# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Stephen M. Holmes' _publ_contact_author_email holmesst@umsl.edu _publ_author_name S.M.Holmes data_h16109 _database_code_depnum_ccdc_archive 'CCDC 810415' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common hexanuclear _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H91 B2 Fe2 N23 Ni O5.50' _chemical_formula_weight 1378.56 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' 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 P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1423(16) _cell_length_b 17.3792(16) _cell_length_c 17.4997(16) _cell_angle_alpha 102.334(5) _cell_angle_beta 108.050(5) _cell_angle_gamma 94.584(5) _cell_volume 3387.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8590 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 26.43 _exptl_crystal_description Rectangular _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas no _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.762 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8962 _exptl_absorpt_correction_T_max 0.9444 _exptl_absorpt_process_details 'sadabs v2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64434 _diffrn_reflns_av_R_equivalents 0.0903 _diffrn_reflns_av_sigmaI/netI 0.0993 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 25.03 _reflns_number_total 11942 _reflns_number_gt 7675 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+5.1968P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11942 _refine_ls_number_parameters 849 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1006 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1146 _refine_ls_wR_factor_gt 0.0948 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.016 _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 Fe1 Fe 0.71999(5) 0.51230(3) 0.26405(3) 0.01224(14) Uani 1 1 d . . . Fe2 Fe 1.12186(4) 0.93490(3) 0.34851(3) 0.00979(14) Uani 1 1 d . . . Ni1 Ni 0.81747(4) 0.79989(3) 0.43963(3) 0.01007(13) Uani 1 1 d . . . B1 B 0.7990(4) 0.4161(3) 0.1265(3) 0.0142(10) Uani 1 1 d . . . H1 H 0.8247 0.3848 0.0819 0.017 Uiso 1 1 calc R . . B2 B 1.1043(4) 0.9379(3) 0.1712(3) 0.0138(10) Uani 1 1 d . . . H2 H 1.0986 0.9392 0.1133 0.017 Uiso 1 1 calc R . . N1 N 0.7918(3) 0.6882(2) 0.36015(19) 0.0127(7) Uani 1 1 d . . . N2 N 0.7440(3) 0.4811(2) 0.4346(2) 0.0236(9) Uani 1 1 d . . . N3 N 0.4716(3) 0.5427(2) 0.2605(2) 0.0243(8) Uani 1 1 d . . . N4 N 1.1609(3) 1.09047(19) 0.4822(2) 0.0140(7) Uani 1 1 d . . . N5 N 1.2942(3) 0.8609(2) 0.4702(2) 0.0216(8) Uani 1 1 d . . . N6 N 0.9366(3) 0.84711(19) 0.39738(19) 0.0130(7) Uani 1 1 d . . . N7 N 0.9046(3) 0.45477(18) 0.20473(19) 0.0143(7) Uani 1 1 d . . . N8 N 0.8853(3) 0.49663(18) 0.27447(19) 0.0129(7) Uani 1 1 d . . . N9 N 0.7146(3) 0.36278(18) 0.14949(19) 0.0149(8) Uani 1 1 d . . . N10 N 0.6677(3) 0.39631(18) 0.2086(2) 0.0140(7) Uani 1 1 d . . . N11 N 0.7354(3) 0.48281(18) 0.09788(19) 0.0138(7) Uani 1 1 d . . . N12 N 0.6942(3) 0.53224(18) 0.15180(19) 0.0131(7) Uani 1 1 d . . . N13 N 1.0094(3) 0.97980(18) 0.19679(18) 0.0117(7) Uani 1 1 d . . . N14 N 0.9997(3) 0.97889(18) 0.27260(19) 0.0116(7) Uani 1 1 d . . . N15 N 1.2242(3) 0.97996(18) 0.23287(18) 0.0118(7) Uani 1 1 d . . . N16 N 1.2432(3) 0.98953(18) 0.31583(19) 0.0114(7) Uani 1 1 d . . . N17 N 1.0880(3) 0.85155(18) 0.17883(19) 0.0125(7) Uani 1 1 d . . . N18 N 1.0979(3) 0.83876(18) 0.25539(19) 0.0107(7) Uani 1 1 d . . . N19 N 1.1181(3) 0.72971(18) 0.59154(19) 0.0147(7) Uani 1 1 d . . . N20 N 0.5638(3) 0.6677(2) 0.4965(2) 0.0254(9) Uani 1 1 d . . . N21 N 0.4738(3) 0.7910(2) 0.2956(2) 0.0242(9) Uani 1 1 d . . . N22 N 0.1454(4) 0.2019(3) 0.2331(3) 0.0466(12) Uani 1 1 d . . . N23 N 0.7058(3) 0.8377(2) 0.1259(2) 0.0304(9) Uani 1 1 d . . . C1 C 0.7669(3) 0.6225(2) 0.3214(2) 0.0127(9) Uani 1 1 d . . . C2 C 0.7367(3) 0.4922(2) 0.3709(3) 0.0167(9) Uani 1 1 d . . . C3 C 0.5639(4) 0.5301(2) 0.2602(2) 0.0174(9) Uani 1 1 d . . . C4 C 1.1450(3) 1.0297(2) 0.4358(2) 0.0117(9) Uani 1 1 d . . . C5 C 1.2327(3) 0.8909(2) 0.4253(2) 0.0133(9) Uani 1 1 d . . . C6 C 1.0067(3) 0.8824(2) 0.3809(2) 0.0117(9) Uani 1 1 d . . . C7 C 0.9910(3) 0.5224(2) 0.3334(2) 0.0146(9) Uani 1 1 d . . . C8 C 1.0787(3) 0.4990(2) 0.3017(2) 0.0146(9) Uani 1 1 d . . . C9 C 1.0215(3) 0.4567(2) 0.2205(3) 0.0166(9) Uani 1 1 d . . . C10 C 1.0715(3) 0.4210(3) 0.1545(3) 0.0233(10) Uani 1 1 d . . . H10A H 1.0496 0.3629 0.1387 0.035 Uiso 1 1 calc R . . H10B H 1.1572 0.4349 0.1763 0.035 Uiso 1 1 calc R . . H10C H 1.0402 0.4421 0.1058 0.035 Uiso 1 1 calc R . . C11 C 1.2078(3) 0.5174(3) 0.3472(3) 0.0282(11) Uani 1 1 d . . . H11A H 1.2486 0.4858 0.3144 0.042 Uiso 1 1 calc R . . H11B H 1.2247 0.5043 0.4010 0.042 Uiso 1 1 calc R . . H11C H 1.2349 0.5743 0.3560 0.042 Uiso 1 1 calc R . . C12 C 1.0093(3) 0.5705(2) 0.4192(2) 0.0179(9) Uani 1 1 d . . . H12A H 0.9377 0.5613 0.4328 0.027 Uiso 1 1 calc R . . H12B H 1.0277 0.6273 0.4222 0.027 Uiso 1 1 calc R . . H12C H 1.0744 0.5547 0.4589 0.027 Uiso 1 1 calc R . . C13 C 0.5910(3) 0.3386(2) 0.2119(2) 0.0159(9) Uani 1 1 d . . . C14 C 0.5870(3) 0.2674(2) 0.1554(2) 0.0171(9) Uani 1 1 d . . . C15 C 0.6659(3) 0.2848(2) 0.1166(2) 0.0170(9) Uani 1 1 d . . . C16 C 0.6965(4) 0.2326(2) 0.0487(3) 0.0251(11) Uani 1 1 d . . . H16A H 0.6864 0.2582 0.0028 0.038 Uiso 1 1 calc R . . H16B H 0.6450 0.1810 0.0289 0.038 Uiso 1 1 calc R . . H16C H 0.7783 0.2245 0.0701 0.038 Uiso 1 1 calc R . . C17 C 0.5134(4) 0.1897(2) 0.1407(3) 0.0314(11) Uani 1 1 d . . . H17A H 0.5193 0.1522 0.0921 0.047 Uiso 1 1 calc R . . H17B H 0.4315 0.1974 0.1308 0.047 Uiso 1 1 calc R . . H17C H 0.5409 0.1682 0.1895 0.047 Uiso 1 1 calc R . . C18 C 0.5166(3) 0.3500(2) 0.2663(3) 0.0207(10) Uani 1 1 d . . . H18A H 0.5583 0.3918 0.3171 0.031 Uiso 1 1 calc R . . H18B H 0.4999 0.3000 0.2808 0.031 Uiso 1 1 calc R . . H18C H 0.4427 0.3657 0.2366 0.031 Uiso 1 1 calc R . . C19 C 0.6377(3) 0.5821(2) 0.1095(2) 0.0144(9) Uani 1 1 d . . . C20 C 0.6419(3) 0.5642(2) 0.0289(2) 0.0177(9) Uani 1 1 d . . . C21 C 0.7054(3) 0.5018(2) 0.0242(2) 0.0160(9) Uani 1 1 d . . . C22 C 0.7408(4) 0.4595(3) -0.0464(3) 0.0242(10) Uani 1 1 d . . . H22A H 0.7215 0.4018 -0.0552 0.036 Uiso 1 1 calc R . . H22B H 0.8255 0.4741 -0.0333 0.036 Uiso 1 1 calc R . . H22C H 0.6987 0.4751 -0.0969 0.036 Uiso 1 1 calc R . . C23 C 0.5889(4) 0.6040(3) -0.0388(3) 0.0269(11) Uani 1 1 d . . . H23A H 0.5710 0.5661 -0.0929 0.040 Uiso 1 1 calc R . . H23B H 0.6444 0.6501 -0.0346 0.040 Uiso 1 1 calc R . . H23C H 0.5165 0.6217 -0.0333 0.040 Uiso 1 1 calc R . . C24 C 0.5780(3) 0.6446(2) 0.1452(3) 0.0207(10) Uani 1 1 d . . . H24A H 0.6310 0.6755 0.1999 0.031 Uiso 1 1 calc R . . H24B H 0.5070 0.6193 0.1511 0.031 Uiso 1 1 calc R . . H24C H 0.5568 0.6802 0.1083 0.031 Uiso 1 1 calc R . . C25 C 0.9070(3) 1.0152(2) 0.2780(2) 0.0140(9) Uani 1 1 d . . . C26 C 0.8573(3) 1.0393(2) 0.2056(2) 0.0172(9) Uani 1 1 d . . . C27 C 0.9246(3) 1.0159(2) 0.1560(2) 0.0173(9) Uani 1 1 d . . . C28 C 0.9124(4) 1.0258(3) 0.0717(3) 0.0277(11) Uani 1 1 d . . . H28A H 0.9114 0.9742 0.0352 0.042 Uiso 1 1 calc R . . H28B H 0.9788 1.0638 0.0749 0.042 Uiso 1 1 calc R . . H28C H 0.8391 1.0459 0.0493 0.042 Uiso 1 1 calc R . . C29 C 0.7537(4) 1.0824(3) 0.1872(3) 0.0316(12) Uani 1 1 d . . . H29A H 0.7342 1.0894 0.1306 0.047 Uiso 1 1 calc R . . H29B H 0.7728 1.1348 0.2268 0.047 Uiso 1 1 calc R . . H29C H 0.6863 1.0513 0.1921 0.047 Uiso 1 1 calc R . . C30 C 0.8634(3) 1.0234(2) 0.3499(2) 0.0184(9) Uani 1 1 d . . . H30A H 0.9302 1.0375 0.4018 0.028 Uiso 1 1 calc R . . H30B H 0.8172 0.9728 0.3455 0.028 Uiso 1 1 calc R . . H30C H 0.8140 1.0654 0.3495 0.028 Uiso 1 1 calc R . . C31 C 1.3506(3) 1.0334(2) 0.3572(2) 0.0130(9) Uani 1 1 d . . . C32 C 1.4009(3) 1.0495(2) 0.2993(2) 0.0155(9) Uani 1 1 d . . . C33 C 1.3194(3) 1.0153(2) 0.2219(2) 0.0153(9) Uani 1 1 d . . . C34 C 1.3283(4) 1.0102(3) 0.1382(2) 0.0231(10) Uani 1 1 d . . . H34A H 1.2972 0.9559 0.1033 0.035 Uiso 1 1 calc R . . H34B H 1.4107 1.0235 0.1434 0.035 Uiso 1 1 calc R . . H34C H 1.2829 1.0478 0.1128 0.035 Uiso 1 1 calc R . . C35 C 1.5220(4) 1.0927(3) 0.3181(3) 0.0327(12) Uani 1 1 d . . . H35A H 1.5572 1.0655 0.2786 0.049 Uiso 1 1 calc R . . H35B H 1.5704 1.0932 0.3747 0.049 Uiso 1 1 calc R . . H35C H 1.5175 1.1477 0.3134 0.049 Uiso 1 1 calc R . . C36 C 1.4030(3) 1.0584(2) 0.4490(2) 0.0150(9) Uani 1 1 d . . . H36A H 1.3832 1.0149 0.4724 0.022 Uiso 1 1 calc R . . H36B H 1.3722 1.1057 0.4703 0.022 Uiso 1 1 calc R . . H36C H 1.4885 1.0710 0.4649 0.022 Uiso 1 1 calc R . . C37 C 1.0743(3) 0.7591(2) 0.2442(2) 0.0130(9) Uani 1 1 d . . . C38 C 1.0493(3) 0.7212(2) 0.1607(3) 0.0178(9) Uani 1 1 d . . . C39 C 1.0598(3) 0.7808(2) 0.1214(2) 0.0163(9) Uani 1 1 d . . . C40 C 1.0428(4) 0.7751(3) 0.0319(2) 0.0262(11) Uani 1 1 d . . . H40A H 1.1004 0.8153 0.0276 0.039 Uiso 1 1 calc R . . H40B H 0.9635 0.7845 0.0040 0.039 Uiso 1 1 calc R . . H40C H 1.0533 0.7218 0.0055 0.039 Uiso 1 1 calc R . . C41 C 1.0151(4) 0.6327(2) 0.1217(3) 0.0313(12) Uani 1 1 d . . . H41A H 1.0068 0.6220 0.0627 0.047 Uiso 1 1 calc R . . H41B H 0.9403 0.6141 0.1273 0.047 Uiso 1 1 calc R . . H41C H 1.0759 0.6046 0.1498 0.047 Uiso 1 1 calc R . . C42 C 1.0743(3) 0.7184(2) 0.3107(2) 0.0165(9) Uani 1 1 d . . . H42A H 1.1302 0.7503 0.3638 0.025 Uiso 1 1 calc R . . H42B H 1.0973 0.6657 0.2974 0.025 Uiso 1 1 calc R . . H42C H 0.9955 0.7123 0.3148 0.025 Uiso 1 1 calc R . . C43 C 1.0462(3) 0.7657(2) 0.5421(2) 0.0166(9) Uani 1 1 d . . . H43A H 1.0787 0.7980 0.5145 0.020 Uiso 1 1 calc R . . C44 C 1.2422(3) 0.7370(3) 0.6012(3) 0.0245(10) Uani 1 1 d . . . H44A H 1.2596 0.7720 0.5679 0.037 Uiso 1 1 calc R . . H44B H 1.2617 0.6842 0.5823 0.037 Uiso 1 1 calc R . . H44C H 1.2890 0.7597 0.6598 0.037 Uiso 1 1 calc R . . C45 C 1.0761(4) 0.6752(3) 0.6327(3) 0.0238(10) Uani 1 1 d . . . H45A H 0.9912 0.6730 0.6198 0.036 Uiso 1 1 calc R . . H45B H 1.1155 0.6941 0.6929 0.036 Uiso 1 1 calc R . . H45C H 1.0934 0.6219 0.6131 0.036 Uiso 1 1 calc R . . C46 C 0.6637(3) 0.6917(2) 0.4871(2) 0.0162(9) Uani 1 1 d . . . H46A H 0.7145 0.6540 0.4800 0.019 Uiso 1 1 calc R . . C47 C 0.4796(4) 0.7212(3) 0.5037(4) 0.0470(15) Uani 1 1 d . . . H47A H 0.5039 0.7714 0.4920 0.071 Uiso 1 1 calc R . . H47B H 0.4762 0.7321 0.5601 0.071 Uiso 1 1 calc R . . H47C H 0.4020 0.6964 0.4638 0.071 Uiso 1 1 calc R . . C48 C 0.5305(4) 0.5849(3) 0.4947(3) 0.0365(13) Uani 1 1 d . . . H48A H 0.5949 0.5554 0.4911 0.055 Uiso 1 1 calc R . . H48B H 0.4603 0.5612 0.4464 0.055 Uiso 1 1 calc R . . H48C H 0.5138 0.5825 0.5456 0.055 Uiso 1 1 calc R . . C49 C 0.5805(3) 0.7756(2) 0.3266(2) 0.0170(9) Uani 1 1 d . . . H49A H 0.5890 0.7222 0.3292 0.020 Uiso 1 1 calc R . . C50 C 0.3718(4) 0.7290(3) 0.2650(3) 0.0391(13) Uani 1 1 d . . . H50A H 0.3972 0.6775 0.2692 0.059 Uiso 1 1 calc R . . H50B H 0.3285 0.7265 0.2068 0.059 Uiso 1 1 calc R . . H50C H 0.3208 0.7411 0.2984 0.059 Uiso 1 1 calc R . . C51 C 0.4530(4) 0.8719(3) 0.2940(3) 0.0392(13) Uani 1 1 d . . . H51A H 0.5255 0.9093 0.3263 0.059 Uiso 1 1 calc R . . H51B H 0.3917 0.8845 0.3181 0.059 Uiso 1 1 calc R . . H51C H 0.4276 0.8764 0.2364 0.059 Uiso 1 1 calc R . . C52 C 0.2058(5) 0.1864(3) 0.1852(3) 0.0466(14) Uani 1 1 d . . . C53 C 0.1652(5) 0.1852(3) 0.3115(3) 0.0449(14) Uani 1 1 d . . . H53A H 0.2457 0.1748 0.3329 0.067 Uiso 1 1 calc R . . H53B H 0.1100 0.1382 0.3056 0.067 Uiso 1 1 calc R . . H53C H 0.1534 0.2311 0.3501 0.067 Uiso 1 1 calc R . . C54 C 0.0267(5) 0.2246(4) 0.1964(4) 0.0561(16) Uani 1 1 d . . . H54A H 0.0106 0.2202 0.1370 0.084 Uiso 1 1 calc R . . H54B H 0.0259 0.2796 0.2245 0.084 Uiso 1 1 calc R . . H54C H -0.0335 0.1886 0.2037 0.084 Uiso 1 1 calc R . . C55 C 0.6253(4) 0.8709(3) 0.1518(4) 0.0520(16) Uani 1 1 d . . . H55A H 0.6247 0.8692 0.2056 0.062 Uiso 1 1 calc R . . C56 C 0.7174(6) 0.8409(4) 0.0484(3) 0.076(2) Uani 1 1 d . . . H56A H 0.6656 0.8761 0.0238 0.114 Uiso 1 1 calc R . . H56B H 0.6958 0.7873 0.0111 0.114 Uiso 1 1 calc R . . H56C H 0.7988 0.8618 0.0569 0.114 Uiso 1 1 calc R . . C57 C 0.7916(4) 0.8025(3) 0.1797(3) 0.0359(12) Uani 1 1 d . . . H57A H 0.7753 0.8058 0.2317 0.054 Uiso 1 1 calc R . . H57B H 0.8702 0.8315 0.1919 0.054 Uiso 1 1 calc R . . H57C H 0.7877 0.7465 0.1522 0.054 Uiso 1 1 calc R . . O1 O 0.9393(2) 0.75998(15) 0.52937(15) 0.0140(6) Uani 1 1 d . . . O2 O 0.6938(2) 0.76164(15) 0.48719(16) 0.0150(6) Uani 1 1 d . . . O3 O 0.6712(2) 0.82580(15) 0.35286(16) 0.0158(6) Uani 1 1 d . . . O4 O 0.1939(4) 0.1969(3) 0.1191(3) 0.0908(18) Uani 1 1 d . . . O5 O 0.5511(4) 0.9039(3) 0.1109(4) 0.109(2) Uani 1 1 d . . . O6 O 0.4494(10) 0.9769(8) -0.0073(7) 0.121(4) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0142(3) 0.0102(3) 0.0108(3) 0.0014(2) 0.0030(2) 0.0020(2) Fe2 0.0099(3) 0.0094(3) 0.0095(3) 0.0017(2) 0.0030(2) 0.0013(2) Ni1 0.0097(3) 0.0088(3) 0.0110(3) 0.0008(2) 0.0037(2) 0.0002(2) B1 0.018(2) 0.014(2) 0.011(3) 0.001(2) 0.008(2) 0.001(2) B2 0.015(2) 0.016(2) 0.010(3) 0.002(2) 0.004(2) 0.002(2) N1 0.0115(17) 0.0162(19) 0.0111(19) 0.0053(16) 0.0039(15) 0.0016(15) N2 0.026(2) 0.026(2) 0.017(2) 0.0083(17) 0.0025(17) 0.0085(17) N3 0.023(2) 0.025(2) 0.025(2) 0.0063(17) 0.0070(18) 0.0041(17) N4 0.0165(18) 0.0113(18) 0.015(2) 0.0026(16) 0.0077(15) 0.0011(15) N5 0.0160(18) 0.021(2) 0.026(2) 0.0099(17) 0.0021(17) -0.0007(16) N6 0.0135(17) 0.0144(18) 0.0097(19) 0.0009(15) 0.0030(15) 0.0040(15) N7 0.0174(18) 0.0114(17) 0.0121(19) -0.0001(14) 0.0045(15) 0.0017(14) N8 0.0158(17) 0.0114(17) 0.0106(19) -0.0006(14) 0.0051(15) 0.0034(14) N9 0.0165(18) 0.0121(18) 0.0118(19) -0.0006(15) 0.0014(15) 0.0011(15) N10 0.0139(17) 0.0117(17) 0.0147(19) 0.0023(15) 0.0030(15) 0.0019(15) N11 0.0174(18) 0.0143(18) 0.0095(19) 0.0015(15) 0.0054(15) 0.0018(15) N12 0.0128(17) 0.0115(17) 0.0117(19) 0.0004(14) 0.0011(15) 0.0022(14) N13 0.0137(17) 0.0153(18) 0.0058(18) 0.0020(14) 0.0037(14) 0.0004(14) N14 0.0109(16) 0.0123(17) 0.0113(19) 0.0037(14) 0.0027(14) 0.0020(14) N15 0.0135(17) 0.0142(17) 0.0060(19) 0.0014(14) 0.0023(14) 0.0006(14) N16 0.0136(17) 0.0100(17) 0.0087(19) 0.0017(14) 0.0020(15) 0.0013(14) N17 0.0125(17) 0.0157(18) 0.0101(19) 0.0011(15) 0.0065(15) 0.0017(14) N18 0.0131(17) 0.0116(17) 0.0084(18) 0.0020(14) 0.0053(14) 0.0028(14) N19 0.0148(17) 0.0149(18) 0.0135(19) 0.0053(15) 0.0021(15) 0.0034(15) N20 0.022(2) 0.0137(19) 0.048(3) 0.0089(18) 0.0212(19) 0.0024(16) N21 0.0141(18) 0.023(2) 0.031(2) 0.0019(17) 0.0038(17) 0.0065(16) N22 0.075(3) 0.052(3) 0.043(3) 0.035(2) 0.038(3) 0.044(3) N23 0.023(2) 0.037(2) 0.023(2) 0.0046(19) 0.0011(18) -0.0077(19) C1 0.012(2) 0.019(2) 0.009(2) 0.0065(19) 0.0053(18) 0.0025(18) C2 0.013(2) 0.014(2) 0.020(3) -0.0011(19) 0.0037(19) 0.0059(17) C3 0.021(2) 0.015(2) 0.014(2) 0.0021(18) 0.0050(19) -0.0016(19) C4 0.012(2) 0.013(2) 0.011(2) 0.0063(19) 0.0025(18) 0.0006(17) C5 0.014(2) 0.011(2) 0.014(2) 0.0002(18) 0.0056(18) 0.0004(17) C6 0.016(2) 0.008(2) 0.007(2) -0.0022(17) 0.0000(18) 0.0063(18) C7 0.016(2) 0.011(2) 0.014(2) 0.0024(17) 0.0019(19) -0.0002(17) C8 0.013(2) 0.014(2) 0.015(2) 0.0051(18) 0.0017(18) 0.0031(17) C9 0.016(2) 0.015(2) 0.021(3) 0.0045(19) 0.0093(19) 0.0052(18) C10 0.021(2) 0.027(2) 0.020(3) -0.001(2) 0.006(2) 0.007(2) C11 0.019(2) 0.037(3) 0.027(3) 0.006(2) 0.007(2) 0.007(2) C12 0.018(2) 0.019(2) 0.012(2) 0.0001(18) 0.0011(19) 0.0035(18) C13 0.012(2) 0.016(2) 0.015(2) 0.0034(18) -0.0024(18) 0.0008(18) C14 0.011(2) 0.016(2) 0.016(2) 0.0041(18) -0.0052(18) -0.0009(17) C15 0.021(2) 0.013(2) 0.011(2) -0.0011(18) 0.0005(19) 0.0019(18) C16 0.031(3) 0.016(2) 0.025(3) 0.001(2) 0.008(2) 0.001(2) C17 0.032(3) 0.021(2) 0.038(3) 0.007(2) 0.008(2) 0.002(2) C18 0.020(2) 0.019(2) 0.023(3) 0.0056(19) 0.008(2) -0.0011(19) C19 0.013(2) 0.015(2) 0.011(2) 0.0030(17) -0.0001(18) -0.0024(17) C20 0.017(2) 0.021(2) 0.007(2) 0.0020(18) -0.0043(18) -0.0069(18) C21 0.014(2) 0.018(2) 0.012(2) 0.0016(18) 0.0016(18) -0.0056(18) C22 0.027(2) 0.029(3) 0.016(3) 0.006(2) 0.007(2) 0.004(2) C23 0.032(3) 0.029(3) 0.016(3) 0.008(2) 0.001(2) 0.004(2) C24 0.022(2) 0.019(2) 0.020(2) 0.0067(19) 0.003(2) 0.0045(19) C25 0.0103(19) 0.015(2) 0.017(2) 0.0030(18) 0.0054(18) -0.0002(17) C26 0.018(2) 0.020(2) 0.016(2) 0.0080(19) 0.0045(19) 0.0067(18) C27 0.014(2) 0.021(2) 0.015(2) 0.0080(19) -0.0002(18) 0.0051(18) C28 0.024(2) 0.041(3) 0.024(3) 0.017(2) 0.009(2) 0.015(2) C29 0.026(2) 0.045(3) 0.035(3) 0.022(2) 0.013(2) 0.022(2) C30 0.018(2) 0.021(2) 0.017(2) 0.0042(19) 0.0058(19) 0.0066(18) C31 0.011(2) 0.011(2) 0.013(2) 0.0031(17) -0.0006(18) 0.0024(17) C32 0.011(2) 0.016(2) 0.019(2) 0.0050(19) 0.0051(19) -0.0027(17) C33 0.013(2) 0.017(2) 0.019(3) 0.0076(19) 0.0081(19) -0.0003(18) C34 0.023(2) 0.029(3) 0.018(3) 0.008(2) 0.007(2) -0.002(2) C35 0.024(2) 0.044(3) 0.026(3) 0.008(2) 0.008(2) -0.010(2) C36 0.012(2) 0.016(2) 0.015(2) 0.0037(18) 0.0019(18) -0.0012(17) C37 0.0089(19) 0.013(2) 0.016(2) -0.0013(18) 0.0054(18) 0.0015(17) C38 0.017(2) 0.015(2) 0.019(3) -0.0013(19) 0.0070(19) 0.0014(18) C39 0.014(2) 0.019(2) 0.013(2) -0.0015(18) 0.0053(18) 0.0023(18) C40 0.037(3) 0.024(2) 0.016(3) -0.001(2) 0.012(2) 0.000(2) C41 0.042(3) 0.020(2) 0.029(3) -0.004(2) 0.015(2) 0.001(2) C42 0.019(2) 0.012(2) 0.019(2) 0.0015(18) 0.0088(19) 0.0024(18) C43 0.019(2) 0.013(2) 0.017(2) 0.0016(18) 0.0069(19) 0.0015(18) C44 0.012(2) 0.028(3) 0.032(3) 0.012(2) 0.003(2) 0.0033(19) C45 0.022(2) 0.025(2) 0.028(3) 0.013(2) 0.007(2) 0.005(2) C46 0.016(2) 0.020(2) 0.012(2) 0.0023(18) 0.0054(18) 0.0029(19) C47 0.037(3) 0.025(3) 0.097(5) 0.015(3) 0.046(3) 0.010(2) C48 0.041(3) 0.021(3) 0.060(4) 0.015(2) 0.032(3) 0.004(2) C49 0.020(2) 0.017(2) 0.017(2) 0.0055(19) 0.0073(19) 0.009(2) C50 0.017(2) 0.031(3) 0.055(4) -0.001(3) 0.000(2) 0.000(2) C51 0.031(3) 0.031(3) 0.061(4) 0.017(3) 0.015(3) 0.019(2) C52 0.061(4) 0.060(4) 0.033(4) 0.018(3) 0.029(3) 0.019(3) C53 0.059(4) 0.050(3) 0.033(3) 0.015(3) 0.018(3) 0.026(3) C54 0.058(4) 0.057(4) 0.059(4) 0.019(3) 0.023(3) 0.015(3) C55 0.030(3) 0.042(3) 0.090(5) 0.025(3) 0.021(3) 0.010(3) C56 0.117(6) 0.067(5) 0.028(4) 0.007(3) 0.015(4) -0.025(4) C57 0.015(2) 0.038(3) 0.046(3) 0.009(3) 0.001(2) 0.002(2) O1 0.0145(14) 0.0138(14) 0.0139(16) 0.0042(12) 0.0043(12) 0.0036(12) O2 0.0140(14) 0.0132(15) 0.0184(16) 0.0028(12) 0.0081(12) -0.0008(12) O3 0.0129(14) 0.0182(15) 0.0146(16) 0.0024(12) 0.0036(12) 0.0012(13) O4 0.077(3) 0.192(6) 0.056(3) 0.077(3) 0.050(3) 0.082(3) O5 0.046(3) 0.085(4) 0.195(6) 0.065(4) 0.015(3) 0.028(3) O6 0.143(12) 0.149(13) 0.069(7) 0.027(8) 0.039(9) -0.003(9) _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 Fe1 C1 1.910(4) . ? Fe1 C2 1.927(5) . ? Fe1 C3 1.927(4) . ? Fe1 N10 1.997(3) . ? Fe1 N12 2.001(3) . ? Fe1 N8 2.004(3) . ? Fe2 C6 1.901(4) . ? Fe2 C5 1.920(4) . ? Fe2 C4 1.927(4) . ? Fe2 N16 1.983(3) . ? Fe2 N14 1.986(3) . ? Fe2 N18 2.000(3) . ? Ni1 N6 2.011(3) . ? Ni1 N4 2.039(3) 2_776 ? Ni1 O2 2.059(2) . ? Ni1 N1 2.068(3) . ? Ni1 O1 2.079(2) . ? Ni1 O3 2.100(3) . ? B1 N9 1.529(5) . ? B1 N11 1.530(5) . ? B1 N7 1.533(5) . ? B2 N15 1.528(5) . ? B2 N17 1.538(5) . ? B2 N13 1.541(5) . ? N1 C1 1.159(5) . ? N2 C2 1.149(5) . ? N3 C3 1.161(5) . ? N4 C4 1.147(5) . ? N4 Ni1 2.039(3) 2_776 ? N5 C5 1.150(5) . ? N6 C6 1.154(4) . ? N7 C9 1.356(5) . ? N7 N8 1.378(4) . ? N8 C7 1.343(5) . ? N9 C15 1.358(5) . ? N9 N10 1.376(4) . ? N10 C13 1.336(5) . ? N11 C21 1.347(5) . ? N11 N12 1.376(4) . ? N12 C19 1.350(5) . ? N13 C27 1.342(5) . ? N13 N14 1.371(4) . ? N14 C25 1.352(5) . ? N15 C33 1.350(5) . ? N15 N16 1.368(4) . ? N16 C31 1.351(5) . ? N17 C39 1.354(5) . ? N17 N18 1.375(4) . ? N18 C37 1.351(5) . ? N19 C43 1.324(5) . ? N19 C45 1.455(5) . ? N19 C44 1.456(5) . ? N20 C46 1.321(5) . ? N20 C47 1.452(5) . ? N20 C48 1.453(5) . ? N21 C49 1.314(5) . ? N21 C51 1.453(5) . ? N21 C50 1.454(5) . ? N22 C52 1.277(6) . ? N22 C53 1.414(6) . ? N22 C54 1.506(6) . ? N23 C55 1.321(6) . ? N23 C56 1.419(6) . ? N23 C57 1.444(5) . ? C7 C8 1.396(5) . ? C7 C12 1.494(5) . ? C8 C9 1.379(5) . ? C8 C11 1.494(5) . ? C9 C10 1.508(5) . ? C13 C14 1.396(5) . ? C13 C18 1.497(6) . ? C14 C15 1.382(6) . ? C14 C17 1.486(5) . ? C15 C16 1.496(5) . ? C19 C20 1.397(5) . ? C19 C24 1.488(5) . ? C20 C21 1.384(6) . ? C20 C23 1.498(5) . ? C21 C22 1.497(6) . ? C25 C26 1.391(5) . ? C25 C30 1.495(5) . ? C26 C27 1.389(6) . ? C26 C29 1.501(5) . ? C27 C28 1.486(5) . ? C31 C32 1.399(5) . ? C31 C36 1.482(5) . ? C32 C33 1.377(5) . ? C32 C35 1.501(5) . ? C33 C34 1.487(5) . ? C37 C38 1.395(5) . ? C37 C42 1.484(5) . ? C38 C39 1.377(5) . ? C38 C41 1.509(5) . ? C39 C40 1.495(5) . ? C43 O1 1.239(4) . ? C46 O2 1.240(4) . ? C49 O3 1.243(4) . ? C52 O4 1.175(6) . ? C55 O5 1.229(6) . ? O6 O6 1.33(2) 2_675 ? 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 C1 Fe1 C2 86.49(16) . . ? C1 Fe1 C3 85.57(16) . . ? C2 Fe1 C3 85.44(16) . . ? C1 Fe1 N10 177.07(15) . . ? C2 Fe1 N10 90.92(15) . . ? C3 Fe1 N10 92.87(15) . . ? C1 Fe1 N12 94.24(14) . . ? C2 Fe1 N12 177.22(14) . . ? C3 Fe1 N12 91.94(15) . . ? N10 Fe1 N12 88.29(13) . . ? C1 Fe1 N8 92.44(14) . . ? C2 Fe1 N8 92.21(14) . . ? C3 Fe1 N8 177.00(15) . . ? N10 Fe1 N8 89.02(12) . . ? N12 Fe1 N8 90.44(12) . . ? C6 Fe2 C5 85.42(15) . . ? C6 Fe2 C4 91.80(15) . . ? C5 Fe2 C4 89.47(16) . . ? C6 Fe2 N16 179.39(15) . . ? C5 Fe2 N16 94.00(14) . . ? C4 Fe2 N16 88.00(14) . . ? C6 Fe2 N14 90.99(14) . . ? C5 Fe2 N14 176.27(15) . . ? C4 Fe2 N14 89.60(14) . . ? N16 Fe2 N14 89.58(12) . . ? C6 Fe2 N18 89.57(14) . . ? C5 Fe2 N18 91.90(14) . . ? C4 Fe2 N18 178.13(14) . . ? N16 Fe2 N18 90.64(12) . . ? N14 Fe2 N18 89.11(12) . . ? N6 Ni1 N4 87.17(12) . 2_776 ? N6 Ni1 O2 174.95(12) . . ? N4 Ni1 O2 88.02(11) 2_776 . ? N6 Ni1 N1 93.87(12) . . ? N4 Ni1 N1 178.77(12) 2_776 . ? O2 Ni1 N1 90.93(11) . . ? N6 Ni1 O1 94.92(11) . . ? N4 Ni1 O1 92.52(11) 2_776 . ? O2 Ni1 O1 86.81(10) . . ? N1 Ni1 O1 88.04(11) . . ? N6 Ni1 O3 95.44(11) . . ? N4 Ni1 O3 90.82(11) 2_776 . ? O2 Ni1 O3 83.10(10) . . ? N1 Ni1 O3 88.43(11) . . ? O1 Ni1 O3 169.25(10) . . ? N9 B1 N11 107.6(3) . . ? N9 B1 N7 108.6(3) . . ? N11 B1 N7 107.8(3) . . ? N15 B2 N17 107.9(3) . . ? N15 B2 N13 108.2(3) . . ? N17 B2 N13 108.0(3) . . ? C1 N1 Ni1 170.2(3) . . ? C4 N4 Ni1 177.1(3) . 2_776 ? C6 N6 Ni1 171.6(3) . . ? C9 N7 N8 109.5(3) . . ? C9 N7 B1 131.6(3) . . ? N8 N7 B1 119.0(3) . . ? C7 N8 N7 106.6(3) . . ? C7 N8 Fe1 135.7(3) . . ? N7 N8 Fe1 117.4(2) . . ? C15 N9 N10 109.5(3) . . ? C15 N9 B1 131.3(3) . . ? N10 N9 B1 119.0(3) . . ? C13 N10 N9 106.7(3) . . ? C13 N10 Fe1 135.5(3) . . ? N9 N10 Fe1 117.8(2) . . ? C21 N11 N12 110.1(3) . . ? C21 N11 B1 131.0(3) . . ? N12 N11 B1 118.8(3) . . ? C19 N12 N11 106.2(3) . . ? C19 N12 Fe1 135.8(3) . . ? N11 N12 Fe1 117.9(2) . . ? C27 N13 N14 109.5(3) . . ? C27 N13 B2 131.9(3) . . ? N14 N13 B2 118.5(3) . . ? C25 N14 N13 106.9(3) . . ? C25 N14 Fe2 135.5(3) . . ? N13 N14 Fe2 117.5(2) . . ? C33 N15 N16 109.8(3) . . ? C33 N15 B2 131.7(3) . . ? N16 N15 B2 118.4(3) . . ? C31 N16 N15 107.3(3) . . ? C31 N16 Fe2 134.8(3) . . ? N15 N16 Fe2 117.8(2) . . ? C39 N17 N18 109.6(3) . . ? C39 N17 B2 131.7(3) . . ? N18 N17 B2 118.6(3) . . ? C37 N18 N17 106.7(3) . . ? C37 N18 Fe2 135.6(3) . . ? N17 N18 Fe2 117.1(2) . . ? C43 N19 C45 122.1(3) . . ? C43 N19 C44 121.2(3) . . ? C45 N19 C44 116.4(3) . . ? C46 N20 C47 121.6(3) . . ? C46 N20 C48 121.1(3) . . ? C47 N20 C48 117.2(3) . . ? C49 N21 C51 121.0(4) . . ? C49 N21 C50 121.7(4) . . ? C51 N21 C50 117.3(3) . . ? C52 N22 C53 127.4(5) . . ? C52 N22 C54 117.0(4) . . ? C53 N22 C54 114.3(4) . . ? C55 N23 C56 121.8(5) . . ? C55 N23 C57 120.2(4) . . ? C56 N23 C57 117.8(5) . . ? N1 C1 Fe1 175.3(3) . . ? N2 C2 Fe1 178.2(4) . . ? N3 C3 Fe1 177.6(4) . . ? N4 C4 Fe2 172.9(3) . . ? N5 C5 Fe2 176.2(3) . . ? N6 C6 Fe2 176.4(3) . . ? N8 C7 C8 109.9(3) . . ? N8 C7 C12 123.9(3) . . ? C8 C7 C12 126.2(3) . . ? C9 C8 C7 105.9(3) . . ? C9 C8 C11 127.8(4) . . ? C7 C8 C11 126.3(4) . . ? N7 C9 C8 108.0(3) . . ? N7 C9 C10 122.3(4) . . ? C8 C9 C10 129.6(4) . . ? N10 C13 C14 110.4(4) . . ? N10 C13 C18 124.5(4) . . ? C14 C13 C18 125.1(4) . . ? C15 C14 C13 105.5(3) . . ? C15 C14 C17 127.7(4) . . ? C13 C14 C17 126.8(4) . . ? N9 C15 C14 108.0(3) . . ? N9 C15 C16 122.2(4) . . ? C14 C15 C16 129.8(4) . . ? N12 C19 C20 110.0(3) . . ? N12 C19 C24 123.5(4) . . ? C20 C19 C24 126.5(4) . . ? C21 C20 C19 105.6(3) . . ? C21 C20 C23 126.9(4) . . ? C19 C20 C23 127.5(4) . . ? N11 C21 C20 108.1(3) . . ? N11 C21 C22 122.3(4) . . ? C20 C21 C22 129.5(4) . . ? N14 C25 C26 109.6(3) . . ? N14 C25 C30 123.9(3) . . ? C26 C25 C30 126.5(3) . . ? C27 C26 C25 105.5(3) . . ? C27 C26 C29 128.2(4) . . ? C25 C26 C29 126.3(4) . . ? N13 C27 C26 108.5(3) . . ? N13 C27 C28 122.0(4) . . ? C26 C27 C28 129.5(4) . . ? N16 C31 C32 108.6(3) . . ? N16 C31 C36 124.0(3) . . ? C32 C31 C36 127.4(3) . . ? C33 C32 C31 106.6(3) . . ? C33 C32 C35 126.9(4) . . ? C31 C32 C35 126.4(4) . . ? N15 C33 C32 107.7(3) . . ? N15 C33 C34 122.3(3) . . ? C32 C33 C34 129.8(3) . . ? N18 C37 C38 109.4(3) . . ? N18 C37 C42 125.1(3) . . ? C38 C37 C42 125.4(3) . . ? C39 C38 C37 106.2(3) . . ? C39 C38 C41 127.4(4) . . ? C37 C38 C41 126.3(4) . . ? N17 C39 C38 108.0(3) . . ? N17 C39 C40 122.3(4) . . ? C38 C39 C40 129.7(4) . . ? O1 C43 N19 124.3(4) . . ? O2 C46 N20 122.6(4) . . ? O3 C49 N21 124.7(4) . . ? O4 C52 N22 131.4(5) . . ? O5 C55 N23 124.4(6) . . ? C43 O1 Ni1 126.3(3) . . ? C46 O2 Ni1 125.9(3) . . ? C49 O3 Ni1 116.5(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.126 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.088 # Attachment '- 2.cif' # {[(Tp*Me)Fe(CN)3]6[Ni(MeOH)3]s}.3H2O.8H2O (2) data_h12709 _database_code_depnum_ccdc_archive 'CCDC 810416' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71.75 H117.50 B3 Fe3 N27 Ni1.50 O8.75' _chemical_formula_weight 1786.47 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' 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.4570(16) _cell_length_b 17.2751(10) _cell_length_c 39.602(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.747(3) _cell_angle_gamma 90.00 _cell_volume 18689.7(19) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7536 _exptl_absorpt_coefficient_mu 0.816 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7314 _exptl_absorpt_correction_T_max 0.8972 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 163831 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 26.42 _reflns_number_total 19201 _reflns_number_gt 14776 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0766P)^2^+161.4222P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19201 _refine_ls_number_parameters 1086 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0974 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.2172 _refine_ls_wR_factor_gt 0.1965 _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_restrained_S_all 1.184 _refine_ls_shift/su_max 12.418 _refine_ls_shift/su_mean 0.125 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 Fe1 Fe 0.51001(2) -0.02203(4) 0.125100(16) 0.02212(16) Uani 1 1 d . . . Fe2 Fe 0.31895(2) 0.06743(5) 0.220289(18) 0.02865(18) Uani 1 1 d . . . Fe3 Fe 0.15037(2) -0.01276(4) 0.063945(17) 0.02289(16) Uani 1 1 d . . . Ni1 Ni 0.5000 0.02452(5) 0.2500 0.01899(18) Uani 1 2 d S . . Ni2 Ni 0.32850(2) 0.02491(4) 0.093981(16) 0.02400(15) Uani 1 1 d . . . B1 B 0.5862(2) 0.0305(4) 0.07911(14) 0.0295(12) Uani 1 1 d . . . H1 H 0.6115 0.0474 0.0642 0.035 Uiso 1 1 calc R . . B2 B 0.2305(2) 0.0230(4) 0.25727(16) 0.0332(13) Uani 1 1 d . . . H2 H 0.2016 0.0087 0.2695 0.040 Uiso 1 1 calc R . . B3 B 0.0544(2) 0.0307(4) 0.09232(15) 0.0310(13) Uani 1 1 d . . . H3 H 0.0232 0.0451 0.1017 0.037 Uiso 1 1 calc R . . N1 N 0.50585(16) 0.0216(4) 0.19946(12) 0.0509(16) Uani 1 1 d . . . N2 N 0.40076(15) 0.0034(3) 0.10310(11) 0.0281(9) Uani 1 1 d . . . N3 N 0.4785(2) -0.1752(4) 0.15497(15) 0.0573(16) Uani 1 1 d . . . N4 N 0.32560(14) 0.0309(2) 0.14496(11) 0.0260(9) Uani 1 1 d . . . N5 N 0.3689(3) 0.2195(5) 0.2042(2) 0.104(3) Uani 1 1 d . . . N6 N 0.42643(17) 0.0270(4) 0.24003(12) 0.063(2) Uani 1 1 d . . . N7 N 0.20737(19) -0.1647(3) 0.06204(14) 0.0473(13) Uani 1 1 d . . . N8 N 0.25519(15) 0.0401(3) 0.08514(11) 0.0301(9) Uani 1 1 d . . . N9 N 0.17238(18) 0.0117(3) -0.00981(12) 0.0396(11) Uani 1 1 d . . . N10 N 0.55972(16) 0.1004(2) 0.09213(11) 0.0320(10) Uani 1 1 d . . . N11 N 0.52362(16) 0.0869(2) 0.11284(12) 0.0339(10) Uani 1 1 d . . . N12 N 0.54890(14) -0.0234(2) 0.05985(10) 0.0223(8) Uani 1 1 d . . . N13 N 0.51289(13) -0.0551(2) 0.07702(9) 0.0206(8) Uani 1 1 d . . . N14 N 0.61009(14) -0.0151(2) 0.11006(10) 0.0260(9) Uani 1 1 d . . . N15 N 0.58112(14) -0.0413(2) 0.13395(9) 0.0233(8) Uani 1 1 d . . . N16 N 0.25623(17) -0.0496(3) 0.24558(12) 0.0366(11) Uani 1 1 d . . . N17 N 0.29681(16) -0.0396(3) 0.22882(11) 0.0337(10) Uani 1 1 d . . . N18 N 0.21493(14) 0.0727(3) 0.22625(11) 0.0284(9) Uani 1 1 d . . . N19 N 0.24971(14) 0.0988(2) 0.20682(10) 0.0265(9) Uani 1 1 d . . . N20 N 0.26798(16) 0.0700(3) 0.28037(11) 0.0336(10) Uani 1 1 d . . . N21 N 0.31062(15) 0.0938(3) 0.26831(11) 0.0347(11) Uani 1 1 d . . . N22 N 0.08120(15) 0.1026(2) 0.08130(11) 0.0284(9) Uani 1 1 d . . . N23 N 0.12386(15) 0.0938(2) 0.06651(11) 0.0282(9) Uani 1 1 d . . . N24 N 0.08917(14) -0.0117(3) 0.11896(11) 0.0278(9) Uani 1 1 d . . . N25 N 0.13523(14) -0.0316(2) 0.11149(11) 0.0268(9) Uani 1 1 d . . . N26 N 0.04484(14) -0.0225(2) 0.06163(11) 0.0266(9) Uani 1 1 d . . . N27 N 0.08376(14) -0.0522(2) 0.04688(10) 0.0258(9) Uani 1 1 d . . . C1 C 0.50670(18) 0.0075(4) 0.17149(13) 0.0361(13) Uani 1 1 d . . . C2 C 0.44103(18) -0.0055(3) 0.11300(12) 0.0258(10) Uani 1 1 d . . . C3 C 0.49132(19) -0.1203(3) 0.14243(13) 0.0320(12) Uani 1 1 d . . . C4 C 0.32467(16) 0.0428(3) 0.17359(13) 0.0263(10) Uani 1 1 d . . . C5 C 0.3476(2) 0.1654(5) 0.21061(18) 0.058(2) Uani 1 1 d . . . C6 C 0.38589(19) 0.0403(4) 0.23252(14) 0.0469(17) Uani 1 1 d . . . C7 C 0.18280(18) -0.1110(3) 0.06207(14) 0.0315(11) Uani 1 1 d . . . C8 C 0.21474(18) 0.0233(3) 0.07786(13) 0.0291(11) Uani 1 1 d . . . C9 C 0.16390(18) 0.0033(3) 0.01757(14) 0.0286(11) Uani 1 1 d . . . C10 C 0.5075(2) 0.1567(3) 0.12178(17) 0.0469(16) Uani 1 1 d . . . C11 C 0.5329(3) 0.2139(4) 0.10701(18) 0.057(2) Uani 1 1 d . . . C12 C 0.5661(3) 0.1775(3) 0.08852(16) 0.0484(17) Uani 1 1 d . . . C13 C 0.6035(3) 0.2122(4) 0.06802(18) 0.068(2) Uani 1 1 d . . . H13A H 0.6125 0.1744 0.0513 0.103 Uiso 1 1 calc R . . H13B H 0.6326 0.2265 0.0831 0.103 Uiso 1 1 calc R . . H13C H 0.5898 0.2584 0.0563 0.103 Uiso 1 1 calc R . . C14 C 0.5267(4) 0.3004(4) 0.1108(2) 0.085(3) Uani 1 1 d . . . H14A H 0.4922 0.3142 0.1054 0.127 Uiso 1 1 calc R . . H14B H 0.5465 0.3274 0.0952 0.127 Uiso 1 1 calc R . . H14C H 0.5374 0.3157 0.1341 0.127 Uiso 1 1 calc R . . C15 C 0.4684(3) 0.1669(4) 0.1453(2) 0.072(2) Uani 1 1 d . . . H15A H 0.4465 0.1220 0.1434 0.108 Uiso 1 1 calc R . . H15B H 0.4496 0.2139 0.1392 0.108 Uiso 1 1 calc R . . H15C H 0.4836 0.1713 0.1687 0.108 Uiso 1 1 calc R . . C16 C 0.48680(17) -0.1028(3) 0.05533(11) 0.0219(9) Uani 1 1 d . . . C17 C 0.50611(18) -0.1018(3) 0.02428(12) 0.0255(10) Uani 1 1 d . . . C18 C 0.54526(18) -0.0513(3) 0.02792(12) 0.0264(10) Uani 1 1 d . . . C19 C 0.5804(2) -0.0306(4) 0.00304(13) 0.0354(12) Uani 1 1 d . . . H19A H 0.5926 0.0220 0.0076 0.053 Uiso 1 1 calc R . . H19B H 0.5638 -0.0333 -0.0200 0.053 Uiso 1 1 calc R . . H19C H 0.6079 -0.0671 0.0052 0.053 Uiso 1 1 calc R . . C20 C 0.4886(2) -0.1460(3) -0.00725(14) 0.0411(14) Uani 1 1 d . . . H20A H 0.4989 -0.1192 -0.0271 0.062 Uiso 1 1 calc R . . H20B H 0.4528 -0.1494 -0.0092 0.062 Uiso 1 1 calc R . . H20C H 0.5026 -0.1982 -0.0060 0.062 Uiso 1 1 calc R . . C21 C 0.44286(18) -0.1471(3) 0.06355(13) 0.0292(11) Uani 1 1 d . . . H21A H 0.4453 -0.1576 0.0880 0.044 Uiso 1 1 calc R . . H21B H 0.4411 -0.1961 0.0511 0.044 Uiso 1 1 calc R . . H21C H 0.4133 -0.1165 0.0570 0.044 Uiso 1 1 calc R . . C22 C 0.61144(17) -0.0781(3) 0.15794(12) 0.0248(10) Uani 1 1 d . . . C23 C 0.65907(18) -0.0768(3) 0.14871(12) 0.0271(10) Uani 1 1 d . . . C24 C 0.65678(18) -0.0362(3) 0.11840(13) 0.0287(11) Uani 1 1 d . . . C25 C 0.69639(19) -0.0178(4) 0.09664(15) 0.0413(14) Uani 1 1 d . . . H25A H 0.6981 0.0383 0.0934 0.062 Uiso 1 1 calc R . . H25B H 0.6894 -0.0432 0.0746 0.062 Uiso 1 1 calc R . . H25C H 0.7278 -0.0365 0.1076 0.062 Uiso 1 1 calc R . . C26 C 0.70348(19) -0.1109(3) 0.16822(14) 0.0354(12) Uani 1 1 d . . . H26A H 0.6955 -0.1621 0.1767 0.053 Uiso 1 1 calc R . . H26B H 0.7143 -0.0770 0.1874 0.053 Uiso 1 1 calc R . . H26C H 0.7297 -0.1157 0.1533 0.053 Uiso 1 1 calc R . . C27 C 0.59493(19) -0.1137(3) 0.18925(13) 0.0328(12) Uani 1 1 d . . . H27A H 0.5844 -0.0729 0.2041 0.049 Uiso 1 1 calc R . . H27B H 0.6221 -0.1428 0.2012 0.049 Uiso 1 1 calc R . . H27C H 0.5675 -0.1489 0.1830 0.049 Uiso 1 1 calc R . . C28 C 0.3139(2) -0.1107(4) 0.22237(14) 0.0430(15) Uani 1 1 d . . . C29 C 0.2841(3) -0.1665(4) 0.23524(15) 0.0478(16) Uani 1 1 d . . . C30 C 0.2486(2) -0.1266(4) 0.24958(15) 0.0434(14) Uani 1 1 d . . . C31 C 0.2077(3) -0.1580(4) 0.26846(18) 0.0544(18) Uani 1 1 d . . . H31A H 0.1868 -0.1152 0.2745 0.082 Uiso 1 1 calc R . . H31B H 0.2216 -0.1842 0.2892 0.082 Uiso 1 1 calc R . . H31C H 0.1882 -0.1949 0.2540 0.082 Uiso 1 1 calc R . . C32 C 0.2900(3) -0.2524(4) 0.23361(19) 0.069(2) Uani 1 1 d . . . H32A H 0.2620 -0.2776 0.2426 0.104 Uiso 1 1 calc R . . H32B H 0.3203 -0.2677 0.2472 0.104 Uiso 1 1 calc R . . H32C H 0.2916 -0.2682 0.2100 0.104 Uiso 1 1 calc R . . C33 C 0.3591(3) -0.1257(4) 0.20529(16) 0.058(2) Uani 1 1 d . . . H33A H 0.3625 -0.0858 0.1881 0.087 Uiso 1 1 calc R . . H33B H 0.3568 -0.1767 0.1944 0.087 Uiso 1 1 calc R . . H33C H 0.3878 -0.1244 0.2222 0.087 Uiso 1 1 calc R . . C34 C 0.22666(18) 0.1401(3) 0.18110(13) 0.0288(11) Uani 1 1 d . . . C35 C 0.17649(18) 0.1406(3) 0.18432(13) 0.0303(11) Uani 1 1 d . . . C36 C 0.17032(17) 0.0983(3) 0.21308(14) 0.0301(11) Uani 1 1 d . . . C37 C 0.12468(19) 0.0840(4) 0.22976(16) 0.0410(14) Uani 1 1 d . . . H37A H 0.1198 0.0282 0.2322 0.062 Uiso 1 1 calc R . . H37B H 0.0966 0.1062 0.2158 0.062 Uiso 1 1 calc R . . H37C H 0.1276 0.1084 0.2522 0.062 Uiso 1 1 calc R . . C38 C 0.1373(2) 0.1774(4) 0.16044(16) 0.0432(14) Uani 1 1 d . . . H38A H 0.1073 0.1822 0.1717 0.065 Uiso 1 1 calc R . . H38B H 0.1310 0.1451 0.1401 0.065 Uiso 1 1 calc R . . H38C H 0.1481 0.2288 0.1539 0.065 Uiso 1 1 calc R . . C39 C 0.2513(2) 0.1785(3) 0.15367(15) 0.0389(13) Uani 1 1 d . . . H39A H 0.2859 0.1870 0.1615 0.058 Uiso 1 1 calc R . . H39B H 0.2355 0.2283 0.1480 0.058 Uiso 1 1 calc R . . H39C H 0.2487 0.1454 0.1335 0.058 Uiso 1 1 calc R . . C40 C 0.33618(19) 0.1328(4) 0.29375(14) 0.0374(13) Uani 1 1 d . . . C41 C 0.3095(2) 0.1349(4) 0.32196(13) 0.0391(14) Uani 1 1 d . . . C42 C 0.2668(2) 0.0948(3) 0.31262(13) 0.0365(13) Uani 1 1 d . . . C43 C 0.2243(2) 0.0794(4) 0.33261(15) 0.0495(16) Uani 1 1 d . . . H43A H 0.1945 0.1020 0.3208 0.074 Uiso 1 1 calc R . . H43B H 0.2306 0.1027 0.3552 0.074 Uiso 1 1 calc R . . H43C H 0.2199 0.0234 0.3349 0.074 Uiso 1 1 calc R . . C44 C 0.3248(2) 0.1730(4) 0.35530(14) 0.0472(16) Uani 1 1 d . . . H44A H 0.2958 0.1832 0.3672 0.071 Uiso 1 1 calc R . . H44B H 0.3414 0.2219 0.3514 0.071 Uiso 1 1 calc R . . H44C H 0.3471 0.1387 0.3692 0.071 Uiso 1 1 calc R . . C45 C 0.3858(2) 0.1649(4) 0.29187(17) 0.0531(19) Uani 1 1 d . . . H45A H 0.3857 0.1985 0.2719 0.080 Uiso 1 1 calc R . . H45B H 0.4091 0.1225 0.2901 0.080 Uiso 1 1 calc R . . H45C H 0.3955 0.1951 0.3124 0.080 Uiso 1 1 calc R . . C46 C 0.1402(2) 0.1651(3) 0.06027(14) 0.0327(12) Uani 1 1 d . . . C47 C 0.1082(2) 0.2198(3) 0.07107(14) 0.0383(13) Uani 1 1 d . . . C48 C 0.0714(2) 0.1790(3) 0.08426(14) 0.0350(12) Uani 1 1 d . . . C49 C 0.0275(2) 0.2070(4) 0.10008(16) 0.0493(16) Uani 1 1 d . . . H49A H 0.0279 0.2637 0.1011 0.074 Uiso 1 1 calc R . . H49B H 0.0280 0.1861 0.1231 0.074 Uiso 1 1 calc R . . H49C H -0.0023 0.1897 0.0864 0.074 Uiso 1 1 calc R . . C50 C 0.1143(3) 0.3063(3) 0.07001(19) 0.0535(18) Uani 1 1 d . . . H50A H 0.0869 0.3312 0.0799 0.080 Uiso 1 1 calc R . . H50B H 0.1148 0.3231 0.0464 0.080 Uiso 1 1 calc R . . H50C H 0.1451 0.3209 0.0831 0.080 Uiso 1 1 calc R . . C51 C 0.1855(2) 0.1816(4) 0.04396(17) 0.0456(15) Uani 1 1 d . . . H51A H 0.1926 0.1381 0.0294 0.068 Uiso 1 1 calc R . . H51B H 0.2129 0.1890 0.0615 0.068 Uiso 1 1 calc R . . H51C H 0.1808 0.2287 0.0302 0.068 Uiso 1 1 calc R . . C52 C 0.15745(18) -0.0667(3) 0.13921(12) 0.0274(10) Uani 1 1 d . . . C53 C 0.12483(19) -0.0715(3) 0.16404(13) 0.0295(11) Uani 1 1 d . . . C54 C 0.08244(19) -0.0360(3) 0.15040(13) 0.0301(11) Uani 1 1 d . . . C55 C 0.0352(2) -0.0224(4) 0.16567(15) 0.0409(13) Uani 1 1 d . . . H55A H 0.0081 -0.0450 0.1510 0.061 Uiso 1 1 calc R . . H55B H 0.0299 0.0334 0.1679 0.061 Uiso 1 1 calc R . . H55C H 0.0369 -0.0467 0.1881 0.061 Uiso 1 1 calc R . . C56 C 0.1352(2) -0.1089(4) 0.19787(14) 0.0395(13) Uani 1 1 d . . . H56A H 0.1502 -0.1597 0.1951 0.059 Uiso 1 1 calc R . . H56B H 0.1046 -0.1154 0.2083 0.059 Uiso 1 1 calc R . . H56C H 0.1577 -0.0763 0.2125 0.059 Uiso 1 1 calc R . . C57 C 0.20916(19) -0.0934(4) 0.14269(14) 0.0361(12) Uani 1 1 d . . . H57A H 0.2302 -0.0524 0.1350 0.054 Uiso 1 1 calc R . . H57B H 0.2121 -0.1397 0.1288 0.054 Uiso 1 1 calc R . . H57C H 0.2193 -0.1055 0.1665 0.054 Uiso 1 1 calc R . . C58 C 0.06511(19) -0.0987(3) 0.02146(13) 0.0276(10) Uani 1 1 d . . . C59 C 0.01411(19) -0.0984(3) 0.02006(14) 0.0325(12) Uani 1 1 d . . . C60 C 0.00276(18) -0.0503(3) 0.04560(14) 0.0302(11) Uani 1 1 d . . . C61 C -0.0464(2) -0.0289(4) 0.05625(17) 0.0449(15) Uani 1 1 d . . . H61A H -0.0476 0.0270 0.0601 0.067 Uiso 1 1 calc R . . H61B H -0.0517 -0.0563 0.0772 0.067 Uiso 1 1 calc R . . H61C H -0.0720 -0.0435 0.0383 0.067 Uiso 1 1 calc R . . C62 C -0.0220(2) -0.1403(4) -0.00439(17) 0.0476(16) Uani 1 1 d . . . H62A H -0.0463 -0.1035 -0.0147 0.071 Uiso 1 1 calc R . . H62B H -0.0386 -0.1804 0.0078 0.071 Uiso 1 1 calc R . . H62C H -0.0048 -0.1645 -0.0222 0.071 Uiso 1 1 calc R . . C63 C 0.0965(2) -0.1417(3) -0.00085(14) 0.0360(12) Uani 1 1 d . . . H63A H 0.1274 -0.1559 0.0122 0.054 Uiso 1 1 calc R . . H63B H 0.1033 -0.1087 -0.0200 0.054 Uiso 1 1 calc R . . H63C H 0.0795 -0.1886 -0.0094 0.054 Uiso 1 1 calc R . . O1 O 0.4893(2) -0.0951(4) 0.23604(16) 0.0253(14) Uani 0.50 1 d P . . C64 C 0.5000 -0.1595(6) 0.2500 0.098(6) Uani 1 2 d S . . O2 O 0.4848(3) 0.1429(4) 0.24140(17) 0.0291(15) Uani 0.50 1 d P . . C65 C 0.4965(5) 0.2080(7) 0.2396(3) 0.045(3) Uani 0.50 1 d P . . O3 O 0.31272(14) -0.0954(2) 0.08988(10) 0.0371(9) Uani 1 1 d . . . C66 C 0.3299(3) -0.1502(4) 0.11407(18) 0.0508(16) Uani 1 1 d . . . H66A H 0.3292 -0.2016 0.1036 0.076 Uiso 1 1 calc R . . H66B H 0.3089 -0.1502 0.1327 0.076 Uiso 1 1 calc R . . H66C H 0.3635 -0.1374 0.1229 0.076 Uiso 1 1 calc R . . O4 O 0.33064(14) 0.0164(3) 0.04108(10) 0.0417(10) Uani 1 1 d . . . C67 C 0.2980(2) 0.0640(6) 0.01730(18) 0.067(2) Uani 1 1 d . . . H67A H 0.3100 0.0632 -0.0052 0.100 Uiso 1 1 calc R . . H67B H 0.2977 0.1173 0.0256 0.100 Uiso 1 1 calc R . . H67C H 0.2647 0.0428 0.0157 0.100 Uiso 1 1 calc R . . O5 O 0.34227(15) 0.1427(2) 0.08887(12) 0.0448(10) Uani 1 1 d . . . C68 C 0.3839(3) 0.1721(5) 0.0705(3) 0.074(3) Uani 1 1 d . . . H68A H 0.4002 0.2150 0.0833 0.111 Uiso 1 1 calc R . . H68B H 0.3712 0.1903 0.0479 0.111 Uiso 1 1 calc R . . H68C H 0.4075 0.1302 0.0683 0.111 Uiso 1 1 calc R . . O6 O 0.2912(2) 0.2750(3) 0.08569(16) 0.0776(16) Uani 1 1 d . . . C69 C 0.2897(4) 0.3208(7) 0.0543(3) 0.096(3) Uani 1 1 d . . . O7 O 0.3242(3) -0.1119(4) 0.00326(16) 0.107(3) Uani 1 1 d . . . C70 C 0.3150(3) -0.1883(6) 0.0147(3) 0.092(3) Uani 1 1 d . . . O8 O 0.2402(3) -0.0721(5) -0.04397(19) 0.0365(17) Uani 0.50 1 d P A 1 C71 C 0.2201(6) -0.1400(7) -0.0573(4) 0.052(3) Uani 0.50 1 d P A 1 O81 O 0.2840(6) -0.1638(8) -0.0543(4) 0.103(4) Uani 0.50 1 d P B 2 O9 O 0.3925(3) 0.3442(5) 0.1731(2) 0.147(3) Uiso 1 1 d . . . C72 C 0.4201(5) 0.3995(9) 0.2005(4) 0.164(5) Uiso 1 1 d . . . O10 O 0.8215(3) -0.1090(4) 0.12834(18) 0.119(2) Uiso 1 1 d . . . C73 C 0.8463(6) -0.0488(9) 0.1084(4) 0.162(5) Uiso 1 1 d . . . O11 O 0.4888(4) -0.3233(7) 0.1877(3) 0.189(4) Uiso 1 1 d . . . C74 C 0.4376(9) -0.3414(14) 0.1831(6) 0.238(9) Uiso 1 1 d . . . O12 O 0.5000 -0.3994(12) 0.2500 0.241(7) Uiso 1 2 d S . . 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 Fe1 0.0193(3) 0.0296(4) 0.0170(3) -0.0024(3) -0.0003(2) 0.0074(3) Fe2 0.0146(3) 0.0439(4) 0.0267(4) -0.0142(3) -0.0014(3) 0.0026(3) Fe3 0.0169(3) 0.0247(3) 0.0260(4) 0.0007(3) -0.0028(3) 0.0027(3) Ni1 0.0156(4) 0.0227(4) 0.0176(4) 0.000 -0.0031(3) 0.000 Ni2 0.0162(3) 0.0290(3) 0.0264(3) -0.0026(3) 0.0002(2) 0.0022(2) B1 0.027(3) 0.037(3) 0.024(3) 0.007(2) -0.001(2) -0.007(2) B2 0.024(3) 0.045(4) 0.030(3) 0.004(3) 0.001(2) 0.002(3) B3 0.019(3) 0.041(3) 0.032(3) -0.005(3) -0.003(2) 0.010(2) N1 0.016(2) 0.109(5) 0.026(3) -0.025(3) -0.0051(18) 0.021(3) N2 0.020(2) 0.035(2) 0.029(2) -0.0003(18) 0.0026(17) 0.0093(17) N3 0.049(3) 0.065(4) 0.061(4) 0.037(3) 0.021(3) 0.009(3) N4 0.0152(18) 0.032(2) 0.029(2) -0.0056(18) -0.0033(16) 0.0069(16) N5 0.107(6) 0.097(5) 0.124(7) -0.075(5) 0.091(5) -0.074(5) N6 0.021(2) 0.144(6) 0.021(2) -0.033(3) -0.0041(19) 0.018(3) N7 0.046(3) 0.044(3) 0.054(3) 0.009(2) 0.016(2) 0.018(2) N8 0.021(2) 0.042(2) 0.027(2) 0.0013(19) -0.0010(17) 0.0002(18) N9 0.036(3) 0.049(3) 0.034(3) 0.004(2) 0.001(2) -0.001(2) N10 0.036(2) 0.029(2) 0.028(2) 0.0021(18) -0.0121(19) -0.0058(19) N11 0.034(2) 0.023(2) 0.041(3) -0.0068(19) -0.014(2) 0.0059(18) N12 0.0199(19) 0.029(2) 0.0179(19) 0.0040(16) 0.0026(15) 0.0002(16) N13 0.0185(18) 0.026(2) 0.0174(18) 0.0023(15) 0.0021(14) 0.0012(15) N14 0.021(2) 0.034(2) 0.021(2) 0.0026(17) -0.0028(16) -0.0002(17) N15 0.0211(19) 0.033(2) 0.0154(18) -0.0015(16) -0.0008(15) 0.0056(16) N16 0.034(2) 0.042(3) 0.032(2) 0.004(2) -0.005(2) 0.005(2) N17 0.029(2) 0.047(3) 0.024(2) -0.0018(19) -0.0028(18) 0.012(2) N18 0.0159(19) 0.038(2) 0.031(2) -0.0016(19) -0.0012(16) -0.0009(17) N19 0.0198(19) 0.035(2) 0.025(2) -0.0057(18) 0.0011(16) 0.0005(17) N20 0.026(2) 0.049(3) 0.024(2) -0.002(2) -0.0016(17) 0.008(2) N21 0.0166(19) 0.060(3) 0.026(2) -0.014(2) -0.0020(17) 0.006(2) N22 0.025(2) 0.029(2) 0.030(2) -0.0075(18) -0.0061(17) 0.0076(17) N23 0.029(2) 0.025(2) 0.029(2) -0.0024(17) -0.0058(17) 0.0008(17) N24 0.0189(19) 0.035(2) 0.029(2) -0.0052(18) -0.0006(16) 0.0043(17) N25 0.0171(19) 0.035(2) 0.027(2) -0.0010(18) -0.0030(16) 0.0014(17) N26 0.0176(19) 0.030(2) 0.031(2) -0.0019(18) -0.0028(16) 0.0021(16) N27 0.022(2) 0.026(2) 0.028(2) -0.0028(17) -0.0039(16) 0.0032(16) C1 0.017(2) 0.062(4) 0.027(3) -0.015(3) -0.005(2) 0.014(2) C2 0.026(3) 0.031(3) 0.020(2) -0.0024(19) 0.0042(19) 0.008(2) C3 0.031(3) 0.042(3) 0.024(3) 0.007(2) 0.006(2) 0.012(2) C4 0.012(2) 0.034(3) 0.032(3) -0.007(2) -0.0017(18) 0.0031(19) C5 0.038(3) 0.078(5) 0.063(4) -0.046(4) 0.029(3) -0.024(3) C6 0.022(3) 0.094(5) 0.023(3) -0.029(3) -0.003(2) 0.013(3) C7 0.025(2) 0.033(3) 0.037(3) 0.010(2) 0.005(2) 0.009(2) C8 0.023(3) 0.038(3) 0.024(2) 0.004(2) -0.0035(19) 0.000(2) C9 0.021(2) 0.030(3) 0.033(3) 0.002(2) -0.003(2) 0.003(2) C10 0.050(4) 0.032(3) 0.053(4) -0.014(3) -0.024(3) 0.012(3) C11 0.081(5) 0.027(3) 0.054(4) -0.008(3) -0.035(4) 0.003(3) C12 0.068(4) 0.029(3) 0.041(3) 0.010(3) -0.033(3) -0.016(3) C13 0.093(6) 0.051(4) 0.051(4) 0.023(3) -0.037(4) -0.041(4) C14 0.128(8) 0.027(3) 0.088(6) -0.010(4) -0.046(6) 0.003(4) C15 0.071(5) 0.049(4) 0.091(6) -0.036(4) -0.012(4) 0.033(4) C16 0.022(2) 0.023(2) 0.020(2) 0.0007(18) -0.0023(18) 0.0049(18) C17 0.029(2) 0.029(2) 0.017(2) -0.0021(19) -0.0014(19) 0.008(2) C18 0.027(2) 0.032(3) 0.020(2) 0.003(2) 0.0051(19) 0.007(2) C19 0.034(3) 0.050(3) 0.025(3) 0.008(2) 0.009(2) 0.008(2) C20 0.057(4) 0.040(3) 0.025(3) -0.008(2) -0.003(3) 0.003(3) C21 0.026(2) 0.027(3) 0.033(3) -0.005(2) -0.003(2) -0.004(2) C22 0.025(2) 0.029(2) 0.020(2) -0.0045(19) -0.0002(18) 0.007(2) C23 0.025(2) 0.030(3) 0.024(2) -0.010(2) -0.0068(19) 0.006(2) C24 0.022(2) 0.035(3) 0.029(3) -0.007(2) 0.000(2) -0.003(2) C25 0.023(3) 0.062(4) 0.039(3) 0.000(3) 0.003(2) -0.009(3) C26 0.026(3) 0.038(3) 0.039(3) -0.007(2) -0.009(2) 0.009(2) C27 0.030(3) 0.044(3) 0.024(3) 0.006(2) 0.001(2) 0.015(2) C28 0.057(4) 0.040(3) 0.028(3) -0.001(2) -0.013(3) 0.020(3) C29 0.067(4) 0.042(3) 0.030(3) 0.003(3) -0.019(3) 0.013(3) C30 0.051(4) 0.041(3) 0.034(3) 0.006(3) -0.016(3) -0.002(3) C31 0.055(4) 0.051(4) 0.053(4) 0.012(3) -0.018(3) -0.014(3) C32 0.107(7) 0.046(4) 0.050(4) 0.002(3) -0.018(4) 0.018(4) C33 0.074(5) 0.066(4) 0.032(3) 0.000(3) -0.001(3) 0.041(4) C34 0.029(3) 0.028(3) 0.029(3) -0.009(2) 0.001(2) 0.005(2) C35 0.027(2) 0.030(3) 0.032(3) -0.011(2) -0.009(2) 0.004(2) C36 0.015(2) 0.034(3) 0.039(3) -0.010(2) -0.005(2) 0.002(2) C37 0.021(3) 0.045(3) 0.056(4) -0.007(3) 0.002(2) -0.002(2) C38 0.040(3) 0.040(3) 0.045(3) -0.008(3) -0.018(3) 0.009(3) C39 0.050(3) 0.030(3) 0.039(3) 0.000(2) 0.017(3) 0.012(3) C40 0.025(3) 0.052(3) 0.034(3) -0.020(3) -0.005(2) 0.013(2) C41 0.041(3) 0.051(3) 0.023(3) -0.009(2) -0.007(2) 0.024(3) C42 0.038(3) 0.047(3) 0.023(3) 0.002(2) -0.002(2) 0.014(3) C43 0.053(4) 0.069(4) 0.027(3) 0.008(3) 0.008(3) 0.016(3) C44 0.056(4) 0.057(4) 0.026(3) -0.012(3) -0.008(3) 0.020(3) C45 0.024(3) 0.083(5) 0.051(4) -0.044(4) -0.004(3) 0.005(3) C46 0.035(3) 0.027(3) 0.033(3) 0.000(2) -0.011(2) 0.002(2) C47 0.047(3) 0.027(3) 0.036(3) -0.004(2) -0.019(3) 0.004(2) C48 0.039(3) 0.031(3) 0.032(3) -0.005(2) -0.013(2) 0.011(2) C49 0.053(4) 0.048(4) 0.045(4) -0.009(3) -0.008(3) 0.027(3) C50 0.064(4) 0.030(3) 0.061(4) -0.007(3) -0.018(3) 0.008(3) C51 0.042(3) 0.035(3) 0.057(4) 0.007(3) -0.007(3) -0.006(3) C52 0.024(2) 0.031(3) 0.026(2) 0.002(2) -0.0031(19) 0.000(2) C53 0.029(3) 0.035(3) 0.024(2) -0.004(2) -0.001(2) -0.005(2) C54 0.028(3) 0.034(3) 0.027(3) -0.010(2) -0.001(2) -0.002(2) C55 0.034(3) 0.052(4) 0.037(3) -0.009(3) 0.007(2) 0.006(3) C56 0.047(3) 0.045(3) 0.025(3) 0.000(2) -0.002(2) -0.005(3) C57 0.026(3) 0.049(3) 0.032(3) 0.014(2) -0.004(2) 0.005(2) C58 0.034(3) 0.022(2) 0.026(2) 0.0020(19) -0.003(2) 0.000(2) C59 0.029(3) 0.034(3) 0.032(3) 0.005(2) -0.013(2) -0.005(2) C60 0.019(2) 0.033(3) 0.036(3) 0.006(2) -0.010(2) 0.000(2) C61 0.023(3) 0.058(4) 0.051(4) 0.004(3) -0.008(2) 0.004(3) C62 0.047(4) 0.038(3) 0.052(4) -0.001(3) -0.025(3) -0.009(3) C63 0.046(3) 0.031(3) 0.029(3) -0.006(2) -0.003(2) 0.000(2) O1 0.032(4) 0.023(3) 0.019(3) -0.006(3) -0.007(3) -0.002(3) C64 0.175(15) 0.024(5) 0.112(11) 0.000 0.103(11) 0.000 O2 0.042(5) 0.023(3) 0.023(4) 0.001(3) 0.005(3) -0.003(3) C65 0.041(7) 0.047(7) 0.048(9) 0.012(5) 0.011(8) 0.014(6) O3 0.043(2) 0.0264(19) 0.042(2) -0.0065(16) 0.0033(17) -0.0020(16) C66 0.051(4) 0.043(3) 0.058(4) 0.004(3) 0.002(3) 0.007(3) O4 0.0254(19) 0.072(3) 0.027(2) 0.0045(19) 0.0026(15) -0.0019(19) C67 0.033(3) 0.125(7) 0.042(4) 0.026(4) 0.000(3) 0.008(4) O5 0.036(2) 0.030(2) 0.065(3) 0.0078(19) -0.006(2) 0.0010(17) C68 0.048(4) 0.055(4) 0.121(8) 0.024(5) 0.016(4) 0.000(4) O6 0.094(4) 0.058(3) 0.084(4) 0.009(3) 0.026(3) 0.010(3) C69 0.080(6) 0.120(8) 0.090(7) 0.050(6) 0.030(5) 0.015(6) O7 0.116(5) 0.133(6) 0.080(4) -0.063(4) 0.050(4) -0.085(5) C70 0.062(5) 0.084(6) 0.135(9) -0.062(6) 0.037(5) -0.023(5) O8 0.033(4) 0.044(4) 0.034(4) 0.003(3) 0.012(3) -0.002(3) C71 0.075(9) 0.029(6) 0.054(8) -0.021(6) 0.023(7) -0.013(6) O81 0.133(13) 0.069(8) 0.109(11) -0.004(8) 0.025(9) 0.005(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 1.918(5) . ? Fe1 C3 1.920(6) . ? Fe1 C2 1.928(5) . ? Fe1 N15 1.977(4) . ? Fe1 N11 1.988(5) . ? Fe1 N13 1.997(4) . ? Fe2 C6 1.912(5) . ? Fe2 C5 1.920(8) . ? Fe2 C4 1.920(5) . ? Fe2 N17 1.986(5) . ? Fe2 N21 1.991(4) . ? Fe2 N19 1.997(4) . ? Fe3 C8 1.903(5) . ? Fe3 C7 1.921(5) . ? Fe3 C9 1.930(5) . ? Fe3 N23 1.985(4) . ? Fe3 N25 1.995(4) . ? Fe3 N27 2.004(4) . ? Ni1 N6 2.020(5) . ? Ni1 N6 2.020(5) 2_655 ? Ni1 N1 2.024(5) . ? Ni1 N1 2.024(5) 2_655 ? Ni1 O2 2.108(7) . ? Ni1 O2 2.108(7) 2_655 ? Ni1 O1 2.151(6) . ? Ni1 O1 2.151(6) 2_655 ? Ni2 N2 2.015(4) . ? Ni2 N8 2.025(4) . ? Ni2 N4 2.031(4) . ? Ni2 O5 2.082(4) . ? Ni2 O4 2.107(4) . ? Ni2 O3 2.126(4) . ? B1 N10 1.526(8) . ? B1 N12 1.530(7) . ? B1 N14 1.547(7) . ? B1 H1 1.0000 . ? B2 N18 1.524(7) . ? B2 N16 1.533(8) . ? B2 N20 1.539(8) . ? B2 H2 1.0000 . ? B3 N26 1.525(7) . ? B3 N22 1.528(8) . ? B3 N24 1.535(7) . ? B3 H3 1.0000 . ? N1 C1 1.136(7) . ? N2 C2 1.146(6) . ? N3 C3 1.142(7) . ? N4 C4 1.155(6) . ? N5 C5 1.146(9) . ? N6 C6 1.146(7) . ? N7 C7 1.147(7) . ? N8 C8 1.156(6) . ? N9 C9 1.141(7) . ? N10 C12 1.352(7) . ? N10 N11 1.369(7) . ? N11 C10 1.345(7) . ? N12 C18 1.348(6) . ? N12 N13 1.369(5) . ? N13 C16 1.345(6) . ? N14 C24 1.342(6) . ? N14 N15 1.372(6) . ? N15 C22 1.357(6) . ? N16 C30 1.359(8) . ? N16 N17 1.364(7) . ? N17 C28 1.348(7) . ? N18 C36 1.357(6) . ? N18 N19 1.362(6) . ? N19 C34 1.349(7) . ? N20 C42 1.351(7) . ? N20 N21 1.371(6) . ? N21 C40 1.349(7) . ? N22 C48 1.355(7) . ? N22 N23 1.369(6) . ? N23 C46 1.343(7) . ? N24 C54 1.344(7) . ? N24 N25 1.371(6) . ? N25 C52 1.346(6) . ? N26 C60 1.350(6) . ? N26 N27 1.368(6) . ? N27 C58 1.348(6) . ? C10 C11 1.373(10) . ? C10 C15 1.500(11) . ? C11 C12 1.379(11) . ? C11 C14 1.513(9) . ? C12 C13 1.496(10) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.387(7) . ? C16 C21 1.491(7) . ? C17 C18 1.380(7) . ? C17 C20 1.501(7) . ? C18 C19 1.490(7) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.393(7) . ? C22 C27 1.495(7) . ? C23 C24 1.386(7) . ? C23 C26 1.497(7) . ? C24 C25 1.488(7) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.393(10) . ? C28 C33 1.494(9) . ? C29 C30 1.364(9) . ? C29 C32 1.495(9) . ? C30 C31 1.509(10) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.396(7) . ? C34 C39 1.491(8) . ? C35 C36 1.378(8) . ? C35 C38 1.500(7) . ? C36 C37 1.495(7) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.396(8) . ? C40 C45 1.480(8) . ? C41 C42 1.380(9) . ? C41 C44 1.497(7) . ? C42 C43 1.499(8) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.386(8) . ? C46 C51 1.485(8) . ? C47 C48 1.377(9) . ? C47 C50 1.505(8) . ? C48 C49 1.495(8) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.397(7) . ? C52 C57 1.486(7) . ? C53 C54 1.377(7) . ? C53 C56 1.490(7) . ? C54 C55 1.502(7) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.396(7) . ? C58 C63 1.493(7) . ? C59 C60 1.369(8) . ? C59 C62 1.501(7) . ? C60 C61 1.499(8) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? O1 O1 1.199(12) 2_655 ? O1 C64 1.263(11) . ? C64 O1 1.263(11) 2_655 ? O2 O2 1.024(14) 2_655 ? O2 C65 1.175(14) . ? O2 C65 1.421(13) 2_655 ? C65 C65 0.83(2) 2_655 ? C65 O2 1.421(13) 2_655 ? O3 C66 1.395(7) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? O4 C67 1.482(8) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? O5 C68 1.504(8) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? O6 C69 1.469(10) . ? O7 C70 1.426(13) . ? O8 C71 1.378(14) . ? O9 C72 1.582(16) . ? O10 C73 1.506(16) . ? O11 C74 1.44(2) . ? 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 C1 Fe1 C3 81.5(3) . . ? C1 Fe1 C2 93.4(2) . . ? C3 Fe1 C2 85.9(2) . . ? C1 Fe1 N15 90.89(18) . . ? C3 Fe1 N15 94.7(2) . . ? C2 Fe1 N15 175.72(18) . . ? C1 Fe1 N11 90.6(2) . . ? C3 Fe1 N11 171.0(2) . . ? C2 Fe1 N11 90.2(2) . . ? N15 Fe1 N11 89.79(18) . . ? C1 Fe1 N13 178.7(2) . . ? C3 Fe1 N13 97.20(19) . . ? C2 Fe1 N13 86.40(17) . . ? N15 Fe1 N13 89.33(15) . . ? N11 Fe1 N13 90.68(18) . . ? C6 Fe2 C5 82.2(3) . . ? C6 Fe2 C4 91.2(2) . . ? C5 Fe2 C4 85.9(2) . . ? C6 Fe2 N17 91.8(3) . . ? C5 Fe2 N17 173.1(2) . . ? C4 Fe2 N17 90.7(2) . . ? C6 Fe2 N21 90.76(19) . . ? C5 Fe2 N21 94.4(2) . . ? C4 Fe2 N21 178.07(18) . . ? N17 Fe2 N21 89.1(2) . . ? C6 Fe2 N19 178.2(3) . . ? C5 Fe2 N19 96.0(3) . . ? C4 Fe2 N19 88.32(18) . . ? N17 Fe2 N19 89.91(18) . . ? N21 Fe2 N19 89.76(17) . . ? C8 Fe3 C7 83.1(2) . . ? C8 Fe3 C9 88.1(2) . . ? C7 Fe3 C9 87.5(2) . . ? C8 Fe3 N23 90.9(2) . . ? C7 Fe3 N23 173.9(2) . . ? C9 Fe3 N23 91.2(2) . . ? C8 Fe3 N25 93.17(19) . . ? C7 Fe3 N25 92.0(2) . . ? C9 Fe3 N25 178.6(2) . . ? N23 Fe3 N25 89.45(18) . . ? C8 Fe3 N27 177.0(2) . . ? C7 Fe3 N27 95.6(2) . . ? C9 Fe3 N27 89.09(19) . . ? N23 Fe3 N27 90.30(17) . . ? N25 Fe3 N27 89.64(17) . . ? N6 Ni1 N6 177.6(4) . 2_655 ? N6 Ni1 N1 89.08(18) . . ? N6 Ni1 N1 90.98(18) 2_655 . ? N6 Ni1 N1 90.98(18) . 2_655 ? N6 Ni1 N1 89.08(18) 2_655 2_655 ? N1 Ni1 N1 177.1(4) . 2_655 ? N6 Ni1 O2 76.7(3) . . ? N6 Ni1 O2 100.9(3) 2_655 . ? N1 Ni1 O2 84.2(3) . . ? N1 Ni1 O2 98.6(3) 2_655 . ? N6 Ni1 O2 100.9(3) . 2_655 ? N6 Ni1 O2 76.7(3) 2_655 2_655 ? N1 Ni1 O2 98.6(3) . 2_655 ? N1 Ni1 O2 84.2(3) 2_655 2_655 ? O2 Ni1 O2 28.1(4) . 2_655 ? N6 Ni1 O1 82.1(3) . . ? N6 Ni1 O1 100.3(3) 2_655 . ? N1 Ni1 O1 75.2(3) . . ? N1 Ni1 O1 102.0(3) 2_655 . ? O2 Ni1 O1 150.5(2) . . ? O2 Ni1 O1 173.2(3) 2_655 . ? N6 Ni1 O1 100.3(3) . 2_655 ? N6 Ni1 O1 82.1(3) 2_655 2_655 ? N1 Ni1 O1 102.0(3) . 2_655 ? N1 Ni1 O1 75.2(3) 2_655 2_655 ? O2 Ni1 O1 173.2(3) . 2_655 ? O2 Ni1 O1 150.5(2) 2_655 2_655 ? O1 Ni1 O1 32.4(3) . 2_655 ? N2 Ni2 N8 176.80(19) . . ? N2 Ni2 N4 88.12(16) . . ? N8 Ni2 N4 91.60(16) . . ? N2 Ni2 O5 90.71(17) . . ? N8 Ni2 O5 92.49(17) . . ? N4 Ni2 O5 94.14(18) . . ? N2 Ni2 O4 92.31(16) . . ? N8 Ni2 O4 87.90(16) . . ? N4 Ni2 O4 178.73(18) . . ? O5 Ni2 O4 87.04(18) . . ? N2 Ni2 O3 91.33(17) . . ? N8 Ni2 O3 85.53(17) . . ? N4 Ni2 O3 95.62(16) . . ? O5 Ni2 O3 170.09(17) . . ? O4 Ni2 O3 83.18(17) . . ? N10 B1 N12 109.4(4) . . ? N10 B1 N14 108.3(4) . . ? N12 B1 N14 107.1(4) . . ? N10 B1 H1 110.7 . . ? N12 B1 H1 110.7 . . ? N14 B1 H1 110.6 . . ? N18 B2 N16 108.5(5) . . ? N18 B2 N20 107.3(5) . . ? N16 B2 N20 108.0(4) . . ? N18 B2 H2 110.9 . . ? N16 B2 H2 110.9 . . ? N20 B2 H2 111.0 . . ? N26 B3 N22 108.1(4) . . ? N26 B3 N24 107.8(4) . . ? N22 B3 N24 107.5(4) . . ? N26 B3 H3 111.1 . . ? N22 B3 H3 111.1 . . ? N24 B3 H3 111.1 . . ? C1 N1 Ni1 168.6(6) . . ? C2 N2 Ni2 170.0(4) . . ? C4 N4 Ni2 172.7(4) . . ? C6 N6 Ni1 168.9(8) . . ? C8 N8 Ni2 157.5(4) . . ? C12 N10 N11 110.0(5) . . ? C12 N10 B1 132.2(5) . . ? N11 N10 B1 117.8(4) . . ? C10 N11 N10 106.4(5) . . ? C10 N11 Fe1 135.2(5) . . ? N10 N11 Fe1 118.2(3) . . ? C18 N12 N13 109.4(4) . . ? C18 N12 B1 132.0(4) . . ? N13 N12 B1 118.5(4) . . ? C16 N13 N12 107.1(4) . . ? C16 N13 Fe1 135.7(3) . . ? N12 N13 Fe1 117.3(3) . . ? C24 N14 N15 110.3(4) . . ? C24 N14 B1 130.7(4) . . ? N15 N14 B1 119.1(4) . . ? C22 N15 N14 106.2(4) . . ? C22 N15 Fe1 136.8(3) . . ? N14 N15 Fe1 116.9(3) . . ? C30 N16 N17 108.9(5) . . ? C30 N16 B2 133.2(5) . . ? N17 N16 B2 117.9(5) . . ? C28 N17 N16 107.1(5) . . ? C28 N17 Fe2 134.2(4) . . ? N16 N17 Fe2 118.6(3) . . ? C36 N18 N19 109.4(4) . . ? C36 N18 B2 131.5(5) . . ? N19 N18 B2 119.1(4) . . ? C34 N19 N18 107.4(4) . . ? C34 N19 Fe2 135.0(4) . . ? N18 N19 Fe2 117.5(3) . . ? C42 N20 N21 109.7(4) . . ? C42 N20 B2 130.6(5) . . ? N21 N20 B2 119.7(4) . . ? C40 N21 N20 106.7(4) . . ? C40 N21 Fe2 136.6(4) . . ? N20 N21 Fe2 116.6(3) . . ? C48 N22 N23 109.3(4) . . ? C48 N22 B3 131.4(5) . . ? N23 N22 B3 119.2(4) . . ? C46 N23 N22 107.0(4) . . ? C46 N23 Fe3 135.3(4) . . ? N22 N23 Fe3 117.3(3) . . ? C54 N24 N25 109.7(4) . . ? C54 N24 B3 130.7(4) . . ? N25 N24 B3 119.6(4) . . ? C52 N25 N24 106.8(4) . . ? C52 N25 Fe3 136.3(3) . . ? N24 N25 Fe3 116.5(3) . . ? C60 N26 N27 109.5(4) . . ? C60 N26 B3 131.4(4) . . ? N27 N26 B3 119.1(4) . . ? C58 N27 N26 106.7(4) . . ? C58 N27 Fe3 136.0(4) . . ? N26 N27 Fe3 117.0(3) . . ? N1 C1 Fe1 176.6(6) . . ? N2 C2 Fe1 174.4(4) . . ? N3 C3 Fe1 174.0(5) . . ? N4 C4 Fe2 175.7(4) . . ? N5 C5 Fe2 172.8(7) . . ? N6 C6 Fe2 177.4(7) . . ? N7 C7 Fe3 171.6(5) . . ? N8 C8 Fe3 174.6(5) . . ? N9 C9 Fe3 178.8(5) . . ? N11 C10 C11 109.7(6) . . ? N11 C10 C15 122.9(6) . . ? C11 C10 C15 127.3(6) . . ? C10 C11 C12 106.9(5) . . ? C10 C11 C14 127.0(8) . . ? C12 C11 C14 126.1(8) . . ? N10 C12 C11 107.0(6) . . ? N10 C12 C13 123.8(7) . . ? C11 C12 C13 129.2(6) . . ? C12 C13 H13A 109.4 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N13 C16 C17 109.4(4) . . ? N13 C16 C21 124.4(4) . . ? C17 C16 C21 126.1(4) . . ? C18 C17 C16 106.2(4) . . ? C18 C17 C20 126.1(5) . . ? C16 C17 C20 127.7(5) . . ? N12 C18 C17 108.0(4) . . ? N12 C18 C19 122.8(5) . . ? C17 C18 C19 129.2(5) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.4 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N15 C22 C23 109.6(4) . . ? N15 C22 C27 123.9(4) . . ? C23 C22 C27 126.5(4) . . ? C24 C23 C22 105.8(4) . . ? C24 C23 C26 127.6(5) . . ? C22 C23 C26 126.6(5) . . ? N14 C24 C23 108.0(4) . . ? N14 C24 C25 122.4(5) . . ? C23 C24 C25 129.6(5) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.4 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.4 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N17 C28 C29 109.4(6) . . ? N17 C28 C33 124.3(6) . . ? C29 C28 C33 126.2(6) . . ? C30 C29 C28 105.9(6) . . ? C30 C29 C32 127.2(7) . . ? C28 C29 C32 126.9(7) . . ? N16 C30 C29 108.7(6) . . ? N16 C30 C31 122.7(6) . . ? C29 C30 C31 128.6(6) . . ? C30 C31 H31A 109.4 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.4 . . ? C29 C32 H32B 109.6 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N19 C34 C35 109.1(5) . . ? N19 C34 C39 124.9(5) . . ? C35 C34 C39 126.0(5) . . ? C36 C35 C34 106.0(4) . . ? C36 C35 C38 127.3(5) . . ? C34 C35 C38 126.6(5) . . ? N18 C36 C35 108.1(4) . . ? N18 C36 C37 122.7(5) . . ? C35 C36 C37 129.1(5) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.4 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N21 C40 C41 109.6(5) . . ? N21 C40 C45 124.2(5) . . ? C41 C40 C45 126.1(5) . . ? C42 C41 C40 105.8(5) . . ? C42 C41 C44 127.8(6) . . ? C40 C41 C44 126.5(6) . . ? N20 C42 C41 108.2(5) . . ? N20 C42 C43 122.5(5) . . ? C41 C42 C43 129.3(5) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C40 C45 H45A 109.4 . . ? C40 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C40 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N23 C46 C47 109.6(5) . . ? N23 C46 C51 124.5(5) . . ? C47 C46 C51 125.9(5) . . ? C48 C47 C46 106.3(5) . . ? C48 C47 C50 127.3(6) . . ? C46 C47 C50 126.4(6) . . ? N22 C48 C47 107.8(5) . . ? N22 C48 C49 121.8(6) . . ? C47 C48 C49 130.3(5) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.4 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.4 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C46 C51 H51A 109.5 . . ? C46 C51 H51B 109.4 . . ? H51A C51 H51B 109.5 . . ? C46 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N25 C52 C53 109.3(4) . . ? N25 C52 C57 124.5(5) . . ? C53 C52 C57 126.2(5) . . ? C54 C53 C52 105.9(5) . . ? C54 C53 C56 128.6(5) . . ? C52 C53 C56 125.5(5) . . ? N24 C54 C53 108.2(4) . . ? N24 C54 C55 121.9(5) . . ? C53 C54 C55 129.9(5) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.4 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.4 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C52 C57 H57A 109.4 . . ? C52 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C52 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N27 C58 C59 109.4(5) . . ? N27 C58 C63 122.7(5) . . ? C59 C58 C63 127.9(5) . . ? C60 C59 C58 105.9(4) . . ? C60 C59 C62 125.8(5) . . ? C58 C59 C62 128.3(5) . . ? N26 C60 C59 108.4(4) . . ? N26 C60 C61 122.1(5) . . ? C59 C60 C61 129.5(5) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.4 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C59 C62 H62A 109.5 . . ? C59 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C59 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C58 C63 H63A 109.5 . . ? C58 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C58 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O1 O1 C64 61.7(3) 2_655 . ? O1 O1 Ni1 73.82(17) 2_655 . ? C64 O1 Ni1 135.5(5) . . ? O1 C64 O1 56.6(7) . 2_655 ? O2 O2 C65 80.2(8) 2_655 . ? O2 O2 C65 54.5(6) 2_655 2_655 ? C65 O2 C65 35.7(10) . 2_655 ? O2 O2 Ni1 75.94(18) 2_655 . ? C65 O2 Ni1 152.6(9) . . ? C65 O2 Ni1 128.8(7) 2_655 . ? C65 C65 O2 88.6(9) 2_655 . ? C65 C65 O2 55.7(8) 2_655 2_655 ? O2 C65 O2 45.2(7) . 2_655 ? C66 O3 Ni2 124.0(4) . . ? O3 C66 H66A 109.5 . . ? O3 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? O3 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C67 O4 Ni2 121.2(4) . . ? O4 C67 H67A 109.5 . . ? O4 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? O4 C67 H67C 109.4 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C68 O5 Ni2 122.1(4) . . ? O5 C68 H68A 109.5 . . ? O5 C68 H68B 109.4 . . ? H68A C68 H68B 109.5 . . ? O5 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Ni1 N1 C1 -75(2) . . . . ? N6 Ni1 N1 C1 108(2) 2_655 . . . ? N1 Ni1 N1 C1 17(2) 2_655 . . . ? O2 Ni1 N1 C1 -151(2) . . . . ? O2 Ni1 N1 C1 -176(2) 2_655 . . . ? O1 Ni1 N1 C1 7(2) . . . . ? O1 Ni1 N1 C1 26(2) 2_655 . . . ? N8 Ni2 N2 C2 -98(4) . . . . ? N4 Ni2 N2 C2 -13(3) . . . . ? O5 Ni2 N2 C2 81(3) . . . . ? O4 Ni2 N2 C2 168(3) . . . . ? O3 Ni2 N2 C2 -108(3) . . . . ? N2 Ni2 N4 C4 93(3) . . . . ? N8 Ni2 N4 C4 -90(3) . . . . ? O5 Ni2 N4 C4 3(3) . . . . ? O4 Ni2 N4 C4 -157(7) . . . . ? O3 Ni2 N4 C4 -176(3) . . . . ? N6 Ni1 N6 C6 21(2) 2_655 . . . ? N1 Ni1 N6 C6 -70(2) . . . . ? N1 Ni1 N6 C6 112(2) 2_655 . . . ? O2 Ni1 N6 C6 14(2) . . . . ? O2 Ni1 N6 C6 28(2) 2_655 . . . ? O1 Ni1 N6 C6 -146(2) . . . . ? O1 Ni1 N6 C6 -172(2) 2_655 . . . ? N2 Ni2 N8 C8 -21(4) . . . . ? N4 Ni2 N8 C8 -105.6(11) . . . . ? O5 Ni2 N8 C8 160.2(11) . . . . ? O4 Ni2 N8 C8 73.2(11) . . . . ? O3 Ni2 N8 C8 -10.1(11) . . . . ? N12 B1 N10 C12 -126.1(5) . . . . ? N14 B1 N10 C12 117.6(6) . . . . ? N12 B1 N10 N11 57.5(5) . . . . ? N14 B1 N10 N11 -58.9(5) . . . . ? C12 N10 N11 C10 0.5(6) . . . . ? B1 N10 N11 C10 177.7(4) . . . . ? C12 N10 N11 Fe1 -175.7(3) . . . . ? B1 N10 N11 Fe1 1.5(5) . . . . ? C1 Fe1 N11 C10 -39.1(5) . . . . ? C3 Fe1 N11 C10 -9.9(16) . . . . ? C2 Fe1 N11 C10 54.3(5) . . . . ? N15 Fe1 N11 C10 -130.0(5) . . . . ? N13 Fe1 N11 C10 140.7(5) . . . . ? C1 Fe1 N11 N10 135.7(4) . . . . ? C3 Fe1 N11 N10 164.9(12) . . . . ? C2 Fe1 N11 N10 -130.9(4) . . . . ? N15 Fe1 N11 N10 44.8(3) . . . . ? N13 Fe1 N11 N10 -44.5(3) . . . . ? N10 B1 N12 C18 123.4(5) . . . . ? N14 B1 N12 C18 -119.5(5) . . . . ? N10 B1 N12 N13 -61.1(5) . . . . ? N14 B1 N12 N13 56.1(6) . . . . ? C18 N12 N13 C16 -0.2(5) . . . . ? B1 N12 N13 C16 -176.7(4) . . . . ? C18 N12 N13 Fe1 -179.5(3) . . . . ? B1 N12 N13 Fe1 4.0(5) . . . . ? C1 Fe1 N13 C16 33(9) . . . . ? C3 Fe1 N13 C16 37.8(5) . . . . ? C2 Fe1 N13 C16 -47.6(5) . . . . ? N15 Fe1 N13 C16 132.5(5) . . . . ? N11 Fe1 N13 C16 -137.7(5) . . . . ? C1 Fe1 N13 N12 -148(8) . . . . ? C3 Fe1 N13 N12 -143.2(3) . . . . ? C2 Fe1 N13 N12 131.3(3) . . . . ? N15 Fe1 N13 N12 -48.6(3) . . . . ? N11 Fe1 N13 N12 41.2(3) . . . . ? N10 B1 N14 C24 -124.0(5) . . . . ? N12 B1 N14 C24 118.1(5) . . . . ? N10 B1 N14 N15 56.8(6) . . . . ? N12 B1 N14 N15 -61.0(6) . . . . ? C24 N14 N15 C22 1.3(5) . . . . ? B1 N14 N15 C22 -179.4(4) . . . . ? C24 N14 N15 Fe1 -176.4(3) . . . . ? B1 N14 N15 Fe1 2.9(5) . . . . ? C1 Fe1 N15 C22 46.3(5) . . . . ? C3 Fe1 N15 C22 -35.3(5) . . . . ? C2 Fe1 N15 C22 -134(3) . . . . ? N11 Fe1 N15 C22 136.9(5) . . . . ? N13 Fe1 N15 C22 -132.5(5) . . . . ? C1 Fe1 N15 N14 -137.0(4) . . . . ? C3 Fe1 N15 N14 141.4(4) . . . . ? C2 Fe1 N15 N14 43(3) . . . . ? N11 Fe1 N15 N14 -46.4(3) . . . . ? N13 Fe1 N15 N14 44.2(3) . . . . ? N18 B2 N16 C30 -124.8(6) . . . . ? N20 B2 N16 C30 119.2(6) . . . . ? N18 B2 N16 N17 58.7(6) . . . . ? N20 B2 N16 N17 -57.4(6) . . . . ? C30 N16 N17 C28 0.3(6) . . . . ? B2 N16 N17 C28 177.7(4) . . . . ? C30 N16 N17 Fe2 -178.1(3) . . . . ? B2 N16 N17 Fe2 -0.8(6) . . . . ? C6 Fe2 N17 C28 -40.9(5) . . . . ? C5 Fe2 N17 C28 -11(2) . . . . ? C4 Fe2 N17 C28 50.3(5) . . . . ? N21 Fe2 N17 C28 -131.6(5) . . . . ? N19 Fe2 N17 C28 138.6(5) . . . . ? C6 Fe2 N17 N16 137.1(4) . . . . ? C5 Fe2 N17 N16 167(2) . . . . ? C4 Fe2 N17 N16 -131.8(4) . . . . ? N21 Fe2 N17 N16 46.3(4) . . . . ? N19 Fe2 N17 N16 -43.4(4) . . . . ? N16 B2 N18 C36 121.1(6) . . . . ? N20 B2 N18 C36 -122.4(6) . . . . ? N16 B2 N18 N19 -59.1(6) . . . . ? N20 B2 N18 N19 57.4(6) . . . . ? C36 N18 N19 C34 -0.8(5) . . . . ? B2 N18 N19 C34 179.3(4) . . . . ? C36 N18 N19 Fe2 -178.9(3) . . . . ? B2 N18 N19 Fe2 1.2(6) . . . . ? C6 Fe2 N19 C34 30(7) . . . . ? C5 Fe2 N19 C34 42.1(5) . . . . ? C4 Fe2 N19 C34 -43.6(5) . . . . ? N17 Fe2 N19 C34 -134.3(5) . . . . ? N21 Fe2 N19 C34 136.6(5) . . . . ? C6 Fe2 N19 N18 -153(7) . . . . ? C5 Fe2 N19 N18 -140.4(4) . . . . ? C4 Fe2 N19 N18 133.9(4) . . . . ? N17 Fe2 N19 N18 43.1(4) . . . . ? N21 Fe2 N19 N18 -46.0(4) . . . . ? N18 B2 N20 C42 119.6(6) . . . . ? N16 B2 N20 C42 -123.6(6) . . . . ? N18 B2 N20 N21 -59.8(6) . . . . ? N16 B2 N20 N21 57.0(6) . . . . ? C42 N20 N21 C40 0.9(6) . . . . ? B2 N20 N21 C40 -179.6(5) . . . . ? C42 N20 N21 Fe2 -177.4(4) . . . . ? B2 N20 N21 Fe2 2.1(6) . . . . ? C6 Fe2 N21 C40 44.3(6) . . . . ? C5 Fe2 N21 C40 -38.0(6) . . . . ? C4 Fe2 N21 C40 -139(6) . . . . ? N17 Fe2 N21 C40 136.1(6) . . . . ? N19 Fe2 N21 C40 -134.0(6) . . . . ? C6 Fe2 N21 N20 -138.1(4) . . . . ? C5 Fe2 N21 N20 139.7(4) . . . . ? C4 Fe2 N21 N20 39(7) . . . . ? N17 Fe2 N21 N20 -46.3(4) . . . . ? N19 Fe2 N21 N20 43.6(4) . . . . ? N26 B3 N22 C48 127.1(5) . . . . ? N24 B3 N22 C48 -116.7(5) . . . . ? N26 B3 N22 N23 -55.3(5) . . . . ? N24 B3 N22 N23 60.9(6) . . . . ? C48 N22 N23 C46 -0.2(5) . . . . ? B3 N22 N23 C46 -178.3(4) . . . . ? C48 N22 N23 Fe3 173.3(3) . . . . ? B3 N22 N23 Fe3 -4.8(5) . . . . ? C8 Fe3 N23 C46 35.0(5) . . . . ? C7 Fe3 N23 C46 25(2) . . . . ? C9 Fe3 N23 C46 -53.1(5) . . . . ? N25 Fe3 N23 C46 128.1(5) . . . . ? N27 Fe3 N23 C46 -142.2(5) . . . . ? C8 Fe3 N23 N22 -136.2(3) . . . . ? C7 Fe3 N23 N22 -146.5(18) . . . . ? C9 Fe3 N23 N22 135.6(3) . . . . ? N25 Fe3 N23 N22 -43.1(3) . . . . ? N27 Fe3 N23 N22 46.5(3) . . . . ? N26 B3 N24 C54 -116.4(6) . . . . ? N22 B3 N24 C54 127.2(5) . . . . ? N26 B3 N24 N25 62.3(6) . . . . ? N22 B3 N24 N25 -54.1(6) . . . . ? C54 N24 N25 C52 -1.7(5) . . . . ? B3 N24 N25 C52 179.3(4) . . . . ? C54 N24 N25 Fe3 172.7(3) . . . . ? B3 N24 N25 Fe3 -6.3(6) . . . . ? C8 Fe3 N25 C52 -48.1(5) . . . . ? C7 Fe3 N25 C52 35.1(5) . . . . ? C9 Fe3 N25 C52 102(8) . . . . ? N23 Fe3 N25 C52 -139.0(5) . . . . ? N27 Fe3 N25 C52 130.7(5) . . . . ? C8 Fe3 N25 N24 139.6(4) . . . . ? C7 Fe3 N25 N24 -137.2(4) . . . . ? C9 Fe3 N25 N24 -70(8) . . . . ? N23 Fe3 N25 N24 48.7(4) . . . . ? N27 Fe3 N25 N24 -41.6(3) . . . . ? N22 B3 N26 C60 -120.6(6) . . . . ? N24 B3 N26 C60 123.5(5) . . . . ? N22 B3 N26 N27 62.2(5) . . . . ? N24 B3 N26 N27 -53.7(6) . . . . ? C60 N26 N27 C58 0.1(5) . . . . ? B3 N26 N27 C58 177.9(4) . . . . ? C60 N26 N27 Fe3 175.3(3) . . . . ? B3 N26 N27 Fe3 -6.9(6) . . . . ? C8 Fe3 N27 C58 20(4) . . . . ? C7 Fe3 N27 C58 -45.7(5) . . . . ? C9 Fe3 N27 C58 41.7(5) . . . . ? N23 Fe3 N27 C58 132.9(5) . . . . ? N25 Fe3 N27 C58 -137.6(5) . . . . ? C8 Fe3 N27 N26 -154(4) . . . . ? C7 Fe3 N27 N26 140.9(4) . . . . ? C9 Fe3 N27 N26 -131.7(4) . . . . ? N23 Fe3 N27 N26 -40.5(4) . . . . ? N25 Fe3 N27 N26 49.0(4) . . . . ? Ni1 N1 C1 Fe1 -44(11) . . . . ? C3 Fe1 C1 N1 41(9) . . . . ? C2 Fe1 C1 N1 127(9) . . . . ? N15 Fe1 C1 N1 -53(9) . . . . ? N11 Fe1 C1 N1 -143(9) . . . . ? N13 Fe1 C1 N1 47(15) . . . . ? Ni2 N2 C2 Fe1 -171(3) . . . . ? C1 Fe1 C2 N2 172(5) . . . . ? C3 Fe1 C2 N2 -107(5) . . . . ? N15 Fe1 C2 N2 -8(7) . . . . ? N11 Fe1 C2 N2 81(5) . . . . ? N13 Fe1 C2 N2 -9(5) . . . . ? C1 Fe1 C3 N3 24(5) . . . . ? C2 Fe1 C3 N3 -70(5) . . . . ? N15 Fe1 C3 N3 114(5) . . . . ? N11 Fe1 C3 N3 -6(6) . . . . ? N13 Fe1 C3 N3 -156(5) . . . . ? Ni2 N4 C4 Fe2 60(8) . . . . ? C6 Fe2 C4 N4 -158(6) . . . . ? C5 Fe2 C4 N4 -76(6) . . . . ? N17 Fe2 C4 N4 110(6) . . . . ? N21 Fe2 C4 N4 25(11) . . . . ? N19 Fe2 C4 N4 20(6) . . . . ? C6 Fe2 C5 N5 28(6) . . . . ? C4 Fe2 C5 N5 -64(6) . . . . ? N17 Fe2 C5 N5 -3(8) . . . . ? N21 Fe2 C5 N5 118(6) . . . . ? N19 Fe2 C5 N5 -152(6) . . . . ? Ni1 N6 C6 Fe2 -25(13) . . . . ? C5 Fe2 C6 N6 22(12) . . . . ? C4 Fe2 C6 N6 108(12) . . . . ? N17 Fe2 C6 N6 -162(12) . . . . ? N21 Fe2 C6 N6 -72(12) . . . . ? N19 Fe2 C6 N6 35(16) . . . . ? C8 Fe3 C7 N7 -2(3) . . . . ? C9 Fe3 C7 N7 86(3) . . . . ? N23 Fe3 C7 N7 8(5) . . . . ? N25 Fe3 C7 N7 -95(3) . . . . ? N27 Fe3 C7 N7 175(3) . . . . ? Ni2 N8 C8 Fe3 -18(6) . . . . ? C7 Fe3 C8 N8 21(5) . . . . ? C9 Fe3 C8 N8 -67(5) . . . . ? N23 Fe3 C8 N8 -158(5) . . . . ? N25 Fe3 C8 N8 112(5) . . . . ? N27 Fe3 C8 N8 -45(8) . . . . ? C8 Fe3 C9 N9 76(27) . . . . ? C7 Fe3 C9 N9 -7(27) . . . . ? N23 Fe3 C9 N9 167(100) . . . . ? N25 Fe3 C9 N9 -74(30) . . . . ? N27 Fe3 C9 N9 -103(27) . . . . ? N10 N11 C10 C11 0.0(6) . . . . ? Fe1 N11 C10 C11 175.2(4) . . . . ? N10 N11 C10 C15 -178.4(6) . . . . ? Fe1 N11 C10 C15 -3.1(9) . . . . ? N11 C10 C11 C12 -0.5(7) . . . . ? C15 C10 C11 C12 177.8(6) . . . . ? N11 C10 C11 C14 -179.2(6) . . . . ? C15 C10 C11 C14 -0.9(11) . . . . ? N11 N10 C12 C11 -0.8(6) . . . . ? B1 N10 C12 C11 -177.5(5) . . . . ? N11 N10 C12 C13 178.8(5) . . . . ? B1 N10 C12 C13 2.1(9) . . . . ? C10 C11 C12 N10 0.8(7) . . . . ? C14 C11 C12 N10 179.5(6) . . . . ? C10 C11 C12 C13 -178.8(6) . . . . ? C14 C11 C12 C13 -0.1(11) . . . . ? N12 N13 C16 C17 0.1(5) . . . . ? Fe1 N13 C16 C17 179.1(3) . . . . ? N12 N13 C16 C21 -177.7(4) . . . . ? Fe1 N13 C16 C21 1.3(7) . . . . ? N13 C16 C17 C18 0.1(5) . . . . ? C21 C16 C17 C18 177.8(5) . . . . ? N13 C16 C17 C20 -179.8(5) . . . . ? C21 C16 C17 C20 -2.1(8) . . . . ? N13 N12 C18 C17 0.3(5) . . . . ? B1 N12 C18 C17 176.2(5) . . . . ? N13 N12 C18 C19 -177.4(4) . . . . ? B1 N12 C18 C19 -1.5(8) . . . . ? C16 C17 C18 N12 -0.2(5) . . . . ? C20 C17 C18 N12 179.7(5) . . . . ? C16 C17 C18 C19 177.3(5) . . . . ? C20 C17 C18 C19 -2.8(9) . . . . ? N14 N15 C22 C23 -1.5(5) . . . . ? Fe1 N15 C22 C23 175.4(4) . . . . ? N14 N15 C22 C27 178.4(5) . . . . ? Fe1 N15 C22 C27 -4.7(8) . . . . ? N15 C22 C23 C24 1.2(6) . . . . ? C27 C22 C23 C24 -178.7(5) . . . . ? N15 C22 C23 C26 179.9(5) . . . . ? C27 C22 C23 C26 0.0(8) . . . . ? N15 N14 C24 C23 -0.5(6) . . . . ? B1 N14 C24 C23 -179.7(5) . . . . ? N15 N14 C24 C25 178.2(5) . . . . ? B1 N14 C24 C25 -1.0(8) . . . . ? C22 C23 C24 N14 -0.4(6) . . . . ? C26 C23 C24 N14 -179.1(5) . . . . ? C22 C23 C24 C25 -179.0(5) . . . . ? C26 C23 C24 C25 2.3(9) . . . . ? N16 N17 C28 C29 -0.2(6) . . . . ? Fe2 N17 C28 C29 177.9(4) . . . . ? N16 N17 C28 C33 -177.9(5) . . . . ? Fe2 N17 C28 C33 0.2(9) . . . . ? N17 C28 C29 C30 0.0(6) . . . . ? C33 C28 C29 C30 177.7(6) . . . . ? N17 C28 C29 C32 -180.0(6) . . . . ? C33 C28 C29 C32 -2.3(10) . . . . ? N17 N16 C30 C29 -0.3(6) . . . . ? B2 N16 C30 C29 -177.1(5) . . . . ? N17 N16 C30 C31 177.4(5) . . . . ? B2 N16 C30 C31 0.7(9) . . . . ? C28 C29 C30 N16 0.2(6) . . . . ? C32 C29 C30 N16 -179.8(6) . . . . ? C28 C29 C30 C31 -177.4(6) . . . . ? C32 C29 C30 C31 2.6(10) . . . . ? N18 N19 C34 C35 0.3(5) . . . . ? Fe2 N19 C34 C35 177.9(4) . . . . ? N18 N19 C34 C39 -179.4(5) . . . . ? Fe2 N19 C34 C39 -1.8(8) . . . . ? N19 C34 C35 C36 0.3(6) . . . . ? C39 C34 C35 C36 180.0(5) . . . . ? N19 C34 C35 C38 -177.6(5) . . . . ? C39 C34 C35 C38 2.2(8) . . . . ? N19 N18 C36 C35 1.0(6) . . . . ? B2 N18 C36 C35 -179.2(5) . . . . ? N19 N18 C36 C37 -175.9(5) . . . . ? B2 N18 C36 C37 3.9(9) . . . . ? C34 C35 C36 N18 -0.8(6) . . . . ? C38 C35 C36 N18 177.1(5) . . . . ? C34 C35 C36 C37 175.9(5) . . . . ? C38 C35 C36 C37 -6.3(9) . . . . ? N20 N21 C40 C41 -0.9(6) . . . . ? Fe2 N21 C40 C41 176.9(4) . . . . ? N20 N21 C40 C45 176.8(6) . . . . ? Fe2 N21 C40 C45 -5.4(10) . . . . ? N21 C40 C41 C42 0.6(7) . . . . ? C45 C40 C41 C42 -177.0(6) . . . . ? N21 C40 C41 C44 -179.6(5) . . . . ? C45 C40 C41 C44 2.8(10) . . . . ? N21 N20 C42 C41 -0.5(6) . . . . ? B2 N20 C42 C41 -180.0(5) . . . . ? N21 N20 C42 C43 178.7(5) . . . . ? B2 N20 C42 C43 -0.7(9) . . . . ? C40 C41 C42 N20 -0.1(6) . . . . ? C44 C41 C42 N20 -179.8(5) . . . . ? C40 C41 C42 C43 -179.2(6) . . . . ? C44 C41 C42 C43 1.0(10) . . . . ? N22 N23 C46 C47 0.1(6) . . . . ? Fe3 N23 C46 C47 -171.7(4) . . . . ? N22 N23 C46 C51 -179.3(5) . . . . ? Fe3 N23 C46 C51 8.8(8) . . . . ? N23 C46 C47 C48 0.0(6) . . . . ? C51 C46 C47 C48 179.4(5) . . . . ? N23 C46 C47 C50 177.3(5) . . . . ? C51 C46 C47 C50 -3.3(9) . . . . ? N23 N22 C48 C47 0.2(6) . . . . ? B3 N22 C48 C47 178.0(5) . . . . ? N23 N22 C48 C49 -178.9(5) . . . . ? B3 N22 C48 C49 -1.2(8) . . . . ? C46 C47 C48 N22 -0.2(6) . . . . ? C50 C47 C48 N22 -177.4(5) . . . . ? C46 C47 C48 C49 178.9(5) . . . . ? C50 C47 C48 C49 1.7(10) . . . . ? N24 N25 C52 C53 2.0(6) . . . . ? Fe3 N25 C52 C53 -170.8(4) . . . . ? N24 N25 C52 C57 -176.2(5) . . . . ? Fe3 N25 C52 C57 11.1(8) . . . . ? N25 C52 C53 C54 -1.5(6) . . . . ? C57 C52 C53 C54 176.6(5) . . . . ? N25 C52 C53 C56 177.8(5) . . . . ? C57 C52 C53 C56 -4.1(9) . . . . ? N25 N24 C54 C53 0.8(6) . . . . ? B3 N24 C54 C53 179.6(5) . . . . ? N25 N24 C54 C55 180.0(5) . . . . ? B3 N24 C54 C55 -1.2(8) . . . . ? C52 C53 C54 N24 0.4(6) . . . . ? C56 C53 C54 N24 -178.8(5) . . . . ? C52 C53 C54 C55 -178.7(5) . . . . ? C56 C53 C54 C55 2.1(9) . . . . ? N26 N27 C58 C59 0.0(5) . . . . ? Fe3 N27 C58 C59 -173.8(4) . . . . ? N26 N27 C58 C63 179.7(4) . . . . ? Fe3 N27 C58 C63 5.9(8) . . . . ? N27 C58 C59 C60 -0.2(6) . . . . ? C63 C58 C59 C60 -179.8(5) . . . . ? N27 C58 C59 C62 178.8(5) . . . . ? C63 C58 C59 C62 -0.9(9) . . . . ? N27 N26 C60 C59 -0.2(6) . . . . ? B3 N26 C60 C59 -177.6(5) . . . . ? N27 N26 C60 C61 179.3(5) . . . . ? B3 N26 C60 C61 1.9(9) . . . . ? C58 C59 C60 N26 0.2(6) . . . . ? C62 C59 C60 N26 -178.8(5) . . . . ? C58 C59 C60 C61 -179.3(5) . . . . ? C62 C59 C60 C61 1.7(9) . . . . ? N6 Ni1 O1 O1 -123.9(7) . . . 2_655 ? N6 Ni1 O1 O1 56.7(7) 2_655 . . 2_655 ? N1 Ni1 O1 O1 145.0(7) . . . 2_655 ? N1 Ni1 O1 O1 -34.5(7) 2_655 . . 2_655 ? O2 Ni1 O1 O1 -167.9(5) . . . 2_655 ? O2 Ni1 O1 O1 120(2) 2_655 . . 2_655 ? N6 Ni1 O1 C64 -123.9(7) . . . . ? N6 Ni1 O1 C64 56.7(7) 2_655 . . . ? N1 Ni1 O1 C64 145.0(7) . . . . ? N1 Ni1 O1 C64 -34.5(7) 2_655 . . . ? O2 Ni1 O1 C64 -167.9(5) . . . . ? O2 Ni1 O1 C64 120(2) 2_655 . . . ? O1 Ni1 O1 C64 0.000(3) 2_655 . . . ? Ni1 O1 C64 O1 0.000(3) . . . 2_655 ? N6 Ni1 O2 O2 148.8(8) . . . 2_655 ? N6 Ni1 O2 O2 -30.8(8) 2_655 . . 2_655 ? N1 Ni1 O2 O2 -120.7(8) . . . 2_655 ? N1 Ni1 O2 O2 59.9(8) 2_655 . . 2_655 ? O1 Ni1 O2 O2 -166.1(6) . . . 2_655 ? O1 Ni1 O2 O2 84(2) 2_655 . . 2_655 ? N6 Ni1 O2 C65 179(100) . . . . ? N6 Ni1 O2 C65 -0.6(17) 2_655 . . . ? N1 Ni1 O2 C65 -90.5(17) . . . . ? N1 Ni1 O2 C65 90.1(17) 2_655 . . . ? O2 Ni1 O2 C65 30.3(14) 2_655 . . . ? O1 Ni1 O2 C65 -135.8(16) . . . . ? O1 Ni1 O2 C65 115(3) 2_655 . . . ? N6 Ni1 O2 C65 134.6(9) . . . 2_655 ? N6 Ni1 O2 C65 -45.1(9) 2_655 . . 2_655 ? N1 Ni1 O2 C65 -135.0(9) . . . 2_655 ? N1 Ni1 O2 C65 45.6(9) 2_655 . . 2_655 ? O2 Ni1 O2 C65 -14.3(8) 2_655 . . 2_655 ? O1 Ni1 O2 C65 179.6(8) . . . 2_655 ? O1 Ni1 O2 C65 70(2) 2_655 . . 2_655 ? O2 O2 C65 C65 -40(2) 2_655 . . 2_655 ? Ni1 O2 C65 C65 -69(3) . . . 2_655 ? C65 O2 C65 O2 40(2) 2_655 . . 2_655 ? Ni1 O2 C65 O2 -29.7(13) . . . 2_655 ? N2 Ni2 O3 C66 51.2(5) . . . . ? N8 Ni2 O3 C66 -128.2(5) . . . . ? N4 Ni2 O3 C66 -37.1(5) . . . . ? O5 Ni2 O3 C66 153.0(9) . . . . ? O4 Ni2 O3 C66 143.4(5) . . . . ? N2 Ni2 O4 C67 -147.0(5) . . . . ? N8 Ni2 O4 C67 36.2(5) . . . . ? N4 Ni2 O4 C67 103(8) . . . . ? O5 Ni2 O4 C67 -56.4(5) . . . . ? O3 Ni2 O4 C67 121.9(5) . . . . ? N2 Ni2 O5 C68 40.9(5) . . . . ? N8 Ni2 O5 C68 -139.1(5) . . . . ? N4 Ni2 O5 C68 129.1(5) . . . . ? O4 Ni2 O5 C68 -51.3(5) . . . . ? O3 Ni2 O5 C68 -60.9(11) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.620 _refine_diff_density_min -0.902 _refine_diff_density_rms 0.114