# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Holmes, Stephen' _publ_contact_author_email holmesst@umsl.edu _publ_section_title ; A Cyano-based Octanuclear {FeIII4NiII4} Single-Molecule Magnet ; loop_ _publ_author_name S.Holmes R.Clerac # Attachment '1.cif.txt' # [NEt4][(Tp*Me)Fe(CN)3].H2O (1) data_1 _database_code_depnum_ccdc_archive 'CCDC 768189' #TrackingRef '1.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H28 B Fe N9, C8 H20 N,H2 O' _chemical_formula_sum 'C29 H50 B Fe N10 O' _chemical_formula_weight 621.45 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2~1~/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9051(6) _cell_length_b 16.1219(11) _cell_length_c 20.3990(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.661(2) _cell_angle_gamma 90.00 _cell_volume 3250.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9604 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 31.18 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas no _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 0.503 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8310 _exptl_absorpt_correction_T_max 0.9021 _exptl_absorpt_process_details 'sadabs v2008/1' _exptl_special_details ; All water and B-H H atoms were located and refined freely. All other H atoms were added in their calculated positions and were treated using appropriate riding models. ; _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_reflns_number 88196 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 31.24 _reflns_number_total 10545 _reflns_number_gt 9177 _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^)+(0.0869P)^2^+2.9824P] 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 10545 _refine_ls_number_parameters 463 _refine_ls_number_restraints 216 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1503 _refine_ls_wR_factor_gt 0.1414 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 1.00132(2) 0.187967(13) 0.163780(10) 0.01280(7) Uani 1 1 d . . . O1 O 0.13207(16) 0.50973(10) 0.14344(8) 0.0325(3) Uani 1 1 d . . . N1 N 0.84031(12) 0.17292(8) 0.21715(6) 0.0139(2) Uani 1 1 d . . . N2 N 0.72753(12) 0.13762(8) 0.18694(6) 0.0143(2) Uani 1 1 d . . . N3 N 0.97246(12) 0.07306(8) 0.12788(6) 0.0147(2) Uani 1 1 d . . . N4 N 0.84363(12) 0.05179(8) 0.10595(6) 0.0154(2) Uani 1 1 d . . . N5 N 0.88020(13) 0.23206(8) 0.08919(6) 0.0164(2) Uani 1 1 d . . . N6 N 0.76077(13) 0.19141(8) 0.07506(6) 0.0147(2) Uani 1 1 d . . . N7 N 1.18581(14) 0.12024(10) 0.27812(7) 0.0219(3) Uani 1 1 d . . . N8 N 1.04292(16) 0.36588(10) 0.21522(9) 0.0267(3) Uani 1 1 d . . . N9 N 1.25932(16) 0.21051(11) 0.08937(8) 0.0259(3) Uani 1 1 d . . . B1 B 0.72851(16) 0.11361(11) 0.11418(8) 0.0151(3) Uani 1 1 d . . . C1 C 0.81137(15) 0.18871(9) 0.27954(8) 0.0161(3) Uani 1 1 d . . . C2 C 0.67841(15) 0.16356(10) 0.28932(8) 0.0176(3) Uani 1 1 d . . . C3 C 0.62882(15) 0.13137(10) 0.22931(7) 0.0159(3) Uani 1 1 d . . . C4 C 0.90869(17) 0.22571(11) 0.32998(8) 0.0218(3) Uani 1 1 d . . . H4A H 0.9942 0.2376 0.3102 0.033 Uiso 1 1 calc R . . H4B H 0.9249 0.1866 0.3664 0.033 Uiso 1 1 calc R . . H4C H 0.8710 0.2773 0.3465 0.033 Uiso 1 1 calc R . . C5 C 0.6046(2) 0.17219(13) 0.35081(9) 0.0279(4) Uani 1 1 d . . . H5A H 0.5134 0.1491 0.3436 0.042 Uiso 1 1 calc R . . H5B H 0.5985 0.2310 0.3624 0.042 Uiso 1 1 calc R . . H5C H 0.6538 0.1422 0.3867 0.042 Uiso 1 1 calc R . . C6 C 0.49343(16) 0.09546(12) 0.21003(9) 0.0228(3) Uani 1 1 d . . . H6A H 0.4904 0.0785 0.1638 0.034 Uiso 1 1 calc R . . H6B H 0.4233 0.1372 0.2160 0.034 Uiso 1 1 calc R . . H6C H 0.4775 0.0471 0.2376 0.034 Uiso 1 1 calc R . . C7 C 1.05291(15) 0.00959(10) 0.11212(7) 0.0161(3) Uani 1 1 d . . . C8 C 0.97521(16) -0.05210(10) 0.07928(8) 0.0177(3) Uani 1 1 d . . . C9 C 0.84364(16) -0.02309(10) 0.07634(8) 0.0172(3) Uani 1 1 d . . . C10 C 1.20161(16) 0.00636(11) 0.12862(9) 0.0208(3) Uani 1 1 d . . . H10A H 1.2306 0.0575 0.1514 0.031 Uiso 1 1 calc R . . H10B H 1.2491 0.0008 0.0881 0.031 Uiso 1 1 calc R . . H10C H 1.2229 -0.0414 0.1572 0.031 Uiso 1 1 calc R . . C11 C 1.02628(19) -0.13118(11) 0.05169(9) 0.0243(3) Uani 1 1 d . . . H11A H 0.9501 -0.1630 0.0316 0.036 Uiso 1 1 calc R . . H11B H 1.0719 -0.1639 0.0870 0.036 Uiso 1 1 calc R . . H11C H 1.0903 -0.1185 0.0184 0.036 Uiso 1 1 calc R . . C12 C 0.71728(18) -0.06314(11) 0.04801(9) 0.0244(3) Uani 1 1 d . . . H12A H 0.6402 -0.0263 0.0537 0.037 Uiso 1 1 calc R . . H12B H 0.7032 -0.1158 0.0706 0.037 Uiso 1 1 calc R . . H12C H 0.7255 -0.0736 0.0011 0.037 Uiso 1 1 calc R . . C13 C 0.88680(17) 0.29325(11) 0.04452(8) 0.0210(3) Uani 1 1 d . . . C14 C 0.77072(17) 0.29142(11) 0.00146(8) 0.0211(3) Uani 1 1 d . . . C15 C 0.69434(15) 0.22562(10) 0.02197(7) 0.0174(3) Uani 1 1 d . . . C16 C 1.0033(2) 0.35154(14) 0.04161(11) 0.0346(5) Uani 1 1 d . . . H16A H 1.0708 0.3391 0.0775 0.052 Uiso 1 1 calc R . . H16B H 0.9713 0.4087 0.0460 0.052 Uiso 1 1 calc R . . H16C H 1.0442 0.3452 -0.0006 0.052 Uiso 1 1 calc R . . C17 C 0.7365(2) 0.34692(15) -0.05568(10) 0.0349(5) Uani 1 1 d . . . H17A H 0.6486 0.3308 -0.0767 0.052 Uiso 1 1 calc R . . H17B H 0.8062 0.3420 -0.0875 0.052 Uiso 1 1 calc R . . H17C H 0.7322 0.4045 -0.0405 0.052 Uiso 1 1 calc R . . C18 C 0.56223(17) 0.19337(12) -0.00646(9) 0.0242(3) Uani 1 1 d . . . H18A H 0.5345 0.1458 0.0194 0.036 Uiso 1 1 calc R . . H18B H 0.5717 0.1760 -0.0520 0.036 Uiso 1 1 calc R . . H18C H 0.4937 0.2371 -0.0055 0.036 Uiso 1 1 calc R . . C19 C 1.11802(14) 0.14686(10) 0.23535(8) 0.0164(3) Uani 1 1 d . . . C20 C 1.02942(15) 0.29864(10) 0.19663(8) 0.0184(3) Uani 1 1 d . . . C21 C 1.16165(16) 0.20249(10) 0.11664(8) 0.0181(3) Uani 1 1 d . . . N10 N 0.54463(16) 0.40683(9) 0.17080(7) 0.0223(3) Uani 1 1 d . . . C22 C 0.5659(3) 0.49467(18) 0.15103(16) 0.0183(5) Uani 0.50 1 d PU A 1 H22A H 0.4805 0.5163 0.1296 0.022 Uiso 0.50 1 calc PR A 1 H22B H 0.5875 0.5282 0.1910 0.022 Uiso 0.50 1 calc PR A 1 C23 C 0.6759(4) 0.5052(3) 0.1055(2) 0.0266(7) Uani 0.50 1 d PU A 1 H23A H 0.6846 0.5641 0.0945 0.040 Uiso 0.50 1 calc PR A 1 H23B H 0.6542 0.4734 0.0652 0.040 Uiso 0.50 1 calc PR A 1 H23C H 0.7613 0.4852 0.1266 0.040 Uiso 0.50 1 calc PR A 1 C24 C 0.4949(3) 0.35444(18) 0.11038(14) 0.0147(5) Uani 0.50 1 d PU A 1 H24A H 0.5741 0.3419 0.0849 0.018 Uiso 0.50 1 calc PR A 1 H24B H 0.4610 0.3009 0.1266 0.018 Uiso 0.50 1 calc PR A 1 C25 C 0.3872(7) 0.3906(3) 0.0643(4) 0.0265(11) Uani 0.50 1 d PU A 1 H25A H 0.3655 0.3514 0.0284 0.040 Uiso 0.50 1 calc PR A 1 H25B H 0.4196 0.4427 0.0462 0.040 Uiso 0.50 1 calc PR A 1 H25C H 0.3060 0.4013 0.0880 0.040 Uiso 0.50 1 calc PR A 1 C26 C 0.6636(3) 0.36568(17) 0.20240(14) 0.0125(5) Uani 0.50 1 d PU A 1 H26A H 0.7351 0.3628 0.1707 0.015 Uiso 0.50 1 calc PR A 1 H26B H 0.6390 0.3081 0.2136 0.015 Uiso 0.50 1 calc PR A 1 C27 C 0.7201(15) 0.4088(11) 0.2641(9) 0.0212(17) Uani 0.50 1 d PU A 1 H27A H 0.7993 0.3783 0.2825 0.032 Uiso 0.50 1 calc PR A 1 H27B H 0.6509 0.4104 0.2963 0.032 Uiso 0.50 1 calc PR A 1 H27C H 0.7466 0.4655 0.2534 0.032 Uiso 0.50 1 calc PR A 1 C28 C 0.4246(3) 0.40942(19) 0.21730(15) 0.0155(5) Uani 0.50 1 d PU A 1 H28A H 0.4480 0.4487 0.2536 0.019 Uiso 0.50 1 calc PR A 1 H28B H 0.3434 0.4313 0.1922 0.019 Uiso 0.50 1 calc PR A 1 C29 C 0.389(2) 0.3254(12) 0.2469(10) 0.030(3) Uani 0.50 1 d PU A 1 H29A H 0.3137 0.3324 0.2752 0.045 Uiso 0.50 1 calc PR A 1 H29B H 0.4681 0.3038 0.2729 0.045 Uiso 0.50 1 calc PR A 1 H29C H 0.3632 0.2864 0.2114 0.045 Uiso 0.50 1 calc PR A 1 C22' C 0.6702(5) 0.3932(3) 0.1262(2) 0.0370(9) Uani 0.50 1 d PU A 2 H22C H 0.7400 0.3601 0.1513 0.044 Uiso 0.50 1 calc PR A 2 H22D H 0.6394 0.3607 0.0869 0.044 Uiso 0.50 1 calc PR A 2 C23' C 0.7347(8) 0.4744(4) 0.1038(3) 0.0513(15) Uani 0.50 1 d PU A 2 H23D H 0.8099 0.4616 0.0765 0.077 Uiso 0.50 1 calc PR A 2 H23E H 0.7686 0.5062 0.1424 0.077 Uiso 0.50 1 calc PR A 2 H23F H 0.6667 0.5072 0.0782 0.077 Uiso 0.50 1 calc PR A 2 C24' C 0.4433(5) 0.4576(3) 0.1364(3) 0.0443(11) Uani 0.50 1 d PU A 2 H24C H 0.4831 0.5125 0.1278 0.053 Uiso 0.50 1 calc PR A 2 H24D H 0.3676 0.4662 0.1651 0.053 Uiso 0.50 1 calc PR A 2 C25' C 0.3861(10) 0.4199(5) 0.0700(5) 0.0464(19) Uani 0.50 1 d PU A 2 H25D H 0.3189 0.4578 0.0492 0.070 Uiso 0.50 1 calc PR A 2 H25E H 0.3433 0.3664 0.0782 0.070 Uiso 0.50 1 calc PR A 2 H25F H 0.4600 0.4118 0.0410 0.070 Uiso 0.50 1 calc PR A 2 C26' C 0.6068(4) 0.4570(3) 0.2310(2) 0.0331(8) Uani 0.50 1 d PU A 2 H26C H 0.6424 0.5100 0.2146 0.040 Uiso 0.50 1 calc PR A 2 H26D H 0.5333 0.4707 0.2598 0.040 Uiso 0.50 1 calc PR A 2 C27' C 0.719(2) 0.4145(13) 0.2720(11) 0.034(4) Uani 0.50 1 d PU A 2 H27D H 0.7497 0.4507 0.3085 0.051 Uiso 0.50 1 calc PR A 2 H27E H 0.7945 0.4028 0.2447 0.051 Uiso 0.50 1 calc PR A 2 H27F H 0.6849 0.3623 0.2894 0.051 Uiso 0.50 1 calc PR A 2 C28' C 0.5054(5) 0.3225(3) 0.1901(2) 0.0348(9) Uani 0.50 1 d PU A 2 H28C H 0.5859 0.2922 0.2088 0.042 Uiso 0.50 1 calc PR A 2 H28D H 0.4681 0.2918 0.1510 0.042 Uiso 0.50 1 calc PR A 2 C29' C 0.396(2) 0.3279(15) 0.2427(11) 0.038(5) Uani 0.50 1 d PU A 2 H29D H 0.3699 0.2718 0.2555 0.058 Uiso 0.50 1 calc PR A 2 H29E H 0.3159 0.3574 0.2238 0.058 Uiso 0.50 1 calc PR A 2 H29F H 0.4334 0.3579 0.2815 0.058 Uiso 0.50 1 calc PR A 2 H1 H 0.635(2) 0.0884(13) 0.0958(10) 0.014(5) Uiso 1 1 d . . . H1A H 0.178(3) 0.545(2) 0.1699(17) 0.053(9) Uiso 1 1 d . . . H1B H 0.100(3) 0.473(2) 0.1734(16) 0.048(8) Uiso 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 Fe1 0.01110(10) 0.01339(11) 0.01357(11) 0.00010(7) -0.00179(7) -0.00214(6) O1 0.0408(8) 0.0269(7) 0.0291(7) -0.0015(6) -0.0020(6) -0.0116(6) N1 0.0123(5) 0.0152(5) 0.0140(5) -0.0007(4) -0.0016(4) -0.0013(4) N2 0.0116(5) 0.0168(6) 0.0142(5) 0.0006(4) -0.0011(4) -0.0027(4) N3 0.0123(5) 0.0163(6) 0.0154(5) -0.0008(4) -0.0010(4) -0.0026(4) N4 0.0130(5) 0.0166(6) 0.0165(6) -0.0023(4) -0.0007(4) -0.0036(4) N5 0.0139(5) 0.0184(6) 0.0162(6) 0.0030(5) -0.0032(4) -0.0044(4) N6 0.0123(5) 0.0178(6) 0.0137(5) 0.0007(4) -0.0023(4) -0.0026(4) N7 0.0186(6) 0.0264(7) 0.0203(6) 0.0013(5) -0.0011(5) 0.0026(5) N8 0.0277(7) 0.0192(7) 0.0332(8) -0.0026(6) 0.0015(6) -0.0034(5) N9 0.0225(7) 0.0293(8) 0.0263(7) -0.0008(6) 0.0049(5) -0.0036(6) B1 0.0141(6) 0.0172(7) 0.0137(7) 0.0002(5) -0.0011(5) -0.0029(5) C1 0.0161(6) 0.0165(6) 0.0152(6) -0.0004(5) -0.0013(5) 0.0013(5) C2 0.0169(6) 0.0199(7) 0.0161(6) 0.0003(5) 0.0015(5) 0.0012(5) C3 0.0140(6) 0.0176(6) 0.0162(6) 0.0013(5) 0.0013(5) -0.0005(5) C4 0.0202(7) 0.0272(8) 0.0177(7) -0.0072(6) -0.0022(5) -0.0004(6) C5 0.0273(8) 0.0364(10) 0.0206(8) -0.0032(7) 0.0069(6) 0.0017(7) C6 0.0140(6) 0.0316(9) 0.0229(7) 0.0003(6) 0.0021(5) -0.0049(6) C7 0.0165(6) 0.0166(6) 0.0154(6) -0.0005(5) 0.0029(5) -0.0016(5) C8 0.0211(6) 0.0161(6) 0.0162(6) -0.0020(5) 0.0034(5) -0.0029(5) C9 0.0197(6) 0.0167(7) 0.0152(6) -0.0026(5) 0.0005(5) -0.0052(5) C10 0.0163(6) 0.0210(7) 0.0252(8) -0.0015(6) 0.0027(5) 0.0014(5) C11 0.0301(8) 0.0186(7) 0.0247(8) -0.0052(6) 0.0068(6) -0.0008(6) C12 0.0240(7) 0.0233(8) 0.0254(8) -0.0077(6) -0.0020(6) -0.0084(6) C13 0.0199(7) 0.0227(7) 0.0197(7) 0.0064(6) -0.0040(5) -0.0052(6) C14 0.0206(7) 0.0249(8) 0.0171(7) 0.0065(6) -0.0036(5) -0.0026(6) C15 0.0156(6) 0.0228(7) 0.0133(6) 0.0008(5) -0.0021(5) -0.0001(5) C16 0.0304(9) 0.0366(10) 0.0351(10) 0.0203(8) -0.0108(8) -0.0177(8) C17 0.0353(10) 0.0400(11) 0.0277(9) 0.0178(8) -0.0102(7) -0.0082(8) C18 0.0179(7) 0.0341(9) 0.0194(7) 0.0041(6) -0.0069(6) -0.0044(6) C19 0.0139(6) 0.0166(6) 0.0185(7) -0.0004(5) 0.0003(5) -0.0016(5) C20 0.0150(6) 0.0188(7) 0.0210(7) 0.0010(5) -0.0013(5) -0.0024(5) C21 0.0173(6) 0.0191(7) 0.0178(7) -0.0010(5) -0.0004(5) -0.0032(5) N10 0.0305(7) 0.0160(6) 0.0201(6) -0.0024(5) 0.0005(5) 0.0039(5) C22 0.0258(14) 0.0082(11) 0.0203(14) -0.0003(10) -0.0022(11) -0.0004(10) C23 0.0326(19) 0.0200(17) 0.0278(19) -0.0027(14) 0.0064(15) -0.0029(14) C24 0.0197(12) 0.0120(12) 0.0121(11) -0.0047(9) -0.0006(9) -0.0016(9) C25 0.0287(19) 0.026(3) 0.024(2) 0.004(2) -0.0054(14) -0.003(2) C26 0.0117(10) 0.0121(11) 0.0136(11) -0.0022(9) -0.0009(9) 0.0041(9) C27 0.018(3) 0.030(4) 0.016(3) -0.006(3) -0.0014(19) 0.003(2) C28 0.0134(11) 0.0180(13) 0.0154(12) -0.0026(10) 0.0024(9) 0.0073(10) C29 0.025(5) 0.029(6) 0.036(5) 0.010(4) 0.001(4) -0.003(4) C22' 0.044(2) 0.032(2) 0.036(2) -0.0070(17) 0.0080(17) 0.0014(17) C23' 0.078(4) 0.047(3) 0.031(2) -0.004(2) 0.022(3) -0.028(3) C24' 0.046(2) 0.033(2) 0.052(3) 0.002(2) -0.010(2) 0.0098(19) C25' 0.045(3) 0.043(4) 0.048(4) 0.014(4) -0.018(3) -0.001(4) C26' 0.037(2) 0.0277(18) 0.035(2) -0.0069(16) 0.0059(16) 0.0016(15) C27' 0.035(5) 0.037(5) 0.031(7) -0.006(4) -0.002(4) 0.002(3) C28' 0.039(2) 0.0262(18) 0.039(2) 0.0016(16) -0.0012(17) -0.0023(15) C29' 0.024(5) 0.045(9) 0.047(8) -0.004(6) 0.006(4) -0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C20 1.9200(17) . ? Fe1 C19 1.9213(15) . ? Fe1 C21 1.9227(16) . ? Fe1 N1 2.0024(13) . ? Fe1 N3 2.0058(13) . ? Fe1 N5 2.0067(13) . ? O1 H1A 0.89(4) . ? O1 H1B 0.92(3) . ? N1 C1 1.347(2) . ? N1 N2 1.3651(16) . ? N2 C3 1.3494(19) . ? N2 B1 1.535(2) . ? N3 C7 1.348(2) . ? N3 N4 1.3687(16) . ? N4 C9 1.350(2) . ? N4 B1 1.532(2) . ? N5 C13 1.347(2) . ? N5 N6 1.3669(17) . ? N6 C15 1.3487(19) . ? N6 B1 1.531(2) . ? N7 C19 1.149(2) . ? N8 C20 1.153(2) . ? N9 C21 1.154(2) . ? B1 H1 1.06(2) . ? C1 C2 1.404(2) . ? C1 C4 1.489(2) . ? C2 C3 1.390(2) . ? C2 C5 1.498(2) . ? C3 C6 1.490(2) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.401(2) . ? C7 C10 1.491(2) . ? C8 C9 1.382(2) . ? C8 C11 1.495(2) . ? C9 C12 1.492(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.402(2) . ? C13 C16 1.492(2) . ? C14 C15 1.383(2) . ? C14 C17 1.491(2) . ? C15 C18 1.491(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? N10 C24' 1.442(5) . ? N10 C26 1.465(3) . ? N10 C28' 1.474(5) . ? N10 C22 1.491(3) . ? N10 C24 1.549(3) . ? N10 C26' 1.564(5) . ? N10 C28 1.568(3) . ? N10 C22' 1.602(5) . ? C22 C23 1.487(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.494(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.513(19) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.53(2) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C22' C23' 1.540(7) . ? C22' H22C 0.9900 . ? C22' H22D 0.9900 . ? C23' H23D 0.9800 . ? C23' H23E 0.9800 . ? C23' H23F 0.9800 . ? C24' C25' 1.558(10) . ? C24' H24C 0.9900 . ? C24' H24D 0.9900 . ? C25' H25D 0.9800 . ? C25' H25E 0.9800 . ? C25' H25F 0.9800 . ? C26' C27' 1.51(2) . ? C26' H26C 0.9900 . ? C26' H26D 0.9900 . ? C27' H27D 0.9800 . ? C27' H27E 0.9800 . ? C27' H27F 0.9800 . ? C28' C29' 1.58(2) . ? C28' H28C 0.9900 . ? C28' H28D 0.9900 . ? C29' H29D 0.9800 . ? C29' H29E 0.9800 . ? C29' H29F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 Fe1 C19 89.34(7) . . ? C20 Fe1 C21 87.45(7) . . ? C19 Fe1 C21 86.90(7) . . ? C20 Fe1 N1 91.47(6) . . ? C19 Fe1 N1 90.37(6) . . ? C21 Fe1 N1 177.07(6) . . ? C20 Fe1 N3 179.01(6) . . ? C19 Fe1 N3 91.36(6) . . ? C21 Fe1 N3 91.88(6) . . ? N1 Fe1 N3 89.24(5) . . ? C20 Fe1 N5 90.10(6) . . ? C19 Fe1 N5 179.42(6) . . ? C21 Fe1 N5 92.90(6) . . ? N1 Fe1 N5 89.82(5) . . ? N3 Fe1 N5 89.20(5) . . ? H1A O1 H1B 101(3) . . ? C1 N1 N2 106.74(12) . . ? C1 N1 Fe1 135.72(10) . . ? N2 N1 Fe1 117.53(10) . . ? C3 N2 N1 110.34(12) . . ? C3 N2 B1 130.56(12) . . ? N1 N2 B1 119.09(12) . . ? C7 N3 N4 106.55(12) . . ? C7 N3 Fe1 135.67(10) . . ? N4 N3 Fe1 117.31(10) . . ? C9 N4 N3 110.09(13) . . ? C9 N4 B1 130.71(13) . . ? N3 N4 B1 119.10(12) . . ? C13 N5 N6 106.69(12) . . ? C13 N5 Fe1 136.03(11) . . ? N6 N5 Fe1 117.23(10) . . ? C15 N6 N5 110.15(12) . . ? C15 N6 B1 130.26(13) . . ? N5 N6 B1 119.30(12) . . ? N6 B1 N4 107.12(12) . . ? N6 B1 N2 108.18(12) . . ? N4 B1 N2 108.71(12) . . ? N6 B1 H1 109.7(12) . . ? N4 B1 H1 110.6(12) . . ? N2 B1 H1 112.3(12) . . ? N1 C1 C2 109.74(13) . . ? N1 C1 C4 124.15(14) . . ? C2 C1 C4 126.10(15) . . ? C3 C2 C1 105.34(13) . . ? C3 C2 C5 127.47(15) . . ? C1 C2 C5 127.16(15) . . ? N2 C3 C2 107.84(13) . . ? N2 C3 C6 122.46(14) . . ? C2 C3 C6 129.70(14) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 109.73(13) . . ? N3 C7 C10 124.27(14) . . ? C8 C7 C10 125.99(14) . . ? C9 C8 C7 105.55(14) . . ? C9 C8 C11 127.80(15) . . ? C7 C8 C11 126.62(15) . . ? N4 C9 C8 108.07(13) . . ? N4 C9 C12 122.44(15) . . ? C8 C9 C12 129.48(15) . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N5 C13 C14 109.57(14) . . ? N5 C13 C16 123.99(14) . . ? C14 C13 C16 126.42(15) . . ? C15 C14 C13 105.62(14) . . ? C15 C14 C17 126.53(15) . . ? C13 C14 C17 127.84(16) . . ? N6 C15 C14 107.96(13) . . ? N6 C15 C18 122.74(14) . . ? C14 C15 C18 129.30(14) . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N7 C19 Fe1 178.08(14) . . ? N8 C20 Fe1 177.94(16) . . ? N9 C21 Fe1 178.66(16) . . ? C24' N10 C26 170.4(3) . . ? C24' N10 C28' 117.8(3) . . ? C26 N10 C28' 71.6(2) . . ? C24' N10 C22 55.6(3) . . ? C26 N10 C22 115.2(2) . . ? C28' N10 C22 172.8(3) . . ? C24' N10 C24 75.3(3) . . ? C26 N10 C24 108.02(18) . . ? C28' N10 C24 68.5(2) . . ? C22 N10 C24 110.24(19) . . ? C24' N10 C26' 108.4(3) . . ? C26 N10 C26' 67.9(2) . . ? C28' N10 C26' 111.4(3) . . ? C22 N10 C26' 70.4(2) . . ? C24 N10 C26' 175.3(2) . . ? C24' N10 C28 75.4(3) . . ? C26 N10 C28 111.44(18) . . ? C28' N10 C28 68.9(2) . . ? C22 N10 C28 105.29(19) . . ? C24 N10 C28 106.31(18) . . ? C26' N10 C28 77.7(2) . . ? C24' N10 C22' 110.1(3) . . ? C26 N10 C22' 63.6(2) . . ? C28' N10 C22' 104.6(3) . . ? C22 N10 C22' 81.3(2) . . ? C24 N10 C22' 72.1(2) . . ? C26' N10 C22' 103.6(3) . . ? C28 N10 C22' 173.2(2) . . ? C23 C22 N10 113.6(3) . . ? C23 C22 H22A 108.9 . . ? N10 C22 H22A 108.9 . . ? C23 C22 H22B 108.9 . . ? N10 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 N10 117.8(3) . . ? C25 C24 H24A 107.9 . . ? N10 C24 H24A 107.9 . . ? C25 C24 H24B 107.9 . . ? N10 C24 H24B 107.9 . . ? H24A C24 H24B 107.2 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N10 C26 C27 113.7(6) . . ? N10 C26 H26A 108.8 . . ? C27 C26 H26A 108.8 . . ? N10 C26 H26B 108.8 . . ? C27 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 N10 114.6(8) . . ? C29 C28 H28A 108.6 . . ? N10 C28 H28A 108.6 . . ? C29 C28 H28B 108.6 . . ? N10 C28 H28B 108.6 . . ? H28A C28 H28B 107.6 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C23' C22' N10 113.8(4) . . ? C23' C22' H22C 108.8 . . ? N10 C22' H22C 108.8 . . ? C23' C22' H22D 108.8 . . ? N10 C22' H22D 108.8 . . ? H22C C22' H22D 107.7 . . ? C22' C23' H23D 109.5 . . ? C22' C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? C22' C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? N10 C24' C25' 113.9(5) . . ? N10 C24' H24C 108.8 . . ? C25' C24' H24C 108.8 . . ? N10 C24' H24D 108.8 . . ? C25' C24' H24D 108.8 . . ? H24C C24' H24D 107.7 . . ? C24' C25' H25D 109.5 . . ? C24' C25' H25E 109.5 . . ? H25D C25' H25E 109.5 . . ? C24' C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? C27' C26' N10 116.0(9) . . ? C27' C26' H26C 108.3 . . ? N10 C26' H26C 108.3 . . ? C27' C26' H26D 108.3 . . ? N10 C26' H26D 108.3 . . ? H26C C26' H26D 107.4 . . ? C26' C27' H27D 109.5 . . ? C26' C27' H27E 109.5 . . ? H27D C27' H27E 109.5 . . ? C26' C27' H27F 109.5 . . ? H27D C27' H27F 109.5 . . ? H27E C27' H27F 109.5 . . ? N10 C28' C29' 109.6(9) . . ? N10 C28' H28C 109.7 . . ? C29' C28' H28C 109.7 . . ? N10 C28' H28D 109.7 . . ? C29' C28' H28D 109.7 . . ? H28C C28' H28D 108.2 . . ? C28' C29' H29D 109.5 . . ? C28' C29' H29E 109.5 . . ? H29D C29' H29E 109.5 . . ? C28' C29' H29F 109.5 . . ? H29D C29' H29F 109.5 . . ? H29E C29' H29F 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 C20 Fe1 N1 C1 -45.51(16) . . . . ? C19 Fe1 N1 C1 43.84(16) . . . . ? C21 Fe1 N1 C1 22.6(13) . . . . ? N3 Fe1 N1 C1 135.19(15) . . . . ? N5 Fe1 N1 C1 -135.61(15) . . . . ? C20 Fe1 N1 N2 135.24(11) . . . . ? C19 Fe1 N1 N2 -135.41(11) . . . . ? C21 Fe1 N1 N2 -156.6(12) . . . . ? N3 Fe1 N1 N2 -44.06(11) . . . . ? N5 Fe1 N1 N2 45.14(11) . . . . ? C1 N1 N2 C3 0.18(17) . . . . ? Fe1 N1 N2 C3 179.63(10) . . . . ? C1 N1 N2 B1 179.02(13) . . . . ? Fe1 N1 N2 B1 -1.52(17) . . . . ? C20 Fe1 N3 C7 83(3) . . . . ? C19 Fe1 N3 C7 -51.64(16) . . . . ? C21 Fe1 N3 C7 35.30(16) . . . . ? N1 Fe1 N3 C7 -142.00(15) . . . . ? N5 Fe1 N3 C7 128.18(15) . . . . ? C20 Fe1 N3 N4 -88(3) . . . . ? C19 Fe1 N3 N4 137.44(11) . . . . ? C21 Fe1 N3 N4 -135.61(11) . . . . ? N1 Fe1 N3 N4 47.09(11) . . . . ? N5 Fe1 N3 N4 -42.74(11) . . . . ? C7 N3 N4 C9 -0.72(17) . . . . ? Fe1 N3 N4 C9 172.67(10) . . . . ? C7 N3 N4 B1 -177.51(13) . . . . ? Fe1 N3 N4 B1 -4.12(17) . . . . ? C20 Fe1 N5 C13 48.74(18) . . . . ? C19 Fe1 N5 C13 31(6) . . . . ? C21 Fe1 N5 C13 -38.71(18) . . . . ? N1 Fe1 N5 C13 140.21(18) . . . . ? N3 Fe1 N5 C13 -130.55(18) . . . . ? C20 Fe1 N5 N6 -134.44(12) . . . . ? C19 Fe1 N5 N6 -152(6) . . . . ? C21 Fe1 N5 N6 138.11(12) . . . . ? N1 Fe1 N5 N6 -42.98(11) . . . . ? N3 Fe1 N5 N6 46.26(11) . . . . ? C13 N5 N6 C15 0.83(18) . . . . ? Fe1 N5 N6 C15 -176.86(10) . . . . ? C13 N5 N6 B1 175.22(14) . . . . ? Fe1 N5 N6 B1 -2.48(18) . . . . ? C15 N6 B1 N4 115.70(17) . . . . ? N5 N6 B1 N4 -57.39(17) . . . . ? C15 N6 B1 N2 -127.27(16) . . . . ? N5 N6 B1 N2 59.64(17) . . . . ? C9 N4 B1 N6 -114.58(17) . . . . ? N3 N4 B1 N6 61.45(16) . . . . ? C9 N4 B1 N2 128.74(16) . . . . ? N3 N4 B1 N2 -55.23(17) . . . . ? C3 N2 B1 N6 121.38(16) . . . . ? N1 N2 B1 N6 -57.19(17) . . . . ? C3 N2 B1 N4 -122.62(16) . . . . ? N1 N2 B1 N4 58.81(17) . . . . ? N2 N1 C1 C2 -0.24(17) . . . . ? Fe1 N1 C1 C2 -179.55(12) . . . . ? N2 N1 C1 C4 178.57(14) . . . . ? Fe1 N1 C1 C4 -0.7(2) . . . . ? N1 C1 C2 C3 0.21(18) . . . . ? C4 C1 C2 C3 -178.57(15) . . . . ? N1 C1 C2 C5 -178.03(16) . . . . ? C4 C1 C2 C5 3.2(3) . . . . ? N1 N2 C3 C2 -0.05(17) . . . . ? B1 N2 C3 C2 -178.72(15) . . . . ? N1 N2 C3 C6 179.75(14) . . . . ? B1 N2 C3 C6 1.1(3) . . . . ? C1 C2 C3 N2 -0.10(17) . . . . ? C5 C2 C3 N2 178.14(17) . . . . ? C1 C2 C3 C6 -179.87(16) . . . . ? C5 C2 C3 C6 -1.6(3) . . . . ? N4 N3 C7 C8 0.68(17) . . . . ? Fe1 N3 C7 C8 -170.91(12) . . . . ? N4 N3 C7 C10 -178.44(14) . . . . ? Fe1 N3 C7 C10 10.0(2) . . . . ? N3 C7 C8 C9 -0.39(18) . . . . ? C10 C7 C8 C9 178.71(15) . . . . ? N3 C7 C8 C11 177.90(15) . . . . ? C10 C7 C8 C11 -3.0(3) . . . . ? N3 N4 C9 C8 0.48(18) . . . . ? B1 N4 C9 C8 176.78(15) . . . . ? N3 N4 C9 C12 179.36(14) . . . . ? B1 N4 C9 C12 -4.3(3) . . . . ? C7 C8 C9 N4 -0.06(18) . . . . ? C11 C8 C9 N4 -178.33(16) . . . . ? C7 C8 C9 C12 -178.84(17) . . . . ? C11 C8 C9 C12 2.9(3) . . . . ? N6 N5 C13 C14 -0.2(2) . . . . ? Fe1 N5 C13 C14 176.89(13) . . . . ? N6 N5 C13 C16 -178.61(19) . . . . ? Fe1 N5 C13 C16 -1.6(3) . . . . ? N5 C13 C14 C15 -0.5(2) . . . . ? C16 C13 C14 C15 177.9(2) . . . . ? N5 C13 C14 C17 -179.23(19) . . . . ? C16 C13 C14 C17 -0.8(3) . . . . ? N5 N6 C15 C14 -1.19(18) . . . . ? B1 N6 C15 C14 -174.77(16) . . . . ? N5 N6 C15 C18 178.44(15) . . . . ? B1 N6 C15 C18 4.9(3) . . . . ? C13 C14 C15 N6 1.0(2) . . . . ? C17 C14 C15 N6 179.75(19) . . . . ? C13 C14 C15 C18 -178.55(18) . . . . ? C17 C14 C15 C18 0.1(3) . . . . ? C20 Fe1 C19 N7 150(4) . . . . ? C21 Fe1 C19 N7 -123(4) . . . . ? N1 Fe1 C19 N7 58(4) . . . . ? N3 Fe1 C19 N7 -31(4) . . . . ? N5 Fe1 C19 N7 167(15) . . . . ? C19 Fe1 C20 N8 -163(5) . . . . ? C21 Fe1 C20 N8 110(5) . . . . ? N1 Fe1 C20 N8 -72(5) . . . . ? N3 Fe1 C20 N8 63(7) . . . . ? N5 Fe1 C20 N8 17(5) . . . . ? C20 Fe1 C21 N9 93(7) . . . . ? C19 Fe1 C21 N9 4(7) . . . . ? N1 Fe1 C21 N9 25(8) . . . . ? N3 Fe1 C21 N9 -88(7) . . . . ? N5 Fe1 C21 N9 -177(100) . . . . ? C24' N10 C22 C23 -119.4(4) . . . . ? C26 N10 C22 C23 57.6(3) . . . . ? C28' N10 C22 C23 -143(2) . . . . ? C24 N10 C22 C23 -64.9(3) . . . . ? C26' N10 C22 C23 110.1(3) . . . . ? C28 N10 C22 C23 -179.2(3) . . . . ? C22' N10 C22 C23 2.3(3) . . . . ? C24' N10 C24 C25 -0.2(4) . . . . ? C26 N10 C24 C25 -170.9(4) . . . . ? C28' N10 C24 C25 128.2(4) . . . . ? C22 N10 C24 C25 -44.2(4) . . . . ? C26' N10 C24 C25 -142(3) . . . . ? C28 N10 C24 C25 69.4(4) . . . . ? C22' N10 C24 C25 -117.5(4) . . . . ? C24' N10 C26 C27 73.4(19) . . . . ? C28' N10 C26 C27 -118.8(8) . . . . ? C22 N10 C26 C27 58.5(8) . . . . ? C24 N10 C26 C27 -177.8(8) . . . . ? C26' N10 C26 C27 4.6(8) . . . . ? C28 N10 C26 C27 -61.4(8) . . . . ? C22' N10 C26 C27 123.7(8) . . . . ? C24' N10 C28 C29 135.5(9) . . . . ? C26 N10 C28 C29 -51.5(9) . . . . ? C28' N10 C28 C29 7.5(9) . . . . ? C22 N10 C28 C29 -177.0(8) . . . . ? C24 N10 C28 C29 66.0(9) . . . . ? C26' N10 C28 C29 -111.5(9) . . . . ? C22' N10 C28 C29 -9(2) . . . . ? C24' N10 C22' C23' 56.3(5) . . . . ? C26 N10 C22' C23' -115.9(5) . . . . ? C28' N10 C22' C23' -176.2(4) . . . . ? C22 N10 C22' C23' 7.9(4) . . . . ? C24 N10 C22' C23' 122.6(4) . . . . ? C26' N10 C22' C23' -59.4(5) . . . . ? C28 N10 C22' C23' -160.1(18) . . . . ? C26 N10 C24' C25' 106.9(16) . . . . ? C28' N10 C24' C25' -60.0(6) . . . . ? C22 N10 C24' C25' 123.3(6) . . . . ? C24 N10 C24' C25' -4.5(5) . . . . ? C26' N10 C24' C25' 172.4(5) . . . . ? C28 N10 C24' C25' -116.2(6) . . . . ? C22' N10 C24' C25' 59.7(6) . . . . ? C24' N10 C26' C27' -178.2(10) . . . . ? C26 N10 C26' C27' -7.5(10) . . . . ? C28' N10 C26' C27' 50.7(10) . . . . ? C22 N10 C26' C27' -136.7(10) . . . . ? C24 N10 C26' C27' -38(3) . . . . ? C28 N10 C26' C27' 111.9(10) . . . . ? C22' N10 C26' C27' -61.3(10) . . . . ? C24' N10 C28' C29' -65.6(9) . . . . ? C26 N10 C28' C29' 116.7(9) . . . . ? C22 N10 C28' C29' -43(2) . . . . ? C24 N10 C28' C29' -124.5(9) . . . . ? C26' N10 C28' C29' 60.5(9) . . . . ? C28 N10 C28' C29' -6.1(9) . . . . ? C22' N10 C28' C29' 171.9(9) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 31.24 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.740 _refine_diff_density_min -0.725 _refine_diff_density_rms 0.088 # Attachment '2.cif.txt' # {[(Tp*Me)Fe(CN)3]4[Ni(tren)]4[ClO4]}.7H2O.4MeCN (2) data_2 _database_code_depnum_ccdc_archive 'CCDC 768190' #TrackingRef '2.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Octa-Fe4Ni4 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C116 H212 B4 Cl4 Fe4 N56 Ni4 O24' _chemical_formula_weight 3418.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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 P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.0577(10) _cell_length_b 14.5679(11) _cell_length_c 23.4120(18) _cell_angle_alpha 75.052(3) _cell_angle_beta 77.373(3) _cell_angle_gamma 62.117(3) _cell_volume 4067.5(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9849 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 27.71 _exptl_crystal_description Rectangular _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1796 _exptl_absorpt_coefficient_mu 0.942 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7269 _exptl_absorpt_correction_T_max 0.9076 _exptl_absorpt_process_details 'sadabs v2008/1' _exptl_special_details ; All NH and BH H atoms were located but not refined. All other H atoms were added in their calculated positions and were treated using appropriate riding models. ; _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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 87956 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.09 _reflns_number_total 18879 _reflns_number_gt 12905 _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^)+(0.0734P)^2^+14.8582P] 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 18879 _refine_ls_number_parameters 1026 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1037 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1897 _refine_ls_wR_factor_gt 0.1525 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.009 _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 0.99763(5) 0.37367(4) 0.38903(2) 0.01354(13) Uani 1 1 d . . . Fe2 Fe 0.70027(5) 0.50279(5) 0.12678(3) 0.02234(15) Uani 1 1 d . . . Ni1 Ni 1.21305(4) 0.56285(4) 0.40747(2) 0.01619(12) Uani 1 1 d . . . Ni2 Ni 0.76615(4) 0.70272(4) 0.24962(2) 0.01793(13) Uani 1 1 d . . . B1 B 1.0941(4) 0.1396(4) 0.3806(2) 0.0197(9) Uani 1 1 d . . . H1 H 1.1259 0.0636 0.3772 0.024 Uiso 1 1 calc R . . B2 B 0.8081(5) 0.3433(5) 0.0422(2) 0.0311(12) Uani 1 1 d . . . H2 H 0.8439 0.2912 0.0146 0.037 Uiso 1 1 calc R . . N1 N 0.8629(3) 0.5677(3) 0.30199(15) 0.0192(7) Uani 1 1 d . . . N2 N 1.1165(3) 0.5009(3) 0.39612(15) 0.0188(7) Uani 1 1 d . . . N3 N 0.8413(3) 0.4513(3) 0.49969(15) 0.0180(7) Uani 1 1 d . . . N4 N 0.7780(3) 0.6186(3) 0.18451(16) 0.0218(8) Uani 1 1 d . . . N5 N 0.5889(3) 0.4720(4) 0.25424(19) 0.0357(10) Uani 1 1 d . . . N6 N 0.5073(5) 0.7218(4) 0.1054(3) 0.0528(14) Uani 1 1 d . . . N7 N 0.9710(3) 0.1936(3) 0.37864(15) 0.0174(7) Uani 1 1 d . . . N8 N 0.9138(3) 0.2964(3) 0.38518(14) 0.0164(7) Uani 1 1 d . . . N9 N 1.1440(3) 0.2009(3) 0.32947(16) 0.0195(7) Uani 1 1 d . . . N10 N 1.1046(3) 0.3083(3) 0.32367(15) 0.0191(7) Uani 1 1 d . . . N11 N 1.1161(3) 0.1517(3) 0.43877(15) 0.0178(7) Uani 1 1 d . . . N12 N 1.0872(3) 0.2505(3) 0.44796(15) 0.0166(7) Uani 1 1 d . . . N13 N 0.6871(3) 0.3736(3) 0.05586(18) 0.0292(9) Uani 1 1 d . . . N14 N 0.6273(3) 0.4378(3) 0.09637(17) 0.0287(9) Uani 1 1 d . . . N15 N 0.8220(3) 0.4444(3) 0.01505(16) 0.0274(9) Uani 1 1 d . . . N16 N 0.7746(3) 0.5266(3) 0.04513(16) 0.0260(8) Uani 1 1 d . . . N17 N 0.8587(3) 0.2986(3) 0.10104(17) 0.0278(9) Uani 1 1 d . . . N18 N 0.8259(3) 0.3632(3) 0.14217(16) 0.0223(8) Uani 1 1 d . . . N19 N 1.1000(3) 0.7247(3) 0.40470(18) 0.0270(8) Uani 1 1 d . . . H19A H 1.0723 0.7520 0.3687 0.032 Uiso 1 1 calc R . . H19B H 1.0436 0.7304 0.4344 0.032 Uiso 1 1 calc R . . N20 N 1.3471(3) 0.4158(3) 0.42591(18) 0.0260(8) Uani 1 1 d . . . H20A H 1.3309 0.3779 0.4614 0.031 Uiso 1 1 calc R . . H20B H 1.3631 0.3778 0.3964 0.031 Uiso 1 1 calc R . . N21 N 1.2636(3) 0.5866(3) 0.31632(16) 0.0259(8) Uani 1 1 d . . . H21A H 1.3102 0.5226 0.3051 0.031 Uiso 1 1 calc R . . H21B H 1.2046 0.6169 0.2954 0.031 Uiso 1 1 calc R . . N22 N 1.3202(3) 0.6222(3) 0.41267(16) 0.0215(8) Uani 1 1 d . . . N23 N 0.7549(3) 0.7925(3) 0.30969(17) 0.0239(8) Uani 1 1 d . . . H23A H 0.7084 0.7849 0.3429 0.029 Uiso 1 1 calc R . . H23E H 0.8220 0.7695 0.3215 0.029 Uiso 1 1 calc R . . N24 N 0.8878(3) 0.7393(3) 0.19233(18) 0.0283(9) Uani 1 1 d . . . H24A H 0.9315 0.7440 0.2145 0.034 Uiso 1 1 calc R . . H24E H 0.9303 0.6866 0.1706 0.034 Uiso 1 1 calc R . . N25 N 0.6193(3) 0.6886(3) 0.28381(16) 0.0222(8) Uani 1 1 d . . . H25A H 0.6234 0.6289 0.2748 0.027 Uiso 1 1 calc R . . H25B H 0.6088 0.6825 0.3245 0.027 Uiso 1 1 calc R . . N26 N 0.6613(3) 0.8489(3) 0.20479(16) 0.0238(8) Uani 1 1 d . . . C1 C 0.9130(3) 0.4952(3) 0.33486(18) 0.0173(8) Uani 1 1 d . . . C2 C 1.0724(3) 0.4530(3) 0.39314(17) 0.0163(8) Uani 1 1 d . . . C3 C 0.8968(3) 0.4295(3) 0.45608(18) 0.0155(8) Uani 1 1 d . . . C4 C 0.7559(4) 0.5727(3) 0.16033(18) 0.0212(9) Uani 1 1 d . . . C5 C 0.6298(4) 0.4818(4) 0.2064(2) 0.0278(10) Uani 1 1 d . . . C6 C 0.5790(4) 0.6392(4) 0.1126(2) 0.0319(11) Uani 1 1 d . . . C7 C 0.8088(3) 0.3233(3) 0.38308(17) 0.0168(8) Uani 1 1 d . . . C8 C 0.7989(3) 0.2360(3) 0.37545(18) 0.0190(8) Uani 1 1 d . . . C9 C 0.9030(4) 0.1556(3) 0.37240(19) 0.0202(8) Uani 1 1 d . . . C10 C 0.9412(4) 0.0457(4) 0.3634(2) 0.0292(10) Uani 1 1 d . . . H10A H 1.0143 0.0214 0.3420 0.044 Uiso 1 1 calc R . . H10B H 0.8920 0.0442 0.3401 0.044 Uiso 1 1 calc R . . H10C H 0.9423 -0.0007 0.4021 0.044 Uiso 1 1 calc R . . C11 C 0.6966(4) 0.2337(4) 0.3689(2) 0.0279(10) Uani 1 1 d . . . H11A H 0.7143 0.1686 0.3554 0.042 Uiso 1 1 calc R . . H11B H 0.6570 0.2948 0.3397 0.042 Uiso 1 1 calc R . . H11C H 0.6515 0.2360 0.4074 0.042 Uiso 1 1 calc R . . C12 C 0.7186(3) 0.4302(3) 0.38561(19) 0.0190(8) Uani 1 1 d . . . H12A H 0.7439 0.4736 0.3980 0.028 Uiso 1 1 calc R . . H12B H 0.6586 0.4244 0.4143 0.028 Uiso 1 1 calc R . . H12C H 0.6937 0.4632 0.3462 0.028 Uiso 1 1 calc R . . C13 C 1.1611(4) 0.3405(4) 0.27572(19) 0.0255(10) Uani 1 1 d . . . C14 C 1.2386(4) 0.2515(4) 0.2507(2) 0.0330(11) Uani 1 1 d . . . C15 C 1.2259(4) 0.1657(4) 0.2859(2) 0.0287(10) Uani 1 1 d . . . C16 C 1.2879(4) 0.0519(4) 0.2819(2) 0.0388(13) Uani 1 1 d . . . H16A H 1.2374 0.0223 0.2832 0.058 Uiso 1 1 calc R . . H16B H 1.3311 0.0142 0.3154 0.058 Uiso 1 1 calc R . . H16C H 1.3360 0.0442 0.2444 0.058 Uiso 1 1 calc R . . C17 C 1.3196(6) 0.2533(5) 0.1972(3) 0.0526(17) Uani 1 1 d . . . H17A H 1.3323 0.1993 0.1749 0.079 Uiso 1 1 calc R . . H17B H 1.3879 0.2387 0.2101 0.079 Uiso 1 1 calc R . . H17C H 1.2916 0.3230 0.1716 0.079 Uiso 1 1 calc R . . C18 C 1.1419(4) 0.4520(4) 0.2524(2) 0.0316(11) Uani 1 1 d . . . H18A H 1.1081 0.4925 0.2848 0.047 Uiso 1 1 calc R . . H18B H 1.0938 0.4823 0.2211 0.047 Uiso 1 1 calc R . . H18C H 1.2111 0.4547 0.2360 0.047 Uiso 1 1 calc R . . C19 C 1.1280(3) 0.2385(3) 0.49778(18) 0.0169(8) Uani 1 1 d . . . C20 C 1.1824(4) 0.1308(3) 0.5212(2) 0.0214(9) Uani 1 1 d . . . C21 C 1.1735(4) 0.0783(3) 0.4823(2) 0.0215(9) Uani 1 1 d . . . C22 C 1.2155(5) -0.0368(4) 0.4837(2) 0.0336(12) Uani 1 1 d . . . H22A H 1.1546 -0.0542 0.4879 0.050 Uiso 1 1 calc R . . H22B H 1.2577 -0.0769 0.5175 0.050 Uiso 1 1 calc R . . H22C H 1.2619 -0.0552 0.4466 0.050 Uiso 1 1 calc R . . C23 C 1.2412(4) 0.0842(4) 0.5756(2) 0.0312(11) Uani 1 1 d . . . H23B H 1.2799 0.0072 0.5790 0.047 Uiso 1 1 calc R . . H23C H 1.1890 0.1019 0.6110 0.047 Uiso 1 1 calc R . . H23D H 1.2933 0.1129 0.5722 0.047 Uiso 1 1 calc R . . C24 C 1.1181(4) 0.3269(3) 0.52364(19) 0.0205(9) Uani 1 1 d . . . H24B H 1.0538 0.3912 0.5113 0.031 Uiso 1 1 calc R . . H24C H 1.1828 0.3394 0.5094 0.031 Uiso 1 1 calc R . . H24D H 1.1114 0.3081 0.5672 0.031 Uiso 1 1 calc R . . C25 C 0.5244(4) 0.4508(4) 0.1009(2) 0.0339(12) Uani 1 1 d . . . C26 C 0.5196(5) 0.3932(5) 0.0628(2) 0.0370(13) Uani 1 1 d . . . C27 C 0.6235(5) 0.3455(4) 0.0354(2) 0.0345(12) Uani 1 1 d . . . C28 C 0.6662(6) 0.2753(5) -0.0088(3) 0.0517(17) Uani 1 1 d . . . H28A H 0.7181 0.2934 -0.0390 0.077 Uiso 1 1 calc R . . H28B H 0.6063 0.2840 -0.0279 0.077 Uiso 1 1 calc R . . H28C H 0.7025 0.2018 0.0112 0.077 Uiso 1 1 calc R . . C29 C 0.4206(5) 0.3868(5) 0.0527(3) 0.0483(16) Uani 1 1 d . . . H29A H 0.4150 0.4031 0.0099 0.072 Uiso 1 1 calc R . . H29B H 0.3557 0.4379 0.0726 0.072 Uiso 1 1 calc R . . H29C H 0.4267 0.3154 0.0690 0.072 Uiso 1 1 calc R . . C30 C 0.4321(5) 0.5126(5) 0.1419(3) 0.0441(14) Uani 1 1 d . . . H30A H 0.4454 0.5681 0.1501 0.066 Uiso 1 1 calc R . . H30B H 0.4254 0.4655 0.1793 0.066 Uiso 1 1 calc R . . H30C H 0.3649 0.5448 0.1234 0.066 Uiso 1 1 calc R . . C31 C 0.8003(4) 0.6044(4) 0.0114(2) 0.0297(11) Uani 1 1 d . . . C32 C 0.8648(4) 0.5703(5) -0.0398(2) 0.0348(12) Uani 1 1 d . . . C33 C 0.8777(4) 0.4697(5) -0.0368(2) 0.0329(11) Uani 1 1 d . . . C34 C 0.9388(6) 0.3967(6) -0.0796(3) 0.0528(16) Uani 1 1 d . . . H34A H 0.9840 0.3268 -0.0582 0.079 Uiso 1 1 calc R . . H34B H 0.9851 0.4238 -0.1091 0.079 Uiso 1 1 calc R . . H34C H 0.8879 0.3912 -0.0996 0.079 Uiso 1 1 calc R . . C35 C 0.9143(5) 0.6311(6) -0.0884(3) 0.0509(16) Uani 1 1 d . . . H35A H 0.9356 0.6008 -0.1246 0.076 Uiso 1 1 calc R . . H35B H 0.9783 0.6269 -0.0756 0.076 Uiso 1 1 calc R . . H35C H 0.8612 0.7052 -0.0966 0.076 Uiso 1 1 calc R . . C36 C 0.7634(6) 0.7084(5) 0.0283(2) 0.0447(15) Uani 1 1 d . . . H36A H 0.6884 0.7324 0.0471 0.067 Uiso 1 1 calc R . . H36B H 0.7677 0.7598 -0.0074 0.067 Uiso 1 1 calc R . . H36C H 0.8099 0.7015 0.0564 0.067 Uiso 1 1 calc R . . C37 C 0.8940(4) 0.3106(4) 0.18444(19) 0.0249(10) Uani 1 1 d . . . C38 C 0.9690(4) 0.2131(4) 0.1714(2) 0.0286(10) Uani 1 1 d . . . C39 C 0.9452(4) 0.2076(4) 0.1179(2) 0.0306(11) Uani 1 1 d . . . C40 C 1.0024(5) 0.1207(5) 0.0827(3) 0.0452(14) Uani 1 1 d . . . H40A H 0.9493 0.1128 0.0658 0.068 Uiso 1 1 calc R . . H40B H 1.0431 0.0545 0.1087 0.068 Uiso 1 1 calc R . . H40C H 1.0525 0.1376 0.0505 0.068 Uiso 1 1 calc R . . C41 C 1.0622(4) 0.1316(4) 0.2048(2) 0.0341(11) Uani 1 1 d . . . H41A H 1.0447 0.1380 0.2469 0.051 Uiso 1 1 calc R . . H41B H 1.1271 0.1427 0.1883 0.051 Uiso 1 1 calc R . . H41C H 1.0756 0.0610 0.2010 0.051 Uiso 1 1 calc R . . C42 C 0.8886(4) 0.3561(4) 0.23603(19) 0.0274(10) Uani 1 1 d . . . H42A H 0.8129 0.3907 0.2530 0.041 Uiso 1 1 calc R . . H42B H 0.9184 0.4079 0.2226 0.041 Uiso 1 1 calc R . . H42C H 0.9308 0.2995 0.2663 0.041 Uiso 1 1 calc R . . C43 C 1.1555(5) 0.7847(4) 0.4128(3) 0.0416(13) Uani 1 1 d . . . H43A H 1.1056 0.8389 0.4372 0.050 Uiso 1 1 calc R . . H43B H 1.1751 0.8213 0.3736 0.050 Uiso 1 1 calc R . . C44 C 1.2566(4) 0.7124(4) 0.4431(2) 0.0295(10) Uani 1 1 d . . . H44A H 1.2998 0.7509 0.4412 0.035 Uiso 1 1 calc R . . H44B H 1.2367 0.6877 0.4854 0.035 Uiso 1 1 calc R . . C45 C 1.4410(4) 0.4322(4) 0.4293(2) 0.0353(12) Uani 1 1 d . . . H45A H 1.4842 0.4329 0.3898 0.042 Uiso 1 1 calc R . . H45B H 1.4877 0.3736 0.4579 0.042 Uiso 1 1 calc R . . C46 C 1.4031(4) 0.5350(4) 0.4491(2) 0.0325(11) Uani 1 1 d . . . H46A H 1.3722 0.5291 0.4914 0.039 Uiso 1 1 calc R . . H46B H 1.4655 0.5508 0.4457 0.039 Uiso 1 1 calc R . . C47 C 1.3182(5) 0.6552(5) 0.3024(2) 0.0341(12) Uani 1 1 d . . . H47A H 1.2641 0.7293 0.2919 0.041 Uiso 1 1 calc R . . H47B H 1.3723 0.6371 0.2671 0.041 Uiso 1 1 calc R . . C48 C 1.3735(5) 0.6470(5) 0.3520(2) 0.0455(15) Uani 1 1 d . . . H48A H 1.3771 0.7146 0.3483 0.055 Uiso 1 1 calc R . . H48B H 1.4488 0.5913 0.3480 0.055 Uiso 1 1 calc R . . C49 C 0.7144(4) 0.9050(4) 0.2805(2) 0.0342(11) Uani 1 1 d . . . H49A H 0.7753 0.9186 0.2565 0.041 Uiso 1 1 calc R . . H49B H 0.6822 0.9504 0.3111 0.041 Uiso 1 1 calc R . . C50 C 0.6300(4) 0.9313(4) 0.2408(2) 0.0317(11) Uani 1 1 d . . . H50A H 0.5607 0.9403 0.2658 0.038 Uiso 1 1 calc R . . H50B H 0.6181 0.9993 0.2136 0.038 Uiso 1 1 calc R . . C51 C 0.8363(5) 0.8418(4) 0.1514(2) 0.0394(13) Uani 1 1 d . . . H51A H 0.8786 0.8379 0.1115 0.047 Uiso 1 1 calc R . . H51B H 0.8369 0.8989 0.1665 0.047 Uiso 1 1 calc R . . C52 C 0.7213(4) 0.8670(4) 0.1462(2) 0.0336(11) Uani 1 1 d . . . H52A H 0.6837 0.9418 0.1270 0.040 Uiso 1 1 calc R . . H52B H 0.7218 0.8224 0.1205 0.040 Uiso 1 1 calc R . . C53 C 0.5270(4) 0.7830(4) 0.2574(2) 0.0293(10) Uani 1 1 d . . . H53A H 0.4908 0.8333 0.2854 0.035 Uiso 1 1 calc R . . H53B H 0.4736 0.7617 0.2507 0.035 Uiso 1 1 calc R . . C54 C 0.5655(4) 0.8365(4) 0.1988(2) 0.0282(10) Uani 1 1 d . . . H54A H 0.5842 0.7938 0.1678 0.034 Uiso 1 1 calc R . . H54B H 0.5064 0.9068 0.1863 0.034 Uiso 1 1 calc R . . N27 N 0.5091(8) 1.1481(8) 0.3191(6) 0.127(4) Uani 1 1 d . . . C55 C 0.4588(9) 1.1343(8) 0.3658(5) 0.103(4) Uani 1 1 d . . . C56 C 0.3927(12) 1.1287(13) 0.4118(7) 0.178(8) Uani 1 1 d . . . H56A H 0.4332 1.0834 0.4456 0.267 Uiso 1 1 calc R . . H56B H 0.3479 1.0988 0.4044 0.267 Uiso 1 1 calc R . . H56C H 0.3461 1.1995 0.4210 0.267 Uiso 1 1 calc R . . N28 N 0.7263(15) 0.1084(9) 0.1230(5) 0.185(7) Uani 1 1 d . . . C57 C 0.7165(12) 0.1489(9) 0.1636(5) 0.110(4) Uani 1 1 d . . . C58 C 0.7054(8) 0.1940(7) 0.2096(5) 0.089(3) Uani 1 1 d . . . H58A H 0.7736 0.1594 0.2273 0.133 Uiso 1 1 calc R . . H58B H 0.6476 0.1863 0.2396 0.133 Uiso 1 1 calc R . . H58C H 0.6869 0.2692 0.1954 0.133 Uiso 1 1 calc R . . Cl1 Cl 0.53390(10) 0.78563(11) 0.43448(5) 0.0331(3) Uani 1 1 d . . . Cl2 Cl 1.03242(14) 0.85213(12) 0.24662(8) 0.0519(4) Uani 1 1 d . . . O1 O 0.5234(4) 0.8756(4) 0.3869(2) 0.0668(14) Uani 1 1 d . . . O2 O 0.6437(4) 0.7249(5) 0.4393(3) 0.089(2) Uani 1 1 d . . . O3 O 0.4821(6) 0.8194(5) 0.4890(2) 0.111(3) Uani 1 1 d . . . O4 O 0.4914(8) 0.7289(8) 0.4207(3) 0.150(4) Uani 1 1 d . . . O5 O 1.0983(4) 0.8751(4) 0.2733(2) 0.0563(12) Uani 1 1 d . . . O6 O 0.9530(5) 0.9406(5) 0.2183(3) 0.100(2) Uani 1 1 d . . . O7 O 0.9875(9) 0.7975(8) 0.2900(5) 0.205(7) Uani 1 1 d . . . O8 O 1.0946(8) 0.7854(12) 0.2076(7) 0.270(10) Uani 1 1 d . . . O9 O 0.4392(4) 0.3750(4) 0.2954(2) 0.0527(11) Uani 1 1 d D . . H9W1 H 0.468(5) 0.340(4) 0.2602(15) 0.063 Uiso 1 1 d D . . H9W2 H 0.437(6) 0.311(3) 0.3249(19) 0.063 Uiso 1 1 d D . . O10 O 0.3137(11) 0.8800(11) 0.1670(7) 0.074(4) Uani 0.50 1 d P A 1 O101 O 0.332(2) 0.9072(16) 0.1039(10) 0.077(7) Uani 0.25 1 d P B 2 O102 O 0.271(2) 0.875(2) 0.1440(15) 0.091(9) Uani 0.25 1 d P B 2 O11 O 0.3286(13) 1.0711(9) 0.1113(6) 0.116(6) Uani 0.50 1 d P . . O12 O 1.0541(16) 0.8719(14) 0.0631(7) 0.135(6) Uani 0.50 1 d P . . O13 O 0.8531(17) 0.0152(15) 0.0271(9) 0.153(7) Uani 0.50 1 d P . . O14 O 0.699(3) -0.0252(18) -0.0036(12) 0.104(10) Uani 0.25 1 d P . . O15 O 0.493(2) 1.093(2) 0.0813(14) 0.117(11) Uani 0.25 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 0.0103(3) 0.0155(3) 0.0172(3) -0.0031(2) -0.0015(2) -0.0075(2) Fe2 0.0230(3) 0.0307(4) 0.0201(3) -0.0022(2) -0.0036(2) -0.0180(3) Ni1 0.0130(3) 0.0202(3) 0.0198(3) -0.0026(2) -0.00107(19) -0.0117(2) Ni2 0.0173(3) 0.0191(3) 0.0197(3) -0.0006(2) -0.0033(2) -0.0107(2) B1 0.016(2) 0.019(2) 0.025(2) -0.0064(18) -0.0062(18) -0.0063(19) B2 0.039(3) 0.037(3) 0.026(3) -0.009(2) -0.005(2) -0.022(3) N1 0.0181(18) 0.0202(18) 0.0218(17) -0.0023(14) -0.0043(14) -0.0103(15) N2 0.0150(18) 0.0215(18) 0.0225(17) -0.0030(14) -0.0017(14) -0.0108(15) N3 0.0126(17) 0.0222(18) 0.0232(18) -0.0031(14) -0.0030(14) -0.0109(14) N4 0.022(2) 0.0240(19) 0.0204(17) 0.0010(14) -0.0047(14) -0.0130(16) N5 0.024(2) 0.049(3) 0.029(2) -0.0042(19) 0.0018(17) -0.016(2) N6 0.049(3) 0.041(3) 0.074(4) -0.015(3) -0.032(3) -0.012(3) N7 0.0153(17) 0.0162(17) 0.0230(17) -0.0042(13) -0.0029(13) -0.0081(14) N8 0.0145(17) 0.0201(17) 0.0176(16) -0.0033(13) -0.0018(13) -0.0100(14) N9 0.0140(17) 0.0210(18) 0.0238(18) -0.0076(14) -0.0025(14) -0.0059(14) N10 0.0143(18) 0.0220(18) 0.0219(17) -0.0051(14) -0.0008(13) -0.0088(14) N11 0.0145(17) 0.0149(17) 0.0239(18) -0.0048(13) -0.0052(14) -0.0044(14) N12 0.0139(17) 0.0144(16) 0.0229(17) -0.0045(13) -0.0016(13) -0.0071(14) N13 0.035(2) 0.036(2) 0.029(2) -0.0036(17) -0.0098(17) -0.0241(19) N14 0.029(2) 0.040(2) 0.0254(19) 0.0010(17) -0.0086(16) -0.0236(19) N15 0.027(2) 0.041(2) 0.0194(18) -0.0062(16) -0.0019(15) -0.0185(18) N16 0.032(2) 0.035(2) 0.0175(17) 0.0004(15) -0.0039(15) -0.0228(18) N17 0.030(2) 0.035(2) 0.0254(19) -0.0088(17) -0.0042(16) -0.0185(19) N18 0.026(2) 0.027(2) 0.0191(17) -0.0050(14) -0.0011(14) -0.0159(17) N19 0.021(2) 0.024(2) 0.036(2) 0.0001(16) -0.0054(16) -0.0113(16) N20 0.0151(18) 0.031(2) 0.033(2) -0.0125(17) 0.0007(15) -0.0088(16) N21 0.030(2) 0.034(2) 0.0217(18) -0.0018(16) -0.0035(16) -0.0227(18) N22 0.022(2) 0.032(2) 0.0205(17) -0.0069(15) 0.0017(14) -0.0204(17) N23 0.022(2) 0.0243(19) 0.0259(19) -0.0049(15) -0.0044(15) -0.0100(16) N24 0.026(2) 0.033(2) 0.033(2) -0.0086(17) 0.0035(16) -0.0205(18) N25 0.023(2) 0.0214(18) 0.0258(19) -0.0009(15) -0.0051(15) -0.0129(16) N26 0.027(2) 0.0231(19) 0.0249(19) 0.0021(15) -0.0069(15) -0.0157(16) C1 0.016(2) 0.023(2) 0.021(2) -0.0068(17) 0.0011(16) -0.0149(17) C2 0.0118(19) 0.0150(19) 0.0176(19) -0.0018(15) -0.0001(15) -0.0036(16) C3 0.014(2) 0.0151(19) 0.022(2) -0.0004(15) -0.0068(16) -0.0098(16) C4 0.021(2) 0.023(2) 0.019(2) -0.0003(16) -0.0034(16) -0.0110(18) C5 0.023(2) 0.034(3) 0.031(2) -0.002(2) -0.0067(19) -0.017(2) C6 0.033(3) 0.037(3) 0.032(3) -0.009(2) -0.012(2) -0.017(2) C7 0.014(2) 0.021(2) 0.0170(18) -0.0019(15) -0.0013(15) -0.0103(16) C8 0.017(2) 0.024(2) 0.020(2) -0.0014(16) -0.0021(16) -0.0134(17) C9 0.018(2) 0.022(2) 0.024(2) -0.0017(16) -0.0060(16) -0.0116(17) C10 0.028(3) 0.023(2) 0.044(3) -0.007(2) -0.011(2) -0.013(2) C11 0.020(2) 0.025(2) 0.043(3) -0.006(2) -0.005(2) -0.0121(19) C12 0.012(2) 0.021(2) 0.024(2) -0.0058(16) -0.0021(16) -0.0076(17) C13 0.021(2) 0.039(3) 0.020(2) -0.0035(18) 0.0014(17) -0.019(2) C14 0.024(3) 0.045(3) 0.029(2) -0.012(2) 0.0077(19) -0.016(2) C15 0.017(2) 0.039(3) 0.030(2) -0.016(2) 0.0023(18) -0.008(2) C16 0.024(3) 0.040(3) 0.041(3) -0.017(2) 0.004(2) -0.003(2) C17 0.053(4) 0.061(4) 0.048(4) -0.023(3) 0.025(3) -0.034(3) C18 0.039(3) 0.036(3) 0.026(2) -0.004(2) 0.004(2) -0.026(2) C19 0.0114(19) 0.021(2) 0.021(2) -0.0035(16) -0.0022(15) -0.0095(16) C20 0.018(2) 0.019(2) 0.028(2) -0.0037(17) -0.0073(17) -0.0077(17) C21 0.019(2) 0.017(2) 0.029(2) -0.0001(17) -0.0096(17) -0.0072(17) C22 0.043(3) 0.018(2) 0.042(3) -0.003(2) -0.021(2) -0.009(2) C23 0.038(3) 0.024(2) 0.038(3) 0.000(2) -0.022(2) -0.014(2) C24 0.020(2) 0.022(2) 0.023(2) -0.0025(17) -0.0072(17) -0.0115(18) C25 0.032(3) 0.048(3) 0.033(3) 0.009(2) -0.011(2) -0.031(2) C26 0.043(3) 0.049(3) 0.034(3) 0.009(2) -0.018(2) -0.035(3) C27 0.052(3) 0.045(3) 0.027(2) 0.002(2) -0.019(2) -0.036(3) C28 0.074(5) 0.065(4) 0.045(3) -0.005(3) -0.024(3) -0.049(4) C29 0.056(4) 0.074(4) 0.041(3) 0.008(3) -0.019(3) -0.053(4) C30 0.031(3) 0.065(4) 0.047(3) -0.003(3) -0.009(2) -0.030(3) C31 0.032(3) 0.042(3) 0.023(2) 0.002(2) -0.0072(19) -0.025(2) C32 0.033(3) 0.059(4) 0.022(2) -0.001(2) -0.003(2) -0.031(3) C33 0.028(3) 0.054(3) 0.022(2) -0.006(2) -0.0023(19) -0.023(2) C34 0.051(4) 0.069(4) 0.033(3) -0.010(3) 0.005(3) -0.025(3) C35 0.049(4) 0.080(5) 0.035(3) 0.003(3) 0.000(3) -0.046(4) C36 0.071(4) 0.047(3) 0.031(3) 0.005(2) -0.009(3) -0.043(3) C37 0.029(3) 0.033(3) 0.022(2) 0.0000(18) -0.0032(18) -0.023(2) C38 0.032(3) 0.030(3) 0.028(2) -0.0029(19) -0.0030(19) -0.018(2) C39 0.032(3) 0.033(3) 0.032(2) -0.008(2) -0.002(2) -0.018(2) C40 0.050(4) 0.043(3) 0.041(3) -0.015(3) -0.014(3) -0.011(3) C41 0.034(3) 0.037(3) 0.033(3) -0.008(2) -0.007(2) -0.015(2) C42 0.028(3) 0.037(3) 0.019(2) -0.0016(19) -0.0031(18) -0.017(2) C43 0.045(3) 0.023(3) 0.063(4) -0.007(2) -0.015(3) -0.016(2) C44 0.032(3) 0.025(2) 0.042(3) -0.007(2) -0.007(2) -0.019(2) C45 0.018(2) 0.044(3) 0.044(3) -0.007(2) -0.005(2) -0.014(2) C46 0.020(2) 0.049(3) 0.038(3) -0.015(2) -0.003(2) -0.018(2) C47 0.038(3) 0.053(3) 0.025(2) -0.002(2) 0.002(2) -0.036(3) C48 0.057(4) 0.075(4) 0.031(3) -0.003(3) 0.006(2) -0.058(4) C49 0.035(3) 0.028(3) 0.043(3) -0.009(2) -0.008(2) -0.014(2) C50 0.036(3) 0.023(2) 0.038(3) -0.003(2) -0.011(2) -0.013(2) C51 0.047(3) 0.039(3) 0.036(3) -0.002(2) 0.008(2) -0.030(3) C52 0.042(3) 0.030(3) 0.028(2) 0.002(2) -0.002(2) -0.020(2) C53 0.018(2) 0.030(3) 0.038(3) 0.002(2) -0.0086(19) -0.010(2) C54 0.026(2) 0.026(2) 0.033(2) -0.0007(19) -0.013(2) -0.010(2) N27 0.086(7) 0.103(7) 0.187(11) -0.031(7) 0.026(7) -0.052(6) C55 0.075(7) 0.080(6) 0.115(8) -0.003(6) 0.030(6) -0.026(5) C56 0.131(12) 0.247(18) 0.245(18) -0.185(16) 0.100(12) -0.136(13) N28 0.38(2) 0.111(8) 0.119(9) 0.039(7) -0.106(12) -0.155(12) C57 0.179(12) 0.085(7) 0.099(8) 0.030(6) -0.057(8) -0.091(8) C58 0.097(7) 0.078(6) 0.113(8) -0.035(6) 0.020(6) -0.060(6) Cl1 0.0209(6) 0.0498(7) 0.0298(6) -0.0081(5) -0.0014(4) -0.0166(5) Cl2 0.0511(9) 0.0424(8) 0.0685(10) -0.0080(7) -0.0325(8) -0.0157(7) O1 0.061(3) 0.062(3) 0.045(3) 0.008(2) -0.007(2) -0.009(2) O2 0.030(3) 0.100(4) 0.094(4) 0.037(3) -0.007(2) -0.020(3) O3 0.105(5) 0.101(5) 0.038(3) -0.011(3) 0.012(3) 0.018(4) O4 0.248(10) 0.277(11) 0.070(4) -0.018(5) -0.010(5) -0.244(10) O5 0.064(3) 0.050(3) 0.071(3) -0.009(2) -0.023(2) -0.032(2) O6 0.071(4) 0.086(4) 0.135(5) 0.063(4) -0.062(4) -0.050(3) O7 0.241(11) 0.216(9) 0.242(10) 0.188(9) -0.215(10) -0.205(9) O8 0.114(8) 0.348(17) 0.352(18) -0.296(16) -0.095(10) 0.043(10) O9 0.047(3) 0.059(3) 0.047(2) -0.010(2) 0.005(2) -0.024(2) O10 0.050(8) 0.065(7) 0.110(11) -0.028(7) -0.014(7) -0.022(6) O101 0.097(18) 0.047(12) 0.060(13) -0.006(10) -0.009(12) -0.014(12) O102 0.045(15) 0.056(15) 0.11(2) -0.022(15) 0.016(15) 0.017(12) O11 0.153(14) 0.053(7) 0.085(9) -0.011(6) 0.040(9) -0.022(8) O12 0.157(17) 0.148(15) 0.112(12) -0.036(11) 0.000(11) -0.076(13) O13 0.152(17) 0.143(16) 0.146(16) 0.017(12) -0.009(13) -0.075(13) O14 0.17(3) 0.054(14) 0.098(19) -0.007(13) -0.047(19) -0.041(16) O15 0.068(17) 0.070(16) 0.15(3) 0.029(16) -0.015(16) 0.000(13) _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 C2 1.920(4) . ? Fe1 C1 1.921(4) . ? Fe1 C3 1.935(4) . ? Fe1 N10 1.979(4) . ? Fe1 N8 2.001(3) . ? Fe1 N12 2.019(3) . ? Fe2 C4 1.921(4) . ? Fe2 C6 1.924(5) . ? Fe2 C5 1.932(5) . ? Fe2 N18 1.982(4) . ? Fe2 N16 1.997(4) . ? Fe2 N14 2.007(4) . ? Ni1 N2 2.038(4) . ? Ni1 N21 2.089(4) . ? Ni1 N22 2.093(4) . ? Ni1 N20 2.105(4) . ? Ni1 N3 2.131(4) 2_766 ? Ni1 N19 2.133(4) . ? Ni2 N1 2.050(4) . ? Ni2 N23 2.091(4) . ? Ni2 N26 2.097(4) . ? Ni2 N24 2.119(4) . ? Ni2 N4 2.126(4) . ? Ni2 N25 2.130(4) . ? B1 N11 1.529(6) . ? B1 N7 1.536(6) . ? B1 N9 1.547(6) . ? B1 H1 1.0000 . ? B2 N13 1.525(7) . ? B2 N15 1.530(7) . ? B2 N17 1.536(7) . ? B2 H2 1.0000 . ? N1 C1 1.152(5) . ? N2 C2 1.151(5) . ? N3 C3 1.157(5) . ? N3 Ni1 2.131(4) 2_766 ? N4 C4 1.153(6) . ? N5 C5 1.148(6) . ? N6 C6 1.152(7) . ? N7 C9 1.357(5) . ? N7 N8 1.360(5) . ? N8 C7 1.348(5) . ? N9 C15 1.353(6) . ? N9 N10 1.373(5) . ? N10 C13 1.341(5) . ? N11 C21 1.351(5) . ? N11 N12 1.364(5) . ? N12 C19 1.347(5) . ? N13 C27 1.352(6) . ? N13 N14 1.362(6) . ? N14 C25 1.352(6) . ? N15 C33 1.358(6) . ? N15 N16 1.363(6) . ? N16 C31 1.354(6) . ? N17 C39 1.351(7) . ? N17 N18 1.376(5) . ? N18 C37 1.349(6) . ? N19 C43 1.482(6) . ? N19 H19A 0.9200 . ? N19 H19B 0.9200 . ? N20 C45 1.468(6) . ? N20 H20A 0.9200 . ? N20 H20B 0.9200 . ? N21 C47 1.461(6) . ? N21 H21A 0.9200 . ? N21 H21B 0.9200 . ? N22 C44 1.462(6) . ? N22 C46 1.480(6) . ? N22 C48 1.494(6) . ? N23 C49 1.481(6) . ? N23 H23A 0.9200 . ? N23 H23E 0.9200 . ? N24 C51 1.492(7) . ? N24 H24A 0.9200 . ? N24 H24E 0.9200 . ? N25 C53 1.483(6) . ? N25 H25A 0.9200 . ? N25 H25B 0.9200 . ? N26 C52 1.476(6) . ? N26 C54 1.479(6) . ? N26 C50 1.487(6) . ? C7 C8 1.399(6) . ? C7 C12 1.485(6) . ? C8 C9 1.383(6) . ? C8 C11 1.496(6) . ? C9 C10 1.488(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.414(7) . ? C13 C18 1.485(7) . ? C14 C15 1.374(7) . ? C14 C17 1.502(7) . ? C15 C16 1.486(7) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.402(6) . ? C19 C24 1.498(6) . ? C20 C21 1.388(6) . ? C20 C23 1.501(6) . ? C21 C22 1.490(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C23 H23D 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C24 H24D 0.9800 . ? C25 C26 1.402(8) . ? C25 C30 1.492(8) . ? C26 C27 1.379(8) . ? C26 C29 1.510(7) . ? C27 C28 1.476(8) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.386(7) . ? C31 C36 1.485(8) . ? C32 C33 1.374(8) . ? C32 C35 1.508(7) . ? C33 C34 1.480(8) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.380(7) . ? C37 C42 1.493(6) . ? C38 C39 1.396(7) . ? C38 C41 1.500(7) . ? C39 C40 1.491(7) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.512(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.499(7) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.486(7) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.514(7) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.507(8) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.516(7) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? N27 C55 1.191(13) . ? C55 C56 1.273(15) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? N28 C57 1.195(15) . ? C57 C58 1.346(14) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? Cl1 O4 1.352(6) . ? Cl1 O2 1.388(5) . ? Cl1 O3 1.408(5) . ? Cl1 O1 1.455(5) . ? Cl2 O7 1.355(8) . ? Cl2 O8 1.363(9) . ? Cl2 O6 1.372(5) . ? Cl2 O5 1.417(4) . ? O9 H9W1 0.994(19) . ? O9 H9W2 1.019(19) . ? O101 O102 1.28(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe1 C1 86.12(16) . . ? C2 Fe1 C3 89.19(16) . . ? C1 Fe1 C3 90.85(17) . . ? C2 Fe1 N10 91.85(16) . . ? C1 Fe1 N10 92.50(16) . . ? C3 Fe1 N10 176.55(16) . . ? C2 Fe1 N8 177.57(16) . . ? C1 Fe1 N8 92.20(15) . . ? C3 Fe1 N8 89.08(15) . . ? N10 Fe1 N8 89.97(14) . . ? C2 Fe1 N12 91.59(15) . . ? C1 Fe1 N12 177.30(15) . . ? C3 Fe1 N12 87.69(15) . . ? N10 Fe1 N12 89.00(14) . . ? N8 Fe1 N12 90.04(14) . . ? C4 Fe2 C6 85.16(19) . . ? C4 Fe2 C5 84.25(19) . . ? C6 Fe2 C5 87.8(2) . . ? C4 Fe2 N18 93.96(17) . . ? C6 Fe2 N18 179.10(18) . . ? C5 Fe2 N18 91.95(18) . . ? C4 Fe2 N16 94.27(17) . . ? C6 Fe2 N16 92.0(2) . . ? C5 Fe2 N16 178.52(18) . . ? N18 Fe2 N16 88.23(16) . . ? C4 Fe2 N14 174.08(19) . . ? C6 Fe2 N14 90.59(19) . . ? C5 Fe2 N14 91.48(18) . . ? N18 Fe2 N14 90.28(16) . . ? N16 Fe2 N14 89.99(16) . . ? N2 Ni1 N21 92.19(14) . . ? N2 Ni1 N22 175.25(14) . . ? N21 Ni1 N22 83.57(14) . . ? N2 Ni1 N20 94.92(15) . . ? N21 Ni1 N20 94.23(16) . . ? N22 Ni1 N20 83.30(15) . . ? N2 Ni1 N3 89.91(13) . 2_766 ? N21 Ni1 N3 176.47(15) . 2_766 ? N22 Ni1 N3 94.44(13) . 2_766 ? N20 Ni1 N3 88.41(14) . 2_766 ? N2 Ni1 N19 100.80(15) . . ? N21 Ni1 N19 92.86(16) . . ? N22 Ni1 N19 81.61(15) . . ? N20 Ni1 N19 162.48(15) . . ? N3 Ni1 N19 83.96(15) 2_766 . ? N1 Ni2 N23 90.15(14) . . ? N1 Ni2 N26 173.40(15) . . ? N23 Ni2 N26 83.66(15) . . ? N1 Ni2 N24 99.18(15) . . ? N23 Ni2 N24 91.78(16) . . ? N26 Ni2 N24 83.33(16) . . ? N1 Ni2 N4 92.45(14) . . ? N23 Ni2 N4 176.69(14) . . ? N26 Ni2 N4 93.82(14) . . ? N24 Ni2 N4 85.79(15) . . ? N1 Ni2 N25 95.78(14) . . ? N23 Ni2 N25 96.86(15) . . ? N26 Ni2 N25 82.75(14) . . ? N24 Ni2 N25 162.69(15) . . ? N4 Ni2 N25 84.92(14) . . ? N11 B1 N7 108.2(3) . . ? N11 B1 N9 106.7(3) . . ? N7 B1 N9 107.8(3) . . ? N11 B1 H1 111.3 . . ? N7 B1 H1 111.3 . . ? N9 B1 H1 111.3 . . ? N13 B2 N15 107.9(4) . . ? N13 B2 N17 108.7(4) . . ? N15 B2 N17 106.7(4) . . ? N13 B2 H2 111.1 . . ? N15 B2 H2 111.1 . . ? N17 B2 H2 111.1 . . ? C1 N1 Ni2 175.1(4) . . ? C2 N2 Ni1 170.7(3) . . ? C3 N3 Ni1 158.4(3) . 2_766 ? C4 N4 Ni2 158.6(4) . . ? C9 N7 N8 109.9(3) . . ? C9 N7 B1 130.9(4) . . ? N8 N7 B1 119.2(3) . . ? C7 N8 N7 107.2(3) . . ? C7 N8 Fe1 135.1(3) . . ? N7 N8 Fe1 117.5(3) . . ? C15 N9 N10 109.8(4) . . ? C15 N9 B1 130.1(4) . . ? N10 N9 B1 120.0(3) . . ? C13 N10 N9 107.3(3) . . ? C13 N10 Fe1 135.6(3) . . ? N9 N10 Fe1 116.5(3) . . ? C21 N11 N12 110.1(3) . . ? C21 N11 B1 130.5(4) . . ? N12 N11 B1 118.8(3) . . ? C19 N12 N11 106.9(3) . . ? C19 N12 Fe1 135.9(3) . . ? N11 N12 Fe1 117.2(2) . . ? C27 N13 N14 110.0(4) . . ? C27 N13 B2 131.1(5) . . ? N14 N13 B2 118.8(4) . . ? C25 N14 N13 106.9(4) . . ? C25 N14 Fe2 135.1(4) . . ? N13 N14 Fe2 117.4(3) . . ? C33 N15 N16 109.6(4) . . ? C33 N15 B2 130.8(4) . . ? N16 N15 B2 119.6(4) . . ? C31 N16 N15 107.1(4) . . ? C31 N16 Fe2 135.5(3) . . ? N15 N16 Fe2 117.0(3) . . ? C39 N17 N18 109.6(4) . . ? C39 N17 B2 130.6(4) . . ? N18 N17 B2 118.9(4) . . ? C37 N18 N17 106.6(4) . . ? C37 N18 Fe2 136.2(3) . . ? N17 N18 Fe2 117.2(3) . . ? C43 N19 Ni1 109.3(3) . . ? C43 N19 H19A 109.8 . . ? Ni1 N19 H19A 109.8 . . ? C43 N19 H19B 109.8 . . ? Ni1 N19 H19B 109.8 . . ? H19A N19 H19B 108.3 . . ? C45 N20 Ni1 109.7(3) . . ? C45 N20 H20A 109.7 . . ? Ni1 N20 H20A 109.7 . . ? C45 N20 H20B 109.7 . . ? Ni1 N20 H20B 109.7 . . ? H20A N20 H20B 108.2 . . ? C47 N21 Ni1 110.2(3) . . ? C47 N21 H21A 109.6 . . ? Ni1 N21 H21A 109.6 . . ? C47 N21 H21B 109.6 . . ? Ni1 N21 H21B 109.6 . . ? H21A N21 H21B 108.1 . . ? C44 N22 C46 111.3(4) . . ? C44 N22 C48 114.8(4) . . ? C46 N22 C48 109.1(4) . . ? C44 N22 Ni1 106.2(3) . . ? C46 N22 Ni1 105.0(3) . . ? C48 N22 Ni1 110.1(3) . . ? C49 N23 Ni2 109.1(3) . . ? C49 N23 H23A 109.9 . . ? Ni2 N23 H23A 109.9 . . ? C49 N23 H23E 109.9 . . ? Ni2 N23 H23E 109.9 . . ? H23A N23 H23E 108.3 . . ? C51 N24 Ni2 109.6(3) . . ? C51 N24 H24A 109.7 . . ? Ni2 N24 H24A 109.7 . . ? C51 N24 H24E 109.7 . . ? Ni2 N24 H24E 109.7 . . ? H24A N24 H24E 108.2 . . ? C53 N25 Ni2 109.7(3) . . ? C53 N25 H25A 109.7 . . ? Ni2 N25 H25A 109.7 . . ? C53 N25 H25B 109.7 . . ? Ni2 N25 H25B 109.7 . . ? H25A N25 H25B 108.2 . . ? C52 N26 C54 111.4(4) . . ? C52 N26 C50 113.4(4) . . ? C54 N26 C50 110.7(4) . . ? C52 N26 Ni2 105.8(3) . . ? C54 N26 Ni2 106.1(3) . . ? C50 N26 Ni2 109.1(3) . . ? N1 C1 Fe1 179.4(4) . . ? N2 C2 Fe1 179.3(4) . . ? N3 C3 Fe1 172.3(4) . . ? N4 C4 Fe2 172.1(4) . . ? N5 C5 Fe2 177.5(5) . . ? N6 C6 Fe2 178.0(5) . . ? N8 C7 C8 109.3(4) . . ? N8 C7 C12 125.2(4) . . ? C8 C7 C12 125.5(4) . . ? C9 C8 C7 105.9(4) . . ? C9 C8 C11 127.8(4) . . ? C7 C8 C11 126.3(4) . . ? N7 C9 C8 107.7(4) . . ? N7 C9 C10 123.0(4) . . ? C8 C9 C10 129.3(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N10 C13 C14 108.6(4) . . ? N10 C13 C18 124.9(4) . . ? C14 C13 C18 126.4(4) . . ? C15 C14 C13 106.4(4) . . ? C15 C14 C17 128.1(5) . . ? C13 C14 C17 125.5(5) . . ? N9 C15 C14 107.8(4) . . ? N9 C15 C16 122.4(5) . . ? C14 C15 C16 129.8(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N12 C19 C20 109.7(4) . . ? N12 C19 C24 125.1(4) . . ? C20 C19 C24 125.2(4) . . ? C21 C20 C19 105.4(4) . . ? C21 C20 C23 128.2(4) . . ? C19 C20 C23 126.4(4) . . ? N11 C21 C20 107.9(4) . . ? N11 C21 C22 121.8(4) . . ? C20 C21 C22 130.3(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C23 H23D 109.5 . . ? H23B C23 H23D 109.5 . . ? H23C C23 H23D 109.5 . . ? C19 C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C19 C24 H24D 109.5 . . ? H24B C24 H24D 109.5 . . ? H24C C24 H24D 109.5 . . ? N14 C25 C26 109.2(5) . . ? N14 C25 C30 125.1(5) . . ? C26 C25 C30 125.7(5) . . ? C27 C26 C25 105.9(4) . . ? C27 C26 C29 126.9(5) . . ? C25 C26 C29 127.2(6) . . ? N13 C27 C26 108.0(5) . . ? N13 C27 C28 122.3(5) . . ? C26 C27 C28 129.6(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N16 C31 C32 108.9(5) . . ? N16 C31 C36 124.1(4) . . ? C32 C31 C36 127.0(5) . . ? C33 C32 C31 106.9(4) . . ? C33 C32 C35 126.9(5) . . ? C31 C32 C35 126.2(5) . . ? N15 C33 C32 107.5(4) . . ? N15 C33 C34 123.0(5) . . ? C32 C33 C34 129.6(5) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N18 C37 C38 110.2(4) . . ? N18 C37 C42 123.3(4) . . ? C38 C37 C42 126.5(4) . . ? C37 C38 C39 105.8(4) . . ? C37 C38 C41 127.9(4) . . ? C39 C38 C41 126.2(5) . . ? N17 C39 C38 107.8(4) . . ? N17 C39 C40 123.6(4) . . ? C38 C39 C40 128.6(5) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N19 C43 C44 111.1(4) . . ? N19 C43 H43A 109.4 . . ? C44 C43 H43A 109.4 . . ? N19 C43 H43B 109.4 . . ? C44 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? N22 C44 C43 108.7(4) . . ? N22 C44 H44A 110.0 . . ? C43 C44 H44A 110.0 . . ? N22 C44 H44B 110.0 . . ? C43 C44 H44B 110.0 . . ? H44A C44 H44B 108.3 . . ? N20 C45 C46 109.6(4) . . ? N20 C45 H45A 109.7 . . ? C46 C45 H45A 109.7 . . ? N20 C45 H45B 109.7 . . ? C46 C45 H45B 109.7 . . ? H45A C45 H45B 108.2 . . ? N22 C46 C45 111.1(4) . . ? N22 C46 H46A 109.4 . . ? C45 C46 H46A 109.4 . . ? N22 C46 H46B 109.4 . . ? C45 C46 H46B 109.4 . . ? H46A C46 H46B 108.0 . . ? N21 C47 C48 113.6(4) . . ? N21 C47 H47A 108.8 . . ? C48 C47 H47A 108.8 . . ? N21 C47 H47B 108.8 . . ? C48 C47 H47B 108.8 . . ? H47A C47 H47B 107.7 . . ? C47 C48 N22 114.4(4) . . ? C47 C48 H48A 108.7 . . ? N22 C48 H48A 108.7 . . ? C47 C48 H48B 108.7 . . ? N22 C48 H48B 108.7 . . ? H48A C48 H48B 107.6 . . ? N23 C49 C50 109.8(4) . . ? N23 C49 H49A 109.7 . . ? C50 C49 H49A 109.7 . . ? N23 C49 H49B 109.7 . . ? C50 C49 H49B 109.7 . . ? H49A C49 H49B 108.2 . . ? N26 C50 C49 113.0(4) . . ? N26 C50 H50A 109.0 . . ? C49 C50 H50A 109.0 . . ? N26 C50 H50B 109.0 . . ? C49 C50 H50B 109.0 . . ? H50A C50 H50B 107.8 . . ? N24 C51 C52 110.9(4) . . ? N24 C51 H51A 109.5 . . ? C52 C51 H51A 109.5 . . ? N24 C51 H51B 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 108.0 . . ? N26 C52 C51 111.9(4) . . ? N26 C52 H52A 109.2 . . ? C51 C52 H52A 109.2 . . ? N26 C52 H52B 109.2 . . ? C51 C52 H52B 109.2 . . ? H52A C52 H52B 107.9 . . ? N25 C53 C54 110.8(4) . . ? N25 C53 H53A 109.5 . . ? C54 C53 H53A 109.5 . . ? N25 C53 H53B 109.5 . . ? C54 C53 H53B 109.5 . . ? H53A C53 H53B 108.1 . . ? N26 C54 C53 110.7(4) . . ? N26 C54 H54A 109.5 . . ? C53 C54 H54A 109.5 . . ? N26 C54 H54B 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 108.1 . . ? N27 C55 C56 171.6(16) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N28 C57 C58 179.7(12) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O4 Cl1 O2 110.3(6) . . ? O4 Cl1 O3 110.5(5) . . ? O2 Cl1 O3 108.6(4) . . ? O4 Cl1 O1 109.7(4) . . ? O2 Cl1 O1 107.1(3) . . ? O3 Cl1 O1 110.6(4) . . ? O7 Cl2 O8 105.5(10) . . ? O7 Cl2 O6 110.2(5) . . ? O8 Cl2 O6 109.7(7) . . ? O7 Cl2 O5 107.6(4) . . ? O8 Cl2 O5 110.3(5) . . ? O6 Cl2 O5 113.3(3) . . ? H9W1 O9 H9W2 95(2) . . ? 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 N23 Ni2 N1 C1 34(4) . . . . ? N26 Ni2 N1 C1 13(5) . . . . ? N24 Ni2 N1 C1 125(4) . . . . ? N4 Ni2 N1 C1 -148(4) . . . . ? N25 Ni2 N1 C1 -63(4) . . . . ? N21 Ni1 N2 C2 108(2) . . . . ? N22 Ni1 N2 C2 81(3) . . . . ? N20 Ni1 N2 C2 13(2) . . . . ? N3 Ni1 N2 C2 -75(2) 2_766 . . . ? N19 Ni1 N2 C2 -159(2) . . . . ? N1 Ni2 N4 C4 91.5(9) . . . . ? N23 Ni2 N4 C4 -127(2) . . . . ? N26 Ni2 N4 C4 -86.5(9) . . . . ? N24 Ni2 N4 C4 -169.5(10) . . . . ? N25 Ni2 N4 C4 -4.1(9) . . . . ? N11 B1 N7 C9 -123.6(4) . . . . ? N9 B1 N7 C9 121.4(4) . . . . ? N11 B1 N7 N8 54.8(5) . . . . ? N9 B1 N7 N8 -60.3(4) . . . . ? C9 N7 N8 C7 0.1(4) . . . . ? B1 N7 N8 C7 -178.6(3) . . . . ? C9 N7 N8 Fe1 -175.5(3) . . . . ? B1 N7 N8 Fe1 5.8(4) . . . . ? C2 Fe1 N8 C7 7(4) . . . . ? C1 Fe1 N8 C7 -39.2(4) . . . . ? C3 Fe1 N8 C7 51.6(4) . . . . ? N10 Fe1 N8 C7 -131.7(4) . . . . ? N12 Fe1 N8 C7 139.3(4) . . . . ? C2 Fe1 N8 N7 -179(100) . . . . ? C1 Fe1 N8 N7 134.8(3) . . . . ? C3 Fe1 N8 N7 -134.4(3) . . . . ? N10 Fe1 N8 N7 42.3(3) . . . . ? N12 Fe1 N8 N7 -46.7(3) . . . . ? N11 B1 N9 C15 116.3(5) . . . . ? N7 B1 N9 C15 -127.7(4) . . . . ? N11 B1 N9 N10 -63.7(4) . . . . ? N7 B1 N9 N10 52.4(5) . . . . ? C15 N9 N10 C13 0.9(5) . . . . ? B1 N9 N10 C13 -179.2(4) . . . . ? C15 N9 N10 Fe1 -172.1(3) . . . . ? B1 N9 N10 Fe1 7.9(4) . . . . ? C2 Fe1 N10 C13 -37.6(4) . . . . ? C1 Fe1 N10 C13 48.6(4) . . . . ? C3 Fe1 N10 C13 -145(2) . . . . ? N8 Fe1 N10 C13 140.8(4) . . . . ? N12 Fe1 N10 C13 -129.2(4) . . . . ? C2 Fe1 N10 N9 132.7(3) . . . . ? C1 Fe1 N10 N9 -141.1(3) . . . . ? C3 Fe1 N10 N9 25(3) . . . . ? N8 Fe1 N10 N9 -48.9(3) . . . . ? N12 Fe1 N10 N9 41.1(3) . . . . ? N7 B1 N11 C21 125.8(5) . . . . ? N9 B1 N11 C21 -118.4(5) . . . . ? N7 B1 N11 N12 -63.6(5) . . . . ? N9 B1 N11 N12 52.2(5) . . . . ? C21 N11 N12 C19 0.5(5) . . . . ? B1 N11 N12 C19 -171.9(4) . . . . ? C21 N11 N12 Fe1 -178.7(3) . . . . ? B1 N11 N12 Fe1 8.9(5) . . . . ? C2 Fe1 N12 C19 38.3(4) . . . . ? C1 Fe1 N12 C19 6(4) . . . . ? C3 Fe1 N12 C19 -50.9(4) . . . . ? N10 Fe1 N12 C19 130.1(4) . . . . ? N8 Fe1 N12 C19 -139.9(4) . . . . ? C2 Fe1 N12 N11 -142.8(3) . . . . ? C1 Fe1 N12 N11 -175(3) . . . . ? C3 Fe1 N12 N11 128.1(3) . . . . ? N10 Fe1 N12 N11 -51.0(3) . . . . ? N8 Fe1 N12 N11 39.0(3) . . . . ? N15 B2 N13 C27 119.0(5) . . . . ? N17 B2 N13 C27 -125.6(5) . . . . ? N15 B2 N13 N14 -62.9(5) . . . . ? N17 B2 N13 N14 52.5(6) . . . . ? C27 N13 N14 C25 -0.5(5) . . . . ? B2 N13 N14 C25 -179.0(4) . . . . ? C27 N13 N14 Fe2 -173.6(3) . . . . ? B2 N13 N14 Fe2 7.9(5) . . . . ? C4 Fe2 N14 C25 5.3(19) . . . . ? C6 Fe2 N14 C25 -38.7(5) . . . . ? C5 Fe2 N14 C25 49.1(5) . . . . ? N18 Fe2 N14 C25 141.0(5) . . . . ? N16 Fe2 N14 C25 -130.8(5) . . . . ? C4 Fe2 N14 N13 175.9(15) . . . . ? C6 Fe2 N14 N13 131.9(3) . . . . ? C5 Fe2 N14 N13 -140.3(3) . . . . ? N18 Fe2 N14 N13 -48.4(3) . . . . ? N16 Fe2 N14 N13 39.8(3) . . . . ? N13 B2 N15 C33 -125.9(5) . . . . ? N17 B2 N15 C33 117.5(5) . . . . ? N13 B2 N15 N16 55.1(5) . . . . ? N17 B2 N15 N16 -61.6(6) . . . . ? C33 N15 N16 C31 0.4(5) . . . . ? B2 N15 N16 C31 179.7(4) . . . . ? C33 N15 N16 Fe2 -174.0(3) . . . . ? B2 N15 N16 Fe2 5.2(5) . . . . ? C4 Fe2 N16 C31 -34.8(5) . . . . ? C6 Fe2 N16 C31 50.5(5) . . . . ? C5 Fe2 N16 C31 -32(8) . . . . ? N18 Fe2 N16 C31 -128.7(5) . . . . ? N14 Fe2 N16 C31 141.1(5) . . . . ? C4 Fe2 N16 N15 137.6(3) . . . . ? C6 Fe2 N16 N15 -137.2(3) . . . . ? C5 Fe2 N16 N15 140(8) . . . . ? N18 Fe2 N16 N15 43.7(3) . . . . ? N14 Fe2 N16 N15 -46.6(3) . . . . ? N13 B2 N17 C39 128.3(5) . . . . ? N15 B2 N17 C39 -115.5(6) . . . . ? N13 B2 N17 N18 -63.2(5) . . . . ? N15 B2 N17 N18 53.0(6) . . . . ? C39 N17 N18 C37 0.3(5) . . . . ? B2 N17 N18 C37 -170.4(4) . . . . ? C39 N17 N18 Fe2 179.5(3) . . . . ? B2 N17 N18 Fe2 8.7(5) . . . . ? C4 Fe2 N18 C37 33.7(5) . . . . ? C6 Fe2 N18 C37 21(14) . . . . ? C5 Fe2 N18 C37 -50.7(5) . . . . ? N16 Fe2 N18 C37 127.8(5) . . . . ? N14 Fe2 N18 C37 -142.2(5) . . . . ? C4 Fe2 N18 N17 -145.2(3) . . . . ? C6 Fe2 N18 N17 -157(14) . . . . ? C5 Fe2 N18 N17 130.5(3) . . . . ? N16 Fe2 N18 N17 -51.0(3) . . . . ? N14 Fe2 N18 N17 39.0(3) . . . . ? N2 Ni1 N19 C43 179.5(3) . . . . ? N21 Ni1 N19 C43 -87.7(4) . . . . ? N22 Ni1 N19 C43 -4.6(3) . . . . ? N20 Ni1 N19 C43 26.1(7) . . . . ? N3 Ni1 N19 C43 90.8(4) 2_766 . . . ? N2 Ni1 N20 C45 172.8(3) . . . . ? N21 Ni1 N20 C45 80.2(3) . . . . ? N22 Ni1 N20 C45 -2.8(3) . . . . ? N3 Ni1 N20 C45 -97.5(3) 2_766 . . . ? N19 Ni1 N20 C45 -33.4(7) . . . . ? N2 Ni1 N21 C47 166.6(3) . . . . ? N22 Ni1 N21 C47 -15.6(3) . . . . ? N20 Ni1 N21 C47 -98.3(4) . . . . ? N3 Ni1 N21 C47 40(3) 2_766 . . . ? N19 Ni1 N21 C47 65.7(4) . . . . ? N2 Ni1 N22 C44 151.0(17) . . . . ? N21 Ni1 N22 C44 124.1(3) . . . . ? N20 Ni1 N22 C44 -140.8(3) . . . . ? N3 Ni1 N22 C44 -53.0(3) 2_766 . . . ? N19 Ni1 N22 C44 30.3(3) . . . . ? N2 Ni1 N22 C46 -91.1(18) . . . . ? N21 Ni1 N22 C46 -118.0(3) . . . . ? N20 Ni1 N22 C46 -22.9(3) . . . . ? N3 Ni1 N22 C46 65.0(3) 2_766 . . . ? N19 Ni1 N22 C46 148.2(3) . . . . ? N2 Ni1 N22 C48 26.2(19) . . . . ? N21 Ni1 N22 C48 -0.7(4) . . . . ? N20 Ni1 N22 C48 94.3(4) . . . . ? N3 Ni1 N22 C48 -177.8(4) 2_766 . . . ? N19 Ni1 N22 C48 -94.6(4) . . . . ? N1 Ni2 N23 C49 163.9(3) . . . . ? N26 Ni2 N23 C49 -18.4(3) . . . . ? N24 Ni2 N23 C49 64.7(3) . . . . ? N4 Ni2 N23 C49 22(3) . . . . ? N25 Ni2 N23 C49 -100.2(3) . . . . ? N1 Ni2 N24 C51 -176.0(3) . . . . ? N23 Ni2 N24 C51 -85.6(3) . . . . ? N26 Ni2 N24 C51 -2.2(3) . . . . ? N4 Ni2 N24 C51 92.1(3) . . . . ? N25 Ni2 N24 C51 34.5(7) . . . . ? N1 Ni2 N25 C53 175.4(3) . . . . ? N23 Ni2 N25 C53 84.5(3) . . . . ? N26 Ni2 N25 C53 1.8(3) . . . . ? N24 Ni2 N25 C53 -34.9(7) . . . . ? N4 Ni2 N25 C53 -92.7(3) . . . . ? N1 Ni2 N26 C52 138.0(12) . . . . ? N23 Ni2 N26 C52 117.7(3) . . . . ? N24 Ni2 N26 C52 25.2(3) . . . . ? N4 Ni2 N26 C52 -60.1(3) . . . . ? N25 Ni2 N26 C52 -144.5(3) . . . . ? N1 Ni2 N26 C54 -103.6(13) . . . . ? N23 Ni2 N26 C54 -123.8(3) . . . . ? N24 Ni2 N26 C54 143.6(3) . . . . ? N4 Ni2 N26 C54 58.3(3) . . . . ? N25 Ni2 N26 C54 -26.1(3) . . . . ? N1 Ni2 N26 C50 15.7(14) . . . . ? N23 Ni2 N26 C50 -4.6(3) . . . . ? N24 Ni2 N26 C50 -97.1(3) . . . . ? N4 Ni2 N26 C50 177.6(3) . . . . ? N25 Ni2 N26 C50 93.2(3) . . . . ? Ni2 N1 C1 Fe1 -167(100) . . . . ? C2 Fe1 C1 N1 89(41) . . . . ? C3 Fe1 C1 N1 178(100) . . . . ? N10 Fe1 C1 N1 -3(41) . . . . ? N8 Fe1 C1 N1 -93(41) . . . . ? N12 Fe1 C1 N1 121(41) . . . . ? Ni1 N2 C2 Fe1 100(38) . . . . ? C1 Fe1 C2 N2 95(39) . . . . ? C3 Fe1 C2 N2 4(39) . . . . ? N10 Fe1 C2 N2 -172(100) . . . . ? N8 Fe1 C2 N2 49(41) . . . . ? N12 Fe1 C2 N2 -83(39) . . . . ? Ni1 N3 C3 Fe1 21(3) 2_766 . . . ? C2 Fe1 C3 N3 -113(3) . . . . ? C1 Fe1 C3 N3 160(3) . . . . ? N10 Fe1 C3 N3 -6(5) . . . . ? N8 Fe1 C3 N3 68(3) . . . . ? N12 Fe1 C3 N3 -22(3) . . . . ? Ni2 N4 C4 Fe2 13(4) . . . . ? C6 Fe2 C4 N4 53(3) . . . . ? C5 Fe2 C4 N4 -35(3) . . . . ? N18 Fe2 C4 N4 -127(3) . . . . ? N16 Fe2 C4 N4 145(3) . . . . ? N14 Fe2 C4 N4 9(4) . . . . ? C4 Fe2 C5 N5 14(11) . . . . ? C6 Fe2 C5 N5 -71(11) . . . . ? N18 Fe2 C5 N5 108(11) . . . . ? N16 Fe2 C5 N5 11(16) . . . . ? N14 Fe2 C5 N5 -162(11) . . . . ? C4 Fe2 C6 N6 -18(17) . . . . ? C5 Fe2 C6 N6 66(18) . . . . ? N18 Fe2 C6 N6 -6(27) . . . . ? N16 Fe2 C6 N6 -112(18) . . . . ? N14 Fe2 C6 N6 158(18) . . . . ? N7 N8 C7 C8 0.4(4) . . . . ? Fe1 N8 C7 C8 174.7(3) . . . . ? N7 N8 C7 C12 -177.0(4) . . . . ? Fe1 N8 C7 C12 -2.6(6) . . . . ? N8 C7 C8 C9 -0.6(5) . . . . ? C12 C7 C8 C9 176.7(4) . . . . ? N8 C7 C8 C11 -177.8(4) . . . . ? C12 C7 C8 C11 -0.5(7) . . . . ? N8 N7 C9 C8 -0.4(5) . . . . ? B1 N7 C9 C8 178.0(4) . . . . ? N8 N7 C9 C10 179.0(4) . . . . ? B1 N7 C9 C10 -2.6(7) . . . . ? C7 C8 C9 N7 0.6(5) . . . . ? C11 C8 C9 N7 177.8(4) . . . . ? C7 C8 C9 C10 -178.7(4) . . . . ? C11 C8 C9 C10 -1.6(8) . . . . ? N9 N10 C13 C14 -0.3(5) . . . . ? Fe1 N10 C13 C14 170.6(3) . . . . ? N9 N10 C13 C18 177.9(4) . . . . ? Fe1 N10 C13 C18 -11.1(7) . . . . ? N10 C13 C14 C15 -0.3(6) . . . . ? C18 C13 C14 C15 -178.5(5) . . . . ? N10 C13 C14 C17 -178.7(5) . . . . ? C18 C13 C14 C17 3.1(9) . . . . ? N10 N9 C15 C14 -1.0(5) . . . . ? B1 N9 C15 C14 179.0(4) . . . . ? N10 N9 C15 C16 177.5(4) . . . . ? B1 N9 C15 C16 -2.4(7) . . . . ? C13 C14 C15 N9 0.8(6) . . . . ? C17 C14 C15 N9 179.2(6) . . . . ? C13 C14 C15 C16 -177.6(5) . . . . ? C17 C14 C15 C16 0.8(10) . . . . ? N11 N12 C19 C20 -0.8(5) . . . . ? Fe1 N12 C19 C20 178.2(3) . . . . ? N11 N12 C19 C24 178.4(4) . . . . ? Fe1 N12 C19 C24 -2.6(7) . . . . ? N12 C19 C20 C21 0.8(5) . . . . ? C24 C19 C20 C21 -178.4(4) . . . . ? N12 C19 C20 C23 178.5(5) . . . . ? C24 C19 C20 C23 -0.6(7) . . . . ? N12 N11 C21 C20 -0.1(5) . . . . ? B1 N11 C21 C20 171.2(4) . . . . ? N12 N11 C21 C22 179.9(4) . . . . ? B1 N11 C21 C22 -8.9(7) . . . . ? C19 C20 C21 N11 -0.4(5) . . . . ? C23 C20 C21 N11 -178.1(5) . . . . ? C19 C20 C21 C22 179.7(5) . . . . ? C23 C20 C21 C22 2.0(9) . . . . ? N13 N14 C25 C26 0.4(5) . . . . ? Fe2 N14 C25 C26 171.7(4) . . . . ? N13 N14 C25 C30 177.8(5) . . . . ? Fe2 N14 C25 C30 -10.9(8) . . . . ? N14 C25 C26 C27 -0.1(6) . . . . ? C30 C25 C26 C27 -177.5(5) . . . . ? N14 C25 C26 C29 -178.6(5) . . . . ? C30 C25 C26 C29 4.0(9) . . . . ? N14 N13 C27 C26 0.5(5) . . . . ? B2 N13 C27 C26 178.7(5) . . . . ? N14 N13 C27 C28 -179.5(5) . . . . ? B2 N13 C27 C28 -1.2(8) . . . . ? C25 C26 C27 N13 -0.2(6) . . . . ? C29 C26 C27 N13 178.3(5) . . . . ? C25 C26 C27 C28 179.7(5) . . . . ? C29 C26 C27 C28 -1.7(9) . . . . ? N15 N16 C31 C32 -0.4(5) . . . . ? Fe2 N16 C31 C32 172.6(4) . . . . ? N15 N16 C31 C36 179.5(5) . . . . ? Fe2 N16 C31 C36 -7.6(8) . . . . ? N16 C31 C32 C33 0.2(6) . . . . ? C36 C31 C32 C33 -179.7(5) . . . . ? N16 C31 C32 C35 -177.8(5) . . . . ? C36 C31 C32 C35 2.3(9) . . . . ? N16 N15 C33 C32 -0.3(5) . . . . ? B2 N15 C33 C32 -179.5(5) . . . . ? N16 N15 C33 C34 179.7(5) . . . . ? B2 N15 C33 C34 0.6(8) . . . . ? C31 C32 C33 N15 0.1(6) . . . . ? C35 C32 C33 N15 178.1(5) . . . . ? C31 C32 C33 C34 -179.9(6) . . . . ? C35 C32 C33 C34 -2.0(10) . . . . ? N17 N18 C37 C38 -0.7(5) . . . . ? Fe2 N18 C37 C38 -179.6(3) . . . . ? N17 N18 C37 C42 177.3(4) . . . . ? Fe2 N18 C37 C42 -1.6(7) . . . . ? N18 C37 C38 C39 0.7(5) . . . . ? C42 C37 C38 C39 -177.2(4) . . . . ? N18 C37 C38 C41 177.0(5) . . . . ? C42 C37 C38 C41 -0.9(8) . . . . ? N18 N17 C39 C38 0.1(5) . . . . ? B2 N17 C39 C38 169.4(5) . . . . ? N18 N17 C39 C40 -178.8(5) . . . . ? B2 N17 C39 C40 -9.5(9) . . . . ? C37 C38 C39 N17 -0.5(6) . . . . ? C41 C38 C39 N17 -176.9(5) . . . . ? C37 C38 C39 C40 178.3(5) . . . . ? C41 C38 C39 C40 1.9(9) . . . . ? Ni1 N19 C43 C44 -21.7(6) . . . . ? C46 N22 C44 C43 -164.3(4) . . . . ? C48 N22 C44 C43 71.2(5) . . . . ? Ni1 N22 C44 C43 -50.6(4) . . . . ? N19 C43 C44 N22 48.8(6) . . . . ? Ni1 N20 C45 C46 28.3(5) . . . . ? C44 N22 C46 C45 160.3(4) . . . . ? C48 N22 C46 C45 -72.1(5) . . . . ? Ni1 N22 C46 C45 45.9(4) . . . . ? N20 C45 C46 N22 -50.9(6) . . . . ? Ni1 N21 C47 C48 29.4(6) . . . . ? N21 C47 C48 N22 -31.4(8) . . . . ? C44 N22 C48 C47 -102.6(6) . . . . ? C46 N22 C48 C47 131.8(5) . . . . ? Ni1 N22 C48 C47 17.1(6) . . . . ? Ni2 N23 C49 C50 37.5(5) . . . . ? C52 N26 C50 C49 -90.6(5) . . . . ? C54 N26 C50 C49 143.4(4) . . . . ? Ni2 N26 C50 C49 27.0(5) . . . . ? N23 C49 C50 N26 -43.6(6) . . . . ? Ni2 N24 C51 C52 -21.4(5) . . . . ? C54 N26 C52 C51 -159.8(4) . . . . ? C50 N26 C52 C51 74.5(5) . . . . ? Ni2 N26 C52 C51 -45.0(5) . . . . ? N24 C51 C52 N26 45.4(6) . . . . ? Ni2 N25 C53 C54 22.8(5) . . . . ? C52 N26 C54 C53 161.1(4) . . . . ? C50 N26 C54 C53 -71.7(5) . . . . ? Ni2 N26 C54 C53 46.5(4) . . . . ? N25 C53 C54 N26 -47.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.359 _refine_diff_density_min -1.045 _refine_diff_density_rms 0.123