# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jing-Lin Zuo' _publ_contact_author_email zuojl@nju.edu.cn loop_ _publ_author_name 'Jing-Lin Zuo' 'Xin Chen' 'Xiao-Ming Li' 'Yi-Zhi Li' 'Dong-Ping Li' ; Cai-Feng Wang ; 'Xiao-Zeng You' data_71031am _database_code_depnum_ccdc_archive 'CCDC 737795' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H104 B2 Fe2 N30 Ni3, 4(Cl O4), 2(H2 O)' _chemical_formula_sum 'C60 H108 B2 Cl4 Fe2 N30 Ni3 O18' _chemical_formula_weight 1989.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 Triclinic _symmetry_space_group_name_H-M P1 _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 13.9984(12) _cell_length_b 14.177(3) _cell_length_c 14.8798(18) _cell_angle_alpha 116.5840(10) _cell_angle_beta 103.726(3) _cell_angle_gamma 99.945(2) _cell_volume 2429.6(6) _cell_formula_units_Z 1 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1653 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 24.59 _exptl_crystal_description plate _exptl_crystal_colour Red-brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 1.043 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7449 _exptl_absorpt_correction_T_max 0.7879 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13158 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11158 _reflns_number_gt 9092 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.04P)^2^+1.22P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.012(12) _chemical_absolute_configuration unk _refine_ls_number_reflns 11158 _refine_ls_number_parameters 1099 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.0943 _refine_ls_wR_factor_gt 0.0926 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.000 _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 B1 B 0.9376(6) 0.8506(6) 0.7790(6) 0.0352(18) Uani 1 1 d . . . H11B H 1.0109 0.8922 0.8241 0.042 Uiso 1 1 calc R . . B2 B 0.0942(6) 1.0383(6) 0.2754(6) 0.0347(17) Uani 1 1 d . . . H22E H 0.0223 0.9944 0.2265 0.042 Uiso 1 1 calc R . . C1 C 0.8295(5) 0.5697(5) 0.6702(5) 0.0417(18) Uani 1 1 d . . . H1 H 0.7769 0.5048 0.6151 0.050 Uiso 1 1 calc R . . C2 C 0.9199(5) 0.5675(5) 0.7256(5) 0.0329(15) Uani 1 1 d . . . H2 H 0.9349 0.5106 0.7353 0.040 Uiso 1 1 calc R . . C3 C 0.9864(5) 0.6773(5) 0.7654(5) 0.0437(19) Uani 1 1 d . . . H3 H 1.0585 0.6999 0.7907 0.052 Uiso 1 1 calc R . . C4 C 0.7388(5) 0.9033(5) 0.8634(5) 0.0313(14) Uani 1 1 d . . . H4 H 0.6703 0.8763 0.8562 0.038 Uiso 1 1 calc R . . C5 C 0.8144(5) 0.9869(5) 0.9585(5) 0.0361(15) Uani 1 1 d . . . H5 H 0.8083 1.0367 1.0223 0.043 Uiso 1 1 calc R . . C6 C 0.9012(6) 0.9765(5) 0.9333(6) 0.049(2) Uani 1 1 d . . . H6 H 0.9679 1.0053 0.9839 0.059 Uiso 1 1 calc R . . C7 C 0.8075(6) 0.7827(6) 0.5073(6) 0.052(2) Uani 1 1 d . . . H7 H 0.7482 0.7489 0.4458 0.062 Uiso 1 1 calc R . . C8 C 0.9052(5) 0.8345(5) 0.5243(5) 0.0385(16) Uani 1 1 d . . . H8 H 0.9248 0.8334 0.4684 0.046 Uiso 1 1 calc R . . C9 C 0.9762(5) 0.8902(6) 0.6296(6) 0.0401(17) Uani 1 1 d . . . H9 H 1.0451 0.9342 0.6567 0.048 Uiso 1 1 calc R . . C10 C 0.2158(4) 1.1037(5) 0.5611(5) 0.0337(16) Uani 1 1 d . . . H10 H 0.2720 1.1358 0.6250 0.040 Uiso 1 1 calc R . . C11 C 0.1175(5) 1.0501(5) 0.5448(5) 0.0360(16) Uani 1 1 d . . . H11 H 0.0955 1.0360 0.5931 0.043 Uiso 1 1 calc R . . C12 C 0.0542(5) 1.0194(5) 0.4382(5) 0.0292(14) Uani 1 1 d . . . H12 H -0.0169 0.9826 0.4043 0.035 Uiso 1 1 calc R . . C13 C 0.3330(5) 0.9869(5) 0.2165(5) 0.0349(15) Uani 1 1 d . . . H13 H 0.4030 0.9966 0.2270 0.042 Uiso 1 1 calc R . . C14 C 0.2455(5) 0.9094(5) 0.1331(4) 0.0344(16) Uani 1 1 d . . . H14 H 0.2563 0.8519 0.0779 0.041 Uiso 1 1 calc R . . C15 C 0.1470(5) 0.9032(5) 0.1185(5) 0.0340(15) Uani 1 1 d . . . H15 H 0.0847 0.8554 0.0620 0.041 Uiso 1 1 calc R . . C16 C 0.2372(5) 1.3525(6) 0.3824(6) 0.0479(19) Uani 1 1 d . . . H16 H 0.2939 1.4131 0.4041 0.057 Uiso 1 1 calc R . . C17 C 0.1273(5) 1.3268(5) 0.3485(5) 0.0314(15) Uani 1 1 d . . . H17 H 0.1002 1.3843 0.3773 0.038 Uiso 1 1 calc R . . C18 C 0.0553(5) 1.2149(5) 0.2710(5) 0.0413(18) Uani 1 1 d . . . H18 H -0.0111 1.1883 0.2206 0.050 Uiso 1 1 calc R . . C19 C 0.6258(5) 0.6484(5) 0.6797(5) 0.0316(15) Uani 1 1 d . . . C20 C 0.6825(5) 0.5802(5) 0.4903(5) 0.0348(15) Uani 1 1 d . . . C21 C 0.6127(5) 0.7930(5) 0.5907(5) 0.0375(16) Uani 1 1 d . . . C22 C 0.4232(5) 1.1278(5) 0.4872(5) 0.0374(16) Uani 1 1 d . . . C23 C 0.4358(5) 1.2452(5) 0.3798(6) 0.0390(17) Uani 1 1 d . . . C24 C 0.3822(4) 1.3089(5) 0.5516(5) 0.0334(16) Uani 1 1 d . . . C25 C 0.7099(6) 0.3723(8) 0.1764(6) 0.053(2) Uani 1 1 d . . . H25 H 0.6692 0.2972 0.1156 0.064 Uiso 1 1 calc R . . C26 C 0.7891(4) 0.4362(5) 0.1490(5) 0.0374(15) Uani 1 1 d . . . H26A H 0.7533 0.4370 0.0852 0.045 Uiso 1 1 calc R . . H26B H 0.8218 0.5126 0.2080 0.045 Uiso 1 1 calc R . . C27 C 0.8683(5) 0.3817(6) 0.1305(6) 0.0412(18) Uani 1 1 d . . . H27A H 0.9205 0.4212 0.1157 0.049 Uiso 1 1 calc R . . H27B H 0.8379 0.3047 0.0721 0.049 Uiso 1 1 calc R . . C28 C 0.9129(5) 0.3905(5) 0.2395(5) 0.0384(16) Uani 1 1 d . . . H28A H 0.9748 0.3685 0.2409 0.046 Uiso 1 1 calc R . . H28B H 0.9353 0.4687 0.2942 0.046 Uiso 1 1 calc R . . C29 C 0.8509(5) 0.3296(5) 0.2734(5) 0.0398(17) Uani 1 1 d . . . H29A H 0.8907 0.3434 0.3436 0.048 Uiso 1 1 calc R . . H29B H 0.8278 0.2502 0.2223 0.048 Uiso 1 1 calc R . . C30 C 0.7575(5) 0.3727(6) 0.2783(6) 0.0483(19) Uani 1 1 d . . . H30 H 0.7845 0.4505 0.3371 0.058 Uiso 1 1 calc R . . C31 C 0.3361(5) 0.2385(5) 0.1107(5) 0.0424(19) Uani 1 1 d . . . H31 H 0.3542 0.2161 0.0460 0.051 Uiso 1 1 calc R . . C32 C 0.2202(5) 0.1665(5) 0.0883(5) 0.0399(15) Uani 1 1 d . . . H32A H 0.2100 0.0873 0.0479 0.048 Uiso 1 1 calc R . . H32B H 0.2102 0.1842 0.1557 0.048 Uiso 1 1 calc R . . C33 C 0.1427(5) 0.1994(5) 0.0221(5) 0.0345(15) Uani 1 1 d . . . H33A H 0.1459 0.1688 -0.0495 0.041 Uiso 1 1 calc R . . H33B H 0.0729 0.1650 0.0146 0.041 Uiso 1 1 calc R . . C34 C 0.1623(5) 0.3254(5) 0.0706(5) 0.0410(18) Uani 1 1 d . . . H34A H 0.1128 0.3382 0.0230 0.049 Uiso 1 1 calc R . . H34B H 0.1524 0.3561 0.1392 0.049 Uiso 1 1 calc R . . C35 C 0.2693(5) 0.3820(5) 0.0863(5) 0.0415(17) Uani 1 1 d . . . H35A H 0.2810 0.4608 0.1130 0.050 Uiso 1 1 calc R . . H35B H 0.2824 0.3492 0.0194 0.050 Uiso 1 1 calc R . . C36 C 0.3387(6) 0.3638(6) 0.1695(6) 0.049(2) Uani 1 1 d . . . H36 H 0.3158 0.3815 0.2308 0.059 Uiso 1 1 calc R . . C37 C 0.3259(5) 0.8095(5) 0.3464(5) 0.0356(15) Uani 1 1 d . . . H37 H 0.3039 0.8648 0.3319 0.043 Uiso 1 1 calc R . . C38 C 0.2673(5) 0.6975(5) 0.2485(5) 0.0347(15) Uani 1 1 d . . . H38A H 0.2898 0.6404 0.2580 0.042 Uiso 1 1 calc R . . H38B H 0.2793 0.6953 0.1861 0.042 Uiso 1 1 calc R . . C39 C 0.1511(4) 0.6774(5) 0.2330(5) 0.0331(14) Uani 1 1 d . . . H39A H 0.1107 0.6035 0.1722 0.040 Uiso 1 1 calc R . . H39B H 0.1281 0.7312 0.2176 0.040 Uiso 1 1 calc R . . C40 C 0.1327(4) 0.6888(4) 0.3356(4) 0.0288(14) Uani 1 1 d . . . H40A H 0.0592 0.6741 0.3243 0.035 Uiso 1 1 calc R . . H40B H 0.1552 0.6350 0.3511 0.035 Uiso 1 1 calc R . . C41 C 0.1924(5) 0.8039(5) 0.4280(5) 0.0320(15) Uani 1 1 d . . . H41A H 0.1720 0.8577 0.4109 0.038 Uiso 1 1 calc R . . H41B H 0.1769 0.8134 0.4911 0.038 Uiso 1 1 calc R . . C42 C 0.3059(5) 0.8237(4) 0.4510(5) 0.0311(14) Uani 1 1 d . . . H42 H 0.3252 0.7674 0.4656 0.037 Uiso 1 1 calc R . . C43 C 0.7200(4) 1.1422(5) 0.6941(4) 0.0300(13) Uani 1 1 d . . . H43 H 0.7014 1.1799 0.6544 0.036 Uiso 1 1 calc R . . C44 C 0.8089(4) 1.2329(5) 0.7973(4) 0.0302(14) Uani 1 1 d . . . H44A H 0.7887 1.2989 0.8294 0.036 Uiso 1 1 calc R . . H44B H 0.8226 1.2074 0.8482 0.036 Uiso 1 1 calc R . . C45 C 0.9059(4) 1.2617(5) 0.7757(5) 0.0329(14) Uani 1 1 d . . . H45A H 0.9615 1.3168 0.8431 0.039 Uiso 1 1 calc R . . H45B H 0.8943 1.2943 0.7306 0.039 Uiso 1 1 calc R . . C46 C 0.9382(4) 1.1597(4) 0.7202(4) 0.0318(14) Uani 1 1 d . . . H46A H 1.0057 1.1816 0.7158 0.038 Uiso 1 1 calc R . . H46B H 0.9424 1.1215 0.7604 0.038 Uiso 1 1 calc R . . C47 C 0.8567(5) 1.0840(5) 0.6083(5) 0.0334(15) Uani 1 1 d . . . H47A H 0.8768 1.0197 0.5690 0.040 Uiso 1 1 calc R . . H47B H 0.8515 1.1236 0.5694 0.040 Uiso 1 1 calc R . . C48 C 0.7491(4) 1.0448(4) 0.6165(5) 0.0262(12) Uani 1 1 d . . . H48 H 0.7558 0.9970 0.6473 0.031 Uiso 1 1 calc R . . C49 C 0.7060(5) 0.5501(5) 0.9014(5) 0.0352(16) Uani 1 1 d . . . H49 H 0.6788 0.5313 0.9483 0.042 Uiso 1 1 calc R . . C50 C 0.8150(4) 0.5381(5) 0.9095(5) 0.0366(15) Uani 1 1 d . . . H50A H 0.8121 0.4614 0.8858 0.044 Uiso 1 1 calc R . . H50B H 0.8419 0.5607 0.8654 0.044 Uiso 1 1 calc R . . C51 C 0.8844(4) 0.6149(4) 1.0294(4) 0.0270(13) Uani 1 1 d . . . H51A H 0.8562 0.5904 1.0718 0.032 Uiso 1 1 calc R . . H51B H 0.9534 0.6081 1.0390 0.032 Uiso 1 1 calc R . . C52 C 0.8923(5) 0.7335(5) 1.0698(5) 0.0397(16) Uani 1 1 d . . . H52A H 0.9325 0.7756 1.1463 0.048 Uiso 1 1 calc R . . H52B H 0.9312 0.7604 1.0353 0.048 Uiso 1 1 calc R . . C53 C 0.7939(5) 0.7585(5) 1.0534(5) 0.0406(16) Uani 1 1 d . . . H53A H 0.8060 0.8340 1.0671 0.049 Uiso 1 1 calc R . . H53B H 0.7612 0.7507 1.1014 0.049 Uiso 1 1 calc R . . C54 C 0.7257(5) 0.6749(5) 0.9368(5) 0.0320(15) Uani 1 1 d . . . H54 H 0.7611 0.6890 0.8925 0.038 Uiso 1 1 calc R . . C55 C 0.3178(5) 0.5756(5) 0.8175(5) 0.0402(17) Uani 1 1 d . . . H55 H 0.3489 0.6569 0.8592 0.048 Uiso 1 1 calc R . . C56 C 0.1951(5) 0.5456(6) 0.7721(5) 0.0446(19) Uani 1 1 d . . . H56A H 0.1750 0.5769 0.7273 0.053 Uiso 1 1 calc R . . H56B H 0.1617 0.4655 0.7299 0.053 Uiso 1 1 calc R . . C57 C 0.1648(5) 0.5976(5) 0.8731(5) 0.0336(14) Uani 1 1 d . . . H57A H 0.2057 0.6757 0.9204 0.040 Uiso 1 1 calc R . . H57B H 0.0919 0.5915 0.8527 0.040 Uiso 1 1 calc R . . C58 C 0.1861(5) 0.5344(6) 0.9269(5) 0.0405(17) Uani 1 1 d . . . H58A H 0.1522 0.5486 0.9793 0.049 Uiso 1 1 calc R . . H58B H 0.1603 0.4552 0.8747 0.049 Uiso 1 1 calc R . . C59 C 0.2987(4) 0.5710(5) 0.9801(4) 0.0321(14) Uani 1 1 d . . . H59A H 0.3168 0.5380 1.0238 0.039 Uiso 1 1 calc R . . H59B H 0.3260 0.6514 1.0258 0.039 Uiso 1 1 calc R . . C60 C 0.3403(6) 0.5325(5) 0.8915(6) 0.0406(18) Uani 1 1 d . . . H60 H 0.3132 0.4510 0.8490 0.049 Uiso 1 1 calc R . . Cl1 Cl 0.47790(15) 0.22525(14) 0.86296(14) 0.0360(4) Uani 1 1 d . . . Cl2 Cl 0.70514(11) 0.03742(12) 0.27150(12) 0.0258(3) Uani 1 1 d . . . Cl3 Cl 0.59253(14) 0.69341(14) 0.21292(14) 0.0396(4) Uani 1 1 d . . . Cl4 Cl 0.46197(12) 0.91676(12) 0.93827(12) 0.0302(3) Uani 1 1 d . . . Fe1 Fe 0.71793(10) 0.72365(10) 0.63795(10) 0.0422(3) Uani 1 1 d . . . Fe2 Fe 0.33286(9) 1.17957(9) 0.42175(10) 0.0381(3) Uani 1 1 d . . . N1 N 0.8187(4) 0.6820(4) 0.7022(4) 0.0372(14) Uani 1 1 d . . . N2 N 0.9257(4) 0.7466(4) 0.7603(4) 0.0382(15) Uani 1 1 d . . . N3 N 0.7750(4) 0.8638(5) 0.7804(5) 0.0482(19) Uani 1 1 d . . . N4 N 0.8797(4) 0.9229(4) 0.8330(4) 0.0361(14) Uani 1 1 d . . . N5 N 0.8191(4) 0.7934(5) 0.6036(5) 0.0445(16) Uani 1 1 d . . . N6 N 0.9218(4) 0.8650(4) 0.6805(4) 0.0361(14) Uani 1 1 d . . . N7 N 0.2210(5) 1.1042(5) 0.4663(5) 0.0462(15) Uani 1 1 d . . . N8 N 0.1141(4) 1.0522(4) 0.4004(4) 0.0318(12) Uani 1 1 d . . . N9 N 0.2800(4) 1.0504(4) 0.2847(4) 0.0290(12) Uani 1 1 d . . . N10 N 0.1729(4) 0.9965(4) 0.2209(4) 0.0292(12) Uani 1 1 d . . . N11 N 0.2209(4) 1.2413(4) 0.3676(4) 0.0354(14) Uani 1 1 d . . . N12 N 0.1212(4) 1.1627(4) 0.2994(4) 0.0292(12) Uani 1 1 d . . . N13 N 0.5743(5) 0.6173(5) 0.7141(4) 0.0402(14) Uani 1 1 d . . . N14 N 0.6337(5) 0.5027(4) 0.4180(4) 0.0370(14) Uani 1 1 d . . . N15 N 0.5515(4) 0.8179(4) 0.5496(4) 0.0358(13) Uani 1 1 d . . . N16 N 0.4703(3) 1.0767(4) 0.5066(4) 0.0225(10) Uani 1 1 d . . . N17 N 0.4927(4) 1.3023(4) 0.3623(4) 0.0298(12) Uani 1 1 d . . . N18 N 0.4111(4) 1.3956(4) 0.6390(4) 0.0349(13) Uani 1 1 d . . . N19 N 0.6465(4) 0.4440(4) 0.2053(4) 0.0405(13) Uani 1 1 d . . . H19A H 0.6063 0.4426 0.1474 0.049 Uiso 1 1 calc R . . H19B H 0.6858 0.5147 0.2555 0.049 Uiso 1 1 calc R . . N20 N 0.6792(4) 0.3133(4) 0.3013(4) 0.0386(13) Uani 1 1 d . . . H20A H 0.7046 0.3297 0.3700 0.046 Uiso 1 1 calc R . . H20B H 0.6632 0.2393 0.2581 0.046 Uiso 1 1 calc R . . N21 N 0.4057(4) 0.2282(4) 0.1943(4) 0.0343(12) Uani 1 1 d . . . H21A H 0.4192 0.1635 0.1640 0.041 Uiso 1 1 calc R . . H21B H 0.3748 0.2280 0.2409 0.041 Uiso 1 1 calc R . . N22 N 0.4446(4) 0.4286(4) 0.2034(4) 0.0365(12) Uani 1 1 d . . . H22A H 0.4554 0.5002 0.2515 0.044 Uiso 1 1 calc R . . H22B H 0.4589 0.4258 0.1466 0.044 Uiso 1 1 calc R . . N23 N 0.4384(4) 0.8363(4) 0.3699(4) 0.0265(11) Uani 1 1 d . . . H23A H 0.4551 0.8623 0.3285 0.032 Uiso 1 1 calc R . . H23B H 0.4556 0.7738 0.3530 0.032 Uiso 1 1 calc R . . N24 N 0.3757(4) 0.9355(4) 0.5395(4) 0.0293(12) Uani 1 1 d . . . H24A H 0.3769 0.9429 0.6031 0.035 Uiso 1 1 calc R . . H24B H 0.3519 0.9880 0.5329 0.035 Uiso 1 1 calc R . . N25 N 0.6209(4) 1.0878(4) 0.6929(4) 0.0393(15) Uani 1 1 d . . . H25A H 0.5884 1.1382 0.7177 0.047 Uiso 1 1 calc R . . H25B H 0.6322 1.0599 0.7368 0.047 Uiso 1 1 calc R . . N26 N 0.6675(4) 0.9743(4) 0.5080(4) 0.0379(14) Uani 1 1 d . . . H26C H 0.6758 0.9073 0.4733 0.046 Uiso 1 1 calc R . . H26D H 0.6697 1.0070 0.4685 0.046 Uiso 1 1 calc R . . N27 N 0.6347(4) 0.4820(4) 0.7874(4) 0.0358(12) Uani 1 1 d . . . H27C H 0.6156 0.4091 0.7660 0.043 Uiso 1 1 calc R . . H27D H 0.6648 0.4924 0.7440 0.043 Uiso 1 1 calc R . . N28 N 0.6292(4) 0.7015(4) 0.9162(4) 0.0331(12) Uani 1 1 d . . . H28C H 0.6353 0.7513 0.8943 0.040 Uiso 1 1 calc R . . H28D H 0.6133 0.7301 0.9761 0.040 Uiso 1 1 calc R . . N29 N 0.3496(4) 0.5320(4) 0.7235(4) 0.0429(14) Uani 1 1 d . . . H29C H 0.3456 0.5740 0.6928 0.051 Uiso 1 1 calc R . . H29D H 0.3094 0.4614 0.6743 0.051 Uiso 1 1 calc R . . N30 N 0.4538(4) 0.5662(4) 0.9323(4) 0.0360(12) Uani 1 1 d . . . H30A H 0.4754 0.5244 0.9587 0.043 Uiso 1 1 calc R . . H30B H 0.4807 0.6382 0.9852 0.043 Uiso 1 1 calc R . . Ni1 Ni 0.54343(8) 0.36070(9) 0.27577(9) 0.02768(18) Uani 1 1 d . . . Ni2 Ni 0.52530(9) 0.95748(9) 0.53503(10) 0.03088(16) Uani 1 1 d . . . Ni3 Ni 0.50691(9) 0.54018(9) 0.78675(9) 0.0356(2) Uani 1 1 d . . . O1 O 0.9950(7) 0.6048(7) 0.5152(7) 0.028(2) Uani 0.40 1 d P . . H1C H 0.9577 0.6087 0.4635 0.034 Uiso 0.40 1 d PR . . H1D H 1.0459 0.6649 0.5563 0.034 Uiso 0.40 1 d PR . . O2 O 0.2662(8) -0.0021(8) 0.7184(8) 0.042(3) Uani 0.40 1 d P . . H2C H 0.3039 -0.0170 0.7611 0.051 Uiso 0.40 1 d PR . . H2B H 0.2290 0.0335 0.7484 0.064 Uiso 0.40 1 d PR . . O3 O 1.0030(8) 0.3624(9) 0.5561(8) 0.040(3) Uani 0.40 1 d P . . H3B H 0.9426 0.3499 0.5590 0.047 Uiso 0.40 1 d PR . . H3C H 1.0002 0.3184 0.4929 0.047 Uiso 0.40 1 d PR . . O4 O 0.2520(7) 0.6449(10) 0.5890(8) 0.046(3) Uani 0.40 1 d P . . H4E H 0.2051 0.5923 0.5816 0.055 Uiso 0.40 1 d PR . . H4B H 0.3014 0.6216 0.5739 0.055 Uiso 0.40 1 d PR . . O5 O 0.6682(8) 0.3016(9) 0.5115(10) 0.046(3) Uani 0.40 1 d P . . H5C H 0.6824 0.2844 0.5600 0.055 Uiso 0.40 1 d PR . . H5D H 0.6430 0.2425 0.4498 0.055 Uiso 0.40 1 d PR . . O11 O 0.5008(3) 0.1343(3) 0.8733(3) 0.0314(9) Uani 1 1 d . . . O12 O 0.5194(3) 0.2372(3) 0.7911(3) 0.0405(12) Uani 1 1 d . . . O13 O 0.3655(3) 0.1830(3) 0.8113(3) 0.0420(12) Uani 1 1 d . . . O14 O 0.4949(3) 0.3211(3) 0.9519(3) 0.0316(9) Uani 1 1 d . . . O21 O 0.7824(3) -0.0041(3) 0.3033(3) 0.0328(10) Uani 1 1 d . . . O22 O 0.7531(3) 0.1521(3) 0.3333(3) 0.0362(10) Uani 1 1 d . . . O23 O 0.6779(3) -0.0118(3) 0.1558(3) 0.0317(10) Uani 1 1 d . . . O24 O 0.6281(3) 0.0060(3) 0.2981(3) 0.0366(10) Uani 1 1 d . . . O31 O 0.5038(4) 0.6454(4) 0.2294(4) 0.0448(12) Uani 1 1 d . . . O32 O 0.6728(3) 0.7801(3) 0.2942(3) 0.0319(9) Uani 1 1 d . . . O33 O 0.5496(3) 0.7220(3) 0.1454(3) 0.0399(11) Uani 1 1 d . . . O34 O 0.6254(3) 0.6095(3) 0.1534(3) 0.0296(9) Uani 1 1 d . . . O41 O 0.4347(3) 0.8743(3) 0.9961(3) 0.0332(10) Uani 1 1 d . . . O42 O 0.3672(3) 0.8919(3) 0.8662(3) 0.0309(10) Uani 1 1 d . . . O43 O 0.5078(3) 1.0268(3) 1.0038(3) 0.0330(10) Uani 1 1 d . . . O44 O 0.5235(3) 0.8583(3) 0.8846(3) 0.0351(10) 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 B1 0.030(4) 0.028(3) 0.037(4) 0.008(3) 0.014(3) 0.009(3) B2 0.036(4) 0.041(4) 0.035(4) 0.020(3) 0.021(3) 0.017(3) C1 0.039(4) 0.022(3) 0.031(3) -0.002(2) -0.005(3) 0.001(3) C2 0.024(3) 0.030(3) 0.040(4) 0.012(3) 0.017(3) 0.010(3) C3 0.036(4) 0.040(4) 0.036(4) 0.022(3) -0.016(3) 0.003(3) C4 0.031(3) 0.029(3) 0.040(3) 0.022(3) 0.005(3) 0.021(3) C5 0.042(4) 0.032(3) 0.027(3) 0.014(3) 0.006(3) 0.010(3) C6 0.041(4) 0.034(3) 0.033(4) -0.010(3) 0.007(3) 0.010(3) C7 0.044(4) 0.036(4) 0.032(4) -0.005(3) 0.006(3) -0.009(3) C8 0.038(4) 0.024(3) 0.045(4) 0.016(3) 0.011(3) 0.001(3) C9 0.033(3) 0.039(3) 0.043(4) 0.017(3) 0.010(3) 0.016(3) C10 0.016(3) 0.033(3) 0.041(4) 0.014(3) 0.000(2) 0.012(3) C11 0.035(3) 0.028(3) 0.032(3) 0.020(3) -0.005(3) -0.009(3) C12 0.021(3) 0.035(3) 0.019(3) 0.007(2) 0.004(2) 0.007(2) C13 0.031(3) 0.032(3) 0.034(3) 0.015(3) -0.002(3) 0.016(3) C14 0.040(3) 0.037(3) 0.016(3) 0.005(2) 0.000(2) 0.027(3) C15 0.034(3) 0.022(3) 0.023(3) 0.000(2) 0.001(3) 0.000(2) C16 0.027(3) 0.053(4) 0.061(5) 0.040(4) 0.004(3) -0.005(3) C17 0.037(3) 0.033(3) 0.020(3) 0.006(2) 0.020(3) 0.010(3) C18 0.023(3) 0.039(3) 0.032(3) 0.004(3) -0.006(3) 0.005(3) C19 0.041(3) 0.037(3) 0.013(3) 0.009(2) 0.004(2) 0.024(3) C20 0.040(4) 0.034(3) 0.023(3) 0.009(2) 0.012(3) 0.008(3) C21 0.029(3) 0.021(3) 0.040(4) 0.009(3) -0.003(3) -0.003(2) C22 0.043(4) 0.021(3) 0.025(3) 0.000(2) 0.002(3) 0.009(3) C23 0.032(3) 0.024(3) 0.048(4) 0.008(3) 0.015(3) 0.010(3) C24 0.016(3) 0.024(3) 0.035(3) -0.001(2) 0.000(2) 0.010(2) C25 0.036(4) 0.082(6) 0.042(4) 0.029(4) 0.019(3) 0.021(4) C26 0.027(3) 0.029(3) 0.038(3) 0.007(3) 0.007(3) 0.005(2) C27 0.028(3) 0.037(3) 0.037(4) 0.006(3) 0.010(3) 0.001(3) C28 0.032(3) 0.035(3) 0.038(3) 0.006(3) 0.017(3) 0.017(3) C29 0.038(4) 0.024(3) 0.035(4) 0.000(3) 0.012(3) 0.004(3) C30 0.033(4) 0.043(4) 0.036(4) 0.007(3) -0.005(3) 0.000(3) C31 0.036(4) 0.036(3) 0.023(3) -0.004(3) 0.002(3) 0.008(3) C32 0.036(3) 0.049(4) 0.024(3) 0.014(3) 0.004(3) 0.012(3) C33 0.037(3) 0.039(3) 0.046(4) 0.023(3) 0.032(3) 0.027(3) C34 0.034(3) 0.033(3) 0.033(3) -0.002(3) 0.009(3) 0.017(3) C35 0.036(3) 0.035(3) 0.034(3) 0.000(3) 0.015(3) 0.014(3) C36 0.039(4) 0.040(4) 0.036(4) -0.002(3) 0.003(3) 0.014(3) C37 0.042(3) 0.033(3) 0.026(3) 0.022(3) -0.001(3) -0.004(3) C38 0.036(3) 0.033(3) 0.019(3) 0.006(2) 0.003(2) 0.007(3) C39 0.031(3) 0.036(3) 0.031(3) 0.012(3) 0.012(2) 0.020(3) C40 0.029(3) 0.015(2) 0.031(3) 0.002(2) 0.006(2) 0.016(2) C41 0.031(3) 0.036(3) 0.020(3) 0.010(2) 0.003(2) 0.014(3) C42 0.037(3) 0.014(2) 0.030(3) 0.002(2) 0.010(3) 0.011(2) C43 0.022(3) 0.038(3) 0.016(3) 0.007(2) -0.002(2) 0.012(2) C44 0.019(3) 0.045(3) 0.022(3) 0.014(3) 0.003(2) 0.015(3) C45 0.029(3) 0.029(3) 0.033(3) 0.016(3) 0.000(3) 0.006(3) C46 0.030(3) 0.026(3) 0.021(3) 0.000(2) 0.011(2) -0.002(2) C47 0.037(4) 0.033(3) 0.027(3) 0.014(3) 0.009(3) 0.013(3) C48 0.031(3) 0.019(3) 0.038(3) 0.021(2) 0.015(2) 0.006(2) C49 0.030(3) 0.034(3) 0.019(3) -0.002(3) 0.010(3) 0.004(3) C50 0.021(3) 0.041(3) 0.029(3) 0.005(3) 0.007(2) 0.005(3) C51 0.031(3) 0.021(3) 0.023(3) 0.002(2) 0.013(2) 0.015(2) C52 0.039(4) 0.032(3) 0.034(3) 0.005(3) 0.014(3) 0.011(3) C53 0.036(3) 0.035(3) 0.030(3) 0.003(3) 0.009(3) 0.006(3) C54 0.021(3) 0.040(3) 0.025(3) 0.012(3) 0.009(2) 0.001(3) C55 0.040(4) 0.023(3) 0.033(3) 0.002(3) 0.003(3) 0.005(3) C56 0.042(4) 0.037(3) 0.021(3) 0.000(3) -0.003(3) -0.002(3) C57 0.037(3) 0.026(3) 0.032(3) 0.008(2) 0.012(3) 0.016(3) C58 0.031(4) 0.046(4) 0.028(3) 0.013(3) -0.003(3) 0.013(3) C59 0.027(3) 0.027(3) 0.027(3) 0.001(2) 0.008(2) 0.013(2) C60 0.049(4) 0.024(3) 0.042(4) 0.007(3) 0.023(3) 0.015(3) Cl1 0.0433(9) 0.0291(7) 0.0248(7) 0.0086(6) 0.0065(6) 0.0104(6) Cl2 0.0252(6) 0.0232(6) 0.0248(7) 0.0066(5) 0.0129(5) 0.0091(5) Cl3 0.0332(8) 0.0314(8) 0.0298(8) 0.0039(6) -0.0006(6) 0.0054(7) Cl4 0.0264(7) 0.0256(6) 0.0303(7) 0.0048(5) 0.0132(6) 0.0119(5) Fe1 0.0395(6) 0.0367(5) 0.0296(5) 0.0075(4) 0.0002(4) 0.0094(4) Fe2 0.0243(5) 0.0247(4) 0.0325(5) -0.0032(4) -0.0017(4) 0.0004(4) N1 0.026(3) 0.027(3) 0.035(3) 0.002(2) 0.001(2) 0.007(2) N2 0.025(3) 0.026(3) 0.036(3) -0.004(2) 0.008(2) 0.004(2) N3 0.026(3) 0.052(4) 0.033(3) -0.001(3) -0.004(2) 0.022(3) N4 0.040(3) 0.019(2) 0.030(3) -0.001(2) 0.012(2) 0.005(2) N5 0.033(3) 0.036(3) 0.047(4) 0.018(3) -0.001(3) 0.001(2) N6 0.031(3) 0.026(2) 0.027(3) -0.007(2) 0.013(2) 0.005(2) N7 0.038(3) 0.046(3) 0.037(3) 0.013(3) 0.008(3) 0.005(3) N8 0.032(3) 0.033(3) 0.029(3) 0.014(2) 0.011(2) 0.011(2) N9 0.028(3) 0.017(2) 0.027(3) 0.006(2) -0.001(2) 0.000(2) N10 0.025(3) 0.024(2) 0.024(3) 0.004(2) -0.001(2) 0.011(2) N11 0.031(3) 0.029(3) 0.023(3) -0.002(2) 0.002(2) 0.011(2) N12 0.028(3) 0.029(3) 0.022(3) 0.008(2) 0.005(2) 0.009(2) N13 0.057(4) 0.035(3) 0.021(3) 0.012(2) 0.008(3) 0.015(3) N14 0.044(3) 0.028(3) 0.025(3) 0.008(2) 0.007(2) 0.004(2) N15 0.031(3) 0.027(2) 0.025(3) 0.001(2) -0.003(2) 0.006(2) N16 0.019(2) 0.015(2) 0.022(2) 0.0033(17) 0.0078(18) -0.0027(17) N17 0.025(2) 0.029(3) 0.025(3) 0.006(2) 0.007(2) 0.011(2) N18 0.028(3) 0.035(3) 0.024(3) 0.012(2) -0.004(2) -0.002(2) N19 0.041(3) 0.036(3) 0.030(3) 0.012(2) 0.012(2) -0.007(2) N20 0.024(2) 0.032(3) 0.035(3) 0.007(2) -0.002(2) 0.001(2) N21 0.028(2) 0.035(3) 0.036(3) 0.013(2) 0.015(2) 0.011(2) N22 0.044(3) 0.029(2) 0.035(3) 0.011(2) 0.021(2) 0.015(2) N23 0.036(3) 0.017(2) 0.025(3) 0.0116(19) 0.007(2) 0.009(2) N24 0.032(3) 0.021(2) 0.025(3) 0.011(2) -0.002(2) 0.003(2) N25 0.036(3) 0.032(3) 0.025(3) 0.001(2) 0.004(2) 0.005(2) N26 0.030(3) 0.030(3) 0.038(3) 0.004(2) 0.013(2) 0.013(2) N27 0.041(3) 0.030(2) 0.023(2) 0.007(2) 0.005(2) 0.009(2) N28 0.030(3) 0.029(2) 0.020(2) 0.0002(19) 0.007(2) 0.003(2) N29 0.037(3) 0.036(3) 0.026(3) 0.001(2) -0.003(2) 0.006(2) N30 0.045(3) 0.025(2) 0.031(3) 0.010(2) 0.011(2) 0.013(2) Ni1 0.0243(4) 0.0245(4) 0.0274(4) 0.0069(3) 0.0133(3) 0.0047(3) Ni2 0.0252(3) 0.0274(3) 0.0306(3) 0.0098(3) 0.0041(3) 0.0096(3) Ni3 0.0254(4) 0.0348(4) 0.0250(4) 0.0062(3) 0.0040(3) -0.0061(3) O1 0.028(5) 0.026(5) 0.026(5) 0.007(4) 0.015(4) 0.005(4) O2 0.041(6) 0.033(5) 0.034(6) 0.006(4) 0.006(5) 0.010(5) O3 0.037(6) 0.053(6) 0.032(6) 0.020(5) 0.021(5) 0.014(5) O4 0.020(5) 0.065(7) 0.033(6) 0.026(5) -0.010(4) -0.003(5) O5 0.033(6) 0.051(7) 0.063(8) 0.037(6) 0.012(5) 0.022(5) O11 0.037(2) 0.029(2) 0.020(2) 0.0110(16) 0.0057(17) 0.0031(18) O12 0.027(2) 0.029(2) 0.031(2) 0.0032(18) -0.0140(18) 0.0009(18) O13 0.040(2) 0.029(2) 0.035(2) -0.0025(18) 0.018(2) 0.0088(19) O14 0.0217(19) 0.0279(19) 0.029(2) 0.0063(16) 0.0085(16) -0.0046(16) O21 0.0253(19) 0.034(2) 0.024(2) 0.0041(16) 0.0069(16) 0.0090(17) O22 0.035(2) 0.0278(19) 0.032(2) 0.0054(17) 0.0102(18) 0.0104(18) O23 0.027(2) 0.034(2) 0.023(2) 0.0092(17) 0.0071(17) 0.0028(17) O24 0.031(2) 0.038(2) 0.041(2) 0.0158(19) 0.0211(18) 0.0126(18) O31 0.034(2) 0.039(2) 0.026(2) 0.0011(19) -0.0047(19) -0.002(2) O32 0.028(2) 0.0247(19) 0.027(2) 0.0011(16) 0.0114(17) 0.0062(16) O33 0.025(2) 0.033(2) 0.028(2) 0.0003(18) -0.0090(18) 0.0007(18) O34 0.026(2) 0.0228(18) 0.029(2) 0.0034(16) 0.0077(16) 0.0139(16) O41 0.024(2) 0.034(2) 0.029(2) 0.0119(17) -0.0043(16) 0.0110(17) O42 0.033(2) 0.032(2) 0.0131(19) 0.0029(16) 0.0042(16) 0.0063(17) O43 0.028(2) 0.031(2) 0.025(2) 0.0073(17) -0.0034(16) 0.0134(17) O44 0.0256(19) 0.042(2) 0.0170(19) 0.0040(16) -0.0022(15) 0.0087(18) _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 B1 N2 1.343(8) . ? B1 N4 1.488(7) . ? B1 N6 1.540(9) . ? B1 H11B 0.9800 . ? B2 N10 1.562(7) . ? B2 N12 1.589(8) . ? B2 N8 1.728(8) . ? B2 H22E 0.9800 . ? C1 C2 1.351(9) . ? C1 N1 1.490(7) . ? C1 H1 0.9300 . ? C2 C3 1.433(9) . ? C2 H2 0.9300 . ? C3 N2 1.419(7) . ? C3 H3 0.9300 . ? C4 N3 1.368(7) . ? C4 C5 1.372(8) . ? C4 H4 0.9300 . ? C5 C6 1.367(10) . ? C5 H5 0.9300 . ? C6 N4 1.260(7) . ? C6 H6 0.9300 . ? C7 N5 1.339(8) . ? C7 C8 1.340(10) . ? C7 H7 0.9300 . ? C8 C9 1.396(9) . ? C8 H8 0.9300 . ? C9 N6 1.305(8) . ? C9 H9 0.9300 . ? C10 C11 1.358(9) . ? C10 N7 1.432(7) . ? C10 H10 0.9300 . ? C11 C12 1.440(8) . ? C11 H11 0.9300 . ? C12 N8 1.248(7) . ? C12 H12 0.9300 . ? C13 C14 1.357(8) . ? C13 N9 1.470(7) . ? C13 H13 0.9300 . ? C14 C15 1.325(9) . ? C14 H14 0.9300 . ? C15 N10 1.404(6) . ? C15 H15 0.9300 . ? C16 C17 1.424(9) . ? C16 N11 1.459(8) . ? C16 H16 0.9300 . ? C17 C18 1.456(8) . ? C17 H17 0.9300 . ? C18 N12 1.382(7) . ? C18 H18 0.9300 . ? C19 N13 1.114(7) . ? C19 Fe1 1.919(8) . ? C20 N14 1.079(6) . ? C20 Fe1 2.085(6) . ? C21 N15 1.132(7) . ? C21 Fe1 2.064(7) . ? C22 N16 1.143(7) . ? C22 Fe2 1.860(7) . ? C23 N17 1.193(8) . ? C23 Fe2 1.953(8) . ? C24 N18 1.229(5) . ? C24 Fe2 1.826(5) . ? C25 N19 1.452(8) . ? C25 C30 1.501(11) . ? C25 C26 1.552(10) . ? C25 H25 0.9800 . ? C26 C27 1.468(9) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.532(10) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.447(10) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.539(9) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 N20 1.466(8) . ? C30 H30 0.9800 . ? C31 N21 1.467(8) . ? C31 C36 1.579(9) . ? C31 C32 1.629(10) . ? C31 H31 0.9800 . ? C32 C33 1.565(9) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.539(8) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.482(9) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.531(11) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 N22 1.433(8) . ? C36 H36 0.9800 . ? C37 N23 1.469(6) . ? C37 C38 1.493(7) . ? C37 C42 1.577(9) . ? C37 H37 0.9800 . ? C38 C39 1.545(8) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.551(9) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.492(7) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.491(8) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 N24 1.479(5) . ? C42 H42 0.9800 . ? C43 N25 1.457(6) . ? C43 C44 1.527(7) . ? C43 C48 1.548(8) . ? C43 H43 0.9800 . ? C44 C45 1.499(9) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.520(8) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.518(8) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.566(9) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 N26 1.482(6) . ? C48 H48 0.9800 . ? C49 N27 1.484(6) . ? C49 C50 1.547(8) . ? C49 C54 1.553(9) . ? C49 H49 0.9800 . ? C50 C51 1.544(7) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.483(8) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.473(8) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.519(8) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 N28 1.465(6) . ? C54 H54 0.9800 . ? C55 N29 1.468(7) . ? C55 C60 1.480(11) . ? C55 C56 1.590(9) . ? C55 H55 0.9800 . ? C56 C57 1.550(9) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.467(9) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.462(8) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C60 1.485(9) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 N30 1.463(7) . ? C60 H60 0.9800 . ? Cl1 O14 1.336(4) . ? Cl1 O12 1.390(6) . ? Cl1 O11 1.445(4) . ? Cl1 O13 1.454(4) . ? Cl2 O24 1.309(4) . ? Cl2 O22 1.390(4) . ? Cl2 O21 1.403(4) . ? Cl2 O23 1.455(4) . ? Cl3 O33 1.304(5) . ? Cl3 O32 1.336(4) . ? Cl3 O34 1.361(4) . ? Cl3 O31 1.439(5) . ? Cl4 O41 1.338(5) . ? Cl4 O43 1.338(4) . ? Cl4 O42 1.364(4) . ? Cl4 O44 1.431(4) . ? Fe1 N1 1.845(6) . ? Fe1 N5 1.886(7) . ? Fe1 N3 1.990(5) . ? Fe2 N9 1.880(5) . ? Fe2 N11 2.093(5) . ? Fe2 N7 2.141(7) . ? N1 N2 1.427(7) . ? N3 N4 1.381(8) . ? N5 N6 1.442(7) . ? N7 N8 1.421(8) . ? N9 N10 1.419(7) . ? N11 N12 1.413(7) . ? N13 Ni3 2.108(7) . ? N14 Ni1 2.041(5) . ? N15 Ni2 2.166(6) . ? N16 Ni2 2.136(5) . ? N17 Ni1 2.007(6) 1_565 ? N18 Ni3 2.110(5) 1_565 ? N19 Ni1 2.410(5) . ? N19 H19A 0.9000 . ? N19 H19B 0.9000 . ? N20 Ni1 2.130(5) . ? N20 H20A 0.9000 . ? N20 H20B 0.9000 . ? N21 Ni1 2.078(5) . ? N21 H21A 0.9000 . ? N21 H21B 0.9000 . ? N22 Ni1 2.164(5) . ? N22 H22A 0.9000 . ? N22 H22B 0.9000 . ? N23 Ni2 2.134(5) . ? N23 H23A 0.9000 . ? N23 H23B 0.9000 . ? N24 Ni2 2.085(5) . ? N24 H24A 0.9000 . ? N24 H24B 0.9000 . ? N25 Ni2 2.120(5) . ? N25 H25A 0.9000 . ? N25 H25B 0.9000 . ? N26 Ni2 2.117(5) . ? N26 H26C 0.9000 . ? N26 H26D 0.9000 . ? N27 Ni3 2.095(5) . ? N27 H27C 0.9000 . ? N27 H27D 0.9000 . ? N28 Ni3 2.239(4) . ? N28 H28C 0.9000 . ? N28 H28D 0.9000 . ? N29 Ni3 2.139(5) . ? N29 H29C 0.9000 . ? N29 H29D 0.9000 . ? N30 Ni3 2.350(5) . ? N30 H30A 0.9000 . ? N30 H30B 0.9000 . ? Ni1 N17 2.007(6) 1_545 ? Ni3 N18 2.110(5) 1_545 ? O1 H1C 0.8511 . ? O1 H1D 0.8510 . ? O2 H2C 0.8513 . ? O2 H2B 0.8510 . ? O3 H3B 0.8495 . ? O3 H3C 0.8512 . ? O4 H4E 0.8505 . ? O4 H4B 0.8506 . ? O5 H5C 0.8511 . ? O5 H5D 0.8517 . ? 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 N2 B1 N4 124.8(6) . . ? N2 B1 N6 116.4(5) . . ? N4 B1 N6 99.1(5) . . ? N2 B1 H11B 104.9 . . ? N4 B1 H11B 104.9 . . ? N6 B1 H11B 104.9 . . ? N10 B2 N12 101.6(5) . . ? N10 B2 N8 116.3(5) . . ? N12 B2 N8 104.1(4) . . ? N10 B2 H22E 111.4 . . ? N12 B2 H22E 111.4 . . ? N8 B2 H22E 111.4 . . ? C2 C1 N1 116.3(5) . . ? C2 C1 H1 121.9 . . ? N1 C1 H1 121.9 . . ? C1 C2 C3 100.6(6) . . ? C1 C2 H2 129.7 . . ? C3 C2 H2 129.7 . . ? N2 C3 C2 109.9(5) . . ? N2 C3 H3 125.0 . . ? C2 C3 H3 125.0 . . ? N3 C4 C5 112.8(6) . . ? N3 C4 H4 123.6 . . ? C5 C4 H4 123.6 . . ? C6 C5 C4 100.3(6) . . ? C6 C5 H5 129.8 . . ? C4 C5 H5 129.8 . . ? N4 C6 C5 111.6(6) . . ? N4 C6 H6 124.2 . . ? C5 C6 H6 124.2 . . ? N5 C7 C8 100.3(6) . . ? N5 C7 H7 129.8 . . ? C8 C7 H7 129.8 . . ? C7 C8 C9 117.1(7) . . ? C7 C8 H8 121.5 . . ? C9 C8 H8 121.5 . . ? N6 C9 C8 102.7(6) . . ? N6 C9 H9 128.7 . . ? C8 C9 H9 128.7 . . ? C11 C10 N7 110.7(5) . . ? C11 C10 H10 124.7 . . ? N7 C10 H10 124.7 . . ? C10 C11 C12 106.6(6) . . ? C10 C11 H11 126.7 . . ? C12 C11 H11 126.7 . . ? N8 C12 C11 106.1(5) . . ? N8 C12 H12 126.9 . . ? C11 C12 H12 126.9 . . ? C14 C13 N9 96.1(5) . . ? C14 C13 H13 131.9 . . ? N9 C13 H13 131.9 . . ? C15 C14 C13 129.8(6) . . ? C15 C14 H14 115.1 . . ? C13 C14 H14 115.1 . . ? C14 C15 N10 92.5(4) . . ? C14 C15 H15 133.8 . . ? N10 C15 H15 133.8 . . ? C17 C16 N11 87.1(5) . . ? C17 C16 H16 136.5 . . ? N11 C16 H16 136.5 . . ? C16 C17 C18 123.3(6) . . ? C16 C17 H17 118.3 . . ? C18 C17 H17 118.3 . . ? N12 C18 C17 94.3(5) . . ? N12 C18 H18 132.8 . . ? C17 C18 H18 132.8 . . ? N13 C19 Fe1 171.5(5) . . ? N14 C20 Fe1 156.3(5) . . ? N15 C21 Fe1 169.6(5) . . ? N16 C22 Fe2 165.8(4) . . ? N17 C23 Fe2 167.7(5) . . ? N18 C24 Fe2 177.3(4) . . ? N19 C25 C30 102.9(6) . . ? N19 C25 C26 102.4(6) . . ? C30 C25 C26 113.4(6) . . ? N19 C25 H25 112.4 . . ? C30 C25 H25 112.4 . . ? C26 C25 H25 112.4 . . ? C27 C26 C25 109.7(6) . . ? C27 C26 H26A 109.7 . . ? C25 C26 H26A 109.7 . . ? C27 C26 H26B 109.7 . . ? C25 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? C26 C27 C28 100.1(5) . . ? C26 C27 H27A 111.8 . . ? C28 C27 H27A 111.8 . . ? C26 C27 H27B 111.8 . . ? C28 C27 H27B 111.8 . . ? H27A C27 H27B 109.5 . . ? C29 C28 C27 121.0(6) . . ? C29 C28 H28A 107.1 . . ? C27 C28 H28A 107.1 . . ? C29 C28 H28B 107.1 . . ? C27 C28 H28B 107.1 . . ? H28A C28 H28B 106.8 . . ? C28 C29 C30 105.6(6) . . ? C28 C29 H29A 110.6 . . ? C30 C29 H29A 110.6 . . ? C28 C29 H29B 110.6 . . ? C30 C29 H29B 110.6 . . ? H29A C29 H29B 108.7 . . ? N20 C30 C25 111.1(5) . . ? N20 C30 C29 114.2(6) . . ? C25 C30 C29 109.8(6) . . ? N20 C30 H30 107.1 . . ? C25 C30 H30 107.1 . . ? C29 C30 H30 107.1 . . ? N21 C31 C36 104.5(5) . . ? N21 C31 C32 104.8(6) . . ? C36 C31 C32 104.8(6) . . ? N21 C31 H31 113.9 . . ? C36 C31 H31 113.9 . . ? C32 C31 H31 113.9 . . ? C33 C32 C31 106.1(6) . . ? C33 C32 H32A 110.5 . . ? C31 C32 H32A 110.5 . . ? C33 C32 H32B 110.5 . . ? C31 C32 H32B 110.5 . . ? H32A C32 H32B 108.7 . . ? C34 C33 C32 115.2(5) . . ? C34 C33 H33A 108.5 . . ? C32 C33 H33A 108.5 . . ? C34 C33 H33B 108.5 . . ? C32 C33 H33B 108.5 . . ? H33A C33 H33B 107.5 . . ? C35 C34 C33 110.4(5) . . ? C35 C34 H34A 109.6 . . ? C33 C34 H34A 109.6 . . ? C35 C34 H34B 109.6 . . ? C33 C34 H34B 109.6 . . ? H34A C34 H34B 108.1 . . ? C34 C35 C36 104.2(6) . . ? C34 C35 H35A 110.9 . . ? C36 C35 H35A 110.9 . . ? C34 C35 H35B 110.9 . . ? C36 C35 H35B 110.9 . . ? H35A C35 H35B 108.9 . . ? N22 C36 C35 109.6(7) . . ? N22 C36 C31 105.2(5) . . ? C35 C36 C31 107.6(5) . . ? N22 C36 H36 111.4 . . ? C35 C36 H36 111.4 . . ? C31 C36 H36 111.4 . . ? N23 C37 C38 111.7(5) . . ? N23 C37 C42 107.9(4) . . ? C38 C37 C42 114.1(5) . . ? N23 C37 H37 107.6 . . ? C38 C37 H37 107.6 . . ? C42 C37 H37 107.6 . . ? C37 C38 C39 107.1(5) . . ? C37 C38 H38A 110.3 . . ? C39 C38 H38A 110.3 . . ? C37 C38 H38B 110.3 . . ? C39 C38 H38B 110.3 . . ? H38A C38 H38B 108.5 . . ? C38 C39 C40 110.5(5) . . ? C38 C39 H39A 109.5 . . ? C40 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 108.1 . . ? C41 C40 C39 109.2(5) . . ? C41 C40 H40A 109.8 . . ? C39 C40 H40A 109.8 . . ? C41 C40 H40B 109.8 . . ? C39 C40 H40B 109.8 . . ? H40A C40 H40B 108.3 . . ? C42 C41 C40 110.0(5) . . ? C42 C41 H41A 109.7 . . ? C40 C41 H41A 109.7 . . ? C42 C41 H41B 109.7 . . ? C40 C41 H41B 109.7 . . ? H41A C41 H41B 108.2 . . ? N24 C42 C41 116.4(4) . . ? N24 C42 C37 106.0(4) . . ? C41 C42 C37 107.0(5) . . ? N24 C42 H42 109.1 . . ? C41 C42 H42 109.1 . . ? C37 C42 H42 109.1 . . ? N25 C43 C44 123.3(5) . . ? N25 C43 C48 103.9(4) . . ? C44 C43 C48 115.8(4) . . ? N25 C43 H43 103.9 . . ? C44 C43 H43 103.9 . . ? C48 C43 H43 103.9 . . ? C45 C44 C43 111.5(5) . . ? C45 C44 H44A 109.3 . . ? C43 C44 H44A 109.3 . . ? C45 C44 H44B 109.3 . . ? C43 C44 H44B 109.3 . . ? H44A C44 H44B 108.0 . . ? C44 C45 C46 111.6(5) . . ? C44 C45 H45A 109.3 . . ? C46 C45 H45A 109.3 . . ? C44 C45 H45B 109.3 . . ? C46 C45 H45B 109.3 . . ? H45A C45 H45B 108.0 . . ? C47 C46 C45 107.5(5) . . ? C47 C46 H46A 110.2 . . ? C45 C46 H46A 110.2 . . ? C47 C46 H46B 110.2 . . ? C45 C46 H46B 110.2 . . ? H46A C46 H46B 108.5 . . ? C46 C47 C48 109.7(5) . . ? C46 C47 H47A 109.7 . . ? C48 C47 H47A 109.7 . . ? C46 C47 H47B 109.7 . . ? C48 C47 H47B 109.7 . . ? H47A C47 H47B 108.2 . . ? N26 C48 C43 113.3(4) . . ? N26 C48 C47 110.6(4) . . ? C43 C48 C47 113.0(4) . . ? N26 C48 H48 106.5 . . ? C43 C48 H48 106.5 . . ? C47 C48 H48 106.5 . . ? N27 C49 C50 109.7(4) . . ? N27 C49 C54 108.2(5) . . ? C50 C49 C54 102.7(5) . . ? N27 C49 H49 111.9 . . ? C50 C49 H49 111.9 . . ? C54 C49 H49 111.9 . . ? C51 C50 C49 105.9(4) . . ? C51 C50 H50A 110.5 . . ? C49 C50 H50A 110.5 . . ? C51 C50 H50B 110.5 . . ? C49 C50 H50B 110.5 . . ? H50A C50 H50B 108.7 . . ? C52 C51 C50 112.8(5) . . ? C52 C51 H51A 109.0 . . ? C50 C51 H51A 109.0 . . ? C52 C51 H51B 109.0 . . ? C50 C51 H51B 109.0 . . ? H51A C51 H51B 107.8 . . ? C53 C52 C51 116.7(5) . . ? C53 C52 H52A 108.1 . . ? C51 C52 H52A 108.1 . . ? C53 C52 H52B 108.1 . . ? C51 C52 H52B 108.1 . . ? H52A C52 H52B 107.3 . . ? C52 C53 C54 106.0(5) . . ? C52 C53 H53A 110.5 . . ? C54 C53 H53A 110.5 . . ? C52 C53 H53B 110.5 . . ? C54 C53 H53B 110.5 . . ? H53A C53 H53B 108.7 . . ? N28 C54 C53 107.4(4) . . ? N28 C54 C49 112.5(4) . . ? C53 C54 C49 116.2(6) . . ? N28 C54 H54 106.8 . . ? C53 C54 H54 106.8 . . ? C49 C54 H54 106.8 . . ? N29 C55 C60 118.4(5) . . ? N29 C55 C56 106.4(5) . . ? C60 C55 C56 106.3(6) . . ? N29 C55 H55 108.5 . . ? C60 C55 H55 108.5 . . ? C56 C55 H55 108.5 . . ? C57 C56 C55 105.1(5) . . ? C57 C56 H56A 110.7 . . ? C55 C56 H56A 110.7 . . ? C57 C56 H56B 110.7 . . ? C55 C56 H56B 110.7 . . ? H56A C56 H56B 108.8 . . ? C58 C57 C56 105.9(5) . . ? C58 C57 H57A 110.5 . . ? C56 C57 H57A 110.5 . . ? C58 C57 H57B 110.5 . . ? C56 C57 H57B 110.5 . . ? H57A C57 H57B 108.7 . . ? C59 C58 C57 107.1(6) . . ? C59 C58 H58A 110.3 . . ? C57 C58 H58A 110.3 . . ? C59 C58 H58B 110.3 . . ? C57 C58 H58B 110.3 . . ? H58A C58 H58B 108.5 . . ? C58 C59 C60 105.3(5) . . ? C58 C59 H59A 110.7 . . ? C60 C59 H59A 110.7 . . ? C58 C59 H59B 110.7 . . ? C60 C59 H59B 110.7 . . ? H59A C59 H59B 108.8 . . ? N30 C60 C55 103.0(5) . . ? N30 C60 C59 111.9(5) . . ? C55 C60 C59 116.7(6) . . ? N30 C60 H60 108.3 . . ? C55 C60 H60 108.3 . . ? C59 C60 H60 108.3 . . ? O14 Cl1 O12 114.3(3) . . ? O14 Cl1 O11 118.9(3) . . ? O12 Cl1 O11 108.7(3) . . ? O14 Cl1 O13 103.4(2) . . ? O12 Cl1 O13 107.6(3) . . ? O11 Cl1 O13 102.5(3) . . ? O24 Cl2 O22 111.4(3) . . ? O24 Cl2 O21 106.7(3) . . ? O22 Cl2 O21 103.2(2) . . ? O24 Cl2 O23 113.0(3) . . ? O22 Cl2 O23 116.0(3) . . ? O21 Cl2 O23 105.5(2) . . ? O33 Cl3 O32 109.1(3) . . ? O33 Cl3 O34 103.6(3) . . ? O32 Cl3 O34 110.9(2) . . ? O33 Cl3 O31 101.4(3) . . ? O32 Cl3 O31 121.9(3) . . ? O34 Cl3 O31 108.1(3) . . ? O41 Cl4 O43 108.1(3) . . ? O41 Cl4 O42 100.9(3) . . ? O43 Cl4 O42 111.8(3) . . ? O41 Cl4 O44 109.1(3) . . ? O43 Cl4 O44 115.3(3) . . ? O42 Cl4 O44 110.6(2) . . ? N1 Fe1 N5 88.0(3) . . ? N1 Fe1 C19 86.1(2) . . ? N5 Fe1 C19 174.15(19) . . ? N1 Fe1 N3 83.8(2) . . ? N5 Fe1 N3 85.5(3) . . ? C19 Fe1 N3 93.8(2) . . ? N1 Fe1 C21 170.65(17) . . ? N5 Fe1 C21 92.2(2) . . ? C19 Fe1 C21 93.6(3) . . ? N3 Fe1 C21 86.87(17) . . ? N1 Fe1 C20 90.23(19) . . ? N5 Fe1 C20 87.43(19) . . ? C19 Fe1 C20 92.6(3) . . ? N3 Fe1 C20 170.94(18) . . ? C21 Fe1 C20 99.1(3) . . ? C24 Fe2 C22 86.8(3) . . ? C24 Fe2 N9 177.1(2) . . ? C22 Fe2 N9 95.91(17) . . ? C24 Fe2 C23 88.8(3) . . ? C22 Fe2 C23 93.9(3) . . ? N9 Fe2 C23 89.96(18) . . ? C24 Fe2 N11 88.31(19) . . ? C22 Fe2 N11 170.6(2) . . ? N9 Fe2 N11 89.2(2) . . ? C23 Fe2 N11 94.0(2) . . ? C24 Fe2 N7 92.1(2) . . ? C22 Fe2 N7 85.2(2) . . ? N9 Fe2 N7 89.2(2) . . ? C23 Fe2 N7 178.68(18) . . ? N11 Fe2 N7 87.0(3) . . ? N2 N1 C1 98.3(4) . . ? N2 N1 Fe1 125.7(5) . . ? C1 N1 Fe1 130.4(3) . . ? B1 N2 C3 140.0(4) . . ? B1 N2 N1 108.7(5) . . ? C3 N2 N1 110.4(4) . . ? C4 N3 N4 101.3(4) . . ? C4 N3 Fe1 131.8(4) . . ? N4 N3 Fe1 123.1(4) . . ? C6 N4 N3 110.5(5) . . ? C6 N4 B1 124.3(5) . . ? N3 N4 B1 107.9(4) . . ? C7 N5 N6 111.2(5) . . ? C7 N5 Fe1 125.8(3) . . ? N6 N5 Fe1 122.9(5) . . ? C9 N6 N5 108.0(5) . . ? C9 N6 B1 139.6(4) . . ? N5 N6 B1 107.8(5) . . ? N8 N7 C10 99.4(5) . . ? N8 N7 Fe2 122.3(5) . . ? C10 N7 Fe2 137.2(4) . . ? C12 N8 N7 117.0(5) . . ? C12 N8 B2 132.0(4) . . ? N7 N8 B2 110.8(5) . . ? N10 N9 C13 104.5(4) . . ? N10 N9 Fe2 124.3(4) . . ? C13 N9 Fe2 131.1(3) . . ? C15 N10 N9 116.9(4) . . ? C15 N10 B2 125.7(4) . . ? N9 N10 B2 117.1(4) . . ? N12 N11 C16 116.6(4) . . ? N12 N11 Fe2 115.9(4) . . ? C16 N11 Fe2 127.2(3) . . ? C18 N12 N11 109.6(4) . . ? C18 N12 B2 128.6(4) . . ? N11 N12 B2 121.4(4) . . ? C19 N13 Ni3 165.1(5) . . ? C20 N14 Ni1 176.4(5) . . ? C21 N15 Ni2 142.2(4) . . ? C22 N16 Ni2 167.2(4) . . ? C23 N17 Ni1 157.3(4) . 1_565 ? C24 N18 Ni3 161.9(4) . 1_565 ? C25 N19 Ni1 101.9(4) . . ? C25 N19 H19A 111.4 . . ? Ni1 N19 H19A 111.4 . . ? C25 N19 H19B 111.4 . . ? Ni1 N19 H19B 111.4 . . ? H19A N19 H19B 109.2 . . ? C30 N20 Ni1 109.6(3) . . ? C30 N20 H20A 109.8 . . ? Ni1 N20 H20A 109.8 . . ? C30 N20 H20B 109.8 . . ? Ni1 N20 H20B 109.8 . . ? H20A N20 H20B 108.2 . . ? C31 N21 Ni1 109.7(3) . . ? C31 N21 H21A 109.7 . . ? Ni1 N21 H21A 109.7 . . ? C31 N21 H21B 109.7 . . ? Ni1 N21 H21B 109.7 . . ? H21A N21 H21B 108.2 . . ? C36 N22 Ni1 108.1(3) . . ? C36 N22 H22A 110.1 . . ? Ni1 N22 H22A 110.1 . . ? C36 N22 H22B 110.1 . . ? Ni1 N22 H22B 110.1 . . ? H22A N22 H22B 108.4 . . ? C37 N23 Ni2 112.0(3) . . ? C37 N23 H23A 109.2 . . ? Ni2 N23 H23A 109.2 . . ? C37 N23 H23B 109.2 . . ? Ni2 N23 H23B 109.2 . . ? H23A N23 H23B 107.9 . . ? C42 N24 Ni2 109.9(3) . . ? C42 N24 H24A 109.7 . . ? Ni2 N24 H24A 109.7 . . ? C42 N24 H24B 109.7 . . ? Ni2 N24 H24B 109.7 . . ? H24A N24 H24B 108.2 . . ? C43 N25 Ni2 110.8(3) . . ? C43 N25 H25A 109.5 . . ? Ni2 N25 H25A 109.5 . . ? C43 N25 H25B 109.5 . . ? Ni2 N25 H25B 109.5 . . ? H25A N25 H25B 108.1 . . ? C48 N26 Ni2 105.2(3) . . ? C48 N26 H26C 110.7 . . ? Ni2 N26 H26C 110.7 . . ? C48 N26 H26D 110.7 . . ? Ni2 N26 H26D 110.7 . . ? H26C N26 H26D 108.8 . . ? C49 N27 Ni3 104.0(2) . . ? C49 N27 H27C 111.0 . . ? Ni3 N27 H27C 111.0 . . ? C49 N27 H27D 111.0 . . ? Ni3 N27 H27D 111.0 . . ? H27C N27 H27D 109.0 . . ? C54 N28 Ni3 105.7(2) . . ? C54 N28 H28C 110.6 . . ? Ni3 N28 H28C 110.6 . . ? C54 N28 H28D 110.6 . . ? Ni3 N28 H28D 110.6 . . ? H28C N28 H28D 108.7 . . ? C55 N29 Ni3 104.4(3) . . ? C55 N29 H29C 110.9 . . ? Ni3 N29 H29C 110.9 . . ? C55 N29 H29D 110.9 . . ? Ni3 N29 H29D 110.9 . . ? H29C N29 H29D 108.9 . . ? C60 N30 Ni3 107.0(3) . . ? C60 N30 H30A 110.3 . . ? Ni3 N30 H30A 110.3 . . ? C60 N30 H30B 110.3 . . ? Ni3 N30 H30B 110.3 . . ? H30A N30 H30B 108.6 . . ? N17 Ni1 N14 87.4(2) 1_545 . ? N17 Ni1 N21 63.3(2) 1_545 . ? N14 Ni1 N21 145.6(2) . . ? N17 Ni1 N20 91.4(2) 1_545 . ? N14 Ni1 N20 82.6(2) . . ? N21 Ni1 N20 113.92(19) . . ? N17 Ni1 N22 117.3(2) 1_545 . ? N14 Ni1 N22 99.7(2) . . ? N21 Ni1 N22 80.2(2) . . ? N20 Ni1 N22 151.3(2) . . ? N17 Ni1 N19 165.51(19) 1_545 . ? N14 Ni1 N19 82.6(2) . . ? N21 Ni1 N19 129.30(19) . . ? N20 Ni1 N19 77.0(2) . . ? N22 Ni1 N19 74.9(2) . . ? N24 Ni2 N26 172.0(2) . . ? N24 Ni2 N25 103.9(2) . . ? N26 Ni2 N25 82.7(2) . . ? N24 Ni2 N23 80.43(19) . . ? N26 Ni2 N23 92.6(2) . . ? N25 Ni2 N23 173.6(3) . . ? N24 Ni2 N16 72.74(19) . . ? N26 Ni2 N16 103.2(2) . . ? N25 Ni2 N16 88.9(2) . . ? N23 Ni2 N16 87.96(18) . . ? N24 Ni2 N15 98.2(2) . . ? N26 Ni2 N15 85.1(2) . . ? N25 Ni2 N15 98.6(2) . . ? N23 Ni2 N15 85.29(18) . . ? N16 Ni2 N15 169.51(19) . . ? N27 Ni3 N13 81.9(2) . . ? N27 Ni3 N18 92.0(2) . 1_545 ? N13 Ni3 N18 94.0(2) . 1_545 ? N27 Ni3 N29 155.31(18) . . ? N13 Ni3 N29 98.9(2) . . ? N18 Ni3 N29 63.3(2) 1_545 . ? N27 Ni3 N28 82.51(18) . . ? N13 Ni3 N28 71.3(2) . . ? N18 Ni3 N28 164.9(2) 1_545 . ? N29 Ni3 N28 121.33(19) . . ? N27 Ni3 N30 113.4(2) . . ? N13 Ni3 N30 146.21(18) . . ? N18 Ni3 N30 114.4(2) 1_545 . ? N29 Ni3 N30 79.5(2) . . ? N28 Ni3 N30 80.67(18) . . ? H1C O1 H1D 109.4 . . ? H2C O2 H2B 109.5 . . ? H3B O3 H3C 109.4 . . ? H4E O4 H4B 109.3 . . ? H5C O5 H5D 109.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -22.4(8) . . . . ? C1 C2 C3 N2 18.4(7) . . . . ? N3 C4 C5 C6 -13.7(7) . . . . ? C4 C5 C6 N4 18.8(8) . . . . ? N5 C7 C8 C9 -8.0(8) . . . . ? C7 C8 C9 N6 4.8(8) . . . . ? N7 C10 C11 C12 -3.2(7) . . . . ? C10 C11 C12 N8 1.1(7) . . . . ? N9 C13 C14 C15 5.2(9) . . . . ? C13 C14 C15 N10 -4.6(9) . . . . ? N11 C16 C17 C18 -32.0(8) . . . . ? C16 C17 C18 N12 30.3(9) . . . . ? N19 C25 C26 C27 173.1(5) . . . . ? C30 C25 C26 C27 62.9(8) . . . . ? C25 C26 C27 C28 -59.5(6) . . . . ? C26 C27 C28 C29 67.1(7) . . . . ? C27 C28 C29 C30 -61.1(7) . . . . ? N19 C25 C30 N20 69.1(7) . . . . ? C26 C25 C30 N20 178.9(5) . . . . ? N19 C25 C30 C29 -163.5(5) . . . . ? C26 C25 C30 C29 -53.7(8) . . . . ? C28 C29 C30 N20 174.4(5) . . . . ? C28 C29 C30 C25 48.7(7) . . . . ? N21 C31 C32 C33 166.2(4) . . . . ? C36 C31 C32 C33 56.5(7) . . . . ? C31 C32 C33 C34 -51.4(7) . . . . ? C32 C33 C34 C35 56.7(8) . . . . ? C33 C34 C35 C36 -63.9(6) . . . . ? C34 C35 C36 N22 -171.6(4) . . . . ? C34 C35 C36 C31 74.4(7) . . . . ? N21 C31 C36 N22 61.9(7) . . . . ? C32 C31 C36 N22 171.9(5) . . . . ? N21 C31 C36 C35 178.8(5) . . . . ? C32 C31 C36 C35 -71.3(8) . . . . ? N23 C37 C38 C39 179.0(5) . . . . ? C42 C37 C38 C39 56.3(7) . . . . ? C37 C38 C39 C40 -56.1(7) . . . . ? C38 C39 C40 C41 61.0(6) . . . . ? C39 C40 C41 C42 -63.8(7) . . . . ? C40 C41 C42 N24 178.8(5) . . . . ? C40 C41 C42 C37 60.5(7) . . . . ? N23 C37 C42 N24 51.2(5) . . . . ? C38 C37 C42 N24 175.9(5) . . . . ? N23 C37 C42 C41 176.1(4) . . . . ? C38 C37 C42 C41 -59.2(7) . . . . ? N25 C43 C44 C45 171.8(5) . . . . ? C48 C43 C44 C45 42.3(8) . . . . ? C43 C44 C45 C46 -56.3(7) . . . . ? C44 C45 C46 C47 67.6(6) . . . . ? C45 C46 C47 C48 -62.5(7) . . . . ? N25 C43 C48 N26 55.3(5) . . . . ? C44 C43 C48 N26 -166.3(5) . . . . ? N25 C43 C48 C47 -177.9(4) . . . . ? C44 C43 C48 C47 -39.5(8) . . . . ? C46 C47 C48 N26 177.8(4) . . . . ? C46 C47 C48 C43 49.6(7) . . . . ? N27 C49 C50 C51 177.8(5) . . . . ? C54 C49 C50 C51 62.9(6) . . . . ? C49 C50 C51 C52 -60.7(7) . . . . ? C50 C51 C52 C53 53.8(8) . . . . ? C51 C52 C53 C54 -47.2(8) . . . . ? C52 C53 C54 N28 -176.9(5) . . . . ? C52 C53 C54 C49 56.2(8) . . . . ? N27 C49 C54 N28 53.2(6) . . . . ? C50 C49 C54 N28 169.2(5) . . . . ? N27 C49 C54 C53 177.5(5) . . . . ? C50 C49 C54 C53 -66.5(7) . . . . ? N29 C55 C56 C57 -177.3(5) . . . . ? C60 C55 C56 C57 55.7(6) . . . . ? C55 C56 C57 C58 -67.6(6) . . . . ? C56 C57 C58 C59 75.1(6) . . . . ? C57 C58 C59 C60 -66.8(6) . . . . ? N29 C55 C60 N30 62.3(6) . . . . ? C56 C55 C60 N30 -178.3(4) . . . . ? N29 C55 C60 C59 -174.7(5) . . . . ? C56 C55 C60 C59 -55.2(7) . . . . ? C58 C59 C60 N30 178.2(5) . . . . ? C58 C59 C60 C55 59.9(7) . . . . ? N15 C21 Fe1 N5 84(3) . . . . ? N15 C21 Fe1 C19 -97(3) . . . . ? N15 C21 Fe1 N3 169(3) . . . . ? N15 C21 Fe1 C20 -4(3) . . . . ? N14 C20 Fe1 N1 123.1(14) . . . . ? N14 C20 Fe1 N5 -148.9(14) . . . . ? N14 C20 Fe1 C19 37.0(14) . . . . ? N14 C20 Fe1 C21 -57.0(14) . . . . ? N16 C22 Fe2 C24 -179(3) . . . . ? N16 C22 Fe2 N9 0(3) . . . . ? N16 C22 Fe2 N7 88(3) . . . . ? N17 C23 Fe2 C24 -45(3) . . . . ? N17 C23 Fe2 C22 -132(3) . . . . ? N17 C23 Fe2 N9 132(3) . . . . ? C2 C1 N1 N2 17.2(7) . . . . ? C2 C1 N1 Fe1 171.1(4) . . . . ? N5 Fe1 N1 N2 35.9(5) . . . . ? C19 Fe1 N1 N2 -144.1(5) . . . . ? C20 Fe1 N1 N2 123.3(5) . . . . ? N5 Fe1 N1 C1 -111.7(5) . . . . ? C19 Fe1 N1 C1 68.3(5) . . . . ? C20 Fe1 N1 C1 -24.3(5) . . . . ? N4 B1 N2 C3 -138.0(6) . . . . ? N6 B1 N2 C3 97.9(8) . . . . ? N4 B1 N2 N1 54.8(7) . . . . ? N6 B1 N2 N1 -69.3(5) . . . . ? C2 C3 N2 B1 -176.2(6) . . . . ? C2 C3 N2 N1 -9.1(6) . . . . ? C1 N1 N2 B1 167.6(5) . . . . ? Fe1 N1 N2 B1 12.0(7) . . . . ? C1 N1 N2 C3 -3.7(6) . . . . ? Fe1 N1 N2 C3 -159.3(4) . . . . ? C5 C4 N3 N4 4.5(6) . . . . ? C5 C4 N3 Fe1 162.1(4) . . . . ? N1 Fe1 N3 C4 -103.8(6) . . . . ? N5 Fe1 N3 C4 167.8(6) . . . . ? C19 Fe1 N3 C4 -18.1(5) . . . . ? N1 Fe1 N3 N4 49.8(6) . . . . ? N5 Fe1 N3 N4 -38.6(6) . . . . ? C19 Fe1 N3 N4 135.5(6) . . . . ? C5 C6 N4 N3 -17.7(7) . . . . ? C5 C6 N4 B1 -148.5(6) . . . . ? C4 N3 N4 C6 7.8(6) . . . . ? Fe1 N3 N4 C6 -152.4(4) . . . . ? C4 N3 N4 B1 146.8(4) . . . . ? Fe1 N3 N4 B1 -13.5(8) . . . . ? N2 B1 N4 C6 79.1(8) . . . . ? N6 B1 N4 C6 -149.6(5) . . . . ? N2 B1 N4 N3 -52.7(7) . . . . ? N6 B1 N4 N3 78.6(5) . . . . ? C8 C7 N5 N6 7.8(6) . . . . ? C8 C7 N5 Fe1 -171.1(4) . . . . ? N3 Fe1 N5 N6 37.1(5) . . . . ? C21 Fe1 N5 N6 123.8(5) . . . . ? C20 Fe1 N5 N6 -137.1(5) . . . . ? C8 C9 N6 N5 0.6(5) . . . . ? C8 C9 N6 B1 151.9(5) . . . . ? C7 N5 N6 C9 -5.7(6) . . . . ? Fe1 N5 N6 C9 173.3(3) . . . . ? C7 N5 N6 B1 -166.6(5) . . . . ? Fe1 N5 N6 B1 12.4(6) . . . . ? N2 B1 N6 C9 -94.4(7) . . . . ? N4 B1 N6 C9 129.1(5) . . . . ? N2 B1 N6 N5 56.9(6) . . . . ? N4 B1 N6 N5 -79.6(4) . . . . ? C11 C10 N7 N8 3.9(5) . . . . ? C11 C10 N7 Fe2 172.1(4) . . . . ? C24 Fe2 N7 N8 128.9(5) . . . . ? C22 Fe2 N7 N8 -144.5(5) . . . . ? N9 Fe2 N7 N8 -48.5(5) . . . . ? N11 Fe2 N7 N8 40.7(5) . . . . ? C24 Fe2 N7 C10 -37.3(6) . . . . ? N9 Fe2 N7 C10 145.3(6) . . . . ? N11 Fe2 N7 C10 -125.5(6) . . . . ? C11 C12 N8 N7 1.6(5) . . . . ? C11 C12 N8 B2 176.3(4) . . . . ? Fe2 N7 N8 C12 -174.0(3) . . . . ? C10 N7 N8 B2 -179.2(3) . . . . ? Fe2 N7 N8 B2 10.2(6) . . . . ? N10 B2 N8 C12 -130.9(5) . . . . ? N12 B2 N8 C12 118.2(5) . . . . ? N10 B2 N8 N7 44.0(5) . . . . ? C14 C13 N9 N10 -2.8(5) . . . . ? C14 C13 N9 Fe2 -179.1(4) . . . . ? C22 Fe2 N9 N10 132.9(5) . . . . ? C23 Fe2 N9 N10 -133.2(5) . . . . ? N7 Fe2 N9 N10 47.8(5) . . . . ? C22 Fe2 N9 C13 -51.4(5) . . . . ? C23 Fe2 N9 C13 42.5(4) . . . . ? N11 Fe2 N9 C13 136.5(5) . . . . ? N7 Fe2 N9 C13 -136.5(5) . . . . ? C14 C15 N10 N9 1.5(6) . . . . ? C14 C15 N10 B2 -171.5(5) . . . . ? C13 N9 N10 C15 0.9(6) . . . . ? Fe2 N9 N10 C15 177.5(3) . . . . ? C13 N9 N10 B2 174.6(4) . . . . ? Fe2 N9 N10 B2 -8.8(7) . . . . ? N12 B2 N10 C15 -123.2(5) . . . . ? N8 B2 N10 C15 124.4(5) . . . . ? N12 B2 N10 N9 63.7(5) . . . . ? N8 B2 N10 N9 -48.6(5) . . . . ? C17 C16 N11 N12 20.8(5) . . . . ? C17 C16 N11 Fe2 -166.7(4) . . . . ? C24 Fe2 N11 N12 -141.8(4) . . . . ? N9 Fe2 N11 N12 39.6(5) . . . . ? C23 Fe2 N11 N12 129.6(4) . . . . ? N7 Fe2 N11 N12 -49.6(4) . . . . ? C24 Fe2 N11 C16 45.7(5) . . . . ? N9 Fe2 N11 C16 -132.9(4) . . . . ? C23 Fe2 N11 C16 -43.0(4) . . . . ? N7 Fe2 N11 C16 137.9(4) . . . . ? C17 C18 N12 N11 -10.6(5) . . . . ? C17 C18 N12 B2 162.5(4) . . . . ? C16 N11 N12 C18 -7.3(6) . . . . ? Fe2 N11 N12 C18 179.3(3) . . . . ? C16 N11 N12 B2 179.1(5) . . . . ? Fe2 N11 N12 B2 5.7(6) . . . . ? N10 B2 N12 C18 126.7(5) . . . . ? N8 B2 N12 C18 -112.1(5) . . . . ? N10 B2 N12 N11 -61.0(5) . . . . ? N8 B2 N12 N11 60.2(5) . . . . ? Fe1 C21 N15 Ni2 -129(3) . . . . ? Fe2 C22 N16 Ni2 -64(4) . . . . ? Fe2 C23 N17 Ni1 -100(3) . . . 1_565 ? C30 C25 N19 Ni1 -53.0(5) . . . . ? C26 C25 N19 Ni1 -170.9(4) . . . . ? C25 C30 N20 Ni1 -44.3(6) . . . . ? C29 C30 N20 Ni1 -169.2(4) . . . . ? C42 C37 N23 Ni2 -30.6(5) . . . . ? C41 C42 N24 Ni2 -167.0(5) . . . . ? C37 C42 N24 Ni2 -48.2(4) . . . . ? C44 C43 N25 Ni2 -174.8(4) . . . . ? C48 C43 N25 Ni2 -40.5(4) . . . . ? C43 C48 N26 Ni2 -40.6(5) . . . . ? C47 C48 N26 Ni2 -168.6(4) . . . . ? C50 C49 N27 Ni3 -165.6(4) . . . . ? C54 C49 N27 Ni3 -54.3(5) . . . . ? C53 C54 N28 Ni3 -151.5(4) . . . . ? C49 C54 N28 Ni3 -22.5(5) . . . . ? C60 C55 N29 Ni3 -47.7(5) . . . . ? C56 C55 N29 Ni3 -167.1(4) . . . . ? C55 C60 N30 Ni3 -39.6(4) . . . . ? C59 C60 N30 Ni3 -165.8(4) . . . . ? C31 N21 Ni1 N17 146.1(3) . . . 1_545 ? C31 N21 Ni1 N14 111.5(4) . . . . ? C31 N21 Ni1 N20 -135.1(3) . . . . ? C31 N21 Ni1 N22 18.6(3) . . . . ? C31 N21 Ni1 N19 -42.5(4) . . . . ? C30 N20 Ni1 N17 -162.2(3) . . . 1_545 ? C30 N20 Ni1 N14 -75.0(3) . . . . ? C30 N20 Ni1 N21 136.6(3) . . . . ? C30 N20 Ni1 N22 21.5(5) . . . . ? C30 N20 Ni1 N19 9.1(3) . . . . ? C36 N22 Ni1 N17 -36.3(3) . . . 1_545 ? C36 N22 Ni1 N14 -128.4(3) . . . . ? C36 N22 Ni1 N21 16.7(3) . . . . ? C36 N22 Ni1 N20 139.5(3) . . . . ? C36 N22 Ni1 N19 152.1(3) . . . . ? C25 N19 Ni1 N17 62.9(8) . . . 1_545 ? C25 N19 Ni1 N14 109.7(3) . . . . ? C25 N19 Ni1 N21 -84.8(3) . . . . ? C25 N19 Ni1 N20 25.6(3) . . . . ? C25 N19 Ni1 N22 -148.2(3) . . . . ? C42 N24 Ni2 N25 -159.3(3) . . . . ? C42 N24 Ni2 N23 25.5(3) . . . . ? C42 N24 Ni2 N16 116.3(3) . . . . ? C42 N24 Ni2 N15 -58.3(3) . . . . ? C48 N26 Ni2 N25 12.6(3) . . . . ? C48 N26 Ni2 N23 -171.8(3) . . . . ? C48 N26 Ni2 N16 99.7(3) . . . . ? C48 N26 Ni2 N15 -86.7(3) . . . . ? C43 N25 Ni2 N24 -158.4(3) . . . . ? C43 N25 Ni2 N26 17.0(3) . . . . ? C43 N25 Ni2 N16 -86.5(3) . . . . ? C43 N25 Ni2 N15 100.9(4) . . . . ? C37 N23 Ni2 N24 4.1(3) . . . . ? C37 N23 Ni2 N26 -171.9(3) . . . . ? C37 N23 Ni2 N16 -68.7(3) . . . . ? C37 N23 Ni2 N15 103.2(3) . . . . ? C22 N16 Ni2 N24 -17.9(15) . . . . ? C22 N16 Ni2 N26 154.9(15) . . . . ? C22 N16 Ni2 N25 -122.8(16) . . . . ? C22 N16 Ni2 N23 62.7(16) . . . . ? C22 N16 Ni2 N15 13(3) . . . . ? C21 N15 Ni2 N24 -138.7(7) . . . . ? C21 N15 Ni2 N26 48.7(7) . . . . ? C21 N15 Ni2 N25 -33.2(7) . . . . ? C21 N15 Ni2 N23 141.7(7) . . . . ? C21 N15 Ni2 N16 -168.2(8) . . . . ? C49 N27 Ni3 N13 104.9(3) . . . . ? C49 N27 Ni3 N18 -161.3(3) . . . 1_545 ? C49 N27 Ni3 N29 -161.3(5) . . . . ? C49 N27 Ni3 N28 32.8(3) . . . . ? C49 N27 Ni3 N30 -43.6(3) . . . . ? C19 N13 Ni3 N27 -3.5(15) . . . . ? C19 N13 Ni3 N18 -94.9(15) . . . 1_545 ? C19 N13 Ni3 N29 -158.6(15) . . . . ? C19 N13 Ni3 N28 81.3(15) . . . . ? C19 N13 Ni3 N30 117.0(15) . . . . ? C55 N29 Ni3 N27 138.4(4) . . . . ? C55 N29 Ni3 N13 -131.7(3) . . . . ? C55 N29 Ni3 N18 138.3(4) . . . 1_545 ? C55 N29 Ni3 N28 -58.1(4) . . . . ? C55 N29 Ni3 N30 14.1(3) . . . . ? C54 N28 Ni3 N27 -5.8(3) . . . . ? C54 N28 Ni3 N13 -89.7(3) . . . . ? C54 N28 Ni3 N18 -75.1(9) . . . 1_545 ? C54 N28 Ni3 N29 -178.9(3) . . . . ? C54 N28 Ni3 N30 109.5(3) . . . . ? C60 N30 Ni3 N27 -142.6(3) . . . . ? C60 N30 Ni3 N13 105.8(4) . . . . ? C60 N30 Ni3 N18 -38.8(3) . . . 1_545 ? C60 N30 Ni3 N29 15.3(3) . . . . ? C60 N30 Ni3 N28 139.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.635 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.071 # Attachment '737796-revised.cif' data_xx _database_code_depnum_ccdc_archive 'CCDC 737796' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H104 B2 Fe2 N30 Ni3, 4(Cl O4), 2(H2 O)' _chemical_formula_sum 'C60 H108 B2 Cl4 Fe2 N30 Ni3 O18' _chemical_formula_weight 1989.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 Triclinic _symmetry_space_group_name_H-M P1 _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 14.000(2) _cell_length_b 14.1403(11) _cell_length_c 14.868(3) _cell_angle_alpha 116.613(4) _cell_angle_beta 103.801(3) _cell_angle_gamma 99.856(3) _cell_volume 2421.0(6) _cell_formula_units_Z 1 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1653 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 24.59 _exptl_crystal_description plate _exptl_crystal_colour Red-brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 1.047 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.78 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13128 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11107 _reflns_number_gt 9136 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.06P)^2^+1.99P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.018(15) _chemical_absolute_configuration unk _refine_ls_number_reflns 11107 _refine_ls_number_parameters 1099 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1181 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.000 _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 B1 B 0.9372(7) 0.8491(8) 0.7752(7) 0.035(2) Uani 1 1 d . . . H11B H 1.0107 0.8906 0.8196 0.043 Uiso 1 1 calc R . . B2 B 0.0963(7) 1.0372(7) 0.2737(7) 0.0339(19) Uani 1 1 d . . . H22E H 0.0242 0.9916 0.2264 0.041 Uiso 1 1 calc R . . C1 C 0.8313(6) 0.5684(7) 0.6754(7) 0.047(2) Uani 1 1 d . . . H1 H 0.7761 0.5027 0.6278 0.057 Uiso 1 1 calc R . . C2 C 0.9198(6) 0.5665(7) 0.7226(6) 0.0363(18) Uani 1 1 d . . . H2 H 0.9357 0.5066 0.7257 0.044 Uiso 1 1 calc R . . C3 C 0.9930(6) 0.6840(7) 0.7722(7) 0.046(2) Uani 1 1 d . . . H3 H 1.0651 0.7098 0.8024 0.055 Uiso 1 1 calc R . . C4 C 0.7369(5) 0.9073(6) 0.8611(6) 0.0366(18) Uani 1 1 d . . . H4 H 0.6658 0.8853 0.8466 0.044 Uiso 1 1 calc R . . C5 C 0.8035(5) 0.9866(6) 0.9626(5) 0.0256(14) Uani 1 1 d . . . H5 H 0.7904 1.0255 1.0255 0.031 Uiso 1 1 calc R . . C6 C 0.8992(5) 0.9922(6) 0.9438(6) 0.0363(19) Uani 1 1 d . . . H6 H 0.9643 1.0354 0.9974 0.044 Uiso 1 1 calc R . . C7 C 0.8110(6) 0.7838(7) 0.5077(6) 0.044(2) Uani 1 1 d . . . H7 H 0.7526 0.7487 0.4451 0.053 Uiso 1 1 calc R . . C8 C 0.9104(6) 0.8405(6) 0.5268(6) 0.0339(17) Uani 1 1 d . . . H8 H 0.9292 0.8429 0.4718 0.041 Uiso 1 1 calc R . . C9 C 0.9825(6) 0.8944(7) 0.6321(7) 0.0379(18) Uani 1 1 d . . . H9 H 1.0518 0.9377 0.6604 0.045 Uiso 1 1 calc R . . C10 C 0.2118(6) 1.1055(8) 0.5557(7) 0.049(2) Uani 1 1 d . . . H10 H 0.2645 1.1387 0.6225 0.059 Uiso 1 1 calc R . . C11 C 0.1080(6) 1.0478(7) 0.5303(6) 0.0386(18) Uani 1 1 d . . . H11 H 0.0811 1.0305 0.5746 0.046 Uiso 1 1 calc R . . C12 C 0.0524(6) 1.0212(7) 0.4252(6) 0.0377(19) Uani 1 1 d . . . H12 H -0.0187 0.9862 0.3881 0.045 Uiso 1 1 calc R . . C13 C 0.3321(6) 0.9864(7) 0.2160(6) 0.0385(18) Uani 1 1 d . . . H13 H 0.4019 0.9952 0.2264 0.046 Uiso 1 1 calc R . . C14 C 0.2412(6) 0.9093(6) 0.1298(6) 0.0350(17) Uani 1 1 d . . . H14 H 0.2495 0.8546 0.0701 0.042 Uiso 1 1 calc R . . C15 C 0.1391(6) 0.9050(7) 0.1228(6) 0.0358(17) Uani 1 1 d . . . H15 H 0.0738 0.8577 0.0715 0.043 Uiso 1 1 calc R . . C16 C 0.2279(6) 1.3506(7) 0.3818(6) 0.0343(17) Uani 1 1 d . . . H16 H 0.2851 1.4145 0.4151 0.041 Uiso 1 1 calc R . . C17 C 0.1154(6) 1.3288(7) 0.3258(7) 0.046(2) Uani 1 1 d . . . H17 H 0.0862 1.3832 0.3259 0.056 Uiso 1 1 calc R . . C18 C 0.0607(6) 1.2150(7) 0.2735(6) 0.0378(18) Uani 1 1 d . . . H18 H -0.0080 1.1821 0.2264 0.045 Uiso 1 1 calc R . . C19 C 0.7258(5) 0.5619(6) 0.8810(6) 0.0336(15) Uani 1 1 d . . . H19 H 0.7506 0.5995 0.8453 0.040 Uiso 1 1 calc R . . C20 C 0.8082(5) 0.5146(6) 0.9136(6) 0.0386(17) Uani 1 1 d . . . H20A H 0.7911 0.4808 0.9543 0.046 Uiso 1 1 calc R . . H20B H 0.8202 0.4608 0.8519 0.046 Uiso 1 1 calc R . . C21 C 0.8990(5) 0.6211(7) 0.9829(7) 0.051(2) Uani 1 1 d . . . H21A H 0.9076 0.6580 0.9425 0.062 Uiso 1 1 calc R . . H21B H 0.9621 0.6038 1.0031 0.062 Uiso 1 1 calc R . . C22 C 0.8807(5) 0.6992(6) 1.0850(6) 0.0341(15) Uani 1 1 d . . . H22A H 0.8651 0.6590 1.1209 0.041 Uiso 1 1 calc R . . H22B H 0.9438 0.7617 1.1339 0.041 Uiso 1 1 calc R . . C23 C 0.7929(5) 0.7429(6) 1.0601(6) 0.0385(17) Uani 1 1 d . . . H23A H 0.8135 0.7954 1.0377 0.046 Uiso 1 1 calc R . . H23B H 0.7764 0.7816 1.1242 0.046 Uiso 1 1 calc R . . C24 C 0.6967(5) 0.6447(6) 0.9697(5) 0.0336(15) Uani 1 1 d . . . H24 H 0.6679 0.6050 1.0018 0.040 Uiso 1 1 calc R . . C25 C 0.3733(6) 0.6020(7) 0.9133(6) 0.0410(18) Uani 1 1 d . . . H25 H 0.3995 0.6803 0.9338 0.049 Uiso 1 1 calc R . . C26 C 0.3236(6) 0.5815(8) 0.9882(6) 0.050(2) Uani 1 1 d . . . H26A H 0.3140 0.5055 0.9728 0.060 Uiso 1 1 calc R . . H26B H 0.3681 0.6321 1.0630 0.060 Uiso 1 1 calc R . . C27 C 0.2219(6) 0.6010(8) 0.9681(7) 0.053(2) Uani 1 1 d . . . H27A H 0.2350 0.6795 0.9914 0.064 Uiso 1 1 calc R . . H27B H 0.1900 0.5870 1.0141 0.064 Uiso 1 1 calc R . . C28 C 0.1424(6) 0.5333(6) 0.8532(7) 0.0384(18) Uani 1 1 d . . . H28A H 0.1131 0.4568 0.8347 0.046 Uiso 1 1 calc R . . H28B H 0.0864 0.5648 0.8480 0.046 Uiso 1 1 calc R . . C29 C 0.1945(6) 0.5354(7) 0.7763(7) 0.0438(18) Uani 1 1 d . . . H29A H 0.1995 0.6053 0.7775 0.053 Uiso 1 1 calc R . . H29B H 0.1502 0.4756 0.7041 0.053 Uiso 1 1 calc R . . C30 C 0.3016(5) 0.5235(7) 0.7975(6) 0.0393(18) Uani 1 1 d . . . H30 H 0.2932 0.4473 0.7835 0.047 Uiso 1 1 calc R . . C31 C 0.7307(6) 1.1108(8) 0.7030(6) 0.048(2) Uani 1 1 d . . . H31 H 0.7425 1.0566 0.7248 0.058 Uiso 1 1 calc R . . C32 C 0.8180(6) 1.2168(7) 0.7825(6) 0.0381(18) Uani 1 1 d . . . H32A H 0.8161 1.2415 0.8542 0.046 Uiso 1 1 calc R . . H32B H 0.8096 1.2743 0.7656 0.046 Uiso 1 1 calc R . . C33 C 0.9248(5) 1.2006(6) 0.7812(6) 0.0387(18) Uani 1 1 d . . . H33A H 0.9805 1.2704 0.8318 0.046 Uiso 1 1 calc R . . H33B H 0.9356 1.1454 0.8009 0.046 Uiso 1 1 calc R . . C34 C 0.9226(6) 1.1613(7) 0.6676(6) 0.0414(19) Uani 1 1 d . . . H34A H 0.9899 1.1554 0.6645 0.050 Uiso 1 1 calc R . . H34B H 0.9087 1.2157 0.6479 0.050 Uiso 1 1 calc R . . C35 C 0.8392(5) 1.0482(7) 0.5878(6) 0.0420(19) Uani 1 1 d . . . H35A H 0.8516 0.9936 0.6078 0.050 Uiso 1 1 calc R . . H35B H 0.8408 1.0224 0.5159 0.050 Uiso 1 1 calc R . . C36 C 0.7324(5) 1.0619(7) 0.5898(6) 0.0355(17) Uani 1 1 d . . . H36 H 0.7073 1.1002 0.5528 0.043 Uiso 1 1 calc R . . C37 C 0.2941(5) 0.8542(7) 0.4486(5) 0.042(2) Uani 1 1 d . . . H37 H 0.2736 0.9107 0.4348 0.050 Uiso 1 1 calc R . . C38 C 0.2070(5) 0.7856(5) 0.4600(5) 0.0283(14) Uani 1 1 d . . . H38A H 0.2248 0.7260 0.4684 0.034 Uiso 1 1 calc R . . H38B H 0.1881 0.8316 0.5200 0.034 Uiso 1 1 calc R . . C39 C 0.1217(5) 0.7407(6) 0.3527(6) 0.0363(17) Uani 1 1 d . . . H39A H 0.1168 0.8022 0.3411 0.044 Uiso 1 1 calc R . . H39B H 0.0561 0.7097 0.3561 0.044 Uiso 1 1 calc R . . C40 C 0.1380(5) 0.6514(5) 0.2571(5) 0.0307(15) Uani 1 1 d . . . H40A H 0.0819 0.6280 0.1911 0.037 Uiso 1 1 calc R . . H40B H 0.1377 0.5868 0.2648 0.037 Uiso 1 1 calc R . . C41 C 0.2424(5) 0.6983(6) 0.2510(5) 0.0315(16) Uani 1 1 d . . . H41A H 0.2319 0.7367 0.2112 0.038 Uiso 1 1 calc R . . H41B H 0.2653 0.6365 0.2111 0.038 Uiso 1 1 calc R . . C42 C 0.3287(5) 0.7794(7) 0.3618(6) 0.0333(17) Uani 1 1 d . . . H42 H 0.3448 0.7280 0.3861 0.040 Uiso 1 1 calc R . . C43 C 0.7251(5) 0.3241(7) 0.2218(6) 0.0410(18) Uani 1 1 d . . . H43 H 0.6734 0.2870 0.1488 0.049 Uiso 1 1 calc R . . C44 C 0.8183(5) 0.2775(6) 0.2127(6) 0.0354(16) Uani 1 1 d . . . H44A H 0.8592 0.2925 0.2830 0.042 Uiso 1 1 calc R . . H44B H 0.7916 0.1972 0.1644 0.042 Uiso 1 1 calc R . . C45 C 0.8881(6) 0.3297(7) 0.1709(6) 0.043(2) Uani 1 1 d . . . H45A H 0.8523 0.3014 0.0950 0.051 Uiso 1 1 calc R . . H45B H 0.9509 0.3091 0.1784 0.051 Uiso 1 1 calc R . . C46 C 0.9167(5) 0.4578(6) 0.2340(6) 0.0348(16) Uani 1 1 d . . . H46A H 0.9546 0.4864 0.3095 0.042 Uiso 1 1 calc R . . H46B H 0.9612 0.4897 0.2069 0.042 Uiso 1 1 calc R . . C47 C 0.8186(6) 0.4927(7) 0.2227(6) 0.0432(18) Uani 1 1 d . . . H47A H 0.7807 0.4633 0.1470 0.052 Uiso 1 1 calc R . . H47B H 0.8386 0.5735 0.2591 0.052 Uiso 1 1 calc R . . C48 C 0.7469(5) 0.4508(6) 0.2700(6) 0.0370(16) Uani 1 1 d . . . H48 H 0.7826 0.4881 0.3481 0.044 Uiso 1 1 calc R . . C49 C 0.3148(5) 0.2601(7) 0.1520(6) 0.0417(18) Uani 1 1 d . . . H49 H 0.2980 0.2885 0.2177 0.050 Uiso 1 1 calc R . . C50 C 0.2177(5) 0.1739(7) 0.0592(6) 0.0433(19) Uani 1 1 d . . . H50A H 0.1908 0.1160 0.0733 0.052 Uiso 1 1 calc R . . H50B H 0.2327 0.1395 -0.0064 0.052 Uiso 1 1 calc R . . C51 C 0.1383(6) 0.2326(7) 0.0469(6) 0.047(2) Uani 1 1 d . . . H51A H 0.0763 0.1774 -0.0138 0.056 Uiso 1 1 calc R . . H51B H 0.1197 0.2590 0.1107 0.056 Uiso 1 1 calc R . . C52 C 0.1686(5) 0.3304(7) 0.0303(6) 0.046(2) Uani 1 1 d . . . H52A H 0.1141 0.3645 0.0293 0.055 Uiso 1 1 calc R . . H52B H 0.1797 0.3055 -0.0375 0.055 Uiso 1 1 calc R . . C53 C 0.2693(6) 0.4147(7) 0.1249(7) 0.0441(19) Uani 1 1 d . . . H53A H 0.2958 0.4745 0.1131 0.053 Uiso 1 1 calc R . . H53B H 0.2550 0.4471 0.1911 0.053 Uiso 1 1 calc R . . C54 C 0.3491(5) 0.3584(6) 0.1355(6) 0.0349(16) Uani 1 1 d . . . H54 H 0.3664 0.3309 0.0701 0.042 Uiso 1 1 calc R . . C55 C 0.6199(5) 0.6474(8) 0.6762(6) 0.0398(19) Uani 1 1 d . . . C56 C 0.6820(5) 0.5811(6) 0.4936(6) 0.0371(18) Uani 1 1 d . . . C57 C 0.6144(6) 0.7919(6) 0.5876(5) 0.0312(16) Uani 1 1 d . . . C58 C 0.4249(6) 1.1267(6) 0.4845(6) 0.0380(18) Uani 1 1 d . . . C59 C 0.4320(6) 1.2454(6) 0.3779(6) 0.0374(19) Uani 1 1 d . . . C60 C 0.3848(5) 1.3106(6) 0.5576(6) 0.0316(16) Uani 1 1 d . . . Cl1 Cl 0.47613(17) 0.22343(18) 0.86242(17) 0.0361(4) Uani 1 1 d . . . Cl2 Cl 0.70530(14) 0.03716(17) 0.27215(16) 0.0351(4) Uani 1 1 d . . . Cl3 Cl 0.59187(17) 0.6931(2) 0.21319(18) 0.0479(5) Uani 1 1 d . . . Cl4 Cl 0.46223(15) 0.91683(18) 0.93833(17) 0.0415(4) Uani 1 1 d . . . Fe1 Fe 0.71872(11) 0.72366(13) 0.63838(11) 0.0383(3) Uani 1 1 d . . . Fe2 Fe 0.33340(10) 1.17949(12) 0.42204(11) 0.0366(3) Uani 1 1 d . . . N1 N 0.8193(5) 0.6809(6) 0.6998(5) 0.0388(15) Uani 1 1 d . . . N2 N 0.9258(5) 0.7435(6) 0.7614(5) 0.0399(16) Uani 1 1 d . . . N3 N 0.7746(5) 0.8607(6) 0.7817(5) 0.0461(19) Uani 1 1 d . . . N4 N 0.8822(5) 0.9228(5) 0.8319(5) 0.0322(14) Uani 1 1 d . . . N5 N 0.8202(5) 0.7923(5) 0.6027(5) 0.0352(15) Uani 1 1 d . . . N6 N 0.9221(5) 0.8655(5) 0.6817(5) 0.0357(15) Uani 1 1 d . . . N7 N 0.2233(5) 1.1050(5) 0.4657(5) 0.0376(15) Uani 1 1 d . . . N8 N 0.1207(4) 1.0555(5) 0.3891(5) 0.0300(13) Uani 1 1 d . . . N9 N 0.2798(5) 1.0477(5) 0.2834(5) 0.0315(14) Uani 1 1 d . . . N10 N 0.1744(5) 0.9979(5) 0.2214(5) 0.0338(14) Uani 1 1 d . . . N11 N 0.2196(4) 1.2400(5) 0.3676(5) 0.0305(14) Uani 1 1 d . . . N12 N 0.1199(4) 1.1584(5) 0.2999(5) 0.0294(13) Uani 1 1 d . . . N13 N 0.6314(4) 0.4683(5) 0.8009(4) 0.0293(13) Uani 1 1 d . . . H13A H 0.6171 0.4193 0.8228 0.035 Uiso 1 1 calc R . . H13B H 0.6393 0.4325 0.7370 0.035 Uiso 1 1 calc R . . N14 N 0.6168(4) 0.6903(5) 0.9339(4) 0.0326(13) Uani 1 1 d . . . H14A H 0.6438 0.7428 0.9203 0.039 Uiso 1 1 calc R . . H14B H 0.5870 0.7190 0.9830 0.039 Uiso 1 1 calc R . . N15 N 0.4527(4) 0.5443(5) 0.9123(5) 0.0359(13) Uani 1 1 d . . . H15A H 0.4245 0.4745 0.8978 0.043 Uiso 1 1 calc R . . H15B H 0.5052 0.5819 0.9765 0.043 Uiso 1 1 calc R . . N16 N 0.3523(4) 0.5366(5) 0.7232(5) 0.0382(14) Uani 1 1 d . . . H16A H 0.3516 0.6004 0.7238 0.046 Uiso 1 1 calc R . . H16B H 0.3198 0.4788 0.6553 0.046 Uiso 1 1 calc R . . N17 N 0.6231(4) 1.1103(5) 0.6954(5) 0.0342(14) Uani 1 1 d . . . H17A H 0.6128 1.1719 0.6967 0.041 Uiso 1 1 calc R . . H17B H 0.6090 1.1064 0.7499 0.041 Uiso 1 1 calc R . . N18 N 0.6741(4) 0.9454(5) 0.5355(4) 0.0352(14) Uani 1 1 d . . . H18A H 0.6981 0.9132 0.5724 0.042 Uiso 1 1 calc R . . H18B H 0.6748 0.9081 0.4683 0.042 Uiso 1 1 calc R . . N19 N 0.3832(4) 0.9074(5) 0.5543(4) 0.0327(13) Uani 1 1 d . . . H19A H 0.3850 0.8589 0.5778 0.039 Uiso 1 1 calc R . . H19B H 0.3743 0.9681 0.6040 0.039 Uiso 1 1 calc R . . N20 N 0.4312(4) 0.8383(5) 0.3736(4) 0.0310(13) Uani 1 1 d . . . H20C H 0.4240 0.8738 0.3364 0.037 Uiso 1 1 calc R . . H20D H 0.4633 0.7883 0.3453 0.037 Uiso 1 1 calc R . . N21 N 0.6739(5) 0.3037(5) 0.2873(5) 0.0429(15) Uani 1 1 d . . . H21C H 0.7175 0.3404 0.3563 0.051 Uiso 1 1 calc R . . H21D H 0.6532 0.2303 0.2641 0.051 Uiso 1 1 calc R . . N22 N 0.6435(4) 0.4661(5) 0.2491(5) 0.0382(14) Uani 1 1 d . . . H22C H 0.6169 0.4502 0.1807 0.046 Uiso 1 1 calc R . . H22D H 0.6494 0.5375 0.2933 0.046 Uiso 1 1 calc R . . N23 N 0.4030(4) 0.2188(5) 0.1698(5) 0.0387(15) Uani 1 1 d . . . H23C H 0.4090 0.1754 0.1063 0.046 Uiso 1 1 calc R . . H23D H 0.3923 0.1775 0.2003 0.046 Uiso 1 1 calc R . . N24 N 0.4464(4) 0.4311(5) 0.2299(5) 0.0419(16) Uani 1 1 d . . . H24A H 0.4287 0.4709 0.2866 0.050 Uiso 1 1 calc R . . H24B H 0.4811 0.4800 0.2164 0.050 Uiso 1 1 calc R . . N25 N 0.5729(5) 0.6140(5) 0.7130(5) 0.0349(15) Uani 1 1 d . . . N26 N 0.6330(5) 0.5015(6) 0.4183(6) 0.0451(18) Uani 1 1 d . . . N27 N 0.5529(4) 0.8189(5) 0.5514(4) 0.0282(13) Uani 1 1 d . . . N28 N 0.4723(4) 1.0752(5) 0.5075(5) 0.0305(13) Uani 1 1 d . . . N29 N 0.4894(5) 1.3002(6) 0.3628(5) 0.0363(15) Uani 1 1 d . . . N30 N 0.4120(4) 1.3964(5) 0.6395(5) 0.0262(13) Uani 1 1 d . . . Ni1 Ni 0.50733(10) 0.54050(11) 0.78709(10) 0.0295(2) Uani 1 1 d . . . Ni2 Ni 0.52291(11) 0.95368(12) 0.53367(11) 0.02888(17) Uani 1 1 d . . . Ni3 Ni 0.54535(10) 0.36066(12) 0.27519(11) 0.0387(3) Uani 1 1 d . . . O1 O -0.0005(9) 0.6067(11) 0.5177(10) 0.039(3) Uani 0.40 1 d P . . H1C H -0.0377 0.6106 0.4660 0.046 Uiso 0.40 1 d PR . . H1D H 0.0504 0.6668 0.5588 0.046 Uiso 0.40 1 d PR . . O2 O 0.2676(8) -0.0036(9) 0.7173(10) 0.040(3) Uani 0.40 1 d P . . H2C H 0.3052 -0.0185 0.7600 0.047 Uiso 0.40 1 d PR . . H2B H 0.2304 0.0320 0.7473 0.059 Uiso 0.40 1 d PR . . O3 O 1.0002(9) 0.3618(12) 0.5541(13) 0.051(4) Uani 0.40 1 d P . . H3B H 0.9398 0.3493 0.5570 0.061 Uiso 0.40 1 d PR . . H3C H 0.9974 0.3178 0.4909 0.061 Uiso 0.40 1 d PR . . O4 O 0.2498(8) 0.6389(11) 0.5945(8) 0.032(3) Uani 0.40 1 d P . . H4E H 0.2029 0.5863 0.5871 0.038 Uiso 0.40 1 d PR . . H4B H 0.2992 0.6156 0.5795 0.038 Uiso 0.40 1 d PR . . O5 O 0.6669(10) 0.2966(12) 0.5078(12) 0.051(3) Uani 0.40 1 d P . . H5C H 0.6810 0.2795 0.5563 0.061 Uiso 0.40 1 d PR . . H5D H 0.6417 0.2375 0.4461 0.061 Uiso 0.40 1 d PR . . O11 O 0.4998(4) 0.1331(4) 0.8748(4) 0.0400(12) Uani 1 1 d . . . O12 O 0.5200(4) 0.2360(4) 0.7919(3) 0.0359(12) Uani 1 1 d . . . O13 O 0.3665(4) 0.1823(4) 0.8100(4) 0.0440(13) Uani 1 1 d . . . O14 O 0.4954(4) 0.3236(4) 0.9524(4) 0.0335(11) Uani 1 1 d . . . O21 O 0.7823(3) -0.0058(4) 0.3024(4) 0.0379(12) Uani 1 1 d . . . O22 O 0.7522(4) 0.1511(5) 0.3348(4) 0.0463(13) Uani 1 1 d . . . O23 O 0.6778(4) -0.0106(5) 0.1579(4) 0.0466(15) Uani 1 1 d . . . O24 O 0.6250(4) 0.0056(5) 0.2944(5) 0.0493(14) Uani 1 1 d . . . O31 O 0.5057(4) 0.6430(5) 0.2304(4) 0.0447(14) Uani 1 1 d . . . O32 O 0.6714(4) 0.7793(4) 0.2955(3) 0.0344(11) Uani 1 1 d . . . O33 O 0.5497(4) 0.7246(4) 0.1449(4) 0.0421(13) Uani 1 1 d . . . O34 O 0.6251(3) 0.6099(4) 0.1520(4) 0.0400(13) Uani 1 1 d . . . O41 O 0.4336(4) 0.8733(4) 0.9967(4) 0.0423(13) Uani 1 1 d . . . O42 O 0.3665(4) 0.8909(5) 0.8649(4) 0.0483(15) Uani 1 1 d . . . O43 O 0.5101(3) 1.0279(4) 1.0049(4) 0.0317(10) Uani 1 1 d . . . O44 O 0.5230(4) 0.8592(5) 0.8853(4) 0.0420(12) 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 B1 0.028(4) 0.039(5) 0.032(4) 0.012(4) 0.009(3) 0.012(3) B2 0.038(4) 0.026(4) 0.033(4) 0.012(4) 0.013(3) 0.007(3) C1 0.031(4) 0.030(4) 0.048(5) 0.007(4) -0.006(3) 0.004(3) C2 0.030(4) 0.040(4) 0.045(4) 0.025(4) 0.016(3) 0.014(3) C3 0.031(4) 0.036(5) 0.040(4) 0.006(4) -0.007(3) 0.007(3) C4 0.022(3) 0.022(4) 0.045(4) 0.005(3) 0.008(3) 0.004(3) C5 0.028(3) 0.023(3) 0.032(4) 0.017(3) 0.012(3) 0.013(3) C6 0.023(3) 0.021(4) 0.039(4) 0.000(3) 0.009(3) -0.006(3) C7 0.051(5) 0.029(4) 0.028(4) 0.002(3) 0.010(3) 0.003(3) C8 0.047(4) 0.021(3) 0.040(4) 0.014(3) 0.020(3) 0.021(3) C9 0.035(4) 0.033(4) 0.049(5) 0.022(4) 0.016(3) 0.015(3) C10 0.036(4) 0.063(6) 0.037(4) 0.018(4) 0.011(3) 0.015(4) C11 0.038(4) 0.036(4) 0.028(4) 0.010(3) 0.007(3) 0.006(3) C12 0.036(4) 0.055(5) 0.027(4) 0.018(4) 0.017(3) 0.028(4) C13 0.040(4) 0.033(4) 0.034(4) 0.011(3) 0.015(3) 0.008(3) C14 0.044(4) 0.018(3) 0.036(4) 0.008(3) 0.018(3) 0.004(3) C15 0.042(4) 0.030(4) 0.022(4) 0.008(3) 0.004(3) 0.011(3) C16 0.039(4) 0.030(4) 0.028(4) 0.013(3) 0.011(3) 0.007(3) C17 0.050(5) 0.033(4) 0.042(5) 0.016(4) 0.000(4) 0.015(4) C18 0.040(4) 0.046(5) 0.038(4) 0.037(4) 0.005(3) 0.006(3) C19 0.030(3) 0.032(4) 0.036(4) 0.012(3) 0.017(3) 0.010(3) C20 0.031(3) 0.024(4) 0.042(4) 0.007(3) 0.007(3) 0.004(3) C21 0.025(4) 0.034(4) 0.058(5) -0.002(4) 0.019(3) -0.006(3) C22 0.036(4) 0.027(4) 0.036(4) 0.015(3) 0.014(3) 0.003(3) C23 0.034(4) 0.037(4) 0.030(4) 0.008(3) 0.009(3) 0.008(3) C24 0.039(4) 0.027(4) 0.028(3) 0.010(3) 0.010(3) 0.011(3) C25 0.040(4) 0.038(4) 0.034(4) 0.007(3) 0.015(3) 0.020(3) C26 0.039(4) 0.054(5) 0.043(4) 0.010(4) 0.018(3) 0.019(4) C27 0.042(4) 0.051(5) 0.048(5) 0.007(4) 0.021(4) 0.019(4) C28 0.035(4) 0.028(4) 0.062(5) 0.032(4) 0.015(4) 0.009(3) C29 0.045(4) 0.042(4) 0.047(4) 0.021(4) 0.016(3) 0.025(4) C30 0.022(3) 0.036(4) 0.044(4) 0.014(4) 0.003(3) 0.001(3) C31 0.034(4) 0.056(6) 0.024(4) -0.002(4) 0.011(3) 0.008(4) C32 0.043(4) 0.040(4) 0.024(4) 0.013(3) 0.009(3) 0.011(3) C33 0.037(4) 0.025(4) 0.036(4) 0.006(3) 0.014(3) -0.006(3) C34 0.036(4) 0.044(5) 0.033(4) 0.014(4) 0.010(3) 0.008(3) C35 0.035(4) 0.052(5) 0.026(4) 0.009(4) 0.018(3) 0.008(3) C36 0.031(4) 0.041(4) 0.025(4) 0.011(3) 0.008(3) 0.010(3) C37 0.033(4) 0.048(5) 0.020(3) 0.005(3) 0.003(3) 0.004(3) C38 0.033(3) 0.017(3) 0.029(3) 0.004(3) 0.010(3) 0.019(3) C39 0.040(4) 0.031(4) 0.027(4) 0.012(3) 0.006(3) 0.003(3) C40 0.041(4) 0.008(3) 0.028(3) 0.008(3) -0.005(3) 0.002(3) C41 0.046(4) 0.023(3) 0.021(3) 0.009(3) 0.006(3) 0.013(3) C42 0.026(4) 0.044(4) 0.026(4) 0.016(3) 0.002(3) 0.017(3) C43 0.023(3) 0.042(5) 0.043(4) 0.020(4) -0.006(3) 0.006(3) C44 0.026(3) 0.034(4) 0.037(4) 0.021(3) -0.008(3) 0.007(3) C45 0.043(4) 0.031(4) 0.033(4) 0.005(3) 0.007(3) 0.003(3) C46 0.037(4) 0.034(4) 0.029(3) 0.014(3) 0.015(3) 0.004(3) C47 0.047(4) 0.041(4) 0.040(4) 0.018(4) 0.018(3) 0.014(3) C48 0.034(4) 0.039(4) 0.029(4) 0.010(3) 0.012(3) 0.011(3) C49 0.031(4) 0.039(4) 0.047(4) 0.024(4) 0.004(3) 0.000(3) C50 0.038(4) 0.040(4) 0.032(4) 0.007(3) 0.013(3) 0.002(3) C51 0.040(4) 0.048(5) 0.023(4) 0.008(4) -0.007(3) 0.002(4) C52 0.030(4) 0.057(5) 0.049(5) 0.022(4) 0.024(3) 0.014(3) C53 0.044(4) 0.041(5) 0.046(5) 0.020(4) 0.018(4) 0.015(4) C54 0.035(4) 0.035(4) 0.031(4) 0.014(3) 0.014(3) 0.006(3) C55 0.029(4) 0.059(5) 0.031(4) 0.029(4) -0.002(3) 0.010(3) C56 0.024(3) 0.026(4) 0.040(4) 0.004(3) 0.004(3) 0.006(3) C57 0.040(4) 0.037(4) 0.020(3) 0.013(3) 0.013(3) 0.019(3) C58 0.041(4) 0.028(4) 0.026(4) 0.001(3) 0.004(3) 0.014(3) C59 0.040(4) 0.020(4) 0.039(4) 0.001(3) 0.019(3) 0.013(3) C60 0.016(3) 0.027(4) 0.032(4) 0.001(3) 0.005(3) 0.006(3) Cl1 0.0486(10) 0.0217(8) 0.0271(9) 0.0054(7) 0.0110(7) 0.0103(7) Cl2 0.0314(8) 0.0327(9) 0.0330(9) 0.0081(7) 0.0101(7) 0.0188(7) Cl3 0.0445(11) 0.0371(11) 0.0274(9) -0.0012(8) 0.0024(8) -0.0005(8) Cl4 0.0360(9) 0.0347(10) 0.0431(10) 0.0084(8) 0.0183(8) 0.0142(7) Fe1 0.0401(6) 0.0342(6) 0.0267(6) 0.0101(5) 0.0018(5) 0.0101(5) Fe2 0.0254(5) 0.0267(6) 0.0301(6) -0.0003(5) -0.0004(4) 0.0031(4) N1 0.030(3) 0.040(4) 0.042(4) 0.021(3) 0.007(3) 0.010(3) N2 0.033(3) 0.028(4) 0.032(4) 0.001(3) 0.000(3) 0.008(3) N3 0.026(3) 0.048(5) 0.033(4) 0.001(3) 0.000(3) 0.011(3) N4 0.033(3) 0.017(3) 0.040(3) 0.009(3) 0.019(3) 0.001(2) N5 0.032(3) 0.026(3) 0.034(3) 0.011(3) 0.002(3) 0.006(3) N6 0.034(3) 0.030(3) 0.028(3) 0.003(3) 0.012(2) 0.011(3) N7 0.042(3) 0.022(3) 0.030(3) 0.003(3) 0.008(3) 0.003(3) N8 0.035(3) 0.018(3) 0.032(3) 0.007(2) 0.013(2) 0.013(2) N9 0.036(3) 0.022(3) 0.029(3) 0.009(3) 0.007(3) 0.008(3) N10 0.036(3) 0.023(3) 0.026(3) 0.004(3) 0.005(2) 0.009(3) N11 0.032(3) 0.021(3) 0.019(3) -0.002(2) 0.005(2) 0.006(2) N12 0.027(3) 0.026(3) 0.029(3) 0.009(3) 0.010(2) 0.007(2) N13 0.035(3) 0.026(3) 0.029(3) 0.013(2) 0.017(2) 0.009(2) N14 0.027(3) 0.035(3) 0.026(3) 0.007(3) 0.011(2) 0.011(2) N15 0.031(3) 0.045(4) 0.038(3) 0.024(3) 0.013(2) 0.017(3) N16 0.031(3) 0.035(3) 0.028(3) 0.007(3) -0.001(2) 0.004(3) N17 0.040(3) 0.026(3) 0.028(3) 0.008(3) 0.012(2) 0.011(3) N18 0.030(3) 0.039(4) 0.025(3) 0.008(3) 0.008(2) 0.011(2) N19 0.031(3) 0.030(3) 0.030(3) 0.011(3) 0.007(2) 0.012(2) N20 0.034(3) 0.025(3) 0.028(3) 0.010(3) 0.005(2) 0.017(2) N21 0.042(3) 0.029(3) 0.036(3) 0.008(3) 0.002(3) 0.006(3) N22 0.029(3) 0.027(3) 0.041(3) 0.013(3) 0.000(2) -0.001(2) N23 0.037(3) 0.018(3) 0.042(4) 0.001(3) 0.015(3) 0.004(2) N24 0.035(3) 0.022(3) 0.045(4) 0.004(3) 0.009(3) 0.002(3) N25 0.044(4) 0.022(3) 0.024(3) 0.005(3) 0.008(3) 0.005(3) N26 0.035(4) 0.034(4) 0.038(4) 0.002(3) 0.005(3) 0.005(3) N27 0.026(3) 0.021(3) 0.012(2) -0.005(2) -0.006(2) 0.004(2) N28 0.027(3) 0.023(3) 0.031(3) 0.006(3) 0.009(2) 0.005(2) N29 0.025(3) 0.038(4) 0.028(3) 0.005(3) 0.007(2) 0.007(3) N30 0.033(3) 0.009(3) 0.031(3) 0.009(2) 0.008(2) 0.004(2) Ni1 0.0249(4) 0.0234(5) 0.0303(5) 0.0043(4) 0.0145(4) 0.0058(4) Ni2 0.0269(3) 0.0299(4) 0.0246(4) 0.0114(3) 0.0049(3) 0.0106(3) Ni3 0.0325(5) 0.0411(6) 0.0262(5) 0.0111(4) 0.0067(4) -0.0023(4) O1 0.036(6) 0.035(7) 0.039(7) 0.013(6) 0.014(5) 0.013(5) O2 0.032(6) 0.015(5) 0.038(7) -0.002(5) -0.013(5) 0.012(5) O3 0.032(6) 0.050(9) 0.074(10) 0.036(8) 0.013(6) 0.012(6) O4 0.036(6) 0.049(8) 0.024(6) 0.021(6) 0.019(5) 0.024(5) O5 0.045(7) 0.053(9) 0.053(8) 0.029(7) 0.009(6) 0.022(7) O11 0.043(3) 0.037(3) 0.023(2) 0.007(2) 0.001(2) 0.015(2) O12 0.035(3) 0.042(3) 0.012(2) 0.004(2) -0.0037(18) 0.012(2) O13 0.040(3) 0.034(3) 0.031(3) -0.004(2) 0.008(2) 0.017(2) O14 0.032(2) 0.025(3) 0.030(2) 0.005(2) 0.0143(19) 0.0021(19) O21 0.028(2) 0.038(3) 0.028(2) 0.002(2) 0.0080(19) 0.012(2) O22 0.051(3) 0.037(3) 0.041(3) 0.011(3) 0.018(2) 0.015(2) O23 0.024(2) 0.052(4) 0.032(3) 0.002(3) 0.003(2) 0.005(2) O24 0.035(3) 0.049(3) 0.052(3) 0.013(3) 0.018(2) 0.018(2) O31 0.048(3) 0.043(3) 0.010(2) -0.004(2) 0.002(2) 0.005(2) O32 0.047(3) 0.034(3) 0.015(2) 0.004(2) 0.0161(19) 0.013(2) O33 0.036(3) 0.029(3) 0.020(2) -0.009(2) 0.001(2) -0.007(2) O34 0.023(2) 0.024(3) 0.042(3) 0.003(2) 0.006(2) -0.0156(19) O41 0.031(2) 0.024(3) 0.047(3) 0.007(2) 0.003(2) -0.001(2) O42 0.049(3) 0.041(3) 0.027(3) -0.006(2) 0.011(2) 0.022(3) O43 0.035(2) 0.034(3) 0.033(3) 0.021(2) 0.0100(19) 0.018(2) O44 0.042(3) 0.045(3) 0.023(2) 0.009(2) -0.003(2) 0.021(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 B1 N2 1.388(10) . ? B1 N4 1.479(9) . ? B1 N6 1.483(10) . ? B1 H11B 0.9800 . ? B2 N10 1.528(9) . ? B2 N12 1.532(9) . ? B2 N8 1.555(9) . ? B2 H22E 0.9800 . ? C1 C2 1.280(11) . ? C1 N1 1.515(9) . ? C1 H1 0.9300 . ? C2 C3 1.520(12) . ? C2 H2 0.9300 . ? C3 N2 1.392(9) . ? C3 H3 0.9300 . ? C4 N3 1.351(8) . ? C4 C5 1.364(10) . ? C4 H4 0.9300 . ? C5 C6 1.430(9) . ? C5 H5 0.9300 . ? C6 N4 1.434(7) . ? C6 H6 0.9300 . ? C7 N5 1.334(8) . ? C7 C8 1.373(10) . ? C7 H7 0.9300 . ? C8 C9 1.401(11) . ? C8 H8 0.9300 . ? C9 N6 1.368(8) . ? C9 H9 0.9300 . ? C10 N7 1.382(9) . ? C10 C11 1.407(11) . ? C10 H10 0.9300 . ? C11 C12 1.409(10) . ? C11 H11 0.9300 . ? C12 N8 1.326(8) . ? C12 H12 0.9300 . ? C13 C14 1.395(11) . ? C13 N9 1.442(8) . ? C13 H13 0.9300 . ? C14 C15 1.397(10) . ? C14 N10 1.944(7) . ? C14 H14 0.9300 . ? C15 N10 1.351(7) . ? C15 H15 0.9300 . ? C16 N11 1.462(8) . ? C16 C17 1.499(11) . ? C16 H16 0.9300 . ? C17 C18 1.398(12) . ? C17 H17 0.9300 . ? C18 N12 1.354(8) . ? C18 H18 0.9300 . ? C19 N13 1.469(7) . ? C19 C20 1.518(10) . ? C19 C24 1.521(9) . ? C19 H19 0.9800 . ? C20 C21 1.508(10) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.540(10) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.509(10) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.540(9) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N14 1.490(7) . ? C24 H24 0.9800 . ? C25 N15 1.486(7) . ? C25 C30 1.512(10) . ? C25 C26 1.549(11) . ? C25 H25 0.9800 . ? C26 C27 1.483(11) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.529(11) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.504(11) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.511(10) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 N16 1.506(8) . ? C30 H30 0.9800 . ? C31 N17 1.483(8) . ? C31 C32 1.495(11) . ? C31 C36 1.514(10) . ? C31 H31 0.9800 . ? C32 C33 1.554(10) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.513(10) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.526(10) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.546(10) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 N18 1.437(8) . ? C36 H36 0.9800 . ? C37 C42 1.507(10) . ? C37 N19 1.509(7) . ? C37 C38 1.516(10) . ? C37 H37 0.9800 . ? C38 C39 1.515(9) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.521(10) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.539(9) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.540(9) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 N20 1.457(7) . ? C42 H42 0.9800 . ? C43 N21 1.435(8) . ? C43 C48 1.540(11) . ? C43 C44 1.566(10) . ? C43 H43 0.9800 . ? C44 C45 1.530(10) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.540(10) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.534(10) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.536(10) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 N22 1.480(7) . ? C48 H48 0.9800 . ? C49 N23 1.471(8) . ? C49 C50 1.507(10) . ? C49 C54 1.536(10) . ? C49 H49 0.9800 . ? C50 C51 1.521(12) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.518(12) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.538(11) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.496(11) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 N24 1.482(7) . ? C54 H54 0.9800 . ? C55 N25 1.118(8) . ? C55 Fe1 1.949(8) . ? C56 N26 1.110(7) . ? C56 Fe1 2.047(7) . ? C57 N27 1.119(7) . ? C57 Fe1 2.061(7) . ? C58 N28 1.168(8) . ? C58 Fe2 1.856(8) . ? C59 N29 1.151(8) . ? C59 Fe2 1.936(8) . ? C60 N30 1.182(7) . ? C60 Fe2 1.876(7) . ? Cl1 O14 1.367(5) . ? Cl1 O12 1.394(5) . ? Cl1 O13 1.421(5) . ? Cl1 O11 1.450(6) . ? Cl2 O24 1.308(5) . ? Cl2 O22 1.377(6) . ? Cl2 O21 1.404(5) . ? Cl2 O23 1.436(5) . ? Cl3 O32 1.331(5) . ? Cl3 O33 1.337(6) . ? Cl3 O34 1.363(6) . ? Cl3 O31 1.428(6) . ? Cl4 O43 1.351(5) . ? Cl4 O41 1.361(6) . ? Cl4 O42 1.378(6) . ? Cl4 O44 1.412(5) . ? Fe1 N1 1.831(7) . ? Fe1 N5 1.895(7) . ? Fe1 N3 1.973(7) . ? Fe2 N9 1.904(6) . ? Fe2 N11 2.097(6) . ? Fe2 N7 2.108(7) . ? N1 N2 1.421(8) . ? N3 N4 1.423(8) . ? N5 N6 1.447(8) . ? N7 N8 1.418(9) . ? N9 N10 1.393(8) . ? N11 N12 1.425(8) . ? N13 Ni1 2.174(6) . ? N13 H13A 0.9000 . ? N13 H13B 0.9000 . ? N14 Ni1 2.179(5) . ? N14 H14A 0.9000 . ? N14 H14B 0.9000 . ? N15 Ni1 2.159(5) . ? N15 H15A 0.9000 . ? N15 H15B 0.9000 . ? N16 Ni1 2.132(6) . ? N16 H16A 0.9000 . ? N16 H16B 0.9000 . ? N17 Ni2 2.283(6) . ? N17 H17A 0.9000 . ? N17 H17B 0.9000 . ? N18 Ni2 2.134(5) . ? N18 H18A 0.9000 . ? N18 H18B 0.9000 . ? N19 Ni2 2.092(5) . ? N19 H19A 0.9000 . ? N19 H19B 0.9000 . ? N20 Ni2 2.078(5) . ? N20 H20C 0.9000 . ? N20 H20D 0.9000 . ? N21 Ni3 2.096(7) . ? N21 H21C 0.9000 . ? N21 H21D 0.9000 . ? N22 Ni3 2.081(6) . ? N22 H22C 0.9000 . ? N22 H22D 0.9000 . ? N23 Ni3 2.185(5) . ? N23 H23C 0.9000 . ? N23 H23D 0.9000 . ? N24 Ni3 1.998(7) . ? N24 H24A 0.9000 . ? N24 H24B 0.9000 . ? N25 Ni1 2.079(7) . ? N26 Ni3 2.030(6) . ? N27 Ni2 2.133(6) . ? N28 Ni2 2.120(7) . ? N29 Ni3 2.073(7) 1_565 ? N30 Ni1 2.101(6) 1_565 ? Ni1 N30 2.101(6) 1_545 ? Ni3 N29 2.073(7) 1_545 ? O1 H1C 0.8499 . ? O1 H1D 0.8500 . ? O2 H2C 0.8499 . ? O2 H2B 0.8501 . ? O3 H3B 0.8499 . ? O3 H3C 0.8499 . ? O4 H4E 0.8500 . ? O4 H4B 0.8501 . ? O5 H5C 0.8499 . ? O5 H5D 0.8500 . ? 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 N2 B1 N4 123.1(6) . . ? N2 B1 N6 120.6(6) . . ? N4 B1 N6 99.2(6) . . ? N2 B1 H11B 103.8 . . ? N4 B1 H11B 103.8 . . ? N6 B1 H11B 103.8 . . ? N10 B2 N12 103.1(5) . . ? N10 B2 N8 114.5(6) . . ? N12 B2 N8 100.1(5) . . ? N10 B2 H22E 112.7 . . ? N12 B2 H22E 112.7 . . ? N8 B2 H22E 112.7 . . ? C2 C1 N1 117.9(7) . . ? C2 C1 H1 121.0 . . ? N1 C1 H1 121.0 . . ? C1 C2 C3 104.7(8) . . ? C1 C2 H2 127.6 . . ? C3 C2 H2 127.6 . . ? N2 C3 C2 103.1(6) . . ? N2 C3 H3 128.4 . . ? C2 C3 H3 128.4 . . ? N3 C4 C5 119.8(6) . . ? N3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 99.2(6) . . ? C4 C5 H5 130.4 . . ? C6 C5 H5 130.4 . . ? C5 C6 N4 111.4(5) . . ? C5 C6 H6 124.3 . . ? N4 C6 H6 124.3 . . ? N5 C7 C8 101.6(6) . . ? N5 C7 H7 129.2 . . ? C8 C7 H7 129.2 . . ? C7 C8 C9 117.7(7) . . ? C7 C8 H8 121.2 . . ? C9 C8 H8 121.2 . . ? N6 C9 C8 100.3(6) . . ? N6 C9 H9 129.9 . . ? C8 C9 H9 129.9 . . ? N7 C10 C11 109.3(7) . . ? N7 C10 H10 125.4 . . ? C11 C10 H10 125.4 . . ? C10 C11 C12 107.0(7) . . ? C10 C11 H11 126.5 . . ? C12 C11 H11 126.5 . . ? N8 C12 C11 107.0(6) . . ? N8 C12 H12 126.5 . . ? C11 C12 H12 126.5 . . ? C14 C13 N9 95.1(6) . . ? C14 C13 H13 132.5 . . ? N9 C13 H13 132.5 . . ? C13 C14 C15 127.4(7) . . ? C13 C14 N10 83.4(5) . . ? C13 C14 H14 116.3 . . ? C15 C14 H14 116.3 . . ? N10 C14 H14 160.3 . . ? N10 C15 C14 90.0(5) . . ? N10 C15 H15 135.0 . . ? C14 C15 H15 135.0 . . ? N11 C16 C17 97.9(6) . . ? N11 C16 H16 131.0 . . ? C17 C16 H16 131.0 . . ? C18 C17 C16 110.2(7) . . ? C18 C17 H17 124.9 . . ? C16 C17 H17 124.9 . . ? N12 C18 C17 111.7(7) . . ? N12 C18 H18 124.1 . . ? C17 C18 H18 124.1 . . ? N13 C19 C20 108.2(5) . . ? N13 C19 C24 108.3(5) . . ? C20 C19 C24 117.5(6) . . ? N13 C19 H19 107.5 . . ? C20 C19 H19 107.5 . . ? C24 C19 H19 107.5 . . ? C21 C20 C19 99.0(7) . . ? C21 C20 H20A 112.0 . . ? C19 C20 H20A 112.0 . . ? C21 C20 H20B 112.0 . . ? C19 C20 H20B 112.0 . . ? H20A C20 H20B 109.6 . . ? C20 C21 C22 110.0(6) . . ? C20 C21 H21A 109.7 . . ? C22 C21 H21A 109.7 . . ? C20 C21 H21B 109.7 . . ? C22 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? C23 C22 C21 112.3(6) . . ? C23 C22 H22A 109.1 . . ? C21 C22 H22A 109.1 . . ? C23 C22 H22B 109.1 . . ? C21 C22 H22B 109.1 . . ? H22A C22 H22B 107.9 . . ? C22 C23 C24 109.5(6) . . ? C22 C23 H23A 109.8 . . ? C24 C23 H23A 109.8 . . ? C22 C23 H23B 109.8 . . ? C24 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? N14 C24 C19 115.5(5) . . ? N14 C24 C23 108.8(5) . . ? C19 C24 C23 111.5(6) . . ? N14 C24 H24 106.9 . . ? C19 C24 H24 106.9 . . ? C23 C24 H24 106.9 . . ? N15 C25 C30 97.6(5) . . ? N15 C25 C26 102.2(6) . . ? C30 C25 C26 109.2(6) . . ? N15 C25 H25 115.3 . . ? C30 C25 H25 115.3 . . ? C26 C25 H25 115.3 . . ? C27 C26 C25 107.5(7) . . ? C27 C26 H26A 110.2 . . ? C25 C26 H26A 110.2 . . ? C27 C26 H26B 110.2 . . ? C25 C26 H26B 110.2 . . ? H26A C26 H26B 108.5 . . ? C26 C27 C28 118.2(7) . . ? C26 C27 H27A 107.7 . . ? C28 C27 H27A 107.7 . . ? C26 C27 H27B 107.7 . . ? C28 C27 H27B 107.7 . . ? H27A C27 H27B 107.1 . . ? C29 C28 C27 109.5(6) . . ? C29 C28 H28A 109.8 . . ? C27 C28 H28A 109.8 . . ? C29 C28 H28B 109.8 . . ? C27 C28 H28B 109.8 . . ? H28A C28 H28B 108.2 . . ? C28 C29 C30 116.3(7) . . ? C28 C29 H29A 108.2 . . ? C30 C29 H29A 108.2 . . ? C28 C29 H29B 108.2 . . ? C30 C29 H29B 108.2 . . ? H29A C29 H29B 107.4 . . ? N16 C30 C29 113.0(6) . . ? N16 C30 C25 109.8(5) . . ? C29 C30 C25 112.8(6) . . ? N16 C30 H30 106.9 . . ? C29 C30 H30 106.9 . . ? C25 C30 H30 106.9 . . ? N17 C31 C32 118.6(7) . . ? N17 C31 C36 107.3(6) . . ? C32 C31 C36 112.9(7) . . ? N17 C31 H31 105.7 . . ? C32 C31 H31 105.7 . . ? C36 C31 H31 105.7 . . ? C31 C32 C33 111.3(6) . . ? C31 C32 H32A 109.4 . . ? C33 C32 H32A 109.4 . . ? C31 C32 H32B 109.4 . . ? C33 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 106.8(6) . . ? C34 C33 H33A 110.4 . . ? C32 C33 H33A 110.4 . . ? C34 C33 H33B 110.4 . . ? C32 C33 H33B 110.4 . . ? H33A C33 H33B 108.6 . . ? C33 C34 C35 110.9(6) . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 108.0 . . ? C34 C35 C36 108.2(6) . . ? C34 C35 H35A 110.0 . . ? C36 C35 H35A 110.0 . . ? C34 C35 H35B 110.0 . . ? C36 C35 H35B 110.0 . . ? H35A C35 H35B 108.4 . . ? N18 C36 C31 105.3(6) . . ? N18 C36 C35 97.6(6) . . ? C31 C36 C35 111.1(6) . . ? N18 C36 H36 113.8 . . ? C31 C36 H36 113.8 . . ? C35 C36 H36 113.8 . . ? C42 C37 N19 107.3(5) . . ? C42 C37 C38 110.5(6) . . ? N19 C37 C38 104.9(5) . . ? C42 C37 H37 111.3 . . ? N19 C37 H37 111.3 . . ? C38 C37 H37 111.3 . . ? C39 C38 C37 100.3(6) . . ? C39 C38 H38A 111.7 . . ? C37 C38 H38A 111.7 . . ? C39 C38 H38B 111.7 . . ? C37 C38 H38B 111.7 . . ? H38A C38 H38B 109.5 . . ? C38 C39 C40 114.0(6) . . ? C38 C39 H39A 108.7 . . ? C40 C39 H39A 108.7 . . ? C38 C39 H39B 108.7 . . ? C40 C39 H39B 108.7 . . ? H39A C39 H39B 107.6 . . ? C39 C40 C41 109.7(5) . . ? C39 C40 H40A 109.7 . . ? C41 C40 H40A 109.7 . . ? C39 C40 H40B 109.7 . . ? C41 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? C40 C41 C42 114.0(5) . . ? C40 C41 H41A 108.8 . . ? C42 C41 H41A 108.8 . . ? C40 C41 H41B 108.8 . . ? C42 C41 H41B 108.8 . . ? H41A C41 H41B 107.7 . . ? N20 C42 C37 110.4(6) . . ? N20 C42 C41 122.5(6) . . ? C37 C42 C41 115.6(6) . . ? N20 C42 H42 101.4 . . ? C37 C42 H42 101.4 . . ? C41 C42 H42 101.4 . . ? N21 C43 C48 101.4(6) . . ? N21 C43 C44 114.9(6) . . ? C48 C43 C44 118.1(6) . . ? N21 C43 H43 107.2 . . ? C48 C43 H43 107.2 . . ? C44 C43 H43 107.2 . . ? C45 C44 C43 112.1(6) . . ? C45 C44 H44A 109.2 . . ? C43 C44 H44A 109.2 . . ? C45 C44 H44B 109.2 . . ? C43 C44 H44B 109.2 . . ? H44A C44 H44B 107.9 . . ? C44 C45 C46 110.5(6) . . ? C44 C45 H45A 109.6 . . ? C46 C45 H45A 109.6 . . ? C44 C45 H45B 109.6 . . ? C46 C45 H45B 109.6 . . ? H45A C45 H45B 108.1 . . ? C47 C46 C45 110.6(6) . . ? C47 C46 H46A 109.5 . . ? C45 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 108.1 . . ? C46 C47 C48 112.6(6) . . ? C46 C47 H47A 109.1 . . ? C48 C47 H47A 109.1 . . ? C46 C47 H47B 109.1 . . ? C48 C47 H47B 109.1 . . ? H47A C47 H47B 107.8 . . ? N22 C48 C47 116.5(6) . . ? N22 C48 C43 105.4(5) . . ? C47 C48 C43 109.2(6) . . ? N22 C48 H48 108.5 . . ? C47 C48 H48 108.5 . . ? C43 C48 H48 108.5 . . ? N23 C49 C50 115.0(6) . . ? N23 C49 C54 108.5(5) . . ? C50 C49 C54 109.7(6) . . ? N23 C49 H49 107.8 . . ? C50 C49 H49 107.8 . . ? C54 C49 H49 107.8 . . ? C49 C50 C51 107.8(6) . . ? C49 C50 H50A 110.1 . . ? C51 C50 H50A 110.1 . . ? C49 C50 H50B 110.1 . . ? C51 C50 H50B 110.1 . . ? H50A C50 H50B 108.5 . . ? C52 C51 C50 118.0(7) . . ? C52 C51 H51A 107.8 . . ? C50 C51 H51A 107.8 . . ? C52 C51 H51B 107.8 . . ? C50 C51 H51B 107.8 . . ? H51A C51 H51B 107.1 . . ? C51 C52 C53 106.9(7) . . ? C51 C52 H52A 110.3 . . ? C53 C52 H52A 110.3 . . ? C51 C52 H52B 110.3 . . ? C53 C52 H52B 110.3 . . ? H52A C52 H52B 108.6 . . ? C54 C53 C52 110.4(7) . . ? C54 C53 H53A 109.6 . . ? C52 C53 H53A 109.6 . . ? C54 C53 H53B 109.6 . . ? C52 C53 H53B 109.6 . . ? H53A C53 H53B 108.1 . . ? N24 C54 C53 114.4(5) . . ? N24 C54 C49 102.4(5) . . ? C53 C54 C49 114.3(6) . . ? N24 C54 H54 108.5 . . ? C53 C54 H54 108.5 . . ? C49 C54 H54 108.5 . . ? N25 C55 Fe1 169.8(6) . . ? N26 C56 Fe1 158.3(6) . . ? N27 C57 Fe1 173.2(6) . . ? N28 C58 Fe2 167.9(6) . . ? N29 C59 Fe2 169.3(6) . . ? N30 C60 Fe2 174.8(6) . . ? O14 Cl1 O12 111.9(3) . . ? O14 Cl1 O13 104.9(3) . . ? O12 Cl1 O13 107.7(3) . . ? O14 Cl1 O11 119.1(3) . . ? O12 Cl1 O11 108.8(3) . . ? O13 Cl1 O11 103.5(3) . . ? O24 Cl2 O22 110.9(3) . . ? O24 Cl2 O21 109.5(4) . . ? O22 Cl2 O21 103.8(3) . . ? O24 Cl2 O23 110.3(3) . . ? O22 Cl2 O23 116.5(4) . . ? O21 Cl2 O23 105.3(3) . . ? O32 Cl3 O33 108.5(3) . . ? O32 Cl3 O34 111.2(3) . . ? O33 Cl3 O34 102.6(3) . . ? O32 Cl3 O31 120.8(3) . . ? O33 Cl3 O31 104.3(3) . . ? O34 Cl3 O31 107.8(3) . . ? O43 Cl4 O41 108.4(3) . . ? O43 Cl4 O42 113.1(3) . . ? O41 Cl4 O42 100.3(4) . . ? O43 Cl4 O44 114.2(3) . . ? O41 Cl4 O44 109.6(3) . . ? O42 Cl4 O44 110.3(3) . . ? N1 Fe1 N5 87.2(3) . . ? N1 Fe1 C55 89.3(2) . . ? N5 Fe1 C55 176.3(2) . . ? N1 Fe1 N3 83.8(3) . . ? N5 Fe1 N3 87.4(3) . . ? C55 Fe1 N3 93.4(2) . . ? N1 Fe1 C56 89.4(2) . . ? N5 Fe1 C56 87.8(2) . . ? C55 Fe1 C56 91.0(3) . . ? N3 Fe1 C56 171.9(2) . . ? N1 Fe1 C57 172.5(2) . . ? N5 Fe1 C57 91.5(2) . . ? C55 Fe1 C57 92.1(3) . . ? N3 Fe1 C57 88.7(2) . . ? C56 Fe1 C57 97.9(3) . . ? C58 Fe2 C60 86.3(3) . . ? C58 Fe2 N9 94.7(2) . . ? C60 Fe2 N9 179.0(2) . . ? C58 Fe2 C59 94.4(4) . . ? C60 Fe2 C59 90.0(3) . . ? N9 Fe2 C59 89.7(2) . . ? C58 Fe2 N11 171.6(2) . . ? C60 Fe2 N11 89.8(2) . . ? N9 Fe2 N11 89.2(2) . . ? C59 Fe2 N11 93.0(3) . . ? C58 Fe2 N7 86.4(3) . . ? C60 Fe2 N7 91.3(2) . . ? N9 Fe2 N7 88.9(3) . . ? C59 Fe2 N7 178.4(2) . . ? N11 Fe2 N7 86.3(3) . . ? N2 N1 C1 95.8(5) . . ? N2 N1 Fe1 127.8(5) . . ? C1 N1 Fe1 133.4(4) . . ? B1 N2 C3 135.3(5) . . ? B1 N2 N1 105.9(5) . . ? C3 N2 N1 117.0(6) . . ? C4 N3 N4 103.2(5) . . ? C4 N3 Fe1 134.3(4) . . ? N4 N3 Fe1 121.4(5) . . ? N3 N4 C6 105.7(5) . . ? N3 N4 B1 107.0(5) . . ? C6 N4 B1 132.8(5) . . ? C7 N5 N6 110.6(5) . . ? C7 N5 Fe1 127.7(4) . . ? N6 N5 Fe1 121.7(5) . . ? C9 N6 N5 109.3(5) . . ? C9 N6 B1 137.5(5) . . ? N5 N6 B1 107.8(5) . . ? C10 N7 N8 104.1(5) . . ? C10 N7 Fe2 139.9(4) . . ? N8 N7 Fe2 114.4(5) . . ? C12 N8 N7 112.3(5) . . ? C12 N8 B2 125.5(5) . . ? N7 N8 B2 122.1(5) . . ? N10 N9 C13 105.7(5) . . ? N10 N9 Fe2 123.1(5) . . ? C13 N9 Fe2 130.9(4) . . ? C15 N10 N9 121.6(5) . . ? C15 N10 B2 118.9(5) . . ? N9 N10 B2 118.7(5) . . ? C15 N10 C14 45.9(4) . . ? N9 N10 C14 75.7(4) . . ? B2 N10 C14 163.9(4) . . ? N12 N11 C16 114.7(5) . . ? N12 N11 Fe2 114.9(5) . . ? C16 N11 Fe2 130.2(3) . . ? C18 N12 N11 104.6(5) . . ? C18 N12 B2 132.9(5) . . ? N11 N12 B2 122.4(5) . . ? C19 N13 Ni1 106.2(3) . . ? C19 N13 H13A 110.5 . . ? Ni1 N13 H13A 110.5 . . ? C19 N13 H13B 110.5 . . ? Ni1 N13 H13B 110.5 . . ? H13A N13 H13B 108.7 . . ? C24 N14 Ni1 101.1(3) . . ? C24 N14 H14A 111.6 . . ? Ni1 N14 H14A 111.6 . . ? C24 N14 H14B 111.6 . . ? Ni1 N14 H14B 111.6 . . ? H14A N14 H14B 109.4 . . ? C25 N15 Ni1 105.4(3) . . ? C25 N15 H15A 110.7 . . ? Ni1 N15 H15A 110.7 . . ? C25 N15 H15B 110.7 . . ? Ni1 N15 H15B 110.7 . . ? H15A N15 H15B 108.8 . . ? C30 N16 Ni1 104.2(3) . . ? C30 N16 H16A 110.9 . . ? Ni1 N16 H16A 110.9 . . ? C30 N16 H16B 110.9 . . ? Ni1 N16 H16B 110.9 . . ? H16A N16 H16B 108.9 . . ? C31 N17 Ni2 103.8(3) . . ? C31 N17 H17A 111.0 . . ? Ni2 N17 H17A 111.0 . . ? C31 N17 H17B 111.0 . . ? Ni2 N17 H17B 111.0 . . ? H17A N17 H17B 109.0 . . ? C36 N18 Ni2 101.0(3) . . ? C36 N18 H18A 111.6 . . ? Ni2 N18 H18A 111.6 . . ? C36 N18 H18B 111.6 . . ? Ni2 N18 H18B 111.6 . . ? H18A N18 H18B 109.4 . . ? C37 N19 Ni2 109.6(3) . . ? C37 N19 H19A 109.7 . . ? Ni2 N19 H19A 109.7 . . ? C37 N19 H19B 109.7 . . ? Ni2 N19 H19B 109.7 . . ? H19A N19 H19B 108.2 . . ? C42 N20 Ni2 112.4(3) . . ? C42 N20 H20C 109.1 . . ? Ni2 N20 H20C 109.1 . . ? C42 N20 H20D 109.1 . . ? Ni2 N20 H20D 109.1 . . ? H20C N20 H20D 107.9 . . ? C43 N21 Ni3 107.5(4) . . ? C43 N21 H21C 110.2 . . ? Ni3 N21 H21C 110.2 . . ? C43 N21 H21D 110.2 . . ? Ni3 N21 H21D 110.2 . . ? H21C N21 H21D 108.5 . . ? C48 N22 Ni3 109.2(4) . . ? C48 N22 H22C 109.8 . . ? Ni3 N22 H22C 109.8 . . ? C48 N22 H22D 109.8 . . ? Ni3 N22 H22D 109.8 . . ? H22C N22 H22D 108.3 . . ? C49 N23 Ni3 109.3(3) . . ? C49 N23 H23C 109.8 . . ? Ni3 N23 H23C 109.8 . . ? C49 N23 H23D 109.8 . . ? Ni3 N23 H23D 109.8 . . ? H23C N23 H23D 108.3 . . ? C54 N24 Ni3 118.8(4) . . ? C54 N24 H24A 107.6 . . ? Ni3 N24 H24A 107.6 . . ? C54 N24 H24B 107.6 . . ? Ni3 N24 H24B 107.6 . . ? H24A N24 H24B 107.0 . . ? C55 N25 Ni1 169.5(5) . . ? C56 N26 Ni3 176.4(7) . . ? C57 N27 Ni2 144.2(4) . . ? C58 N28 Ni2 166.4(4) . . ? C59 N29 Ni3 156.8(5) . 1_565 ? C60 N30 Ni1 161.2(4) . 1_565 ? N25 Ni1 N30 92.9(2) . 1_545 ? N25 Ni1 N16 97.2(3) . . ? N30 Ni1 N16 64.0(2) 1_545 . ? N25 Ni1 N15 153.6(2) . . ? N30 Ni1 N15 109.1(2) 1_545 . ? N16 Ni1 N15 80.5(2) . . ? N25 Ni1 N13 90.4(2) . . ? N30 Ni1 N13 92.0(2) 1_545 . ? N16 Ni1 N13 155.0(2) . . ? N15 Ni1 N13 102.8(2) . . ? N25 Ni1 N14 83.0(2) . . ? N30 Ni1 N14 174.9(2) 1_545 . ? N16 Ni1 N14 119.4(2) . . ? N15 Ni1 N14 75.6(2) . . ? N13 Ni1 N14 85.0(2) . . ? N20 Ni2 N19 81.1(2) . . ? N20 Ni2 N28 86.9(2) . . ? N19 Ni2 N28 87.9(2) . . ? N20 Ni2 N27 88.4(2) . . ? N19 Ni2 N27 85.6(2) . . ? N28 Ni2 N27 172.5(2) . . ? N20 Ni2 N18 102.0(2) . . ? N19 Ni2 N18 152.9(2) . . ? N28 Ni2 N18 118.9(2) . . ? N27 Ni2 N18 67.8(2) . . ? N20 Ni2 N17 166.2(2) . . ? N19 Ni2 N17 103.7(2) . . ? N28 Ni2 N17 80.5(2) . . ? N27 Ni2 N17 104.7(2) . . ? N18 Ni2 N17 79.7(2) . . ? N24 Ni3 N26 94.7(3) . . ? N24 Ni3 N29 107.5(3) . 1_545 ? N26 Ni3 N29 87.0(3) . 1_545 ? N24 Ni3 N22 80.6(3) . . ? N26 Ni3 N22 70.8(3) . . ? N29 Ni3 N22 157.1(2) 1_545 . ? N24 Ni3 N21 158.2(3) . . ? N26 Ni3 N21 87.5(3) . . ? N29 Ni3 N21 94.2(3) 1_545 . ? N22 Ni3 N21 79.7(3) . . ? N24 Ni3 N23 77.6(2) . . ? N26 Ni3 N23 151.4(3) . . ? N29 Ni3 N23 69.7(2) 1_545 . ? N22 Ni3 N23 133.2(2) . . ? N21 Ni3 N23 109.9(2) . . ? H1C O1 H1D 109.5 . . ? H2C O2 H2B 109.5 . . ? H3B O3 H3C 109.5 . . ? H4E O4 H4B 109.5 . . ? H5C O5 H5D 109.5 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.465 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.075