.8 . . ? C5T C6T C7T 115(3) . . ? C5T C6T H6T1 108.5 . . ? C7T C6T H6T1 108.5 . . ? C5T C6T H6T2 108.5 . . ? C7T C6T H6T2 108.5 . . ? H6T1 C6T H6T2 107.5 . . ? C8T C7T C6T 102(3) . . ? C8T C7T H7T1 111.4 . . ? C6T C7T H7T1 111.4 . . ? C8T C7T H7T2 111.4 . . ? C6T C7T H7T2 111.4 . . ? H7T1 C7T H7T2 109.2 . . ? O2T C8T C7T 101(2) . . ? O2T C8T H8T1 111.6 . . ? C7T C8T H8T1 111.6 . . ? O2T C8T H8T2 111.6 . . ? C7T C8T H8T2 111.6 . . ? H8T1 C8T H8T2 109.4 . . ? F1 P1 F2 179.31(19) . . ? F1 P1 F5 90.8(2) . . ? F2 P1 F5 88.86(19) . . ? F1 P1 F4 89.09(16) . . ? F2 P1 F4 90.32(15) . . ? F5 P1 F4 90.57(16) . . ? F1 P1 F3 90.91(19) . . ? F2 P1 F3 89.43(15) . . ? F5 P1 F3 178.2(2) . . ? F4 P1 F3 89.90(15) . . ? F1 P1 F6 90.24(16) . . ? F2 P1 F6 90.36(16) . . ? F5 P1 F6 90.69(16) . . ? F4 P1 F6 178.58(17) . . ? F3 P1 F6 88.86(14) . . ? F11A P2 F8A 96.3(10) . . ? F11A P2 F7 132.5(10) . . ? F8A P2 F7 114.4(5) . . ? F11A P2 F10 102.3(8) . . ? F8A P2 F10 113.1(6) . . ? F7 P2 F10 97.8(3) . . ? F11A P2 F10A 106.6(11) . . ? F8A P2 F10A 95.6(9) . . ? F10 P2 F10A 136.4(8) . . ? F8A P2 F11 134.4(6) . . ? F7 P2 F11 93.7(4) . . ? F10 P2 F11 96.6(3) . . ? F10A P2 F11 84.3(7) . . ? F11A P2 F9 127.4(9) . . ? F7 P2 F9 94.3(3) . . ? F10 P2 F9 91.2(3) . . ? F10A P2 F9 96.4(7) . . ? F11 P2 F9 168.0(4) . . ? F11A P2 F9A 79.5(10) . . ? F8A P2 F9A 94.4(7) . . ? F7 P2 F9A 129.4(6) . . ? F10A P2 F9A 167.6(9) . . ? F11 P2 F9A 93.9(5) . . ? F9 P2 F9A 87.9(5) . . ? F8A P2 F8 63.8(5) . . ? F7 P2 F8 172.8(3) . . ? F10 P2 F8 89.1(3) . . ? F10A P2 F8 134.0(8) . . ? F11 P2 F8 83.7(3) . . ? F9 P2 F8 87.3(3) . . ? F9A P2 F8 57.6(5) . . ? F11A P2 F12 76.2(8) . . ? F8A P2 F12 63.2(5) . . ? F7 P2 F12 86.1(2) . . ? F10 P2 F12 175.6(3) . . ? F10A P2 F12 47.8(7) . . ? F11 P2 F12 85.1(3) . . ? F9 P2 F12 86.5(3) . . ? F9A P2 F12 144.4(5) . . ? F8 P2 F12 87.0(3) . . ? F11A P2 F7A 89.0(9) . . ? F8A P2 F7A 174.1(7) . . ? F7 P2 F7A 63.0(4) . . ? F10 P2 F7A 63.0(5) . . ? F10A P2 F7A 85.3(8) . . ? F11 P2 F7A 51.5(5) . . ? F9 P2 F7A 140.5(5) . . ? F9A P2 F7A 84.0(6) . . ? F8 P2 F7A 119.4(5) . . ? F12 P2 F7A 120.8(5) . . ? F11A P2 F12A 168.2(10) . . ? F8A P2 F12A 88.4(8) . . ? F7 P2 F12A 53.3(6) . . ? F10 P2 F12A 65.9(6) . . ? F10A P2 F12A 83.6(9) . . ? F11 P2 F12A 136.4(7) . . ? F9 P2 F12A 55.3(6) . . ? F9A P2 F12A 89.4(7) . . ? F8 P2 F12A 132.3(6) . . ? F12 P2 F12A 115.5(6) . . ? F7A P2 F12A 85.9(7) . . ? N5 Ni1 N6 79.57(13) . . ? N5 Ni1 N2 93.80(12) . . ? N6 Ni1 N2 98.29(12) . . ? N5 Ni1 N3 170.66(12) . 2_556 ? N6 Ni1 N3 95.16(14) . 2_556 ? N2 Ni1 N3 94.60(11) . 2_556 ? N5 Ni1 N1 96.88(11) . . ? N6 Ni1 N1 175.37(12) . . ? N2 Ni1 N1 78.89(11) . . ? N3 Ni1 N1 88.76(11) 2_556 . ? N5 Ni1 N4 93.76(12) . 2_556 ? N6 Ni1 N4 88.20(12) . 2_556 ? N2 Ni1 N4 170.81(12) . 2_556 ? N3 Ni1 N4 78.27(12) 2_556 2_556 ? N1 Ni1 N4 95.02(11) . 2_556 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C2 C3 C4 0.1(6) . . . . ? C1 C2 C3 C4 179.3(4) . . . . ? C2 C3 C4 C5 -0.1(6) . . . . ? C3 C4 C5 N1 0.1(6) . . . . ? C3 C4 C5 C7 -180.0(3) . . . . ? C3 C2 C6 N1 -0.1(6) . . . . ? C1 C2 C6 N1 -179.3(4) . . . . ? N1 C5 C7 N2 1.3(4) . . . . ? C4 C5 C7 N2 -178.6(3) . . . . ? N1 C5 C7 C8 -178.1(3) . . . . ? C4 C5 C7 C8 2.0(6) . . . . ? N2 C7 C8 C9 1.4(6) . . . . ? C5 C7 C8 C9 -179.3(4) . . . . ? C7 C8 C9 C10 -1.8(6) . . . . ? C8 C9 C10 C11 1.6(6) . . . . ? C8 C9 C10 C12 -176.4(4) . . . . ? C9 C10 C11 N2 -0.9(6) . . . . ? C12 C10 C11 N2 177.0(4) . . . . ? C9 C10 C12 O1 -156.6(4) . . . . ? C11 C10 C12 O1 25.6(6) . . . . ? O1 C13 C14 O2 -2.3(5) . . . . ? C18 C13 C14 O2 178.7(4) . . . . ? O1 C13 C14 C15 177.9(4) . . . . ? C18 C13 C14 C15 -1.0(7) . . . . ? O2 C14 C15 C16 -177.9(4) . . . . ? C13 C14 C15 C16 1.9(7) . . . . ? C14 C15 C16 C17 -1.2(8) . . . . ? C15 C16 C17 C18 -0.3(10) . . . . ? C16 C17 C18 C13 1.3(10) . . . . ? O1 C13 C18 C17 -179.4(5) . . . . ? C14 C13 C18 C17 -0.6(8) . . . . ? O2 C19 C20 C24 6.4(6) . . . . ? O2 C19 C20 C21 -171.9(4) . . . . ? C24 C20 C21 C22 -1.4(6) . . . . ? C19 C20 C21 C22 177.0(4) . . . . ? C20 C21 C22 C23 0.3(7) . . . . ? C21 C22 C23 N3 1.9(6) . . . . ? C21 C22 C23 C25 -177.2(4) . . . . ? C21 C20 C24 N3 0.5(6) . . . . ? C19 C20 C24 N3 -177.8(4) . . . . ? N3 C23 C25 N4 5.5(5) . . . . ? C22 C23 C25 N4 -175.4(3) . . . . ? N3 C23 C25 C26 -173.8(4) . . . . ? C22 C23 C25 C26 5.3(6) . . . . ? N4 C25 C26 C27 -1.7(6) . . . . ? C23 C25 C26 C27 177.6(4) . . . . ? C25 C26 C27 C28 0.3(7) . . . . ? C26 C27 C28 C29 1.1(7) . . . . ? C26 C27 C28 C30 180.0(5) . . . . ? C27 C28 C29 N4 -1.4(6) . . . . ? C30 C28 C29 N4 179.7(4) . . . . ? C36 C32 C33 C34 -1.5(8) . . . . ? C31 C32 C33 C34 179.0(6) . . . . ? C32 C33 C34 C35 -1.7(9) . . . . ? C33 C34 C35 N5 4.6(9) . . . . ? C33 C34 C35 C37 -175.3(5) . . . . ? C33 C32 C36 N5 2.0(7) . . . . ? C31 C32 C36 N5 -178.5(4) . . . . ? N5 C35 C37 N6 10.3(6) . . . . ? C34 C35 C37 N6 -169.8(5) . . . . ? N5 C35 C37 C38 -173.1(12) . . . . ? C34 C35 C37 C38 6.8(14) . . . . ? N5 C35 C37 C38A -158.0(7) . . . . ? C34 C35 C37 C38A 22.0(9) . . . . ? N6 C37 C38 C39 -6(2) . . . . ? C35 C37 C38 C39 176.8(14) . . . . ? C38A C37 C38 C39 143(4) . . . . ? C37 C38 C39 C40 7(3) . . . . ? C38 C39 C40 C41 -3(3) . . . . ? C38 C39 C40 C42 -176.2(17) . . . . ? C39 C40 C41 N6 0(2) . . . . ? C42 C40 C41 N6 173.2(12) . . . . ? C41 C40 C42 O3 2(2) . . . . ? C39 C40 C42 O3 175.3(13) . . . . ? C40 C42 O3 C43 -86.5(14) . . . . ? C40 C42 O3 C43 -180.0(8) . . . 2_556 ? C42 O3 C43 C44 10.1(12) . . . . ? C43 O3 C43 C44 136.4(7) 2_556 . . . ? O3 O3 C43 C44 -174.5(8) 2_556 . . . ? C42 O3 C43 O3 -175.4(9) . . . 2_556 ? C43 O3 C43 O3 -49.1(4) 2_556 . . 2_556 ? C42 O3 C43 C43 -126.3(10) . . . 2_556 ? O3 O3 C43 C43 49.1(4) 2_556 . . 2_556 ? O3 C43 C44 C45 -176.7(7) . . . . ? O3 C43 C44 C45 26(3) 2_556 . . . ? C43 C43 C44 C45 -89.7(15) 2_556 . . . ? C45A C45 C44 C43 2.9(13) 2_556 . . . ? N6 C37 C38A C39A 8.4(15) . . . . ? C38 C37 C38A C39A -31(2) . . . . ? C35 C37 C38A C39A 174.4(9) . . . . ? C37 C38A C39A C40A -2.9(16) . . . . ? C38A C39A C40A C41A 0.6(18) . . . . ? C38A C39A C40A C42A -178.2(11) . . . . ? C39A C40A C41A N6 -3(3) . . . . ? C42A C40A C41A N6 175.9(16) . . . . ? C39A C40A C42A O3A 174.9(9) . . . . ? C41A C40A C42A O3A -3.7(17) . . . . ? C40A C42A O3A C43A 178.2(9) . . . . ? C42A O3A C43A C44A 7.4(15) . . . . ? O3A C43A C44A C45A 175.2(10) . . . . ? C43A C44A C45A C45 9.9(16) . . . 2_556 ? C2 C6 N1 C5 0.0(5) . . . . ? C2 C6 N1 Ni1 -175.7(3) . . . . ? C4 C5 N1 C6 0.0(5) . . . . ? C7 C5 N1 C6 -180.0(3) . . . . ? C4 C5 N1 Ni1 176.2(3) . . . . ? C7 C5 N1 Ni1 -3.7(4) . . . . ? C10 C11 N2 C7 0.5(5) . . . . ? C10 C11 N2 Ni1 178.4(3) . . . . ? C8 C7 N2 C11 -0.7(5) . . . . ? C5 C7 N2 C11 179.9(3) . . . . ? C8 C7 N2 Ni1 -178.9(3) . . . . ? C5 C7 N2 Ni1 1.7(4) . . . . ? C22 C23 N3 C24 -2.8(5) . . . . ? C25 C23 N3 C24 176.4(3) . . . . ? C22 C23 N3 Ni1 171.9(3) . . . 2_556 ? C25 C23 N3 Ni1 -8.9(4) . . . 2_556 ? C20 C24 N3 C23 1.6(5) . . . . ? C20 C24 N3 Ni1 -172.6(3) . . . 2_556 ? C28 C29 N4 C25 0.1(5) . . . . ? C28 C29 N4 Ni1 -178.2(3) . . . 2_556 ? C26 C25 N4 C29 1.5(5) . . . . ? C23 C25 N4 C29 -177.8(3) . . . . ? C26 C25 N4 Ni1 180.0(3) . . . 2_556 ? C23 C25 N4 Ni1 0.7(4) . . . 2_556 ? C32 C36 N5 C35 0.8(6) . . . . ? C32 C36 N5 Ni1 -179.7(3) . . . . ? C34 C35 N5 C36 -4.1(6) . . . . ? C37 C35 N5 C36 175.8(4) . . . . ? C34 C35 N5 Ni1 176.3(4) . . . . ? C37 C35 N5 Ni1 -3.8(5) . . . . ? C40A C41A N6 C37 6(2) . . . . ? C40A C41A N6 C41 176(7) . . . . ? C40A C41A N6 Ni1 -152.8(13) . . . . ? C38 C37 N6 C41A 7.3(14) . . . . ? C35 C37 N6 C41A -175.3(11) . . . . ? C38A C37 N6 C41A -9.7(14) . . . . ? C38 C37 N6 C41 3.4(13) . . . . ? C35 C37 N6 C41 -179.2(9) . . . . ? C38A C37 N6 C41 -13.7(13) . . . . ? C38 C37 N6 Ni1 171.2(9) . . . . ? C35 C37 N6 Ni1 -11.4(5) . . . . ? C38A C37 N6 Ni1 154.1(8) . . . . ? C40 C41 N6 C41A -13(4) . . . . ? C40 C41 N6 C37 -0.6(19) . . . . ? C40 C41 N6 Ni1 -167.9(11) . . . . ? C14 C13 O1 C12 176.2(4) . . . . ? C18 C13 O1 C12 -5.0(7) . . . . ? C10 C12 O1 C13 -179.2(4) . . . . ? C13 C14 O2 C19 -167.1(4) . . . . ? C15 C14 O2 C19 12.6(6) . . . . ? C20 C19 O2 C14 -91.2(5) . . . . ? C1T O1T C4T C3T 31(2) . . . . ? C4T O1T C1T C2T -39(2) . . . . ? O1T C1T C2T C3T 29(2) . . . . ? C1T C2T C3T C4T -6(2) . . . . ? O1T C4T C3T C2T -16(2) . . . . ? C8T O2T C5T C6T 34(5) . . . . ? O2T C5T C6T C7T -30(5) . . . . ? C5T C6T C7T C8T 19(6) . . . . ? C5T O2T C8T C7T -26(6) . . . . ? C6T C7T C8T O2T 3(5) . . . . ? C36 N5 Ni1 N6 178.9(3) . . . . ? C35 N5 Ni1 N6 -1.6(3) . . . . ? C36 N5 Ni1 N2 81.1(3) . . . . ? C35 N5 Ni1 N2 -99.4(3) . . . . ? C36 N5 Ni1 N1 1.9(3) . . . . ? C35 N5 Ni1 N1 -178.6(3) . . . . ? C36 N5 Ni1 N4 -93.7(3) . . . 2_556 ? C35 N5 Ni1 N4 85.8(3) . . . 2_556 ? C41A N6 Ni1 N5 166.0(14) . . . . ? C37 N6 Ni1 N5 7.2(3) . . . . ? C41 N6 Ni1 N5 176.1(8) . . . . ? C41A N6 Ni1 N2 -101.7(13) . . . . ? C37 N6 Ni1 N2 99.6(3) . . . . ? C41 N6 Ni1 N2 -91.6(8) . . . . ? C41A N6 Ni1 N3 -6.2(13) . . . 2_556 ? C37 N6 Ni1 N3 -165.0(3) . . . 2_556 ? C41 N6 Ni1 N3 3.9(8) . . . 2_556 ? C41A N6 Ni1 N4 71.8(13) . . . 2_556 ? C37 N6 Ni1 N4 -86.9(3) . . . 2_556 ? C41 N6 Ni1 N4 81.9(8) . . . 2_556 ? C11 N2 Ni1 N5 82.9(3) . . . . ? C7 N2 Ni1 N5 -99.1(2) . . . . ? C11 N2 Ni1 N6 2.9(3) . . . . ? C7 N2 Ni1 N6 -179.1(2) . . . . ? C11 N2 Ni1 N3 -93.0(3) . . . 2_556 ? C7 N2 Ni1 N3 85.0(2) . . . 2_556 ? C11 N2 Ni1 N1 179.2(3) . . . . ? C7 N2 Ni1 N1 -2.8(2) . . . . ? C6 N1 Ni1 N5 -87.9(3) . . . . ? C5 N1 Ni1 N5 96.1(2) . . . . ? C6 N1 Ni1 N2 179.5(3) . . . . ? C5 N1 Ni1 N2 3.6(2) . . . . ? C6 N1 Ni1 N3 84.6(3) . . . 2_556 ? C5 N1 Ni1 N3 -91.4(2) . . . 2_556 ? C6 N1 Ni1 N4 6.5(3) . . . 2_556 ? C5 N1 Ni1 N4 -169.5(2) . . . 2_556 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.084 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.125 data_lfl11sad _database_code_depnum_ccdc_archive 'CCDC 824370' #TrackingRef '- combined lindoy.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C90 H78 N12 Ni2 O6), 4(P F6), 1.75(C2 H3 N), 5.25(C4 H8 O), 0.25(H2 O)' _chemical_formula_sum 'C114.50 H125.75 F24 N13.75 Ni2 O11.50 P4' _chemical_formula_weight 2575.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0096 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0667 0.0580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3147 0.7232 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-p 2ybc' _symmetry_intl_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 26.028(2) _cell_length_b 22.7450(17) _cell_length_c 21.4660(16) _cell_angle_alpha 90.00 _cell_angle_beta 113.663(2) _cell_angle_gamma 90.00 _cell_volume 11639.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20870 _cell_measurement_theta_min 2.288 _cell_measurement_theta_max 19.267 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5330 _exptl_absorpt_coefficient_mu 0.259 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5994 _exptl_absorpt_correction_T_max 0.7444 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; The crystal was coated in Exxon Paratone N hydrocarbon oil and mounted on a thin mohair fibre attached to a copper pin. Upon mounting on the diffractometer, the crystal was quenched to 100(K) under a cold nitrogen gas stream supplied by an Oxford Cryosystems Cryostream and data were collected at this temperature. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.49594 _diffrn_radiation_source 'ChemMatCARS, APS, Argonne National Lab, USA' _diffrn_radiation_monochromator 'Double Diamond 111' _diffrn_measurement_device_type 'Bruker Kappa with SMART 6000 CCD detector' _diffrn_measurement_method \w+\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 99393 _diffrn_reflns_av_R_equivalents 0.0847 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 19.31 _reflns_number_total 27767 _reflns_number_gt 16878 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.1 (CCDC, 2005)' _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^)+(0.1010P)^2^+7.1972P] 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 27767 _refine_ls_number_parameters 1577 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1184 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.1880 _refine_ls_wR_factor_gt 0.1574 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.017 _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 C1 C -0.06998(18) 0.1722(2) 0.1257(2) 0.0364(10) Uani 1 1 d . . . H1A H -0.0566 0.2099 0.1159 0.055 Uiso 1 1 calc R . . H1B H -0.0928 0.1791 0.1519 0.055 Uiso 1 1 calc R . . H1C H -0.0927 0.1524 0.0830 0.055 Uiso 1 1 calc R . . C2 C -0.02049(15) 0.13417(18) 0.16645(19) 0.0253(8) Uani 1 1 d . . . C3 C 0.00252(15) 0.13547(16) 0.23706(18) 0.0213(7) Uani 1 1 d . . . H3 H -0.0137 0.1613 0.2590 0.026 Uiso 1 1 calc R . . C4 C 0.06921(14) 0.06531(15) 0.24554(16) 0.0162(7) Uani 1 1 d . . . C5 C 0.04874(16) 0.06162(19) 0.17532(19) 0.0275(9) Uani 1 1 d . . . H5 H 0.0654 0.0354 0.1543 0.033 Uiso 1 1 calc R . . C6 C 0.00353(17) 0.09665(19) 0.13575(19) 0.0304(9) Uani 1 1 d . . . H6 H -0.0107 0.0946 0.0875 0.036 Uiso 1 1 calc R . . C7 C 0.11687(13) 0.02972(15) 0.29172(17) 0.0159(7) Uani 1 1 d . . . C8 C 0.17458(13) 0.00823(14) 0.40310(17) 0.0157(6) Uani 1 1 d . . . H8 H 0.1845 0.0144 0.4503 0.019 Uiso 1 1 calc R . . C9 C 0.20596(14) -0.03132(14) 0.38385(18) 0.0171(7) Uani 1 1 d . . . C10 C 0.19064(15) -0.04087(16) 0.31541(18) 0.0214(7) Uani 1 1 d . . . H10 H 0.2108 -0.0682 0.3003 0.026 Uiso 1 1 calc R . . C11 C 0.14519(15) -0.01013(16) 0.26835(18) 0.0209(7) Uani 1 1 d . . . H11 H 0.1339 -0.0165 0.2209 0.025 Uiso 1 1 calc R . . C12 C 0.25632(14) -0.05870(15) 0.43902(18) 0.0192(7) Uani 1 1 d . . . H12A H 0.2879 -0.0304 0.4543 0.023 Uiso 1 1 calc R . . H12B H 0.2474 -0.0685 0.4785 0.023 Uiso 1 1 calc R . . C13 C 0.32028(15) -0.13729(16) 0.45794(19) 0.0228(8) Uani 1 1 d . . . C14 C 0.35106(14) -0.11684(14) 0.52343(17) 0.0164(7) Uani 1 1 d . . . H14 H 0.3384 -0.0839 0.5406 0.020 Uiso 1 1 calc R . . C15 C 0.40078(14) -0.14534(15) 0.56348(17) 0.0175(7) Uani 1 1 d . . . C16 C 0.41830(16) -0.19510(16) 0.53988(19) 0.0255(8) Uani 1 1 d . . . H16 H 0.4517 -0.2150 0.5678 0.031 Uiso 1 1 calc R . . C17 C 0.38626(19) -0.21501(19) 0.4750(2) 0.0358(10) Uani 1 1 d . . . H17 H 0.3980 -0.2490 0.4585 0.043 Uiso 1 1 calc R . . C18 C 0.33736(18) -0.18660(18) 0.4334(2) 0.0343(10) Uani 1 1 d . . . H18 H 0.3159 -0.2007 0.3888 0.041 Uiso 1 1 calc R . . C19 C 0.42412(14) -0.06861(15) 0.64592(18) 0.0188(7) Uani 1 1 d . . . H19A H 0.3910 -0.0704 0.6575 0.023 Uiso 1 1 calc R . . H19B H 0.4161 -0.0405 0.6079 0.023 Uiso 1 1 calc R . . C20 C 0.47475(14) -0.04924(15) 0.70643(18) 0.0177(7) Uani 1 1 d . . . C21 C 0.50762(13) -0.00344(14) 0.70139(17) 0.0148(6) Uani 1 1 d . . . H21 H 0.4979 0.0147 0.6583 0.018 Uiso 1 1 calc R . . C22 C 0.56679(14) -0.00921(15) 0.81465(17) 0.0188(7) Uani 1 1 d . . . C23 C 0.53725(16) -0.05670(17) 0.82357(19) 0.0259(8) Uani 1 1 d . . . H23 H 0.5488 -0.0752 0.8667 0.031 Uiso 1 1 calc R . . C24 C 0.49101(16) -0.07681(16) 0.7692(2) 0.0256(8) Uani 1 1 d . . . H24 H 0.4703 -0.1094 0.7746 0.031 Uiso 1 1 calc R . . C25 C 0.61436(16) 0.01799(18) 0.87131(18) 0.0252(8) Uani 1 1 d . . . C26 C 0.67641(19) 0.0955(2) 0.9048(2) 0.0377(10) Uani 1 1 d . . . H26 H 0.6910 0.1301 0.8931 0.045 Uiso 1 1 calc R . . C27 C 0.6985(3) 0.0780(3) 0.9728(2) 0.0649(18) Uani 1 1 d . . . C28 C 0.6773(3) 0.0271(3) 0.9876(2) 0.0666(18) Uani 1 1 d U . . H28 H 0.6919 0.0129 1.0330 0.080 Uiso 1 1 calc R . . C29 C 0.6351(2) -0.0039(2) 0.9373(2) 0.0445(12) Uani 1 1 d . . . H29 H 0.6207 -0.0392 0.9477 0.053 Uiso 1 1 calc R . . C30 C 0.7430(3) 0.1153(4) 1.0258(3) 0.099(3) Uani 1 1 d U . . H30A H 0.7250 0.1477 1.0395 0.148 Uiso 1 1 calc R . . H30B H 0.7685 0.1312 1.0065 0.148 Uiso 1 1 calc R . . H30C H 0.7643 0.0910 1.0656 0.148 Uiso 1 1 calc R . . C31 C -0.09620(16) 0.1959(2) 0.4305(2) 0.0327(9) Uani 1 1 d . . . H31A H -0.0859 0.1848 0.4781 0.049 Uiso 1 1 calc R . . H31B H -0.1183 0.1643 0.4008 0.049 Uiso 1 1 calc R . . H31C H -0.1185 0.2321 0.4206 0.049 Uiso 1 1 calc R . . C32 C -0.04406(14) 0.20587(17) 0.41844(18) 0.0225(8) Uani 1 1 d . . . C33 C -0.01506(14) 0.15896(16) 0.40582(17) 0.0185(7) Uani 1 1 d . . . H33 H -0.0296 0.1205 0.4047 0.022 Uiso 1 1 calc R . . C34 C 0.05217(14) 0.21927(16) 0.39591(17) 0.0179(7) Uani 1 1 d . . . C35 C 0.02574(16) 0.26843(17) 0.4069(2) 0.0285(9) Uani 1 1 d . . . H35 H 0.0405 0.3066 0.4067 0.034 Uiso 1 1 calc R . . C36 C -0.02257(16) 0.26114(19) 0.4183(2) 0.0313(9) Uani 1 1 d . . . H36 H -0.0410 0.2946 0.4262 0.038 Uiso 1 1 calc R . . C37 C 0.10647(14) 0.22258(16) 0.38872(18) 0.0185(7) Uani 1 1 d . . . C38 C 0.18274(13) 0.17011(15) 0.39067(16) 0.0147(6) Uani 1 1 d . . . H38 H 0.2004 0.1333 0.3920 0.018 Uiso 1 1 calc R . . C39 C 0.21177(14) 0.22055(15) 0.38919(17) 0.0173(7) Uani 1 1 d . . . C40 C 0.18432(15) 0.27426(16) 0.3838(2) 0.0255(8) Uani 1 1 d . . . H40 H 0.2021 0.3100 0.3808 0.031 Uiso 1 1 calc R . . C41 C 0.13122(16) 0.27490(17) 0.3829(2) 0.0278(9) Uani 1 1 d . . . H41 H 0.1117 0.3110 0.3784 0.033 Uiso 1 1 calc R . . C42 C 0.27106(14) 0.21672(16) 0.39532(17) 0.0187(7) Uani 1 1 d . . . H42A H 0.2927 0.2510 0.4209 0.022 Uiso 1 1 calc R . . H42B H 0.2890 0.1806 0.4203 0.022 Uiso 1 1 calc R . . C43 C 0.31772(13) 0.19357(14) 0.32280(17) 0.0144(6) Uani 1 1 d . . . C44 C 0.36581(13) 0.17720(14) 0.37870(16) 0.0149(6) Uani 1 1 d . . . H44 H 0.3694 0.1853 0.4237 0.018 Uiso 1 1 calc R . . C45 C 0.40829(13) 0.14876(14) 0.36713(16) 0.0145(6) Uani 1 1 d . . . C46 C 0.40451(14) 0.13928(15) 0.30182(18) 0.0181(7) Uani 1 1 d . . . H46 H 0.4337 0.1192 0.2947 0.022 Uiso 1 1 calc R . . C47 C 0.35791(15) 0.15929(16) 0.24682(17) 0.0197(7) Uani 1 1 d . . . H47 H 0.3561 0.1545 0.2020 0.024 Uiso 1 1 calc R . . C48 C 0.31385(14) 0.18637(15) 0.25676(17) 0.0182(7) Uani 1 1 d . . . H48 H 0.2817 0.1997 0.2191 0.022 Uiso 1 1 calc R . . C49 C 0.46223(14) 0.13734(16) 0.48657(16) 0.0188(7) Uani 1 1 d . . . H49A H 0.4283 0.1245 0.4929 0.023 Uiso 1 1 calc R . . H49B H 0.4680 0.1798 0.4973 0.023 Uiso 1 1 calc R . . C50 C 0.51249(14) 0.10286(15) 0.53264(17) 0.0160(7) Uani 1 1 d . . . C51 C 0.53392(13) 0.11188(15) 0.60236(17) 0.0148(6) Uani 1 1 d . . . H51 H 0.5171 0.1411 0.6196 0.018 Uiso 1 1 calc R . . C52 C 0.60185(13) 0.04004(14) 0.62282(17) 0.0148(6) Uani 1 1 d . . . C53 C 0.58293(14) 0.02861(15) 0.55390(17) 0.0182(7) Uani 1 1 d . . . H53 H 0.6008 -0.0005 0.5378 0.022 Uiso 1 1 calc R . . C54 C 0.53773(14) 0.05996(15) 0.50842(17) 0.0180(7) Uani 1 1 d . . . H54 H 0.5241 0.0521 0.4610 0.022 Uiso 1 1 calc R . . C55 C 0.64976(13) 0.00893(14) 0.67450(17) 0.0155(6) Uani 1 1 d . . . C56 C 0.70515(14) -0.00324(15) 0.78896(19) 0.0217(7) Uani 1 1 d . . . H56 H 0.7134 0.0071 0.8349 0.026 Uiso 1 1 calc R . . C57 C 0.73864(14) -0.04486(15) 0.7767(2) 0.0241(8) Uani 1 1 d . . . C58 C 0.72600(14) -0.05929(15) 0.7096(2) 0.0223(8) Uani 1 1 d . . . H58 H 0.7480 -0.0877 0.6988 0.027 Uiso 1 1 calc R . . C59 C 0.68165(14) -0.03262(15) 0.65822(19) 0.0200(7) Uani 1 1 d . . . H59 H 0.6729 -0.0425 0.6121 0.024 Uiso 1 1 calc R . . C60 C 0.78606(17) -0.07343(18) 0.8350(2) 0.0370(11) Uani 1 1 d . . . H60A H 0.8105 -0.0430 0.8644 0.055 Uiso 1 1 calc R . . H60B H 0.8078 -0.0983 0.8171 0.055 Uiso 1 1 calc R . . H60C H 0.7708 -0.0976 0.8613 0.055 Uiso 1 1 calc R . . C61 C -0.09586(17) -0.0633(2) 0.2642(2) 0.0333(9) Uani 1 1 d . . . H61A H -0.0832 -0.0835 0.2326 0.050 Uiso 1 1 calc R . . H61B H -0.1179 -0.0286 0.2421 0.050 Uiso 1 1 calc R . . H61C H -0.1191 -0.0901 0.2777 0.050 Uiso 1 1 calc R . . C62 C -0.04569(15) -0.04463(18) 0.32637(19) 0.0261(8) Uani 1 1 d . . . C63 C -0.01701(14) 0.00647(16) 0.32606(18) 0.0195(7) Uani 1 1 d . . . H63 H -0.0292 0.0287 0.2852 0.023 Uiso 1 1 calc R . . C64 C 0.04450(15) -0.00419(16) 0.43847(18) 0.0211(7) Uani 1 1 d . . . C65 C 0.01879(19) -0.0563(2) 0.4428(2) 0.0383(11) Uani 1 1 d . . . H65 H 0.0323 -0.0783 0.4839 0.046 Uiso 1 1 calc R . . C66 C -0.02701(19) -0.0760(2) 0.3865(2) 0.0389(11) Uani 1 1 d . . . H66 H -0.0456 -0.1112 0.3893 0.047 Uiso 1 1 calc R . . C67 C 0.09177(14) 0.02190(16) 0.49675(18) 0.0200(7) Uani 1 1 d . . . C68 C 0.15149(13) 0.10167(15) 0.53452(17) 0.0164(7) Uani 1 1 d . . . H68 H 0.1642 0.1385 0.5253 0.020 Uiso 1 1 calc R . . C69 C 0.17585(14) 0.07949(16) 0.60035(17) 0.0194(7) Uani 1 1 d . . . C70 C 0.15729(16) 0.02622(18) 0.61329(19) 0.0276(8) Uani 1 1 d . . . H70 H 0.1737 0.0092 0.6573 0.033 Uiso 1 1 calc R . . C71 C 0.11453(17) -0.00212(18) 0.5614(2) 0.0308(9) Uani 1 1 d . . . H71 H 0.1006 -0.0384 0.5700 0.037 Uiso 1 1 calc R . . C72 C 0.22411(15) 0.11250(18) 0.65238(17) 0.0222(8) Uani 1 1 d . . . H72A H 0.2601 0.0969 0.6537 0.027 Uiso 1 1 calc R . . H72B H 0.2217 0.1547 0.6401 0.027 Uiso 1 1 calc R . . C73 C 0.26899(14) 0.12338(16) 0.77228(17) 0.0176(7) Uani 1 1 d . . . C74 C 0.31456(14) 0.14948(15) 0.76490(17) 0.0182(7) Uani 1 1 d . . . H74 H 0.3134 0.1578 0.7210 0.022 Uiso 1 1 calc R . . C75 C 0.36177(14) 0.16319(15) 0.82292(18) 0.0188(7) Uani 1 1 d . . . C76 C 0.36275(16) 0.15389(18) 0.88753(18) 0.0254(8) Uani 1 1 d . . . H76 H 0.3946 0.1647 0.9271 0.030 Uiso 1 1 calc R . . C77 C 0.31643(16) 0.12870(18) 0.89285(18) 0.0262(8) Uani 1 1 d . . . H77 H 0.3167 0.1220 0.9367 0.031 Uiso 1 1 calc R . . C78 C 0.26949(15) 0.11296(16) 0.83573(18) 0.0220(7) Uani 1 1 d . . . H78 H 0.2381 0.0952 0.8403 0.026 Uiso 1 1 calc R . . C79 C 0.41330(14) 0.18439(17) 0.75605(17) 0.0217(7) Uani 1 1 d . . . H79A H 0.3894 0.2158 0.7266 0.026 Uiso 1 1 calc R . . H79B H 0.3996 0.1461 0.7337 0.026 Uiso 1 1 calc R . . C80 C 0.47268(14) 0.19336(16) 0.76543(17) 0.0194(7) Uani 1 1 d . . . C81 C 0.50245(13) 0.14694(15) 0.75453(16) 0.0167(7) Uani 1 1 d . . . H81 H 0.4850 0.1094 0.7447 0.020 Uiso 1 1 calc R . . C82 C 0.57921(14) 0.20543(15) 0.77085(16) 0.0170(7) Uani 1 1 d . . . C83 C 0.55311(15) 0.25313(15) 0.78579(18) 0.0211(7) Uani 1 1 d . . . H83 H 0.5720 0.2898 0.7980 0.025 Uiso 1 1 calc R . . C84 C 0.49945(15) 0.24692(16) 0.78281(18) 0.0222(8) Uani 1 1 d . . . H84 H 0.4810 0.2794 0.7927 0.027 Uiso 1 1 calc R . . C85 C 0.63418(14) 0.20881(15) 0.76673(17) 0.0195(7) Uani 1 1 d . . . C86 C 0.70577(14) 0.15813(16) 0.75344(18) 0.0200(7) Uani 1 1 d . . . H86 H 0.7215 0.1216 0.7487 0.024 Uiso 1 1 calc R . . C87 C 0.73494(15) 0.20922(16) 0.75330(19) 0.0223(8) Uani 1 1 d . . . C88 C 0.71070(17) 0.26116(17) 0.7597(2) 0.0314(9) Uani 1 1 d . . . H88 H 0.7287 0.2973 0.7591 0.038 Uiso 1 1 calc R . . C89 C 0.66036(17) 0.26136(17) 0.7669(2) 0.0302(9) Uani 1 1 d . . . H89 H 0.6440 0.2974 0.7720 0.036 Uiso 1 1 calc R . . C90 C 0.78949(16) 0.20669(18) 0.7441(2) 0.0304(9) Uani 1 1 d . . . H90A H 0.7963 0.2447 0.7274 0.046 Uiso 1 1 calc R . . H90B H 0.7872 0.1759 0.7112 0.046 Uiso 1 1 calc R . . H90C H 0.8203 0.1978 0.7879 0.046 Uiso 1 1 calc R . . N1 N 0.04609(11) 0.10249(12) 0.27595(14) 0.0159(6) Uani 1 1 d . . . N2 N 0.13113(11) 0.03819(12) 0.35881(14) 0.0139(5) Uani 1 1 d . . . N3 N 0.55260(11) 0.01692(12) 0.75411(14) 0.0153(6) Uani 1 1 d . . . N4 N 0.63612(13) 0.06661(14) 0.85566(15) 0.0230(7) Uani 1 1 d . . . N5 N 0.03181(11) 0.16491(13) 0.39528(13) 0.0148(6) Uani 1 1 d . . . N6 N 0.13114(11) 0.17010(12) 0.39036(14) 0.0141(5) Uani 1 1 d . . . N7 N 0.57720(11) 0.08141(12) 0.64649(14) 0.0137(5) Uani 1 1 d . . . N8 N 0.66167(11) 0.02340(12) 0.73989(14) 0.0161(6) Uani 1 1 d . . . N9 N 0.02705(11) 0.02648(13) 0.38013(14) 0.0160(6) Uani 1 1 d . . . N10 N 0.11106(11) 0.07354(12) 0.48354(14) 0.0152(6) Uani 1 1 d . . . N11 N 0.55451(11) 0.15211(12) 0.75704(13) 0.0150(6) Uani 1 1 d . . . N12 N 0.65662(11) 0.15745(12) 0.75987(14) 0.0161(6) Uani 1 1 d . . . F1 F 0.0902(2) 0.8944(2) 1.0220(2) 0.150(3) Uani 1 1 d . . . F2 F 0.18810(10) 0.92129(12) 1.16463(14) 0.0460(7) Uani 1 1 d . . . F3 F 0.11138(12) 0.96926(13) 1.09463(14) 0.0520(8) Uani 1 1 d . . . F4 F 0.1687(2) 0.84704(16) 1.08964(19) 0.0984(16) Uani 1 1 d . . . F5 F 0.10620(15) 0.87812(19) 1.1310(2) 0.0911(13) Uani 1 1 d . . . F6 F 0.1745(3) 0.9401(2) 1.0572(3) 0.137(2) Uani 1 1 d . . . F7 F 0.19173(11) 0.86084(14) 0.71652(16) 0.0534(8) Uani 1 1 d . . . F8 F 0.12391(12) 0.91691(12) 0.79746(14) 0.0463(7) Uani 1 1 d . . . F9 F 0.11440(11) 0.83560(11) 0.73321(13) 0.0406(6) Uani 1 1 d . . . F10 F 0.20127(13) 0.94195(15) 0.78108(18) 0.0662(9) Uani 1 1 d . . . F11 F 0.19482(15) 0.85169(15) 0.82315(15) 0.0736(11) Uani 1 1 d . . . F12 F 0.12006(10) 0.92446(11) 0.69060(13) 0.0375(6) Uani 1 1 d . . . F13 F 0.29286(13) 0.07979(12) 0.46879(13) 0.0453(7) Uani 1 1 d . . . F14 F 0.35616(13) 0.09184(13) 0.63041(13) 0.0486(7) Uani 1 1 d . . . F15 F 0.29329(14) 0.02969(12) 0.56018(14) 0.0547(8) Uani 1 1 d . . . F16 F 0.35668(10) 0.14245(10) 0.53913(13) 0.0323(5) Uani 1 1 d . . . F17 F 0.37363(13) 0.04489(12) 0.54677(15) 0.0543(8) Uani 1 1 d . . . F18 F 0.27539(12) 0.12663(13) 0.54981(15) 0.0501(7) Uani 1 1 d . . . F19 F 0.48232(12) 0.28131(12) 0.52917(13) 0.0445(7) Uani 1 1 d . . . F20 F 0.42833(11) 0.30596(11) 0.63657(11) 0.0363(6) Uani 1 1 d . . . F21 F 0.39804(11) 0.26550(11) 0.53084(12) 0.0374(6) Uani 1 1 d . . . F22 F 0.51274(11) 0.32196(12) 0.63437(13) 0.0455(7) Uani 1 1 d . . . F23 F 0.43454(14) 0.35678(11) 0.54961(12) 0.0490(8) Uani 1 1 d . . . F24 F 0.47538(12) 0.23027(11) 0.61603(12) 0.0416(6) Uani 1 1 d . . . P1 P 0.13989(6) 0.90749(6) 1.09180(6) 0.0409(3) Uani 1 1 d . . . P2 P 0.15836(4) 0.88853(5) 0.75765(6) 0.0315(2) Uani 1 1 d . . . P3 P 0.32618(5) 0.08629(4) 0.55112(5) 0.0245(2) Uani 1 1 d . . . P4 P 0.45565(5) 0.29320(4) 0.58322(5) 0.0264(2) Uani 1 1 d . . . Ni1 Ni 0.079383(17) 0.097160(18) 0.38163(2) 0.01308(10) Uani 1 1 d . . . Ni2 Ni 0.606423(17) 0.084503(18) 0.75192(2) 0.01370(10) Uani 1 1 d . . . O1 O 0.27199(11) -0.11039(11) 0.41409(13) 0.0265(6) Uani 1 1 d . . . O2 O 0.43593(10) -0.12570(10) 0.62663(12) 0.0192(5) Uani 1 1 d . . . O3 O 0.27069(10) 0.21568(11) 0.32831(12) 0.0185(5) Uani 1 1 d . . . O4 O 0.45546(10) 0.12700(11) 0.41840(12) 0.0204(5) Uani 1 1 d . . . O5 O 0.22188(10) 0.10570(12) 0.71740(12) 0.0211(5) Uani 1 1 d . . . O6 O 0.40993(10) 0.18563(12) 0.82060(12) 0.0233(6) Uani 1 1 d . . . O1T O 0.1942(3) 0.6417(3) 1.0154(3) 0.0997(18) Uani 1 1 d . . . C1T C 0.1710(3) 0.6785(4) 0.9563(4) 0.088(2) Uani 1 1 d . . . H1T1 H 0.1295 0.6797 0.9394 0.106 Uiso 1 1 calc R . . H1T2 H 0.1812 0.6635 0.9195 0.106 Uiso 1 1 calc R . . C2T C 0.1961(3) 0.7405(4) 0.9790(4) 0.098(3) Uani 1 1 d . . . H2T1 H 0.2063 0.7588 0.9438 0.118 Uiso 1 1 calc R . . H2T2 H 0.1688 0.7662 0.9873 0.118 Uiso 1 1 calc R . . C3T C 0.2455(3) 0.7318(3) 1.0412(4) 0.083(2) Uani 1 1 d . . . H3T1 H 0.2795 0.7286 1.0316 0.100 Uiso 1 1 calc R . . H3T2 H 0.2503 0.7648 1.0732 0.100 Uiso 1 1 calc R . . C4T C 0.2348(3) 0.6774(4) 1.0686(4) 0.084(2) Uani 1 1 d . . . H4T1 H 0.2203 0.6862 1.1038 0.100 Uiso 1 1 calc R . . H4T2 H 0.2703 0.6552 1.0905 0.100 Uiso 1 1 calc R . . O2T O 0.88776(18) 0.69032(18) 0.8568(2) 0.0421(10) Uani 0.75 1 d P A 1 C5T C 0.8561(3) 0.7236(3) 0.7981(3) 0.052(2) Uani 0.75 1 d P A 1 H5T1 H 0.8169 0.7274 0.7937 0.062 Uiso 0.75 1 calc PR A 1 H5T2 H 0.8558 0.7036 0.7570 0.062 Uiso 0.75 1 calc PR A 1 C6T C 0.8816(3) 0.7813(3) 0.8049(3) 0.0393(14) Uani 0.75 1 d P A 1 H6T1 H 0.8536 0.8114 0.7794 0.047 Uiso 0.75 1 calc PR A 1 H6T2 H 0.9124 0.7811 0.7888 0.047 Uiso 0.75 1 calc PR A 1 C7T C 0.9035(4) 0.7918(3) 0.8799(4) 0.060(2) Uani 0.75 1 d P A 1 H7T1 H 0.9361 0.8188 0.8952 0.072 Uiso 0.75 1 calc PR A 1 H7T2 H 0.8741 0.8081 0.8931 0.072 Uiso 0.75 1 calc PR A 1 C8T C 0.9201(3) 0.7323(3) 0.9075(3) 0.0474(16) Uani 0.75 1 d P A 1 H8T1 H 0.9606 0.7262 0.9194 0.057 Uiso 0.75 1 calc PR A 1 H8T2 H 0.9131 0.7272 0.9492 0.057 Uiso 0.75 1 calc PR A 1 C9T C 0.9271(6) 0.2097(5) 0.7339(13) 0.0734(13) Uiso 0.45 1 d PD B 1 H9T1 H 0.8998 0.2228 0.6888 0.088 Uiso 0.45 1 calc PR B 1 H9T2 H 0.9204 0.2329 0.7689 0.088 Uiso 0.45 1 calc PR B 1 O3T O 0.9798(4) 0.2207(4) 0.7387(6) 0.0734(13) Uiso 0.45 1 d PD B 1 C10T C 0.9173(6) 0.1452(5) 0.7431(8) 0.0734(13) Uiso 0.45 1 d PD B 1 H10A H 0.8774 0.1338 0.7193 0.088 Uiso 0.45 1 calc PR B 1 H10B H 0.9314 0.1336 0.7916 0.088 Uiso 0.45 1 calc PR B 1 C11T C 0.9539(6) 0.1213(5) 0.7080(8) 0.0734(13) Uiso 0.45 1 d PD B 1 H11A H 0.9319 0.1151 0.6587 0.088 Uiso 0.45 1 calc PR B 1 H11B H 0.9727 0.0841 0.7290 0.088 Uiso 0.45 1 calc PR B 1 C12T C 0.9968(6) 0.1730(5) 0.7219(10) 0.0734(13) Uiso 0.45 1 d PD B 1 H12C H 1.0328 0.1614 0.7587 0.088 Uiso 0.45 1 calc PR B 1 H12D H 1.0038 0.1801 0.6804 0.088 Uiso 0.45 1 calc PR B 1 C9A C 0.9240(9) 0.1943(12) 0.7360(19) 0.0734(13) Uiso 0.30 1 d PD C 2 H9A1 H 0.9159 0.2346 0.7470 0.088 Uiso 0.30 1 calc PR C 2 H9A2 H 0.9208 0.1665 0.7698 0.088 Uiso 0.30 1 calc PR C 2 O3TA O 0.9747(7) 0.1912(8) 0.7340(8) 0.0734(13) Uiso 0.30 1 d PD C 2 C10A C 0.9785(8) 0.1731(11) 0.6776(10) 0.0734(13) Uiso 0.30 1 d PD C 2 H10C H 1.0087 0.1436 0.6876 0.088 Uiso 0.30 1 calc PR C 2 H10D H 0.9858 0.2064 0.6526 0.088 Uiso 0.30 1 calc PR C 2 C11A C 0.8852(9) 0.1770(11) 0.6638(12) 0.0734(13) Uiso 0.30 1 d P C 2 H11C H 0.8545 0.1514 0.6641 0.088 Uiso 0.30 1 calc PR C 2 H11D H 0.8685 0.2124 0.6362 0.088 Uiso 0.30 1 calc PR C 2 C12A C 0.9206(8) 0.1456(11) 0.6367(12) 0.0734(13) Uiso 0.30 1 d PD C 2 H12E H 0.9084 0.1527 0.5873 0.088 Uiso 0.30 1 calc PR C 2 H12F H 0.9207 0.1028 0.6450 0.088 Uiso 0.30 1 calc PR C 2 O3TB O 1.0195(6) 0.1517(8) 0.7864(8) 0.0734(13) Uiso 0.25 1 d PD D 3 C9B C 1.0133(12) 0.1996(14) 0.7342(15) 0.0734(13) Uiso 0.25 1 d P D 3 H9B1 H 1.0432 0.1978 0.7167 0.088 Uiso 0.25 1 calc PR D 3 H9B2 H 1.0117 0.2394 0.7518 0.088 Uiso 0.25 1 calc PR D 3 C10B C 0.9508(9) 0.1772(13) 0.6764(9) 0.0734(13) Uiso 0.25 1 d PD D 3 H10E H 0.9304 0.2099 0.6460 0.088 Uiso 0.25 1 calc PR D 3 H10F H 0.9551 0.1443 0.6486 0.088 Uiso 0.25 1 calc PR D 3 C11B C 0.9701(9) 0.1198(11) 0.7720(14) 0.0734(13) Uiso 0.25 1 d PD D 3 H11E H 0.9647 0.1123 0.8144 0.088 Uiso 0.25 1 calc PR D 3 H11F H 0.9721 0.0815 0.7511 0.088 Uiso 0.25 1 calc PR D 3 C12B C 0.9205(6) 0.1570(13) 0.7220(12) 0.0734(13) Uiso 0.25 1 d PD D 3 H12G H 0.8868 0.1330 0.6968 0.088 Uiso 0.25 1 calc PR D 3 H12H H 0.9106 0.1904 0.7447 0.088 Uiso 0.25 1 calc PR D 3 C16T C 0.1091(4) 0.1041(4) 0.9797(4) 0.068(2) Uani 0.75 1 d P . . H16A H 0.1217 0.1450 0.9934 0.082 Uiso 0.75 1 calc PR . . H16B H 0.1413 0.0771 1.0000 0.082 Uiso 0.75 1 calc PR . . C13T C 0.0590(4) 0.0865(3) 1.0005(4) 0.064(2) Uani 0.75 1 d P . . H13A H 0.0731 0.0721 1.0480 0.077 Uiso 0.75 1 calc PR . . H13B H 0.0332 0.1199 0.9949 0.077 Uiso 0.75 1 calc PR . . C14T C 0.0308(4) 0.0372(4) 0.9495(4) 0.062(2) Uani 0.75 1 d P . . H14A H 0.0502 -0.0009 0.9649 0.075 Uiso 0.75 1 calc PR . . H14B H -0.0092 0.0329 0.9413 0.075 Uiso 0.75 1 calc PR . . C15T C 0.0377(5) 0.0596(4) 0.8883(5) 0.087(3) Uani 0.75 1 d P . . H15A H 0.0445 0.0267 0.8624 0.104 Uiso 0.75 1 calc PR . . H15B H 0.0036 0.0809 0.8582 0.104 Uiso 0.75 1 calc PR . . O4T O 0.0851(2) 0.0986(2) 0.9124(3) 0.0549(13) Uani 0.75 1 d P . . O5T O 0.34846(19) -0.09962(15) 0.7386(2) 0.0616(11) Uani 1 1 d . . . C20T C 0.3046(3) -0.0600(3) 0.7050(4) 0.0677(18) Uani 1 1 d . F . H20A H 0.2678 -0.0782 0.6964 0.081 Uiso 1 1 calc R E 1 H20B H 0.3051 -0.0476 0.6610 0.081 Uiso 1 1 calc R E 1 C18T C 0.3418(7) -0.0384(13) 0.8232(10) 0.109(10) Uani 0.50 1 d P F 1 H18A H 0.3721 -0.0133 0.8549 0.131 Uiso 0.50 1 calc PR F 1 H18B H 0.3135 -0.0457 0.8423 0.131 Uiso 0.50 1 calc PR F 1 C17T C 0.3636(4) -0.0928(3) 0.8084(4) 0.083(2) Uani 0.50 1 d P F 1 H17A H 0.4050 -0.0929 0.8321 0.100 Uiso 0.50 1 calc PR F 1 H17B H 0.3489 -0.1263 0.8257 0.100 Uiso 0.50 1 calc PR F 1 C19T C 0.3146(4) -0.0106(3) 0.7502(5) 0.100(3) Uani 0.50 1 d P F 1 H19C H 0.2790 0.0097 0.7433 0.120 Uiso 0.50 1 calc PR F 1 H19D H 0.3404 0.0180 0.7430 0.120 Uiso 0.50 1 calc PR F 1 C18A C 0.3645(9) -0.0258(16) 0.8109(16) 0.160(16) Uani 0.50 1 d P F 2 H18C H 0.3616 -0.0111 0.8528 0.192 Uiso 0.50 1 calc PR F 2 H18D H 0.3990 -0.0099 0.8083 0.192 Uiso 0.50 1 calc PR F 2 C17A C 0.3636(4) -0.0928(3) 0.8084(4) 0.083(2) Uani 0.50 1 d P F 2 H17C H 0.4008 -0.1100 0.8356 0.100 Uiso 0.50 1 calc PR F 2 H17D H 0.3352 -0.1095 0.8232 0.100 Uiso 0.50 1 calc PR F 2 C19A C 0.3146(4) -0.0106(3) 0.7502(5) 0.100(3) Uani 0.50 1 d P F 2 H19E H 0.2820 -0.0039 0.7621 0.120 Uiso 0.50 1 calc PR F 2 H19F H 0.3212 0.0255 0.7287 0.120 Uiso 0.50 1 calc PR F 2 C23T C 0.5345(3) 0.4326(3) 0.5010(4) 0.0494(17) Uani 0.75 1 d P G 1 H23A H 0.5586 0.4674 0.5197 0.059 Uiso 0.75 1 calc PR G 1 H23B H 0.5095 0.4276 0.5253 0.059 Uiso 0.75 1 calc PR G 1 C21T C 0.5695(3) 0.3781(3) 0.5074(3) 0.0437(15) Uiso 0.75 1 d P G 1 H21A H 0.5632 0.3489 0.5378 0.052 Uiso 0.75 1 calc PR G 1 H21B H 0.6099 0.3880 0.5254 0.052 Uiso 0.75 1 calc PR G 1 C22T C 0.5490(3) 0.3546(3) 0.4344(3) 0.0402(15) Uani 0.75 1 d P G 1 H22A H 0.5800 0.3355 0.4264 0.048 Uiso 0.75 1 calc PR G 1 H22B H 0.5183 0.3257 0.4252 0.048 Uiso 0.75 1 calc PR G 1 O6T O 0.5291(2) 0.40635(19) 0.3917(2) 0.0435(10) Uani 0.75 1 d P G 1 C24T C 0.5005(3) 0.4392(3) 0.4249(4) 0.0473(18) Uani 0.75 1 d P G 1 H24A H 0.4621 0.4238 0.4122 0.057 Uiso 0.75 1 calc PR G 1 H24B H 0.4980 0.4811 0.4116 0.057 Uiso 0.75 1 calc PR G 1 C5A C 0.5288(12) 0.3756(12) 0.4439(14) 0.0774(19) Uiso 0.25 1 d PD H 2 H5A1 H 0.5071 0.3390 0.4345 0.116 Uiso 0.25 1 calc PR H 2 H5A2 H 0.5391 0.3870 0.4915 0.116 Uiso 0.25 1 calc PR H 2 H5A3 H 0.5628 0.3697 0.4357 0.116 Uiso 0.25 1 calc PR H 2 C6A C 0.4926(15) 0.4253(12) 0.3963(13) 0.0774(19) Uiso 0.25 1 d PD H 2 N3A N 0.4661(9) 0.4513(10) 0.3489(11) 0.0774(19) Uiso 0.25 1 d PD H 2 C1A C 0.2963(2) 0.2695(3) 0.5714(3) 0.0600(16) Uani 1 1 d D . . H1A1 H 0.3208 0.2613 0.6190 0.090 Uiso 1 1 calc R . . H1A2 H 0.3020 0.3102 0.5604 0.090 Uiso 1 1 calc R . . H1A3 H 0.3055 0.2426 0.5418 0.090 Uiso 1 1 calc R . . C2A C 0.2391(3) 0.2615(3) 0.5614(3) 0.0656(16) Uani 1 1 d D . . N1A N 0.1939(3) 0.2540(3) 0.5555(4) 0.107(2) Uani 1 1 d . . . C3A C 0.8192(6) 0.9881(6) 1.0765(7) 0.0774(19) Uiso 0.50 1 d P I 1 H3A1 H 0.8576 0.9785 1.0827 0.116 Uiso 0.50 1 calc PR I 1 H3A2 H 0.8170 0.9899 1.1210 0.116 Uiso 0.50 1 calc PR I 1 H3A3 H 0.8085 1.0262 1.0538 0.116 Uiso 0.50 1 calc PR I 1 N2A N 0.7524(5) 0.9071(5) 1.0016(6) 0.0774(19) Uiso 0.50 1 d P I 1 C4A C 0.7816(6) 0.9434(7) 1.0356(8) 0.0774(19) Uiso 0.50 1 d P I 1 O1W O 0.8174(8) 0.7492(9) 0.8631(10) 0.080(5) Uiso 0.25 1 d P J 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 C1 0.040(2) 0.045(3) 0.017(2) 0.0069(18) 0.0031(17) 0.0154(19) C2 0.0243(18) 0.030(2) 0.0162(18) 0.0037(15) 0.0028(14) 0.0072(15) C3 0.0250(18) 0.0225(19) 0.0148(17) 0.0009(14) 0.0063(14) 0.0033(14) C4 0.0189(16) 0.0184(17) 0.0096(16) -0.0013(13) 0.0037(12) -0.0011(12) C5 0.030(2) 0.037(2) 0.0141(18) -0.0041(16) 0.0062(15) 0.0099(16) C6 0.032(2) 0.043(3) 0.0102(17) -0.0018(16) 0.0021(15) 0.0065(17) C7 0.0180(16) 0.0144(17) 0.0141(16) -0.0006(13) 0.0052(13) -0.0029(12) C8 0.0179(15) 0.0142(16) 0.0133(16) 0.0002(13) 0.0046(12) -0.0011(12) C9 0.0213(17) 0.0108(16) 0.0188(17) -0.0008(13) 0.0075(13) -0.0008(12) C10 0.0246(18) 0.0182(18) 0.0198(18) -0.0033(14) 0.0073(14) 0.0037(14) C11 0.0262(18) 0.0211(19) 0.0152(17) -0.0017(14) 0.0082(14) 0.0021(14) C12 0.0195(16) 0.0142(17) 0.0200(18) -0.0021(14) 0.0039(13) 0.0030(13) C13 0.0283(19) 0.0151(18) 0.0208(19) 0.0036(14) 0.0055(15) 0.0057(14) C14 0.0219(16) 0.0078(15) 0.0185(17) 0.0019(13) 0.0071(13) 0.0015(12) C15 0.0249(17) 0.0106(16) 0.0164(17) 0.0049(13) 0.0077(14) 0.0012(13) C16 0.031(2) 0.0169(18) 0.023(2) 0.0031(15) 0.0050(15) 0.0093(15) C17 0.052(3) 0.023(2) 0.026(2) -0.0025(17) 0.0097(19) 0.0178(19) C18 0.046(2) 0.022(2) 0.024(2) -0.0050(16) 0.0029(18) 0.0145(18) C19 0.0218(17) 0.0101(16) 0.0216(18) 0.0017(13) 0.0057(14) 0.0016(12) C20 0.0210(17) 0.0122(16) 0.0175(17) -0.0028(13) 0.0051(13) 0.0016(12) C21 0.0208(16) 0.0109(16) 0.0125(16) 0.0018(12) 0.0064(13) 0.0032(12) C22 0.0235(17) 0.0162(17) 0.0133(16) 0.0044(13) 0.0038(13) 0.0060(13) C23 0.037(2) 0.0208(19) 0.0169(18) 0.0077(15) 0.0083(16) 0.0013(15) C24 0.034(2) 0.0166(18) 0.027(2) 0.0071(15) 0.0132(16) -0.0016(15) C25 0.0300(19) 0.028(2) 0.0126(17) 0.0020(15) 0.0030(14) -0.0005(15) C26 0.048(3) 0.038(3) 0.018(2) -0.0084(18) 0.0036(18) -0.013(2) C27 0.079(4) 0.083(4) 0.012(2) -0.006(2) -0.004(2) -0.037(3) C28 0.077(4) 0.087(4) 0.014(2) 0.012(2) -0.005(2) -0.032(3) C29 0.054(3) 0.051(3) 0.017(2) 0.007(2) 0.0023(19) -0.014(2) C30 0.125(5) 0.115(5) 0.026(3) -0.016(3) -0.002(3) -0.069(5) C31 0.025(2) 0.038(2) 0.042(3) 0.002(2) 0.0204(18) 0.0068(17) C32 0.0169(17) 0.032(2) 0.0202(18) 0.0024(15) 0.0089(14) 0.0049(14) C33 0.0187(16) 0.0231(19) 0.0152(17) 0.0024(14) 0.0084(13) -0.0001(13) C34 0.0172(16) 0.0197(18) 0.0166(17) 0.0021(14) 0.0065(13) 0.0033(13) C35 0.029(2) 0.0180(19) 0.043(2) -0.0005(17) 0.0189(18) 0.0002(15) C36 0.027(2) 0.030(2) 0.041(2) 0.0028(18) 0.0184(18) 0.0107(16) C37 0.0190(16) 0.0190(18) 0.0183(17) 0.0017(14) 0.0082(13) 0.0024(13) C38 0.0195(16) 0.0158(17) 0.0104(15) -0.0004(12) 0.0075(12) 0.0022(12) C39 0.0176(16) 0.0192(18) 0.0145(17) 0.0007(13) 0.0056(13) 0.0009(13) C40 0.0275(19) 0.0160(18) 0.036(2) -0.0001(16) 0.0156(16) -0.0035(14) C41 0.0254(19) 0.0170(19) 0.043(2) 0.0007(17) 0.0154(17) 0.0028(14) C42 0.0198(17) 0.0223(18) 0.0172(17) -0.0001(14) 0.0107(13) 0.0003(13) C43 0.0184(16) 0.0092(15) 0.0177(17) 0.0016(13) 0.0093(13) -0.0015(12) C44 0.0204(16) 0.0140(16) 0.0113(16) 0.0002(12) 0.0073(13) -0.0013(12) C45 0.0167(15) 0.0130(16) 0.0126(16) 0.0010(12) 0.0045(12) -0.0004(12) C46 0.0241(17) 0.0148(17) 0.0187(18) 0.0004(14) 0.0119(14) 0.0020(13) C47 0.0271(18) 0.0223(19) 0.0115(16) 0.0021(14) 0.0096(14) 0.0010(14) C48 0.0253(17) 0.0137(17) 0.0136(17) 0.0040(13) 0.0059(13) 0.0007(13) C49 0.0223(17) 0.0235(19) 0.0102(16) -0.0009(14) 0.0059(13) 0.0048(14) C50 0.0183(16) 0.0159(17) 0.0139(16) 0.0007(13) 0.0065(13) -0.0010(12) C51 0.0171(16) 0.0142(16) 0.0153(16) -0.0031(13) 0.0088(13) 0.0002(12) C52 0.0171(15) 0.0098(15) 0.0203(17) -0.0012(13) 0.0103(13) -0.0016(12) C53 0.0226(17) 0.0169(17) 0.0180(17) -0.0052(14) 0.0111(14) 0.0007(13) C54 0.0248(17) 0.0189(18) 0.0115(16) -0.0038(13) 0.0086(13) -0.0008(13) C55 0.0163(15) 0.0097(16) 0.0207(17) -0.0005(13) 0.0077(13) -0.0022(12) C56 0.0207(17) 0.0160(18) 0.0217(19) -0.0037(14) 0.0014(14) -0.0013(13) C57 0.0185(17) 0.0095(16) 0.037(2) -0.0009(15) 0.0041(15) 0.0010(13) C58 0.0184(17) 0.0124(17) 0.037(2) -0.0009(15) 0.0127(15) 0.0016(13) C59 0.0208(17) 0.0136(17) 0.028(2) -0.0018(14) 0.0119(15) -0.0022(13) C60 0.028(2) 0.022(2) 0.045(3) 0.0012(19) -0.0017(18) 0.0096(16) C61 0.031(2) 0.037(2) 0.026(2) -0.0038(18) 0.0055(17) -0.0132(17) C62 0.0240(19) 0.028(2) 0.0203(19) -0.0036(16) 0.0033(15) -0.0088(15) C63 0.0183(16) 0.0238(19) 0.0157(17) -0.0015(14) 0.0060(13) -0.0025(13) C64 0.0259(18) 0.0195(18) 0.0160(17) 0.0003(14) 0.0062(14) -0.0040(14) C65 0.046(3) 0.036(3) 0.021(2) 0.0093(18) 0.0012(18) -0.017(2) C66 0.048(3) 0.031(2) 0.031(2) 0.0040(19) 0.009(2) -0.022(2) C67 0.0232(17) 0.0207(18) 0.0161(17) -0.0006(14) 0.0078(14) -0.0044(13) C68 0.0183(16) 0.0190(18) 0.0128(16) -0.0020(13) 0.0072(13) -0.0004(12) C69 0.0189(16) 0.027(2) 0.0115(16) -0.0011(14) 0.0053(13) -0.0003(13) C70 0.031(2) 0.031(2) 0.0159(18) 0.0058(16) 0.0039(15) -0.0030(16) C71 0.039(2) 0.028(2) 0.0184(19) 0.0065(16) 0.0050(16) -0.0101(17) C72 0.0213(17) 0.033(2) 0.0113(17) -0.0017(15) 0.0051(13) -0.0046(14) C73 0.0206(16) 0.0207(18) 0.0118(16) -0.0033(13) 0.0068(13) 0.0037(13) C74 0.0230(17) 0.0208(18) 0.0097(16) -0.0001(13) 0.0054(13) 0.0051(13) C75 0.0239(17) 0.0168(17) 0.0165(17) -0.0052(14) 0.0089(14) 0.0030(13) C76 0.0301(19) 0.032(2) 0.0102(17) -0.0029(15) 0.0041(14) 0.0079(16) C77 0.032(2) 0.034(2) 0.0111(17) 0.0007(15) 0.0077(15) 0.0060(16) C78 0.0284(19) 0.0241(19) 0.0149(17) -0.0007(14) 0.0103(14) 0.0033(14) C79 0.0217(17) 0.027(2) 0.0132(17) -0.0029(14) 0.0040(13) 0.0037(14) C80 0.0227(17) 0.0242(19) 0.0094(16) -0.0010(14) 0.0044(13) 0.0046(14) C81 0.0182(16) 0.0196(18) 0.0113(16) -0.0043(13) 0.0049(12) -0.0007(13) C82 0.0209(16) 0.0172(17) 0.0100(16) -0.0016(13) 0.0031(13) 0.0009(13) C83 0.0262(18) 0.0133(17) 0.0198(18) -0.0040(14) 0.0048(14) 0.0001(13) C84 0.0262(18) 0.0198(18) 0.0172(18) -0.0075(14) 0.0051(14) 0.0078(14) C85 0.0211(17) 0.0171(18) 0.0157(17) -0.0040(14) 0.0025(13) 0.0001(13) C86 0.0214(17) 0.0169(18) 0.0206(18) -0.0045(14) 0.0072(14) -0.0018(13) C87 0.0205(17) 0.0227(19) 0.0203(18) -0.0011(15) 0.0047(14) -0.0014(14) C88 0.031(2) 0.0169(19) 0.046(3) -0.0034(18) 0.0153(18) -0.0063(15) C89 0.034(2) 0.0125(18) 0.049(3) -0.0058(17) 0.0219(19) 0.0002(15) C90 0.027(2) 0.026(2) 0.038(2) -0.0008(18) 0.0133(17) -0.0066(16) N1 0.0160(13) 0.0165(15) 0.0134(14) -0.0013(11) 0.0042(11) -0.0010(10) N2 0.0158(13) 0.0132(14) 0.0117(13) 0.0002(11) 0.0043(10) -0.0004(10) N3 0.0207(14) 0.0120(14) 0.0121(14) 0.0018(11) 0.0055(11) 0.0031(10) N4 0.0270(16) 0.0241(17) 0.0118(15) -0.0055(12) 0.0015(12) 0.0013(12) N5 0.0146(13) 0.0203(15) 0.0086(13) 0.0000(11) 0.0035(10) 0.0017(10) N6 0.0157(13) 0.0158(14) 0.0109(13) -0.0007(11) 0.0054(10) 0.0002(10) N7 0.0179(13) 0.0088(13) 0.0146(14) -0.0014(11) 0.0067(11) 0.0001(10) N8 0.0177(14) 0.0100(13) 0.0150(14) -0.0021(11) 0.0007(11) -0.0013(10) N9 0.0173(13) 0.0178(15) 0.0129(14) -0.0013(11) 0.0061(11) -0.0004(11) N10 0.0171(13) 0.0174(15) 0.0111(13) -0.0007(11) 0.0057(11) 0.0011(10) N11 0.0217(14) 0.0132(14) 0.0085(13) -0.0004(11) 0.0043(11) 0.0002(11) N12 0.0176(14) 0.0135(14) 0.0148(14) -0.0031(11) 0.0038(11) -0.0003(10) F1 0.195(5) 0.096(3) 0.049(2) -0.045(2) -0.066(3) 0.072(3) F2 0.0341(14) 0.0411(16) 0.0469(17) -0.0087(13) -0.0003(12) 0.0000(11) F3 0.0513(16) 0.0497(18) 0.0398(16) -0.0082(13) 0.0023(13) 0.0172(13) F4 0.157(4) 0.057(2) 0.055(2) -0.0142(18) 0.015(2) 0.056(2) F5 0.062(2) 0.093(3) 0.108(3) 0.018(2) 0.023(2) -0.034(2) F6 0.214(6) 0.130(4) 0.145(5) 0.076(4) 0.154(5) 0.078(4) F7 0.0315(14) 0.066(2) 0.061(2) -0.0128(16) 0.0176(13) 0.0140(13) F8 0.0621(18) 0.0473(17) 0.0372(15) -0.0017(13) 0.0279(14) 0.0051(13) F9 0.0499(15) 0.0382(15) 0.0311(14) 0.0019(11) 0.0136(12) -0.0063(12) F10 0.0472(18) 0.065(2) 0.082(2) -0.0311(19) 0.0211(16) -0.0186(15) F11 0.087(2) 0.064(2) 0.0285(16) -0.0034(15) -0.0209(15) 0.0309(18) F12 0.0417(14) 0.0389(15) 0.0345(14) 0.0149(11) 0.0182(11) 0.0126(11) F13 0.0748(19) 0.0356(15) 0.0244(13) 0.0006(11) 0.0186(13) -0.0069(13) F14 0.0692(19) 0.0499(17) 0.0217(13) -0.0095(12) 0.0131(13) -0.0145(14) F15 0.102(2) 0.0338(15) 0.0373(16) -0.0083(12) 0.0377(16) -0.0323(15) F16 0.0393(13) 0.0247(12) 0.0418(15) 0.0030(10) 0.0255(11) -0.0031(10) F17 0.085(2) 0.0373(16) 0.0586(19) 0.0183(14) 0.0481(17) 0.0359(15) F18 0.0513(17) 0.0552(18) 0.0624(19) 0.0014(15) 0.0423(15) 0.0037(13) F19 0.0668(18) 0.0438(16) 0.0330(14) -0.0189(12) 0.0306(13) -0.0138(13) F20 0.0559(15) 0.0361(14) 0.0187(12) -0.0025(10) 0.0167(11) 0.0087(11) F21 0.0504(15) 0.0335(14) 0.0219(12) -0.0071(10) 0.0076(11) -0.0011(11) F22 0.0499(16) 0.0496(17) 0.0319(14) -0.0197(13) 0.0110(12) -0.0110(13) F23 0.103(2) 0.0186(13) 0.0170(12) 0.0004(10) 0.0148(14) 0.0073(13) F24 0.0696(18) 0.0224(13) 0.0250(13) 0.0019(10) 0.0107(12) 0.0176(12) P1 0.0585(8) 0.0334(7) 0.0210(6) -0.0061(5) 0.0058(5) 0.0083(5) P2 0.0268(5) 0.0338(6) 0.0264(6) -0.0007(5) 0.0030(4) 0.0070(4) P3 0.0443(6) 0.0149(5) 0.0229(5) -0.0031(4) 0.0225(4) -0.0017(4) P4 0.0471(6) 0.0169(5) 0.0127(5) -0.0031(4) 0.0092(4) 0.0034(4) Ni1 0.0149(2) 0.0138(2) 0.0097(2) 0.00032(16) 0.00401(15) 0.00082(15) Ni2 0.0174(2) 0.0107(2) 0.0107(2) -0.00254(16) 0.00324(16) 0.00113(15) O1 0.0305(14) 0.0174(13) 0.0217(14) -0.0050(11) 0.0001(11) 0.0105(10) O2 0.0250(12) 0.0103(12) 0.0180(13) 0.0017(10) 0.0041(10) 0.0047(9) O3 0.0200(12) 0.0213(13) 0.0151(12) 0.0043(10) 0.0079(9) 0.0052(9) O4 0.0185(12) 0.0313(15) 0.0110(12) -0.0017(10) 0.0055(9) 0.0058(10) O5 0.0207(12) 0.0329(15) 0.0089(11) -0.0003(10) 0.0050(9) -0.0006(10) O6 0.0234(13) 0.0340(15) 0.0115(12) -0.0085(11) 0.0059(10) -0.0021(11) O1T 0.133(5) 0.106(4) 0.086(4) 0.010(3) 0.070(4) 0.052(4) C1T 0.093(5) 0.116(7) 0.075(5) 0.008(5) 0.053(4) 0.041(5) C2T 0.098(6) 0.088(6) 0.083(6) 0.019(5) 0.010(5) 0.000(5) C3T 0.104(6) 0.086(5) 0.063(4) 0.016(4) 0.036(4) 0.039(4) C4T 0.073(5) 0.125(7) 0.071(5) 0.020(5) 0.047(4) 0.042(4) O2T 0.049(2) 0.027(2) 0.036(2) -0.0024(18) 0.0022(19) 0.0062(18) C5T 0.068(4) 0.029(3) 0.026(3) 0.015(3) -0.014(3) -0.018(3) C6T 0.057(4) 0.025(3) 0.035(3) 0.000(2) 0.018(3) -0.014(3) C7T 0.103(6) 0.037(4) 0.049(4) -0.011(3) 0.041(4) -0.040(4) C8T 0.042(4) 0.058(5) 0.034(4) -0.013(3) 0.006(3) -0.002(3) C16T 0.109(7) 0.044(4) 0.041(4) -0.007(3) 0.019(4) -0.024(4) C13T 0.094(6) 0.036(4) 0.045(4) 0.010(3) 0.009(4) -0.001(4) C14T 0.069(5) 0.056(5) 0.047(4) 0.015(4) 0.008(4) -0.005(4) C15T 0.130(9) 0.069(6) 0.065(6) -0.018(5) 0.043(6) -0.050(6) O4T 0.063(3) 0.037(3) 0.070(4) -0.001(2) 0.032(3) -0.019(2) O5T 0.103(3) 0.0304(19) 0.070(3) 0.0151(18) 0.054(3) 0.0246(19) C20T 0.071(4) 0.069(4) 0.085(5) 0.025(4) 0.053(4) 0.022(3) C18T 0.042(10) 0.17(2) 0.075(12) -0.067(12) -0.019(8) 0.059(13) C17T 0.121(6) 0.077(5) 0.069(5) 0.004(4) 0.056(5) 0.032(4) C19T 0.093(6) 0.045(4) 0.151(9) -0.026(5) 0.040(6) 0.005(4) C18A 0.063(15) 0.22(3) 0.18(2) -0.15(2) 0.026(15) 0.031(17) C17A 0.121(6) 0.077(5) 0.069(5) 0.004(4) 0.056(5) 0.032(4) C19A 0.093(6) 0.045(4) 0.151(9) -0.026(5) 0.040(6) 0.005(4) C23T 0.063(4) 0.045(4) 0.051(4) -0.007(3) 0.034(4) 0.000(3) C22T 0.047(4) 0.034(4) 0.040(4) -0.002(3) 0.017(3) 0.008(3) O6T 0.060(3) 0.036(2) 0.038(3) -0.005(2) 0.024(2) -0.005(2) C24T 0.054(4) 0.053(4) 0.045(4) 0.005(3) 0.030(4) 0.013(3) C1A 0.056(3) 0.068(4) 0.045(3) -0.034(3) 0.010(3) -0.003(3) C2A 0.083(5) 0.068(4) 0.053(4) 0.004(3) 0.034(3) 0.005(3) N1A 0.096(5) 0.120(6) 0.125(6) 0.032(5) 0.066(5) 0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.506(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C6 1.373(5) . ? C2 C3 1.389(5) . ? C3 N1 1.336(4) . ? C3 H3 0.9500 . ? C4 N1 1.349(4) . ? C4 C5 1.385(5) . ? C4 C7 1.480(5) . ? C5 C6 1.392(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 N2 1.349(4) . ? C7 C11 1.383(5) . ? C8 N2 1.336(4) . ? C8 C9 1.385(5) . ? C8 H8 0.9500 . ? C9 C10 1.376(5) . ? C9 C12 1.504(5) . ? C10 C11 1.396(5) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 O1 1.418(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O1 1.375(4) . ? C13 C18 1.386(5) . ? C13 C14 1.389(5) . ? C14 C15 1.393(5) . ? C14 H14 0.9500 . ? C15 O2 1.371(4) . ? C15 C16 1.390(5) . ? C16 C17 1.381(6) . ? C16 H16 0.9500 . ? C17 C18 1.387(6) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 O2 1.433(4) . ? C19 C20 1.498(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.380(5) . ? C20 C24 1.390(5) . ? C21 N3 1.342(4) . ? C21 H21 0.9500 . ? C22 N3 1.339(4) . ? C22 C23 1.383(5) . ? C22 C25 1.479(5) . ? C23 C24 1.375(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 N4 1.345(5) . ? C25 C29 1.390(5) . ? C26 N4 1.326(5) . ? C26 C27 1.396(6) . ? C26 H26 0.9500 . ? C27 C28 1.372(8) . ? C27 C30 1.515(7) . ? C28 C29 1.384(7) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.498(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C36 1.376(6) . ? C32 C33 1.395(5) . ? C33 N5 1.334(4) . ? C33 H33 0.9500 . ? C34 N5 1.343(5) . ? C34 C35 1.382(5) . ? C34 C37 1.484(5) . ? C35 C36 1.384(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 N6 1.349(4) . ? C37 C41 1.382(5) . ? C38 N6 1.340(4) . ? C38 C39 1.381(5) . ? C38 H38 0.9500 . ? C39 C40 1.396(5) . ? C39 C42 1.498(4) . ? C40 C41 1.375(5) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 O3 1.435(4) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 O3 1.372(4) . ? C43 C48 1.390(5) . ? C43 C44 1.393(5) . ? C44 C45 1.387(4) . ? C44 H44 0.9500 . ? C45 O4 1.371(4) . ? C45 C46 1.382(5) . ? C46 C47 1.387(5) . ? C46 H46 0.9500 . ? C47 C48 1.392(5) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 O4 1.421(4) . ? C49 C50 1.505(5) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.387(5) . ? C50 C54 1.389(5) . ? C51 N7 1.338(4) . ? C51 H51 0.9500 . ? C52 N7 1.348(4) . ? C52 C53 1.383(5) . ? C52 C55 1.475(5) . ? C53 C54 1.387(5) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 N8 1.351(4) . ? C55 C59 1.392(5) . ? C56 N8 1.342(4) . ? C56 C57 1.382(5) . ? C56 H56 0.9500 . ? C57 C58 1.383(6) . ? C57 C60 1.507(5) . ? C58 C59 1.376(5) . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.506(5) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C66 1.381(6) . ? C62 C63 1.383(5) . ? C63 N9 1.342(4) . ? C63 H63 0.9500 . ? C64 N9 1.343(4) . ? C64 C65 1.383(5) . ? C64 C67 1.482(5) . ? C65 C66 1.389(6) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 N10 1.351(4) . ? C67 C71 1.384(5) . ? C68 N10 1.338(4) . ? C68 C69 1.391(5) . ? C68 H68 0.9500 . ? C69 C70 1.373(5) . ? C69 C72 1.504(5) . ? C70 C71 1.379(5) . ? C70 H70 0.9500 . ? C71 H71 0.9500 . ? C72 O5 1.428(4) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 O5 1.376(4) . ? C73 C78 1.377(5) . ? C73 C74 1.391(5) . ? C74 C75 1.389(5) . ? C74 H74 0.9500 . ? C75 O6 1.373(4) . ? C75 C76 1.393(5) . ? C76 C77 1.380(6) . ? C76 H76 0.9500 . ? C77 C78 1.386(5) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 O6 1.423(4) . ? C79 C80 1.490(5) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 C84 1.378(5) . ? C80 C81 1.384(5) . ? C81 N11 1.339(4) . ? C81 H81 0.9500 . ? C82 N11 1.349(4) . ? C82 C83 1.384(5) . ? C82 C85 1.471(5) . ? C83 C84 1.379(5) . ? C83 H83 0.9500 . ? C84 H84 0.9500 . ? C85 N12 1.340(4) . ? C85 C89 1.375(5) . ? C86 N12 1.341(4) . ? C86 C87 1.389(5) . ? C86 H86 0.9500 . ? C87 C88 1.372(5) . ? C87 C90 1.511(5) . ? C88 C89 1.380(6) . ? C88 H88 0.9500 . ? C89 H89 0.9500 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? N1 Ni1 2.082(3) . ? N2 Ni1 2.093(3) . ? N3 Ni2 2.093(3) . ? N4 Ni2 2.083(3) . ? N5 Ni1 2.070(3) . ? N6 Ni1 2.098(3) . ? N7 Ni2 2.079(3) . ? N8 Ni2 2.089(3) . ? N9 Ni1 2.099(3) . ? N10 Ni1 2.075(3) . ? N11 Ni2 2.079(3) . ? N12 Ni2 2.076(3) . ? F1 P1 1.566(4) . ? F2 P1 1.594(3) . ? F3 P1 1.601(3) . ? F4 P1 1.575(3) . ? F5 P1 1.587(4) . ? F6 P1 1.565(5) . ? F7 P2 1.596(3) . ? F8 P2 1.602(3) . ? F9 P2 1.598(3) . ? F10 P2 1.589(3) . ? F11 P2 1.584(3) . ? F12 P2 1.607(3) . ? F13 P3 1.633(3) . ? F14 P3 1.567(3) . ? F15 P3 1.601(3) . ? F16 P3 1.579(2) . ? F17 P3 1.585(3) . ? F18 P3 1.600(3) . ? F19 P4 1.596(3) . ? F20 P4 1.599(2) . ? F21 P4 1.599(3) . ? F22 P4 1.591(3) . ? F23 P4 1.611(3) . ? F24 P4 1.587(3) . ? O1T C1T 1.436(9) . ? O1T C4T 1.453(10) . ? C1T C2T 1.548(11) . ? C1T H1T1 0.9900 . ? C1T H1T2 0.9900 . ? C2T C3T 1.446(10) . ? C2T H2T1 0.9900 . ? C2T H2T2 0.9900 . ? C3T C4T 1.445(10) . ? C3T H3T1 0.9900 . ? C3T H3T2 0.9900 . ? C4T H4T1 0.9900 . ? C4T H4T2 0.9900 . ? O2T C5T 1.417(7) . ? O2T C8T 1.439(7) . ? C5T C6T 1.452(8) . ? C5T H5T1 0.9900 . ? C5T H5T2 0.9900 . ? C6T C7T 1.495(9) . ? C6T H6T1 0.9900 . ? C6T H6T2 0.9900 . ? C7T C8T 1.470(10) . ? C7T H7T1 0.9900 . ? C7T H7T2 0.9900 . ? C8T H8T1 0.9900 . ? C8T H8T2 0.9900 . ? C9T O3T 1.357(9) . ? C9T C10T 1.516(9) . ? C9T H9T1 0.9900 . ? C9T H9T2 0.9900 . ? O3T C12T 1.276(9) . ? C10T C11T 1.531(9) . ? C10T H10A 0.9900 . ? C10T H10B 0.9900 . ? C11T C12T 1.567(9) . ? C11T H11A 0.9900 . ? C11T H11B 0.9900 . ? C12T H12C 0.9900 . ? C12T H12D 0.9900 . ? C9A O3TA 1.339(10) . ? C9A C11A 1.52(4) . ? C9A H9A1 0.9900 . ? C9A H9A2 0.9900 . ? O3TA C10A 1.319(10) . ? C10A C12A 1.539(10) . ? C10A H10C 0.9900 . ? C10A H10D 0.9900 . ? C11A C12A 1.46(3) . ? C11A H11C 0.9900 . ? C11A H11D 0.9900 . ? C12A H12E 0.9900 . ? C12A H12F 0.9900 . ? O3TB C11B 1.40(3) . ? O3TB C9B 1.52(3) . ? C9B C10B 1.68(4) . ? C9B H9B1 0.9900 . ? C9B H9B2 0.9900 . ? C10B C12B 1.552(10) . ? C10B H10E 0.9900 . ? C10B H10F 0.9900 . ? C11B C12B 1.557(10) . ? C11B H11E 0.9900 . ? C11B H11F 0.9900 . ? C12B H12G 0.9900 . ? C12B H12H 0.9900 . ? C16T O4T 1.331(9) . ? C16T C13T 1.588(12) . ? C16T H16A 0.9900 . ? C16T H16B 0.9900 . ? C13T C14T 1.533(11) . ? C13T H13A 0.9900 . ? C13T H13B 0.9900 . ? C14T C15T 1.486(11) . ? C14T H14A 0.9900 . ? C14T H14B 0.9900 . ? C15T O4T 1.436(9) . ? C15T H15A 0.9900 . ? C15T H15B 0.9900 . ? O5T C17T 1.395(8) . ? O5T C20T 1.405(7) . ? C20T C19T 1.439(10) . ? C20T H20A 0.9900 . ? C20T H20B 0.9900 . ? C18T C17T 1.45(2) . ? C18T C19T 1.57(3) . ? C18T H18A 0.9900 . ? C18T H18B 0.9900 . ? C17T H17A 0.9900 . ? C17T H17B 0.9900 . ? C19T H19C 0.9900 . ? C19T H19D 0.9900 . ? C18A H18C 0.9900 . ? C18A H18D 0.9900 . ? C23T C21T 1.512(9) . ? C23T C24T 1.520(10) . ? C23T H23A 0.9900 . ? C23T H23B 0.9900 . ? C21T C22T 1.535(9) . ? C21T H21A 0.9900 . ? C21T H21B 0.9900 . ? C22T O6T 1.454(8) . ? C22T H22A 0.9900 . ? C22T H22B 0.9900 . ? O6T C24T 1.429(8) . ? C24T H24A 0.9900 . ? C24T H24B 0.9900 . ? C5A C6A 1.561(9) . ? C5A H5A1 0.9800 . ? C5A H5A2 0.9800 . ? C5A H5A3 0.9800 . ? C6A N3A 1.140(9) . ? C1A C2A 1.428(7) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C2A N1A 1.145(8) . ? C3A C4A 1.439(19) . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3A H3A3 0.9800 . ? N2A C4A 1.160(17) . ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C6 C2 C3 117.2(3) . . ? C6 C2 C1 121.8(3) . . ? C3 C2 C1 121.0(3) . . ? N1 C3 C2 123.8(3) . . ? N1 C3 H3 118.1 . . ? C2 C3 H3 118.1 . . ? N1 C4 C5 120.9(3) . . ? N1 C4 C7 115.8(3) . . ? C5 C4 C7 123.3(3) . . ? C4 C5 C6 119.4(3) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C2 C6 C5 119.9(3) . . ? C2 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? N2 C7 C11 121.5(3) . . ? N2 C7 C4 115.8(3) . . ? C11 C7 C4 122.8(3) . . ? N2 C8 C9 123.5(3) . . ? N2 C8 H8 118.3 . . ? C9 C8 H8 118.3 . . ? C10 C9 C8 117.9(3) . . ? C10 C9 C12 124.2(3) . . ? C8 C9 C12 117.8(3) . . ? C9 C10 C11 119.4(3) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C7 C11 C10 119.1(3) . . ? C7 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? O1 C12 C9 109.8(3) . . ? O1 C12 H12A 109.7 . . ? C9 C12 H12A 109.7 . . ? O1 C12 H12B 109.7 . . ? C9 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? O1 C13 C18 116.4(3) . . ? O1 C13 C14 122.7(3) . . ? C18 C13 C14 120.9(3) . . ? C13 C14 C15 118.9(3) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? O2 C15 C16 116.1(3) . . ? O2 C15 C14 123.0(3) . . ? C16 C15 C14 120.9(3) . . ? C17 C16 C15 118.7(3) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C16 C17 C18 121.5(4) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C13 C18 C17 118.9(4) . . ? C13 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? O2 C19 C20 107.5(3) . . ? O2 C19 H19A 110.2 . . ? C20 C19 H19A 110.2 . . ? O2 C19 H19B 110.2 . . ? C20 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? C21 C20 C24 117.4(3) . . ? C21 C20 C19 120.8(3) . . ? C24 C20 C19 121.9(3) . . ? N3 C21 C20 123.6(3) . . ? N3 C21 H21 118.2 . . ? C20 C21 H21 118.2 . . ? N3 C22 C23 121.9(3) . . ? N3 C22 C25 115.2(3) . . ? C23 C22 C25 122.8(3) . . ? C24 C23 C22 119.2(3) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C23 C24 C20 119.7(3) . . ? C23 C24 H24 120.2 . . ? C20 C24 H24 120.2 . . ? N4 C25 C29 121.2(4) . . ? N4 C25 C22 115.9(3) . . ? C29 C25 C22 122.9(4) . . ? N4 C26 C27 123.6(4) . . ? N4 C26 H26 118.2 . . ? C27 C26 H26 118.2 . . ? C28 C27 C26 116.5(4) . . ? C28 C27 C30 123.8(5) . . ? C26 C27 C30 119.7(5) . . ? C27 C28 C29 121.1(4) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C28 C29 C25 118.3(4) . . ? C28 C29 H29 120.9 . . ? C25 C29 H29 120.9 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C36 C32 C33 116.5(3) . . ? C36 C32 C31 122.4(3) . . ? C33 C32 C31 121.1(4) . . ? N5 C33 C32 123.9(3) . . ? N5 C33 H33 118.0 . . ? C32 C33 H33 118.0 . . ? N5 C34 C35 121.7(3) . . ? N5 C34 C37 115.7(3) . . ? C35 C34 C37 122.5(3) . . ? C34 C35 C36 118.9(4) . . ? C34 C35 H35 120.6 . . ? C36 C35 H35 120.6 . . ? C32 C36 C35 120.6(4) . . ? C32 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? N6 C37 C41 122.0(3) . . ? N6 C37 C34 114.6(3) . . ? C41 C37 C34 123.4(3) . . ? N6 C38 C39 123.8(3) . . ? N6 C38 H38 118.1 . . ? C39 C38 H38 118.1 . . ? C38 C39 C40 117.5(3) . . ? C38 C39 C42 120.2(3) . . ? C40 C39 C42 122.2(3) . . ? C41 C40 C39 119.2(3) . . ? C41 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C40 C41 C37 119.5(3) . . ? C40 C41 H41 120.3 . . ? C37 C41 H41 120.3 . . ? O3 C42 C39 108.7(3) . . ? O3 C42 H42A 109.9 . . ? C39 C42 H42A 109.9 . . ? O3 C42 H42B 109.9 . . ? C39 C42 H42B 109.9 . . ? H42A C42 H42B 108.3 . . ? O3 C43 C48 115.4(3) . . ? O3 C43 C44 123.2(3) . . ? C48 C43 C44 121.3(3) . . ? C45 C44 C43 118.4(3) . . ? C45 C44 H44 120.8 . . ? C43 C44 H44 120.8 . . ? O4 C45 C46 115.7(3) . . ? O4 C45 C44 123.1(3) . . ? C46 C45 C44 121.1(3) . . ? C45 C46 C47 119.6(3) . . ? C45 C46 H46 120.2 . . ? C47 C46 H46 120.2 . . ? C46 C47 C48 120.5(3) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C43 C48 C47 118.8(3) . . ? C43 C48 H48 120.6 . . ? C47 C48 H48 120.6 . . ? O4 C49 C50 107.8(3) . . ? O4 C49 H49A 110.1 . . ? C50 C49 H49A 110.1 . . ? O4 C49 H49B 110.1 . . ? C50 C49 H49B 110.1 . . ? H49A C49 H49B 108.5 . . ? C51 C50 C54 117.5(3) . . ? C51 C50 C49 119.9(3) . . ? C54 C50 C49 122.5(3) . . ? N7 C51 C50 123.2(3) . . ? N7 C51 H51 118.4 . . ? C50 C51 H51 118.4 . . ? N7 C52 C53 121.0(3) . . ? N7 C52 C55 116.0(3) . . ? C53 C52 C55 123.0(3) . . ? C52 C53 C54 119.6(3) . . ? C52 C53 H53 120.2 . . ? C54 C53 H53 120.2 . . ? C53 C54 C50 119.5(3) . . ? C53 C54 H54 120.2 . . ? C50 C54 H54 120.2 . . ? N8 C55 C59 121.0(3) . . ? N8 C55 C52 115.9(3) . . ? C59 C55 C52 123.1(3) . . ? N8 C56 C57 123.9(3) . . ? N8 C56 H56 118.1 . . ? C57 C56 H56 118.1 . . ? C56 C57 C58 117.2(3) . . ? C56 C57 C60 120.4(4) . . ? C58 C57 C60 122.4(3) . . ? C59 C58 C57 120.1(3) . . ? C59 C58 H58 119.9 . . ? C57 C58 H58 119.9 . . ? C58 C59 C55 119.4(3) . . ? C58 C59 H59 120.3 . . ? C55 C59 H59 120.3 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 H61A 109.5 . . ? C62 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C62 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C66 C62 C63 116.8(3) . . ? C66 C62 C61 122.4(4) . . ? C63 C62 C61 120.8(4) . . ? N9 C63 C62 123.8(3) . . ? N9 C63 H63 118.1 . . ? C62 C63 H63 118.1 . . ? N9 C64 C65 121.1(3) . . ? N9 C64 C67 115.8(3) . . ? C65 C64 C67 123.1(3) . . ? C64 C65 C66 119.1(4) . . ? C64 C65 H65 120.4 . . ? C66 C65 H65 120.4 . . ? C62 C66 C65 120.3(4) . . ? C62 C66 H66 119.9 . . ? C65 C66 H66 119.9 . . ? N10 C67 C71 120.5(3) . . ? N10 C67 C64 115.1(3) . . ? C71 C67 C64 124.4(3) . . ? N10 C68 C69 123.1(3) . . ? N10 C68 H68 118.5 . . ? C69 C68 H68 118.5 . . ? C70 C69 C68 118.1(3) . . ? C70 C69 C72 123.2(3) . . ? C68 C69 C72 118.5(3) . . ? C69 C70 C71 119.0(3) . . ? C69 C70 H70 120.5 . . ? C71 C70 H70 120.5 . . ? C70 C71 C67 120.5(4) . . ? C70 C71 H71 119.7 . . ? C67 C71 H71 119.7 . . ? O5 C72 C69 108.8(3) . . ? O5 C72 H72A 109.9 . . ? C69 C72 H72A 109.9 . . ? O5 C72 H72B 109.9 . . ? C69 C72 H72B 109.9 . . ? H72A C72 H72B 108.3 . . ? O5 C73 C78 116.6(3) . . ? O5 C73 C74 122.3(3) . . ? C78 C73 C74 121.1(3) . . ? C75 C74 C73 118.8(3) . . ? C75 C74 H74 120.6 . . ? C73 C74 H74 120.6 . . ? O6 C75 C74 122.9(3) . . ? O6 C75 C76 116.1(3) . . ? C74 C75 C76 121.0(3) . . ? C77 C76 C75 118.5(3) . . ? C77 C76 H76 120.7 . . ? C75 C76 H76 120.7 . . ? C76 C77 C78 121.5(3) . . ? C76 C77 H77 119.2 . . ? C78 C77 H77 119.2 . . ? C73 C78 C77 119.0(4) . . ? C73 C78 H78 120.5 . . ? C77 C78 H78 120.5 . . ? O6 C79 C80 109.4(3) . . ? O6 C79 H79A 109.8 . . ? C80 C79 H79A 109.8 . . ? O6 C79 H79B 109.8 . . ? C80 C79 H79B 109.8 . . ? H79A C79 H79B 108.3 . . ? C84 C80 C81 117.6(3) . . ? C84 C80 C79 122.8(3) . . ? C81 C80 C79 119.6(3) . . ? N11 C81 C80 123.5(3) . . ? N11 C81 H81 118.2 . . ? C80 C81 H81 118.2 . . ? N11 C82 C83 121.4(3) . . ? N11 C82 C85 115.0(3) . . ? C83 C82 C85 123.6(3) . . ? C84 C83 C82 119.4(3) . . ? C84 C83 H83 120.3 . . ? C82 C83 H83 120.3 . . ? C80 C84 C83 119.7(3) . . ? C80 C84 H84 120.2 . . ? C83 C84 H84 120.2 . . ? N12 C85 C89 121.4(3) . . ? N12 C85 C82 116.0(3) . . ? C89 C85 C82 122.6(3) . . ? N12 C86 C87 123.7(3) . . ? N12 C86 H86 118.1 . . ? C87 C86 H86 118.1 . . ? C88 C87 C86 116.5(3) . . ? C88 C87 C90 122.6(4) . . ? C86 C87 C90 120.8(3) . . ? C87 C88 C89 120.6(4) . . ? C87 C88 H88 119.7 . . ? C89 C88 H88 119.7 . . ? C85 C89 C88 119.2(4) . . ? C85 C89 H89 120.4 . . ? C88 C89 H89 120.4 . . ? C87 C90 H90A 109.5 . . ? C87 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C87 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C3 N1 C4 118.8(3) . . ? C3 N1 Ni1 126.2(2) . . ? C4 N1 Ni1 114.8(2) . . ? C8 N2 C7 118.6(3) . . ? C8 N2 Ni1 126.9(2) . . ? C7 N2 Ni1 114.5(2) . . ? C22 N3 C21 118.2(3) . . ? C22 N3 Ni2 114.9(2) . . ? C21 N3 Ni2 126.8(2) . . ? C26 N4 C25 119.1(3) . . ? C26 N4 Ni2 126.1(3) . . ? C25 N4 Ni2 114.5(2) . . ? C33 N5 C34 118.4(3) . . ? C33 N5 Ni1 126.0(2) . . ? C34 N5 Ni1 115.5(2) . . ? C38 N6 C37 117.7(3) . . ? C38 N6 Ni1 127.4(2) . . ? C37 N6 Ni1 114.6(2) . . ? C51 N7 C52 119.2(3) . . ? C51 N7 Ni2 126.1(2) . . ? C52 N7 Ni2 114.4(2) . . ? C56 N8 C55 118.4(3) . . ? C56 N8 Ni2 127.5(2) . . ? C55 N8 Ni2 114.1(2) . . ? C63 N9 C64 118.8(3) . . ? C63 N9 Ni1 126.7(2) . . ? C64 N9 Ni1 114.1(2) . . ? C68 N10 C67 118.7(3) . . ? C68 N10 Ni1 126.0(2) . . ? C67 N10 Ni1 115.0(2) . . ? C81 N11 C82 118.2(3) . . ? C81 N11 Ni2 127.0(2) . . ? C82 N11 Ni2 114.5(2) . . ? C85 N12 C86 118.5(3) . . ? C85 N12 Ni2 114.7(2) . . ? C86 N12 Ni2 126.6(2) . . ? F6 P1 F1 92.7(4) . . ? F6 P1 F4 91.6(3) . . ? F1 P1 F4 91.4(2) . . ? F6 P1 F5 175.8(3) . . ? F1 P1 F5 90.5(3) . . ? F4 P1 F5 91.1(3) . . ? F6 P1 F2 89.8(3) . . ? F1 P1 F2 177.0(3) . . ? F4 P1 F2 90.24(18) . . ? F5 P1 F2 87.00(19) . . ? F6 P1 F3 88.1(2) . . ? F1 P1 F3 89.22(19) . . ? F4 P1 F3 179.3(2) . . ? F5 P1 F3 89.2(2) . . ? F2 P1 F3 89.11(15) . . ? F11 P2 F10 91.7(2) . . ? F11 P2 F7 90.97(19) . . ? F10 P2 F7 90.42(18) . . ? F11 P2 F9 89.31(18) . . ? F10 P2 F9 178.99(19) . . ? F7 P2 F9 89.87(16) . . ? F11 P2 F8 90.23(18) . . ? F10 P2 F8 89.77(17) . . ? F7 P2 F8 178.78(17) . . ? F9 P2 F8 89.92(15) . . ? F11 P2 F12 178.39(19) . . ? F10 P2 F12 89.96(18) . . ? F7 P2 F12 89.13(15) . . ? F9 P2 F12 89.09(14) . . ? F8 P2 F12 89.67(14) . . ? F14 P3 F16 92.76(15) . . ? F14 P3 F17 92.96(17) . . ? F16 P3 F17 90.93(15) . . ? F14 P3 F18 91.19(16) . . ? F16 P3 F18 89.96(14) . . ? F17 P3 F18 175.71(18) . . ? F14 P3 F15 89.44(15) . . ? F16 P3 F15 177.64(17) . . ? F17 P3 F15 89.81(17) . . ? F18 P3 F15 89.14(17) . . ? F14 P3 F13 177.92(17) . . ? F16 P3 F13 88.87(14) . . ? F17 P3 F13 88.30(16) . . ? F18 P3 F13 87.52(16) . . ? F15 P3 F13 88.91(15) . . ? F24 P4 F22 91.04(16) . . ? F24 P4 F19 90.69(15) . . ? F22 P4 F19 90.74(15) . . ? F24 P4 F20 90.20(14) . . ? F22 P4 F20 89.53(14) . . ? F19 P4 F20 179.06(16) . . ? F24 P4 F21 90.11(14) . . ? F22 P4 F21 178.81(16) . . ? F19 P4 F21 88.90(14) . . ? F20 P4 F21 90.81(14) . . ? F24 P4 F23 179.04(18) . . ? F22 P4 F23 89.79(16) . . ? F19 P4 F23 89.79(15) . . ? F20 P4 F23 89.32(14) . . ? F21 P4 F23 89.07(15) . . ? N5 Ni1 N10 92.90(11) . . ? N5 Ni1 N1 95.73(11) . . ? N10 Ni1 N1 168.33(11) . . ? N5 Ni1 N2 170.99(11) . . ? N10 Ni1 N2 93.44(11) . . ? N1 Ni1 N2 78.93(11) . . ? N5 Ni1 N6 78.33(11) . . ? N10 Ni1 N6 98.13(11) . . ? N1 Ni1 N6 91.31(11) . . ? N2 Ni1 N6 94.42(10) . . ? N5 Ni1 N9 98.69(11) . . ? N10 Ni1 N9 78.38(11) . . ? N1 Ni1 N9 92.53(11) . . ? N2 Ni1 N9 88.87(11) . . ? N6 Ni1 N9 175.36(11) . . ? N12 Ni2 N11 78.78(11) . . ? N12 Ni2 N7 93.43(11) . . ? N11 Ni2 N7 96.95(10) . . ? N12 Ni2 N4 96.71(12) . . ? N11 Ni2 N4 93.33(11) . . ? N7 Ni2 N4 166.78(12) . . ? N12 Ni2 N8 95.75(11) . . ? N11 Ni2 N8 173.17(11) . . ? N7 Ni2 N8 79.18(11) . . ? N4 Ni2 N8 91.35(12) . . ? N12 Ni2 N3 171.87(11) . . ? N11 Ni2 N3 94.99(11) . . ? N7 Ni2 N3 92.51(11) . . ? N4 Ni2 N3 78.29(12) . . ? N8 Ni2 N3 90.82(11) . . ? C13 O1 C12 115.7(3) . . ? C15 O2 C19 116.5(3) . . ? C43 O3 C42 116.4(3) . . ? C45 O4 C49 117.9(3) . . ? C73 O5 C72 115.7(3) . . ? C75 O6 C79 116.2(3) . . ? C1T O1T C4T 106.5(6) . . ? O1T C1T C2T 106.1(7) . . ? O1T C1T H1T1 110.5 . . ? C2T C1T H1T1 110.5 . . ? O1T C1T H1T2 110.5 . . ? C2T C1T H1T2 110.5 . . ? H1T1 C1T H1T2 108.7 . . ? C3T C2T C1T 105.9(7) . . ? C3T C2T H2T1 110.6 . . ? C1T C2T H2T1 110.6 . . ? C3T C2T H2T2 110.6 . . ? C1T C2T H2T2 110.6 . . ? H2T1 C2T H2T2 108.7 . . ? C4T C3T C2T 104.3(7) . . ? C4T C3T H3T1 110.9 . . ? C2T C3T H3T1 110.9 . . ? C4T C3T H3T2 110.9 . . ? C2T C3T H3T2 110.9 . . ? H3T1 C3T H3T2 108.9 . . ? C3T C4T O1T 110.9(6) . . ? C3T C4T H4T1 109.5 . . ? O1T C4T H4T1 109.5 . . ? C3T C4T H4T2 109.5 . . ? O1T C4T H4T2 109.5 . . ? H4T1 C4T H4T2 108.1 . . ? C5T O2T C8T 105.8(5) . . ? O2T C5T C6T 108.3(5) . . ? O2T C5T H5T1 110.0 . . ? C6T C5T H5T1 110.0 . . ? O2T C5T H5T2 110.0 . . ? C6T C5T H5T2 110.0 . . ? H5T1 C5T H5T2 108.4 . . ? C5T C6T C7T 102.3(5) . . ? C5T C6T H6T1 111.3 . . ? C7T C6T H6T1 111.3 . . ? C5T C6T H6T2 111.3 . . ? C7T C6T H6T2 111.3 . . ? H6T1 C6T H6T2 109.2 . . ? C8T C7T C6T 102.2(6) . . ? C8T C7T H7T1 111.3 . . ? C6T C7T H7T1 111.3 . . ? C8T C7T H7T2 111.3 . . ? C6T C7T H7T2 111.3 . . ? H7T1 C7T H7T2 109.2 . . ? O2T C8T C7T 108.5(5) . . ? O2T C8T H8T1 110.0 . . ? C7T C8T H8T1 110.0 . . ? O2T C8T H8T2 110.0 . . ? C7T C8T H8T2 110.0 . . ? H8T1 C8T H8T2 108.4 . . ? O3T C9T C10T 112.8(9) . . ? O3T C9T H9T1 109.0 . . ? C10T C9T H9T1 109.0 . . ? O3T C9T H9T2 109.0 . . ? C10T C9T H9T2 109.0 . . ? H9T1 C9T H9T2 107.8 . . ? C12T O3T C9T 106.0(10) . . ? C9T C10T C11T 96.2(9) . . ? C9T C10T H10A 112.5 . . ? C11T C10T H10A 112.5 . . ? C9T C10T H10B 112.5 . . ? C11T C10T H10B 112.5 . . ? H10A C10T H10B 110.0 . . ? C10T C11T C12T 100.2(8) . . ? C10T C11T H11A 111.7 . . ? C12T C11T H11A 111.7 . . ? C10T C11T H11B 111.7 . . ? C12T C11T H11B 111.7 . . ? H11A C11T H11B 109.5 . . ? O3T C12T C11T 113.0(9) . . ? O3T C12T H12C 109.0 . . ? C11T C12T H12C 109.0 . . ? O3T C12T H12D 109.0 . . ? C11T C12T H12D 109.0 . . ? H12C C12T H12D 107.8 . . ? O3TA C9A C11A 102(2) . . ? O3TA C9A H9A1 111.3 . . ? C11A C9A H9A1 111.3 . . ? O3TA C9A H9A2 111.3 . . ? C11A C9A H9A2 111.3 . . ? H9A1 C9A H9A2 109.2 . . ? C10A O3TA C9A 119(2) . . ? O3TA C10A C12A 103.6(17) . . ? O3TA C10A H10C 111.0 . . ? C12A C10A H10C 111.0 . . ? O3TA C10A H10D 111.0 . . ? C12A C10A H10D 111.0 . . ? H10C C10A H10D 109.0 . . ? C12A C11A C9A 105.4(18) . . ? C12A C11A H11C 110.7 . . ? C9A C11A H11C 110.7 . . ? C12A C11A H11D 110.7 . . ? C9A C11A H11D 110.7 . . ? H11C C11A H11D 108.8 . . ? C11A C12A C10A 101.7(18) . . ? C11A C12A H12E 111.4 . . ? C10A C12A H12E 111.4 . . ? C11A C12A H12F 111.4 . . ? C10A C12A H12F 111.4 . . ? H12E C12A H12F 109.3 . . ? C11B O3TB C9B 113.1(15) . . ? O3TB C9B C10B 96.4(18) . . ? O3TB C9B H9B1 112.5 . . ? C10B C9B H9B1 112.5 . . ? O3TB C9B H9B2 112.5 . . ? C10B C9B H9B2 112.5 . . ? H9B1 C9B H9B2 110.0 . . ? C12B C10B C9B 102.1(15) . . ? C12B C10B H10E 111.3 . . ? C9B C10B H10E 111.3 . . ? C12B C10B H10F 111.3 . . ? C9B C10B H10F 111.3 . . ? H10E C10B H10F 109.2 . . ? O3TB C11B C12B 107.7(16) . . ? O3TB C11B H11E 110.2 . . ? C12B C11B H11E 110.2 . . ? O3TB C11B H11F 110.2 . . ? C12B C11B H11F 110.2 . . ? H11E C11B H11F 108.5 . . ? C10B C12B C11B 96.1(15) . . ? C10B C12B H12G 112.5 . . ? C11B C12B H12G 112.5 . . ? C10B C12B H12H 112.5 . . ? C11B C12B H12H 112.5 . . ? H12G C12B H12H 110.0 . . ? O4T C16T C13T 101.6(6) . . ? O4T C16T H16A 111.4 . . ? C13T C16T H16A 111.4 . . ? O4T C16T H16B 111.4 . . ? C13T C16T H16B 111.4 . . ? H16A C16T H16B 109.3 . . ? C14T C13T C16T 101.2(7) . . ? C14T C13T H13A 111.5 . . ? C16T C13T H13A 111.5 . . ? C14T C13T H13B 111.5 . . ? C16T C13T H13B 111.5 . . ? H13A C13T H13B 109.3 . . ? C15T C14T C13T 100.9(7) . . ? C15T C14T H14A 111.6 . . ? C13T C14T H14A 111.6 . . ? C15T C14T H14B 111.6 . . ? C13T C14T H14B 111.6 . . ? H14A C14T H14B 109.4 . . ? O4T C15T C14T 106.5(7) . . ? O4T C15T H15A 110.4 . . ? C14T C15T H15A 110.4 . . ? O4T C15T H15B 110.4 . . ? C14T C15T H15B 110.4 . . ? H15A C15T H15B 108.6 . . ? C16T O4T C15T 114.2(6) . . ? C17T O5T C20T 107.5(5) . . ? O5T C20T C19T 105.4(6) . . ? O5T C20T H20A 110.7 . . ? C19T C20T H20A 110.7 . . ? O5T C20T H20B 110.7 . . ? C19T C20T H20B 110.7 . . ? H20A C20T H20B 108.8 . . ? C17T C18T C19T 100.7(11) . . ? C17T C18T H18A 111.6 . . ? C19T C18T H18A 111.6 . . ? C17T C18T H18B 111.6 . . ? C19T C18T H18B 111.6 . . ? H18A C18T H18B 109.4 . . ? O5T C17T C18T 111.4(10) . . ? O5T C17T H17A 109.4 . . ? C18T C17T H17A 109.4 . . ? O5T C17T H17B 109.4 . . ? C18T C17T H17B 109.4 . . ? H17A C17T H17B 108.0 . . ? C20T C19T C18T 104.2(10) . . ? C20T C19T H19C 110.9 . . ? C18T C19T H19C 110.9 . . ? C20T C19T H19D 110.9 . . ? C18T C19T H19D 110.9 . . ? H19C C19T H19D 108.9 . . ? H18C C18A H18D 109.2 . . ? C21T C23T C24T 104.3(5) . . ? C21T C23T H23A 110.9 . . ? C24T C23T H23A 110.9 . . ? C21T C23T H23B 110.9 . . ? C24T C23T H23B 110.9 . . ? H23A C23T H23B 108.9 . . ? C23T C21T C22T 104.1(5) . . ? C23T C21T H21A 110.9 . . ? C22T C21T H21A 110.9 . . ? C23T C21T H21B 110.9 . . ? C22T C21T H21B 110.9 . . ? H21A C21T H21B 109.0 . . ? O6T C22T C21T 104.5(5) . . ? O6T C22T H22A 110.8 . . ? C21T C22T H22A 110.8 . . ? O6T C22T H22B 110.8 . . ? C21T C22T H22B 110.8 . . ? H22A C22T H22B 108.9 . . ? C24T O6T C22T 103.6(5) . . ? O6T C24T C23T 106.9(6) . . ? O6T C24T H24A 110.3 . . ? C23T C24T H24A 110.3 . . ? O6T C24T H24B 110.3 . . ? C23T C24T H24B 110.3 . . ? H24A C24T H24B 108.6 . . ? C6A C5A H5A1 109.5 . . ? C6A C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? C6A C5A H5A3 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? N3A C6A C5A 162(3) . . ? C2A C1A H1A1 109.5 . . ? C2A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C2A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? N1A C2A C1A 177.6(8) . . ? N2A C4A C3A 177.9(17) . . ? 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 C6 C2 C3 N1 -0.1(6) . . . . ? C1 C2 C3 N1 179.5(4) . . . . ? N1 C4 C5 C6 -0.3(6) . . . . ? C7 C4 C5 C6 179.7(4) . . . . ? C3 C2 C6 C5 0.5(6) . . . . ? C1 C2 C6 C5 -179.1(4) . . . . ? C4 C5 C6 C2 -0.3(6) . . . . ? N1 C4 C7 N2 0.7(4) . . . . ? C5 C4 C7 N2 -179.3(3) . . . . ? N1 C4 C7 C11 -179.6(3) . . . . ? C5 C4 C7 C11 0.3(5) . . . . ? N2 C8 C9 C10 -1.3(5) . . . . ? N2 C8 C9 C12 175.7(3) . . . . ? C8 C9 C10 C11 1.0(5) . . . . ? C12 C9 C10 C11 -175.7(3) . . . . ? N2 C7 C11 C10 -2.0(5) . . . . ? C4 C7 C11 C10 178.4(3) . . . . ? C9 C10 C11 C7 0.6(5) . . . . ? C10 C9 C12 O1 -22.3(5) . . . . ? C8 C9 C12 O1 161.0(3) . . . . ? O1 C13 C14 C15 -177.3(3) . . . . ? C18 C13 C14 C15 2.5(6) . . . . ? C13 C14 C15 O2 175.0(3) . . . . ? C13 C14 C15 C16 -3.0(5) . . . . ? O2 C15 C16 C17 -176.3(4) . . . . ? C14 C15 C16 C17 1.8(6) . . . . ? C15 C16 C17 C18 -0.1(7) . . . . ? O1 C13 C18 C17 179.0(4) . . . . ? C14 C13 C18 C17 -0.8(7) . . . . ? C16 C17 C18 C13 -0.4(7) . . . . ? O2 C19 C20 C21 111.2(3) . . . . ? O2 C19 C20 C24 -67.9(4) . . . . ? C24 C20 C21 N3 -2.7(5) . . . . ? C19 C20 C21 N3 178.2(3) . . . . ? N3 C22 C23 C24 -1.8(6) . . . . ? C25 C22 C23 C24 175.4(4) . . . . ? C22 C23 C24 C20 0.0(6) . . . . ? C21 C20 C24 C23 2.1(5) . . . . ? C19 C20 C24 C23 -178.8(3) . . . . ? N3 C22 C25 N4 2.3(5) . . . . ? C23 C22 C25 N4 -175.1(4) . . . . ? N3 C22 C25 C29 -179.1(4) . . . . ? C23 C22 C25 C29 3.5(6) . . . . ? N4 C26 C27 C28 1.5(9) . . . . ? N4 C26 C27 C30 -177.7(6) . . . . ? C26 C27 C28 C29 -1.7(11) . . . . ? C30 C27 C28 C29 177.4(7) . . . . ? C27 C28 C29 C25 -0.3(10) . . . . ? N4 C25 C29 C28 2.8(8) . . . . ? C22 C25 C29 C28 -175.8(5) . . . . ? C36 C32 C33 N5 1.3(5) . . . . ? C31 C32 C33 N5 -179.4(3) . . . . ? N5 C34 C35 C36 0.8(6) . . . . ? C37 C34 C35 C36 -175.0(4) . . . . ? C33 C32 C36 C35 -0.7(6) . . . . ? C31 C32 C36 C35 -180.0(4) . . . . ? C34 C35 C36 C32 -0.3(6) . . . . ? N5 C34 C37 N6 -7.3(5) . . . . ? C35 C34 C37 N6 168.8(3) . . . . ? N5 C34 C37 C41 174.7(3) . . . . ? C35 C34 C37 C41 -9.3(6) . . . . ? N6 C38 C39 C40 -3.2(5) . . . . ? N6 C38 C39 C42 175.1(3) . . . . ? C38 C39 C40 C41 2.5(6) . . . . ? C42 C39 C40 C41 -175.6(4) . . . . ? C39 C40 C41 C37 1.2(6) . . . . ? N6 C37 C41 C40 -4.8(6) . . . . ? C34 C37 C41 C40 173.1(4) . . . . ? C38 C39 C42 O3 94.5(4) . . . . ? C40 C39 C42 O3 -87.4(4) . . . . ? O3 C43 C44 C45 172.2(3) . . . . ? C48 C43 C44 C45 -5.4(5) . . . . ? C43 C44 C45 O4 -175.1(3) . . . . ? C43 C44 C45 C46 3.1(5) . . . . ? O4 C45 C46 C47 179.4(3) . . . . ? C44 C45 C46 C47 1.0(5) . . . . ? C45 C46 C47 C48 -3.0(5) . . . . ? O3 C43 C48 C47 -174.3(3) . . . . ? C44 C43 C48 C47 3.6(5) . . . . ? C46 C47 C48 C43 0.7(5) . . . . ? O4 C49 C50 C51 170.1(3) . . . . ? O4 C49 C50 C54 -12.4(5) . . . . ? C54 C50 C51 N7 0.0(5) . . . . ? C49 C50 C51 N7 177.6(3) . . . . ? N7 C52 C53 C54 -0.3(5) . . . . ? C55 C52 C53 C54 -179.7(3) . . . . ? C52 C53 C54 C50 0.7(5) . . . . ? C51 C50 C54 C53 -0.6(5) . . . . ? C49 C50 C54 C53 -178.1(3) . . . . ? N7 C52 C55 N8 3.2(4) . . . . ? C53 C52 C55 N8 -177.4(3) . . . . ? N7 C52 C55 C59 -176.3(3) . . . . ? C53 C52 C55 C59 3.1(5) . . . . ? N8 C56 C57 C58 0.1(5) . . . . ? N8 C56 C57 C60 -178.9(4) . . . . ? C56 C57 C58 C59 -0.1(5) . . . . ? C60 C57 C58 C59 178.9(4) . . . . ? C57 C58 C59 C55 0.0(5) . . . . ? N8 C55 C59 C58 0.0(5) . . . . ? C52 C55 C59 C58 179.5(3) . . . . ? C66 C62 C63 N9 0.0(6) . . . . ? C61 C62 C63 N9 178.2(4) . . . . ? N9 C64 C65 C66 -2.2(7) . . . . ? C67 C64 C65 C66 176.9(4) . . . . ? C63 C62 C66 C65 -0.5(7) . . . . ? C61 C62 C66 C65 -178.7(4) . . . . ? C64 C65 C66 C62 1.6(8) . . . . ? N9 C64 C67 N10 0.3(5) . . . . ? C65 C64 C67 N10 -178.8(4) . . . . ? N9 C64 C67 C71 178.0(4) . . . . ? C65 C64 C67 C71 -1.1(6) . . . . ? N10 C68 C69 C70 -0.1(5) . . . . ? N10 C68 C69 C72 175.2(3) . . . . ? C68 C69 C70 C71 -1.8(6) . . . . ? C72 C69 C70 C71 -176.8(4) . . . . ? C69 C70 C71 C67 1.8(6) . . . . ? N10 C67 C71 C70 -0.1(6) . . . . ? C64 C67 C71 C70 -177.8(4) . . . . ? C70 C69 C72 O5 -38.0(5) . . . . ? C68 C69 C72 O5 147.0(3) . . . . ? O5 C73 C74 C75 -176.6(3) . . . . ? C78 C73 C74 C75 2.2(5) . . . . ? C73 C74 C75 O6 175.9(3) . . . . ? C73 C74 C75 C76 -3.3(5) . . . . ? O6 C75 C76 C77 -176.9(3) . . . . ? C74 C75 C76 C77 2.3(5) . . . . ? C75 C76 C77 C78 -0.3(6) . . . . ? O5 C73 C78 C77 178.6(3) . . . . ? C74 C73 C78 C77 -0.2(5) . . . . ? C76 C77 C78 C73 -0.7(6) . . . . ? O6 C79 C80 C84 -72.5(4) . . . . ? O6 C79 C80 C81 109.5(4) . . . . ? C84 C80 C81 N11 -3.1(5) . . . . ? C79 C80 C81 N11 175.1(3) . . . . ? N11 C82 C83 C84 -3.7(5) . . . . ? C85 C82 C83 C84 174.5(3) . . . . ? C81 C80 C84 C83 2.8(5) . . . . ? C79 C80 C84 C83 -175.3(3) . . . . ? C82 C83 C84 C80 0.4(5) . . . . ? N11 C82 C85 N12 -9.5(4) . . . . ? C83 C82 C85 N12 172.3(3) . . . . ? N11 C82 C85 C89 167.8(3) . . . . ? C83 C82 C85 C89 -10.4(6) . . . . ? N12 C86 C87 C88 -0.5(6) . . . . ? N12 C86 C87 C90 -178.5(3) . . . . ? C86 C87 C88 C89 1.1(6) . . . . ? C90 C87 C88 C89 179.0(4) . . . . ? N12 C85 C89 C88 0.2(6) . . . . ? C82 C85 C89 C88 -177.0(4) . . . . ? C87 C88 C89 C85 -0.9(7) . . . . ? C2 C3 N1 C4 -0.5(5) . . . . ? C2 C3 N1 Ni1 -175.2(3) . . . . ? C5 C4 N1 C3 0.7(5) . . . . ? C7 C4 N1 C3 -179.4(3) . . . . ? C5 C4 N1 Ni1 176.0(3) . . . . ? C7 C4 N1 Ni1 -4.0(4) . . . . ? C9 C8 N2 C7 -0.1(5) . . . . ? C9 C8 N2 Ni1 178.2(2) . . . . ? C11 C7 N2 C8 1.7(5) . . . . ? C4 C7 N2 C8 -178.6(3) . . . . ? C11 C7 N2 Ni1 -176.7(3) . . . . ? C4 C7 N2 Ni1 2.9(4) . . . . ? C23 C22 N3 C21 1.3(5) . . . . ? C25 C22 N3 C21 -176.1(3) . . . . ? C23 C22 N3 Ni2 -176.4(3) . . . . ? C25 C22 N3 Ni2 6.2(4) . . . . ? C20 C21 N3 C22 1.0(5) . . . . ? C20 C21 N3 Ni2 178.4(2) . . . . ? C27 C26 N4 C25 0.8(7) . . . . ? C27 C26 N4 Ni2 -173.3(4) . . . . ? C29 C25 N4 C26 -3.0(6) . . . . ? C22 C25 N4 C26 175.6(4) . . . . ? C29 C25 N4 Ni2 171.8(4) . . . . ? C22 C25 N4 Ni2 -9.6(4) . . . . ? C32 C33 N5 C34 -0.9(5) . . . . ? C32 C33 N5 Ni1 176.4(3) . . . . ? C35 C34 N5 C33 -0.2(5) . . . . ? C37 C34 N5 C33 175.9(3) . . . . ? C35 C34 N5 Ni1 -177.7(3) . . . . ? C37 C34 N5 Ni1 -1.7(4) . . . . ? C39 C38 N6 C37 -0.2(5) . . . . ? C39 C38 N6 Ni1 172.7(2) . . . . ? C41 C37 N6 C38 4.3(5) . . . . ? C34 C37 N6 C38 -173.8(3) . . . . ? C41 C37 N6 Ni1 -169.5(3) . . . . ? C34 C37 N6 Ni1 12.4(4) . . . . ? C50 C51 N7 C52 0.4(5) . . . . ? C50 C51 N7 Ni2 -172.3(2) . . . . ? C53 C52 N7 C51 -0.2(5) . . . . ? C55 C52 N7 C51 179.2(3) . . . . ? C53 C52 N7 Ni2 173.3(2) . . . . ? C55 C52 N7 Ni2 -7.2(3) . . . . ? C57 C56 N8 C55 -0.1(5) . . . . ? C57 C56 N8 Ni2 177.7(3) . . . . ? C59 C55 N8 C56 0.1(5) . . . . ? C52 C55 N8 C56 -179.5(3) . . . . ? C59 C55 N8 Ni2 -178.0(2) . . . . ? C52 C55 N8 Ni2 2.5(3) . . . . ? C62 C63 N9 C64 -0.6(5) . . . . ? C62 C63 N9 Ni1 171.8(3) . . . . ? C65 C64 N9 C63 1.6(5) . . . . ? C67 C64 N9 C63 -177.5(3) . . . . ? C65 C64 N9 Ni1 -171.6(3) . . . . ? C67 C64 N9 Ni1 9.2(4) . . . . ? C69 C68 N10 C67 1.8(5) . . . . ? C69 C68 N10 Ni1 -171.5(2) . . . . ? C71 C67 N10 C68 -1.8(5) . . . . ? C64 C67 N10 C68 176.1(3) . . . . ? C71 C67 N10 Ni1 172.3(3) . . . . ? C64 C67 N10 Ni1 -9.8(4) . . . . ? C80 C81 N11 C82 -0.1(5) . . . . ? C80 C81 N11 Ni2 172.9(2) . . . . ? C83 C82 N11 C81 3.5(5) . . . . ? C85 C82 N11 C81 -174.8(3) . . . . ? C83 C82 N11 Ni2 -170.4(3) . . . . ? C85 C82 N11 Ni2 11.3(4) . . . . ? C89 C85 N12 C86 0.3(5) . . . . ? C82 C85 N12 C86 177.7(3) . . . . ? C89 C85 N12 Ni2 -174.5(3) . . . . ? C82 C85 N12 Ni2 2.8(4) . . . . ? C87 C86 N12 C85 -0.2(5) . . . . ? C87 C86 N12 Ni2 174.0(3) . . . . ? C33 N5 Ni1 N10 -73.4(3) . . . . ? C34 N5 Ni1 N10 104.0(2) . . . . ? C33 N5 Ni1 N1 98.8(3) . . . . ? C34 N5 Ni1 N1 -83.9(2) . . . . ? C33 N5 Ni1 N6 -171.1(3) . . . . ? C34 N5 Ni1 N6 6.3(2) . . . . ? C33 N5 Ni1 N9 5.3(3) . . . . ? C34 N5 Ni1 N9 -177.3(2) . . . . ? C68 N10 Ni1 N5 -76.9(3) . . . . ? C67 N10 Ni1 N5 109.5(2) . . . . ? C68 N10 Ni1 N1 145.4(5) . . . . ? C67 N10 Ni1 N1 -28.2(7) . . . . ? C68 N10 Ni1 N2 96.7(3) . . . . ? C67 N10 Ni1 N2 -76.9(3) . . . . ? C68 N10 Ni1 N6 1.7(3) . . . . ? C67 N10 Ni1 N6 -171.9(2) . . . . ? C68 N10 Ni1 N9 -175.2(3) . . . . ? C67 N10 Ni1 N9 11.2(2) . . . . ? C3 N1 Ni1 N5 -8.2(3) . . . . ? C4 N1 Ni1 N5 176.9(2) . . . . ? C3 N1 Ni1 N10 129.3(5) . . . . ? C4 N1 Ni1 N10 -45.6(6) . . . . ? C3 N1 Ni1 N2 179.2(3) . . . . ? C4 N1 Ni1 N2 4.3(2) . . . . ? C3 N1 Ni1 N6 -86.6(3) . . . . ? C4 N1 Ni1 N6 98.5(2) . . . . ? C3 N1 Ni1 N9 90.8(3) . . . . ? C4 N1 Ni1 N9 -84.1(2) . . . . ? C8 N2 Ni1 N10 -11.1(3) . . . . ? C7 N2 Ni1 N10 167.3(2) . . . . ? C8 N2 Ni1 N1 177.9(3) . . . . ? C7 N2 Ni1 N1 -3.8(2) . . . . ? C8 N2 Ni1 N6 87.4(3) . . . . ? C7 N2 Ni1 N6 -94.3(2) . . . . ? C8 N2 Ni1 N9 -89.3(3) . . . . ? C7 N2 Ni1 N9 89.0(2) . . . . ? C38 N6 Ni1 N5 176.6(3) . . . . ? C37 N6 Ni1 N5 -10.3(2) . . . . ? C38 N6 Ni1 N10 85.3(3) . . . . ? C37 N6 Ni1 N10 -101.6(2) . . . . ? C38 N6 Ni1 N1 -87.8(3) . . . . ? C37 N6 Ni1 N1 85.3(2) . . . . ? C38 N6 Ni1 N2 -8.8(3) . . . . ? C37 N6 Ni1 N2 164.3(2) . . . . ? C63 N9 Ni1 N5 85.1(3) . . . . ? C64 N9 Ni1 N5 -102.2(2) . . . . ? C63 N9 Ni1 N10 176.3(3) . . . . ? C64 N9 Ni1 N10 -11.0(2) . . . . ? C63 N9 Ni1 N1 -11.1(3) . . . . ? C64 N9 Ni1 N1 161.6(2) . . . . ? C63 N9 Ni1 N2 -89.9(3) . . . . ? C64 N9 Ni1 N2 82.7(2) . . . . ? C85 N12 Ni2 N11 2.4(2) . . . . ? C86 N12 Ni2 N11 -172.0(3) . . . . ? C85 N12 Ni2 N7 98.8(2) . . . . ? C86 N12 Ni2 N7 -75.6(3) . . . . ? C85 N12 Ni2 N4 -89.7(3) . . . . ? C86 N12 Ni2 N4 95.9(3) . . . . ? C85 N12 Ni2 N8 178.3(2) . . . . ? C86 N12 Ni2 N8 3.9(3) . . . . ? C81 N11 Ni2 N12 179.1(3) . . . . ? C82 N11 Ni2 N12 -7.6(2) . . . . ? C81 N11 Ni2 N7 87.0(3) . . . . ? C82 N11 Ni2 N7 -99.8(2) . . . . ? C81 N11 Ni2 N4 -84.7(3) . . . . ? C82 N11 Ni2 N4 88.5(2) . . . . ? C81 N11 Ni2 N3 -6.2(3) . . . . ? C82 N11 Ni2 N3 167.1(2) . . . . ? C51 N7 Ni2 N12 -85.2(3) . . . . ? C52 N7 Ni2 N12 101.7(2) . . . . ? C51 N7 Ni2 N11 -6.1(3) . . . . ? C52 N7 Ni2 N11 -179.1(2) . . . . ? C51 N7 Ni2 N4 134.7(5) . . . . ? C52 N7 Ni2 N4 -38.3(6) . . . . ? C51 N7 Ni2 N8 179.6(3) . . . . ? C52 N7 Ni2 N8 6.5(2) . . . . ? C51 N7 Ni2 N3 89.3(3) . . . . ? C52 N7 Ni2 N3 -83.8(2) . . . . ? C26 N4 Ni2 N12 -2.4(4) . . . . ? C25 N4 Ni2 N12 -176.7(3) . . . . ? C26 N4 Ni2 N11 -81.4(4) . . . . ? C25 N4 Ni2 N11 104.2(3) . . . . ? C26 N4 Ni2 N7 137.5(5) . . . . ? C25 N4 Ni2 N7 -36.9(6) . . . . ? C26 N4 Ni2 N8 93.6(4) . . . . ? C25 N4 Ni2 N8 -80.8(3) . . . . ? C26 N4 Ni2 N3 -175.9(4) . . . . ? C25 N4 Ni2 N3 9.8(3) . . . . ? C56 N8 Ni2 N12 85.0(3) . . . . ? C55 N8 Ni2 N12 -97.2(2) . . . . ? C56 N8 Ni2 N7 177.4(3) . . . . ? C55 N8 Ni2 N7 -4.8(2) . . . . ? C56 N8 Ni2 N4 -11.9(3) . . . . ? C55 N8 Ni2 N4 165.9(2) . . . . ? C56 N8 Ni2 N3 -90.2(3) . . . . ? C55 N8 Ni2 N3 87.6(2) . . . . ? C22 N3 Ni2 N11 -101.0(2) . . . . ? C21 N3 Ni2 N11 81.5(3) . . . . ? C22 N3 Ni2 N7 161.8(2) . . . . ? C21 N3 Ni2 N7 -15.7(3) . . . . ? C22 N3 Ni2 N4 -8.6(2) . . . . ? C21 N3 Ni2 N4 173.9(3) . . . . ? C22 N3 Ni2 N8 82.6(2) . . . . ? C21 N3 Ni2 N8 -94.9(3) . . . . ? C18 C13 O1 C12 -177.6(4) . . . . ? C14 C13 O1 C12 2.2(5) . . . . ? C9 C12 O1 C13 175.1(3) . . . . ? C16 C15 O2 C19 168.2(3) . . . . ? C14 C15 O2 C19 -9.8(5) . . . . ? C20 C19 O2 C15 -165.1(3) . . . . ? C48 C43 O3 C42 172.6(3) . . . . ? C44 C43 O3 C42 -5.3(4) . . . . ? C39 C42 O3 C43 -159.5(3) . . . . ? C46 C45 O4 C49 177.9(3) . . . . ? C44 C45 O4 C49 -3.8(5) . . . . ? C50 C49 O4 C45 172.7(3) . . . . ? C78 C73 O5 C72 -175.1(3) . . . . ? C74 C73 O5 C72 3.7(5) . . . . ? C69 C72 O5 C73 167.7(3) . . . . ? C74 C75 O6 C79 -11.1(5) . . . . ? C76 C75 O6 C79 168.1(3) . . . . ? C80 C79 O6 C75 -163.6(3) . . . . ? C4T O1T C1T C2T -5.0(7) . . . . ? O1T C1T C2T C3T 19.1(9) . . . . ? C1T C2T C3T C4T -24.9(9) . . . . ? C2T C3T C4T O1T 23.0(8) . . . . ? C1T O1T C4T C3T -10.9(7) . . . . ? C8T O2T C5T C6T 18.3(8) . . . . ? O2T C5T C6T C7T -33.5(8) . . . . ? C5T C6T C7T C8T 34.4(8) . . . . ? C5T O2T C8T C7T 4.8(8) . . . . ? C6T C7T C8T O2T -24.8(8) . . . . ? C10T C9T O3T C12T 26(2) . . . . ? O3T C9T C10T C11T -35(2) . . . . ? C9T C10T C11T C12T 27.7(15) . . . . ? C9T O3T C12T C11T -4(2) . . . . ? C10T C11T C12T O3T -17.6(19) . . . . ? C11A C9A O3TA C10A -3(3) . . . . ? C9A O3TA C10A C12A -14(3) . . . . ? O3TA C9A C11A C12A 20(3) . . . . ? C9A C11A C12A C10A -28(2) . . . . ? O3TA C10A C12A C11A 26(3) . . . . ? C11B O3TB C9B C10B -12(3) . . . . ? O3TB C9B C10B C12B 38(2) . . . . ? C9B O3TB C11B C12B -19(3) . . . . ? C9B C10B C12B C11B -48(3) . . . . ? O3TB C11B C12B C10B 42(3) . . . . ? O4T C16T C13T C14T 37.2(7) . . . . ? C16T C13T C14T C15T -36.4(9) . . . . ? C13T C14T C15T O4T 24.3(10) . . . . ? C13T C16T O4T C15T -23.5(9) . . . . ? C14T C15T O4T C16T 0.0(11) . . . . ? C17T O5T C20T C19T 31.2(7) . . . . ? C20T O5T C17T C18T -16.1(14) . . . . ? C19T C18T C17T O5T -4.3(17) . . . . ? O5T C20T C19T C18T -33.0(11) . . . . ? C17T C18T C19T C20T 22.6(16) . . . . ? C24T C23T C21T C22T -4.8(7) . . . . ? C23T C21T C22T O6T 27.6(7) . . . . ? C21T C22T O6T C24T -40.7(7) . . . . ? C22T O6T C24T C23T 38.2(7) . . . . ? C21T C23T C24T O6T -20.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 19.31 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.628 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.097 data_lj137sad _database_code_depnum_ccdc_archive 'CCDC 824371' #TrackingRef '- combined lindoy.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C90 H78 N12 Ni2 O6), 1.20(C4 H8 O), 1.95(C2 H3 N), 1.80(H2 O), 4(F6 P)' _chemical_formula_sum 'C98.70 H97.05 F24 N13.95 Ni2 O9 P4' _chemical_formula_weight 2317.49 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' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' H H 0.0000 0.0000 '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_intl_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.9978(6) _cell_length_b 15.0666(6) _cell_length_c 25.7786(11) _cell_angle_alpha 91.398(2) _cell_angle_beta 104.152(2) _cell_angle_gamma 99.563(2) _cell_volume 5556.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7604 _cell_measurement_theta_min 2.078 _cell_measurement_theta_max 24.917 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2378 _exptl_absorpt_coefficient_mu 0.496 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.799 _exptl_absorpt_correction_T_max 0.952 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; The crystal was coated in Exxon Paratone N hydrocarbon oil and mounted on a thin mohair fibre attached to a copper pin. Upon mounting on the diffractometer, the crystal was quenched to 150(K) under a cold nitrogen gas stream supplied by an Oxford Cryosystems Cryostream. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type APEXII-FR591 _diffrn_measurement_method \w+\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 107006 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 0.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 19484 _reflns_number_gt 13655 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX (Bruker-Nonius, 2003)' _computing_cell_refinement 'SAINT (Bruker-Nonius, 2003)' _computing_data_reduction 'SAINT (Bruker-Nonius, 2003), XPREP (Bruker-Nonius, 2003)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXH-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) POV-Ray 3.5 (Cason, 2002) WebLab ViewerPro 3.7 (Molecular Simulations, 2000) ; _computing_publication_material 'enCIFer 1.1 (CCDC, 2005)' _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^)+(0.1364P)^2^+8.2419P] 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 19484 _refine_ls_number_parameters 1534 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1094 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.2408 _refine_ls_wR_factor_gt 0.2194 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 C1 C 0.3509(4) 0.6349(4) 0.5532(2) 0.0568(14) Uani 1 1 d . . . H1A H 0.3426 0.6953 0.5419 0.085 Uiso 1 1 calc R . . H1B H 0.4084 0.6395 0.5818 0.085 Uiso 1 1 calc R . . H1C H 0.2974 0.6076 0.5664 0.085 Uiso 1 1 calc R . . C2 C 0.3573(3) 0.5767(3) 0.5058(2) 0.0438(12) Uani 1 1 d . . . C3 C 0.4311(4) 0.5930(3) 0.4820(2) 0.0454(12) Uani 1 1 d . . . H3 H 0.4811 0.6417 0.4959 0.055 Uiso 1 1 calc R . . C4 C 0.4330(3) 0.5390(3) 0.4380(2) 0.0423(11) Uani 1 1 d . . . H4 H 0.4847 0.5495 0.4224 0.051 Uiso 1 1 calc R . . C5 C 0.3582(3) 0.4692(3) 0.41709(19) 0.0383(11) Uani 1 1 d . . . C6 C 0.2867(3) 0.5047(3) 0.4832(2) 0.0433(11) Uani 1 1 d . . . H6 H 0.2357 0.4918 0.4992 0.052 Uiso 1 1 calc R . . C7 C 0.3491(3) 0.4125(3) 0.36807(19) 0.0379(11) Uani 1 1 d . . . C8 C 0.4165(3) 0.4180(4) 0.3381(2) 0.0448(12) Uani 1 1 d . . . H8 H 0.4748 0.4575 0.3505 0.054 Uiso 1 1 calc R . . C9 C 0.3974(4) 0.3659(4) 0.2907(2) 0.0490(13) Uani 1 1 d . . . H9 H 0.4430 0.3690 0.2706 0.059 Uiso 1 1 calc R . . C10 C 0.3124(4) 0.3091(4) 0.2723(2) 0.0450(12) Uani 1 1 d . . . C11 C 0.2499(3) 0.3052(3) 0.3046(2) 0.0422(11) Uani 1 1 d . . . H11 H 0.1921 0.2646 0.2934 0.051 Uiso 1 1 calc R . . C12 C 0.2860(4) 0.2526(5) 0.2199(2) 0.0643(16) Uani 1 1 d . . . H12A H 0.2754 0.2918 0.1895 0.077 Uiso 1 1 calc R . . H12B H 0.3372 0.2202 0.2173 0.077 Uiso 1 1 calc R . . C13 C 0.1406(4) 0.1610(4) 0.1689(2) 0.0490(13) Uani 1 1 d . . . C14 C 0.1130(4) 0.2187(4) 0.1292(3) 0.0599(15) Uani 1 1 d . . . H14 H 0.1406 0.2808 0.1333 0.072 Uiso 1 1 calc R . . C15 C 0.0451(4) 0.1843(4) 0.0838(3) 0.0598(15) Uani 1 1 d . . . H15 H 0.0267 0.2234 0.0564 0.072 Uiso 1 1 calc R . . C16 C 0.0028(3) 0.0948(4) 0.0769(2) 0.0452(12) Uani 1 1 d . . . C17 C 0.0308(4) 0.0378(4) 0.1163(2) 0.0516(13) Uani 1 1 d . . . H17 H 0.0023 -0.0241 0.1124 0.062 Uiso 1 1 calc R . . C18 C 0.1004(4) 0.0712(4) 0.1615(2) 0.0564(14) Uani 1 1 d . . . H18 H 0.1209 0.0314 0.1881 0.068 Uiso 1 1 calc R . . C19 C -0.1151(3) -0.0221(4) 0.0238(2) 0.0457(12) Uani 1 1 d . . . H19A H -0.1398 -0.0350 0.0556 0.055 Uiso 1 1 calc R . . H19B H -0.0735 -0.0655 0.0207 0.055 Uiso 1 1 calc R . . C20 C -0.1940(3) -0.0318(3) -0.02556(19) 0.0401(11) Uani 1 1 d . . . C21 C -0.2422(3) -0.1155(4) -0.0490(2) 0.0446(12) Uani 1 1 d . . . H21 H -0.2220 -0.1688 -0.0355 0.054 Uiso 1 1 calc R . . C22 C -0.3191(3) -0.1215(3) -0.0918(2) 0.0415(11) Uani 1 1 d . . . H22 H -0.3530 -0.1788 -0.1075 0.050 Uiso 1 1 calc R . . C23 C -0.3467(3) -0.0428(3) -0.11190(18) 0.0365(10) Uani 1 1 d . . . C24 C -0.2224(3) 0.0433(3) -0.04977(18) 0.0390(11) Uani 1 1 d . . . H24 H -0.1876 0.1012 -0.0359 0.047 Uiso 1 1 calc R . . C25 C -0.4337(3) -0.0405(3) -0.15380(17) 0.0370(10) Uani 1 1 d . . . C26 C -0.5021(4) -0.1158(4) -0.1727(2) 0.0482(12) Uani 1 1 d . . . H26 H -0.4930 -0.1733 -0.1604 0.058 Uiso 1 1 calc R . . C27 C -0.5836(4) -0.1069(4) -0.2095(2) 0.0565(14) Uani 1 1 d . . . H27 H -0.6310 -0.1582 -0.2224 0.068 Uiso 1 1 calc R . . C28 C -0.5962(4) -0.0227(4) -0.2275(2) 0.0559(14) Uani 1 1 d . . . C29 C -0.5240(4) 0.0489(4) -0.20713(19) 0.0456(12) Uani 1 1 d . . . H29 H -0.5313 0.1069 -0.2192 0.055 Uiso 1 1 calc R . . C30 C -0.6847(5) -0.0101(5) -0.2679(3) 0.080(2) Uani 1 1 d . . . H30A H -0.6752 0.0497 -0.2819 0.119 Uiso 1 1 calc R . . H30B H -0.7363 -0.0153 -0.2504 0.119 Uiso 1 1 calc R . . H30C H -0.6998 -0.0566 -0.2975 0.119 Uiso 1 1 calc R . . C31 C -0.0061(4) 0.2500(4) 0.5597(2) 0.0582(15) Uani 1 1 d . . . H31A H -0.0458 0.2716 0.5804 0.087 Uiso 1 1 calc R . . H31B H 0.0571 0.2534 0.5827 0.087 Uiso 1 1 calc R . . H31C H -0.0319 0.1874 0.5461 0.087 Uiso 1 1 calc R . . C32 C -0.0023(3) 0.3081(4) 0.5132(2) 0.0458(12) Uani 1 1 d . . . C33 C -0.0696(4) 0.3585(4) 0.4917(2) 0.0536(14) Uani 1 1 d . . . H33 H -0.1222 0.3572 0.5062 0.064 Uiso 1 1 calc R . . C34 C -0.0612(4) 0.4109(4) 0.4495(2) 0.0525(13) Uani 1 1 d . . . H34 H -0.1074 0.4460 0.4351 0.063 Uiso 1 1 calc R . . C35 C 0.0161(3) 0.4119(3) 0.4280(2) 0.0392(11) Uani 1 1 d . . . C36 C 0.0719(3) 0.3118(3) 0.4887(2) 0.0434(12) Uani 1 1 d . . . H36 H 0.1185 0.2767 0.5022 0.052 Uiso 1 1 calc R . . C37 C 0.0333(3) 0.4676(3) 0.3837(2) 0.0408(11) Uani 1 1 d . . . C38 C -0.0164(4) 0.5356(4) 0.3645(2) 0.0507(13) Uani 1 1 d . . . H38 H -0.0677 0.5456 0.3780 0.061 Uiso 1 1 calc R . . C39 C 0.0098(4) 0.5878(4) 0.3261(2) 0.0531(14) Uani 1 1 d . . . H39 H -0.0236 0.6345 0.3131 0.064 Uiso 1 1 calc R . . C40 C 0.0847(4) 0.5734(3) 0.3059(2) 0.0455(12) Uani 1 1 d . . . C41 C 0.1285(3) 0.5024(3) 0.3259(2) 0.0419(11) Uani 1 1 d . . . H41 H 0.1783 0.4896 0.3118 0.050 Uiso 1 1 calc R . . C42 C 0.1209(4) 0.6348(4) 0.2684(2) 0.0541(14) Uani 1 1 d . . . H42A H 0.0671 0.6526 0.2427 0.065 Uiso 1 1 calc R . . H42B H 0.1587 0.6902 0.2893 0.065 Uiso 1 1 calc R . . C43 C 0.1305(4) 0.5462(4) 0.1909(2) 0.0474(12) Uani 1 1 d . . . C44 C 0.0350(4) 0.5176(4) 0.1737(2) 0.0545(14) Uani 1 1 d . . . H44 H -0.0039 0.5312 0.1957 0.065 Uiso 1 1 calc R . . C45 C -0.0047(4) 0.4692(4) 0.1248(2) 0.0497(13) Uani 1 1 d . . . H45 H -0.0704 0.4500 0.1134 0.060 Uiso 1 1 calc R . . C46 C 0.0513(3) 0.4493(3) 0.0930(2) 0.0432(11) Uani 1 1 d . . . C47 C 0.1479(4) 0.4754(4) 0.1105(2) 0.0511(13) Uani 1 1 d . . . H47 H 0.1869 0.4602 0.0890 0.061 Uiso 1 1 calc R . . C48 C 0.1869(4) 0.5240(4) 0.1597(2) 0.0503(13) Uani 1 1 d . . . H48 H 0.2527 0.5419 0.1717 0.060 Uiso 1 1 calc R . . C49 C -0.0787(3) 0.3822(4) 0.0212(2) 0.0455(12) Uani 1 1 d . . . H49A H -0.1049 0.4384 0.0161 0.055 Uiso 1 1 calc R . . H49B H -0.1085 0.3460 0.0459 0.055 Uiso 1 1 calc R . . C50 C -0.0975(3) 0.3294(3) -0.03197(19) 0.0403(11) Uani 1 1 d . . . C51 C -0.0297(4) 0.3279(4) -0.0596(2) 0.0471(12) Uani 1 1 d . . . H51 H 0.0317 0.3608 -0.0454 0.057 Uiso 1 1 calc R . . C52 C -0.0517(3) 0.2777(4) -0.1086(2) 0.0459(12) Uani 1 1 d . . . H52 H -0.0059 0.2776 -0.1283 0.055 Uiso 1 1 calc R . . C53 C -0.1406(3) 0.2280(3) -0.12829(19) 0.0373(10) Uani 1 1 d . . . C54 C -0.1863(3) 0.2810(3) -0.05575(19) 0.0379(10) Uani 1 1 d . . . H54 H -0.2343 0.2837 -0.0380 0.045 Uiso 1 1 calc R . . C55 C -0.1674(3) 0.1670(3) -0.17775(18) 0.0353(10) Uani 1 1 d . . . C56 C -0.1087(4) 0.1598(4) -0.2112(2) 0.0470(12) Uani 1 1 d . . . H56 H -0.0473 0.1944 -0.2029 0.056 Uiso 1 1 calc R . . C57 C -0.1407(4) 0.1015(4) -0.2569(2) 0.0497(13) Uani 1 1 d . . . H57 H -0.1017 0.0973 -0.2806 0.060 Uiso 1 1 calc R . . C58 C -0.2297(4) 0.0491(4) -0.2683(2) 0.0472(13) Uani 1 1 d . . . C59 C -0.2835(4) 0.0594(3) -0.23225(18) 0.0408(11) Uani 1 1 d . . . H59 H -0.3442 0.0238 -0.2389 0.049 Uiso 1 1 calc R . . C60 C -0.2672(4) -0.0190(4) -0.3153(2) 0.0602(15) Uani 1 1 d . . . H60A H -0.2364 -0.0716 -0.3087 0.090 Uiso 1 1 calc R . . H60B H -0.2550 0.0080 -0.3477 0.090 Uiso 1 1 calc R . . H60C H -0.3347 -0.0379 -0.3204 0.090 Uiso 1 1 calc R . . C61 C 0.4041(4) 0.1882(4) 0.5597(3) 0.0660(17) Uani 1 1 d . . . H61A H 0.3871 0.1464 0.5857 0.099 Uiso 1 1 calc R . . H61B H 0.4145 0.2504 0.5751 0.099 Uiso 1 1 calc R . . H61C H 0.4614 0.1760 0.5513 0.099 Uiso 1 1 calc R . . C62 C 0.3270(4) 0.1759(4) 0.5098(2) 0.0530(14) Uani 1 1 d . . . C63 C 0.2805(5) 0.0917(4) 0.4862(3) 0.0602(16) Uani 1 1 d . . . H63 H 0.2984 0.0389 0.5019 0.072 Uiso 1 1 calc R . . C64 C 0.2096(4) 0.0837(4) 0.4408(3) 0.0566(15) Uani 1 1 d . . . H64 H 0.1790 0.0258 0.4246 0.068 Uiso 1 1 calc R . . C65 C 0.1823(4) 0.1616(3) 0.4182(2) 0.0466(13) Uani 1 1 d . . . C66 C 0.2960(3) 0.2500(4) 0.4846(2) 0.0467(12) Uani 1 1 d . . . H66 H 0.3263 0.3085 0.5001 0.056 Uiso 1 1 calc R . . C67 C 0.1075(4) 0.1610(3) 0.3689(2) 0.0503(13) Uani 1 1 d . . . C68 C 0.0619(4) 0.0832(4) 0.3365(3) 0.0634(16) Uani 1 1 d . . . H68 H 0.0741 0.0257 0.3473 0.076 Uiso 1 1 calc R . . C69 C -0.0019(5) 0.0909(4) 0.2883(3) 0.075(2) Uani 1 1 d . . . H69 H -0.0315 0.0387 0.2652 0.090 Uiso 1 1 calc R . . C70 C -0.0220(4) 0.1751(4) 0.2741(3) 0.0611(16) Uani 1 1 d . . . C71 C 0.0224(4) 0.2481(4) 0.3101(3) 0.0544(14) Uani 1 1 d . . . H71 H 0.0059 0.3053 0.3020 0.065 Uiso 1 1 calc R . . C72 C -0.0880(4) 0.1907(5) 0.2226(3) 0.076(2) Uani 1 1 d . . . H72A H -0.1377 0.2210 0.2301 0.092 Uiso 1 1 calc R . . H72B H -0.0541 0.2297 0.2007 0.092 Uiso 1 1 calc R . . C73 C -0.2077(5) 0.1038(5) 0.1540(3) 0.075(2) Uani 1 1 d . . . C74 C -0.2552(5) 0.0180(5) 0.1346(3) 0.082(2) Uani 1 1 d . . . H74 H -0.2302 -0.0336 0.1473 0.098 Uiso 1 1 calc R . . C75 C -0.3404(5) 0.0084(5) 0.0962(3) 0.080(2) Uani 1 1 d . . . H75 H -0.3732 -0.0499 0.0819 0.096 Uiso 1 1 calc R . . C76 C -0.3763(5) 0.0834(5) 0.0791(2) 0.074(2) Uani 1 1 d . . . C77 C -0.3259(5) 0.1707(5) 0.0961(3) 0.0705(19) Uani 1 1 d . . . H77 H -0.3496 0.2223 0.0821 0.085 Uiso 1 1 calc R . . C78 C -0.2409(4) 0.1797(5) 0.1337(3) 0.0695(19) Uani 1 1 d . . . H78 H -0.2053 0.2380 0.1457 0.083 Uiso 1 1 calc R . . C79 C -0.5100(5) 0.1401(8) 0.0293(3) 0.097(3) Uani 1 1 d . . . H79A H -0.4954 0.1837 0.0608 0.117 Uiso 1 1 calc R . . H79B H -0.5783 0.1181 0.0196 0.117 Uiso 1 1 calc R . . C80 C -0.4843(4) 0.1893(5) -0.0170(2) 0.0596(17) Uani 1 1 d . . . C81 C -0.5226(4) 0.2639(6) -0.0354(3) 0.080(2) Uani 1 1 d . . . H81 H -0.5599 0.2894 -0.0162 0.096 Uiso 1 1 calc R . . C82 C -0.5071(4) 0.3012(5) -0.0812(3) 0.0629(17) Uani 1 1 d . . . H82 H -0.5331 0.3525 -0.0937 0.075 Uiso 1 1 calc R . . C83 C -0.4524(3) 0.2627(3) -0.1092(2) 0.0409(11) Uani 1 1 d . . . C84 C -0.4272(4) 0.1560(4) -0.04520(19) 0.0480(13) Uani 1 1 d . . . H84 H -0.3990 0.1059 -0.0327 0.058 Uiso 1 1 calc R . . C85 C -0.4388(3) 0.2914(3) -0.16166(19) 0.0371(10) Uani 1 1 d . . . C86 C -0.4805(4) 0.3581(4) -0.1887(2) 0.0521(14) Uani 1 1 d . . . H86 H -0.5174 0.3905 -0.1729 0.062 Uiso 1 1 calc R . . C87 C -0.4683(4) 0.3774(4) -0.2385(2) 0.0570(15) Uani 1 1 d . . . H87 H -0.4964 0.4236 -0.2569 0.068 Uiso 1 1 calc R . . C88 C -0.4151(3) 0.3299(3) -0.2625(2) 0.0421(11) Uani 1 1 d . . . C89 C -0.3753(3) 0.2646(3) -0.23244(19) 0.0369(10) Uani 1 1 d . . . H89 H -0.3378 0.2316 -0.2474 0.044 Uiso 1 1 calc R . . C90 C -0.4007(4) 0.3468(4) -0.3168(2) 0.0549(14) Uani 1 1 d . . . H90A H -0.3474 0.3957 -0.3138 0.082 Uiso 1 1 calc R . . H90B H -0.4570 0.3640 -0.3395 0.082 Uiso 1 1 calc R . . H90C H -0.3884 0.2919 -0.3328 0.082 Uiso 1 1 calc R . . O3T O 0.4863(8) 0.1782(8) 0.3605(4) 0.0862(19) Uiso 0.45 1 d PD A 1 C9T C 0.5428(12) 0.1227(11) 0.3522(7) 0.0862(19) Uiso 0.45 1 d PD A 1 H9T1 H 0.6084 0.1547 0.3611 0.103 Uiso 0.45 1 calc PR A 1 H9T2 H 0.5251 0.0991 0.3142 0.103 Uiso 0.45 1 calc PR A 1 C10T C 0.5036(14) 0.0921(15) 0.4322(6) 0.0862(19) Uiso 0.45 1 d PD A 1 H10A H 0.4601 0.0486 0.4465 0.103 Uiso 0.45 1 calc PR A 1 H10B H 0.5588 0.1170 0.4617 0.103 Uiso 0.45 1 calc PR A 1 C11T C 0.4570(15) 0.1651(14) 0.4066(7) 0.0862(19) Uiso 0.45 1 d PD A 1 H11A H 0.3882 0.1469 0.3982 0.103 Uiso 0.45 1 calc PR A 1 H11B H 0.4756 0.2209 0.4306 0.103 Uiso 0.45 1 calc PR A 1 C12T C 0.5319(13) 0.0483(11) 0.3877(7) 0.0862(19) Uiso 0.45 1 d PD A 1 H12C H 0.5914 0.0262 0.4010 0.103 Uiso 0.45 1 calc PR A 1 H12D H 0.4830 -0.0026 0.3690 0.103 Uiso 0.45 1 calc PR A 1 O1T O 0.2415(7) 0.0101(9) 0.5901(4) 0.062(3) Uani 0.50 1 d P B 1 C1T C 0.1730(11) 0.0688(12) 0.5915(7) 0.071(4) Uiso 0.50 1 d P B 1 H1T1 H 0.1761 0.0876 0.6291 0.085 Uiso 0.50 1 calc PR B 1 H1T2 H 0.1866 0.1236 0.5724 0.085 Uiso 0.50 1 calc PR B 1 C2T C 0.0867(12) 0.0219(11) 0.5674(7) 0.087(4) Uiso 0.50 1 d P B 1 H2T1 H 0.0704 0.0298 0.5284 0.104 Uiso 0.50 1 calc PR B 1 H2T2 H 0.0386 0.0413 0.5832 0.104 Uiso 0.50 1 calc PR B 1 C3T C 0.0966(11) -0.0837(10) 0.5794(7) 0.079(4) Uiso 0.50 1 d P B 1 H3T1 H 0.0828 -0.1010 0.6138 0.095 Uiso 0.50 1 calc PR B 1 H3T2 H 0.0580 -0.1272 0.5498 0.095 Uiso 0.50 1 calc PR B 1 C4T C 0.1989(14) -0.0714(14) 0.5818(9) 0.092(5) Uiso 0.50 1 d P B 1 H4T1 H 0.2291 -0.1069 0.6107 0.111 Uiso 0.50 1 calc PR B 1 H4T2 H 0.2064 -0.0964 0.5476 0.111 Uiso 0.50 1 calc PR B 1 O2T O 0.0970(17) 0.0180(16) 0.6040(10) 0.097(7) Uiso 0.25 1 d P C 2 C5T C 0.0749(18) -0.064(2) 0.5509(15) 0.092(10) Uiso 0.25 1 d PD C 2 H5T1 H 0.0277 -0.1166 0.5539 0.110 Uiso 0.25 1 calc PR C 2 H5T2 H 0.0566 -0.0392 0.5154 0.110 Uiso 0.25 1 calc PR C 2 C6T C 0.186(2) 0.050(2) 0.6078(12) 0.058(7) Uiso 0.25 1 d P C 2 H6T1 H 0.1908 0.0969 0.5816 0.070 Uiso 0.25 1 calc PR C 2 H6T2 H 0.2153 0.0798 0.6442 0.070 Uiso 0.25 1 calc PR C 2 C7T C 0.1702(16) -0.0843(16) 0.5629(11) 0.056(7) Uiso 0.25 1 d PD C 2 H7T1 H 0.1914 -0.0888 0.5295 0.068 Uiso 0.25 1 calc PR C 2 H7T2 H 0.1725 -0.1420 0.5803 0.068 Uiso 0.25 1 calc PR C 2 C8T C 0.230(2) -0.0087(19) 0.5994(11) 0.040(8) Uiso 0.25 1 d PD C 2 H8T1 H 0.2580 -0.0323 0.6340 0.048 Uiso 0.25 1 calc PR C 2 H8T2 H 0.2813 0.0183 0.5837 0.048 Uiso 0.25 1 calc PR C 2 C7S C 0.6804(10) 0.4384(10) 0.0272(7) 0.056(4) Uiso 0.45 1 d P D 2 C8S C 0.6348(11) 0.5002(11) 0.0114(6) 0.075(4) Uiso 0.45 1 d P D 2 H8S1 H 0.6100 0.5212 0.0404 0.112 Uiso 0.45 1 calc PR D 2 H8S2 H 0.5830 0.4767 -0.0196 0.112 Uiso 0.45 1 calc PR D 2 H8S3 H 0.6760 0.5506 0.0012 0.112 Uiso 0.45 1 calc PR D 2 N4S N 0.7237(11) 0.3747(11) 0.0460(8) 0.076(4) Uiso 0.45 1 d P D 2 C1S C 0.8571(10) 0.8137(8) 0.2710(6) 0.060(3) Uani 0.50 1 d P E 2 C2S C 0.7562(8) 0.7776(8) 0.2476(5) 0.062(3) Uani 0.50 1 d P E 2 H2S1 H 0.7217 0.7826 0.2749 0.092 Uiso 0.50 1 calc PR E 2 H2S2 H 0.7484 0.7141 0.2352 0.092 Uiso 0.50 1 calc PR E 2 H2S3 H 0.7322 0.8124 0.2172 0.092 Uiso 0.50 1 calc PR E 2 N1S N 0.9268(10) 0.8439(10) 0.2862(5) 0.088(4) Uani 0.50 1 d P E 2 C3S C 0.7681(8) 0.5143(10) 0.1988(6) 0.079(4) Uani 0.50 1 d P F 2 H3S1 H 0.7313 0.5235 0.2244 0.118 Uiso 0.50 1 calc PR F 2 H3S2 H 0.7260 0.4942 0.1635 0.118 Uiso 0.50 1 calc PR F 2 H3S3 H 0.8089 0.5712 0.1962 0.118 Uiso 0.50 1 calc PR F 2 C4S C 0.8246(7) 0.4464(6) 0.2169(4) 0.036(2) Uani 0.50 1 d P F 2 N2S N 0.8679(8) 0.4004(6) 0.2349(5) 0.062(3) Uani 0.50 1 d P F 2 C5S C 0.6686(9) 0.3324(7) 0.2916(5) 0.061(3) Uani 0.50 1 d P G 2 H5S1 H 0.6607 0.3303 0.2527 0.091 Uiso 0.50 1 calc PR G 2 H5S2 H 0.6805 0.3953 0.3058 0.091 Uiso 0.50 1 calc PR G 2 H5S3 H 0.6116 0.3002 0.2996 0.091 Uiso 0.50 1 calc PR G 2 C6S C 0.7455(9) 0.2905(8) 0.3159(4) 0.053(3) Uani 0.50 1 d P G 2 N3S N 0.7983(10) 0.2490(9) 0.3313(5) 0.086(4) Uani 0.50 1 d P G 2 O1W O 0.7005(13) 0.3832(13) 0.0081(8) 0.087(5) Uiso 0.30 1 d P H 1 O2W O 0.5325(16) 0.0521(16) 0.4239(10) 0.069(6) Uiso 0.20 1 d P I 2 O3W O 0.6958(15) 0.4215(15) 0.0496(9) 0.067(5) Uiso 0.25 1 d P J 3 O4W O 0.5162(19) 0.002(2) 0.3620(11) 0.062(7) Uiso 0.15 1 d P K 4 O5W O 0.4325(19) 0.2027(19) 0.3978(10) 0.082(7) Uiso 0.20 1 d P L 5 O6W O 0.7414(18) 0.3897(18) 0.0726(12) 0.074(7) Uiso 0.20 1 d P M 6 O7W O 0.4806(14) 0.1318(15) 0.4243(8) 0.064(4) Uiso 0.25 1 d P N 3 O8W O 0.4956(13) 0.0750(13) 0.3321(7) 0.068(5) Uiso 0.25 1 d P O 5 N1 N 0.2857(3) 0.4518(3) 0.44004(16) 0.0377(9) Uani 1 1 d . . . N2 N 0.2670(3) 0.3553(3) 0.35029(16) 0.0391(9) Uani 1 1 d . . . N3 N -0.2959(3) 0.0385(3) -0.09155(15) 0.0365(9) Uani 1 1 d . . . N4 N -0.4455(3) 0.0413(3) -0.17176(15) 0.0381(9) Uani 1 1 d . . . N5 N 0.0809(3) 0.3614(3) 0.44790(16) 0.0377(9) Uani 1 1 d . . . N6 N 0.1050(3) 0.4514(3) 0.36345(16) 0.0397(9) Uani 1 1 d . . . N7 N -0.2080(3) 0.2311(2) -0.10178(15) 0.0342(8) Uani 1 1 d . . . N8 N -0.2534(3) 0.1176(3) -0.18832(14) 0.0358(9) Uani 1 1 d . . . N9 N 0.2271(3) 0.2445(3) 0.44047(18) 0.0426(10) Uani 1 1 d . . . N10 N 0.0864(3) 0.2431(3) 0.3553(2) 0.0493(11) Uani 1 1 d . . . N11 N -0.4111(3) 0.1935(3) -0.09008(15) 0.0373(9) Uani 1 1 d . . . N12 N -0.3865(3) 0.2452(3) -0.18350(15) 0.0357(8) Uani 1 1 d . . . O1 O 0.2028(3) 0.1893(3) 0.21762(16) 0.0734(13) Uani 1 1 d . . . O2 O -0.0643(3) 0.0676(3) 0.02962(16) 0.0593(10) Uani 1 1 d . . . O3 O 0.1769(3) 0.5971(3) 0.23873(14) 0.0538(9) Uani 1 1 d . . . O4 O 0.0198(2) 0.4031(2) 0.04285(14) 0.0485(9) Uani 1 1 d . . . O5 O -0.1277(3) 0.1057(3) 0.1947(2) 0.0900(17) Uani 1 1 d . . . O6 O -0.4648(4) 0.0665(4) 0.04413(17) 0.0856(17) Uani 1 1 d . . . F1 F 0.2505(4) 0.8087(4) 0.47607(19) 0.0611(14) Uani 0.65 1 d P P 1 F2 F 0.3662(6) 0.7697(8) 0.4443(6) 0.0660(18) Uani 0.65 1 d P P 1 F3 F 0.2101(4) 0.7177(3) 0.4017(2) 0.0686(15) Uani 0.65 1 d P P 1 F4 F 0.3019(12) 0.8192(9) 0.3630(5) 0.073(2) Uani 0.65 1 d P P 1 F5 F 0.1869(3) 0.8605(3) 0.3976(2) 0.0510(11) Uani 0.65 1 d P P 1 F6 F 0.3392(4) 0.9107(4) 0.4369(3) 0.0721(18) Uani 0.65 1 d P P 1 F1A F 0.301(3) 0.814(3) 0.3634(16) 0.124(3) Uiso 0.35 1 d P P 2 F2A F 0.2326(14) 0.7582(13) 0.4629(8) 0.124(3) Uiso 0.35 1 d P P 2 F3A F 0.1774(12) 0.8007(13) 0.3788(7) 0.124(3) Uiso 0.35 1 d P P 2 F4A F 0.2571(13) 0.6910(13) 0.3955(7) 0.124(3) Uiso 0.35 1 d P P 2 F5A F 0.2961(14) 0.8999(16) 0.4357(9) 0.124(3) Uiso 0.35 1 d P P 2 F6A F 0.372(2) 0.779(2) 0.4411(16) 0.124(3) Uiso 0.35 1 d P P 2 F7 F 0.6423(4) 0.5977(4) 0.4107(3) 0.0642(16) Uani 0.65 1 d P Q 1 F8 F 0.7736(8) 0.5441(9) 0.4013(7) 0.103(3) Uani 0.65 1 d P Q 1 F9 F 0.6430(5) 0.5201(5) 0.3357(4) 0.102(2) Uani 0.65 1 d P Q 1 F10 F 0.6514(5) 0.6820(5) 0.3360(4) 0.070(2) Uani 0.65 1 d P Q 1 F11 F 0.7673(5) 0.6983(5) 0.4027(3) 0.072(2) Uani 0.65 1 d P Q 1 F12 F 0.7729(5) 0.6158(6) 0.3281(3) 0.082(2) Uani 0.65 1 d P Q 1 F7A F 0.770(2) 0.545(2) 0.4024(11) 0.101(3) Uiso 0.35 1 d P Q 2 F8A F 0.6350(19) 0.6580(13) 0.3357(12) 0.101(3) Uiso 0.35 1 d PD Q 2 F9A F 0.6270(13) 0.5713(13) 0.3881(7) 0.101(3) Uiso 0.35 1 d P Q 2 F10A F 0.6680(12) 0.5491(11) 0.3144(7) 0.101(3) Uiso 0.35 1 d PD Q 2 F11A F 0.7988(14) 0.6504(13) 0.3455(8) 0.101(3) Uiso 0.35 1 d P Q 2 F12A F 0.7597(17) 0.6754(15) 0.4145(9) 0.101(3) Uiso 0.35 1 d P Q 2 P1 P 0.27546(10) 0.80895(11) 0.41884(6) 0.0532(4) Uani 1 1 d . . . P2 P 0.70930(10) 0.60862(11) 0.36750(7) 0.0560(4) Uani 1 1 d . . . P3 P 0.4849(2) 0.39299(13) 0.13958(10) 0.0525(5) Uani 0.80 1 d P R 1 F13 F 0.4436(4) 0.3119(3) 0.1704(2) 0.0846(16) Uani 0.80 1 d P R 1 F14 F 0.5354(3) 0.4452(3) 0.19651(18) 0.0676(12) Uani 0.80 1 d P R 1 F15 F 0.5735(4) 0.3448(3) 0.1437(2) 0.0866(16) Uani 0.80 1 d P R 1 F16 F 0.5280(5) 0.4733(3) 0.1109(2) 0.0874(18) Uani 0.80 1 d P R 1 F17 F 0.4377(5) 0.3366(4) 0.0847(2) 0.105(2) Uani 0.80 1 d P R 1 F18 F 0.3962(4) 0.4386(5) 0.1373(3) 0.098(2) Uani 0.80 1 d P R 1 P3A P 0.4269(11) 0.4068(9) 0.1206(6) 0.083(3) Uani 0.20 1 d P S 2 F13A F 0.3286(17) 0.3426(17) 0.1070(10) 0.103(3) Uiso 0.20 1 d P S 2 F14A F 0.451(2) 0.382(2) 0.0690(12) 0.103(3) Uiso 0.20 1 d P S 2 F15A F 0.536(2) 0.465(2) 0.1376(12) 0.103(3) Uiso 0.20 1 d P S 2 F16A F 0.3858(18) 0.4870(18) 0.0959(11) 0.103(3) Uiso 0.20 1 d P S 2 F17A F 0.477(2) 0.321(2) 0.1432(11) 0.103(3) Uiso 0.20 1 d P S 2 F18A F 0.416(2) 0.4310(19) 0.1747(12) 0.103(3) Uiso 0.20 1 d P S 2 P4 P 0.78977(17) 0.7271(2) 0.09521(15) 0.0619(7) Uani 0.70 1 d P T 1 F19 F 0.7212(4) 0.7119(5) 0.0360(3) 0.105(2) Uani 0.70 1 d P T 1 F20 F 0.8315(3) 0.6405(4) 0.0829(3) 0.0816(16) Uani 0.70 1 d P T 1 F21 F 0.7112(3) 0.6643(4) 0.1143(3) 0.0760(17) Uani 0.70 1 d P T 1 F22 F 0.8611(4) 0.7273(6) 0.1538(2) 0.0733(18) Uani 0.70 1 d P T 1 F23 F 0.7448(5) 0.8114(6) 0.1081(6) 0.166(5) Uani 0.70 1 d P T 1 F24 F 0.8681(4) 0.7877(5) 0.0735(4) 0.108(3) Uani 0.70 1 d P T 1 P4A P 0.8065(8) 0.7721(7) 0.1199(5) 0.095(3) Uani 0.30 1 d P U 2 F19A F 0.8864(15) 0.8398(15) 0.1182(9) 0.128(3) Uiso 0.30 1 d P U 2 F20A F 0.8261(17) 0.7070(19) 0.0710(9) 0.128(3) Uiso 0.30 1 d P U 2 F21A F 0.7408(18) 0.8071(19) 0.0671(9) 0.128(3) Uiso 0.30 1 d P U 2 F22A F 0.7202(18) 0.7078(17) 0.1311(10) 0.128(3) Uiso 0.30 1 d P U 2 F23A F 0.876(2) 0.728(2) 0.1740(11) 0.128(3) Uiso 0.30 1 d P U 2 F24A F 0.7894(15) 0.8351(15) 0.1589(9) 0.128(3) Uiso 0.30 1 d P U 2 Ni1 Ni 0.17598(4) 0.35212(4) 0.40089(3) 0.03826(18) Uani 1 1 d . . . Ni2 Ni -0.33398(4) 0.14559(4) -0.13722(2) 0.03322(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.062(4) 0.045(3) 0.058(3) 0.000(3) 0.013(3) -0.001(3) C2 0.042(3) 0.034(3) 0.055(3) 0.008(2) 0.010(2) 0.007(2) C3 0.043(3) 0.033(3) 0.054(3) 0.012(2) 0.004(2) 0.000(2) C4 0.034(2) 0.044(3) 0.048(3) 0.015(2) 0.011(2) 0.004(2) C5 0.030(2) 0.037(3) 0.050(3) 0.015(2) 0.011(2) 0.009(2) C6 0.040(3) 0.041(3) 0.052(3) 0.006(2) 0.018(2) 0.006(2) C7 0.030(2) 0.039(3) 0.049(3) 0.014(2) 0.011(2) 0.014(2) C8 0.031(2) 0.049(3) 0.057(3) 0.016(2) 0.014(2) 0.009(2) C9 0.041(3) 0.062(4) 0.055(3) 0.013(3) 0.027(2) 0.015(3) C10 0.042(3) 0.052(3) 0.046(3) 0.013(2) 0.018(2) 0.013(2) C11 0.032(2) 0.045(3) 0.052(3) 0.003(2) 0.014(2) 0.007(2) C12 0.065(4) 0.079(4) 0.053(3) 0.001(3) 0.027(3) 0.008(3) C13 0.053(3) 0.055(3) 0.046(3) 0.002(2) 0.025(2) 0.011(3) C14 0.061(4) 0.035(3) 0.081(4) 0.005(3) 0.011(3) 0.010(3) C15 0.057(3) 0.047(3) 0.073(4) 0.024(3) 0.005(3) 0.014(3) C16 0.040(3) 0.046(3) 0.054(3) 0.015(2) 0.015(2) 0.014(2) C17 0.054(3) 0.045(3) 0.054(3) 0.014(2) 0.008(3) 0.009(3) C18 0.058(3) 0.063(4) 0.052(3) 0.020(3) 0.017(3) 0.012(3) C19 0.041(3) 0.047(3) 0.053(3) 0.016(2) 0.016(2) 0.010(2) C20 0.037(2) 0.045(3) 0.045(3) 0.013(2) 0.019(2) 0.012(2) C21 0.043(3) 0.045(3) 0.056(3) 0.014(2) 0.026(2) 0.015(2) C22 0.042(3) 0.041(3) 0.049(3) 0.006(2) 0.024(2) 0.009(2) C23 0.046(3) 0.034(3) 0.039(2) 0.008(2) 0.026(2) 0.008(2) C24 0.041(3) 0.041(3) 0.038(3) 0.007(2) 0.017(2) 0.005(2) C25 0.045(3) 0.039(3) 0.030(2) 0.0015(19) 0.018(2) 0.003(2) C26 0.060(3) 0.041(3) 0.042(3) 0.004(2) 0.017(2) 0.000(3) C27 0.064(4) 0.046(3) 0.048(3) -0.003(2) 0.005(3) -0.008(3) C28 0.058(3) 0.061(4) 0.040(3) -0.001(3) 0.002(3) 0.002(3) C29 0.054(3) 0.044(3) 0.036(3) 0.001(2) 0.011(2) 0.003(2) C30 0.075(4) 0.071(5) 0.067(4) 0.000(3) -0.019(3) -0.002(4) C31 0.052(3) 0.061(4) 0.072(4) 0.011(3) 0.033(3) 0.012(3) C32 0.035(3) 0.044(3) 0.060(3) 0.002(2) 0.018(2) 0.004(2) C33 0.037(3) 0.067(4) 0.067(4) 0.009(3) 0.029(3) 0.015(3) C34 0.038(3) 0.060(4) 0.067(4) 0.006(3) 0.021(3) 0.019(3) C35 0.031(2) 0.039(3) 0.049(3) -0.002(2) 0.015(2) 0.007(2) C36 0.035(3) 0.041(3) 0.059(3) 0.003(2) 0.019(2) 0.010(2) C37 0.035(2) 0.037(3) 0.052(3) -0.001(2) 0.014(2) 0.007(2) C38 0.049(3) 0.056(3) 0.055(3) 0.007(3) 0.019(3) 0.024(3) C39 0.055(3) 0.047(3) 0.058(3) 0.002(3) 0.010(3) 0.021(3) C40 0.046(3) 0.039(3) 0.046(3) -0.003(2) 0.008(2) 0.000(2) C41 0.033(2) 0.043(3) 0.049(3) 0.002(2) 0.013(2) 0.001(2) C42 0.060(3) 0.044(3) 0.053(3) 0.000(2) 0.010(3) 0.001(3) C43 0.047(3) 0.043(3) 0.046(3) 0.007(2) 0.007(2) -0.001(2) C44 0.046(3) 0.059(4) 0.056(3) 0.000(3) 0.017(3) -0.005(3) C45 0.039(3) 0.059(3) 0.046(3) 0.004(2) 0.009(2) -0.003(2) C46 0.042(3) 0.037(3) 0.047(3) 0.005(2) 0.008(2) 0.003(2) C47 0.038(3) 0.052(3) 0.062(3) 0.003(3) 0.013(2) 0.005(2) C48 0.037(3) 0.053(3) 0.057(3) 0.009(3) 0.006(2) 0.004(2) C49 0.031(2) 0.049(3) 0.054(3) 0.001(2) 0.011(2) 0.002(2) C50 0.037(3) 0.040(3) 0.046(3) 0.009(2) 0.014(2) 0.009(2) C51 0.039(3) 0.050(3) 0.054(3) 0.007(2) 0.015(2) 0.006(2) C52 0.035(3) 0.058(3) 0.049(3) 0.007(2) 0.019(2) 0.007(2) C53 0.036(2) 0.037(3) 0.046(3) 0.010(2) 0.018(2) 0.012(2) C54 0.039(3) 0.034(3) 0.045(3) 0.004(2) 0.019(2) 0.008(2) C55 0.038(3) 0.035(3) 0.042(3) 0.015(2) 0.019(2) 0.016(2) C56 0.050(3) 0.047(3) 0.058(3) 0.020(2) 0.029(3) 0.019(2) C57 0.063(3) 0.047(3) 0.055(3) 0.013(2) 0.039(3) 0.018(3) C58 0.062(3) 0.047(3) 0.046(3) 0.013(2) 0.026(3) 0.026(3) C59 0.049(3) 0.042(3) 0.036(3) 0.008(2) 0.010(2) 0.021(2) C60 0.072(4) 0.074(4) 0.044(3) -0.001(3) 0.022(3) 0.027(3) C61 0.054(3) 0.065(4) 0.089(5) 0.027(3) 0.023(3) 0.025(3) C62 0.047(3) 0.046(3) 0.080(4) 0.012(3) 0.037(3) 0.016(3) C63 0.071(4) 0.049(4) 0.079(4) 0.016(3) 0.044(4) 0.025(3) C64 0.073(4) 0.034(3) 0.080(4) 0.002(3) 0.051(4) 0.012(3) C65 0.044(3) 0.043(3) 0.063(3) -0.003(2) 0.034(3) 0.009(2) C66 0.034(3) 0.044(3) 0.071(4) 0.005(2) 0.027(3) 0.012(2) C67 0.047(3) 0.039(3) 0.075(4) -0.005(3) 0.037(3) 0.004(2) C68 0.055(4) 0.048(4) 0.090(5) -0.015(3) 0.030(3) 0.003(3) C69 0.058(4) 0.051(4) 0.113(6) -0.027(4) 0.030(4) -0.009(3) C70 0.035(3) 0.057(4) 0.089(4) -0.022(3) 0.021(3) 0.000(3) C71 0.036(3) 0.045(3) 0.084(4) -0.011(3) 0.024(3) 0.003(2) C72 0.044(3) 0.068(4) 0.105(5) -0.033(4) 0.011(3) -0.007(3) C73 0.057(4) 0.065(4) 0.099(5) -0.037(4) 0.029(4) -0.009(3) C74 0.082(5) 0.067(5) 0.091(5) -0.040(4) 0.032(4) -0.011(4) C75 0.087(5) 0.068(5) 0.073(4) -0.037(4) 0.034(4) -0.034(4) C76 0.073(4) 0.089(5) 0.047(3) -0.032(3) 0.031(3) -0.040(4) C77 0.066(4) 0.074(4) 0.065(4) -0.026(3) 0.031(3) -0.023(3) C78 0.052(4) 0.070(5) 0.076(4) -0.034(4) 0.017(3) -0.015(3) C79 0.055(4) 0.172(10) 0.048(4) -0.032(5) 0.031(3) -0.048(5) C80 0.034(3) 0.093(5) 0.047(3) -0.026(3) 0.021(2) -0.014(3) C81 0.032(3) 0.143(7) 0.066(4) -0.043(4) 0.023(3) 0.008(4) C82 0.036(3) 0.086(5) 0.068(4) -0.025(3) 0.013(3) 0.020(3) C83 0.025(2) 0.048(3) 0.048(3) -0.012(2) 0.011(2) 0.003(2) C84 0.046(3) 0.058(3) 0.040(3) -0.005(2) 0.024(2) -0.008(2) C85 0.027(2) 0.035(3) 0.048(3) -0.010(2) 0.010(2) 0.0017(19) C86 0.048(3) 0.047(3) 0.061(3) -0.012(3) 0.004(3) 0.023(3) C87 0.060(4) 0.044(3) 0.063(4) 0.000(3) -0.002(3) 0.024(3) C88 0.041(3) 0.034(3) 0.050(3) 0.005(2) 0.005(2) 0.010(2) C89 0.034(2) 0.034(3) 0.048(3) 0.008(2) 0.017(2) 0.008(2) C90 0.062(3) 0.049(3) 0.055(3) 0.019(3) 0.008(3) 0.021(3) O1T 0.037(5) 0.083(8) 0.076(7) 0.027(5) 0.034(5) 0.001(4) C1S 0.070(8) 0.045(7) 0.085(9) 0.013(6) 0.059(7) 0.008(6) C2S 0.071(8) 0.043(6) 0.094(9) 0.017(6) 0.056(7) 0.021(6) N1S 0.087(9) 0.102(10) 0.084(9) 0.007(7) 0.051(8) -0.005(8) C3S 0.039(6) 0.083(10) 0.105(11) 0.045(8) 0.004(7) 0.002(6) C4S 0.036(5) 0.021(5) 0.049(6) 0.000(4) 0.022(4) -0.016(4) N2S 0.076(7) 0.023(5) 0.100(8) 0.008(5) 0.050(6) 0.003(5) C5S 0.093(9) 0.028(6) 0.060(7) 0.004(5) 0.010(6) 0.020(6) C6S 0.076(8) 0.045(7) 0.038(6) -0.002(5) 0.024(6) -0.007(6) N3S 0.100(10) 0.083(9) 0.079(8) 0.026(7) 0.020(7) 0.031(8) N1 0.035(2) 0.032(2) 0.051(2) 0.0071(17) 0.0163(18) 0.0079(17) N2 0.0279(19) 0.042(2) 0.050(2) 0.0048(19) 0.0150(17) 0.0071(17) N3 0.042(2) 0.033(2) 0.035(2) 0.0063(16) 0.0134(17) 0.0053(17) N4 0.043(2) 0.040(2) 0.034(2) 0.0029(17) 0.0169(18) 0.0049(18) N5 0.0292(19) 0.031(2) 0.056(2) 0.0025(18) 0.0166(18) 0.0060(16) N6 0.033(2) 0.037(2) 0.050(2) -0.0016(18) 0.0133(18) 0.0057(17) N7 0.037(2) 0.031(2) 0.040(2) 0.0074(16) 0.0189(17) 0.0080(16) N8 0.040(2) 0.040(2) 0.033(2) 0.0094(16) 0.0126(16) 0.0170(18) N9 0.037(2) 0.035(2) 0.065(3) -0.0007(19) 0.028(2) 0.0105(18) N10 0.032(2) 0.043(3) 0.076(3) -0.008(2) 0.025(2) 0.0024(19) N11 0.033(2) 0.041(2) 0.038(2) -0.0061(17) 0.0153(17) -0.0031(17) N12 0.0317(19) 0.032(2) 0.047(2) 0.0042(17) 0.0152(17) 0.0076(16) O1 0.086(3) 0.076(3) 0.049(2) -0.006(2) 0.022(2) -0.019(2) O2 0.044(2) 0.057(2) 0.067(2) 0.0276(19) -0.0017(18) 0.0011(18) O3 0.049(2) 0.056(2) 0.049(2) 0.0057(17) 0.0098(17) -0.0087(18) O4 0.0350(18) 0.054(2) 0.052(2) -0.0015(17) 0.0073(15) 0.0032(16) O5 0.060(3) 0.077(3) 0.117(4) -0.051(3) 0.000(3) 0.010(2) O6 0.086(4) 0.111(4) 0.042(2) -0.012(3) 0.029(2) -0.050(3) F1 0.072(3) 0.083(4) 0.040(3) 0.010(3) 0.032(2) 0.019(3) F2 0.037(3) 0.072(4) 0.106(5) 0.049(3) 0.033(3) 0.030(3) F3 0.061(3) 0.042(3) 0.098(4) -0.010(3) 0.020(3) -0.001(2) F4 0.113(5) 0.079(4) 0.064(3) 0.034(3) 0.066(3) 0.054(4) F5 0.042(2) 0.048(3) 0.074(3) 0.017(2) 0.027(2) 0.018(2) F6 0.047(3) 0.040(3) 0.122(5) -0.009(3) 0.018(3) -0.005(3) F7 0.045(3) 0.071(4) 0.089(5) 0.012(3) 0.039(3) 0.015(3) F8 0.052(3) 0.099(5) 0.199(8) 0.098(5) 0.075(4) 0.055(3) F9 0.088(5) 0.072(5) 0.132(7) -0.032(4) 0.019(5) -0.011(4) F10 0.047(4) 0.088(5) 0.086(4) 0.030(5) 0.023(3) 0.034(4) F11 0.050(3) 0.067(5) 0.085(5) 0.016(3) 0.004(3) -0.006(3) F12 0.080(5) 0.126(7) 0.068(4) 0.025(4) 0.044(4) 0.054(5) P1 0.0430(8) 0.0636(10) 0.0575(9) 0.0138(7) 0.0213(7) 0.0076(7) P2 0.0378(7) 0.0631(10) 0.0690(10) 0.0050(8) 0.0132(7) 0.0146(7) P3 0.0675(14) 0.0301(11) 0.0689(13) -0.0059(8) 0.0385(12) 0.0033(10) F13 0.123(4) 0.045(3) 0.109(4) -0.004(2) 0.087(4) -0.005(3) F14 0.077(3) 0.050(2) 0.075(3) -0.010(2) 0.012(2) 0.019(2) F15 0.091(3) 0.061(3) 0.136(4) 0.000(3) 0.073(3) 0.028(3) F16 0.134(5) 0.049(3) 0.089(4) 0.018(3) 0.053(4) 0.005(3) F17 0.166(6) 0.065(4) 0.080(4) -0.027(3) 0.040(4) -0.003(4) F18 0.064(4) 0.092(5) 0.125(6) -0.035(4) -0.008(3) 0.032(3) P3A 0.077(9) 0.068(8) 0.110(10) 0.003(6) 0.028(8) 0.022(6) P4 0.0335(12) 0.0629(19) 0.092(2) 0.0145(15) 0.0165(13) 0.0155(12) F19 0.049(3) 0.150(7) 0.111(5) 0.034(5) 0.000(3) 0.029(4) F20 0.044(3) 0.084(4) 0.124(5) 0.017(4) 0.029(3) 0.015(3) F21 0.031(2) 0.094(5) 0.110(5) 0.003(3) 0.030(3) 0.013(3) F22 0.045(3) 0.103(4) 0.072(4) 0.010(4) 0.012(3) 0.019(3) F23 0.064(4) 0.081(5) 0.333(15) -0.089(8) 0.013(7) 0.030(4) F24 0.061(3) 0.097(5) 0.188(7) 0.099(5) 0.049(4) 0.033(3) P4A 0.107(8) 0.064(5) 0.121(8) 0.019(5) 0.044(6) 0.008(5) Ni1 0.0294(3) 0.0346(3) 0.0547(4) 0.0003(3) 0.0189(3) 0.0046(2) Ni2 0.0361(3) 0.0332(3) 0.0349(3) 0.0057(2) 0.0170(2) 0.0065(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 C1 C2 1.519(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.381(7) . ? C2 C6 1.387(7) . ? C3 C4 1.387(7) . ? C3 H3 0.9500 . ? C4 C5 1.393(7) . ? C4 H4 0.9500 . ? C5 N1 1.352(6) . ? C5 C7 1.473(7) . ? C6 N1 1.349(6) . ? C6 H6 0.9500 . ? C7 N2 1.350(6) . ? C7 C8 1.408(7) . ? C8 C9 1.378(8) . ? C8 H8 0.9500 . ? C9 C10 1.380(8) . ? C9 H9 0.9500 . ? C10 C11 1.394(7) . ? C10 C12 1.509(8) . ? C11 N2 1.329(6) . ? C11 H11 0.9500 . ? C12 O1 1.426(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C18 1.374(8) . ? C13 O1 1.378(7) . ? C13 C14 1.390(8) . ? C14 C15 1.372(8) . ? C14 H14 0.9500 . ? C15 C16 1.380(8) . ? C15 H15 0.9500 . ? C16 C17 1.378(7) . ? C16 O2 1.380(6) . ? C17 C18 1.380(8) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 O2 1.421(6) . ? C19 C20 1.496(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C24 1.384(7) . ? C20 C21 1.388(7) . ? C21 C22 1.376(7) . ? C21 H21 0.9500 . ? C22 C23 1.391(7) . ? C22 H22 0.9500 . ? C23 N3 1.348(6) . ? C23 C25 1.483(7) . ? C24 N3 1.331(6) . ? C24 H24 0.9500 . ? C25 N4 1.350(6) . ? C25 C26 1.385(7) . ? C26 C27 1.381(8) . ? C26 H26 0.9500 . ? C27 C28 1.386(8) . ? C27 H27 0.9500 . ? C28 C29 1.385(8) . ? C28 C30 1.517(8) . ? C29 N4 1.326(6) . ? C29 H29 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.507(8) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.380(7) . ? C32 C36 1.401(7) . ? C33 C34 1.378(8) . ? C33 H33 0.9500 . ? C34 C35 1.398(7) . ? C34 H34 0.9500 . ? C35 N5 1.345(6) . ? C35 C37 1.482(7) . ? C36 N5 1.325(6) . ? C36 H36 0.9500 . ? C37 N6 1.358(6) . ? C37 C38 1.395(7) . ? C38 C39 1.371(8) . ? C38 H38 0.9500 . ? C39 C40 1.394(8) . ? C39 H39 0.9500 . ? C40 C41 1.392(7) . ? C40 C42 1.488(8) . ? C41 N6 1.329(6) . ? C41 H41 0.9500 . ? C42 O3 1.437(7) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C48 1.374(8) . ? C43 C44 1.381(7) . ? C43 O3 1.396(6) . ? C44 C45 1.386(7) . ? C44 H44 0.9500 . ? C45 C46 1.369(7) . ? C45 H45 0.9500 . ? C46 O4 1.387(6) . ? C46 C47 1.393(7) . ? C47 C48 1.390(8) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 O4 1.423(6) . ? C49 C50 1.507(7) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.380(7) . ? C50 C54 1.392(7) . ? C51 C52 1.392(7) . ? C51 H51 0.9500 . ? C52 C53 1.384(7) . ? C52 H52 0.9500 . ? C53 N7 1.358(6) . ? C53 C55 1.484(7) . ? C54 N7 1.329(6) . ? C54 H54 0.9500 . ? C55 N8 1.338(6) . ? C55 C56 1.390(6) . ? C56 C57 1.386(8) . ? C56 H56 0.9500 . ? C57 C58 1.393(8) . ? C57 H57 0.9500 . ? C58 C59 1.392(7) . ? C58 C60 1.502(8) . ? C59 N8 1.351(6) . ? C59 H59 0.9500 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.489(9) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C63 1.388(9) . ? C62 C66 1.394(8) . ? C63 C64 1.363(9) . ? C63 H63 0.9500 . ? C64 C65 1.401(8) . ? C64 H64 0.9500 . ? C65 N9 1.356(7) . ? C65 C67 1.473(8) . ? C66 N9 1.328(7) . ? C66 H66 0.9500 . ? C67 N10 1.360(7) . ? C67 C68 1.395(8) . ? C68 C69 1.390(10) . ? C68 H68 0.9500 . ? C69 C70 1.390(10) . ? C69 H69 0.9500 . ? C70 C71 1.386(8) . ? C70 C72 1.499(10) . ? C71 N10 1.329(7) . ? C71 H71 0.9500 . ? C72 O5 1.415(7) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.384(9) . ? C73 O5 1.384(9) . ? C73 C78 1.386(10) . ? C74 C75 1.395(11) . ? C74 H74 0.9500 . ? C75 C76 1.368(11) . ? C75 H75 0.9500 . ? C76 O6 1.389(8) . ? C76 C77 1.405(9) . ? C77 C78 1.384(9) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 O6 1.407(11) . ? C79 C80 1.514(10) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 C81 1.388(10) . ? C80 C84 1.394(7) . ? C81 C82 1.374(10) . ? C81 H81 0.9500 . ? C82 C83 1.398(7) . ? C82 H82 0.9500 . ? C83 N11 1.344(6) . ? C83 C85 1.481(7) . ? C84 N11 1.357(6) . ? C84 H84 0.9500 . ? C85 N12 1.340(6) . ? C85 C86 1.385(7) . ? C86 C87 1.371(8) . ? C86 H86 0.9500 . ? C87 C88 1.393(7) . ? C87 H87 0.9500 . ? C88 C89 1.388(6) . ? C88 C90 1.489(7) . ? C89 N12 1.345(6) . ? C89 H89 0.9500 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? O3T C9T 1.333(9) . ? O3T C11T 1.373(9) . ? C9T C12T 1.477(10) . ? C9T H9T1 0.9900 . ? C9T H9T2 0.9900 . ? C10T C11T 1.483(10) . ? C10T C12T 1.491(10) . ? C10T H10A 0.9900 . ? C10T H10B 0.9900 . ? C11T H11A 0.9900 . ? C11T H11B 0.9900 . ? C12T H12C 0.9900 . ? C12T H12D 0.9900 . ? O1T C4T 1.27(2) . ? O1T C1T 1.47(2) . ? C1T C2T 1.36(2) . ? C1T H1T1 0.9900 . ? C1T H1T2 0.9900 . ? C2T C3T 1.65(2) . ? C2T H2T1 0.9900 . ? C2T H2T2 0.9900 . ? C3T C4T 1.50(2) . ? C3T H3T1 0.9900 . ? C3T H3T2 0.9900 . ? C4T H4T1 0.9900 . ? C4T H4T2 0.9900 . ? O2T C6T 1.32(4) . ? O2T C5T 1.75(4) . ? C5T C7T 1.473(10) . ? C5T H5T1 0.9900 . ? C5T H5T2 0.9900 . ? C6T C8T 1.23(4) . ? C6T H6T1 0.9900 . ? C6T H6T2 0.9900 . ? C7T C8T 1.477(10) . ? C7T H7T1 0.9900 . ? C7T H7T2 0.9900 . ? C8T H8T1 0.9900 . ? C8T H8T2 0.9900 . ? C7S C8S 1.26(2) . ? C7S N4S 1.28(2) . ? C8S H8S1 0.9800 . ? C8S H8S2 0.9800 . ? C8S H8S3 0.9800 . ? C1S N1S 1.043(17) . ? C1S C2S 1.487(19) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? C3S C4S 1.450(17) . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? C4S N2S 1.066(13) . ? C5S C6S 1.425(18) . ? C5S H5S1 0.9800 . ? C5S H5S2 0.9800 . ? C5S H5S3 0.9800 . ? C6S N3S 1.094(16) . ? N1 Ni1 2.068(4) . ? N2 Ni1 2.102(4) . ? N3 Ni2 2.094(4) . ? N4 Ni2 2.095(4) . ? N5 Ni1 2.104(4) . ? N6 Ni1 2.098(4) . ? N7 Ni2 2.087(4) . ? N8 Ni2 2.073(4) . ? N9 Ni1 2.089(4) . ? N10 Ni1 2.070(4) . ? N11 Ni2 2.063(4) . ? N12 Ni2 2.077(4) . ? F1 P1 1.609(5) . ? F2 P1 1.576(8) . ? F3 P1 1.535(5) . ? F4 P1 1.589(9) . ? F5 P1 1.635(4) . ? F6 P1 1.655(6) . ? F1A P1 1.57(4) . ? F2A P1 1.59(2) . ? F3A P1 1.560(17) . ? F4A P1 1.816(19) . ? F5A P1 1.39(2) . ? F6A P1 1.56(3) . ? F7 P2 1.668(6) . ? F8 P2 1.605(11) . ? F9 P2 1.596(7) . ? F10 P2 1.629(8) . ? F11 P2 1.603(9) . ? F12 P2 1.548(6) . ? F7A P2 1.58(3) . ? F8A P2 1.52(3) . ? F9A P2 1.49(2) . ? F10A P2 1.549(17) . ? F11A P2 1.62(2) . ? F12A P2 1.51(3) . ? P3 F16 1.564(5) . ? P3 F17 1.574(6) . ? P3 F18 1.585(6) . ? P3 F13 1.595(5) . ? P3 F14 1.596(5) . ? P3 F15 1.600(5) . ? P3A F18A 1.49(3) . ? P3A F14A 1.51(3) . ? P3A F16A 1.53(3) . ? P3A F13A 1.58(3) . ? P3A F17A 1.64(3) . ? P3A F15A 1.67(4) . ? P4 F21 1.570(6) . ? P4 F24 1.586(6) . ? P4 F20 1.595(7) . ? P4 F23 1.597(6) . ? P4 F19 1.606(7) . ? P4 F22 1.623(6) . ? P4A F19A 1.45(2) . ? P4A F24A 1.46(2) . ? P4A F22A 1.57(3) . ? P4A F21A 1.63(3) . ? P4A F20A 1.69(2) . ? P4A F23A 1.74(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C6 116.4(5) . . ? C3 C2 C1 122.8(5) . . ? C6 C2 C1 120.7(5) . . ? C2 C3 C4 120.8(5) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C3 C4 C5 119.1(5) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 120.9(5) . . ? N1 C5 C7 115.2(4) . . ? C4 C5 C7 123.8(4) . . ? N1 C6 C2 124.3(5) . . ? N1 C6 H6 117.9 . . ? C2 C6 H6 117.9 . . ? N2 C7 C8 119.5(5) . . ? N2 C7 C5 115.5(4) . . ? C8 C7 C5 124.9(4) . . ? C9 C8 C7 119.7(5) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 120.3(5) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C11 117.0(5) . . ? C9 C10 C12 123.0(5) . . ? C11 C10 C12 120.0(5) . . ? N2 C11 C10 123.4(5) . . ? N2 C11 H11 118.3 . . ? C10 C11 H11 118.3 . . ? O1 C12 C10 108.9(5) . . ? O1 C12 H12A 109.9 . . ? C10 C12 H12A 109.9 . . ? O1 C12 H12B 109.9 . . ? C10 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? C18 C13 O1 116.8(5) . . ? C18 C13 C14 119.4(5) . . ? O1 C13 C14 123.7(5) . . ? C15 C14 C13 118.8(5) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C14 C15 C16 122.0(5) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C17 C16 C15 118.9(5) . . ? C17 C16 O2 124.0(5) . . ? C15 C16 O2 117.0(5) . . ? C16 C17 C18 119.5(5) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C13 C18 C17 121.3(5) . . ? C13 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? O2 C19 C20 108.7(4) . . ? O2 C19 H19A 109.9 . . ? C20 C19 H19A 109.9 . . ? O2 C19 H19B 109.9 . . ? C20 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? C24 C20 C21 117.0(5) . . ? C24 C20 C19 120.9(5) . . ? C21 C20 C19 122.1(4) . . ? C22 C21 C20 120.2(5) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 119.2(5) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? N3 C23 C22 120.4(5) . . ? N3 C23 C25 115.4(4) . . ? C22 C23 C25 124.1(4) . . ? N3 C24 C20 123.2(5) . . ? N3 C24 H24 118.4 . . ? C20 C24 H24 118.4 . . ? N4 C25 C26 120.5(5) . . ? N4 C25 C23 116.0(4) . . ? C26 C25 C23 123.4(4) . . ? C27 C26 C25 119.7(5) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C28 119.8(5) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C29 C28 C27 116.9(5) . . ? C29 C28 C30 121.7(5) . . ? C27 C28 C30 121.4(5) . . ? N4 C29 C28 123.9(5) . . ? N4 C29 H29 118.0 . . ? C28 C29 H29 118.0 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C36 116.3(5) . . ? C33 C32 C31 123.8(5) . . ? C36 C32 C31 120.0(5) . . ? C34 C33 C32 120.7(5) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 119.3(5) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? N5 C35 C34 120.4(5) . . ? N5 C35 C37 115.8(4) . . ? C34 C35 C37 123.7(4) . . ? N5 C36 C32 123.9(5) . . ? N5 C36 H36 118.1 . . ? C32 C36 H36 118.1 . . ? N6 C37 C38 120.5(5) . . ? N6 C37 C35 115.5(4) . . ? C38 C37 C35 123.9(4) . . ? C39 C38 C37 119.3(5) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C38 C39 C40 120.9(5) . . ? C38 C39 H39 119.6 . . ? C40 C39 H39 119.6 . . ? C41 C40 C39 116.2(5) . . ? C41 C40 C42 121.6(5) . . ? C39 C40 C42 122.1(5) . . ? N6 C41 C40 124.0(5) . . ? N6 C41 H41 118.0 . . ? C40 C41 H41 118.0 . . ? O3 C42 C40 114.8(5) . . ? O3 C42 H42A 108.6 . . ? C40 C42 H42A 108.6 . . ? O3 C42 H42B 108.6 . . ? C40 C42 H42B 108.6 . . ? H42A C42 H42B 107.6 . . ? C48 C43 C44 119.4(5) . . ? C48 C43 O3 115.5(5) . . ? C44 C43 O3 125.2(5) . . ? C43 C44 C45 120.9(5) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C46 C45 C44 119.7(5) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C45 C46 O4 125.1(4) . . ? C45 C46 C47 119.9(5) . . ? O4 C46 C47 115.0(5) . . ? C48 C47 C46 119.8(5) . . ? C48 C47 H47 120.1 . . ? C46 C47 H47 120.1 . . ? C43 C48 C47 120.3(5) . . ? C43 C48 H48 119.9 . . ? C47 C48 H48 119.9 . . ? O4 C49 C50 108.1(4) . . ? O4 C49 H49A 110.1 . . ? C50 C49 H49A 110.1 . . ? O4 C49 H49B 110.1 . . ? C50 C49 H49B 110.1 . . ? H49A C49 H49B 108.4 . . ? C51 C50 C54 117.1(5) . . ? C51 C50 C49 122.6(5) . . ? C54 C50 C49 120.3(4) . . ? C50 C51 C52 119.7(5) . . ? C50 C51 H51 120.2 . . ? C52 C51 H51 120.2 . . ? C53 C52 C51 119.7(5) . . ? C53 C52 H52 120.2 . . ? C51 C52 H52 120.2 . . ? N7 C53 C52 120.8(4) . . ? N7 C53 C55 116.2(4) . . ? C52 C53 C55 123.0(4) . . ? N7 C54 C50 124.1(4) . . ? N7 C54 H54 118.0 . . ? C50 C54 H54 118.0 . . ? N8 C55 C56 121.2(5) . . ? N8 C55 C53 115.2(4) . . ? C56 C55 C53 123.5(5) . . ? C57 C56 C55 119.2(5) . . ? C57 C56 H56 120.4 . . ? C55 C56 H56 120.4 . . ? C56 C57 C58 120.3(5) . . ? C56 C57 H57 119.9 . . ? C58 C57 H57 119.9 . . ? C59 C58 C57 116.9(5) . . ? C59 C58 C60 119.8(5) . . ? C57 C58 C60 123.3(5) . . ? N8 C59 C58 123.0(5) . . ? N8 C59 H59 118.5 . . ? C58 C59 H59 118.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 H61A 109.5 . . ? C62 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C62 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C63 C62 C66 116.0(6) . . ? C63 C62 C61 123.0(5) . . ? C66 C62 C61 121.0(5) . . ? C64 C63 C62 120.9(6) . . ? C64 C63 H63 119.5 . . ? C62 C63 H63 119.5 . . ? C63 C64 C65 119.4(6) . . ? C63 C64 H64 120.3 . . ? C65 C64 H64 120.3 . . ? N9 C65 C64 120.5(5) . . ? N9 C65 C67 115.4(5) . . ? C64 C65 C67 124.0(5) . . ? N9 C66 C62 124.5(5) . . ? N9 C66 H66 117.8 . . ? C62 C66 H66 117.8 . . ? N10 C67 C68 120.7(6) . . ? N10 C67 C65 115.5(5) . . ? C68 C67 C65 123.8(5) . . ? C69 C68 C67 119.3(6) . . ? C69 C68 H68 120.4 . . ? C67 C68 H68 120.4 . . ? C70 C69 C68 119.8(6) . . ? C70 C69 H69 120.1 . . ? C68 C69 H69 120.1 . . ? C71 C70 C69 117.1(6) . . ? C71 C70 C72 119.0(6) . . ? C69 C70 C72 123.9(6) . . ? N10 C71 C70 124.2(6) . . ? N10 C71 H71 117.9 . . ? C70 C71 H71 117.9 . . ? O5 C72 C70 107.8(6) . . ? O5 C72 H72A 110.1 . . ? C70 C72 H72A 110.1 . . ? O5 C72 H72B 110.1 . . ? C70 C72 H72B 110.1 . . ? H72A C72 H72B 108.5 . . ? C74 C73 O5 114.5(7) . . ? C74 C73 C78 121.0(7) . . ? O5 C73 C78 124.5(6) . . ? C73 C74 C75 119.1(8) . . ? C73 C74 H74 120.4 . . ? C75 C74 H74 120.4 . . ? C76 C75 C74 119.7(6) . . ? C76 C75 H75 120.1 . . ? C74 C75 H75 120.1 . . ? C75 C76 O6 115.3(6) . . ? C75 C76 C77 121.4(7) . . ? O6 C76 C77 123.3(8) . . ? C78 C77 C76 118.4(8) . . ? C78 C77 H77 120.8 . . ? C76 C77 H77 120.8 . . ? C77 C78 C73 120.1(6) . . ? C77 C78 H78 120.0 . . ? C73 C78 H78 120.0 . . ? O6 C79 C80 115.2(6) . . ? O6 C79 H79A 108.5 . . ? C80 C79 H79A 108.5 . . ? O6 C79 H79B 108.5 . . ? C80 C79 H79B 108.5 . . ? H79A C79 H79B 107.5 . . ? C81 C80 C84 117.9(6) . . ? C81 C80 C79 121.5(6) . . ? C84 C80 C79 120.4(7) . . ? C82 C81 C80 120.6(5) . . ? C82 C81 H81 119.7 . . ? C80 C81 H81 119.7 . . ? C81 C82 C83 119.0(6) . . ? C81 C82 H82 120.5 . . ? C83 C82 H82 120.5 . . ? N11 C83 C82 120.7(5) . . ? N11 C83 C85 115.5(4) . . ? C82 C83 C85 123.7(5) . . ? N11 C84 C80 121.4(6) . . ? N11 C84 H84 119.3 . . ? C80 C84 H84 119.3 . . ? N12 C85 C86 120.8(5) . . ? N12 C85 C83 115.7(4) . . ? C86 C85 C83 123.4(4) . . ? C87 C86 C85 119.8(5) . . ? C87 C86 H86 120.1 . . ? C85 C86 H86 120.1 . . ? C86 C87 C88 120.7(5) . . ? C86 C87 H87 119.7 . . ? C88 C87 H87 119.7 . . ? C89 C88 C87 115.8(5) . . ? C89 C88 C90 121.2(4) . . ? C87 C88 C90 123.0(5) . . ? N12 C89 C88 124.2(4) . . ? N12 C89 H89 117.9 . . ? C88 C89 H89 117.9 . . ? C88 C90 H90A 109.5 . . ? C88 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C88 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C9T O3T C11T 113.9(14) . . ? O3T C9T C12T 106.3(13) . . ? O3T C9T H9T1 110.5 . . ? C12T C9T H9T1 110.5 . . ? O3T C9T H9T2 110.5 . . ? C12T C9T H9T2 110.5 . . ? H9T1 C9T H9T2 108.7 . . ? C11T C10T C12T 103.8(14) . . ? C11T C10T H10A 111.0 . . ? C12T C10T H10A 111.0 . . ? C11T C10T H10B 111.0 . . ? C12T C10T H10B 111.0 . . ? H10A C10T H10B 109.0 . . ? O3T C11T C10T 105.4(14) . . ? O3T C11T H11A 110.7 . . ? C10T C11T H11A 110.7 . . ? O3T C11T H11B 110.7 . . ? C10T C11T H11B 110.7 . . ? H11A C11T H11B 108.8 . . ? C9T C12T C10T 102.5(13) . . ? C9T C12T H12C 111.3 . . ? C10T C12T H12C 111.3 . . ? C9T C12T H12D 111.3 . . ? C10T C12T H12D 111.3 . . ? H12C C12T H12D 109.2 . . ? C4T O1T C1T 108.7(13) . . ? C2T C1T O1T 108.2(14) . . ? C2T C1T H1T1 110.1 . . ? O1T C1T H1T1 110.1 . . ? C2T C1T H1T2 110.1 . . ? O1T C1T H1T2 110.1 . . ? H1T1 C1T H1T2 108.4 . . ? C1T C2T C3T 103.3(14) . . ? C1T C2T H2T1 111.1 . . ? C3T C2T H2T1 111.1 . . ? C1T C2T H2T2 111.1 . . ? C3T C2T H2T2 111.1 . . ? H2T1 C2T H2T2 109.1 . . ? C4T C3T C2T 95.5(13) . . ? C4T C3T H3T1 112.6 . . ? C2T C3T H3T1 112.6 . . ? C4T C3T H3T2 112.6 . . ? C2T C3T H3T2 112.6 . . ? H3T1 C3T H3T2 110.1 . . ? O1T C4T C3T 114.5(16) . . ? O1T C4T H4T1 108.6 . . ? C3T C4T H4T1 108.6 . . ? O1T C4T H4T2 108.6 . . ? C3T C4T H4T2 108.6 . . ? H4T1 C4T H4T2 107.6 . . ? C6T O2T C5T 100(2) . . ? C7T C5T O2T 96(2) . . ? C7T C5T H5T1 112.6 . . ? O2T C5T H5T1 112.6 . . ? C7T C5T H5T2 112.6 . . ? O2T C5T H5T2 112.6 . . ? H5T1 C5T H5T2 110.1 . . ? C8T C6T O2T 112(3) . . ? C8T C6T H6T1 109.1 . . ? O2T C6T H6T1 109.1 . . ? C8T C6T H6T2 109.1 . . ? O2T C6T H6T2 109.1 . . ? H6T1 C6T H6T2 107.9 . . ? C5T C7T C8T 106(2) . . ? C5T C7T H7T1 110.6 . . ? C8T C7T H7T1 110.6 . . ? C5T C7T H7T2 110.6 . . ? C8T C7T H7T2 110.6 . . ? H7T1 C7T H7T2 108.7 . . ? C6T C8T C7T 113(3) . . ? C6T C8T H8T1 109.0 . . ? C7T C8T H8T1 109.0 . . ? C6T C8T H8T2 109.0 . . ? C7T C8T H8T2 109.0 . . ? H8T1 C8T H8T2 107.8 . . ? C8S C7S N4S 175.9(19) . . ? C7S C8S H8S1 109.5 . . ? C7S C8S H8S2 109.5 . . ? H8S1 C8S H8S2 109.5 . . ? C7S C8S H8S3 109.5 . . ? H8S1 C8S H8S3 109.5 . . ? H8S2 C8S H8S3 109.5 . . ? N1S C1S C2S 175.4(16) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C4S C3S H3S1 109.5 . . ? C4S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? C4S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? N2S C4S C3S 173.1(13) . . ? C6S C5S H5S1 109.5 . . ? C6S C5S H5S2 109.5 . . ? H5S1 C5S H5S2 109.5 . . ? C6S C5S H5S3 109.5 . . ? H5S1 C5S H5S3 109.5 . . ? H5S2 C5S H5S3 109.5 . . ? N3S C6S C5S 171.4(14) . . ? C6 N1 C5 118.4(4) . . ? C6 N1 Ni1 125.3(3) . . ? C5 N1 Ni1 116.1(3) . . ? C11 N2 C7 120.0(4) . . ? C11 N2 Ni1 125.2(3) . . ? C7 N2 Ni1 114.7(3) . . ? C24 N3 C23 119.6(4) . . ? C24 N3 Ni2 126.1(3) . . ? C23 N3 Ni2 113.9(3) . . ? C29 N4 C25 119.1(4) . . ? C29 N4 Ni2 126.8(3) . . ? C25 N4 Ni2 114.0(3) . . ? C36 N5 C35 119.4(4) . . ? C36 N5 Ni1 125.4(3) . . ? C35 N5 Ni1 114.3(3) . . ? C41 N6 C37 119.2(4) . . ? C41 N6 Ni1 126.0(3) . . ? C37 N6 Ni1 114.6(3) . . ? C54 N7 C53 118.6(4) . . ? C54 N7 Ni2 127.5(3) . . ? C53 N7 Ni2 113.7(3) . . ? C55 N8 C59 119.4(4) . . ? C55 N8 Ni2 115.4(3) . . ? C59 N8 Ni2 125.1(3) . . ? C66 N9 C65 118.5(5) . . ? C66 N9 Ni1 126.7(3) . . ? C65 N9 Ni1 114.7(4) . . ? C71 N10 C67 118.8(5) . . ? C71 N10 Ni1 125.2(4) . . ? C67 N10 Ni1 115.0(4) . . ? C83 N11 C84 120.1(4) . . ? C83 N11 Ni2 115.0(3) . . ? C84 N11 Ni2 124.7(4) . . ? C85 N12 C89 118.7(4) . . ? C85 N12 Ni2 114.5(3) . . ? C89 N12 Ni2 126.7(3) . . ? C13 O1 C12 120.0(4) . . ? C16 O2 C19 118.0(4) . . ? C43 O3 C42 117.6(4) . . ? C46 O4 C49 116.9(4) . . ? C73 O5 C72 115.7(6) . . ? C76 O6 C79 118.3(6) . . ? F5A P1 F3 154.2(9) . . ? F5A P1 F3A 102.4(11) . . ? F3 P1 F3A 57.9(7) . . ? F5A P1 F6A 101.5(17) . . ? F3 P1 F6A 101.8(14) . . ? F3A P1 F6A 153.4(17) . . ? F5A P1 F1A 100.1(18) . . ? F3 P1 F1A 92.1(17) . . ? F3A P1 F1A 78.0(17) . . ? F6A P1 F1A 87(2) . . ? F5A P1 F2 105.7(10) . . ? F3 P1 F2 96.6(5) . . ? F3A P1 F2 151.2(9) . . ? F1A P1 F2 91.0(16) . . ? F5A P1 F2A 106.2(11) . . ? F3 P1 F2A 62.1(7) . . ? F3A P1 F2A 92.4(10) . . ? F6A P1 F2A 92.0(14) . . ? F1A P1 F2A 153.4(17) . . ? F2 P1 F2A 85.7(8) . . ? F5A P1 F4 97.2(11) . . ? F3 P1 F4 94.7(7) . . ? F3A P1 F4 78.1(9) . . ? F6A P1 F4 87.6(15) . . ? F2 P1 F4 92.3(7) . . ? F2A P1 F4 156.2(9) . . ? F5A P1 F1 77.5(9) . . ? F3 P1 F1 90.1(3) . . ? F3A P1 F1 102.4(7) . . ? F6A P1 F1 93.9(14) . . ? F1A P1 F1 177.6(16) . . ? F2 P1 F1 89.7(5) . . ? F4 P1 F1 174.6(6) . . ? F5A P1 F5 67.5(9) . . ? F3 P1 F5 89.7(3) . . ? F6A P1 F5 168.5(14) . . ? F1A P1 F5 92.0(15) . . ? F2 P1 F5 173.0(6) . . ? F2A P1 F5 94.4(7) . . ? F4 P1 F5 90.4(5) . . ? F1 P1 F5 87.1(3) . . ? F3 P1 F6 175.9(3) . . ? F3A P1 F6 118.6(8) . . ? F6A P1 F6 82.2(14) . . ? F1A P1 F6 89.0(17) . . ? F2 P1 F6 87.4(5) . . ? F2A P1 F6 117.1(8) . . ? F4 P1 F6 86.4(7) . . ? F1 P1 F6 88.7(4) . . ? F5 P1 F6 86.4(3) . . ? F5A P1 F4A 175.5(10) . . ? F3A P1 F4A 80.3(9) . . ? F6A P1 F4A 75.1(16) . . ? F1A P1 F4A 76.8(16) . . ? F2 P1 F4A 71.2(8) . . ? F2A P1 F4A 77.1(9) . . ? F4 P1 F4A 79.8(8) . . ? F1 P1 F4A 105.5(6) . . ? F5 P1 F4A 115.6(6) . . ? F6 P1 F4A 153.8(6) . . ? F9A P2 F12A 97.8(11) . . ? F9A P2 F8A 78.7(13) . . ? F12A P2 F8A 102.9(13) . . ? F9A P2 F12 156.1(7) . . ? F12A P2 F12 106.0(9) . . ? F8A P2 F12 97.6(11) . . ? F9A P2 F10A 91.0(9) . . ? F12A P2 F10A 170.8(10) . . ? F8A P2 F10A 76.2(9) . . ? F12 P2 F10A 65.3(7) . . ? F9A P2 F7A 91.1(14) . . ? F12A P2 F7A 81.3(13) . . ? F8A P2 F7A 169.3(15) . . ? F12 P2 F7A 90.5(11) . . ? F10A P2 F7A 101.2(12) . . ? F9A P2 F9 63.5(7) . . ? F12A P2 F9 158.4(9) . . ? F8A P2 F9 84.6(10) . . ? F12 P2 F9 92.7(4) . . ? F7A P2 F9 88.1(11) . . ? F9A P2 F11 110.4(7) . . ? F8A P2 F11 93.1(9) . . ? F12 P2 F11 93.3(4) . . ? F10A P2 F11 153.9(7) . . ? F7A P2 F11 93.3(11) . . ? F9 P2 F11 173.8(4) . . ? F9A P2 F8 93.1(9) . . ? F12A P2 F8 82.2(11) . . ? F8A P2 F8 170.7(11) . . ? F12 P2 F8 88.2(5) . . ? F10A P2 F8 100.0(9) . . ? F9 P2 F8 87.9(7) . . ? F11 P2 F8 93.7(7) . . ? F9A P2 F11A 179.3(10) . . ? F12A P2 F11A 81.6(10) . . ? F8A P2 F11A 101.1(13) . . ? F10A P2 F11A 89.6(9) . . ? F7A P2 F11A 89.2(14) . . ? F9 P2 F11A 117.2(7) . . ? F11 P2 F11A 68.9(7) . . ? F8 P2 F11A 87.2(9) . . ? F9A P2 F10 89.8(8) . . ? F12A P2 F10 93.0(9) . . ? F12 P2 F10 91.0(4) . . ? F10A P2 F10 84.4(8) . . ? F7A P2 F10 174.3(11) . . ? F9 P2 F10 97.4(5) . . ? F11 P2 F10 81.1(5) . . ? F8 P2 F10 174.7(7) . . ? F11A P2 F10 89.8(8) . . ? F12A P2 F7 74.3(9) . . ? F8A P2 F7 84.2(11) . . ? F12 P2 F7 178.0(4) . . ? F10A P2 F7 114.5(7) . . ? F7A P2 F7 87.6(11) . . ? F9 P2 F7 86.6(4) . . ? F11 P2 F7 87.4(4) . . ? F8 P2 F7 89.9(5) . . ? F11A P2 F7 155.9(7) . . ? F10 P2 F7 91.0(4) . . ? F16 P3 F17 92.0(4) . . ? F16 P3 F18 90.2(4) . . ? F17 P3 F18 92.6(4) . . ? F16 P3 F13 178.2(4) . . ? F17 P3 F13 89.6(3) . . ? F18 P3 F13 90.7(4) . . ? F16 P3 F14 90.1(3) . . ? F17 P3 F14 176.6(4) . . ? F18 P3 F14 90.0(3) . . ? F13 P3 F14 88.3(3) . . ? F16 P3 F15 91.8(3) . . ? F17 P3 F15 88.1(4) . . ? F18 P3 F15 177.9(4) . . ? F13 P3 F15 87.3(3) . . ? F14 P3 F15 89.2(3) . . ? F18A P3A F14A 173(2) . . ? F18A P3A F16A 93.2(18) . . ? F14A P3A F16A 91.2(16) . . ? F18A P3A F13A 90.4(17) . . ? F14A P3A F13A 95.2(16) . . ? F16A P3A F13A 93.0(16) . . ? F18A P3A F17A 91.2(17) . . ? F14A P3A F17A 84.1(17) . . ? F16A P3A F17A 174.8(19) . . ? F13A P3A F17A 89.7(15) . . ? F18A P3A F15A 89.6(17) . . ? F14A P3A F15A 84.3(18) . . ? F16A P3A F15A 93.3(16) . . ? F13A P3A F15A 173.7(19) . . ? F17A P3A F15A 83.9(18) . . ? F21 P4 F24 177.4(5) . . ? F21 P4 F20 89.3(3) . . ? F24 P4 F20 89.0(4) . . ? F21 P4 F23 88.4(5) . . ? F24 P4 F23 93.3(6) . . ? F20 P4 F23 177.7(5) . . ? F21 P4 F19 87.2(4) . . ? F24 P4 F19 90.8(4) . . ? F20 P4 F19 89.0(4) . . ? F23 P4 F19 90.7(5) . . ? F21 P4 F22 90.2(4) . . ? F24 P4 F22 91.5(4) . . ? F20 P4 F22 82.9(4) . . ? F23 P4 F22 97.2(6) . . ? F19 P4 F22 171.6(5) . . ? F19A P4A F24A 85.9(14) . . ? F19A P4A F22A 170.0(16) . . ? F24A P4A F22A 84.5(14) . . ? F19A P4A F21A 92.4(13) . . ? F24A P4A F21A 96.2(14) . . ? F22A P4A F21A 91.5(14) . . ? F19A P4A F20A 91.0(13) . . ? F24A P4A F20A 174.7(14) . . ? F22A P4A F20A 98.7(14) . . ? F21A P4A F20A 79.5(14) . . ? F19A P4A F23A 89.2(15) . . ? F24A P4A F23A 87.0(15) . . ? F22A P4A F23A 87.4(15) . . ? F21A P4A F23A 176.5(17) . . ? F20A P4A F23A 97.3(14) . . ? N1 Ni1 N10 168.37(15) . . ? N1 Ni1 N9 96.49(16) . . ? N10 Ni1 N9 78.91(18) . . ? N1 Ni1 N6 89.66(15) . . ? N10 Ni1 N6 96.19(17) . . ? N9 Ni1 N6 171.16(15) . . ? N1 Ni1 N2 78.27(15) . . ? N10 Ni1 N2 91.14(16) . . ? N9 Ni1 N2 91.99(15) . . ? N6 Ni1 N2 95.48(15) . . ? N1 Ni1 N5 100.34(15) . . ? N10 Ni1 N5 90.68(16) . . ? N9 Ni1 N5 94.04(15) . . ? N6 Ni1 N5 78.56(15) . . ? N2 Ni1 N5 173.93(15) . . ? N11 Ni2 N8 171.13(15) . . ? N11 Ni2 N12 79.25(15) . . ? N8 Ni2 N12 93.11(14) . . ? N11 Ni2 N7 96.42(14) . . ? N8 Ni2 N7 79.32(15) . . ? N12 Ni2 N7 92.86(15) . . ? N11 Ni2 N3 97.76(15) . . ? N8 Ni2 N3 90.27(14) . . ? N12 Ni2 N3 173.88(15) . . ? N7 Ni2 N3 92.78(15) . . ? N11 Ni2 N4 91.03(15) . . ? N8 Ni2 N4 94.26(15) . . ? N12 Ni2 N4 95.81(15) . . ? N7 Ni2 N4 169.49(15) . . ? N3 Ni2 N4 78.83(15) . . ? 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 C6 C2 C3 C4 -0.3(7) . . . . ? C1 C2 C3 C4 -178.7(5) . . . . ? C2 C3 C4 C5 1.7(7) . . . . ? C3 C4 C5 N1 -2.2(7) . . . . ? C3 C4 C5 C7 174.8(4) . . . . ? C3 C2 C6 N1 -0.8(7) . . . . ? C1 C2 C6 N1 177.7(5) . . . . ? N1 C5 C7 N2 4.7(6) . . . . ? C4 C5 C7 N2 -172.5(4) . . . . ? N1 C5 C7 C8 -179.1(4) . . . . ? C4 C5 C7 C8 3.7(7) . . . . ? N2 C7 C8 C9 0.7(7) . . . . ? C5 C7 C8 C9 -175.3(4) . . . . ? C7 C8 C9 C10 0.7(8) . . . . ? C8 C9 C10 C11 -2.2(7) . . . . ? C8 C9 C10 C12 178.0(5) . . . . ? C9 C10 C11 N2 2.7(8) . . . . ? C12 C10 C11 N2 -177.6(5) . . . . ? C9 C10 C12 O1 168.8(5) . . . . ? C11 C10 C12 O1 -11.0(8) . . . . ? C18 C13 C14 C15 0.8(9) . . . . ? O1 C13 C14 C15 -174.9(5) . . . . ? C13 C14 C15 C16 0.9(9) . . . . ? C14 C15 C16 C17 -1.2(9) . . . . ? C14 C15 C16 O2 -179.8(5) . . . . ? C15 C16 C17 C18 -0.3(8) . . . . ? O2 C16 C17 C18 178.2(5) . . . . ? O1 C13 C18 C17 173.8(5) . . . . ? C14 C13 C18 C17 -2.2(9) . . . . ? C16 C17 C18 C13 2.0(9) . . . . ? O2 C19 C20 C24 -15.9(6) . . . . ? O2 C19 C20 C21 164.2(4) . . . . ? C24 C20 C21 C22 -5.1(7) . . . . ? C19 C20 C21 C22 174.8(4) . . . . ? C20 C21 C22 C23 1.4(7) . . . . ? C21 C22 C23 N3 3.4(7) . . . . ? C21 C22 C23 C25 -173.2(4) . . . . ? C21 C20 C24 N3 4.4(7) . . . . ? C19 C20 C24 N3 -175.5(4) . . . . ? N3 C23 C25 N4 8.7(6) . . . . ? C22 C23 C25 N4 -174.6(4) . . . . ? N3 C23 C25 C26 -168.7(4) . . . . ? C22 C23 C25 C26 8.0(7) . . . . ? N4 C25 C26 C27 -1.2(7) . . . . ? C23 C25 C26 C27 176.1(5) . . . . ? C25 C26 C27 C28 0.5(8) . . . . ? C26 C27 C28 C29 0.3(9) . . . . ? C26 C27 C28 C30 180.0(6) . . . . ? C27 C28 C29 N4 -0.4(8) . . . . ? C30 C28 C29 N4 179.9(6) . . . . ? C36 C32 C33 C34 -1.6(8) . . . . ? C31 C32 C33 C34 179.3(6) . . . . ? C32 C33 C34 C35 0.6(9) . . . . ? C33 C34 C35 N5 0.9(8) . . . . ? C33 C34 C35 C37 -178.2(5) . . . . ? C33 C32 C36 N5 1.3(8) . . . . ? C31 C32 C36 N5 -179.6(5) . . . . ? N5 C35 C37 N6 8.9(6) . . . . ? C34 C35 C37 N6 -171.9(5) . . . . ? N5 C35 C37 C38 -168.2(5) . . . . ? C34 C35 C37 C38 11.0(8) . . . . ? N6 C37 C38 C39 -1.9(8) . . . . ? C35 C37 C38 C39 175.0(5) . . . . ? C37 C38 C39 C40 0.4(9) . . . . ? C38 C39 C40 C41 1.6(8) . . . . ? C38 C39 C40 C42 -173.6(5) . . . . ? C39 C40 C41 N6 -2.3(8) . . . . ? C42 C40 C41 N6 172.9(5) . . . . ? C41 C40 C42 O3 23.5(7) . . . . ? C39 C40 C42 O3 -161.6(5) . . . . ? C48 C43 C44 C45 -2.0(9) . . . . ? O3 C43 C44 C45 178.3(5) . . . . ? C43 C44 C45 C46 0.1(9) . . . . ? C44 C45 C46 O4 -178.6(5) . . . . ? C44 C45 C46 C47 1.8(8) . . . . ? C45 C46 C47 C48 -1.8(8) . . . . ? O4 C46 C47 C48 178.5(5) . . . . ? C44 C43 C48 C47 1.9(8) . . . . ? O3 C43 C48 C47 -178.4(5) . . . . ? C46 C47 C48 C43 0.0(8) . . . . ? O4 C49 C50 C51 -17.4(7) . . . . ? O4 C49 C50 C54 163.8(4) . . . . ? C54 C50 C51 C52 -1.2(7) . . . . ? C49 C50 C51 C52 180.0(5) . . . . ? C50 C51 C52 C53 -1.7(8) . . . . ? C51 C52 C53 N7 3.3(7) . . . . ? C51 C52 C53 C55 -174.8(4) . . . . ? C51 C50 C54 N7 2.9(7) . . . . ? C49 C50 C54 N7 -178.3(4) . . . . ? N7 C53 C55 N8 -4.3(6) . . . . ? C52 C53 C55 N8 173.9(4) . . . . ? N7 C53 C55 C56 176.1(4) . . . . ? C52 C53 C55 C56 -5.7(7) . . . . ? N8 C55 C56 C57 1.2(7) . . . . ? C53 C55 C56 C57 -179.2(4) . . . . ? C55 C56 C57 C58 -1.7(7) . . . . ? C56 C57 C58 C59 0.7(7) . . . . ? C56 C57 C58 C60 -176.6(5) . . . . ? C57 C58 C59 N8 0.8(7) . . . . ? C60 C58 C59 N8 178.2(4) . . . . ? C66 C62 C63 C64 0.6(8) . . . . ? C61 C62 C63 C64 179.3(5) . . . . ? C62 C63 C64 C65 -1.1(8) . . . . ? C63 C64 C65 N9 1.4(7) . . . . ? C63 C64 C65 C67 179.1(5) . . . . ? C63 C62 C66 N9 -0.4(7) . . . . ? C61 C62 C66 N9 -179.1(5) . . . . ? N9 C65 C67 N10 -6.8(6) . . . . ? C64 C65 C67 N10 175.4(4) . . . . ? N9 C65 C67 C68 171.5(5) . . . . ? C64 C65 C67 C68 -6.3(8) . . . . ? N10 C67 C68 C69 3.9(8) . . . . ? C65 C67 C68 C69 -174.3(5) . . . . ? C67 C68 C69 C70 -2.6(9) . . . . ? C68 C69 C70 C71 -1.3(9) . . . . ? C68 C69 C70 C72 178.7(6) . . . . ? C69 C70 C71 N10 4.3(9) . . . . ? C72 C70 C71 N10 -175.7(5) . . . . ? C71 C70 C72 O5 -176.6(5) . . . . ? C69 C70 C72 O5 3.4(9) . . . . ? O5 C73 C74 C75 175.4(6) . . . . ? C78 C73 C74 C75 -3.4(11) . . . . ? C73 C74 C75 C76 -1.4(10) . . . . ? C74 C75 C76 O6 -175.0(6) . . . . ? C74 C75 C76 C77 5.4(10) . . . . ? C75 C76 C77 C78 -4.5(9) . . . . ? O6 C76 C77 C78 175.9(5) . . . . ? C76 C77 C78 C73 -0.4(9) . . . . ? C74 C73 C78 C77 4.3(10) . . . . ? O5 C73 C78 C77 -174.4(6) . . . . ? O6 C79 C80 C81 -179.1(5) . . . . ? O6 C79 C80 C84 6.3(8) . . . . ? C84 C80 C81 C82 2.3(9) . . . . ? C79 C80 C81 C82 -172.4(6) . . . . ? C80 C81 C82 C83 0.3(9) . . . . ? C81 C82 C83 N11 -3.9(8) . . . . ? C81 C82 C83 C85 173.7(5) . . . . ? C81 C80 C84 N11 -1.6(8) . . . . ? C79 C80 C84 N11 173.1(5) . . . . ? N11 C83 C85 N12 -0.3(6) . . . . ? C82 C83 C85 N12 -178.0(5) . . . . ? N11 C83 C85 C86 176.3(4) . . . . ? C82 C83 C85 C86 -1.4(8) . . . . ? N12 C85 C86 C87 0.0(8) . . . . ? C83 C85 C86 C87 -176.5(5) . . . . ? C85 C86 C87 C88 0.7(9) . . . . ? C86 C87 C88 C89 -1.0(8) . . . . ? C86 C87 C88 C90 179.0(5) . . . . ? C87 C88 C89 N12 0.9(7) . . . . ? C90 C88 C89 N12 -179.1(5) . . . . ? C11T O3T C9T C12T 16(2) . . . . ? C9T O3T C11T C10T 2(2) . . . . ? C12T C10T C11T O3T -18.6(19) . . . . ? O3T C9T C12T C10T -27(2) . . . . ? C11T C10T C12T C9T 27.2(19) . . . . ? C4T O1T C1T C2T -19(2) . . . . ? O1T C1T C2T C3T 29.8(18) . . . . ? C1T C2T C3T C4T -29.1(18) . . . . ? C1T O1T C4T C3T -4(2) . . . . ? C2T C3T C4T O1T 20(2) . . . . ? C6T O2T C5T C7T 31(3) . . . . ? C5T O2T C6T C8T -37(3) . . . . ? O2T C5T C7T C8T -16(3) . . . . ? O2T C6T C8T C7T 29(4) . . . . ? C5T C7T C8T C6T -3(4) . . . . ? C2 C6 N1 C5 0.3(7) . . . . ? C2 C6 N1 Ni1 -173.6(4) . . . . ? C4 C5 N1 C6 1.2(6) . . . . ? C7 C5 N1 C6 -176.1(4) . . . . ? C4 C5 N1 Ni1 175.7(3) . . . . ? C7 C5 N1 Ni1 -1.6(5) . . . . ? C10 C11 N2 C7 -1.3(7) . . . . ? C10 C11 N2 Ni1 -179.7(4) . . . . ? C8 C7 N2 C11 -0.4(6) . . . . ? C5 C7 N2 C11 176.0(4) . . . . ? C8 C7 N2 Ni1 178.1(3) . . . . ? C5 C7 N2 Ni1 -5.5(5) . . . . ? C20 C24 N3 C23 0.3(7) . . . . ? C20 C24 N3 Ni2 -171.3(3) . . . . ? C22 C23 N3 C24 -4.2(6) . . . . ? C25 C23 N3 C24 172.6(4) . . . . ? C22 C23 N3 Ni2 168.3(3) . . . . ? C25 C23 N3 Ni2 -14.8(5) . . . . ? C28 C29 N4 C25 -0.3(7) . . . . ? C28 C29 N4 Ni2 -178.4(4) . . . . ? C26 C25 N4 C29 1.0(7) . . . . ? C23 C25 N4 C29 -176.4(4) . . . . ? C26 C25 N4 Ni2 179.4(3) . . . . ? C23 C25 N4 Ni2 1.9(5) . . . . ? C32 C36 N5 C35 0.1(8) . . . . ? C32 C36 N5 Ni1 -168.3(4) . . . . ? C34 C35 N5 C36 -1.3(7) . . . . ? C37 C35 N5 C36 178.0(4) . . . . ? C34 C35 N5 Ni1 168.4(4) . . . . ? C37 C35 N5 Ni1 -12.4(5) . . . . ? C40 C41 N6 C37 0.9(7) . . . . ? C40 C41 N6 Ni1 -173.5(4) . . . . ? C38 C37 N6 C41 1.3(7) . . . . ? C35 C37 N6 C41 -175.9(4) . . . . ? C38 C37 N6 Ni1 176.3(4) . . . . ? C35 C37 N6 Ni1 -0.9(5) . . . . ? C50 C54 N7 C53 -1.4(7) . . . . ? C50 C54 N7 Ni2 173.2(3) . . . . ? C52 C53 N7 C54 -1.7(7) . . . . ? C55 C53 N7 C54 176.5(4) . . . . ? C52 C53 N7 Ni2 -177.1(4) . . . . ? C55 C53 N7 Ni2 1.1(5) . . . . ? C56 C55 N8 C59 0.3(6) . . . . ? C53 C55 N8 C59 -179.3(4) . . . . ? C56 C55 N8 Ni2 -175.1(3) . . . . ? C53 C55 N8 Ni2 5.2(5) . . . . ? C58 C59 N8 C55 -1.3(7) . . . . ? C58 C59 N8 Ni2 173.6(3) . . . . ? C62 C66 N9 C65 0.8(7) . . . . ? C62 C66 N9 Ni1 179.4(4) . . . . ? C64 C65 N9 C66 -1.2(7) . . . . ? C67 C65 N9 C66 -179.2(4) . . . . ? C64 C65 N9 Ni1 180.0(4) . . . . ? C67 C65 N9 Ni1 2.1(5) . . . . ? C70 C71 N10 C67 -3.1(8) . . . . ? C70 C71 N10 Ni1 164.8(4) . . . . ? C68 C67 N10 C71 -1.1(7) . . . . ? C65 C67 N10 C71 177.2(4) . . . . ? C68 C67 N10 Ni1 -170.2(4) . . . . ? C65 C67 N10 Ni1 8.2(5) . . . . ? C82 C83 N11 C84 4.6(7) . . . . ? C85 C83 N11 C84 -173.1(4) . . . . ? C82 C83 N11 Ni2 179.7(4) . . . . ? C85 C83 N11 Ni2 2.0(5) . . . . ? C80 C84 N11 C83 -1.9(7) . . . . ? C80 C84 N11 Ni2 -176.5(4) . . . . ? C86 C85 N12 C89 -0.2(7) . . . . ? C83 C85 N12 C89 176.6(4) . . . . ? C86 C85 N12 Ni2 -178.2(4) . . . . ? C83 C85 N12 Ni2 -1.4(5) . . . . ? C88 C89 N12 C85 -0.3(7) . . . . ? C88 C89 N12 Ni2 177.4(4) . . . . ? C18 C13 O1 C12 140.1(6) . . . . ? C14 C13 O1 C12 -44.1(8) . . . . ? C10 C12 O1 C13 149.2(5) . . . . ? C17 C16 O2 C19 7.4(8) . . . . ? C15 C16 O2 C19 -174.1(5) . . . . ? C20 C19 O2 C16 170.4(4) . . . . ? C48 C43 O3 C42 169.9(5) . . . . ? C44 C43 O3 C42 -10.4(8) . . . . ? C40 C42 O3 C43 86.1(6) . . . . ? C45 C46 O4 C49 5.9(7) . . . . ? C47 C46 O4 C49 -174.5(5) . . . . ? C50 C49 O4 C46 -177.9(4) . . . . ? C74 C73 O5 C72 -167.8(6) . . . . ? C78 C73 O5 C72 11.0(10) . . . . ? C70 C72 O5 C73 163.3(6) . . . . ? C75 C76 O6 C79 173.6(5) . . . . ? C77 C76 O6 C79 -6.7(8) . . . . ? C80 C79 O6 C76 84.4(7) . . . . ? C6 N1 Ni1 N10 -162.1(8) . . . . ? C5 N1 Ni1 N10 23.8(10) . . . . ? C6 N1 Ni1 N9 -96.2(4) . . . . ? C5 N1 Ni1 N9 89.7(3) . . . . ? C6 N1 Ni1 N6 77.5(4) . . . . ? C5 N1 Ni1 N6 -96.7(3) . . . . ? C6 N1 Ni1 N2 173.1(4) . . . . ? C5 N1 Ni1 N2 -1.0(3) . . . . ? C6 N1 Ni1 N5 -0.9(4) . . . . ? C5 N1 Ni1 N5 -175.0(3) . . . . ? C71 N10 Ni1 N1 -106.1(9) . . . . ? C67 N10 Ni1 N1 62.2(10) . . . . ? C71 N10 Ni1 N9 -173.7(4) . . . . ? C67 N10 Ni1 N9 -5.4(3) . . . . ? C71 N10 Ni1 N6 13.8(4) . . . . ? C67 N10 Ni1 N6 -178.0(3) . . . . ? C71 N10 Ni1 N2 -81.9(4) . . . . ? C67 N10 Ni1 N2 86.4(4) . . . . ? C71 N10 Ni1 N5 92.3(4) . . . . ? C67 N10 Ni1 N5 -99.4(4) . . . . ? C66 N9 Ni1 N1 13.8(4) . . . . ? C65 N9 Ni1 N1 -167.5(3) . . . . ? C66 N9 Ni1 N10 -177.0(4) . . . . ? C65 N9 Ni1 N10 1.7(3) . . . . ? C66 N9 Ni1 N2 92.2(4) . . . . ? C65 N9 Ni1 N2 -89.1(3) . . . . ? C66 N9 Ni1 N5 -87.1(4) . . . . ? C65 N9 Ni1 N5 91.6(3) . . . . ? C41 N6 Ni1 N1 69.8(4) . . . . ? C37 N6 Ni1 N1 -104.8(3) . . . . ? C41 N6 Ni1 N10 -100.1(4) . . . . ? C37 N6 Ni1 N10 85.3(3) . . . . ? C41 N6 Ni1 N2 -8.4(4) . . . . ? C37 N6 Ni1 N2 177.0(3) . . . . ? C41 N6 Ni1 N5 170.4(4) . . . . ? C37 N6 Ni1 N5 -4.2(3) . . . . ? C11 N2 Ni1 N1 -178.0(4) . . . . ? C7 N2 Ni1 N1 3.6(3) . . . . ? C11 N2 Ni1 N10 6.9(4) . . . . ? C7 N2 Ni1 N10 -171.6(3) . . . . ? C11 N2 Ni1 N9 85.8(4) . . . . ? C7 N2 Ni1 N9 -92.6(3) . . . . ? C11 N2 Ni1 N6 -89.5(4) . . . . ? C7 N2 Ni1 N6 92.1(3) . . . . ? C36 N5 Ni1 N1 -94.4(4) . . . . ? C35 N5 Ni1 N1 96.6(3) . . . . ? C36 N5 Ni1 N10 81.9(4) . . . . ? C35 N5 Ni1 N10 -87.1(3) . . . . ? C36 N5 Ni1 N9 3.0(4) . . . . ? C35 N5 Ni1 N9 -166.0(3) . . . . ? C36 N5 Ni1 N6 178.1(4) . . . . ? C35 N5 Ni1 N6 9.1(3) . . . . ? C83 N11 Ni2 N12 -2.1(3) . . . . ? C84 N11 Ni2 N12 172.7(4) . . . . ? C83 N11 Ni2 N7 89.6(3) . . . . ? C84 N11 Ni2 N7 -95.5(4) . . . . ? C83 N11 Ni2 N3 -176.7(3) . . . . ? C84 N11 Ni2 N3 -1.8(4) . . . . ? C83 N11 Ni2 N4 -97.8(3) . . . . ? C84 N11 Ni2 N4 77.0(4) . . . . ? C55 N8 Ni2 N12 88.7(3) . . . . ? C59 N8 Ni2 N12 -86.4(4) . . . . ? C55 N8 Ni2 N7 -3.6(3) . . . . ? C59 N8 Ni2 N7 -178.8(4) . . . . ? C55 N8 Ni2 N3 -96.4(3) . . . . ? C59 N8 Ni2 N3 88.5(4) . . . . ? C55 N8 Ni2 N4 -175.2(3) . . . . ? C59 N8 Ni2 N4 9.6(4) . . . . ? C85 N12 Ni2 N11 1.9(3) . . . . ? C89 N12 Ni2 N11 -175.9(4) . . . . ? C85 N12 Ni2 N8 -173.6(3) . . . . ? C89 N12 Ni2 N8 8.6(4) . . . . ? C85 N12 Ni2 N7 -94.1(3) . . . . ? C89 N12 Ni2 N7 88.1(4) . . . . ? C85 N12 Ni2 N4 91.8(3) . . . . ? C89 N12 Ni2 N4 -86.0(4) . . . . ? C54 N7 Ni2 N11 14.2(4) . . . . ? C53 N7 Ni2 N11 -170.9(3) . . . . ? C54 N7 Ni2 N8 -173.7(4) . . . . ? C53 N7 Ni2 N8 1.2(3) . . . . ? C54 N7 Ni2 N12 93.7(4) . . . . ? C53 N7 Ni2 N12 -91.4(3) . . . . ? C54 N7 Ni2 N3 -83.9(4) . . . . ? C53 N7 Ni2 N3 91.0(3) . . . . ? C54 N7 Ni2 N4 -120.7(8) . . . . ? C53 N7 Ni2 N4 54.2(9) . . . . ? C24 N3 Ni2 N11 -86.3(4) . . . . ? C23 N3 Ni2 N11 101.7(3) . . . . ? C24 N3 Ni2 N8 89.9(4) . . . . ? C23 N3 Ni2 N8 -82.1(3) . . . . ? C24 N3 Ni2 N7 10.6(4) . . . . ? C23 N3 Ni2 N7 -161.4(3) . . . . ? C24 N3 Ni2 N4 -175.8(4) . . . . ? C23 N3 Ni2 N4 12.2(3) . . . . ? C29 N4 Ni2 N11 73.1(4) . . . . ? C25 N4 Ni2 N11 -105.1(3) . . . . ? C29 N4 Ni2 N8 -99.7(4) . . . . ? C25 N4 Ni2 N8 82.0(3) . . . . ? C29 N4 Ni2 N12 -6.2(4) . . . . ? C25 N4 Ni2 N12 175.6(3) . . . . ? C29 N4 Ni2 N7 -151.6(7) . . . . ? C25 N4 Ni2 N7 30.1(9) . . . . ? C29 N4 Ni2 N3 170.8(4) . . . . ? C25 N4 Ni2 N3 -7.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.993 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.096