Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_paper _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author ; Prof Mir Wais Hosseini Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e Louis Pasteur, F-67000 Strasbourg, France ; _publ_contact_author_email hosseini@chimie.u-strasbg.fr _publ_contact_author_fax '33 3 90 24 13 23' _publ_contact_author_phone '33 3 90 24 13 25' _publ_requested_category FM loop_ _publ_author_name _publ_author_address D.Salazar-Mendoza ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e Louis Pasteur, F-67000 Strasbourg, France ; S.A.Baudron ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e Louis Pasteur, F-67000 Strasbourg, France ; M.W.Hosseini ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e Louis Pasteur, F-67000 Strasbourg, France ; N.Kyritsakas ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e Louis Pasteur, F-67000 Strasbourg, France ; ; A.De Cian ; ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e Louis Pasteur, F-67000 Strasbourg, France ; _publ_section_title ; Arranging up to Six Ferrocene Carboxamides around Metal Centres ; _publ_contact_author_name 'Prof Mir Wais Hosseini' ###Material relevant to compound 1 at 173K ######## data_e641a _database_code_depnum_ccdc_archive 'CCDC 615867' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H11 Fe N O' _chemical_formula_sum 'C11 H11 Fe N O' _chemical_formula_weight 229.06 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' 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 ' _symmetry_space_group_name_Hall '-P 2yn' 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 5.6124(3) _cell_length_b 13.1456(7) _cell_length_c 12.6100(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.721(2) _cell_angle_gamma 90.00 _cell_volume 925.71(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2422 _cell_measurement_theta_min 3.25 _cell_measurement_theta_max 29.99 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 1.588 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7523 _exptl_absorpt_correction_T_max 0.8323 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5950 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 30.11 _reflns_number_total 2673 _reflns_number_gt 2267 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0402P)^2^+0.0000P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2673 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0701 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0588(3) 0.10279(10) 0.88042(11) 0.0191(3) Uani 1 1 d . . . C2 C 0.1180(3) 0.17451(10) 0.79629(11) 0.0172(3) Uani 1 1 d . . . C3 C -0.0524(3) 0.21423(11) 0.71435(11) 0.0186(3) Uani 1 1 d . . . H3 H -0.2140 0.1975 0.7033 0.022 Uiso 1 1 calc R . . C4 C 0.0717(3) 0.28415(11) 0.65292(10) 0.0217(3) Uani 1 1 d . . . H4 H 0.0045 0.3209 0.5944 0.026 Uiso 1 1 calc R . . C5 C 0.3154(3) 0.28824(12) 0.69626(11) 0.0218(3) Uani 1 1 d . . . H5 H 0.4342 0.3284 0.6712 0.026 Uiso 1 1 calc R . . C6 C 0.3463(3) 0.22005(11) 0.78493(11) 0.0199(3) Uani 1 1 d . . . H6 H 0.4884 0.2075 0.8274 0.024 Uiso 1 1 calc R . . C7 C -0.0176(3) 0.35690(12) 0.95677(12) 0.0267(4) Uani 1 1 d . . . H7 H -0.0556 0.3085 1.0062 0.032 Uiso 1 1 calc R . . C8 C -0.1784(3) 0.39971(12) 0.87498(13) 0.0280(3) Uani 1 1 d . . . H8 H -0.3402 0.3843 0.8612 0.034 Uiso 1 1 calc R . . C9 C -0.0483(3) 0.47057(11) 0.81757(12) 0.0259(3) Uani 1 1 d . . . H9 H -0.1102 0.5096 0.7598 0.031 Uiso 1 1 calc R . . C10 C 0.1917(3) 0.47089(11) 0.86418(12) 0.0226(3) Uani 1 1 d . . . H10 H 0.3154 0.5103 0.8423 0.027 Uiso 1 1 calc R . . C11 C 0.2110(3) 0.40069(11) 0.95019(11) 0.0232(3) Uani 1 1 d . . . H11 H 0.3494 0.3860 0.9944 0.028 Uiso 1 1 calc R . . N1 N 0.2460(3) 0.05674(10) 0.93531(11) 0.0274(3) Uani 1 1 d . . . H1A H 0.2226 0.0142 0.9850 0.033 Uiso 1 1 calc R . . H1B H 0.3894 0.0698 0.9208 0.033 Uiso 1 1 calc R . . O1 O -0.1506(2) 0.08610(8) 0.89885(8) 0.0265(2) Uani 1 1 d . . . Fe1 Fe 0.09609(4) 0.327700(14) 0.810468(14) 0.01462(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0238(8) 0.0140(6) 0.0184(6) -0.0019(5) -0.0031(5) -0.0001(5) C2 0.0194(7) 0.0143(6) 0.0172(6) -0.0032(4) -0.0009(5) 0.0021(5) C3 0.0192(7) 0.0182(6) 0.0179(6) -0.0027(5) -0.0002(5) 0.0027(6) C4 0.0269(8) 0.0234(7) 0.0148(6) -0.0003(5) 0.0023(6) 0.0044(6) C5 0.0242(8) 0.0222(7) 0.0202(6) -0.0007(5) 0.0083(6) 0.0024(6) C6 0.0183(7) 0.0197(6) 0.0217(6) -0.0025(5) 0.0013(6) 0.0043(6) C7 0.0388(10) 0.0218(7) 0.0216(7) -0.0044(6) 0.0143(7) -0.0038(7) C8 0.0204(8) 0.0275(7) 0.0373(8) -0.0127(7) 0.0084(7) -0.0002(6) C9 0.0296(9) 0.0182(7) 0.0294(7) -0.0021(6) 0.0002(6) 0.0078(6) C10 0.0278(8) 0.0149(6) 0.0257(7) -0.0023(5) 0.0057(6) -0.0021(6) C11 0.0283(8) 0.0228(7) 0.0179(6) -0.0041(5) -0.0010(6) 0.0018(6) N1 0.0249(8) 0.0282(6) 0.0281(6) 0.0092(5) -0.0019(5) 0.0034(6) O1 0.0238(6) 0.0253(5) 0.0291(5) 0.0085(4) -0.0034(4) -0.0041(5) Fe1 0.01593(12) 0.01355(11) 0.01453(11) -0.00041(6) 0.00216(8) 0.00157(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.2402(18) . ? C1 N1 1.3433(19) . ? C1 C2 1.4815(19) . ? C2 C6 1.434(2) . ? C2 C3 1.434(2) . ? C2 Fe1 2.0265(13) . ? C3 C4 1.427(2) . ? C3 Fe1 2.0463(15) . ? C3 H3 0.9300 . ? C4 C5 1.422(2) . ? C4 Fe1 2.0589(13) . ? C4 H4 0.9300 . ? C5 C6 1.430(2) . ? C5 Fe1 2.0522(13) . ? C5 H5 0.9300 . ? C6 Fe1 2.0417(14) . ? C6 H6 0.9300 . ? C7 C11 1.416(2) . ? C7 C8 1.418(2) . ? C7 Fe1 2.0475(14) . ? C7 H7 0.9300 . ? C8 C9 1.425(2) . ? C8 Fe1 2.0447(15) . ? C8 H8 0.9300 . ? C9 C10 1.415(2) . ? C9 Fe1 2.0510(14) . ? C9 H9 0.9300 . ? C10 C11 1.420(2) . ? C10 Fe1 2.0537(14) . ? C10 H10 0.9300 . ? C11 Fe1 2.0529(14) . ? C11 H11 0.9300 . ? N1 H1A 0.8600 . ? N1 H1B 0.8600 . ? 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 O1 C1 N1 122.07(13) . . ? O1 C1 C2 122.07(13) . . ? N1 C1 C2 115.86(14) . . ? C6 C2 C3 108.31(12) . . ? C6 C2 C1 127.11(13) . . ? C3 C2 C1 124.51(13) . . ? C6 C2 Fe1 69.92(8) . . ? C3 C2 Fe1 70.12(8) . . ? C1 C2 Fe1 123.32(9) . . ? C4 C3 C2 107.39(13) . . ? C4 C3 Fe1 70.13(8) . . ? C2 C3 Fe1 68.64(8) . . ? C4 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? Fe1 C3 H3 126.5 . . ? C5 C4 C3 108.56(13) . . ? C5 C4 Fe1 69.50(8) . . ? C3 C4 Fe1 69.18(8) . . ? C5 C4 H4 125.7 . . ? C3 C4 H4 125.7 . . ? Fe1 C4 H4 127.2 . . ? C4 C5 C6 108.29(13) . . ? C4 C5 Fe1 70.02(8) . . ? C6 C5 Fe1 69.16(8) . . ? C4 C5 H5 125.9 . . ? C6 C5 H5 125.9 . . ? Fe1 C5 H5 126.5 . . ? C5 C6 C2 107.44(13) . . ? C5 C6 Fe1 69.95(8) . . ? C2 C6 Fe1 68.79(8) . . ? C5 C6 H6 126.3 . . ? C2 C6 H6 126.3 . . ? Fe1 C6 H6 126.5 . . ? C11 C7 C8 108.11(14) . . ? C11 C7 Fe1 70.00(8) . . ? C8 C7 Fe1 69.63(8) . . ? C11 C7 H7 125.9 . . ? C8 C7 H7 125.9 . . ? Fe1 C7 H7 126.0 . . ? C7 C8 C9 107.93(15) . . ? C7 C8 Fe1 69.84(9) . . ? C9 C8 Fe1 69.88(8) . . ? C7 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? Fe1 C8 H8 125.8 . . ? C10 C9 C8 107.80(14) . . ? C10 C9 Fe1 69.94(8) . . ? C8 C9 Fe1 69.41(8) . . ? C10 C9 H9 126.1 . . ? C8 C9 H9 126.1 . . ? Fe1 C9 H9 126.1 . . ? C9 C10 C11 108.20(14) . . ? C9 C10 Fe1 69.73(8) . . ? C11 C10 Fe1 69.74(8) . . ? C9 C10 H10 125.9 . . ? C11 C10 H10 125.9 . . ? Fe1 C10 H10 126.2 . . ? C7 C11 C10 107.95(15) . . ? C7 C11 Fe1 69.59(8) . . ? C10 C11 Fe1 69.80(8) . . ? C7 C11 H11 126.0 . . ? C10 C11 H11 126.0 . . ? Fe1 C11 H11 126.2 . . ? C1 N1 H1A 120.0 . . ? C1 N1 H1B 120.0 . . ? H1A N1 H1B 120.0 . . ? C2 Fe1 C6 41.29(6) . . ? C2 Fe1 C8 123.36(6) . . ? C6 Fe1 C8 160.21(6) . . ? C2 Fe1 C3 41.24(6) . . ? C6 Fe1 C3 69.34(6) . . ? C8 Fe1 C3 107.14(6) . . ? C2 Fe1 C7 107.03(6) . . ? C6 Fe1 C7 123.58(6) . . ? C8 Fe1 C7 40.53(7) . . ? C3 Fe1 C7 121.69(6) . . ? C2 Fe1 C9 160.30(7) . . ? C6 Fe1 C9 157.31(7) . . ? C8 Fe1 C9 40.71(6) . . ? C3 Fe1 C9 123.64(6) . . ? C7 Fe1 C9 68.22(6) . . ? C2 Fe1 C5 68.96(6) . . ? C6 Fe1 C5 40.89(6) . . ? C8 Fe1 C5 157.60(7) . . ? C3 Fe1 C5 68.74(6) . . ? C7 Fe1 C5 160.43(7) . . ? C9 Fe1 C5 121.96(6) . . ? C2 Fe1 C11 121.57(6) . . ? C6 Fe1 C11 107.28(6) . . ? C8 Fe1 C11 68.10(7) . . ? C3 Fe1 C11 157.47(6) . . ? C7 Fe1 C11 40.41(7) . . ? C9 Fe1 C11 68.06(6) . . ? C5 Fe1 C11 124.14(7) . . ? C2 Fe1 C10 157.48(6) . . ? C6 Fe1 C10 121.74(6) . . ? C8 Fe1 C10 68.09(6) . . ? C3 Fe1 C10 160.24(6) . . ? C7 Fe1 C10 68.02(6) . . ? C9 Fe1 C10 40.33(7) . . ? C5 Fe1 C10 107.93(6) . . ? C11 Fe1 C10 40.46(6) . . ? C2 Fe1 C4 68.74(6) . . ? C6 Fe1 C4 68.63(6) . . ? C8 Fe1 C4 122.17(7) . . ? C3 Fe1 C4 40.70(6) . . ? C7 Fe1 C4 157.64(7) . . ? C9 Fe1 C4 107.95(6) . . ? C5 Fe1 C4 40.48(6) . . ? C11 Fe1 C4 160.57(6) . . ? C10 Fe1 C4 124.27(6) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 30.11 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.405 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.066 ###Material relevant to compound 2 at 173K ######## data_e623a _database_code_depnum_ccdc_archive 'CCDC 615868' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H66 Co Fe6 N6 O6, 2(B F4), (H2O)' _chemical_formula_sum 'C66 H68 B2 Co F8 Fe6 N6 O7' _chemical_formula_weight 1624.91 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' F F 0.0171 0.0103 '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' Co Co 0.3494 0.9721 '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 ' _symmetry_space_group_name_Hall '-P 2yn' 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 22.4039(5) _cell_length_b 13.9424(3) _cell_length_c 23.4953(6) _cell_angle_alpha 90.00 _cell_angle_beta 115.8790(10) _cell_angle_gamma 90.00 _cell_volume 6603.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6904 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.67 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3308 _exptl_absorpt_coefficient_mu 1.607 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6618 _exptl_absorpt_correction_T_max 0.8558 _exptl_absorpt_process_details sadabs _exptl_special_details ; A fluorine atom on one BF4 anion shows positional disorder which was modeled over two sites. The hydrogen atoms on the water molecule have not been introduced, although they are taken into account in the formula. One Cp shows high thermal parameters. No clear explanation for this was found ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68077 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 27.65 _reflns_number_total 15263 _reflns_number_gt 11474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0783P)^2^+1.8104P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15263 _refine_ls_number_parameters 869 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1100 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.33274(14) -0.1603(2) 0.53260(13) 0.0257(6) Uani 1 1 d . . . C2 C 0.34942(15) -0.2614(2) 0.53085(14) 0.0282(6) Uani 1 1 d . . . C3 C 0.30616(16) -0.3313(2) 0.48810(14) 0.0310(7) Uani 1 1 d . . . H3 H 0.2617 -0.3194 0.4543 0.037 Uiso 1 1 calc R . . C4 C 0.33911(18) -0.4208(2) 0.50410(17) 0.0387(8) Uani 1 1 d . . . H4 H 0.3207 -0.4822 0.4836 0.046 Uiso 1 1 calc R . . C5 C 0.40218(18) -0.4076(2) 0.5551(2) 0.0451(9) Uani 1 1 d . . . H5 H 0.4351 -0.4579 0.5760 0.054 Uiso 1 1 calc R . . C6 C 0.40904(16) -0.3091(2) 0.57183(17) 0.0371(7) Uani 1 1 d . . . H6 H 0.4478 -0.2793 0.6058 0.045 Uiso 1 1 calc R . . C7 C 0.2759(2) -0.3029(3) 0.62109(19) 0.0544(11) Uani 1 1 d . . . H7 H 0.2558 -0.2389 0.6118 0.065 Uiso 1 1 calc R . . C8 C 0.2452(2) -0.3887(3) 0.59109(18) 0.0515(10) Uani 1 1 d . . . H8 H 0.2002 -0.3947 0.5570 0.062 Uiso 1 1 calc R . . C9 C 0.2905(2) -0.4645(3) 0.61813(19) 0.0511(10) Uani 1 1 d . . . H9 H 0.2827 -0.5323 0.6062 0.061 Uiso 1 1 calc R . . C10 C 0.3497(2) -0.4248(3) 0.66531(18) 0.0561(11) Uani 1 1 d . . . H10 H 0.3901 -0.4602 0.6921 0.067 Uiso 1 1 calc R . . C11 C 0.3400(2) -0.3248(3) 0.66632(17) 0.0561(11) Uani 1 1 d . . . H11 H 0.3725 -0.2786 0.6944 0.067 Uiso 1 1 calc R . . C12 C 0.39035(13) 0.08006(18) 0.47763(12) 0.0206(5) Uani 1 1 d . . . C13 C 0.45899(13) 0.10605(19) 0.52015(12) 0.0219(5) Uani 1 1 d . . . C14 C 0.51133(14) 0.13158(19) 0.50359(14) 0.0248(6) Uani 1 1 d . . . H14 H 0.5095 0.1290 0.4612 0.030 Uiso 1 1 calc R . . C15 C 0.56647(14) 0.1612(2) 0.55989(14) 0.0288(6) Uani 1 1 d . . . H15 H 0.6090 0.1844 0.5628 0.035 Uiso 1 1 calc R . . C16 C 0.54888(15) 0.1537(2) 0.61064(14) 0.0293(6) Uani 1 1 d . . . H16 H 0.5772 0.1713 0.6547 0.035 Uiso 1 1 calc R . . C17 C 0.48269(14) 0.12014(19) 0.58676(13) 0.0239(6) Uani 1 1 d . . . H17 H 0.4577 0.1085 0.6115 0.029 Uiso 1 1 calc R . . C18 C 0.40183(16) 0.3236(2) 0.49071(17) 0.0406(8) Uani 1 1 d . . . H18 H 0.3586 0.2981 0.4612 0.049 Uiso 1 1 calc R . . C19 C 0.45396(18) 0.3500(2) 0.47513(19) 0.0447(9) Uani 1 1 d . . . H19 H 0.4531 0.3463 0.4331 0.054 Uiso 1 1 calc R . . C20 C 0.50704(19) 0.3823(2) 0.5307(2) 0.0504(10) Uani 1 1 d . . . H20 H 0.5500 0.4047 0.5342 0.060 Uiso 1 1 calc R . . C21 C 0.48851(19) 0.3766(2) 0.5806(2) 0.0477(9) Uani 1 1 d . . . H21 H 0.5161 0.3945 0.6247 0.057 Uiso 1 1 calc R . . C22 C 0.42250(18) 0.3404(2) 0.55574(18) 0.0415(8) Uani 1 1 d . . . H22 H 0.3964 0.3290 0.5795 0.050 Uiso 1 1 calc R . . C23 C 0.17351(14) 0.1915(2) 0.40108(13) 0.0251(6) Uani 1 1 d . . . C24 C 0.16681(15) 0.2970(2) 0.39867(14) 0.0271(6) Uani 1 1 d . . . C25 C 0.21224(16) 0.3608(2) 0.44516(15) 0.0314(7) Uani 1 1 d . . . H25 H 0.2551 0.3434 0.4798 0.038 Uiso 1 1 calc R . . C26 C 0.18397(17) 0.4539(2) 0.43172(17) 0.0368(7) Uani 1 1 d . . . H26 H 0.2035 0.5120 0.4564 0.044 Uiso 1 1 calc R . . C27 C 0.12250(18) 0.4486(2) 0.37796(16) 0.0361(7) Uani 1 1 d . . . H27 H 0.0919 0.5023 0.3591 0.043 Uiso 1 1 calc R . . C28 C 0.11082(16) 0.3516(2) 0.35699(14) 0.0309(7) Uani 1 1 d . . . H28 H 0.0718 0.3270 0.3206 0.037 Uiso 1 1 calc R . . C29 C 0.1017(2) 0.2528(3) 0.4953(2) 0.0495(10) Uani 1 1 d . . . H29 H 0.1144 0.1852 0.4964 0.059 Uiso 1 1 calc R . . C30 C 0.14005(19) 0.3242(3) 0.53808(16) 0.0472(9) Uani 1 1 d . . . H30 H 0.1835 0.3154 0.5742 0.057 Uiso 1 1 calc R . . C31 C 0.10402(19) 0.4113(3) 0.51915(16) 0.0420(8) Uani 1 1 d . . . H31 H 0.1183 0.4737 0.5399 0.050 Uiso 1 1 calc R . . C32 C 0.04430(17) 0.3926(3) 0.46529(17) 0.0395(8) Uani 1 1 d . . . H32 H 0.0097 0.4397 0.4420 0.047 Uiso 1 1 calc R . . C33 C 0.04294(19) 0.2943(3) 0.45054(18) 0.0458(9) Uani 1 1 d . . . H33 H 0.0073 0.2610 0.4153 0.055 Uiso 1 1 calc R . . C34 C 0.11536(14) -0.0489(2) 0.46289(13) 0.0266(6) Uani 1 1 d . . . C35 C 0.04647(14) -0.0789(2) 0.42546(13) 0.0255(6) Uani 1 1 d . . . C36 C 0.01582(15) -0.0891(2) 0.35785(14) 0.0306(6) Uani 1 1 d . . . H36 H 0.0349 -0.0706 0.3290 0.037 Uiso 1 1 calc R . . C37 C -0.04730(15) -0.1317(2) 0.34078(15) 0.0359(7) Uani 1 1 d . . . H37 H -0.0789 -0.1496 0.2978 0.043 Uiso 1 1 calc R . . C38 C -0.05593(15) -0.1475(2) 0.39596(15) 0.0346(7) Uani 1 1 d . . . H38 H -0.0946 -0.1779 0.3975 0.042 Uiso 1 1 calc R . . C39 C 0.00113(14) -0.1150(2) 0.44887(14) 0.0284(6) Uani 1 1 d . . . H39 H 0.0085 -0.1168 0.4932 0.034 Uiso 1 1 calc R . . C40 C 0.11532(17) -0.2888(2) 0.44619(18) 0.0409(8) Uani 1 1 d . . . H40 H 0.1586 -0.2605 0.4732 0.049 Uiso 1 1 calc R . . C41 C 0.08838(18) -0.3023(2) 0.38043(17) 0.0396(8) Uani 1 1 d . . . H41 H 0.1095 -0.2836 0.3533 0.048 Uiso 1 1 calc R . . C42 C 0.0250(2) -0.3448(2) 0.35947(19) 0.0474(9) Uani 1 1 d . . . H42 H -0.0049 -0.3613 0.3156 0.057 Uiso 1 1 calc R . . C43 C 0.0121(2) -0.3587(2) 0.4126(2) 0.0463(9) Uani 1 1 d . . . H43 H -0.0281 -0.3871 0.4122 0.056 Uiso 1 1 calc R . . C44 C 0.06769(19) -0.3250(3) 0.46656(19) 0.0464(9) Uani 1 1 d . . . H44 H 0.0727 -0.3257 0.5101 0.056 Uiso 1 1 calc R . . C45 C 0.20972(13) -0.06067(19) 0.32813(12) 0.0215(5) Uani 1 1 d . . . C46 C 0.22317(15) -0.0620(2) 0.27268(13) 0.0250(6) Uani 1 1 d . . . C47 C 0.17495(18) -0.0700(2) 0.20821(14) 0.0367(8) Uani 1 1 d . . . H47 H 0.1270 -0.0779 0.1931 0.044 Uiso 1 1 calc R . . C48 C 0.2098(2) -0.0637(2) 0.17017(15) 0.0447(9) Uani 1 1 d . . . H48 H 0.1898 -0.0658 0.1238 0.054 Uiso 1 1 calc R . . C49 C 0.27772(19) -0.0530(2) 0.21007(16) 0.0401(8) Uani 1 1 d . . . H49 H 0.3129 -0.0463 0.1962 0.048 Uiso 1 1 calc R . . C50 C 0.28689(16) -0.0510(2) 0.27345(14) 0.0297(6) Uani 1 1 d . . . H50 H 0.3293 -0.0442 0.3111 0.036 Uiso 1 1 calc R . . C51 C 0.22174(17) 0.1776(2) 0.27266(16) 0.0362(7) Uani 1 1 d . . . H51 H 0.2247 0.1789 0.3155 0.043 Uiso 1 1 calc R . . C52 C 0.16293(18) 0.1682(3) 0.21624(19) 0.0471(9) Uani 1 1 d . . . H52 H 0.1179 0.1627 0.2129 0.056 Uiso 1 1 calc R . . C53 C 0.1808(2) 0.1689(3) 0.16482(17) 0.0501(10) Uani 1 1 d . . . H53 H 0.1502 0.1642 0.1198 0.060 Uiso 1 1 calc R . . C54 C 0.25021(19) 0.1785(2) 0.19059(16) 0.0418(8) Uani 1 1 d . . . H54 H 0.2765 0.1808 0.1665 0.050 Uiso 1 1 calc R . . C55 C 0.27555(17) 0.1835(2) 0.25704(16) 0.0362(7) Uani 1 1 d . . . H55 H 0.3224 0.1900 0.2870 0.043 Uiso 1 1 calc R . . C56 C 0.28497(15) 0.1077(2) 0.59998(13) 0.0322(7) Uani 1 1 d . . . C57 C 0.26440(16) 0.1198(3) 0.65106(14) 0.0458(9) Uani 1 1 d . . . C58 C 0.2807(2) 0.1974(4) 0.69512(16) 0.0585(12) Uani 1 1 d . . . H58 H 0.3075 0.2537 0.6967 0.070 Uiso 1 1 calc R . . C59 C 0.2505(2) 0.1780(5) 0.7361(2) 0.0820(14) Uani 1 1 d . . . H59 H 0.2539 0.2183 0.7716 0.098 Uiso 1 1 calc R . . C60 C 0.2170(2) 0.0925(5) 0.71870(19) 0.0820(14) Uani 1 1 d . . . H60 H 0.1929 0.0620 0.7400 0.098 Uiso 1 1 calc R . . C61 C 0.22548(18) 0.0526(4) 0.66662(16) 0.0652(14) Uani 1 1 d . . . H61 H 0.2068 -0.0077 0.6447 0.078 Uiso 1 1 calc R . . C62 C 0.4142(2) 0.0837(4) 0.7964(2) 0.0721(14) Uani 1 1 d . . . H62 H 0.4412 0.1411 0.8010 0.087 Uiso 1 1 calc R . . C63 C 0.3804(2) 0.0603(5) 0.83263(19) 0.0767(16) Uani 1 1 d . . . H63 H 0.3798 0.0990 0.8672 0.092 Uiso 1 1 calc R . . C64 C 0.3486(3) -0.0245(6) 0.8120(3) 0.101(2) Uani 1 1 d . . . H64 H 0.3215 -0.0572 0.8294 0.121 Uiso 1 1 calc R . . C65 C 0.3609(3) -0.0581(5) 0.7618(3) 0.099(2) Uani 1 1 d . . . H65 H 0.3444 -0.1180 0.7383 0.119 Uiso 1 1 calc R . . C66 C 0.4018(2) 0.0099(5) 0.7517(2) 0.0782(17) Uani 1 1 d . . . H66 H 0.4186 0.0064 0.7196 0.094 Uiso 1 1 calc R . . N1 N 0.37497(13) -0.10745(18) 0.58019(12) 0.0364(6) Uani 1 1 d . . . H1A H 0.3670 -0.0476 0.5825 0.044 Uiso 1 1 calc R . . H1B H 0.4103 -0.1331 0.6087 0.044 Uiso 1 1 calc R . . N2 N 0.37187(12) 0.07698(18) 0.41623(11) 0.0291(5) Uani 1 1 d . . . H2A H 0.3317 0.0620 0.3909 0.035 Uiso 1 1 calc R . . H2B H 0.4000 0.0899 0.4015 0.035 Uiso 1 1 calc R . . N3 N 0.12456(13) 0.14160(18) 0.35753(12) 0.0337(6) Uani 1 1 d . . . H3A H 0.1266 0.0800 0.3573 0.040 Uiso 1 1 calc R . . H3B H 0.0907 0.1708 0.3294 0.040 Uiso 1 1 calc R . . N4 N 0.13820(15) -0.0443(2) 0.52460(12) 0.0470(8) Uani 1 1 d . . . H4A H 0.1786 -0.0275 0.5475 0.056 Uiso 1 1 calc R . . H4B H 0.1127 -0.0582 0.5422 0.056 Uiso 1 1 calc R . . N5 N 0.15740(13) -0.10833(18) 0.32495(12) 0.0320(6) Uani 1 1 d . . . H5A H 0.1480 -0.1086 0.3568 0.038 Uiso 1 1 calc R . . H5B H 0.1327 -0.1391 0.2911 0.038 Uiso 1 1 calc R . . N6 N 0.32836(14) 0.1681(2) 0.59658(13) 0.0402(7) Uani 1 1 d . . . H6A H 0.3409 0.1624 0.5670 0.048 Uiso 1 1 calc R . . H6B H 0.3442 0.2134 0.6240 0.048 Uiso 1 1 calc R . . O1 O 0.28073(10) -0.12680(14) 0.48987(9) 0.0278(4) Uani 1 1 d . . . O2 O 0.35022(9) 0.06141(13) 0.50072(8) 0.0226(4) Uani 1 1 d . . . O3 O 0.22383(10) 0.15355(13) 0.44299(9) 0.0271(4) Uani 1 1 d . . . O4 O 0.15133(9) -0.02900(14) 0.43547(9) 0.0257(4) Uani 1 1 d . . . O5 O 0.24698(9) -0.01487(14) 0.37695(8) 0.0238(4) Uani 1 1 d . . . O6 O 0.26104(10) 0.04103(16) 0.56061(9) 0.0305(5) Uani 1 1 d . . . Fe1 Fe 0.32912(2) -0.36414(3) 0.579902(19) 0.02736(11) Uani 1 1 d . . . Fe2 Fe 0.48413(2) 0.24434(3) 0.541943(19) 0.02392(10) Uani 1 1 d . . . Fe3 Fe 0.12300(2) 0.35899(3) 0.448017(19) 0.02520(10) Uani 1 1 d . . . Fe4 Fe 0.02719(2) -0.21748(3) 0.402835(19) 0.02568(10) Uani 1 1 d . . . Fe5 Fe 0.22551(2) 0.05735(3) 0.224202(18) 0.02509(10) Uani 1 1 d . . . Fe6 Fe 0.31498(2) 0.07070(5) 0.74075(2) 0.05060(16) Uani 1 1 d . . . Co1 Co 0.252075(17) 0.01358(3) 0.466722(16) 0.01977(9) Uani 1 1 d . . . B1 B 0.4521(3) 0.3416(5) 0.7392(3) 0.0806(19) Uani 1 1 d . . . F1 F 0.39893(15) 0.3286(2) 0.68429(12) 0.0855(9) Uani 1 1 d . A . F2A F 0.4501(5) 0.3179(7) 0.7924(2) 0.141(4) Uani 0.712(16) 1 d P A 1 F2B F 0.4127(10) 0.3836(13) 0.7669(8) 0.105(8) Uani 0.288(16) 1 d P A 2 F3 F 0.48483(19) 0.4244(3) 0.73756(19) 0.1308(15) Uani 1 1 d . A . F4 F 0.4965(2) 0.2712(3) 0.7436(3) 0.178(2) Uani 1 1 d . A . B2 B 0.54660(19) 0.8350(3) 0.70816(17) 0.0410(9) Uani 1 1 d . . . F5 F 0.48166(9) 0.84022(16) 0.69897(9) 0.0486(5) Uani 1 1 d . . . F6 F 0.58582(13) 0.8965(2) 0.75301(12) 0.0806(9) Uani 1 1 d . . . F7 F 0.54813(11) 0.8525(2) 0.65061(10) 0.0626(7) Uani 1 1 d . . . F8 F 0.56896(14) 0.7418(2) 0.72700(13) 0.0765(8) Uani 1 1 d . . . O7 O 0.42008(16) 0.4094(2) 0.88600(14) 0.0605(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0284(15) 0.0250(14) 0.0249(13) 0.0046(11) 0.0125(12) -0.0007(12) C2 0.0303(16) 0.0270(15) 0.0322(15) 0.0011(12) 0.0180(13) -0.0009(12) C3 0.0390(18) 0.0294(15) 0.0314(15) -0.0024(12) 0.0217(14) -0.0037(13) C4 0.044(2) 0.0288(16) 0.056(2) -0.0098(14) 0.0338(18) -0.0029(14) C5 0.0373(19) 0.0285(17) 0.077(3) -0.0028(17) 0.0316(19) 0.0062(14) C6 0.0257(16) 0.0276(16) 0.059(2) -0.0003(14) 0.0192(16) 0.0017(13) C7 0.082(3) 0.054(2) 0.052(2) 0.0144(18) 0.052(2) 0.021(2) C8 0.047(2) 0.074(3) 0.045(2) 0.0129(19) 0.0307(18) -0.001(2) C9 0.070(3) 0.042(2) 0.054(2) 0.0120(17) 0.039(2) -0.0071(19) C10 0.064(3) 0.061(3) 0.0382(19) 0.0247(18) 0.0184(19) 0.006(2) C11 0.087(3) 0.054(2) 0.0338(19) -0.0027(17) 0.032(2) -0.009(2) C12 0.0206(13) 0.0143(12) 0.0258(13) 0.0011(10) 0.0092(11) 0.0002(10) C13 0.0212(14) 0.0196(13) 0.0226(13) 0.0003(10) 0.0074(11) 0.0005(11) C14 0.0202(14) 0.0238(14) 0.0303(14) -0.0010(11) 0.0110(12) 0.0009(11) C15 0.0191(14) 0.0247(14) 0.0388(16) -0.0004(12) 0.0092(12) 0.0019(11) C16 0.0244(15) 0.0258(14) 0.0286(14) -0.0010(11) 0.0033(12) 0.0020(12) C17 0.0219(14) 0.0216(13) 0.0235(13) 0.0009(10) 0.0054(11) 0.0002(11) C18 0.0274(17) 0.0293(16) 0.057(2) 0.0123(15) 0.0107(15) 0.0122(13) C19 0.046(2) 0.0347(18) 0.056(2) 0.0224(16) 0.0242(18) 0.0154(16) C20 0.039(2) 0.0234(16) 0.086(3) 0.0144(17) 0.024(2) 0.0023(14) C21 0.048(2) 0.0217(16) 0.063(2) -0.0075(15) 0.0142(19) 0.0062(15) C22 0.041(2) 0.0250(16) 0.065(2) 0.0016(15) 0.0289(18) 0.0089(14) C23 0.0273(15) 0.0266(14) 0.0250(13) -0.0004(11) 0.0149(12) 0.0018(12) C24 0.0318(16) 0.0257(14) 0.0300(14) 0.0020(11) 0.0192(13) 0.0056(12) C25 0.0291(16) 0.0310(16) 0.0410(17) -0.0024(13) 0.0219(14) -0.0034(13) C26 0.046(2) 0.0243(15) 0.055(2) -0.0031(14) 0.0359(17) -0.0066(14) C27 0.049(2) 0.0286(16) 0.0441(18) 0.0102(13) 0.0332(17) 0.0089(14) C28 0.0364(17) 0.0322(16) 0.0286(15) 0.0086(12) 0.0184(13) 0.0085(13) C29 0.074(3) 0.0342(19) 0.065(2) 0.0130(17) 0.053(2) 0.0017(18) C30 0.048(2) 0.068(3) 0.0307(17) 0.0118(17) 0.0224(16) 0.0074(19) C31 0.054(2) 0.047(2) 0.0391(18) -0.0081(15) 0.0326(17) -0.0083(17) C32 0.0338(18) 0.049(2) 0.0460(19) 0.0007(16) 0.0269(16) 0.0020(15) C33 0.047(2) 0.054(2) 0.048(2) -0.0093(17) 0.0320(18) -0.0232(18) C34 0.0265(15) 0.0288(15) 0.0273(14) -0.0027(11) 0.0144(12) -0.0026(12) C35 0.0250(15) 0.0279(14) 0.0264(14) 0.0014(11) 0.0140(12) 0.0014(12) C36 0.0266(15) 0.0375(16) 0.0277(14) 0.0073(12) 0.0117(12) 0.0020(13) C37 0.0212(15) 0.052(2) 0.0277(15) 0.0051(14) 0.0044(12) 0.0003(14) C38 0.0189(15) 0.0443(19) 0.0405(17) 0.0072(14) 0.0128(13) -0.0005(13) C39 0.0252(15) 0.0341(16) 0.0302(15) 0.0007(12) 0.0159(12) 0.0020(12) C40 0.0351(18) 0.0350(18) 0.054(2) 0.0058(15) 0.0207(16) 0.0084(14) C41 0.047(2) 0.0302(16) 0.055(2) -0.0007(15) 0.0350(18) 0.0030(15) C42 0.055(2) 0.0347(18) 0.059(2) -0.0156(16) 0.031(2) -0.0099(17) C43 0.049(2) 0.0297(17) 0.073(3) 0.0031(17) 0.039(2) -0.0035(15) C44 0.055(2) 0.0415(19) 0.054(2) 0.0186(17) 0.0336(19) 0.0156(18) C45 0.0217(14) 0.0208(13) 0.0215(12) 0.0000(10) 0.0092(11) 0.0012(11) C46 0.0302(15) 0.0241(14) 0.0213(13) -0.0022(10) 0.0119(12) -0.0042(12) C47 0.0424(19) 0.0383(17) 0.0246(14) -0.0071(13) 0.0101(14) -0.0175(15) C48 0.071(3) 0.044(2) 0.0271(16) -0.0122(14) 0.0296(17) -0.0195(18) C49 0.058(2) 0.0347(17) 0.0437(19) -0.0038(14) 0.0373(18) 0.0030(16) C50 0.0339(17) 0.0276(15) 0.0324(15) 0.0007(12) 0.0188(13) 0.0048(13) C51 0.046(2) 0.0255(15) 0.0408(17) 0.0024(13) 0.0222(16) 0.0049(14) C52 0.0350(19) 0.042(2) 0.060(2) 0.0145(17) 0.0172(17) 0.0136(16) C53 0.051(2) 0.051(2) 0.0345(18) 0.0207(16) 0.0062(16) 0.0099(18) C54 0.053(2) 0.0384(18) 0.0395(18) 0.0110(14) 0.0250(17) -0.0023(16) C55 0.0384(18) 0.0279(16) 0.0390(17) 0.0003(13) 0.0138(15) -0.0060(14) C56 0.0233(15) 0.0493(19) 0.0194(13) -0.0030(13) 0.0051(12) 0.0044(14) C57 0.0229(16) 0.091(3) 0.0189(14) -0.0036(16) 0.0047(12) 0.0137(17) C58 0.050(2) 0.093(3) 0.0273(17) -0.0094(19) 0.0119(16) 0.032(2) C59 0.042(2) 0.173(5) 0.0340(16) -0.001(2) 0.0192(15) 0.033(2) C60 0.042(2) 0.173(5) 0.0340(16) -0.001(2) 0.0192(15) 0.033(2) C61 0.0273(19) 0.142(4) 0.0260(17) 0.001(2) 0.0116(15) -0.003(2) C62 0.028(2) 0.115(4) 0.054(3) 0.020(3) 0.0003(19) 0.007(2) C63 0.043(2) 0.146(5) 0.0266(19) 0.006(2) 0.0015(18) 0.010(3) C64 0.061(3) 0.172(7) 0.048(3) 0.045(4) 0.005(3) -0.002(4) C65 0.085(4) 0.092(4) 0.079(4) 0.006(3) -0.002(3) 0.027(4) C66 0.050(3) 0.133(5) 0.046(2) 0.025(3) 0.016(2) 0.048(3) N1 0.0334(15) 0.0250(13) 0.0338(14) 0.0025(11) -0.0011(11) 0.0048(11) N2 0.0223(12) 0.0431(15) 0.0211(11) -0.0024(10) 0.0087(10) -0.0095(11) N3 0.0323(15) 0.0252(13) 0.0332(13) -0.0038(10) 0.0046(11) 0.0039(11) N4 0.0364(16) 0.083(2) 0.0265(13) -0.0125(14) 0.0184(12) -0.0268(16) N5 0.0363(15) 0.0364(14) 0.0268(12) -0.0095(10) 0.0169(11) -0.0152(12) N6 0.0448(17) 0.0479(17) 0.0298(14) -0.0169(12) 0.0180(13) -0.0103(14) O1 0.0264(11) 0.0247(10) 0.0267(10) 0.0048(8) 0.0064(9) -0.0004(8) O2 0.0212(10) 0.0249(10) 0.0196(9) -0.0008(7) 0.0070(8) -0.0028(8) O3 0.0260(11) 0.0240(10) 0.0277(10) -0.0009(8) 0.0085(9) 0.0014(8) O4 0.0223(10) 0.0325(11) 0.0241(9) 0.0012(8) 0.0117(8) -0.0047(8) O5 0.0244(10) 0.0275(10) 0.0193(9) -0.0016(7) 0.0094(8) -0.0063(8) O6 0.0265(11) 0.0459(13) 0.0197(9) -0.0012(9) 0.0107(8) -0.0027(9) Fe1 0.0299(2) 0.0248(2) 0.0283(2) 0.00525(16) 0.01356(18) 0.00277(17) Fe2 0.0198(2) 0.01867(19) 0.0299(2) 0.00150(15) 0.00765(17) 0.00109(15) Fe3 0.0279(2) 0.0245(2) 0.0281(2) 0.00031(16) 0.01670(18) -0.00108(17) Fe4 0.0233(2) 0.0286(2) 0.0266(2) -0.00066(16) 0.01225(17) -0.00254(17) Fe5 0.0248(2) 0.0301(2) 0.01906(19) 0.00206(15) 0.00836(16) -0.00153(17) Fe6 0.0273(3) 0.1015(5) 0.0202(2) 0.0000(2) 0.00782(19) 0.0103(3) Co1 0.01897(19) 0.02254(18) 0.01678(17) 0.00071(13) 0.00685(14) -0.00198(14) B1 0.079(4) 0.066(4) 0.055(3) -0.005(3) -0.009(3) -0.004(3) F1 0.080(2) 0.093(2) 0.0543(15) -0.0223(15) 0.0018(14) -0.0138(16) F2A 0.253(9) 0.118(7) 0.036(3) -0.018(3) 0.050(4) -0.027(6) F2B 0.201(17) 0.080(11) 0.063(8) -0.023(8) 0.084(10) -0.013(10) F3 0.108(3) 0.103(3) 0.124(3) -0.009(2) -0.003(2) -0.033(2) F4 0.135(4) 0.135(4) 0.208(6) 0.062(4) 0.023(4) 0.059(3) B2 0.0284(19) 0.065(3) 0.0263(17) 0.0066(17) 0.0085(15) 0.0005(18) F5 0.0275(10) 0.0728(15) 0.0408(11) 0.0062(10) 0.0105(9) 0.0096(10) F6 0.0619(17) 0.122(2) 0.0562(15) -0.0319(15) 0.0242(13) -0.0370(16) F7 0.0499(14) 0.106(2) 0.0341(11) 0.0114(12) 0.0204(10) -0.0056(13) F8 0.0715(18) 0.0847(19) 0.0758(18) 0.0359(14) 0.0345(15) 0.0409(15) O7 0.079(2) 0.0543(17) 0.0703(19) 0.0001(14) 0.0529(17) 0.0045(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.250(3) . ? C1 N1 1.328(4) . ? C1 C2 1.464(4) . ? C2 C6 1.425(4) . ? C2 C3 1.431(4) . ? C2 Fe1 2.011(3) . ? C3 C4 1.415(4) . ? C3 Fe1 2.039(3) . ? C3 H3 0.9800 . ? C4 C5 1.411(5) . ? C4 Fe1 2.048(3) . ? C4 H4 0.9800 . ? C5 C6 1.417(5) . ? C5 Fe1 2.054(3) . ? C5 H5 0.9800 . ? C6 Fe1 2.031(3) . ? C6 H6 0.9800 . ? C7 C11 1.397(6) . ? C7 C8 1.406(6) . ? C7 Fe1 2.024(4) . ? C7 H7 0.9800 . ? C8 C9 1.410(6) . ? C8 Fe1 2.038(4) . ? C8 H8 0.9800 . ? C9 C10 1.418(6) . ? C9 Fe1 2.047(3) . ? C9 H9 0.9800 . ? C10 C11 1.413(6) . ? C10 Fe1 2.036(3) . ? C10 H10 0.9800 . ? C11 Fe1 2.013(4) . ? C11 H11 0.9800 . ? C12 O2 1.263(3) . ? C12 N2 1.317(3) . ? C12 C13 1.467(4) . ? C13 C17 1.430(4) . ? C13 C14 1.432(4) . ? C13 Fe2 2.011(3) . ? C14 C15 1.421(4) . ? C14 Fe2 2.033(3) . ? C14 H14 0.9800 . ? C15 C16 1.414(4) . ? C15 Fe2 2.060(3) . ? C15 H15 0.9800 . ? C16 C17 1.417(4) . ? C16 Fe2 2.064(3) . ? C16 H16 0.9800 . ? C17 Fe2 2.034(3) . ? C17 H17 0.9800 . ? C18 C22 1.409(5) . ? C18 C19 1.417(5) . ? C18 Fe2 2.033(3) . ? C18 H18 0.9800 . ? C19 C20 1.402(6) . ? C19 Fe2 2.041(3) . ? C19 H19 0.9800 . ? C20 C21 1.406(6) . ? C20 Fe2 2.037(3) . ? C20 H20 0.9800 . ? C21 C22 1.424(5) . ? C21 Fe2 2.039(3) . ? C21 H21 0.9800 . ? C22 Fe2 2.049(3) . ? C22 H22 0.9800 . ? C23 O3 1.245(3) . ? C23 N3 1.324(4) . ? C23 C24 1.477(4) . ? C24 C28 1.428(4) . ? C24 C25 1.432(4) . ? C24 Fe3 2.012(3) . ? C25 C26 1.418(4) . ? C25 Fe3 2.030(3) . ? C25 H25 0.9800 . ? C26 C27 1.407(5) . ? C26 Fe3 2.054(3) . ? C26 H26 0.9800 . ? C27 C28 1.424(4) . ? C27 Fe3 2.062(3) . ? C27 H27 0.9800 . ? C28 Fe3 2.037(3) . ? C28 H28 0.9800 . ? C29 C33 1.403(6) . ? C29 C30 1.410(6) . ? C29 Fe3 2.029(3) . ? C29 H29 0.9800 . ? C30 C31 1.418(5) . ? C30 Fe3 2.038(3) . ? C30 H30 0.9800 . ? C31 C32 1.408(5) . ? C31 Fe3 2.031(3) . ? C31 H31 0.9800 . ? C32 C33 1.411(5) . ? C32 Fe3 2.029(3) . ? C32 H32 0.9800 . ? C33 Fe3 2.032(3) . ? C33 H33 0.9800 . ? C34 O4 1.263(3) . ? C34 N4 1.312(4) . ? C34 C35 1.465(4) . ? C35 C36 1.436(4) . ? C35 C39 1.440(4) . ? C35 Fe4 2.001(3) . ? C36 C37 1.420(4) . ? C36 Fe4 2.037(3) . ? C36 H36 0.9800 . ? C37 C38 1.409(4) . ? C37 Fe4 2.054(3) . ? C37 H37 0.9800 . ? C38 C39 1.414(4) . ? C38 Fe4 2.045(3) . ? C38 H38 0.9800 . ? C39 Fe4 2.026(3) . ? C39 H39 0.9800 . ? C40 C41 1.404(5) . ? C40 C44 1.438(5) . ? C40 Fe4 2.042(3) . ? C40 H40 0.9800 . ? C41 C42 1.414(5) . ? C41 Fe4 2.046(3) . ? C41 H41 0.9800 . ? C42 C43 1.413(5) . ? C42 Fe4 2.037(3) . ? C42 H42 0.9800 . ? C43 C44 1.415(6) . ? C43 Fe4 2.028(3) . ? C43 H43 0.9800 . ? C44 Fe4 2.031(3) . ? C44 H44 0.9800 . ? C45 O5 1.259(3) . ? C45 N5 1.321(4) . ? C45 C46 1.460(4) . ? C46 C50 1.428(4) . ? C46 C47 1.430(4) . ? C46 Fe5 2.031(3) . ? C47 C48 1.424(5) . ? C47 Fe5 2.051(3) . ? C47 H47 0.9800 . ? C48 C49 1.403(5) . ? C48 Fe5 2.048(3) . ? C48 H48 0.9800 . ? C49 C50 1.412(4) . ? C49 Fe5 2.046(3) . ? C49 H49 0.9800 . ? C50 Fe5 2.030(3) . ? C50 H50 0.9800 . ? C51 C55 1.407(5) . ? C51 C52 1.409(5) . ? C51 Fe5 2.049(3) . ? C51 H51 0.9800 . ? C52 C53 1.429(5) . ? C52 Fe5 2.040(3) . ? C52 H52 0.9800 . ? C53 C54 1.408(5) . ? C53 Fe5 2.037(3) . ? C53 H53 0.9800 . ? C54 C55 1.411(5) . ? C54 Fe5 2.040(3) . ? C54 H54 0.9800 . ? C55 Fe5 2.048(3) . ? C55 H55 0.9800 . ? C56 O6 1.255(4) . ? C56 N6 1.315(4) . ? C56 C57 1.471(4) . ? C57 C58 1.430(5) . ? C57 C61 1.431(6) . ? C57 Fe6 2.027(3) . ? C58 C59 1.424(6) . ? C58 Fe6 2.035(5) . ? C58 H58 0.9800 . ? C59 C60 1.372(8) . ? C59 Fe6 2.050(5) . ? C59 H59 0.9800 . ? C60 C61 1.430(6) . ? C60 Fe6 2.046(4) . ? C60 H60 0.9800 . ? C61 Fe6 2.017(4) . ? C61 H61 0.9800 . ? C62 C63 1.404(6) . ? C62 C66 1.408(7) . ? C62 Fe6 2.037(4) . ? C62 H62 0.9800 . ? C63 C64 1.356(8) . ? C63 Fe6 2.017(4) . ? C63 H63 0.9800 . ? C64 C65 1.405(9) . ? C64 Fe6 2.008(5) . ? C64 H64 0.9800 . ? C65 C66 1.407(8) . ? C65 Fe6 2.021(6) . ? C65 H65 0.9800 . ? C66 Fe6 2.032(4) . ? C66 H66 0.9800 . ? N1 H1A 0.8600 . ? N1 H1B 0.8600 . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? N5 H5A 0.8600 . ? N5 H5B 0.8600 . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? O1 Co1 2.0576(19) . ? O2 Co1 2.0939(19) . ? O3 Co1 2.0523(19) . ? O4 Co1 2.1306(19) . ? O5 Co1 2.0996(18) . ? O6 Co1 2.1601(19) . ? B1 F2A 1.312(9) . ? B1 F1 1.332(6) . ? B1 F4 1.369(8) . ? B1 F3 1.377(7) . ? B1 F2B 1.431(16) . ? B2 F6 1.345(5) . ? B2 F5 1.376(4) . ? B2 F7 1.389(4) . ? B2 F8 1.393(5) . ? 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 O1 C1 N1 122.7(3) . . ? O1 C1 C2 119.8(3) . . ? N1 C1 C2 117.4(3) . . ? C6 C2 C3 107.7(3) . . ? C6 C2 C1 127.3(3) . . ? C3 C2 C1 124.9(3) . . ? C6 C2 Fe1 70.12(18) . . ? C3 C2 Fe1 70.38(17) . . ? C1 C2 Fe1 123.1(2) . . ? C4 C3 C2 107.4(3) . . ? C4 C3 Fe1 70.08(19) . . ? C2 C3 Fe1 68.26(17) . . ? C4 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? Fe1 C3 H3 126.3 . . ? C5 C4 C3 108.8(3) . . ? C5 C4 Fe1 70.1(2) . . ? C3 C4 Fe1 69.40(17) . . ? C5 C4 H4 125.6 . . ? C3 C4 H4 125.6 . . ? Fe1 C4 H4 125.6 . . ? C4 C5 C6 108.0(3) . . ? C4 C5 Fe1 69.68(19) . . ? C6 C5 Fe1 68.86(19) . . ? C4 C5 H5 126.0 . . ? C6 C5 H5 126.0 . . ? Fe1 C5 H5 126.0 . . ? C5 C6 C2 108.0(3) . . ? C5 C6 Fe1 70.54(19) . . ? C2 C6 Fe1 68.60(17) . . ? C5 C6 H6 126.0 . . ? C2 C6 H6 126.0 . . ? Fe1 C6 H6 126.0 . . ? C11 C7 C8 108.1(4) . . ? C11 C7 Fe1 69.3(2) . . ? C8 C7 Fe1 70.3(2) . . ? C11 C7 H7 125.9 . . ? C8 C7 H7 125.9 . . ? Fe1 C7 H7 125.9 . . ? C7 C8 C9 108.3(4) . . ? C7 C8 Fe1 69.2(2) . . ? C9 C8 Fe1 70.2(2) . . ? C7 C8 H8 125.9 . . ? C9 C8 H8 125.9 . . ? Fe1 C8 H8 125.9 . . ? C8 C9 C10 107.7(4) . . ? C8 C9 Fe1 69.4(2) . . ? C10 C9 Fe1 69.3(2) . . ? C8 C9 H9 126.2 . . ? C10 C9 H9 126.2 . . ? Fe1 C9 H9 126.2 . . ? C11 C10 C9 107.5(4) . . ? C11 C10 Fe1 68.7(2) . . ? C9 C10 Fe1 70.1(2) . . ? C11 C10 H10 126.3 . . ? C9 C10 H10 126.3 . . ? Fe1 C10 H10 126.3 . . ? C7 C11 C10 108.5(4) . . ? C7 C11 Fe1 70.2(2) . . ? C10 C11 Fe1 70.5(2) . . ? C7 C11 H11 125.8 . . ? C10 C11 H11 125.8 . . ? Fe1 C11 H11 125.8 . . ? O2 C12 N2 121.4(2) . . ? O2 C12 C13 119.3(2) . . ? N2 C12 C13 119.3(2) . . ? C17 C13 C14 107.8(2) . . ? C17 C13 C12 123.9(3) . . ? C14 C13 C12 128.0(2) . . ? C17 C13 Fe2 70.17(15) . . ? C14 C13 Fe2 70.09(15) . . ? C12 C13 Fe2 120.26(18) . . ? C15 C14 C13 107.6(3) . . ? C15 C14 Fe2 70.70(16) . . ? C13 C14 Fe2 68.44(15) . . ? C15 C14 H14 126.2 . . ? C13 C14 H14 126.2 . . ? Fe2 C14 H14 126.2 . . ? C16 C15 C14 108.3(3) . . ? C16 C15 Fe2 70.11(17) . . ? C14 C15 Fe2 68.67(16) . . ? C16 C15 H15 125.8 . . ? C14 C15 H15 125.8 . . ? Fe2 C15 H15 125.8 . . ? C15 C16 C17 108.6(3) . . ? C15 C16 Fe2 69.80(17) . . ? C17 C16 Fe2 68.64(16) . . ? C15 C16 H16 125.7 . . ? C17 C16 H16 125.7 . . ? Fe2 C16 H16 125.7 . . ? C16 C17 C13 107.7(3) . . ? C16 C17 Fe2 70.92(16) . . ? C13 C17 Fe2 68.44(15) . . ? C16 C17 H17 126.2 . . ? C13 C17 H17 126.2 . . ? Fe2 C17 H17 126.2 . . ? C22 C18 C19 108.6(3) . . ? C22 C18 Fe2 70.41(19) . . ? C19 C18 Fe2 69.96(18) . . ? C22 C18 H18 125.7 . . ? C19 C18 H18 125.7 . . ? Fe2 C18 H18 125.7 . . ? C20 C19 C18 107.6(4) . . ? C20 C19 Fe2 69.8(2) . . ? C18 C19 Fe2 69.34(18) . . ? C20 C19 H19 126.2 . . ? C18 C19 H19 126.2 . . ? Fe2 C19 H19 126.2 . . ? C19 C20 C21 108.6(3) . . ? C19 C20 Fe2 70.0(2) . . ? C21 C20 Fe2 69.9(2) . . ? C19 C20 H20 125.7 . . ? C21 C20 H20 125.7 . . ? Fe2 C20 H20 125.7 . . ? C20 C21 C22 108.1(3) . . ? C20 C21 Fe2 69.8(2) . . ? C22 C21 Fe2 69.98(19) . . ? C20 C21 H21 126.0 . . ? C22 C21 H21 126.0 . . ? Fe2 C21 H21 126.0 . . ? C18 C22 C21 107.1(3) . . ? C18 C22 Fe2 69.19(19) . . ? C21 C22 Fe2 69.23(19) . . ? C18 C22 H22 126.5 . . ? C21 C22 H22 126.5 . . ? Fe2 C22 H22 126.5 . . ? O3 C23 N3 123.1(3) . . ? O3 C23 C24 119.7(3) . . ? N3 C23 C24 117.2(3) . . ? C28 C24 C25 108.1(3) . . ? C28 C24 C23 127.0(3) . . ? C25 C24 C23 124.3(3) . . ? C28 C24 Fe3 70.28(16) . . ? C25 C24 Fe3 69.90(16) . . ? C23 C24 Fe3 118.2(2) . . ? C26 C25 C24 107.4(3) . . ? C26 C25 Fe3 70.62(18) . . ? C24 C25 Fe3 68.59(17) . . ? C26 C25 H25 126.3 . . ? C24 C25 H25 126.3 . . ? Fe3 C25 H25 126.3 . . ? C27 C26 C25 108.6(3) . . ? C27 C26 Fe3 70.32(18) . . ? C25 C26 Fe3 68.75(17) . . ? C27 C26 H26 125.7 . . ? C25 C26 H26 125.7 . . ? Fe3 C26 H26 125.7 . . ? C26 C27 C28 108.7(3) . . ? C26 C27 Fe3 69.71(18) . . ? C28 C27 Fe3 68.73(16) . . ? C26 C27 H27 125.6 . . ? C28 C27 H27 125.6 . . ? Fe3 C27 H27 125.6 . . ? C27 C28 C24 107.2(3) . . ? C27 C28 Fe3 70.64(18) . . ? C24 C28 Fe3 68.41(16) . . ? C27 C28 H28 126.4 . . ? C24 C28 H28 126.4 . . ? Fe3 C28 H28 126.4 . . ? C33 C29 C30 108.8(3) . . ? C33 C29 Fe3 69.90(19) . . ? C30 C29 Fe3 70.1(2) . . ? C33 C29 H29 125.6 . . ? C30 C29 H29 125.6 . . ? Fe3 C29 H29 125.6 . . ? C29 C30 C31 107.2(3) . . ? C29 C30 Fe3 69.4(2) . . ? C31 C30 Fe3 69.37(19) . . ? C29 C30 H30 126.4 . . ? C31 C30 H30 126.4 . . ? Fe3 C30 H30 126.4 . . ? C32 C31 C30 108.1(3) . . ? C32 C31 Fe3 69.63(19) . . ? C30 C31 Fe3 69.85(19) . . ? C32 C31 H31 125.9 . . ? C30 C31 H31 125.9 . . ? Fe3 C31 H31 125.9 . . ? C31 C32 C33 108.1(3) . . ? C31 C32 Fe3 69.80(19) . . ? C33 C32 Fe3 69.76(19) . . ? C31 C32 H32 125.9 . . ? C33 C32 H32 125.9 . . ? Fe3 C32 H32 125.9 . . ? C29 C33 C32 107.7(3) . . ? C29 C33 Fe3 69.7(2) . . ? C32 C33 Fe3 69.58(19) . . ? C29 C33 H33 126.1 . . ? C32 C33 H33 126.1 . . ? Fe3 C33 H33 126.1 . . ? O4 C34 N4 121.7(3) . . ? O4 C34 C35 119.8(2) . . ? N4 C34 C35 118.5(3) . . ? C36 C35 C39 108.1(3) . . ? C36 C35 C34 124.2(3) . . ? C39 C35 C34 127.2(3) . . ? C36 C35 Fe4 70.55(17) . . ? C39 C35 Fe4 70.00(17) . . ? C34 C35 Fe4 119.0(2) . . ? C37 C36 C35 106.9(3) . . ? C37 C36 Fe4 70.31(18) . . ? C35 C36 Fe4 67.79(16) . . ? C37 C36 H36 126.6 . . ? C35 C36 H36 126.6 . . ? Fe4 C36 H36 126.6 . . ? C38 C37 C36 109.0(3) . . ? C38 C37 Fe4 69.56(18) . . ? C36 C37 Fe4 69.06(17) . . ? C38 C37 H37 125.5 . . ? C36 C37 H37 125.5 . . ? Fe4 C37 H37 125.5 . . ? C37 C38 C39 108.9(3) . . ? C37 C38 Fe4 70.23(18) . . ? C39 C38 Fe4 68.96(17) . . ? C37 C38 H38 125.5 . . ? C39 C38 H38 125.5 . . ? Fe4 C38 H38 125.5 . . ? C38 C39 C35 107.1(3) . . ? C38 C39 Fe4 70.41(18) . . ? C35 C39 Fe4 68.09(16) . . ? C38 C39 H39 126.4 . . ? C35 C39 H39 126.4 . . ? Fe4 C39 H39 126.4 . . ? C41 C40 C44 107.1(3) . . ? C41 C40 Fe4 70.0(2) . . ? C44 C40 Fe4 68.93(19) . . ? C41 C40 H40 126.4 . . ? C44 C40 H40 126.4 . . ? Fe4 C40 H40 126.4 . . ? C40 C41 C42 108.9(3) . . ? C40 C41 Fe4 69.76(19) . . ? C42 C41 Fe4 69.4(2) . . ? C40 C41 H41 125.6 . . ? C42 C41 H41 125.6 . . ? Fe4 C41 H41 125.6 . . ? C43 C42 C41 108.2(3) . . ? C43 C42 Fe4 69.3(2) . . ? C41 C42 Fe4 70.06(19) . . ? C43 C42 H42 125.9 . . ? C41 C42 H42 125.9 . . ? Fe4 C42 H42 125.9 . . ? C42 C43 C44 107.8(3) . . ? C42 C43 Fe4 70.0(2) . . ? C44 C43 Fe4 69.7(2) . . ? C42 C43 H43 126.1 . . ? C44 C43 H43 126.1 . . ? Fe4 C43 H43 126.1 . . ? C43 C44 C40 108.0(3) . . ? C43 C44 Fe4 69.5(2) . . ? C40 C44 Fe4 69.71(19) . . ? C43 C44 H44 126.0 . . ? C40 C44 H44 126.0 . . ? Fe4 C44 H44 126.0 . . ? O5 C45 N5 121.7(2) . . ? O5 C45 C46 120.5(2) . . ? N5 C45 C46 117.8(2) . . ? C50 C46 C47 108.1(3) . . ? C50 C46 C45 125.6(3) . . ? C47 C46 C45 126.3(3) . . ? C50 C46 Fe5 69.39(16) . . ? C47 C46 Fe5 70.24(17) . . ? C45 C46 Fe5 123.8(2) . . ? C48 C47 C46 107.0(3) . . ? C48 C47 Fe5 69.58(18) . . ? C46 C47 Fe5 68.74(16) . . ? C48 C47 H47 126.5 . . ? C46 C47 H47 126.5 . . ? Fe5 C47 H47 126.5 . . ? C49 C48 C47 108.6(3) . . ? C49 C48 Fe5 69.87(18) . . ? C47 C48 Fe5 69.76(18) . . ? C49 C48 H48 125.7 . . ? C47 C48 H48 125.7 . . ? Fe5 C48 H48 125.7 . . ? C48 C49 C50 108.9(3) . . ? C48 C49 Fe5 70.0(2) . . ? C50 C49 Fe5 69.13(17) . . ? C48 C49 H49 125.6 . . ? C50 C49 H49 125.6 . . ? Fe5 C49 H49 125.6 . . ? C49 C50 C46 107.5(3) . . ? C49 C50 Fe5 70.34(19) . . ? C46 C50 Fe5 69.42(16) . . ? C49 C50 H50 126.3 . . ? C46 C50 H50 126.3 . . ? Fe5 C50 H50 126.3 . . ? C55 C51 C52 108.4(3) . . ? C55 C51 Fe5 69.84(18) . . ? C52 C51 Fe5 69.5(2) . . ? C55 C51 H51 125.8 . . ? C52 C51 H51 125.8 . . ? Fe5 C51 H51 125.8 . . ? C51 C52 C53 107.6(3) . . ? C51 C52 Fe5 70.20(19) . . ? C53 C52 Fe5 69.4(2) . . ? C51 C52 H52 126.2 . . ? C53 C52 H52 126.2 . . ? Fe5 C52 H52 126.2 . . ? C54 C53 C52 107.5(3) . . ? C54 C53 Fe5 69.92(19) . . ? C52 C53 Fe5 69.59(19) . . ? C54 C53 H53 126.2 . . ? C52 C53 H53 126.2 . . ? Fe5 C53 H53 126.2 . . ? C53 C54 C55 108.4(3) . . ? C53 C54 Fe5 69.7(2) . . ? C55 C54 Fe5 70.09(18) . . ? C53 C54 H54 125.8 . . ? C55 C54 H54 125.8 . . ? Fe5 C54 H54 125.8 . . ? C51 C55 C54 108.0(3) . . ? C51 C55 Fe5 69.98(18) . . ? C54 C55 Fe5 69.53(19) . . ? C51 C55 H55 126.0 . . ? C54 C55 H55 126.0 . . ? Fe5 C55 H55 126.0 . . ? O6 C56 N6 121.3(3) . . ? O6 C56 C57 120.0(3) . . ? N6 C56 C57 118.7(3) . . ? C58 C57 C61 107.5(3) . . ? C58 C57 C56 127.2(4) . . ? C61 C57 C56 125.2(4) . . ? C58 C57 Fe6 69.7(2) . . ? C61 C57 Fe6 68.9(2) . . ? C56 C57 Fe6 125.3(2) . . ? C59 C58 C57 107.4(5) . . ? C59 C58 Fe6 70.2(3) . . ? C57 C58 Fe6 69.1(2) . . ? C59 C58 H58 126.3 . . ? C57 C58 H58 126.3 . . ? Fe6 C58 H58 126.3 . . ? C60 C59 C58 108.8(4) . . ? C60 C59 Fe6 70.3(3) . . ? C58 C59 Fe6 69.0(2) . . ? C60 C59 H59 125.6 . . ? C58 C59 H59 125.6 . . ? Fe6 C59 H59 125.6 . . ? C59 C60 C61 109.5(5) . . ? C59 C60 Fe6 70.6(3) . . ? C61 C60 Fe6 68.3(2) . . ? C59 C60 H60 125.2 . . ? C61 C60 H60 125.2 . . ? Fe6 C60 H60 125.2 . . ? C60 C61 C57 106.7(5) . . ? C60 C61 Fe6 70.5(2) . . ? C57 C61 Fe6 69.6(2) . . ? C60 C61 H61 126.6 . . ? C57 C61 H61 126.6 . . ? Fe6 C61 H61 126.6 . . ? C63 C62 C66 107.4(5) . . ? C63 C62 Fe6 69.0(2) . . ? C66 C62 Fe6 69.6(3) . . ? C63 C62 H62 126.3 . . ? C66 C62 H62 126.3 . . ? Fe6 C62 H62 126.3 . . ? C64 C63 C62 108.9(5) . . ? C64 C63 Fe6 70.0(3) . . ? C62 C63 Fe6 70.5(2) . . ? C64 C63 H63 125.5 . . ? C62 C63 H63 125.5 . . ? Fe6 C63 H63 125.5 . . ? C63 C64 C65 109.0(6) . . ? C63 C64 Fe6 70.7(3) . . ? C65 C64 Fe6 70.1(3) . . ? C63 C64 H64 125.5 . . ? C65 C64 H64 125.5 . . ? Fe6 C64 H64 125.5 . . ? C64 C65 C66 107.3(6) . . ? C64 C65 Fe6 69.1(4) . . ? C66 C65 Fe6 70.1(3) . . ? C64 C65 H65 126.3 . . ? C66 C65 H65 126.3 . . ? Fe6 C65 H65 126.3 . . ? C65 C66 C62 107.4(5) . . ? C65 C66 Fe6 69.3(3) . . ? C62 C66 Fe6 70.0(3) . . ? C65 C66 H66 126.3 . . ? C62 C66 H66 126.3 . . ? Fe6 C66 H66 126.3 . . ? C1 N1 H1A 120.0 . . ? C1 N1 H1B 120.0 . . ? H1A N1 H1B 120.0 . . ? C12 N2 H2A 120.0 . . ? C12 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C23 N3 H3A 120.0 . . ? C23 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C34 N4 H4A 120.0 . . ? C34 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C45 N5 H5A 120.0 . . ? C45 N5 H5B 120.0 . . ? H5A N5 H5B 120.0 . . ? C56 N6 H6A 120.0 . . ? C56 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C1 O1 Co1 129.90(19) . . ? C12 O2 Co1 136.67(17) . . ? C23 O3 Co1 133.14(19) . . ? C34 O4 Co1 134.53(18) . . ? C45 O5 Co1 137.30(18) . . ? C56 O6 Co1 134.7(2) . . ? C2 Fe1 C11 115.21(15) . . ? C2 Fe1 C7 107.56(14) . . ? C11 Fe1 C7 40.50(17) . . ? C2 Fe1 C6 41.29(13) . . ? C11 Fe1 C6 105.53(17) . . ? C7 Fe1 C6 127.80(16) . . ? C2 Fe1 C10 148.20(15) . . ? C11 Fe1 C10 40.85(17) . . ? C7 Fe1 C10 68.36(17) . . ? C6 Fe1 C10 114.77(16) . . ? C2 Fe1 C8 130.23(14) . . ? C11 Fe1 C8 68.15(18) . . ? C7 Fe1 C8 40.50(17) . . ? C6 Fe1 C8 167.40(16) . . ? C10 Fe1 C8 68.16(17) . . ? C2 Fe1 C3 41.36(12) . . ? C11 Fe1 C3 150.37(15) . . ? C7 Fe1 C3 118.81(14) . . ? C6 Fe1 C3 69.03(14) . . ? C10 Fe1 C3 168.44(15) . . ? C8 Fe1 C3 110.69(15) . . ? C2 Fe1 C9 169.37(15) . . ? C11 Fe1 C9 68.41(17) . . ? C7 Fe1 C9 68.20(16) . . ? C6 Fe1 C9 149.01(15) . . ? C10 Fe1 C9 40.63(16) . . ? C8 Fe1 C9 40.40(16) . . ? C3 Fe1 C9 131.15(15) . . ? C2 Fe1 C4 68.81(12) . . ? C11 Fe1 C4 166.26(17) . . ? C7 Fe1 C4 152.81(17) . . ? C6 Fe1 C4 68.24(14) . . ? C10 Fe1 C4 129.27(16) . . ? C8 Fe1 C4 120.30(16) . . ? C3 Fe1 C4 40.52(13) . . ? C9 Fe1 C4 110.19(15) . . ? C2 Fe1 C5 68.89(13) . . ? C11 Fe1 C5 127.30(18) . . ? C7 Fe1 C5 165.71(18) . . ? C6 Fe1 C5 40.60(13) . . ? C10 Fe1 C5 106.92(17) . . ? C8 Fe1 C5 151.82(16) . . ? C3 Fe1 C5 68.33(15) . . ? C9 Fe1 C5 117.66(16) . . ? C4 Fe1 C5 40.23(15) . . ? C13 Fe2 C18 106.81(13) . . ? C13 Fe2 C14 41.47(11) . . ? C18 Fe2 C14 121.84(13) . . ? C13 Fe2 C17 41.39(10) . . ? C18 Fe2 C17 123.63(13) . . ? C14 Fe2 C17 69.31(11) . . ? C13 Fe2 C20 158.49(15) . . ? C18 Fe2 C20 67.97(14) . . ? C14 Fe2 C20 122.09(15) . . ? C17 Fe2 C20 158.84(15) . . ? C13 Fe2 C21 159.10(15) . . ? C18 Fe2 C21 68.10(15) . . ? C14 Fe2 C21 158.62(14) . . ? C17 Fe2 C21 123.24(14) . . ? C20 Fe2 C21 40.35(16) . . ? C13 Fe2 C19 122.29(14) . . ? C18 Fe2 C19 40.70(14) . . ? C14 Fe2 C19 106.26(14) . . ? C17 Fe2 C19 159.69(14) . . ? C20 Fe2 C19 40.22(16) . . ? C21 Fe2 C19 67.97(16) . . ? C13 Fe2 C22 122.26(13) . . ? C18 Fe2 C22 40.41(15) . . ? C14 Fe2 C22 158.24(13) . . ? C17 Fe2 C22 108.09(13) . . ? C20 Fe2 C22 68.21(15) . . ? C21 Fe2 C22 40.79(14) . . ? C19 Fe2 C22 68.28(15) . . ? C13 Fe2 C15 68.85(11) . . ? C18 Fe2 C15 157.92(14) . . ? C14 Fe2 C15 40.63(11) . . ? C17 Fe2 C15 68.31(12) . . ? C20 Fe2 C15 107.68(14) . . ? C21 Fe2 C15 123.57(14) . . ? C19 Fe2 C15 121.99(14) . . ? C22 Fe2 C15 160.14(14) . . ? C13 Fe2 C16 68.63(11) . . ? C18 Fe2 C16 160.36(14) . . ? C14 Fe2 C16 68.23(11) . . ? C17 Fe2 C16 40.44(11) . . ? C20 Fe2 C16 123.25(14) . . ? C21 Fe2 C16 108.95(14) . . ? C19 Fe2 C16 157.97(14) . . ? C22 Fe2 C16 124.65(14) . . ? C15 Fe2 C16 40.09(12) . . ? C24 Fe3 C29 106.96(13) . . ? C24 Fe3 C32 154.08(14) . . ? C29 Fe3 C32 68.10(15) . . ? C24 Fe3 C25 41.51(12) . . ? C29 Fe3 C25 119.82(15) . . ? C32 Fe3 C25 163.37(13) . . ? C24 Fe3 C31 163.40(14) . . ? C29 Fe3 C31 68.18(15) . . ? C32 Fe3 C31 40.57(14) . . ? C25 Fe3 C31 125.85(14) . . ? C24 Fe3 C33 119.00(14) . . ? C29 Fe3 C33 40.42(16) . . ? C32 Fe3 C33 40.66(15) . . ? C25 Fe3 C33 154.36(14) . . ? C31 Fe3 C33 68.34(14) . . ? C24 Fe3 C28 41.31(12) . . ? C29 Fe3 C28 125.59(15) . . ? C32 Fe3 C28 119.45(14) . . ? C25 Fe3 C28 69.42(13) . . ? C31 Fe3 C28 154.39(14) . . ? C33 Fe3 C28 107.02(14) . . ? C24 Fe3 C30 125.35(14) . . ? C29 Fe3 C30 40.56(16) . . ? C32 Fe3 C30 68.44(15) . . ? C25 Fe3 C30 107.24(14) . . ? C31 Fe3 C30 40.78(15) . . ? C33 Fe3 C30 68.40(16) . . ? C28 Fe3 C30 163.07(14) . . ? C24 Fe3 C26 68.80(12) . . ? C29 Fe3 C26 155.01(17) . . ? C32 Fe3 C26 126.52(14) . . ? C25 Fe3 C26 40.63(12) . . ? C31 Fe3 C26 108.48(14) . . ? C33 Fe3 C26 163.50(15) . . ? C28 Fe3 C26 68.42(13) . . ? C30 Fe3 C26 120.54(16) . . ? C24 Fe3 C27 68.56(12) . . ? C29 Fe3 C27 163.39(17) . . ? C32 Fe3 C27 108.51(14) . . ? C25 Fe3 C27 68.17(13) . . ? C31 Fe3 C27 120.60(14) . . ? C33 Fe3 C27 126.51(15) . . ? C28 Fe3 C27 40.64(12) . . ? C30 Fe3 C27 154.96(16) . . ? C26 Fe3 C27 39.96(14) . . ? C35 Fe4 C39 41.91(11) . . ? C35 Fe4 C43 159.24(14) . . ? C39 Fe4 C43 121.55(14) . . ? C35 Fe4 C44 122.80(15) . . ? C39 Fe4 C44 105.50(14) . . ? C43 Fe4 C44 40.80(16) . . ? C35 Fe4 C42 158.44(13) . . ? C39 Fe4 C42 158.81(14) . . ? C43 Fe4 C42 40.68(15) . . ? C44 Fe4 C42 68.34(16) . . ? C35 Fe4 C36 41.66(11) . . ? C39 Fe4 C36 69.94(12) . . ? C43 Fe4 C36 157.30(15) . . ? C44 Fe4 C36 160.95(15) . . ? C42 Fe4 C36 122.42(14) . . ? C35 Fe4 C40 106.75(13) . . ? C39 Fe4 C40 121.24(13) . . ? C43 Fe4 C40 69.13(15) . . ? C44 Fe4 C40 41.35(14) . . ? C42 Fe4 C40 68.40(16) . . ? C36 Fe4 C40 124.15(13) . . ? C35 Fe4 C38 69.13(12) . . ? C39 Fe4 C38 40.63(12) . . ? C43 Fe4 C38 106.30(14) . . ? C44 Fe4 C38 120.57(14) . . ? C42 Fe4 C38 123.65(15) . . ? C36 Fe4 C38 68.68(12) . . ? C40 Fe4 C38 157.01(14) . . ? C35 Fe4 C41 122.37(13) . . ? C39 Fe4 C41 157.94(14) . . ? C43 Fe4 C41 68.39(14) . . ? C44 Fe4 C41 68.24(14) . . ? C42 Fe4 C41 40.53(14) . . ? C36 Fe4 C41 108.69(13) . . ? C40 Fe4 C41 40.19(14) . . ? C38 Fe4 C41 160.86(14) . . ? C35 Fe4 C37 68.92(13) . . ? C39 Fe4 C37 68.52(12) . . ? C43 Fe4 C37 121.45(15) . . ? C44 Fe4 C37 156.39(14) . . ? C42 Fe4 C37 108.54(15) . . ? C36 Fe4 C37 40.63(12) . . ? C40 Fe4 C37 161.26(14) . . ? C38 Fe4 C37 40.21(12) . . ? C41 Fe4 C37 125.61(14) . . ? C50 Fe5 C46 41.18(12) . . ? C50 Fe5 C53 165.17(15) . . ? C46 Fe5 C53 152.22(15) . . ? C50 Fe5 C52 152.06(14) . . ? C46 Fe5 C52 119.19(14) . . ? C53 Fe5 C52 41.03(15) . . ? C50 Fe5 C54 127.27(14) . . ? C46 Fe5 C54 166.75(13) . . ? C53 Fe5 C54 40.39(15) . . ? C52 Fe5 C54 68.22(15) . . ? C50 Fe5 C49 40.53(12) . . ? C46 Fe5 C49 68.34(12) . . ? C53 Fe5 C49 127.47(15) . . ? C52 Fe5 C49 166.87(15) . . ? C54 Fe5 C49 106.79(14) . . ? C50 Fe5 C55 107.53(13) . . ? C46 Fe5 C55 129.57(12) . . ? C53 Fe5 C55 68.07(15) . . ? C52 Fe5 C55 67.95(15) . . ? C54 Fe5 C55 40.38(13) . . ? C49 Fe5 C55 116.73(14) . . ? C50 Fe5 C48 68.31(14) . . ? C46 Fe5 C48 68.45(12) . . ? C53 Fe5 C48 107.75(16) . . ? C52 Fe5 C48 130.00(17) . . ? C54 Fe5 C48 116.37(14) . . ? C49 Fe5 C48 40.09(15) . . ? C55 Fe5 C48 149.23(14) . . ? C50 Fe5 C51 118.30(13) . . ? C46 Fe5 C51 109.99(12) . . ? C53 Fe5 C51 68.18(15) . . ? C52 Fe5 C51 40.31(14) . . ? C54 Fe5 C51 67.77(14) . . ? C49 Fe5 C51 150.56(15) . . ? C55 Fe5 C51 40.18(13) . . ? C48 Fe5 C51 168.90(15) . . ? C50 Fe5 C47 69.08(13) . . ? C46 Fe5 C47 41.02(11) . . ? C53 Fe5 C47 117.94(15) . . ? C52 Fe5 C47 109.68(15) . . ? C54 Fe5 C47 150.13(13) . . ? C49 Fe5 C47 68.17(15) . . ? C55 Fe5 C47 168.76(13) . . ? C48 Fe5 C47 40.66(13) . . ? C51 Fe5 C47 131.06(14) . . ? C64 Fe6 C63 39.4(2) . . ? C64 Fe6 C61 120.5(2) . . ? C63 Fe6 C61 154.1(2) . . ? C64 Fe6 C65 40.8(3) . . ? C63 Fe6 C65 67.7(2) . . ? C61 Fe6 C65 108.0(2) . . ? C64 Fe6 C57 157.8(3) . . ? C63 Fe6 C57 162.3(2) . . ? C61 Fe6 C57 41.44(17) . . ? C65 Fe6 C57 123.2(2) . . ? C64 Fe6 C66 68.2(2) . . ? C63 Fe6 C66 68.1(2) . . ? C61 Fe6 C66 126.4(2) . . ? C65 Fe6 C66 40.6(2) . . ? C57 Fe6 C66 110.02(16) . . ? C64 Fe6 C58 158.6(2) . . ? C63 Fe6 C58 123.9(2) . . ? C61 Fe6 C58 69.4(2) . . ? C65 Fe6 C58 159.2(2) . . ? C57 Fe6 C58 41.24(15) . . ? C66 Fe6 C58 123.3(2) . . ? C64 Fe6 C62 67.5(2) . . ? C63 Fe6 C62 40.53(19) . . ? C61 Fe6 C62 163.84(18) . . ? C65 Fe6 C62 68.0(2) . . ? C57 Fe6 C62 126.55(18) . . ? C66 Fe6 C62 40.5(2) . . ? C58 Fe6 C62 108.5(2) . . ? C64 Fe6 C60 106.3(2) . . ? C63 Fe6 C60 118.66(18) . . ? C61 Fe6 C60 41.21(16) . . ? C65 Fe6 C60 124.7(3) . . ? C57 Fe6 C60 68.61(16) . . ? C66 Fe6 C60 162.9(3) . . ? C58 Fe6 C60 67.7(2) . . ? C62 Fe6 C60 154.1(2) . . ? C64 Fe6 C59 121.7(2) . . ? C63 Fe6 C59 106.0(2) . . ? C61 Fe6 C59 68.5(2) . . ? C65 Fe6 C59 159.0(3) . . ? C57 Fe6 C59 68.73(15) . . ? C66 Fe6 C59 157.6(3) . . ? C58 Fe6 C59 40.82(17) . . ? C62 Fe6 C59 121.1(2) . . ? C60 Fe6 C59 39.1(2) . . ? O3 Co1 O1 179.45(8) . . ? O3 Co1 O2 87.06(8) . . ? O1 Co1 O2 92.73(8) . . ? O3 Co1 O5 91.81(8) . . ? O1 Co1 O5 87.69(8) . . ? O2 Co1 O5 91.78(7) . . ? O3 Co1 O4 90.95(8) . . ? O1 Co1 O4 89.28(8) . . ? O2 Co1 O4 176.69(8) . . ? O5 Co1 O4 90.93(7) . . ? O3 Co1 O6 89.38(8) . . ? O1 Co1 O6 91.11(8) . . ? O2 Co1 O6 86.56(7) . . ? O5 Co1 O6 177.90(8) . . ? O4 Co1 O6 90.78(7) . . ? F2A B1 F1 120.0(7) . . ? F2A B1 F4 94.1(7) . . ? F1 B1 F4 106.8(5) . . ? F2A B1 F3 118.5(5) . . ? F1 B1 F3 110.5(5) . . ? F4 B1 F3 103.0(6) . . ? F2A B1 F2B 52.0(7) . . ? F1 B1 F2B 91.6(9) . . ? F4 B1 F2B 146.1(11) . . ? F3 B1 F2B 96.4(7) . . ? F6 B2 F5 111.9(3) . . ? F6 B2 F7 111.4(3) . . ? F5 B2 F7 108.1(3) . . ? F6 B2 F8 108.9(3) . . ? F5 B2 F8 108.0(3) . . ? F7 B2 F8 108.4(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.591 _refine_diff_density_min -0.981 _refine_diff_density_rms 0.106 ###Material relevant to compound 3 at 173K ######## data_e316 _database_code_depnum_ccdc_archive 'CCDC 615869' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H66 Co Fe6 N6 O6, 2(B F4)' _chemical_formula_sum 'C66 H66 B2 Co F8 Fe6 N6 O6' _chemical_formula_weight 1606.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' 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 16.8780(6) _cell_length_b 19.5290(8) _cell_length_c 19.3860(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.926(3) _cell_angle_gamma 90.00 _cell_volume 6386.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 17662 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3268 _exptl_absorpt_coefficient_mu 1.659 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8517 _exptl_absorpt_correction_T_max 0.9216 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32722 _diffrn_reflns_av_R_equivalents 0.0961 _diffrn_reflns_av_sigmaI/netI 0.1704 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 29.99 _reflns_number_total 18551 _reflns_number_gt 8621 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0788P)^2^+0.0000P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18551 _refine_ls_number_parameters 842 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1972 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.1969 _refine_ls_wR_factor_gt 0.1583 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.078 _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 Co1 Co 0.40214(4) 0.20468(3) 0.63201(3) 0.02273(17) Uani 1 1 d . . . Fe1 Fe 0.09912(4) 0.06408(4) 0.59925(4) 0.02760(19) Uani 1 1 d . . . C1 C 0.2073(3) 0.0727(3) 0.5585(2) 0.0238(11) Uani 1 1 d . . . C2 C 0.1534(3) 0.1184(3) 0.5246(2) 0.0302(12) Uani 1 1 d . . . H2 H 0.1586 0.1694 0.5228 0.036 Uiso 1 1 calc R . . C3 C 0.0910(3) 0.0797(3) 0.4948(3) 0.0324(13) Uani 1 1 d . . . H3 H 0.0438 0.0987 0.4688 0.039 Uiso 1 1 calc R . . C4 C 0.1045(3) 0.0102(3) 0.5088(2) 0.0308(12) Uani 1 1 d . . . H4 H 0.0692 -0.0287 0.4942 0.037 Uiso 1 1 calc R . . C5 C 0.1771(3) 0.0049(3) 0.5484(2) 0.0287(12) Uani 1 1 d . . . H5 H 0.2022 -0.0384 0.5659 0.034 Uiso 1 1 calc R . . C6 C 0.2798(3) 0.0925(3) 0.5974(2) 0.0236(11) Uani 1 1 d . . . N1 N 0.3222(2) 0.0437(2) 0.6288(2) 0.0296(10) Uani 1 1 d . . . H1A H 0.3666 0.0541 0.6515 0.036 Uiso 1 1 calc R . . H1B H 0.3059 0.0009 0.6270 0.036 Uiso 1 1 calc R . . O1 O 0.30017(19) 0.15449(17) 0.59831(16) 0.0275(8) Uani 1 1 d . . . C7 C 0.0569(4) 0.1304(4) 0.6689(3) 0.0489(17) Uani 1 1 d . . . H7 H 0.0617 0.1814 0.6669 0.059 Uiso 1 1 calc R . . C8 C -0.0059(3) 0.0919(3) 0.6404(3) 0.0376(14) Uani 1 1 d . . . H8 H -0.0535 0.1102 0.6145 0.045 Uiso 1 1 calc R . . C9 C 0.0105(3) 0.0227(3) 0.6549(3) 0.0428(15) Uani 1 1 d . . . H9 H -0.0235 -0.0170 0.6403 0.051 Uiso 1 1 calc R . . C10 C 0.0829(4) 0.0184(4) 0.6923(3) 0.0474(17) Uani 1 1 d . . . H10 H 0.1091 -0.0246 0.7093 0.057 Uiso 1 1 calc R . . C11 C 0.1119(4) 0.0855(4) 0.7021(3) 0.0551(19) Uani 1 1 d . . . H11 H 0.1621 0.0989 0.7275 0.066 Uiso 1 1 calc R . . Fe2 Fe 0.16315(5) 0.41628(4) 0.65527(4) 0.0365(2) Uani 1 1 d . . . C12 C 0.3103(3) 0.3305(3) 0.6884(3) 0.0313(12) Uani 1 1 d . . . C13 C 0.2792(3) 0.3989(3) 0.6758(3) 0.0309(12) Uani 1 1 d . . . C14 C 0.2485(3) 0.4444(3) 0.7259(3) 0.0412(15) Uani 1 1 d . . . H14 H 0.2478 0.4365 0.7768 0.049 Uiso 1 1 calc R . . C15 C 0.2198(3) 0.5040(3) 0.6896(3) 0.0464(16) Uani 1 1 d . . . H15 H 0.1940 0.5447 0.7107 0.056 Uiso 1 1 calc R . . C16 C 0.2330(3) 0.4944(3) 0.6190(3) 0.0452(15) Uani 1 1 d . . . H16 H 0.2180 0.5269 0.5809 0.054 Uiso 1 1 calc R . . C17 C 0.2693(3) 0.4307(3) 0.6112(3) 0.0366(13) Uani 1 1 d . . . H17 H 0.2850 0.4104 0.5663 0.044 Uiso 1 1 calc R . . N2 N 0.3093(3) 0.3048(3) 0.7508(2) 0.0572(16) Uani 1 1 d . . . H2A H 0.3292 0.2638 0.7590 0.069 Uiso 1 1 calc R . . H2B H 0.2889 0.3284 0.7845 0.069 Uiso 1 1 calc R . . O2 O 0.3395(2) 0.29663(17) 0.64028(16) 0.0289(8) Uani 1 1 d . . . C18 C 0.0682(4) 0.3777(5) 0.7072(4) 0.071(2) Uani 1 1 d . . . H18 H 0.0625 0.3758 0.7583 0.085 Uiso 1 1 calc R . . C19 C 0.0426(4) 0.4289(4) 0.6636(4) 0.0617(19) Uani 1 1 d . . . H19 H 0.0166 0.4721 0.6786 0.074 Uiso 1 1 calc R . . C20 C 0.0614(4) 0.4143(5) 0.5966(4) 0.076(2) Uani 1 1 d . . . H20 H 0.0490 0.4435 0.5552 0.091 Uiso 1 1 calc R . . C21 C 0.1008(5) 0.3509(6) 0.5966(5) 0.093(3) Uani 1 1 d . . . H21 H 0.1197 0.3257 0.5554 0.112 Uiso 1 1 calc R . . C22 C 0.1044(5) 0.3282(4) 0.6655(7) 0.097(3) Uani 1 1 d . . . H22 H 0.1280 0.2839 0.6821 0.116 Uiso 1 1 calc R . . Fe3 Fe 0.46187(5) 0.36209(4) 0.38545(4) 0.0340(2) Uani 1 1 d . . . C23 C 0.4027(3) 0.2765(3) 0.4130(2) 0.0300(12) Uani 1 1 d . . . C27 C 0.3622(4) 0.3102(3) 0.3553(3) 0.0375(14) Uani 1 1 d . . . H27 H 0.3068 0.3282 0.3540 0.045 Uiso 1 1 calc R . . C26 C 0.4164(4) 0.3122(3) 0.3009(3) 0.0436(16) Uani 1 1 d . . . H26 H 0.4056 0.3334 0.2546 0.052 Uiso 1 1 calc R . . C25 C 0.4876(4) 0.2816(3) 0.3224(3) 0.0443(16) Uani 1 1 d . . . H25 H 0.5360 0.2770 0.2944 0.053 Uiso 1 1 calc R . . C24 C 0.4804(3) 0.2597(3) 0.3918(3) 0.0397(15) Uani 1 1 d . . . H24 H 0.5225 0.2365 0.4208 0.048 Uiso 1 1 calc R . . C28 C 0.3742(3) 0.2648(3) 0.4819(3) 0.0275(12) Uani 1 1 d . . . N3 N 0.2995(3) 0.2821(2) 0.4946(2) 0.0382(12) Uani 1 1 d . . . H3A H 0.2806 0.2749 0.5357 0.046 Uiso 1 1 calc R . . H3B H 0.2692 0.3006 0.4618 0.046 Uiso 1 1 calc R . . O3 O 0.4187(2) 0.23814(18) 0.52818(16) 0.0294(8) Uani 1 1 d . . . C29 C 0.4580(5) 0.4332(3) 0.4627(3) 0.058(2) Uani 1 1 d . . . H29 H 0.4275 0.4288 0.5059 0.069 Uiso 1 1 calc R . . C30 C 0.5358(4) 0.4121(4) 0.4547(3) 0.0576(19) Uani 1 1 d . . . H30 H 0.5711 0.3902 0.4908 0.069 Uiso 1 1 calc R . . C31 C 0.5565(4) 0.4284(4) 0.3876(4) 0.0594(19) Uani 1 1 d . . . H31 H 0.6091 0.4193 0.3673 0.071 Uiso 1 1 calc R . . C32 C 0.4922(4) 0.4585(3) 0.3535(3) 0.0554(19) Uani 1 1 d . . . H32 H 0.4904 0.4756 0.3048 0.066 Uiso 1 1 calc R . . C33 C 0.4295(4) 0.4616(3) 0.4004(4) 0.0570(19) Uani 1 1 d . . . H33 H 0.3757 0.4817 0.3911 0.068 Uiso 1 1 calc R . . Fe4 Fe 0.71411(5) 0.33625(5) 0.70986(4) 0.0410(2) Uani 1 1 d . . . C34 C 0.5966(3) 0.3252(3) 0.7271(3) 0.0364(14) Uani 1 1 d . . . C35 C 0.6414(3) 0.2745(3) 0.7651(3) 0.0390(14) Uani 1 1 d . . . H35 H 0.6359 0.2237 0.7606 0.047 Uiso 1 1 calc R . . C36 C 0.6944(4) 0.3100(3) 0.8108(3) 0.0448(16) Uani 1 1 d . . . H36 H 0.7341 0.2877 0.8430 0.054 Uiso 1 1 calc R . . C37 C 0.6842(4) 0.3811(3) 0.8028(3) 0.0430(15) Uani 1 1 d . . . H37 H 0.7148 0.4176 0.8282 0.052 Uiso 1 1 calc R . . C38 C 0.6228(3) 0.3918(3) 0.7499(3) 0.0391(14) Uani 1 1 d . . . H38 H 0.6022 0.4369 0.7328 0.047 Uiso 1 1 calc R . . C39 C 0.5333(3) 0.3084(3) 0.6769(3) 0.0387(14) Uani 1 1 d . . . N4 N 0.5021(3) 0.3602(3) 0.6375(3) 0.0623(16) Uani 1 1 d . . . H4A H 0.4642 0.3516 0.6065 0.075 Uiso 1 1 calc R . . H4B H 0.5199 0.4022 0.6432 0.075 Uiso 1 1 calc R . . O4 O 0.5078(2) 0.2495(2) 0.66844(18) 0.0379(9) Uani 1 1 d . . . C40 C 0.7358(4) 0.3102(4) 0.6111(3) 0.0554(19) Uani 1 1 d . . . H40 H 0.6979 0.2872 0.5778 0.066 Uiso 1 1 calc R . . C41 C 0.7914(4) 0.2773(4) 0.6561(3) 0.0551(18) Uani 1 1 d . . . H41 H 0.7988 0.2267 0.6610 0.066 Uiso 1 1 calc R . . C42 C 0.8350(4) 0.3289(3) 0.6935(3) 0.0520(18) Uani 1 1 d . . . H42 H 0.8777 0.3209 0.7297 0.062 Uiso 1 1 calc R . . C43 C 0.8073(4) 0.3940(3) 0.6689(3) 0.0524(18) Uani 1 1 d . . . H43 H 0.8262 0.4399 0.6853 0.063 Uiso 1 1 calc R . . C44 C 0.7462(4) 0.3815(4) 0.6193(3) 0.060(2) Uani 1 1 d . . . H44 H 0.7150 0.4175 0.5938 0.072 Uiso 1 1 calc R . . Fe5 Fe 0.66516(4) 0.03124(4) 0.62874(4) 0.0298(2) Uani 1 1 d . . . C45 C 0.5549(3) 0.0269(3) 0.5856(2) 0.0253(11) Uani 1 1 d . . . C46 C 0.5580(3) -0.0110(3) 0.6489(3) 0.0303(12) Uani 1 1 d . . . H46 H 0.5259 -0.0017 0.6904 0.036 Uiso 1 1 calc R . . C47 C 0.6140(3) -0.0634(3) 0.6425(3) 0.0371(14) Uani 1 1 d . . . H47 H 0.6298 -0.0971 0.6794 0.045 Uiso 1 1 calc R . . C48 C 0.6471(3) -0.0595(3) 0.5761(3) 0.0371(14) Uani 1 1 d . . . H48 H 0.6892 -0.0900 0.5580 0.045 Uiso 1 1 calc R . . C49 C 0.6110(3) -0.0033(3) 0.5409(3) 0.0295(12) Uani 1 1 d . . . H49 H 0.6223 0.0121 0.4930 0.035 Uiso 1 1 calc R . . C50 C 0.5122(3) 0.0916(3) 0.5749(2) 0.0251(11) Uani 1 1 d . . . N5 N 0.5175(3) 0.1243(2) 0.5160(2) 0.0338(11) Uani 1 1 d . . . H5A H 0.4913 0.1628 0.5090 0.041 Uiso 1 1 calc R . . H5B H 0.5472 0.1077 0.4835 0.041 Uiso 1 1 calc R . . O5 O 0.46960(19) 0.11467(17) 0.62252(15) 0.0246(8) Uani 1 1 d . . . C51 C 0.7833(3) 0.0507(4) 0.6320(3) 0.0479(17) Uani 1 1 d . . . H51 H 0.8252 0.0209 0.6125 0.058 Uiso 1 1 calc R . . C52 C 0.7415(4) 0.1028(4) 0.5963(3) 0.0536(18) Uani 1 1 d . . . H52 H 0.7490 0.1163 0.5472 0.064 Uiso 1 1 calc R . . C53 C 0.6860(4) 0.1325(3) 0.6415(3) 0.0452(15) Uani 1 1 d . . . H53 H 0.6483 0.1708 0.6304 0.054 Uiso 1 1 calc R . . C54 C 0.6958(4) 0.0977(3) 0.7062(3) 0.0440(15) Uani 1 1 d . . . H54 H 0.6646 0.1065 0.7482 0.053 Uiso 1 1 calc R . . C55 C 0.7558(3) 0.0478(3) 0.7005(3) 0.0453(16) Uani 1 1 d . . . H55 H 0.7743 0.0151 0.7374 0.054 Uiso 1 1 calc R . . Fe6 Fe 0.41374(4) 0.21768(4) 0.92736(3) 0.0291(2) Uani 1 1 d . . . C56 C 0.3916(3) 0.1449(3) 0.8543(2) 0.0263(12) Uani 1 1 d . . . C57 C 0.4288(3) 0.1150(3) 0.9143(2) 0.0308(12) Uani 1 1 d . . . H57 H 0.4806 0.0900 0.9161 0.037 Uiso 1 1 calc R . . C58 C 0.3797(3) 0.1264(3) 0.9701(3) 0.0374(14) Uani 1 1 d . . . H58 H 0.3907 0.1116 1.0188 0.045 Uiso 1 1 calc R . . C59 C 0.3128(3) 0.1626(3) 0.9458(3) 0.0356(14) Uani 1 1 d . . . H59 H 0.2682 0.1783 0.9746 0.043 Uiso 1 1 calc R . . C60 C 0.3191(3) 0.1746(3) 0.8744(2) 0.0306(12) Uani 1 1 d . . . H60 H 0.2797 0.1990 0.8436 0.037 Uiso 1 1 calc R . . C61 C 0.4222(3) 0.1487(3) 0.7836(2) 0.0267(12) Uani 1 1 d . . . N6 N 0.4928(2) 0.1216(2) 0.7721(2) 0.0317(11) Uani 1 1 d . . . H6A H 0.5110 0.1213 0.7301 0.038 Uiso 1 1 calc R . . H6B H 0.5213 0.1039 0.8065 0.038 Uiso 1 1 calc R . . O6 O 0.37996(19) 0.17437(18) 0.73545(16) 0.0274(8) Uani 1 1 d . . . C62 C 0.5239(4) 0.2569(3) 0.9473(3) 0.0467(16) Uani 1 1 d . . . H62 H 0.5750 0.2309 0.9472 0.056 Uiso 1 1 calc R . . C63 C 0.4756(4) 0.2661(3) 1.0041(3) 0.0436(15) Uani 1 1 d . . . H63 H 0.4865 0.2476 1.0515 0.052 Uiso 1 1 calc R . . C64 C 0.4092(4) 0.3062(3) 0.9832(3) 0.0420(15) Uani 1 1 d . . . H64 H 0.3651 0.3209 1.0130 0.050 Uiso 1 1 calc R . . C65 C 0.4173(4) 0.3224(3) 0.9137(3) 0.0454(16) Uani 1 1 d . . . H65 H 0.3789 0.3499 0.8846 0.054 Uiso 1 1 calc R . . C66 C 0.4877(4) 0.2913(3) 0.8906(3) 0.0490(17) Uani 1 1 d . . . H66 H 0.5082 0.2938 0.8429 0.059 Uiso 1 1 calc R . . B1 B 0.1724(5) 0.4284(4) 0.4052(4) 0.0493(19) Uani 1 1 d . . . F1 F 0.1771(3) 0.3585(2) 0.4153(2) 0.0831(9) Uiso 1 1 d D . . F2 F 0.2372(6) 0.4467(5) 0.3587(5) 0.0831(9) Uiso 0.50 1 d P . . F3 F 0.1048(8) 0.4430(8) 0.3672(6) 0.0831(9) Uiso 0.50 1 d P . . F4 F 0.1879(6) 0.4635(5) 0.4615(5) 0.0831(9) Uiso 0.50 1 d P . . B2 B 0.6706(4) 0.1579(4) 0.3940(3) 0.0417(17) Uani 1 1 d . . . F5 F 0.6580(2) 0.20534(18) 0.34259(17) 0.0537(10) Uani 1 1 d . . . F6 F 0.7406(2) 0.1238(2) 0.3803(2) 0.0723(12) Uani 1 1 d . . . F7 F 0.6107(2) 0.10973(19) 0.39310(17) 0.0603(11) Uani 1 1 d . . . F8 F 0.6748(3) 0.1899(2) 0.45731(17) 0.0734(13) Uani 1 1 d . . . F4A F 0.2391(6) 0.4544(5) 0.3911(4) 0.0831(9) Uiso 0.50 1 d PD . . F2A F 0.1345(6) 0.4603(4) 0.4614(4) 0.0831(9) Uiso 0.50 1 d PD . . F3A F 0.1135(7) 0.4385(8) 0.3548(5) 0.0831(9) Uiso 0.50 1 d PD . . 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 Co1 0.0212(4) 0.0251(4) 0.0220(3) -0.0018(3) 0.0021(3) 0.0000(3) Fe1 0.0222(4) 0.0345(5) 0.0261(4) -0.0022(3) 0.0011(3) -0.0009(3) C1 0.018(3) 0.030(3) 0.023(2) -0.001(2) 0.002(2) -0.002(2) C2 0.033(3) 0.034(3) 0.024(3) 0.000(2) 0.002(2) 0.001(3) C3 0.028(3) 0.042(4) 0.027(3) 0.000(3) -0.001(2) 0.002(3) C4 0.030(3) 0.033(3) 0.029(3) -0.009(2) 0.001(2) -0.004(2) C5 0.029(3) 0.026(3) 0.032(3) 0.000(2) 0.004(2) 0.001(2) C6 0.018(3) 0.034(3) 0.019(2) 0.001(2) 0.009(2) -0.001(2) N1 0.027(2) 0.029(3) 0.033(2) 0.005(2) -0.0021(19) -0.003(2) O1 0.0232(19) 0.028(2) 0.0310(19) 0.0043(16) -0.0011(15) 0.0003(16) C7 0.050(4) 0.055(4) 0.043(4) -0.021(3) 0.020(3) -0.004(3) C8 0.029(3) 0.049(4) 0.035(3) -0.006(3) 0.010(3) 0.007(3) C9 0.038(4) 0.058(4) 0.033(3) -0.001(3) 0.008(3) -0.006(3) C10 0.040(4) 0.072(5) 0.030(3) 0.013(3) 0.009(3) 0.010(3) C11 0.040(4) 0.102(6) 0.023(3) -0.015(4) 0.003(3) -0.013(4) Fe2 0.0344(5) 0.0351(5) 0.0395(4) -0.0018(4) -0.0051(4) 0.0037(4) C12 0.030(3) 0.035(3) 0.029(3) -0.002(3) -0.002(2) 0.005(3) C13 0.029(3) 0.028(3) 0.036(3) -0.001(2) -0.005(2) 0.002(2) C14 0.043(4) 0.040(4) 0.040(3) -0.010(3) -0.010(3) 0.010(3) C15 0.046(4) 0.028(3) 0.064(4) -0.017(3) -0.012(3) 0.010(3) C16 0.041(4) 0.028(3) 0.066(4) 0.010(3) -0.001(3) 0.006(3) C17 0.040(3) 0.028(3) 0.041(3) -0.001(3) 0.002(3) -0.004(3) N2 0.083(4) 0.059(4) 0.031(3) 0.008(3) 0.018(3) 0.044(3) O2 0.037(2) 0.027(2) 0.0234(17) -0.0024(15) 0.0041(16) 0.0041(16) C18 0.039(4) 0.087(6) 0.087(6) 0.027(5) 0.002(4) -0.006(4) C19 0.042(4) 0.075(5) 0.067(5) 0.005(4) -0.013(4) 0.009(4) C20 0.047(5) 0.102(7) 0.077(6) 0.005(5) -0.026(4) -0.013(5) C21 0.051(5) 0.111(9) 0.118(8) -0.058(7) -0.008(5) -0.031(6) C22 0.047(5) 0.046(5) 0.196(11) 0.026(7) -0.025(6) -0.023(4) Fe3 0.0391(5) 0.0342(5) 0.0290(4) 0.0025(4) 0.0066(4) -0.0017(4) C23 0.043(3) 0.026(3) 0.021(3) 0.002(2) 0.002(2) 0.001(2) C27 0.049(4) 0.032(3) 0.031(3) 0.005(3) -0.002(3) -0.001(3) C26 0.072(5) 0.037(4) 0.022(3) 0.001(3) 0.002(3) -0.007(3) C25 0.068(5) 0.030(3) 0.036(3) 0.003(3) 0.023(3) 0.011(3) C24 0.045(4) 0.034(3) 0.040(3) 0.007(3) 0.012(3) 0.008(3) C28 0.029(3) 0.023(3) 0.030(3) -0.003(2) 0.002(2) -0.004(2) N3 0.033(3) 0.055(3) 0.027(2) 0.010(2) 0.002(2) 0.010(2) O3 0.026(2) 0.035(2) 0.0271(18) 0.0051(17) 0.0064(16) 0.0079(17) C29 0.085(6) 0.048(4) 0.042(4) -0.009(3) 0.022(4) -0.030(4) C30 0.060(5) 0.062(5) 0.050(4) -0.008(3) -0.011(4) -0.018(4) C31 0.047(4) 0.064(5) 0.068(5) -0.008(4) 0.013(4) -0.014(4) C32 0.076(5) 0.041(4) 0.051(4) 0.000(3) 0.020(4) -0.017(4) C33 0.062(5) 0.033(4) 0.077(5) -0.013(4) 0.019(4) -0.008(3) Fe4 0.0369(5) 0.0439(5) 0.0424(5) -0.0015(4) 0.0034(4) -0.0078(4) C34 0.026(3) 0.044(4) 0.040(3) -0.001(3) -0.001(2) -0.008(3) C35 0.039(3) 0.038(4) 0.040(3) 0.003(3) 0.007(3) -0.011(3) C36 0.040(4) 0.057(4) 0.037(3) 0.006(3) -0.006(3) -0.010(3) C37 0.051(4) 0.040(4) 0.038(3) 0.001(3) -0.003(3) -0.009(3) C38 0.037(3) 0.041(4) 0.039(3) 0.001(3) 0.001(3) -0.003(3) C39 0.030(3) 0.047(4) 0.039(3) 0.001(3) -0.001(3) -0.004(3) N4 0.074(4) 0.045(4) 0.066(4) 0.022(3) -0.030(3) -0.018(3) O4 0.031(2) 0.036(2) 0.047(2) -0.0011(19) -0.0059(17) -0.0077(18) C40 0.064(5) 0.068(5) 0.035(3) -0.003(3) 0.019(3) -0.006(4) C41 0.057(5) 0.047(4) 0.063(4) -0.003(4) 0.015(4) -0.005(4) C42 0.037(4) 0.057(5) 0.062(4) -0.020(4) 0.011(3) -0.009(3) C43 0.061(5) 0.042(4) 0.055(4) -0.006(3) 0.016(4) -0.009(3) C44 0.075(5) 0.054(5) 0.054(4) 0.011(4) 0.032(4) -0.003(4) Fe5 0.0239(4) 0.0375(5) 0.0281(4) 0.0018(3) 0.0030(3) 0.0018(3) C45 0.024(3) 0.025(3) 0.027(3) 0.001(2) 0.002(2) 0.002(2) C46 0.024(3) 0.033(3) 0.034(3) 0.005(2) 0.005(2) 0.000(2) C47 0.034(3) 0.036(3) 0.041(3) 0.010(3) -0.001(3) 0.000(3) C48 0.040(3) 0.033(3) 0.039(3) -0.005(3) 0.006(3) 0.010(3) C49 0.028(3) 0.033(3) 0.028(3) -0.004(2) 0.002(2) 0.002(2) C50 0.025(3) 0.027(3) 0.023(3) -0.005(2) 0.000(2) -0.008(2) N5 0.043(3) 0.033(3) 0.026(2) 0.006(2) 0.012(2) 0.009(2) O5 0.0233(18) 0.028(2) 0.0222(17) -0.0002(15) 0.0036(14) 0.0030(15) C51 0.025(3) 0.070(5) 0.049(4) -0.004(3) 0.006(3) -0.003(3) C52 0.038(4) 0.069(5) 0.054(4) 0.000(4) 0.006(3) -0.032(4) C53 0.039(4) 0.035(4) 0.061(4) -0.010(3) -0.008(3) -0.005(3) C54 0.039(4) 0.052(4) 0.040(3) -0.009(3) -0.004(3) -0.005(3) C55 0.027(3) 0.057(4) 0.051(4) -0.005(3) -0.006(3) -0.003(3) Fe6 0.0335(5) 0.0309(5) 0.0230(4) -0.0042(3) 0.0007(3) 0.0000(3) C56 0.035(3) 0.023(3) 0.021(2) -0.002(2) 0.002(2) -0.005(2) C57 0.041(3) 0.025(3) 0.025(3) 0.001(2) -0.001(2) 0.002(2) C58 0.052(4) 0.038(3) 0.023(3) 0.000(2) 0.004(3) 0.000(3) C59 0.044(4) 0.040(3) 0.024(3) -0.005(3) 0.013(3) -0.009(3) C60 0.037(3) 0.028(3) 0.026(3) 0.000(2) 0.007(2) -0.006(2) C61 0.033(3) 0.023(3) 0.024(3) -0.003(2) -0.001(2) -0.009(2) N6 0.026(2) 0.045(3) 0.023(2) 0.002(2) 0.0022(19) 0.007(2) O6 0.025(2) 0.031(2) 0.0261(18) -0.0003(16) 0.0022(15) 0.0063(16) C62 0.033(3) 0.045(4) 0.062(4) -0.013(3) -0.006(3) -0.002(3) C63 0.057(4) 0.041(4) 0.032(3) -0.011(3) -0.014(3) -0.001(3) C64 0.039(4) 0.037(4) 0.050(4) -0.021(3) 0.005(3) 0.001(3) C65 0.052(4) 0.033(4) 0.050(4) 0.002(3) -0.015(3) -0.004(3) C66 0.055(4) 0.045(4) 0.047(4) -0.016(3) 0.009(3) -0.026(3) B1 0.063(5) 0.041(5) 0.044(4) -0.004(4) -0.001(4) 0.014(4) B2 0.046(4) 0.044(4) 0.036(4) 0.010(3) 0.006(3) -0.003(3) F5 0.055(2) 0.056(2) 0.051(2) 0.0175(18) 0.0061(17) 0.0063(18) F6 0.052(2) 0.087(3) 0.078(3) 0.024(2) 0.006(2) 0.034(2) F7 0.073(3) 0.061(3) 0.048(2) -0.0105(19) 0.0253(19) -0.023(2) F8 0.108(4) 0.074(3) 0.038(2) -0.009(2) 0.012(2) -0.028(3) _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 Co1 O1 2.067(3) . ? Co1 O4 2.089(4) . ? Co1 O2 2.093(3) . ? Co1 O5 2.106(3) . ? Co1 O6 2.136(3) . ? Co1 O3 2.143(3) . ? Fe1 C7 2.018(5) . ? Fe1 C1 2.021(4) . ? Fe1 C5 2.032(5) . ? Fe1 C2 2.036(5) . ? Fe1 C10 2.040(5) . ? Fe1 C9 2.041(5) . ? Fe1 C8 2.041(5) . ? Fe1 C11 2.042(5) . ? Fe1 C3 2.047(5) . ? Fe1 C4 2.049(5) . ? C1 C2 1.420(7) . ? C1 C5 1.431(7) . ? C1 C6 1.467(7) . ? C2 C3 1.405(7) . ? C2 H2 1.0000 . ? C3 C4 1.401(7) . ? C3 H3 1.0000 . ? C4 C5 1.428(7) . ? C4 H4 1.0000 . ? C5 H5 1.0000 . ? C6 O1 1.257(6) . ? C6 N1 1.328(6) . ? N1 H1A 0.8800 . ? N1 H1B 0.8800 . ? C7 C8 1.397(8) . ? C7 C11 1.416(9) . ? C7 H7 1.0000 . ? C8 C9 1.406(8) . ? C8 H8 1.0000 . ? C9 C10 1.402(8) . ? C9 H9 1.0000 . ? C10 C11 1.410(9) . ? C10 H10 1.0000 . ? C11 H11 1.0000 . ? Fe2 C21 1.987(8) . ? Fe2 C22 1.999(7) . ? Fe2 C13 2.014(5) . ? Fe2 C20 2.028(7) . ? Fe2 C14 2.029(6) . ? Fe2 C17 2.030(5) . ? Fe2 C19 2.061(7) . ? Fe2 C15 2.062(6) . ? Fe2 C18 2.063(7) . ? Fe2 C16 2.065(6) . ? C12 O2 1.259(6) . ? C12 N2 1.310(6) . ? C12 C13 1.452(7) . ? C13 C17 1.403(7) . ? C13 C14 1.426(7) . ? C14 C15 1.436(8) . ? C14 H14 1.0000 . ? C15 C16 1.407(8) . ? C15 H15 1.0000 . ? C16 C17 1.397(8) . ? C16 H16 1.0000 . ? C17 H17 1.0000 . ? N2 H2A 0.8800 . ? N2 H2B 0.8800 . ? C18 C19 1.370(10) . ? C18 C22 1.413(12) . ? C18 H18 1.0000 . ? C19 C20 1.377(10) . ? C19 H19 1.0000 . ? C20 C21 1.405(12) . ? C20 H20 1.0000 . ? C21 C22 1.407(12) . ? C21 H21 1.0000 . ? C22 H22 1.0000 . ? Fe3 C24 2.028(6) . ? Fe3 C23 2.028(5) . ? Fe3 C27 2.032(6) . ? Fe3 C26 2.035(6) . ? Fe3 C33 2.042(6) . ? Fe3 C29 2.045(6) . ? Fe3 C25 2.047(5) . ? Fe3 C30 2.049(6) . ? Fe3 C32 2.053(6) . ? Fe3 C31 2.056(7) . ? C23 C24 1.425(7) . ? C23 C27 1.449(7) . ? C23 C28 1.453(6) . ? C27 C26 1.420(7) . ? C27 H27 1.0000 . ? C26 C25 1.394(8) . ? C26 H26 1.0000 . ? C25 C24 1.420(7) . ? C25 H25 1.0000 . ? C24 H24 1.0000 . ? C28 O3 1.263(6) . ? C28 N3 1.336(6) . ? N3 H3A 0.8800 . ? N3 H3B 0.8800 . ? C29 C30 1.390(9) . ? C29 C33 1.401(10) . ? C29 H29 1.0000 . ? C30 C31 1.394(9) . ? C30 H30 1.0000 . ? C31 C32 1.384(10) . ? C31 H31 1.0000 . ? C32 C33 1.419(8) . ? C32 H32 1.0000 . ? C33 H33 1.0000 . ? Fe4 C40 2.027(6) . ? Fe4 C34 2.034(5) . ? Fe4 C35 2.048(5) . ? Fe4 C41 2.050(6) . ? Fe4 C44 2.053(6) . ? Fe4 C38 2.059(6) . ? Fe4 C36 2.062(6) . ? Fe4 C37 2.081(6) . ? Fe4 C42 2.081(6) . ? Fe4 C43 2.112(6) . ? C34 C35 1.434(8) . ? C34 C38 1.438(8) . ? C34 C39 1.459(8) . ? C35 C36 1.418(8) . ? C35 H35 1.0000 . ? C36 C37 1.407(8) . ? C36 H36 1.0000 . ? C37 C38 1.449(8) . ? C37 H37 1.0000 . ? C38 H38 1.0000 . ? C39 O4 1.237(6) . ? C39 N4 1.361(7) . ? N4 H4A 0.8800 . ? N4 H4B 0.8800 . ? C40 C44 1.410(9) . ? C40 C41 1.415(9) . ? C40 H40 1.0000 . ? C41 C42 1.431(9) . ? C41 H41 1.0000 . ? C42 C43 1.432(9) . ? C42 H42 1.0000 . ? C43 C44 1.408(10) . ? C43 H43 1.0000 . ? C44 H44 1.0000 . ? Fe5 C52 2.016(6) . ? Fe5 C45 2.017(5) . ? Fe5 C49 2.021(5) . ? Fe5 C53 2.023(6) . ? Fe5 C51 2.029(6) . ? Fe5 C46 2.037(5) . ? Fe5 C54 2.038(6) . ? Fe5 C55 2.058(6) . ? Fe5 C47 2.061(6) . ? Fe5 C48 2.062(6) . ? C45 C46 1.432(7) . ? C45 C49 1.434(6) . ? C45 C50 1.467(7) . ? C46 C47 1.403(7) . ? C46 H46 1.0000 . ? C47 C48 1.423(7) . ? C47 H47 1.0000 . ? C48 C49 1.418(7) . ? C48 H48 1.0000 . ? C49 H49 1.0000 . ? C50 O5 1.271(5) . ? C50 N5 1.314(6) . ? N5 H5A 0.8800 . ? N5 H5B 0.8800 . ? C51 C52 1.406(9) . ? C51 C55 1.423(8) . ? C51 H51 1.0000 . ? C52 C53 1.428(8) . ? C52 H52 1.0000 . ? C53 C54 1.432(8) . ? C53 H53 1.0000 . ? C54 C55 1.413(8) . ? C54 H54 1.0000 . ? C55 H55 1.0000 . ? Fe6 C63 2.023(6) . ? Fe6 C56 2.032(5) . ? Fe6 C62 2.036(6) . ? Fe6 C57 2.039(5) . ? Fe6 C64 2.042(5) . ? Fe6 C66 2.048(6) . ? Fe6 C60 2.051(5) . ? Fe6 C58 2.055(6) . ? Fe6 C59 2.056(5) . ? Fe6 C65 2.063(6) . ? C56 C60 1.420(7) . ? C56 C57 1.427(7) . ? C56 C61 1.482(6) . ? C57 C58 1.404(7) . ? C57 H57 1.0000 . ? C58 C59 1.399(8) . ? C58 H58 1.0000 . ? C59 C60 1.412(7) . ? C59 H59 1.0000 . ? C60 H60 1.0000 . ? C61 O6 1.260(6) . ? C61 N6 1.329(6) . ? N6 H6A 0.8800 . ? N6 H6B 0.8800 . ? C62 C63 1.403(8) . ? C62 C66 1.410(9) . ? C62 H62 1.0000 . ? C63 C64 1.415(8) . ? C63 H63 1.0000 . ? C64 C65 1.396(8) . ? C64 H64 1.0000 . ? C65 C66 1.421(8) . ? C65 H65 1.0000 . ? C66 H66 1.0000 . ? B1 F4A 1.273(11) . ? B1 F4 1.308(11) . ? B1 F3 1.368(15) . ? B1 F1 1.379(8) . ? B1 F3A 1.385(14) . ? B1 F2A 1.425(10) . ? B1 F2 1.485(12) . ? B2 F5 1.373(7) . ? B2 F8 1.377(8) . ? B2 F7 1.380(7) . ? B2 F6 1.390(8) . ? 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 O1 Co1 O4 176.40(14) . . ? O1 Co1 O2 90.78(14) . . ? O4 Co1 O2 92.43(15) . . ? O1 Co1 O5 91.34(13) . . ? O4 Co1 O5 85.49(14) . . ? O2 Co1 O5 177.47(13) . . ? O1 Co1 O6 89.71(13) . . ? O4 Co1 O6 88.48(14) . . ? O2 Co1 O6 93.50(12) . . ? O5 Co1 O6 87.88(12) . . ? O1 Co1 O3 88.92(13) . . ? O4 Co1 O3 93.04(14) . . ? O2 Co1 O3 83.83(12) . . ? O5 Co1 O3 94.84(12) . . ? O6 Co1 O3 176.98(13) . . ? C7 Fe1 C1 123.5(2) . . ? C7 Fe1 C5 159.9(2) . . ? C1 Fe1 C5 41.35(19) . . ? C7 Fe1 C2 108.6(2) . . ? C1 Fe1 C2 41.0(2) . . ? C5 Fe1 C2 68.8(2) . . ? C7 Fe1 C10 68.2(3) . . ? C1 Fe1 C10 122.1(2) . . ? C5 Fe1 C10 106.8(2) . . ? C2 Fe1 C10 159.0(2) . . ? C7 Fe1 C9 67.6(2) . . ? C1 Fe1 C9 158.1(2) . . ? C5 Fe1 C9 122.0(2) . . ? C2 Fe1 C9 159.6(2) . . ? C10 Fe1 C9 40.2(2) . . ? C7 Fe1 C8 40.3(2) . . ? C1 Fe1 C8 159.8(2) . . ? C5 Fe1 C8 157.8(2) . . ? C2 Fe1 C8 123.8(2) . . ? C10 Fe1 C8 68.1(2) . . ? C9 Fe1 C8 40.3(2) . . ? C7 Fe1 C11 40.8(3) . . ? C1 Fe1 C11 107.3(2) . . ? C5 Fe1 C11 122.8(3) . . ? C2 Fe1 C11 123.5(3) . . ? C10 Fe1 C11 40.4(3) . . ? C9 Fe1 C11 67.7(2) . . ? C8 Fe1 C11 68.2(2) . . ? C7 Fe1 C3 123.6(3) . . ? C1 Fe1 C3 68.5(2) . . ? C5 Fe1 C3 68.2(2) . . ? C2 Fe1 C3 40.3(2) . . ? C10 Fe1 C3 158.9(3) . . ? C9 Fe1 C3 123.8(2) . . ? C8 Fe1 C3 108.5(2) . . ? C11 Fe1 C3 159.5(3) . . ? C7 Fe1 C4 158.2(3) . . ? C1 Fe1 C4 69.0(2) . . ? C5 Fe1 C4 41.0(2) . . ? C2 Fe1 C4 68.0(2) . . ? C10 Fe1 C4 122.9(3) . . ? C9 Fe1 C4 107.7(2) . . ? C8 Fe1 C4 122.4(2) . . ? C11 Fe1 C4 159.1(3) . . ? C3 Fe1 C4 40.0(2) . . ? C2 C1 C5 107.4(4) . . ? C2 C1 C6 125.6(5) . . ? C5 C1 C6 127.0(5) . . ? C2 C1 Fe1 70.1(3) . . ? C5 C1 Fe1 69.7(3) . . ? C6 C1 Fe1 124.8(3) . . ? C3 C2 C1 108.2(5) . . ? C3 C2 Fe1 70.3(3) . . ? C1 C2 Fe1 68.9(3) . . ? C3 C2 H2 125.9 . . ? C1 C2 H2 125.9 . . ? Fe1 C2 H2 125.9 . . ? C4 C3 C2 109.1(5) . . ? C4 C3 Fe1 70.1(3) . . ? C2 C3 Fe1 69.4(3) . . ? C4 C3 H3 125.5 . . ? C2 C3 H3 125.5 . . ? Fe1 C3 H3 125.5 . . ? C3 C4 C5 107.8(5) . . ? C3 C4 Fe1 69.9(3) . . ? C5 C4 Fe1 68.9(3) . . ? C3 C4 H4 126.1 . . ? C5 C4 H4 126.1 . . ? Fe1 C4 H4 126.1 . . ? C4 C5 C1 107.6(5) . . ? C4 C5 Fe1 70.2(3) . . ? C1 C5 Fe1 68.9(3) . . ? C4 C5 H5 126.2 . . ? C1 C5 H5 126.2 . . ? Fe1 C5 H5 126.2 . . ? O1 C6 N1 122.8(5) . . ? O1 C6 C1 118.9(5) . . ? N1 C6 C1 118.3(5) . . ? C6 N1 H1A 120.0 . . ? C6 N1 H1B 120.0 . . ? H1A N1 H1B 120.0 . . ? C6 O1 Co1 133.2(3) . . ? C8 C7 C11 108.9(6) . . ? C8 C7 Fe1 70.8(3) . . ? C11 C7 Fe1 70.5(3) . . ? C8 C7 H7 125.5 . . ? C11 C7 H7 125.5 . . ? Fe1 C7 H7 125.5 . . ? C7 C8 C9 107.2(6) . . ? C7 C8 Fe1 69.0(3) . . ? C9 C8 Fe1 69.8(3) . . ? C7 C8 H8 126.4 . . ? C9 C8 H8 126.4 . . ? Fe1 C8 H8 126.4 . . ? C10 C9 C8 108.9(6) . . ? C10 C9 Fe1 69.9(3) . . ? C8 C9 Fe1 69.9(3) . . ? C10 C9 H9 125.6 . . ? C8 C9 H9 125.6 . . ? Fe1 C9 H9 125.6 . . ? C9 C10 C11 107.8(6) . . ? C9 C10 Fe1 69.9(3) . . ? C11 C10 Fe1 69.9(3) . . ? C9 C10 H10 126.1 . . ? C11 C10 H10 126.1 . . ? Fe1 C10 H10 126.1 . . ? C10 C11 C7 107.1(6) . . ? C10 C11 Fe1 69.7(3) . . ? C7 C11 Fe1 68.7(3) . . ? C10 C11 H11 126.4 . . ? C7 C11 H11 126.4 . . ? Fe1 C11 H11 126.4 . . ? C21 Fe2 C22 41.3(4) . . ? C21 Fe2 C13 119.8(3) . . ? C22 Fe2 C13 108.5(3) . . ? C21 Fe2 C20 40.9(3) . . ? C22 Fe2 C20 68.0(4) . . ? C13 Fe2 C20 155.1(3) . . ? C21 Fe2 C14 155.5(4) . . ? C22 Fe2 C14 120.6(4) . . ? C13 Fe2 C14 41.3(2) . . ? C20 Fe2 C14 162.2(3) . . ? C21 Fe2 C17 107.8(3) . . ? C22 Fe2 C17 127.5(4) . . ? C13 Fe2 C17 40.6(2) . . ? C20 Fe2 C17 120.6(3) . . ? C14 Fe2 C17 68.3(2) . . ? C21 Fe2 C19 67.5(3) . . ? C22 Fe2 C19 66.5(3) . . ? C13 Fe2 C19 163.8(2) . . ? C20 Fe2 C19 39.3(3) . . ? C14 Fe2 C19 126.5(3) . . ? C17 Fe2 C19 154.7(3) . . ? C21 Fe2 C15 161.7(4) . . ? C22 Fe2 C15 155.4(4) . . ? C13 Fe2 C15 68.8(2) . . ? C20 Fe2 C15 124.9(3) . . ? C14 Fe2 C15 41.1(2) . . ? C17 Fe2 C15 67.3(2) . . ? C19 Fe2 C15 108.9(3) . . ? C21 Fe2 C18 68.9(4) . . ? C22 Fe2 C18 40.7(3) . . ? C13 Fe2 C18 127.4(3) . . ? C20 Fe2 C18 67.0(3) . . ? C14 Fe2 C18 108.3(3) . . ? C17 Fe2 C18 165.2(3) . . ? C19 Fe2 C18 38.8(3) . . ? C15 Fe2 C18 120.3(3) . . ? C21 Fe2 C16 125.2(4) . . ? C22 Fe2 C16 163.7(4) . . ? C13 Fe2 C16 68.3(2) . . ? C20 Fe2 C16 107.8(3) . . ? C14 Fe2 C16 68.3(2) . . ? C17 Fe2 C16 39.9(2) . . ? C19 Fe2 C16 121.0(3) . . ? C15 Fe2 C16 39.9(2) . . ? C18 Fe2 C16 153.8(3) . . ? O2 C12 N2 120.0(5) . . ? O2 C12 C13 120.5(5) . . ? N2 C12 C13 119.5(5) . . ? C17 C13 C14 107.3(5) . . ? C17 C13 C12 126.0(5) . . ? C14 C13 C12 126.6(5) . . ? C17 C13 Fe2 70.3(3) . . ? C14 C13 Fe2 69.9(3) . . ? C12 C13 Fe2 122.1(4) . . ? C13 C14 C15 107.2(5) . . ? C13 C14 Fe2 68.8(3) . . ? C15 C14 Fe2 70.7(3) . . ? C13 C14 H14 126.4 . . ? C15 C14 H14 126.4 . . ? Fe2 C14 H14 126.4 . . ? C16 C15 C14 107.8(5) . . ? C16 C15 Fe2 70.2(3) . . ? C14 C15 Fe2 68.2(3) . . ? C16 C15 H15 126.1 . . ? C14 C15 H15 126.1 . . ? Fe2 C15 H15 126.1 . . ? C17 C16 C15 108.0(5) . . ? C17 C16 Fe2 68.7(3) . . ? C15 C16 Fe2 69.9(3) . . ? C17 C16 H16 126.0 . . ? C15 C16 H16 126.0 . . ? Fe2 C16 H16 126.0 . . ? C16 C17 C13 109.7(5) . . ? C16 C17 Fe2 71.4(3) . . ? C13 C17 Fe2 69.1(3) . . ? C16 C17 H17 125.2 . . ? C13 C17 H17 125.2 . . ? Fe2 C17 H17 125.2 . . ? C12 N2 H2A 120.0 . . ? C12 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C12 O2 Co1 136.0(3) . . ? C19 C18 C22 106.2(8) . . ? C19 C18 Fe2 70.5(4) . . ? C22 C18 Fe2 67.2(4) . . ? C19 C18 H18 126.9 . . ? C22 C18 H18 126.9 . . ? Fe2 C18 H18 126.9 . . ? C18 C19 C20 110.7(8) . . ? C18 C19 Fe2 70.7(4) . . ? C20 C19 Fe2 69.0(4) . . ? C18 C19 H19 124.6 . . ? C20 C19 H19 124.6 . . ? Fe2 C19 H19 124.6 . . ? C19 C20 C21 107.9(8) . . ? C19 C20 Fe2 71.6(4) . . ? C21 C20 Fe2 68.0(4) . . ? C19 C20 H20 126.1 . . ? C21 C20 H20 126.1 . . ? Fe2 C20 H20 126.1 . . ? C20 C21 C22 106.5(8) . . ? C20 C21 Fe2 71.1(5) . . ? C22 C21 Fe2 69.8(5) . . ? C20 C21 H21 126.7 . . ? C22 C21 H21 126.7 . . ? Fe2 C21 H21 126.7 . . ? C21 C22 C18 108.8(8) . . ? C21 C22 Fe2 68.9(5) . . ? C18 C22 Fe2 72.1(4) . . ? C21 C22 H22 125.6 . . ? C18 C22 H22 125.6 . . ? Fe2 C22 H22 125.6 . . ? C24 Fe3 C23 41.1(2) . . ? C24 Fe3 C27 69.5(2) . . ? C23 Fe3 C27 41.8(2) . . ? C24 Fe3 C26 68.2(2) . . ? C23 Fe3 C26 69.0(2) . . ? C27 Fe3 C26 40.9(2) . . ? C24 Fe3 C33 166.3(2) . . ? C23 Fe3 C33 127.7(2) . . ? C27 Fe3 C33 107.0(3) . . ? C26 Fe3 C33 118.3(3) . . ? C24 Fe3 C29 129.3(3) . . ? C23 Fe3 C29 109.8(2) . . ? C27 Fe3 C29 120.2(3) . . ? C26 Fe3 C29 153.5(3) . . ? C33 Fe3 C29 40.1(3) . . ? C24 Fe3 C25 40.8(2) . . ? C23 Fe3 C25 68.9(2) . . ? C27 Fe3 C25 68.6(2) . . ? C26 Fe3 C25 39.9(2) . . ? C33 Fe3 C25 151.5(3) . . ? C29 Fe3 C25 166.2(3) . . ? C24 Fe3 C30 110.0(3) . . ? C23 Fe3 C30 121.0(2) . . ? C27 Fe3 C30 154.9(2) . . ? C26 Fe3 C30 163.8(3) . . ? C33 Fe3 C30 67.3(3) . . ? C29 Fe3 C30 39.7(3) . . ? C25 Fe3 C30 128.3(3) . . ? C24 Fe3 C32 152.1(2) . . ? C23 Fe3 C32 164.9(3) . . ? C27 Fe3 C32 125.7(3) . . ? C26 Fe3 C32 106.7(3) . . ? C33 Fe3 C32 40.5(2) . . ? C29 Fe3 C32 67.2(2) . . ? C25 Fe3 C32 117.7(2) . . ? C30 Fe3 C32 66.9(3) . . ? C24 Fe3 C31 120.2(3) . . ? C23 Fe3 C31 154.6(3) . . ? C27 Fe3 C31 162.7(3) . . ? C26 Fe3 C31 126.1(2) . . ? C33 Fe3 C31 67.0(3) . . ? C29 Fe3 C31 66.5(3) . . ? C25 Fe3 C31 108.4(3) . . ? C30 Fe3 C31 39.7(2) . . ? C32 Fe3 C31 39.4(3) . . ? C24 C23 C27 107.2(4) . . ? C24 C23 C28 124.5(5) . . ? C27 C23 C28 128.2(5) . . ? C24 C23 Fe3 69.4(3) . . ? C27 C23 Fe3 69.2(3) . . ? C28 C23 Fe3 123.5(4) . . ? C26 C27 C23 106.7(5) . . ? C26 C27 Fe3 69.7(3) . . ? C23 C27 Fe3 69.0(3) . . ? C26 C27 H27 126.6 . . ? C23 C27 H27 126.6 . . ? Fe3 C27 H27 126.6 . . ? C25 C26 C27 109.6(5) . . ? C25 C26 Fe3 70.5(3) . . ? C27 C26 Fe3 69.5(3) . . ? C25 C26 H26 125.2 . . ? C27 C26 H26 125.2 . . ? Fe3 C26 H26 125.2 . . ? C26 C25 C24 108.2(5) . . ? C26 C25 Fe3 69.6(3) . . ? C24 C25 Fe3 68.9(3) . . ? C26 C25 H25 125.9 . . ? C24 C25 H25 125.9 . . ? Fe3 C25 H25 125.9 . . ? C25 C24 C23 108.3(5) . . ? C25 C24 Fe3 70.3(3) . . ? C23 C24 Fe3 69.4(3) . . ? C25 C24 H24 125.9 . . ? C23 C24 H24 125.9 . . ? Fe3 C24 H24 125.9 . . ? O3 C28 N3 121.0(4) . . ? O3 C28 C23 120.7(5) . . ? N3 C28 C23 118.3(5) . . ? C28 N3 H3A 120.0 . . ? C28 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C28 O3 Co1 134.4(3) . . ? C30 C29 C33 108.6(6) . . ? C30 C29 Fe3 70.3(4) . . ? C33 C29 Fe3 69.8(4) . . ? C30 C29 H29 125.7 . . ? C33 C29 H29 125.7 . . ? Fe3 C29 H29 125.7 . . ? C29 C30 C31 107.7(7) . . ? C29 C30 Fe3 70.0(4) . . ? C31 C30 Fe3 70.4(4) . . ? C29 C30 H30 126.1 . . ? C31 C30 H30 126.1 . . ? Fe3 C30 H30 126.1 . . ? C32 C31 C30 109.0(6) . . ? C32 C31 Fe3 70.2(4) . . ? C30 C31 Fe3 69.9(4) . . ? C32 C31 H31 125.5 . . ? C30 C31 H31 125.5 . . ? Fe3 C31 H31 125.5 . . ? C31 C32 C33 107.5(6) . . ? C31 C32 Fe3 70.4(4) . . ? C33 C32 Fe3 69.3(3) . . ? C31 C32 H32 126.2 . . ? C33 C32 H32 126.2 . . ? Fe3 C32 H32 126.2 . . ? C29 C33 C32 107.1(7) . . ? C29 C33 Fe3 70.1(4) . . ? C32 C33 Fe3 70.1(4) . . ? C29 C33 H33 126.4 . . ? C32 C33 H33 126.4 . . ? Fe3 C33 H33 126.4 . . ? C40 Fe4 C34 109.7(3) . . ? C40 Fe4 C35 118.5(3) . . ? C34 Fe4 C35 41.1(2) . . ? C40 Fe4 C41 40.6(3) . . ? C34 Fe4 C41 131.6(3) . . ? C35 Fe4 C41 109.7(3) . . ? C40 Fe4 C44 40.4(3) . . ? C34 Fe4 C44 118.2(3) . . ? C35 Fe4 C44 151.6(3) . . ? C41 Fe4 C44 67.5(3) . . ? C40 Fe4 C38 130.5(3) . . ? C34 Fe4 C38 41.1(2) . . ? C35 Fe4 C38 69.1(2) . . ? C41 Fe4 C38 170.1(3) . . ? C44 Fe4 C38 108.6(3) . . ? C40 Fe4 C36 151.0(3) . . ? C34 Fe4 C36 68.1(2) . . ? C35 Fe4 C36 40.4(2) . . ? C41 Fe4 C36 117.9(3) . . ? C44 Fe4 C36 167.0(3) . . ? C38 Fe4 C36 68.0(2) . . ? C40 Fe4 C37 168.7(3) . . ? C34 Fe4 C37 68.7(2) . . ? C35 Fe4 C37 68.1(2) . . ? C41 Fe4 C37 148.6(3) . . ? C44 Fe4 C37 129.6(3) . . ? C38 Fe4 C37 41.0(2) . . ? C36 Fe4 C37 39.7(2) . . ? C40 Fe4 C42 68.3(3) . . ? C34 Fe4 C42 169.9(3) . . ? C35 Fe4 C42 130.3(3) . . ? C41 Fe4 C42 40.5(2) . . ? C44 Fe4 C42 67.2(3) . . ? C38 Fe4 C42 147.6(2) . . ? C36 Fe4 C42 108.5(3) . . ? C37 Fe4 C42 115.4(2) . . ? C40 Fe4 C43 67.6(3) . . ? C34 Fe4 C43 149.4(3) . . ? C35 Fe4 C43 167.9(3) . . ? C41 Fe4 C43 67.3(3) . . ? C44 Fe4 C43 39.5(3) . . ? C38 Fe4 C43 115.9(2) . . ? C36 Fe4 C43 129.5(3) . . ? C37 Fe4 C43 107.8(2) . . ? C42 Fe4 C43 39.9(2) . . ? C35 C34 C38 108.4(5) . . ? C35 C34 C39 123.3(5) . . ? C38 C34 C39 128.3(6) . . ? C35 C34 Fe4 70.0(3) . . ? C38 C34 Fe4 70.4(3) . . ? C39 C34 Fe4 127.6(4) . . ? C36 C35 C34 107.1(5) . . ? C36 C35 Fe4 70.3(3) . . ? C34 C35 Fe4 68.9(3) . . ? C36 C35 H35 126.4 . . ? C34 C35 H35 126.4 . . ? Fe4 C35 H35 126.4 . . ? C37 C36 C35 109.9(6) . . ? C37 C36 Fe4 70.9(3) . . ? C35 C36 Fe4 69.3(3) . . ? C37 C36 H36 125.0 . . ? C35 C36 H36 125.0 . . ? Fe4 C36 H36 125.0 . . ? C36 C37 C38 107.6(5) . . ? C36 C37 Fe4 69.4(3) . . ? C38 C37 Fe4 68.7(3) . . ? C36 C37 H37 126.2 . . ? C38 C37 H37 126.2 . . ? Fe4 C37 H37 126.2 . . ? C34 C38 C37 107.0(5) . . ? C34 C38 Fe4 68.5(3) . . ? C37 C38 Fe4 70.3(3) . . ? C34 C38 H38 126.5 . . ? C37 C38 H38 126.5 . . ? Fe4 C38 H38 126.5 . . ? O4 C39 N4 119.4(5) . . ? O4 C39 C34 122.8(6) . . ? N4 C39 C34 117.9(6) . . ? C39 N4 H4A 120.0 . . ? C39 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C39 O4 Co1 136.4(4) . . ? C44 C40 C41 107.5(7) . . ? C44 C40 Fe4 70.8(4) . . ? C41 C40 Fe4 70.6(4) . . ? C44 C40 H40 126.2 . . ? C41 C40 H40 126.2 . . ? Fe4 C40 H40 126.2 . . ? C40 C41 C42 108.2(6) . . ? C40 C41 Fe4 68.8(4) . . ? C42 C41 Fe4 70.9(3) . . ? C40 C41 H41 125.9 . . ? C42 C41 H41 125.9 . . ? Fe4 C41 H41 125.9 . . ? C41 C42 C43 107.4(6) . . ? C41 C42 Fe4 68.6(4) . . ? C43 C42 Fe4 71.2(4) . . ? C41 C42 H42 126.3 . . ? C43 C42 H42 126.3 . . ? Fe4 C42 H42 126.3 . . ? C44 C43 C42 107.3(6) . . ? C44 C43 Fe4 68.0(4) . . ? C42 C43 Fe4 68.9(3) . . ? C44 C43 H43 126.3 . . ? C42 C43 H43 126.3 . . ? Fe4 C43 H43 126.3 . . ? C43 C44 C40 109.5(7) . . ? C43 C44 Fe4 72.5(4) . . ? C40 C44 Fe4 68.8(3) . . ? C43 C44 H44 125.2 . . ? C40 C44 H44 125.2 . . ? Fe4 C44 H44 125.2 . . ? C52 Fe5 C45 119.4(2) . . ? C52 Fe5 C49 104.1(2) . . ? C45 Fe5 C49 41.59(18) . . ? C52 Fe5 C53 41.4(2) . . ? C45 Fe5 C53 104.3(2) . . ? C49 Fe5 C53 120.1(2) . . ? C52 Fe5 C51 40.7(3) . . ? C45 Fe5 C51 156.0(2) . . ? C49 Fe5 C51 120.3(2) . . ? C53 Fe5 C51 69.3(3) . . ? C52 Fe5 C46 157.1(3) . . ? C45 Fe5 C46 41.37(19) . . ? C49 Fe5 C46 69.4(2) . . ? C53 Fe5 C46 121.6(2) . . ? C51 Fe5 C46 161.4(2) . . ? C52 Fe5 C54 68.9(2) . . ? C45 Fe5 C54 122.7(2) . . ? C49 Fe5 C54 158.4(2) . . ? C53 Fe5 C54 41.3(2) . . ? C51 Fe5 C54 68.5(2) . . ? C46 Fe5 C54 108.7(2) . . ? C52 Fe5 C55 68.5(3) . . ? C45 Fe5 C55 160.3(2) . . ? C49 Fe5 C55 157.8(2) . . ? C53 Fe5 C55 69.0(3) . . ? C51 Fe5 C55 40.7(2) . . ? C46 Fe5 C55 125.3(2) . . ? C54 Fe5 C55 40.4(2) . . ? C52 Fe5 C47 159.5(3) . . ? C45 Fe5 C47 68.4(2) . . ? C49 Fe5 C47 68.3(2) . . ? C53 Fe5 C47 158.9(2) . . ? C51 Fe5 C47 125.4(3) . . ? C46 Fe5 C47 40.0(2) . . ? C54 Fe5 C47 124.9(2) . . ? C55 Fe5 C47 111.0(2) . . ? C52 Fe5 C48 121.8(2) . . ? C45 Fe5 C48 68.9(2) . . ? C49 Fe5 C48 40.6(2) . . ? C53 Fe5 C48 157.3(2) . . ? C51 Fe5 C48 107.8(2) . . ? C46 Fe5 C48 68.3(2) . . ? C54 Fe5 C48 160.3(2) . . ? C55 Fe5 C48 124.3(2) . . ? C47 Fe5 C48 40.4(2) . . ? C46 C45 C49 107.4(4) . . ? C46 C45 C50 124.8(4) . . ? C49 C45 C50 126.9(4) . . ? C46 C45 Fe5 70.1(3) . . ? C49 C45 Fe5 69.4(3) . . ? C50 C45 Fe5 117.7(3) . . ? C47 C46 C45 107.9(4) . . ? C47 C46 Fe5 70.9(3) . . ? C45 C46 Fe5 68.5(3) . . ? C47 C46 H46 126.1 . . ? C45 C46 H46 126.1 . . ? Fe5 C46 H46 126.1 . . ? C46 C47 C48 109.1(5) . . ? C46 C47 Fe5 69.1(3) . . ? C48 C47 Fe5 69.9(3) . . ? C46 C47 H47 125.4 . . ? C48 C47 H47 125.4 . . ? Fe5 C47 H47 125.4 . . ? C49 C48 C47 107.6(4) . . ? C49 C48 Fe5 68.1(3) . . ? C47 C48 Fe5 69.8(3) . . ? C49 C48 H48 126.2 . . ? C47 C48 H48 126.2 . . ? Fe5 C48 H48 126.2 . . ? C48 C49 C45 108.0(4) . . ? C48 C49 Fe5 71.2(3) . . ? C45 C49 Fe5 69.0(3) . . ? C48 C49 H49 126.0 . . ? C45 C49 H49 126.0 . . ? Fe5 C49 H49 126.0 . . ? O5 C50 N5 121.0(5) . . ? O5 C50 C45 119.3(4) . . ? N5 C50 C45 119.7(4) . . ? C50 N5 H5A 120.0 . . ? C50 N5 H5B 120.0 . . ? H5A N5 H5B 120.0 . . ? C50 O5 Co1 132.8(3) . . ? C52 C51 C55 108.4(5) . . ? C52 C51 Fe5 69.1(3) . . ? C55 C51 Fe5 70.7(3) . . ? C52 C51 H51 125.8 . . ? C55 C51 H51 125.8 . . ? Fe5 C51 H51 125.8 . . ? C51 C52 C53 108.7(5) . . ? C51 C52 Fe5 70.2(3) . . ? C53 C52 Fe5 69.6(3) . . ? C51 C52 H52 125.6 . . ? C53 C52 H52 125.6 . . ? Fe5 C52 H52 125.6 . . ? C52 C53 C54 106.6(6) . . ? C52 C53 Fe5 69.0(3) . . ? C54 C53 Fe5 69.9(3) . . ? C52 C53 H53 126.7 . . ? C54 C53 H53 126.7 . . ? Fe5 C53 H53 126.7 . . ? C55 C54 C53 108.7(5) . . ? C55 C54 Fe5 70.6(3) . . ? C53 C54 Fe5 68.8(3) . . ? C55 C54 H54 125.6 . . ? C53 C54 H54 125.6 . . ? Fe5 C54 H54 125.6 . . ? C54 C55 C51 107.6(6) . . ? C54 C55 Fe5 69.1(3) . . ? C51 C55 Fe5 68.5(3) . . ? C54 C55 H55 126.2 . . ? C51 C55 H55 126.2 . . ? Fe5 C55 H55 126.2 . . ? C63 Fe6 C56 156.6(2) . . ? C63 Fe6 C62 40.4(2) . . ? C56 Fe6 C62 122.7(2) . . ? C63 Fe6 C57 119.2(2) . . ? C56 Fe6 C57 41.1(2) . . ? C62 Fe6 C57 106.0(2) . . ? C63 Fe6 C64 40.7(2) . . ? C56 Fe6 C64 162.2(2) . . ? C62 Fe6 C64 68.4(2) . . ? C57 Fe6 C64 154.9(2) . . ? C63 Fe6 C66 67.8(2) . . ? C56 Fe6 C66 110.4(2) . . ? C62 Fe6 C66 40.4(2) . . ? C57 Fe6 C66 124.6(2) . . ? C64 Fe6 C66 68.0(2) . . ? C63 Fe6 C60 159.1(2) . . ? C56 Fe6 C60 40.70(19) . . ? C62 Fe6 C60 160.1(2) . . ? C57 Fe6 C60 68.4(2) . . ? C64 Fe6 C60 124.8(2) . . ? C66 Fe6 C60 126.0(2) . . ? C63 Fe6 C58 104.7(2) . . ? C56 Fe6 C58 68.10(19) . . ? C62 Fe6 C58 121.0(3) . . ? C57 Fe6 C58 40.10(19) . . ? C64 Fe6 C58 120.3(2) . . ? C66 Fe6 C58 158.6(3) . . ? C60 Fe6 C58 67.8(2) . . ? C63 Fe6 C59 121.8(2) . . ? C56 Fe6 C59 67.75(19) . . ? C62 Fe6 C59 157.0(2) . . ? C57 Fe6 C59 67.3(2) . . ? C64 Fe6 C59 107.7(2) . . ? C66 Fe6 C59 161.1(3) . . ? C60 Fe6 C59 40.23(19) . . ? C58 Fe6 C59 39.8(2) . . ? C63 Fe6 C65 67.3(2) . . ? C56 Fe6 C65 127.5(2) . . ? C62 Fe6 C65 67.8(3) . . ? C57 Fe6 C65 162.7(2) . . ? C64 Fe6 C65 39.8(2) . . ? C66 Fe6 C65 40.4(2) . . ? C60 Fe6 C65 111.6(2) . . ? C58 Fe6 C65 157.0(2) . . ? C59 Fe6 C65 124.6(2) . . ? C60 C56 C57 107.7(4) . . ? C60 C56 C61 124.3(5) . . ? C57 C56 C61 128.0(5) . . ? C60 C56 Fe6 70.4(3) . . ? C57 C56 Fe6 69.7(3) . . ? C61 C56 Fe6 123.2(3) . . ? C58 C57 C56 107.9(5) . . ? C58 C57 Fe6 70.6(3) . . ? C56 C57 Fe6 69.2(3) . . ? C58 C57 H57 126.1 . . ? C56 C57 H57 126.1 . . ? Fe6 C57 H57 126.1 . . ? C59 C58 C57 108.2(5) . . ? C59 C58 Fe6 70.1(3) . . ? C57 C58 Fe6 69.3(3) . . ? C59 C58 H58 125.9 . . ? C57 C58 H58 125.9 . . ? Fe6 C58 H58 125.9 . . ? C58 C59 C60 109.1(5) . . ? C58 C59 Fe6 70.1(3) . . ? C60 C59 Fe6 69.7(3) . . ? C58 C59 H59 125.5 . . ? C60 C59 H59 125.5 . . ? Fe6 C59 H59 125.4 . . ? C59 C60 C56 107.1(5) . . ? C59 C60 Fe6 70.1(3) . . ? C56 C60 Fe6 68.9(3) . . ? C59 C60 H60 126.4 . . ? C56 C60 H60 126.4 . . ? Fe6 C60 H60 126.4 . . ? O6 C61 N6 121.5(4) . . ? O6 C61 C56 119.9(5) . . ? N6 C61 C56 118.5(5) . . ? C61 N6 H6A 120.0 . . ? C61 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C61 O6 Co1 133.9(3) . . ? C63 C62 C66 107.6(5) . . ? C63 C62 Fe6 69.3(3) . . ? C66 C62 Fe6 70.2(3) . . ? C63 C62 H62 126.2 . . ? C66 C62 H62 126.2 . . ? Fe6 C62 H62 126.2 . . ? C62 C63 C64 108.8(5) . . ? C62 C63 Fe6 70.3(3) . . ? C64 C63 Fe6 70.3(3) . . ? C62 C63 H63 125.6 . . ? C64 C63 H63 125.6 . . ? Fe6 C63 H63 125.6 . . ? C65 C64 C63 107.4(5) . . ? C65 C64 Fe6 70.9(3) . . ? C63 C64 Fe6 68.9(3) . . ? C65 C64 H64 126.3 . . ? C63 C64 H64 126.3 . . ? Fe6 C64 H64 126.3 . . ? C64 C65 C66 108.5(6) . . ? C64 C65 Fe6 69.3(3) . . ? C66 C65 Fe6 69.2(3) . . ? C64 C65 H65 125.7 . . ? C66 C65 H65 125.7 . . ? Fe6 C65 H65 125.7 . . ? C62 C66 C65 107.7(5) . . ? C62 C66 Fe6 69.4(3) . . ? C65 C66 Fe6 70.3(3) . . ? C62 C66 H66 126.2 . . ? C65 C66 H66 126.2 . . ? Fe6 C66 H66 126.2 . . ? F4A B1 F4 79.4(8) . . ? F4A B1 F3 121.9(10) . . ? F4 B1 F3 118.6(8) . . ? F4A B1 F1 112.3(7) . . ? F4 B1 F1 113.1(7) . . ? F3 B1 F1 109.0(9) . . ? F4A B1 F3A 114.3(8) . . ? F4 B1 F3A 129.2(9) . . ? F1 B1 F3A 106.1(8) . . ? F4A B1 F2A 114.3(8) . . ? F3 B1 F2A 86.1(7) . . ? F1 B1 F2A 110.4(6) . . ? F3A B1 F2A 98.4(8) . . ? F4 B1 F2 104.5(8) . . ? F3 B1 F2 104.0(8) . . ? F1 B1 F2 106.6(6) . . ? F3A B1 F2 93.7(8) . . ? F2A B1 F2 135.8(8) . . ? F5 B2 F8 110.0(5) . . ? F5 B2 F7 110.8(6) . . ? F8 B2 F7 109.7(5) . . ? F5 B2 F6 107.2(5) . . ? F8 B2 F6 111.7(6) . . ? F7 B2 F6 107.4(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.190 _refine_diff_density_min -1.105 _refine_diff_density_rms 0.130 ###Material relevant to compound 4 at 173K ######## data_s359 _database_code_depnum_ccdc_archive 'CCDC 615870' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H66 Fe6 N6 Ni O6, 2(B F4)' _chemical_formula_sum 'C66 H66 B2 F8 Fe6 N6 Ni O6' _chemical_formula_weight 1606.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' B B 0.0013 0.0007 '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 ' _symmetry_space_group_name_Hall '-P 2yn' 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 16.8422(5) _cell_length_b 19.5610(5) _cell_length_c 19.3563(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.055(2) _cell_angle_gamma 90.00 _cell_volume 6372.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8776 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.21 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3272 _exptl_absorpt_coefficient_mu 1.698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8761 _exptl_absorpt_correction_T_max 0.9199 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 85349 _diffrn_reflns_av_R_equivalents 0.0797 _diffrn_reflns_av_sigmaI/netI 0.0916 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 30.02 _reflns_number_total 18539 _reflns_number_gt 10020 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0966P)^2^+1.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18539 _refine_ls_number_parameters 830 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1263 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1831 _refine_ls_wR_factor_gt 0.1432 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.009 _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 Ni1 Ni 0.40258(3) 0.20491(3) 0.63155(3) 0.02007(12) Uani 1 1 d . . . Fe1 Fe 0.09934(3) 0.06534(3) 0.59899(3) 0.02460(14) Uani 1 1 d . . . C1 C 0.2078(2) 0.0737(2) 0.55776(19) 0.0213(8) Uani 1 1 d . . . C2 C 0.1535(2) 0.1204(2) 0.5239(2) 0.0277(9) Uani 1 1 d . . . H2 H 0.1589 0.1713 0.5219 0.033 Uiso 1 1 calc R . . C3 C 0.0900(3) 0.0808(2) 0.4941(2) 0.0301(10) Uani 1 1 d . . . H3 H 0.0424 0.0993 0.4681 0.036 Uiso 1 1 calc R . . C4 C 0.1050(2) 0.0107(2) 0.5087(2) 0.0290(9) Uani 1 1 d . . . H4 H 0.0698 -0.0284 0.4946 0.035 Uiso 1 1 calc R . . C5 C 0.1774(2) 0.0060(2) 0.5482(2) 0.0270(9) Uani 1 1 d . . . H5 H 0.2027 -0.0371 0.5661 0.032 Uiso 1 1 calc R . . C6 C 0.2804(2) 0.0947(2) 0.59682(19) 0.0212(8) Uani 1 1 d . . . N1 N 0.3225(2) 0.04618(18) 0.62992(18) 0.0269(8) Uani 1 1 d . . . H1A H 0.3665 0.0570 0.6533 0.032 Uiso 1 1 calc R . . H1B H 0.3063 0.0034 0.6283 0.032 Uiso 1 1 calc R . . O1 O 0.30086(15) 0.15664(14) 0.59743(14) 0.0237(6) Uani 1 1 d . . . C7 C 0.0559(3) 0.1337(3) 0.6673(3) 0.0466(14) Uani 1 1 d . . . H7 H 0.0602 0.1846 0.6641 0.056 Uiso 1 1 calc R . . C8 C -0.0070(3) 0.0934(3) 0.6393(2) 0.0349(11) Uani 1 1 d . . . H8 H -0.0548 0.1106 0.6126 0.042 Uiso 1 1 calc R . . C9 C 0.0106(3) 0.0241(3) 0.6550(2) 0.0368(11) Uani 1 1 d . . . H9 H -0.0229 -0.0160 0.6408 0.044 Uiso 1 1 calc R . . C10 C 0.0836(3) 0.0210(3) 0.6928(2) 0.0475(14) Uani 1 1 d . . . H10 H 0.1104 -0.0214 0.7108 0.057 Uiso 1 1 calc R . . C11 C 0.1120(3) 0.0894(4) 0.7016(2) 0.0519(16) Uani 1 1 d . . . H11 H 0.1623 0.1036 0.7266 0.062 Uiso 1 1 calc R . . Fe2 Fe 0.16322(4) 0.41562(4) 0.65422(4) 0.03497(17) Uani 1 1 d . . . C12 C 0.3105(3) 0.3284(2) 0.6878(2) 0.0303(10) Uani 1 1 d . . . C13 C 0.2794(3) 0.3970(2) 0.6747(2) 0.0323(10) Uani 1 1 d . . . C14 C 0.2491(3) 0.4436(3) 0.7252(3) 0.0415(12) Uani 1 1 d . . . H14 H 0.2485 0.4362 0.7763 0.050 Uiso 1 1 calc R . . C15 C 0.2219(3) 0.5023(3) 0.6887(3) 0.0489(14) Uani 1 1 d . . . H15 H 0.1963 0.5430 0.7098 0.059 Uiso 1 1 calc R . . C16 C 0.2333(3) 0.4931(3) 0.6186(3) 0.0475(13) Uani 1 1 d . . . H16 H 0.2180 0.5263 0.5811 0.057 Uiso 1 1 calc R . . C17 C 0.2694(3) 0.4281(2) 0.6090(3) 0.0372(11) Uani 1 1 d . . . H17 H 0.2849 0.4080 0.5639 0.045 Uiso 1 1 calc R . . N2 N 0.3084(3) 0.3030(2) 0.7508(2) 0.0588(15) Uani 1 1 d . . . H2A H 0.3279 0.2621 0.7596 0.071 Uiso 1 1 calc R . . H2B H 0.2874 0.3269 0.7840 0.071 Uiso 1 1 calc R . . O2 O 0.34033(17) 0.29489(15) 0.63959(14) 0.0279(6) Uani 1 1 d . . . C18 C 0.0693(3) 0.3758(4) 0.7061(4) 0.075(2) Uani 1 1 d . . . H18 H 0.0642 0.3741 0.7574 0.090 Uiso 1 1 calc R . . C19 C 0.0422(3) 0.4286(4) 0.6619(4) 0.0610(17) Uani 1 1 d . . . H19 H 0.0156 0.4715 0.6769 0.073 Uiso 1 1 calc R . . C20 C 0.0619(4) 0.4132(4) 0.5944(5) 0.0843(14) Uani 1 1 d . . . H20 H 0.0497 0.4416 0.5524 0.101 Uiso 1 1 calc R . . C21 C 0.0996(4) 0.3482(4) 0.5961(5) 0.0843(14) Uani 1 1 d . . . H21 H 0.1189 0.3227 0.5552 0.101 Uiso 1 1 calc R . . C22 C 0.1059(4) 0.3265(4) 0.6651(5) 0.0843(14) Uani 1 1 d . . . H22 H 0.1302 0.2826 0.6819 0.101 Uiso 1 1 calc R . . Fe3 Fe 0.46247(4) 0.36177(4) 0.38585(3) 0.03136(16) Uani 1 1 d . . . C23 C 0.4034(3) 0.2761(2) 0.4136(2) 0.0287(9) Uani 1 1 d . . . C27 C 0.3631(3) 0.3093(2) 0.3559(2) 0.0357(11) Uani 1 1 d . . . H27 H 0.3074 0.3273 0.3548 0.043 Uiso 1 1 calc R . . C26 C 0.4163(3) 0.3116(3) 0.3009(2) 0.0435(13) Uani 1 1 d . . . H26 H 0.4049 0.3327 0.2545 0.052 Uiso 1 1 calc R . . C25 C 0.4894(4) 0.2808(3) 0.3229(3) 0.0461(13) Uani 1 1 d . . . H25 H 0.5379 0.2764 0.2949 0.055 Uiso 1 1 calc R . . C24 C 0.4821(3) 0.2594(3) 0.3920(3) 0.0418(12) Uani 1 1 d . . . H24 H 0.5245 0.2366 0.4212 0.050 Uiso 1 1 calc R . . C28 C 0.3741(3) 0.2642(2) 0.4830(2) 0.0258(9) Uani 1 1 d . . . N3 N 0.2991(2) 0.2804(2) 0.49495(19) 0.0367(9) Uani 1 1 d . . . H3A H 0.2800 0.2733 0.5361 0.044 Uiso 1 1 calc R . . H3B H 0.2685 0.2980 0.4617 0.044 Uiso 1 1 calc R . . O3 O 0.41999(17) 0.23866(15) 0.52966(14) 0.0254(6) Uani 1 1 d . . . C29 C 0.4564(4) 0.4333(3) 0.4627(3) 0.0533(15) Uani 1 1 d . . . H29 H 0.4250 0.4289 0.5053 0.064 Uiso 1 1 calc R . . C30 C 0.5358(4) 0.4114(3) 0.4557(3) 0.0570(16) Uani 1 1 d . . . H30 H 0.5703 0.3895 0.4925 0.068 Uiso 1 1 calc R . . C31 C 0.5582(3) 0.4268(3) 0.3868(3) 0.0556(16) Uani 1 1 d . . . H31 H 0.6110 0.4175 0.3666 0.067 Uiso 1 1 calc R . . C32 C 0.4929(4) 0.4568(3) 0.3531(3) 0.0516(15) Uani 1 1 d . . . H32 H 0.4907 0.4726 0.3040 0.062 Uiso 1 1 calc R . . C33 C 0.4287(4) 0.4610(3) 0.3999(3) 0.0526(15) Uani 1 1 d . . . H33 H 0.3748 0.4808 0.3896 0.063 Uiso 1 1 calc R . . Fe4 Fe 0.71367(4) 0.33678(4) 0.70894(3) 0.03227(16) Uani 1 1 d . . . C34 C 0.5959(2) 0.3244(2) 0.7263(2) 0.0260(9) Uani 1 1 d . . . C35 C 0.6416(3) 0.2743(2) 0.7643(2) 0.0310(10) Uani 1 1 d . . . H35 H 0.6368 0.2236 0.7591 0.037 Uiso 1 1 calc R . . C36 C 0.6948(3) 0.3090(3) 0.8106(2) 0.0362(11) Uani 1 1 d . . . H36 H 0.7347 0.2869 0.8430 0.043 Uiso 1 1 calc R . . C37 C 0.6837(3) 0.3803(3) 0.8019(2) 0.0363(11) Uani 1 1 d . . . H37 H 0.7141 0.4169 0.8272 0.044 Uiso 1 1 calc R . . C38 C 0.6227(3) 0.3909(2) 0.7498(2) 0.0325(10) Uani 1 1 d . . . H38 H 0.6019 0.4360 0.7331 0.039 Uiso 1 1 calc R . . C39 C 0.5318(3) 0.3083(2) 0.6755(2) 0.0306(10) Uani 1 1 d . . . N4 N 0.4998(3) 0.3594(2) 0.6376(2) 0.0476(12) Uani 1 1 d . . . H4A H 0.4604 0.3511 0.6077 0.057 Uiso 1 1 calc R . . H4B H 0.5182 0.4013 0.6427 0.057 Uiso 1 1 calc R . . O4 O 0.50667(17) 0.24879(15) 0.66924(16) 0.0312(7) Uani 1 1 d . . . C40 C 0.7354(3) 0.3089(3) 0.6090(3) 0.0485(14) Uani 1 1 d . . . H40 H 0.6972 0.2854 0.5762 0.058 Uiso 1 1 calc R . . C41 C 0.7909(3) 0.2764(3) 0.6550(3) 0.0463(13) Uani 1 1 d . . . H41 H 0.7983 0.2259 0.6606 0.056 Uiso 1 1 calc R . . C42 C 0.8343(3) 0.3283(3) 0.6922(3) 0.0464(13) Uani 1 1 d . . . H42 H 0.8774 0.3208 0.7283 0.056 Uiso 1 1 calc R . . C43 C 0.8049(3) 0.3927(3) 0.6681(3) 0.0481(14) Uani 1 1 d . . . H43 H 0.8237 0.4386 0.6844 0.058 Uiso 1 1 calc R . . C44 C 0.7445(3) 0.3803(3) 0.6169(3) 0.0486(14) Uani 1 1 d . . . H44 H 0.7135 0.4160 0.5907 0.058 Uiso 1 1 calc R . . Fe5 Fe 0.66481(3) 0.03192(3) 0.62891(3) 0.02600(15) Uani 1 1 d . . . C45 C 0.5537(2) 0.0287(2) 0.5857(2) 0.0241(8) Uani 1 1 d . . . C46 C 0.5557(2) -0.0096(2) 0.6496(2) 0.0281(9) Uani 1 1 d . . . H46 H 0.5237 0.0001 0.6910 0.034 Uiso 1 1 calc R . . C47 C 0.6124(3) -0.0625(2) 0.6434(2) 0.0339(10) Uani 1 1 d . . . H47 H 0.6280 -0.0960 0.6805 0.041 Uiso 1 1 calc R . . C48 C 0.6460(3) -0.0589(2) 0.5766(2) 0.0346(10) Uani 1 1 d . . . H48 H 0.6879 -0.0897 0.5586 0.042 Uiso 1 1 calc R . . C49 C 0.6097(2) -0.0023(2) 0.5408(2) 0.0293(9) Uani 1 1 d . . . H49 H 0.6211 0.0128 0.4928 0.035 Uiso 1 1 calc R . . C50 C 0.5114(2) 0.0934(2) 0.5745(2) 0.0211(8) Uani 1 1 d . . . N5 N 0.5179(2) 0.1258(2) 0.51561(18) 0.0343(9) Uani 1 1 d . . . H5A H 0.4926 0.1646 0.5084 0.041 Uiso 1 1 calc R . . H5B H 0.5476 0.1086 0.4833 0.041 Uiso 1 1 calc R . . O5 O 0.46920(16) 0.11662(14) 0.62205(13) 0.0217(6) Uani 1 1 d . . . C51 C 0.7842(3) 0.0521(3) 0.6319(3) 0.0426(13) Uani 1 1 d . . . H51 H 0.8265 0.0225 0.6127 0.051 Uiso 1 1 calc R . . C52 C 0.7419(3) 0.1043(3) 0.5962(3) 0.0469(14) Uani 1 1 d . . . H52 H 0.7491 0.1180 0.5471 0.056 Uiso 1 1 calc R . . C53 C 0.6870(3) 0.1340(3) 0.6419(3) 0.0402(12) Uani 1 1 d . . . H53 H 0.6493 0.1723 0.6308 0.048 Uiso 1 1 calc R . . C54 C 0.6965(3) 0.0996(3) 0.7070(3) 0.0404(12) Uani 1 1 d . . . H54 H 0.6658 0.1089 0.7493 0.049 Uiso 1 1 calc R . . C55 C 0.7564(3) 0.0497(3) 0.7008(3) 0.0393(12) Uani 1 1 d . . . H55 H 0.7751 0.0173 0.7378 0.047 Uiso 1 1 calc R . . Fe6 Fe 0.41223(4) 0.21746(3) 0.92577(3) 0.02714(15) Uani 1 1 d . . . C56 C 0.3911(3) 0.1454(2) 0.8518(2) 0.0260(9) Uani 1 1 d . . . C57 C 0.4280(3) 0.1148(2) 0.9125(2) 0.0300(10) Uani 1 1 d . . . H57 H 0.4797 0.0896 0.9150 0.036 Uiso 1 1 calc R . . C58 C 0.3771(3) 0.1267(2) 0.9678(2) 0.0377(11) Uani 1 1 d . . . H58 H 0.3879 0.1123 1.0168 0.045 Uiso 1 1 calc R . . C59 C 0.3108(3) 0.1631(2) 0.9440(2) 0.0360(11) Uani 1 1 d . . . H59 H 0.2663 0.1789 0.9729 0.043 Uiso 1 1 calc R . . C60 C 0.3175(3) 0.1756(2) 0.8719(2) 0.0283(9) Uani 1 1 d . . . H60 H 0.2784 0.2005 0.8411 0.034 Uiso 1 1 calc R . . C61 C 0.4222(2) 0.1492(2) 0.7816(2) 0.0227(8) Uani 1 1 d . . . N6 N 0.4930(2) 0.12310(19) 0.77106(18) 0.0308(8) Uani 1 1 d . . . H6A H 0.5119 0.1232 0.7293 0.037 Uiso 1 1 calc R . . H6B H 0.5213 0.1056 0.8058 0.037 Uiso 1 1 calc R . . O6 O 0.37968(16) 0.17484(14) 0.73318(14) 0.0232(6) Uani 1 1 d . . . C62 C 0.5224(3) 0.2564(3) 0.9467(3) 0.0471(14) Uani 1 1 d . . . H62 H 0.5736 0.2306 0.9463 0.057 Uiso 1 1 calc R . . C63 C 0.4741(3) 0.2654(3) 1.0041(3) 0.0425(12) Uani 1 1 d . . . H63 H 0.4848 0.2469 1.0517 0.051 Uiso 1 1 calc R . . C64 C 0.4078(3) 0.3053(3) 0.9824(3) 0.0412(12) Uani 1 1 d . . . H64 H 0.3632 0.3197 1.0119 0.049 Uiso 1 1 calc R . . C65 C 0.4154(3) 0.3212(3) 0.9122(3) 0.0416(12) Uani 1 1 d . . . H65 H 0.3774 0.3488 0.8828 0.050 Uiso 1 1 calc R . . C66 C 0.4862(3) 0.2910(3) 0.8905(3) 0.0470(14) Uani 1 1 d . . . H66 H 0.5070 0.2936 0.8428 0.056 Uiso 1 1 calc R . . B1 B 0.1714(4) 0.4257(4) 0.4047(3) 0.0493(16) Uani 1 1 d . . . F1 F 0.1772(2) 0.3563(2) 0.4147(2) 0.0791(7) Uiso 1 1 d D . . F2 F 0.2378(5) 0.4462(5) 0.3594(4) 0.0791(7) Uiso 0.50 1 d P . . F3 F 0.1045(7) 0.4419(7) 0.3670(6) 0.0791(7) Uiso 0.50 1 d P . . F4 F 0.1870(5) 0.4623(4) 0.4618(4) 0.0791(7) Uiso 0.50 1 d P . . B2 B 0.6708(3) 0.1578(3) 0.3928(3) 0.0385(13) Uani 1 1 d . . . F5 F 0.65843(18) 0.20453(16) 0.34105(16) 0.0511(8) Uani 1 1 d . . . F6 F 0.7404(2) 0.1225(2) 0.3790(2) 0.0771(12) Uani 1 1 d . . . F7 F 0.6104(2) 0.10980(17) 0.39216(16) 0.0574(9) Uani 1 1 d . . . F8 F 0.6751(2) 0.18936(19) 0.45623(16) 0.0707(11) Uani 1 1 d . . . F4A F 0.2379(5) 0.4527(4) 0.3950(4) 0.0791(7) Uiso 0.50 1 d PD . . F2A F 0.1333(5) 0.4585(4) 0.4616(4) 0.0791(7) Uiso 0.50 1 d PD . . F3A F 0.1131(7) 0.4375(7) 0.3544(5) 0.0791(7) Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0185(2) 0.0204(3) 0.0214(2) -0.0005(2) 0.00175(19) 0.0002(2) Fe1 0.0189(3) 0.0304(3) 0.0245(3) -0.0031(3) 0.0013(2) -0.0017(2) C1 0.0193(19) 0.025(2) 0.0199(18) 0.0023(16) 0.0001(14) 0.0004(16) C2 0.028(2) 0.026(2) 0.028(2) 0.0045(18) 0.0014(17) 0.0009(18) C3 0.024(2) 0.040(3) 0.026(2) -0.0036(19) -0.0034(17) 0.0015(19) C4 0.024(2) 0.033(3) 0.031(2) -0.0084(19) -0.0021(17) -0.0026(18) C5 0.024(2) 0.028(2) 0.029(2) -0.0015(18) 0.0024(17) -0.0006(17) C6 0.0170(18) 0.028(2) 0.0190(18) -0.0007(16) 0.0026(14) 0.0003(16) N1 0.0211(17) 0.028(2) 0.0312(19) 0.0080(15) -0.0024(14) -0.0016(14) O1 0.0204(14) 0.0228(15) 0.0279(15) 0.0003(12) 0.0006(11) -0.0018(11) C7 0.046(3) 0.051(3) 0.044(3) -0.023(3) 0.016(2) -0.009(3) C8 0.022(2) 0.045(3) 0.038(3) -0.005(2) 0.0073(18) 0.006(2) C9 0.026(2) 0.047(3) 0.037(3) 0.002(2) 0.0075(19) -0.007(2) C10 0.036(3) 0.076(4) 0.031(3) 0.019(3) 0.005(2) 0.008(3) C11 0.035(3) 0.097(5) 0.024(2) -0.016(3) 0.003(2) -0.016(3) Fe2 0.0317(4) 0.0307(4) 0.0420(4) -0.0023(3) -0.0064(3) 0.0033(3) C12 0.029(2) 0.029(2) 0.033(2) -0.0047(19) 0.0012(18) 0.0052(18) C13 0.032(2) 0.028(2) 0.036(2) -0.0057(19) 0.0002(19) 0.0033(19) C14 0.040(3) 0.034(3) 0.049(3) -0.015(2) -0.014(2) 0.013(2) C15 0.049(3) 0.031(3) 0.066(4) -0.016(3) -0.012(3) 0.010(2) C16 0.046(3) 0.028(3) 0.068(4) 0.009(3) -0.003(3) 0.001(2) C17 0.036(3) 0.032(3) 0.044(3) 0.003(2) 0.003(2) 0.002(2) N2 0.087(4) 0.056(3) 0.035(2) 0.007(2) 0.023(2) 0.043(3) O2 0.0310(16) 0.0262(16) 0.0265(15) -0.0023(12) 0.0026(12) 0.0055(13) C18 0.032(3) 0.097(6) 0.094(5) 0.046(5) -0.001(3) -0.014(3) C19 0.037(3) 0.068(4) 0.077(4) 0.002(4) -0.004(3) 0.013(3) C20 0.052(2) 0.081(3) 0.118(4) -0.020(3) -0.017(3) -0.017(2) C21 0.052(2) 0.081(3) 0.118(4) -0.020(3) -0.017(3) -0.017(2) C22 0.052(2) 0.081(3) 0.118(4) -0.020(3) -0.017(3) -0.017(2) Fe3 0.0349(4) 0.0322(4) 0.0273(3) 0.0037(3) 0.0054(3) -0.0008(3) C23 0.040(3) 0.022(2) 0.024(2) 0.0006(17) 0.0007(18) -0.0013(18) C27 0.043(3) 0.034(3) 0.030(2) 0.003(2) -0.006(2) -0.007(2) C26 0.069(4) 0.036(3) 0.025(2) 0.002(2) 0.001(2) -0.008(3) C25 0.068(4) 0.035(3) 0.036(3) 0.006(2) 0.019(3) 0.010(3) C24 0.050(3) 0.037(3) 0.039(3) 0.012(2) 0.014(2) 0.015(2) C28 0.029(2) 0.022(2) 0.026(2) 0.0005(17) 0.0030(17) -0.0031(17) N3 0.030(2) 0.050(3) 0.029(2) 0.0115(18) 0.0012(16) 0.0073(18) O3 0.0271(15) 0.0243(16) 0.0249(14) 0.0061(12) 0.0038(12) 0.0034(12) C29 0.071(4) 0.048(3) 0.042(3) -0.009(3) 0.015(3) -0.024(3) C30 0.062(4) 0.060(4) 0.048(3) -0.006(3) -0.013(3) -0.014(3) C31 0.042(3) 0.055(4) 0.071(4) -0.004(3) 0.014(3) -0.015(3) C32 0.067(4) 0.036(3) 0.053(3) 0.002(3) 0.023(3) -0.012(3) C33 0.056(4) 0.029(3) 0.074(4) -0.007(3) 0.014(3) 0.001(2) Fe4 0.0298(3) 0.0326(4) 0.0346(4) -0.0010(3) 0.0035(3) -0.0079(3) C34 0.0187(19) 0.029(2) 0.030(2) -0.0002(18) 0.0024(16) -0.0048(17) C35 0.031(2) 0.030(2) 0.032(2) 0.0016(19) 0.0042(18) -0.0054(19) C36 0.034(3) 0.042(3) 0.032(2) 0.003(2) -0.0039(19) -0.006(2) C37 0.035(3) 0.039(3) 0.035(2) -0.008(2) -0.005(2) -0.009(2) C38 0.029(2) 0.033(3) 0.036(2) -0.001(2) 0.0019(19) -0.0018(19) C39 0.032(2) 0.031(3) 0.029(2) 0.0028(19) 0.0010(18) -0.0043(19) N4 0.051(3) 0.037(3) 0.053(3) 0.013(2) -0.025(2) -0.016(2) O4 0.0276(16) 0.0269(17) 0.0388(17) -0.0021(14) -0.0011(13) -0.0077(13) C40 0.054(3) 0.058(4) 0.035(3) -0.005(3) 0.016(2) -0.015(3) C41 0.041(3) 0.041(3) 0.058(3) -0.011(3) 0.012(3) -0.009(2) C42 0.028(3) 0.047(3) 0.065(4) -0.013(3) 0.011(2) -0.005(2) C43 0.040(3) 0.044(3) 0.061(4) -0.007(3) 0.018(3) -0.012(2) C44 0.052(3) 0.050(3) 0.046(3) 0.012(3) 0.023(3) -0.005(3) Fe5 0.0216(3) 0.0285(3) 0.0281(3) 0.0006(3) 0.0030(2) 0.0016(2) C45 0.021(2) 0.023(2) 0.029(2) -0.0007(17) 0.0041(16) 0.0005(16) C46 0.023(2) 0.031(2) 0.031(2) 0.0048(18) 0.0042(17) -0.0027(18) C47 0.031(2) 0.028(2) 0.042(3) 0.008(2) -0.001(2) 0.0014(19) C48 0.033(2) 0.037(3) 0.033(2) -0.003(2) -0.0017(19) 0.009(2) C49 0.029(2) 0.033(2) 0.026(2) -0.0051(18) 0.0013(17) 0.0079(19) C50 0.0175(18) 0.023(2) 0.0228(19) -0.0021(16) -0.0019(15) -0.0031(15) N5 0.045(2) 0.033(2) 0.0248(18) 0.0060(16) 0.0133(16) 0.0124(18) O5 0.0207(14) 0.0230(15) 0.0217(13) -0.0003(11) 0.0033(11) 0.0040(11) C51 0.019(2) 0.058(4) 0.052(3) -0.005(3) 0.005(2) -0.005(2) C52 0.036(3) 0.054(4) 0.051(3) 0.006(3) 0.004(2) -0.026(3) C53 0.040(3) 0.028(3) 0.052(3) -0.003(2) -0.005(2) -0.004(2) C54 0.032(3) 0.042(3) 0.046(3) -0.009(2) -0.002(2) -0.004(2) C55 0.031(3) 0.046(3) 0.041(3) -0.002(2) -0.007(2) 0.004(2) Fe6 0.0299(3) 0.0285(4) 0.0231(3) -0.0042(3) 0.0020(2) -0.0004(3) C56 0.030(2) 0.023(2) 0.026(2) -0.0058(17) 0.0015(17) -0.0042(17) C57 0.039(3) 0.024(2) 0.027(2) 0.0020(18) -0.0018(18) 0.0024(19) C58 0.054(3) 0.034(3) 0.025(2) 0.004(2) 0.007(2) -0.003(2) C59 0.045(3) 0.034(3) 0.030(2) -0.003(2) 0.016(2) -0.004(2) C60 0.035(2) 0.026(2) 0.024(2) -0.0034(17) 0.0057(17) -0.0025(18) C61 0.026(2) 0.021(2) 0.0212(19) -0.0045(16) 0.0019(16) -0.0032(16) N6 0.030(2) 0.039(2) 0.0239(18) 0.0011(16) 0.0025(15) 0.0109(16) O6 0.0228(14) 0.0257(16) 0.0210(14) -0.0007(12) 0.0008(11) 0.0029(12) C62 0.032(3) 0.042(3) 0.067(4) -0.022(3) -0.006(2) 0.001(2) C63 0.051(3) 0.039(3) 0.037(3) -0.011(2) -0.009(2) 0.001(2) C64 0.039(3) 0.036(3) 0.049(3) -0.018(2) 0.007(2) -0.003(2) C65 0.046(3) 0.031(3) 0.047(3) 0.002(2) -0.013(2) -0.004(2) C66 0.055(3) 0.043(3) 0.045(3) -0.011(2) 0.014(3) -0.022(3) B1 0.050(4) 0.054(4) 0.043(3) 0.001(3) -0.012(3) 0.008(3) B2 0.034(3) 0.046(4) 0.036(3) 0.007(3) 0.010(2) -0.001(3) F5 0.0521(19) 0.0494(19) 0.0521(18) 0.0214(15) 0.0070(14) 0.0075(15) F6 0.057(2) 0.087(3) 0.088(3) 0.031(2) 0.013(2) 0.037(2) F7 0.072(2) 0.054(2) 0.0479(18) -0.0073(15) 0.0258(16) -0.0230(17) F8 0.100(3) 0.074(3) 0.0393(18) -0.0062(17) 0.0082(18) -0.029(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 2.045(3) . ? Ni1 O2 2.057(3) . ? Ni1 O4 2.062(3) . ? Ni1 O5 2.071(3) . ? Ni1 O6 2.102(3) . ? Ni1 O3 2.110(3) . ? Fe1 C1 2.026(4) . ? Fe1 C5 2.034(4) . ? Fe1 C7 2.035(5) . ? Fe1 C10 2.039(5) . ? Fe1 C9 2.043(4) . ? Fe1 C11 2.045(5) . ? Fe1 C2 2.050(4) . ? Fe1 C3 2.052(4) . ? Fe1 C4 2.053(4) . ? Fe1 C8 2.054(4) . ? C1 C5 1.430(6) . ? C1 C2 1.435(6) . ? C1 C6 1.472(5) . ? C2 C3 1.425(6) . ? C2 H2 1.0000 . ? C3 C4 1.420(6) . ? C3 H3 1.0000 . ? C4 C5 1.418(6) . ? C4 H4 1.0000 . ? C5 H5 1.0000 . ? C6 O1 1.260(5) . ? C6 N1 1.335(5) . ? N1 H1A 0.8800 . ? N1 H1B 0.8800 . ? C7 C8 1.413(7) . ? C7 C11 1.428(8) . ? C7 H7 1.0000 . ? C8 C9 1.418(7) . ? C8 H8 1.0000 . ? C9 C10 1.411(7) . ? C9 H9 1.0000 . ? C10 C11 1.429(8) . ? C10 H10 1.0000 . ? C11 H11 1.0000 . ? Fe2 C22 2.008(8) . ? Fe2 C13 2.016(5) . ? Fe2 C21 2.016(7) . ? Fe2 C20 2.028(7) . ? Fe2 C17 2.034(5) . ? Fe2 C14 2.034(5) . ? Fe2 C16 2.056(5) . ? Fe2 C18 2.058(6) . ? Fe2 C15 2.062(5) . ? Fe2 C19 2.064(6) . ? C12 O2 1.259(5) . ? C12 N2 1.318(6) . ? C12 C13 1.461(6) . ? C13 C17 1.413(6) . ? C13 C14 1.443(6) . ? C14 C15 1.416(7) . ? C14 H14 1.0000 . ? C15 C16 1.388(8) . ? C15 H15 1.0000 . ? C16 C17 1.426(7) . ? C16 H16 1.0000 . ? C17 H17 1.0000 . ? N2 H2A 0.8800 . ? N2 H2B 0.8800 . ? C18 C22 1.406(10) . ? C18 C19 1.407(9) . ? C18 H18 1.0000 . ? C19 C20 1.392(10) . ? C19 H19 1.0000 . ? C20 C21 1.421(10) . ? C20 H20 1.0000 . ? C21 C22 1.402(11) . ? C21 H21 1.0000 . ? C22 H22 1.0000 . ? Fe3 C27 2.030(5) . ? Fe3 C23 2.032(4) . ? Fe3 C24 2.033(5) . ? Fe3 C32 2.035(5) . ? Fe3 C30 2.044(5) . ? Fe3 C26 2.044(5) . ? Fe3 C33 2.044(5) . ? Fe3 C29 2.047(5) . ? Fe3 C31 2.052(5) . ? Fe3 C25 2.059(5) . ? C23 C27 1.441(6) . ? C23 C24 1.442(6) . ? C23 C28 1.466(6) . ? C27 C26 1.418(7) . ? C27 H27 1.0000 . ? C26 C25 1.423(8) . ? C26 H26 1.0000 . ? C25 C24 1.410(7) . ? C25 H25 1.0000 . ? C24 H24 1.0000 . ? C28 O3 1.270(5) . ? C28 N3 1.331(5) . ? N3 H3A 0.8800 . ? N3 H3B 0.8800 . ? C29 C33 1.396(8) . ? C29 C30 1.415(8) . ? C29 H29 1.0000 . ? C30 C31 1.430(8) . ? C30 H30 1.0000 . ? C31 C32 1.389(8) . ? C31 H31 1.0000 . ? C32 C33 1.436(8) . ? C32 H32 1.0000 . ? C33 H33 1.0000 . ? Fe4 C34 2.039(4) . ? Fe4 C38 2.044(5) . ? Fe4 C35 2.052(4) . ? Fe4 C40 2.055(5) . ? Fe4 C44 2.059(5) . ? Fe4 C43 2.066(5) . ? Fe4 C41 2.068(5) . ? Fe4 C37 2.068(5) . ? Fe4 C42 2.076(5) . ? Fe4 C36 2.077(5) . ? C34 C35 1.433(6) . ? C34 C38 1.445(6) . ? C34 C39 1.469(6) . ? C35 C36 1.417(6) . ? C35 H35 1.0000 . ? C36 C37 1.416(7) . ? C36 H36 1.0000 . ? C37 C38 1.428(6) . ? C37 H37 1.0000 . ? C38 H38 1.0000 . ? C39 O4 1.242(5) . ? C39 N4 1.342(6) . ? N4 H4A 0.8800 . ? N4 H4B 0.8800 . ? C40 C44 1.412(8) . ? C40 C41 1.418(8) . ? C40 H40 1.0000 . ? C41 C42 1.430(7) . ? C41 H41 1.0000 . ? C42 C43 1.426(8) . ? C42 H42 1.0000 . ? C43 C44 1.416(8) . ? C43 H43 1.0000 . ? C44 H44 1.0000 . ? Fe5 C45 2.022(4) . ? Fe5 C49 2.026(4) . ? Fe5 C52 2.036(5) . ? Fe5 C53 2.046(5) . ? Fe5 C51 2.047(5) . ? Fe5 C46 2.060(4) . ? Fe5 C48 2.063(5) . ? Fe5 C54 2.065(5) . ? Fe5 C55 2.068(5) . ? Fe5 C47 2.071(5) . ? C45 C49 1.440(5) . ? C45 C46 1.445(6) . ? C45 C50 1.465(6) . ? C46 C47 1.416(6) . ? C46 H46 1.0000 . ? C47 C48 1.430(6) . ? C47 H47 1.0000 . ? C48 C49 1.431(6) . ? C48 H48 1.0000 . ? C49 H49 1.0000 . ? C50 O5 1.267(4) . ? C50 N5 1.311(5) . ? N5 H5A 0.8800 . ? N5 H5B 0.8800 . ? C51 C52 1.411(8) . ? C51 C55 1.429(7) . ? C51 H51 1.0000 . ? C52 C53 1.427(7) . ? C52 H52 1.0000 . ? C53 C54 1.433(7) . ? C53 H53 1.0000 . ? C54 C55 1.412(7) . ? C54 H54 1.0000 . ? C55 H55 1.0000 . ? Fe6 C56 2.032(4) . ? Fe6 C62 2.034(5) . ? Fe6 C63 2.037(5) . ? Fe6 C66 2.038(5) . ? Fe6 C64 2.040(5) . ? Fe6 C57 2.043(4) . ? Fe6 C60 2.046(4) . ? Fe6 C65 2.047(5) . ? Fe6 C58 2.048(5) . ? Fe6 C59 2.053(5) . ? C56 C60 1.439(6) . ? C56 C57 1.439(6) . ? C56 C61 1.474(5) . ? C57 C58 1.415(6) . ? C57 H57 1.0000 . ? C58 C59 1.389(7) . ? C58 H58 1.0000 . ? C59 C60 1.425(6) . ? C59 H59 1.0000 . ? C60 H60 1.0000 . ? C61 O6 1.263(5) . ? C61 N6 1.319(5) . ? N6 H6A 0.8800 . ? N6 H6B 0.8800 . ? C62 C66 1.402(8) . ? C62 C63 1.413(7) . ? C62 H62 1.0000 . ? C63 C64 1.413(7) . ? C63 H63 1.0000 . ? C64 C65 1.404(7) . ? C64 H64 1.0000 . ? C65 C66 1.408(7) . ? C65 H65 1.0000 . ? C66 H66 1.0000 . ? B1 F4A 1.259(10) . ? B1 F4 1.336(10) . ? B1 F3 1.357(14) . ? B1 F1 1.374(8) . ? B1 F3A 1.378(13) . ? B1 F2A 1.444(10) . ? B1 F2 1.501(11) . ? B2 F5 1.366(6) . ? B2 F8 1.374(7) . ? B2 F7 1.384(6) . ? B2 F6 1.395(6) . ? 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 O1 Ni1 O2 89.78(11) . . ? O1 Ni1 O4 176.79(12) . . ? O2 Ni1 O4 92.65(12) . . ? O1 Ni1 O5 92.10(11) . . ? O2 Ni1 O5 177.63(12) . . ? O4 Ni1 O5 85.53(12) . . ? O1 Ni1 O6 89.62(11) . . ? O2 Ni1 O6 93.30(11) . . ? O4 Ni1 O6 88.14(11) . . ? O5 Ni1 O6 88.16(11) . . ? O1 Ni1 O3 89.17(11) . . ? O2 Ni1 O3 83.76(11) . . ? O4 Ni1 O3 93.18(12) . . ? O5 Ni1 O3 94.82(11) . . ? O6 Ni1 O3 176.82(11) . . ? C1 Fe1 C5 41.25(16) . . ? C1 Fe1 C7 123.58(19) . . ? C5 Fe1 C7 160.54(19) . . ? C1 Fe1 C10 122.19(18) . . ? C5 Fe1 C10 107.1(2) . . ? C7 Fe1 C10 68.9(2) . . ? C1 Fe1 C9 158.10(19) . . ? C5 Fe1 C9 121.9(2) . . ? C7 Fe1 C9 68.1(2) . . ? C10 Fe1 C9 40.44(19) . . ? C1 Fe1 C11 107.45(18) . . ? C5 Fe1 C11 123.6(2) . . ? C7 Fe1 C11 41.0(2) . . ? C10 Fe1 C11 41.0(2) . . ? C9 Fe1 C11 68.2(2) . . ? C1 Fe1 C2 41.23(16) . . ? C5 Fe1 C2 69.26(17) . . ? C7 Fe1 C2 107.2(2) . . ? C10 Fe1 C2 158.6(2) . . ? C9 Fe1 C2 159.40(18) . . ? C11 Fe1 C2 122.3(2) . . ? C1 Fe1 C3 68.69(16) . . ? C5 Fe1 C3 68.53(17) . . ? C7 Fe1 C3 122.0(2) . . ? C10 Fe1 C3 159.4(2) . . ? C9 Fe1 C3 123.43(18) . . ? C11 Fe1 C3 158.2(2) . . ? C2 Fe1 C3 40.66(17) . . ? C1 Fe1 C4 68.70(16) . . ? C5 Fe1 C4 40.62(16) . . ? C7 Fe1 C4 157.5(2) . . ? C10 Fe1 C4 123.2(2) . . ? C9 Fe1 C4 107.65(19) . . ? C11 Fe1 C4 160.0(2) . . ? C2 Fe1 C4 68.56(18) . . ? C3 Fe1 C4 40.47(18) . . ? C1 Fe1 C8 159.86(19) . . ? C5 Fe1 C8 157.50(19) . . ? C7 Fe1 C8 40.44(19) . . ? C10 Fe1 C8 68.4(2) . . ? C9 Fe1 C8 40.5(2) . . ? C11 Fe1 C8 68.4(2) . . ? C2 Fe1 C8 123.03(19) . . ? C3 Fe1 C8 107.43(18) . . ? C4 Fe1 C8 122.02(18) . . ? C5 C1 C2 108.2(4) . . ? C5 C1 C6 127.7(4) . . ? C2 C1 C6 124.1(4) . . ? C5 C1 Fe1 69.7(2) . . ? C2 C1 Fe1 70.3(2) . . ? C6 C1 Fe1 124.3(3) . . ? C3 C2 C1 107.1(4) . . ? C3 C2 Fe1 69.8(2) . . ? C1 C2 Fe1 68.5(2) . . ? C3 C2 H2 126.4 . . ? C1 C2 H2 126.4 . . ? Fe1 C2 H2 126.4 . . ? C4 C3 C2 108.6(4) . . ? C4 C3 Fe1 69.8(2) . . ? C2 C3 Fe1 69.6(2) . . ? C4 C3 H3 125.7 . . ? C2 C3 H3 125.7 . . ? Fe1 C3 H3 125.7 . . ? C5 C4 C3 108.3(4) . . ? C5 C4 Fe1 69.0(2) . . ? C3 C4 Fe1 69.7(2) . . ? C5 C4 H4 125.8 . . ? C3 C4 H4 125.8 . . ? Fe1 C4 H4 125.8 . . ? C4 C5 C1 107.8(4) . . ? C4 C5 Fe1 70.4(2) . . ? C1 C5 Fe1 69.1(2) . . ? C4 C5 H5 126.1 . . ? C1 C5 H5 126.1 . . ? Fe1 C5 H5 126.1 . . ? O1 C6 N1 122.6(4) . . ? O1 C6 C1 119.7(4) . . ? N1 C6 C1 117.7(4) . . ? C6 N1 H1A 120.0 . . ? C6 N1 H1B 120.0 . . ? H1A N1 H1B 120.0 . . ? C6 O1 Ni1 132.3(3) . . ? C8 C7 C11 108.3(5) . . ? C8 C7 Fe1 70.5(3) . . ? C11 C7 Fe1 69.9(3) . . ? C8 C7 H7 125.8 . . ? C11 C7 H7 125.8 . . ? Fe1 C7 H7 125.8 . . ? C7 C8 C9 107.6(5) . . ? C7 C8 Fe1 69.1(3) . . ? C9 C8 Fe1 69.4(2) . . ? C7 C8 H8 126.2 . . ? C9 C8 H8 126.2 . . ? Fe1 C8 H8 126.2 . . ? C10 C9 C8 108.9(5) . . ? C10 C9 Fe1 69.6(3) . . ? C8 C9 Fe1 70.2(3) . . ? C10 C9 H9 125.5 . . ? C8 C9 H9 125.5 . . ? Fe1 C9 H9 125.5 . . ? C9 C10 C11 107.6(5) . . ? C9 C10 Fe1 69.9(3) . . ? C11 C10 Fe1 69.8(3) . . ? C9 C10 H10 126.2 . . ? C11 C10 H10 126.2 . . ? Fe1 C10 H10 126.2 . . ? C7 C11 C10 107.5(4) . . ? C7 C11 Fe1 69.1(3) . . ? C10 C11 Fe1 69.3(3) . . ? C7 C11 H11 126.3 . . ? C10 C11 H11 126.3 . . ? Fe1 C11 H11 126.3 . . ? C22 Fe2 C13 106.9(3) . . ? C22 Fe2 C21 40.8(3) . . ? C13 Fe2 C21 119.0(3) . . ? C22 Fe2 C20 69.0(3) . . ? C13 Fe2 C20 154.1(3) . . ? C21 Fe2 C20 41.1(3) . . ? C22 Fe2 C17 125.7(3) . . ? C13 Fe2 C17 40.83(18) . . ? C21 Fe2 C17 107.2(3) . . ? C20 Fe2 C17 119.5(3) . . ? C22 Fe2 C14 119.7(3) . . ? C13 Fe2 C14 41.73(18) . . ? C21 Fe2 C14 154.6(3) . . ? C20 Fe2 C14 162.8(3) . . ? C17 Fe2 C14 69.1(2) . . ? C22 Fe2 C16 163.7(3) . . ? C13 Fe2 C16 68.5(2) . . ? C21 Fe2 C16 126.5(3) . . ? C20 Fe2 C16 107.9(3) . . ? C17 Fe2 C16 40.8(2) . . ? C14 Fe2 C16 68.0(2) . . ? C22 Fe2 C18 40.5(3) . . ? C13 Fe2 C18 126.4(2) . . ? C21 Fe2 C18 67.8(3) . . ? C20 Fe2 C18 67.9(3) . . ? C17 Fe2 C18 163.5(2) . . ? C14 Fe2 C18 108.2(3) . . ? C16 Fe2 C18 154.7(3) . . ? C22 Fe2 C15 155.1(3) . . ? C13 Fe2 C15 68.51(19) . . ? C21 Fe2 C15 163.2(3) . . ? C20 Fe2 C15 126.0(3) . . ? C17 Fe2 C15 67.8(2) . . ? C14 Fe2 C15 40.4(2) . . ? C16 Fe2 C15 39.4(2) . . ? C18 Fe2 C15 121.4(3) . . ? C22 Fe2 C19 67.6(3) . . ? C13 Fe2 C19 164.2(2) . . ? C21 Fe2 C19 67.3(3) . . ? C20 Fe2 C19 39.7(3) . . ? C17 Fe2 C19 154.4(2) . . ? C14 Fe2 C19 126.8(2) . . ? C16 Fe2 C19 120.9(2) . . ? C18 Fe2 C19 39.9(2) . . ? C15 Fe2 C19 109.8(2) . . ? O2 C12 N2 121.0(4) . . ? O2 C12 C13 119.9(4) . . ? N2 C12 C13 119.1(4) . . ? C17 C13 C14 107.7(4) . . ? C17 C13 C12 125.6(4) . . ? C14 C13 C12 126.6(4) . . ? C17 C13 Fe2 70.3(3) . . ? C14 C13 Fe2 69.8(3) . . ? C12 C13 Fe2 122.6(3) . . ? C15 C14 C13 106.8(5) . . ? C15 C14 Fe2 70.8(3) . . ? C13 C14 Fe2 68.5(3) . . ? C15 C14 H14 126.6 . . ? C13 C14 H14 126.6 . . ? Fe2 C14 H14 126.6 . . ? C16 C15 C14 109.2(5) . . ? C16 C15 Fe2 70.1(3) . . ? C14 C15 Fe2 68.7(3) . . ? C16 C15 H15 125.4 . . ? C14 C15 H15 125.4 . . ? Fe2 C15 H15 125.4 . . ? C15 C16 C17 108.5(5) . . ? C15 C16 Fe2 70.5(3) . . ? C17 C16 Fe2 68.8(3) . . ? C15 C16 H16 125.8 . . ? C17 C16 H16 125.8 . . ? Fe2 C16 H16 125.8 . . ? C13 C17 C16 107.7(4) . . ? C13 C17 Fe2 68.9(3) . . ? C16 C17 Fe2 70.4(3) . . ? C13 C17 H17 126.1 . . ? C16 C17 H17 126.1 . . ? Fe2 C17 H17 126.1 . . ? C12 N2 H2A 120.0 . . ? C12 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C12 O2 Ni1 135.9(3) . . ? C22 C18 C19 107.4(7) . . ? C22 C18 Fe2 67.9(4) . . ? C19 C18 Fe2 70.3(4) . . ? C22 C18 H18 126.3 . . ? C19 C18 H18 126.3 . . ? Fe2 C18 H18 126.3 . . ? C20 C19 C18 109.2(7) . . ? C20 C19 Fe2 68.7(4) . . ? C18 C19 Fe2 69.8(3) . . ? C20 C19 H19 125.3 . . ? C18 C19 H19 125.3 . . ? Fe2 C19 H19 125.3 . . ? C19 C20 C21 107.1(8) . . ? C19 C20 Fe2 71.5(4) . . ? C21 C20 Fe2 69.0(4) . . ? C19 C20 H20 126.4 . . ? C21 C20 H20 126.4 . . ? Fe2 C20 H20 126.4 . . ? C22 C21 C20 108.1(8) . . ? C22 C21 Fe2 69.3(4) . . ? C20 C21 Fe2 69.9(4) . . ? C22 C21 H21 125.9 . . ? C20 C21 H21 125.9 . . ? Fe2 C21 H21 125.9 . . ? C21 C22 C18 108.1(8) . . ? C21 C22 Fe2 69.9(5) . . ? C18 C22 Fe2 71.7(4) . . ? C21 C22 H22 125.9 . . ? C18 C22 H22 125.9 . . ? Fe2 C22 H22 125.9 . . ? C27 Fe3 C23 41.56(17) . . ? C27 Fe3 C24 69.5(2) . . ? C23 Fe3 C24 41.54(18) . . ? C27 Fe3 C32 125.9(2) . . ? C23 Fe3 C32 165.2(2) . . ? C24 Fe3 C32 151.2(2) . . ? C27 Fe3 C30 154.4(2) . . ? C23 Fe3 C30 120.5(2) . . ? C24 Fe3 C30 109.7(2) . . ? C32 Fe3 C30 67.6(3) . . ? C27 Fe3 C26 40.72(19) . . ? C23 Fe3 C26 68.97(18) . . ? C24 Fe3 C26 68.3(2) . . ? C32 Fe3 C26 106.3(2) . . ? C30 Fe3 C26 164.5(2) . . ? C27 Fe3 C33 106.7(2) . . ? C23 Fe3 C33 127.4(2) . . ? C24 Fe3 C33 166.8(2) . . ? C32 Fe3 C33 41.2(2) . . ? C30 Fe3 C33 68.0(3) . . ? C26 Fe3 C33 117.6(2) . . ? C27 Fe3 C29 119.4(2) . . ? C23 Fe3 C29 109.5(2) . . ? C24 Fe3 C29 130.0(2) . . ? C32 Fe3 C29 67.8(2) . . ? C30 Fe3 C29 40.5(2) . . ? C26 Fe3 C29 152.3(3) . . ? C33 Fe3 C29 39.9(2) . . ? C27 Fe3 C31 162.7(2) . . ? C23 Fe3 C31 154.3(2) . . ? C24 Fe3 C31 118.9(2) . . ? C32 Fe3 C31 39.7(2) . . ? C30 Fe3 C31 40.9(2) . . ? C26 Fe3 C31 125.5(2) . . ? C33 Fe3 C31 68.4(2) . . ? C29 Fe3 C31 68.3(2) . . ? C27 Fe3 C25 68.9(2) . . ? C23 Fe3 C25 69.03(19) . . ? C24 Fe3 C25 40.32(19) . . ? C32 Fe3 C25 117.1(2) . . ? C30 Fe3 C25 128.0(3) . . ? C26 Fe3 C25 40.6(2) . . ? C33 Fe3 C25 151.4(2) . . ? C29 Fe3 C25 166.8(3) . . ? C31 Fe3 C25 107.0(2) . . ? C27 C23 C24 106.8(4) . . ? C27 C23 C28 128.1(4) . . ? C24 C23 C28 125.0(4) . . ? C27 C23 Fe3 69.2(3) . . ? C24 C23 Fe3 69.3(3) . . ? C28 C23 Fe3 123.8(3) . . ? C26 C27 C23 107.6(4) . . ? C26 C27 Fe3 70.1(3) . . ? C23 C27 Fe3 69.3(3) . . ? C26 C27 H27 126.2 . . ? C23 C27 H27 126.2 . . ? Fe3 C27 H27 126.2 . . ? C27 C26 C25 109.0(4) . . ? C27 C26 Fe3 69.1(3) . . ? C25 C26 Fe3 70.3(3) . . ? C27 C26 H26 125.5 . . ? C25 C26 H26 125.5 . . ? Fe3 C26 H26 125.5 . . ? C24 C25 C26 107.8(4) . . ? C24 C25 Fe3 68.9(3) . . ? C26 C25 Fe3 69.1(3) . . ? C24 C25 H25 126.1 . . ? C26 C25 H25 126.1 . . ? Fe3 C25 H25 126.1 . . ? C25 C24 C23 108.7(4) . . ? C25 C24 Fe3 70.8(3) . . ? C23 C24 Fe3 69.2(3) . . ? C25 C24 H24 125.6 . . ? C23 C24 H24 125.6 . . ? Fe3 C24 H24 125.6 . . ? O3 C28 N3 121.8(4) . . ? O3 C28 C23 119.9(4) . . ? N3 C28 C23 118.3(4) . . ? C28 N3 H3A 120.0 . . ? C28 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C28 O3 Ni1 133.4(3) . . ? C33 C29 C30 108.8(5) . . ? C33 C29 Fe3 69.9(3) . . ? C30 C29 Fe3 69.6(3) . . ? C33 C29 H29 125.6 . . ? C30 C29 H29 125.6 . . ? Fe3 C29 H29 125.6 . . ? C29 C30 C31 107.9(5) . . ? C29 C30 Fe3 69.9(3) . . ? C31 C30 Fe3 69.9(3) . . ? C29 C30 H30 126.0 . . ? C31 C30 H30 126.0 . . ? Fe3 C30 H30 126.0 . . ? C32 C31 C30 107.2(5) . . ? C32 C31 Fe3 69.5(3) . . ? C30 C31 Fe3 69.2(3) . . ? C32 C31 H31 126.4 . . ? C30 C31 H31 126.4 . . ? Fe3 C31 H31 126.4 . . ? C31 C32 C33 109.3(5) . . ? C31 C32 Fe3 70.8(3) . . ? C33 C32 Fe3 69.7(3) . . ? C31 C32 H32 125.4 . . ? C33 C32 H32 125.4 . . ? Fe3 C32 H32 125.4 . . ? C29 C33 C32 106.9(6) . . ? C29 C33 Fe3 70.2(3) . . ? C32 C33 Fe3 69.0(3) . . ? C29 C33 H33 126.6 . . ? C32 C33 H33 126.6 . . ? Fe3 C33 H33 126.6 . . ? C34 Fe4 C38 41.46(17) . . ? C34 Fe4 C35 41.01(17) . . ? C38 Fe4 C35 68.94(19) . . ? C34 Fe4 C40 109.3(2) . . ? C38 Fe4 C40 131.5(2) . . ? C35 Fe4 C40 117.5(2) . . ? C34 Fe4 C44 118.0(2) . . ? C38 Fe4 C44 109.7(2) . . ? C35 Fe4 C44 150.6(2) . . ? C40 Fe4 C44 40.2(2) . . ? C34 Fe4 C43 150.2(2) . . ? C38 Fe4 C43 116.8(2) . . ? C35 Fe4 C43 167.7(2) . . ? C40 Fe4 C43 67.7(2) . . ? C44 Fe4 C43 40.1(2) . . ? C34 Fe4 C41 130.46(19) . . ? C38 Fe4 C41 170.0(2) . . ? C35 Fe4 C41 108.6(2) . . ? C40 Fe4 C41 40.2(2) . . ? C44 Fe4 C41 67.4(2) . . ? C43 Fe4 C41 67.7(2) . . ? C34 Fe4 C37 68.65(18) . . ? C38 Fe4 C37 40.63(18) . . ? C35 Fe4 C37 67.84(19) . . ? C40 Fe4 C37 170.0(2) . . ? C44 Fe4 C37 131.3(2) . . ? C43 Fe4 C37 108.8(2) . . ? C41 Fe4 C37 148.4(2) . . ? C34 Fe4 C42 168.6(2) . . ? C38 Fe4 C42 148.6(2) . . ? C35 Fe4 C42 129.4(2) . . ? C40 Fe4 C42 67.9(2) . . ? C44 Fe4 C42 67.6(2) . . ? C43 Fe4 C42 40.3(2) . . ? C41 Fe4 C42 40.4(2) . . ? C37 Fe4 C42 116.1(2) . . ? C34 Fe4 C36 68.27(18) . . ? C38 Fe4 C36 68.09(19) . . ? C35 Fe4 C36 40.14(18) . . ? C40 Fe4 C36 149.4(2) . . ? C44 Fe4 C36 168.7(2) . . ? C43 Fe4 C36 129.9(2) . . ? C41 Fe4 C36 116.7(2) . . ? C37 Fe4 C36 39.94(19) . . ? C42 Fe4 C36 108.1(2) . . ? C35 C34 C38 107.3(4) . . ? C35 C34 C39 124.5(4) . . ? C38 C34 C39 128.2(4) . . ? C35 C34 Fe4 70.0(2) . . ? C38 C34 Fe4 69.4(2) . . ? C39 C34 Fe4 127.7(3) . . ? C36 C35 C34 108.3(4) . . ? C36 C35 Fe4 70.9(3) . . ? C34 C35 Fe4 69.0(2) . . ? C36 C35 H35 125.9 . . ? C34 C35 H35 125.9 . . ? Fe4 C35 H35 125.9 . . ? C37 C36 C35 108.5(4) . . ? C37 C36 Fe4 69.7(3) . . ? C35 C36 Fe4 69.0(3) . . ? C37 C36 H36 125.7 . . ? C35 C36 H36 125.7 . . ? Fe4 C36 H36 125.7 . . ? C36 C37 C38 108.5(4) . . ? C36 C37 Fe4 70.4(3) . . ? C38 C37 Fe4 68.8(3) . . ? C36 C37 H37 125.8 . . ? C38 C37 H37 125.8 . . ? Fe4 C37 H37 125.8 . . ? C37 C38 C34 107.5(4) . . ? C37 C38 Fe4 70.6(3) . . ? C34 C38 Fe4 69.1(2) . . ? C37 C38 H38 126.3 . . ? C34 C38 H38 126.3 . . ? Fe4 C38 H38 126.3 . . ? O4 C39 N4 121.1(4) . . ? O4 C39 C34 120.4(4) . . ? N4 C39 C34 118.5(4) . . ? C39 N4 H4A 120.0 . . ? C39 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C39 O4 Ni1 134.9(3) . . ? C44 C40 C41 108.0(5) . . ? C44 C40 Fe4 70.0(3) . . ? C41 C40 Fe4 70.3(3) . . ? C44 C40 H40 126.0 . . ? C41 C40 H40 126.0 . . ? Fe4 C40 H40 126.0 . . ? C40 C41 C42 108.1(5) . . ? C40 C41 Fe4 69.4(3) . . ? C42 C41 Fe4 70.1(3) . . ? C40 C41 H41 125.9 . . ? C42 C41 H41 125.9 . . ? Fe4 C41 H41 125.9 . . ? C43 C42 C41 107.3(5) . . ? C43 C42 Fe4 69.5(3) . . ? C41 C42 Fe4 69.5(3) . . ? C43 C42 H42 126.3 . . ? C41 C42 H42 126.3 . . ? Fe4 C42 H42 126.3 . . ? C44 C43 C42 108.0(5) . . ? C44 C43 Fe4 69.7(3) . . ? C42 C43 Fe4 70.2(3) . . ? C44 C43 H43 126.0 . . ? C42 C43 H43 126.0 . . ? Fe4 C43 H43 126.0 . . ? C40 C44 C43 108.6(5) . . ? C40 C44 Fe4 69.8(3) . . ? C43 C44 Fe4 70.2(3) . . ? C40 C44 H44 125.7 . . ? C43 C44 H44 125.7 . . ? Fe4 C44 H44 125.7 . . ? C45 Fe5 C49 41.66(16) . . ? C45 Fe5 C52 118.9(2) . . ? C49 Fe5 C52 104.2(2) . . ? C45 Fe5 C53 104.07(19) . . ? C49 Fe5 C53 120.1(2) . . ? C52 Fe5 C53 40.9(2) . . ? C45 Fe5 C51 155.56(19) . . ? C49 Fe5 C51 120.47(19) . . ? C52 Fe5 C51 40.4(2) . . ? C53 Fe5 C51 68.5(2) . . ? C45 Fe5 C46 41.43(16) . . ? C49 Fe5 C46 69.45(17) . . ? C52 Fe5 C46 156.4(2) . . ? C53 Fe5 C46 121.4(2) . . ? C51 Fe5 C46 162.1(2) . . ? C45 Fe5 C48 69.32(17) . . ? C49 Fe5 C48 40.96(17) . . ? C52 Fe5 C48 122.3(2) . . ? C53 Fe5 C48 157.7(2) . . ? C51 Fe5 C48 108.3(2) . . ? C46 Fe5 C48 68.51(18) . . ? C45 Fe5 C54 122.24(18) . . ? C49 Fe5 C54 157.92(19) . . ? C52 Fe5 C54 68.4(2) . . ? C53 Fe5 C54 40.8(2) . . ? C51 Fe5 C54 68.2(2) . . ? C46 Fe5 C54 108.61(19) . . ? C48 Fe5 C54 160.4(2) . . ? C45 Fe5 C55 159.94(18) . . ? C49 Fe5 C55 158.32(18) . . ? C52 Fe5 C55 67.9(2) . . ? C53 Fe5 C55 68.0(2) . . ? C51 Fe5 C55 40.6(2) . . ? C46 Fe5 C55 125.73(19) . . ? C48 Fe5 C55 124.91(19) . . ? C54 Fe5 C55 39.94(19) . . ? C45 Fe5 C47 68.63(17) . . ? C49 Fe5 C47 68.55(19) . . ? C52 Fe5 C47 160.3(2) . . ? C53 Fe5 C47 158.6(2) . . ? C51 Fe5 C47 126.2(2) . . ? C46 Fe5 C47 40.09(17) . . ? C48 Fe5 C47 40.49(18) . . ? C54 Fe5 C47 125.0(2) . . ? C55 Fe5 C47 111.7(2) . . ? C49 C45 C46 107.6(4) . . ? C49 C45 C50 126.9(4) . . ? C46 C45 C50 124.8(4) . . ? C49 C45 Fe5 69.3(2) . . ? C46 C45 Fe5 70.7(2) . . ? C50 C45 Fe5 118.2(3) . . ? C47 C46 C45 107.5(4) . . ? C47 C46 Fe5 70.3(3) . . ? C45 C46 Fe5 67.9(2) . . ? C47 C46 H46 126.2 . . ? C45 C46 H46 126.2 . . ? Fe5 C46 H46 126.2 . . ? C46 C47 C48 109.3(4) . . ? C46 C47 Fe5 69.6(3) . . ? C48 C47 Fe5 69.5(3) . . ? C46 C47 H47 125.3 . . ? C48 C47 H47 125.3 . . ? Fe5 C47 H47 125.3 . . ? C47 C48 C49 107.5(4) . . ? C47 C48 Fe5 70.0(3) . . ? C49 C48 Fe5 68.1(3) . . ? C47 C48 H48 126.3 . . ? C49 C48 H48 126.3 . . ? Fe5 C48 H48 126.3 . . ? C48 C49 C45 108.1(4) . . ? C48 C49 Fe5 70.9(3) . . ? C45 C49 Fe5 69.0(2) . . ? C48 C49 H49 126.0 . . ? C45 C49 H49 126.0 . . ? Fe5 C49 H49 126.0 . . ? O5 C50 N5 121.7(4) . . ? O5 C50 C45 119.0(4) . . ? N5 C50 C45 119.4(4) . . ? C50 N5 H5A 120.0 . . ? C50 N5 H5B 120.0 . . ? H5A N5 H5B 120.0 . . ? C50 O5 Ni1 133.1(3) . . ? C52 C51 C55 107.7(5) . . ? C52 C51 Fe5 69.4(3) . . ? C55 C51 Fe5 70.5(3) . . ? C52 C51 H51 126.1 . . ? C55 C51 H51 126.1 . . ? Fe5 C51 H51 126.1 . . ? C51 C52 C53 108.5(5) . . ? C51 C52 Fe5 70.2(3) . . ? C53 C52 Fe5 69.9(3) . . ? C51 C52 H52 125.7 . . ? C53 C52 H52 125.7 . . ? Fe5 C52 H52 125.7 . . ? C52 C53 C54 107.4(5) . . ? C52 C53 Fe5 69.2(3) . . ? C54 C53 Fe5 70.3(3) . . ? C52 C53 H53 126.3 . . ? C54 C53 H53 126.3 . . ? Fe5 C53 H53 126.3 . . ? C55 C54 C53 107.9(5) . . ? C55 C54 Fe5 70.1(3) . . ? C53 C54 Fe5 68.9(3) . . ? C55 C54 H54 126.1 . . ? C53 C54 H54 126.1 . . ? Fe5 C54 H54 126.1 . . ? C54 C55 C51 108.4(5) . . ? C54 C55 Fe5 69.9(3) . . ? C51 C55 Fe5 68.9(3) . . ? C54 C55 H55 125.8 . . ? C51 C55 H55 125.8 . . ? Fe5 C55 H55 125.8 . . ? C56 Fe6 C62 122.38(19) . . ? C56 Fe6 C63 156.3(2) . . ? C62 Fe6 C63 40.6(2) . . ? C56 Fe6 C66 110.30(19) . . ? C62 Fe6 C66 40.3(2) . . ? C63 Fe6 C66 67.8(2) . . ? C56 Fe6 C64 162.5(2) . . ? C62 Fe6 C64 68.2(2) . . ? C63 Fe6 C64 40.6(2) . . ? C66 Fe6 C64 67.7(2) . . ? C56 Fe6 C57 41.37(17) . . ? C62 Fe6 C57 105.8(2) . . ? C63 Fe6 C57 118.8(2) . . ? C66 Fe6 C57 124.6(2) . . ? C64 Fe6 C57 154.5(2) . . ? C56 Fe6 C60 41.34(16) . . ? C62 Fe6 C60 160.2(2) . . ? C63 Fe6 C60 158.80(19) . . ? C66 Fe6 C60 126.0(2) . . ? C64 Fe6 C60 124.62(19) . . ? C57 Fe6 C60 69.15(18) . . ? C56 Fe6 C65 126.98(19) . . ? C62 Fe6 C65 68.0(2) . . ? C63 Fe6 C65 67.9(2) . . ? C66 Fe6 C65 40.3(2) . . ? C64 Fe6 C65 40.2(2) . . ? C57 Fe6 C65 162.5(2) . . ? C60 Fe6 C65 110.81(19) . . ? C56 Fe6 C58 68.52(18) . . ? C62 Fe6 C58 121.3(2) . . ? C63 Fe6 C58 104.5(2) . . ? C66 Fe6 C58 159.0(2) . . ? C64 Fe6 C58 120.0(2) . . ? C57 Fe6 C58 40.47(18) . . ? C60 Fe6 C58 67.94(19) . . ? C65 Fe6 C58 156.8(2) . . ? C56 Fe6 C59 68.70(17) . . ? C62 Fe6 C59 156.7(2) . . ? C63 Fe6 C59 121.1(2) . . ? C66 Fe6 C59 161.1(2) . . ? C64 Fe6 C59 107.26(19) . . ? C57 Fe6 C59 68.00(19) . . ? C60 Fe6 C59 40.70(17) . . ? C65 Fe6 C59 124.1(2) . . ? C58 Fe6 C59 39.6(2) . . ? C60 C56 C57 107.4(4) . . ? C60 C56 C61 124.5(4) . . ? C57 C56 C61 128.0(4) . . ? C60 C56 Fe6 69.9(2) . . ? C57 C56 Fe6 69.8(2) . . ? C61 C56 Fe6 123.8(3) . . ? C58 C57 C56 107.1(4) . . ? C58 C57 Fe6 70.0(3) . . ? C56 C57 Fe6 68.9(2) . . ? C58 C57 H57 126.4 . . ? C56 C57 H57 126.4 . . ? Fe6 C57 H57 126.4 . . ? C59 C58 C57 109.5(4) . . ? C59 C58 Fe6 70.4(3) . . ? C57 C58 Fe6 69.6(3) . . ? C59 C58 H58 125.2 . . ? C57 C58 H58 125.2 . . ? Fe6 C58 H58 125.2 . . ? C58 C59 C60 108.8(4) . . ? C58 C59 Fe6 70.0(3) . . ? C60 C59 Fe6 69.4(3) . . ? C58 C59 H59 125.6 . . ? C60 C59 H59 125.6 . . ? Fe6 C59 H59 125.6 . . ? C59 C60 C56 107.1(4) . . ? C59 C60 Fe6 69.9(3) . . ? C56 C60 Fe6 68.8(2) . . ? C59 C60 H60 126.4 . . ? C56 C60 H60 126.4 . . ? Fe6 C60 H60 126.4 . . ? O6 C61 N6 122.0(4) . . ? O6 C61 C56 119.5(4) . . ? N6 C61 C56 118.4(4) . . ? C61 N6 H6A 120.0 . . ? C61 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C61 O6 Ni1 133.4(3) . . ? C66 C62 C63 107.7(5) . . ? C66 C62 Fe6 70.0(3) . . ? C63 C62 Fe6 69.8(3) . . ? C66 C62 H62 126.2 . . ? C63 C62 H62 126.2 . . ? Fe6 C62 H62 126.2 . . ? C62 C63 C64 107.8(5) . . ? C62 C63 Fe6 69.6(3) . . ? C64 C63 Fe6 69.8(3) . . ? C62 C63 H63 126.1 . . ? C64 C63 H63 126.1 . . ? Fe6 C63 H63 126.1 . . ? C65 C64 C63 108.2(5) . . ? C65 C64 Fe6 70.2(3) . . ? C63 C64 Fe6 69.6(3) . . ? C65 C64 H64 125.9 . . ? C63 C64 H64 125.9 . . ? Fe6 C64 H64 125.9 . . ? C64 C65 C66 107.7(5) . . ? C64 C65 Fe6 69.6(3) . . ? C66 C65 Fe6 69.5(3) . . ? C64 C65 H65 126.2 . . ? C66 C65 H65 126.2 . . ? Fe6 C65 H65 126.2 . . ? C62 C66 C65 108.7(5) . . ? C62 C66 Fe6 69.7(3) . . ? C65 C66 Fe6 70.2(3) . . ? C62 C66 H66 125.7 . . ? C65 C66 H66 125.7 . . ? Fe6 C66 H66 125.7 . . ? F4A B1 F4 75.4(6) . . ? F4A B1 F3 123.1(9) . . ? F4 B1 F3 117.0(8) . . ? F4A B1 F1 112.1(7) . . ? F4 B1 F1 113.8(6) . . ? F3 B1 F1 111.1(8) . . ? F4A B1 F3A 116.0(8) . . ? F4 B1 F3A 127.5(8) . . ? F3 B1 F3A 12.6(8) . . ? F1 B1 F3A 108.1(8) . . ? F4A B1 F2A 110.4(7) . . ? F4 B1 F2A 37.8(4) . . ? F3 B1 F2A 85.6(7) . . ? F1 B1 F2A 111.4(6) . . ? F3A B1 F2A 98.0(7) . . ? F4A B1 F2 27.7(5) . . ? F4 B1 F2 102.2(7) . . ? F3 B1 F2 104.1(7) . . ? F1 B1 F2 107.1(6) . . ? F3A B1 F2 93.9(7) . . ? F2A B1 F2 133.4(7) . . ? F5 B2 F8 110.9(5) . . ? F5 B2 F7 110.8(5) . . ? F8 B2 F7 109.1(4) . . ? F5 B2 F6 107.4(4) . . ? F8 B2 F6 112.1(5) . . ? F7 B2 F6 106.6(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.585 _refine_diff_density_min -1.310 _refine_diff_density_rms 0.134 ###Material relevant to compound 5 at 173K ######## data_e314 _database_code_depnum_ccdc_archive 'CCDC 615871' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H44 Cu F6 Fe4 N4 O10 S2, 2(C4 H8 O)' _chemical_formula_sum 'C54 H60 Cu F6 Fe4 N4 O12 S2' _chemical_formula_weight 1422.12 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Cu Cu 0.3201 1.2651 '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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0110(4) _cell_length_b 12.2570(4) _cell_length_c 12.3360(4) _cell_angle_alpha 110.917(2) _cell_angle_beta 91.7100(19) _cell_angle_gamma 90.4170(13) _cell_volume 1413.04(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5296 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 727 _exptl_absorpt_coefficient_mu 1.531 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7493 _exptl_absorpt_correction_T_max 0.8873 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12436 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0886 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 30.09 _reflns_number_total 8257 _reflns_number_gt 5609 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0134P)^2^+0.4129P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8257 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0900 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.0889 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.0000 0.0000 0.0000 0.02187(10) Uani 1 2 d S . . Fe1 Fe 1.29408(4) 0.37802(3) 0.32260(3) 0.02134(9) Uani 1 1 d . . . C1 C 1.1148(3) 0.2946(2) 0.29763(18) 0.0236(5) Uani 1 1 d . . . C2 C 1.2061(3) 0.2420(2) 0.35393(19) 0.0257(6) Uani 1 1 d . . . H2 H 1.2348 0.1589 0.3237 0.031 Uiso 1 1 calc R . . C3 C 1.2496(3) 0.3294(2) 0.46092(19) 0.0288(6) Uani 1 1 d . . . H3 H 1.3155 0.3187 0.5187 0.035 Uiso 1 1 calc R . . C4 C 1.1848(3) 0.4349(2) 0.47027(19) 0.0303(6) Uani 1 1 d . . . H4 H 1.1983 0.5113 0.5358 0.036 Uiso 1 1 calc R . . C5 C 1.1007(3) 0.4152(2) 0.36991(19) 0.0260(6) Uani 1 1 d . . . H5 H 1.0427 0.4737 0.3530 0.031 Uiso 1 1 calc R . . C6 C 1.0499(3) 0.2328(2) 0.18276(19) 0.0242(5) Uani 1 1 d . . . O1 O 1.08599(19) 0.13076(14) 0.12626(13) 0.0306(4) Uani 1 1 d . . . N1 N 0.9555(2) 0.28462(18) 0.14422(17) 0.0375(6) Uani 1 1 d . . . H1A H 0.9149 0.2478 0.0765 0.045 Uiso 1 1 calc R . . H1B H 0.9327 0.3562 0.1861 0.045 Uiso 1 1 calc R . . C7 C 1.4585(3) 0.3143(2) 0.2283(2) 0.0340(7) Uani 1 1 d . . . H7 H 1.4921 0.2329 0.2066 0.041 Uiso 1 1 calc R . . C8 C 1.3658(3) 0.3536(2) 0.1627(2) 0.0361(7) Uani 1 1 d . . . H8 H 1.3223 0.3050 0.0864 0.043 Uiso 1 1 calc R . . C9 C 1.3442(3) 0.4740(2) 0.2240(2) 0.0368(7) Uani 1 1 d . . . H9 H 1.2831 0.5251 0.1986 0.044 Uiso 1 1 calc R . . C10 C 1.4244(3) 0.5087(2) 0.3278(2) 0.0354(7) Uani 1 1 d . . . H10 H 1.4294 0.5888 0.3886 0.042 Uiso 1 1 calc R . . C11 C 1.4958(3) 0.4104(2) 0.3309(2) 0.0332(6) Uani 1 1 d . . . H11 H 1.5601 0.4087 0.3939 0.040 Uiso 1 1 calc R . . Fe2 Fe 0.75806(4) 0.06682(3) 0.41315(3) 0.02153(9) Uani 1 1 d . . . C12 C 0.7773(3) -0.0660(2) 0.25958(18) 0.0227(5) Uani 1 1 d . . . C13 C 0.6567(3) -0.0804(2) 0.31331(19) 0.0258(6) Uani 1 1 d . . . H13 H 0.5635 -0.0855 0.2801 0.031 Uiso 1 1 calc R . . C14 C 0.6960(3) -0.0888(2) 0.4220(2) 0.0302(6) Uani 1 1 d . . . H14 H 0.6340 -0.0985 0.4802 0.036 Uiso 1 1 calc R . . C15 C 0.8369(3) -0.0787(2) 0.4352(2) 0.0291(6) Uani 1 1 d . . . H15 H 0.8909 -0.0793 0.5045 0.035 Uiso 1 1 calc R . . C16 C 0.8885(3) -0.06420(19) 0.33554(19) 0.0248(5) Uani 1 1 d . . . H16 H 0.9848 -0.0542 0.3211 0.030 Uiso 1 1 calc R . . C17 C 0.7924(3) -0.04685(19) 0.14847(19) 0.0237(5) Uani 1 1 d . . . O2 O 0.90920(18) -0.03630(15) 0.11950(13) 0.0315(4) Uani 1 1 d . . . N2 N 0.6855(2) -0.04313(18) 0.08539(16) 0.0325(5) Uani 1 1 d . . . H2A H 0.6940 -0.0328 0.0189 0.039 Uiso 1 1 calc R . . H2B H 0.6055 -0.0510 0.1096 0.039 Uiso 1 1 calc R . . C18 C 0.6295(3) 0.1989(2) 0.4306(2) 0.0356(7) Uani 1 1 d . . . H18 H 0.5382 0.1913 0.3932 0.043 Uiso 1 1 calc R . . C19 C 0.6614(3) 0.1911(2) 0.5404(2) 0.0343(7) Uani 1 1 d . . . H19 H 0.5963 0.1766 0.5939 0.041 Uiso 1 1 calc R . . C20 C 0.8009(3) 0.2074(2) 0.5610(2) 0.0339(7) Uani 1 1 d . . . H20 H 0.8517 0.2054 0.6313 0.041 Uiso 1 1 calc R . . C21 C 0.8573(3) 0.2260(2) 0.4642(2) 0.0334(6) Uani 1 1 d . . . H21 H 0.9541 0.2394 0.4542 0.040 Uiso 1 1 calc R . . C22 C 0.7506(3) 0.2195(2) 0.3834(2) 0.0357(7) Uani 1 1 d . . . H22 H 0.7593 0.2281 0.3063 0.043 Uiso 1 1 calc R . . C24 C 0.7294(3) 0.5574(3) 0.2067(2) 0.0528(9) Uani 1 1 d . . . H24A H 0.6978 0.6158 0.2796 0.063 Uiso 1 1 calc R . . H24B H 0.6686 0.4882 0.1833 0.063 Uiso 1 1 calc R . . C25 C 0.7325(4) 0.6084(3) 0.1127(3) 0.0531(9) Uani 1 1 d . . . H25A H 0.6831 0.6825 0.1357 0.064 Uiso 1 1 calc R . . H25B H 0.6912 0.5533 0.0396 0.064 Uiso 1 1 calc R . . C26 C 0.8781(4) 0.6299(3) 0.0971(3) 0.0647(11) Uani 1 1 d . . . H26A H 0.8945 0.7110 0.1010 0.078 Uiso 1 1 calc R . . H26B H 0.9093 0.5748 0.0223 0.078 Uiso 1 1 calc R . . C27 C 0.9465(4) 0.6079(3) 0.2012(4) 0.0702(11) Uani 1 1 d . . . H27A H 1.0376 0.5776 0.1818 0.084 Uiso 1 1 calc R . . H27B H 0.9531 0.6810 0.2700 0.084 Uiso 1 1 calc R . . O6 O 0.8646(2) 0.52461(17) 0.22300(17) 0.0512(6) Uani 1 1 d . . . S1 S 0.72193(7) 0.09877(5) -0.13919(5) 0.02317(14) Uani 1 1 d . . . O3 O 0.81486(19) 0.10777(14) -0.04411(13) 0.0313(4) Uani 1 1 d . . . O4 O 0.7775(2) 0.07083(15) -0.25069(14) 0.0407(5) Uani 1 1 d . . . O5 O 0.6000(2) 0.03702(16) -0.13598(17) 0.0416(5) Uani 1 1 d . . . C23 C 0.6718(3) 0.2505(2) -0.1007(2) 0.0322(6) Uani 1 1 d . . . F2 F 0.77752(19) 0.31908(14) -0.09274(16) 0.0592(5) Uani 1 1 d . . . F1 F 0.6138(2) 0.28859(15) -0.00063(15) 0.0708(6) Uani 1 1 d . . . F3 F 0.58811(19) 0.26469(14) -0.17966(14) 0.0518(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0203(3) 0.0261(2) 0.01744(19) 0.00568(16) 0.00003(16) -0.00363(18) Fe1 0.0218(2) 0.02193(18) 0.02081(17) 0.00841(13) 0.00012(14) -0.00139(15) C1 0.0245(15) 0.0257(13) 0.0209(11) 0.0088(10) 0.0000(10) -0.0065(11) C2 0.0304(16) 0.0261(13) 0.0233(12) 0.0120(10) 0.0007(11) -0.0051(11) C3 0.0313(17) 0.0370(15) 0.0204(12) 0.0134(11) -0.0010(11) -0.0071(12) C4 0.0296(17) 0.0366(15) 0.0197(12) 0.0039(10) 0.0020(11) -0.0049(12) C5 0.0210(15) 0.0285(13) 0.0252(12) 0.0052(10) 0.0040(10) -0.0005(11) C6 0.0203(15) 0.0276(13) 0.0252(12) 0.0101(10) -0.0006(10) -0.0074(11) O1 0.0318(12) 0.0289(10) 0.0250(9) 0.0027(7) -0.0065(8) -0.0034(8) N1 0.0402(16) 0.0335(12) 0.0319(12) 0.0047(10) -0.0163(11) -0.0009(11) C7 0.0334(18) 0.0359(15) 0.0350(14) 0.0144(12) 0.0125(13) 0.0061(13) C8 0.0366(19) 0.0502(17) 0.0257(13) 0.0184(12) 0.0061(12) -0.0048(14) C9 0.0319(18) 0.0464(17) 0.0467(16) 0.0342(14) 0.0044(13) -0.0002(14) C10 0.0323(18) 0.0279(14) 0.0479(16) 0.0155(12) 0.0070(13) -0.0051(12) C11 0.0218(16) 0.0413(16) 0.0418(15) 0.0215(13) -0.0009(12) -0.0034(12) Fe2 0.0211(2) 0.02481(18) 0.02100(17) 0.01106(14) 0.00101(14) -0.00064(15) C12 0.0225(15) 0.0258(12) 0.0205(11) 0.0092(9) -0.0006(10) -0.0014(10) C13 0.0215(15) 0.0311(13) 0.0262(12) 0.0123(10) -0.0040(10) -0.0082(11) C14 0.0358(18) 0.0302(14) 0.0298(13) 0.0171(11) 0.0031(12) -0.0067(12) C15 0.0362(18) 0.0285(14) 0.0266(13) 0.0153(11) -0.0050(11) 0.0009(12) C16 0.0235(15) 0.0260(13) 0.0260(12) 0.0108(10) -0.0005(10) 0.0028(11) C17 0.0261(16) 0.0231(12) 0.0198(11) 0.0055(9) 0.0002(10) -0.0033(11) O2 0.0219(11) 0.0508(11) 0.0270(9) 0.0204(8) 0.0027(8) -0.0015(9) N2 0.0236(13) 0.0532(14) 0.0272(11) 0.0228(10) -0.0027(9) -0.0057(11) C18 0.0288(18) 0.0359(15) 0.0431(16) 0.0150(12) 0.0048(13) 0.0113(13) C19 0.0375(19) 0.0344(15) 0.0313(14) 0.0113(11) 0.0106(13) 0.0043(13) C20 0.045(2) 0.0273(14) 0.0269(13) 0.0065(11) 0.0009(12) -0.0034(13) C21 0.0327(18) 0.0243(13) 0.0444(15) 0.0135(11) 0.0049(13) -0.0047(12) C22 0.048(2) 0.0270(14) 0.0376(15) 0.0169(12) 0.0085(14) 0.0088(13) C24 0.043(2) 0.076(2) 0.0375(16) 0.0172(16) 0.0056(15) 0.0043(18) C25 0.066(3) 0.0411(18) 0.0484(18) 0.0112(14) -0.0041(17) 0.0122(17) C26 0.069(3) 0.047(2) 0.085(3) 0.0300(19) 0.034(2) 0.0171(19) C27 0.040(2) 0.046(2) 0.119(3) 0.024(2) -0.005(2) -0.0065(18) O6 0.0588(17) 0.0429(12) 0.0543(13) 0.0208(10) -0.0063(11) 0.0043(12) S1 0.0206(4) 0.0269(3) 0.0234(3) 0.0108(2) -0.0013(2) 0.0001(3) O3 0.0299(12) 0.0329(10) 0.0297(9) 0.0101(7) -0.0090(8) 0.0041(8) O4 0.0544(15) 0.0443(11) 0.0254(9) 0.0141(8) 0.0105(9) 0.0109(10) O5 0.0243(12) 0.0423(11) 0.0662(13) 0.0297(10) -0.0059(10) -0.0101(9) C23 0.0319(18) 0.0335(15) 0.0322(14) 0.0128(12) 0.0006(12) 0.0029(13) F2 0.0457(13) 0.0340(9) 0.0974(14) 0.0245(9) -0.0135(11) -0.0122(9) F1 0.1047(19) 0.0596(12) 0.0515(11) 0.0203(9) 0.0404(11) 0.0424(12) F3 0.0534(13) 0.0430(10) 0.0622(11) 0.0244(8) -0.0226(9) 0.0072(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 Cu1 O2 1.9339(15) . ? Cu1 O2 1.9339(15) 2_755 ? Cu1 O1 1.9630(16) . ? Cu1 O1 1.9630(16) 2_755 ? Cu1 O3 2.4423(17) . ? Fe1 C1 2.019(2) . ? Fe1 C7 2.039(3) . ? Fe1 C2 2.040(2) . ? Fe1 C10 2.041(3) . ? Fe1 C8 2.041(2) . ? Fe1 C9 2.041(2) . ? Fe1 C5 2.046(3) . ? Fe1 C11 2.048(3) . ? Fe1 C4 2.056(2) . ? Fe1 C3 2.057(2) . ? C1 C2 1.423(3) . ? C1 C5 1.439(3) . ? C1 C6 1.475(3) . ? C2 C3 1.424(3) . ? C2 H2 1.0000 . ? C3 C4 1.420(4) . ? C3 H3 1.0000 . ? C4 C5 1.422(3) . ? C4 H4 1.0000 . ? C5 H5 1.0000 . ? C6 O1 1.257(3) . ? C6 N1 1.311(3) . ? N1 H1A 0.8800 . ? N1 H1B 0.8800 . ? C7 C8 1.410(4) . ? C7 C11 1.426(4) . ? C7 H7 1.0000 . ? C8 C9 1.418(4) . ? C8 H8 1.0000 . ? C9 C10 1.419(4) . ? C9 H9 1.0000 . ? C10 C11 1.417(4) . ? C10 H10 1.0000 . ? C11 H11 1.0000 . ? Fe2 C12 2.025(2) . ? Fe2 C13 2.028(2) . ? Fe2 C18 2.031(3) . ? Fe2 C19 2.032(2) . ? Fe2 C22 2.034(2) . ? Fe2 C14 2.043(2) . ? Fe2 C20 2.044(2) . ? Fe2 C16 2.051(2) . ? Fe2 C15 2.058(2) . ? Fe2 C21 2.061(3) . ? C12 C16 1.428(3) . ? C12 C13 1.434(3) . ? C12 C17 1.483(3) . ? C13 C14 1.425(3) . ? C13 H13 1.0000 . ? C14 C15 1.415(4) . ? C14 H14 1.0000 . ? C15 C16 1.415(3) . ? C15 H15 1.0000 . ? C16 H16 1.0000 . ? C17 O2 1.252(3) . ? C17 N2 1.315(3) . ? N2 H2A 0.8800 . ? N2 H2B 0.8800 . ? C18 C19 1.419(3) . ? C18 C22 1.420(4) . ? C18 H18 1.0000 . ? C19 C20 1.412(4) . ? C19 H19 1.0000 . ? C20 C21 1.425(3) . ? C20 H20 1.0000 . ? C21 C22 1.421(4) . ? C21 H21 1.0000 . ? C22 H22 1.0000 . ? C24 O6 1.443(4) . ? C24 C25 1.502(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.509(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.545(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O6 1.409(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? S1 O4 1.4248(17) . ? S1 O5 1.4409(19) . ? S1 O3 1.4473(17) . ? S1 C23 1.825(3) . ? C23 F1 1.309(3) . ? C23 F3 1.325(3) . ? C23 F2 1.327(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O2 180.00(10) . 2_755 ? O2 Cu1 O1 86.65(7) . . ? O2 Cu1 O1 93.35(7) 2_755 . ? O2 Cu1 O1 93.35(7) . 2_755 ? O2 Cu1 O1 86.65(7) 2_755 2_755 ? O1 Cu1 O1 179.998(2) . 2_755 ? O2 Cu1 O3 95.07(7) . . ? O2 Cu1 O3 84.93(7) 2_755 . ? O1 Cu1 O3 97.62(6) . . ? O1 Cu1 O3 82.38(6) 2_755 . ? C1 Fe1 C7 124.85(10) . . ? C1 Fe1 C2 41.04(10) . . ? C7 Fe1 C2 106.98(10) . . ? C1 Fe1 C10 155.65(11) . . ? C7 Fe1 C10 68.36(11) . . ? C2 Fe1 C10 162.22(11) . . ? C1 Fe1 C8 107.31(10) . . ? C7 Fe1 C8 40.46(11) . . ? C2 Fe1 C8 120.02(10) . . ? C10 Fe1 C8 68.35(11) . . ? C1 Fe1 C9 120.37(11) . . ? C7 Fe1 C9 68.33(11) . . ? C2 Fe1 C9 155.31(11) . . ? C10 Fe1 C9 40.68(11) . . ? C8 Fe1 C9 40.68(10) . . ? C1 Fe1 C5 41.44(9) . . ? C7 Fe1 C5 162.63(10) . . ? C2 Fe1 C5 69.36(10) . . ? C10 Fe1 C5 120.25(10) . . ? C8 Fe1 C5 125.54(11) . . ? C9 Fe1 C5 107.50(11) . . ? C1 Fe1 C11 162.22(10) . . ? C7 Fe1 C11 40.83(10) . . ? C2 Fe1 C11 124.86(10) . . ? C10 Fe1 C11 40.54(10) . . ? C8 Fe1 C11 68.39(11) . . ? C9 Fe1 C11 68.41(11) . . ? C5 Fe1 C11 155.03(10) . . ? C1 Fe1 C4 68.51(10) . . ? C7 Fe1 C4 155.37(11) . . ? C2 Fe1 C4 68.38(10) . . ? C10 Fe1 C4 108.26(11) . . ? C8 Fe1 C4 163.04(11) . . ? C9 Fe1 C4 126.03(11) . . ? C5 Fe1 C4 40.56(10) . . ? C11 Fe1 C4 120.61(11) . . ? C1 Fe1 C3 68.59(10) . . ? C7 Fe1 C3 120.34(11) . . ? C2 Fe1 C3 40.67(9) . . ? C10 Fe1 C3 125.59(11) . . ? C8 Fe1 C3 155.06(11) . . ? C9 Fe1 C3 162.83(11) . . ? C5 Fe1 C3 68.66(10) . . ? C11 Fe1 C3 107.59(11) . . ? C4 Fe1 C3 40.40(10) . . ? C2 C1 C5 108.7(2) . . ? C2 C1 C6 124.0(2) . . ? C5 C1 C6 127.3(2) . . ? C2 C1 Fe1 70.27(14) . . ? C5 C1 Fe1 70.30(14) . . ? C6 C1 Fe1 124.36(16) . . ? C1 C2 C3 107.6(2) . . ? C1 C2 Fe1 68.69(13) . . ? C3 C2 Fe1 70.32(13) . . ? C1 C2 H2 126.2 . . ? C3 C2 H2 126.2 . . ? Fe1 C2 H2 126.2 . . ? C4 C3 C2 108.0(2) . . ? C4 C3 Fe1 69.73(13) . . ? C2 C3 Fe1 69.01(12) . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? Fe1 C3 H3 126.0 . . ? C3 C4 C5 109.0(2) . . ? C3 C4 Fe1 69.87(13) . . ? C5 C4 Fe1 69.38(13) . . ? C3 C4 H4 125.5 . . ? C5 C4 H4 125.5 . . ? Fe1 C4 H4 125.5 . . ? C4 C5 C1 106.6(2) . . ? C4 C5 Fe1 70.06(15) . . ? C1 C5 Fe1 68.26(14) . . ? C4 C5 H5 126.7 . . ? C1 C5 H5 126.7 . . ? Fe1 C5 H5 126.7 . . ? O1 C6 N1 122.4(2) . . ? O1 C6 C1 118.2(2) . . ? N1 C6 C1 119.4(2) . . ? C6 O1 Cu1 132.90(17) . . ? C6 N1 H1A 120.0 . . ? C6 N1 H1B 120.0 . . ? H1A N1 H1B 120.0 . . ? C8 C7 C11 108.2(2) . . ? C8 C7 Fe1 69.85(15) . . ? C11 C7 Fe1 69.93(15) . . ? C8 C7 H7 125.9 . . ? C11 C7 H7 125.9 . . ? Fe1 C7 H7 125.9 . . ? C7 C8 C9 108.1(2) . . ? C7 C8 Fe1 69.69(14) . . ? C9 C8 Fe1 69.66(14) . . ? C7 C8 H8 125.9 . . ? C9 C8 H8 125.9 . . ? Fe1 C8 H8 125.9 . . ? C8 C9 C10 107.8(2) . . ? C8 C9 Fe1 69.66(13) . . ? C10 C9 Fe1 69.66(14) . . ? C8 C9 H9 126.1 . . ? C10 C9 H9 126.1 . . ? Fe1 C9 H9 126.1 . . ? C11 C10 C9 108.3(2) . . ? C11 C10 Fe1 70.00(15) . . ? C9 C10 Fe1 69.66(15) . . ? C11 C10 H10 125.8 . . ? C9 C10 H10 125.8 . . ? Fe1 C10 H10 125.8 . . ? C10 C11 C7 107.5(2) . . ? C10 C11 Fe1 69.46(16) . . ? C7 C11 Fe1 69.24(16) . . ? C10 C11 H11 126.3 . . ? C7 C11 H11 126.3 . . ? Fe1 C11 H11 126.3 . . ? C12 Fe2 C13 41.43(9) . . ? C12 Fe2 C18 121.74(10) . . ? C13 Fe2 C18 105.16(11) . . ? C12 Fe2 C19 156.61(11) . . ? C13 Fe2 C19 119.19(11) . . ? C18 Fe2 C19 40.90(10) . . ? C12 Fe2 C22 108.68(10) . . ? C13 Fe2 C22 123.29(11) . . ? C18 Fe2 C22 40.89(11) . . ? C19 Fe2 C22 68.63(10) . . ? C12 Fe2 C14 68.58(9) . . ? C13 Fe2 C14 40.98(9) . . ? C18 Fe2 C14 121.77(12) . . ? C19 Fe2 C14 105.34(10) . . ? C22 Fe2 C14 159.32(12) . . ? C12 Fe2 C20 161.96(11) . . ? C13 Fe2 C20 155.37(10) . . ? C18 Fe2 C20 68.50(12) . . ? C19 Fe2 C20 40.54(11) . . ? C22 Fe2 C20 68.35(11) . . ? C14 Fe2 C20 120.71(10) . . ? C12 Fe2 C16 41.01(9) . . ? C13 Fe2 C16 69.54(10) . . ? C18 Fe2 C16 158.88(9) . . ? C19 Fe2 C16 159.67(10) . . ? C22 Fe2 C16 123.94(10) . . ? C14 Fe2 C16 68.35(10) . . ? C20 Fe2 C16 124.73(11) . . ? C12 Fe2 C15 68.19(9) . . ? C13 Fe2 C15 68.80(10) . . ? C18 Fe2 C15 158.50(11) . . ? C19 Fe2 C15 122.63(10) . . ? C22 Fe2 C15 159.38(12) . . ? C14 Fe2 C15 40.37(10) . . ? C20 Fe2 C15 107.94(10) . . ? C16 Fe2 C15 40.29(9) . . ? C12 Fe2 C21 125.62(10) . . ? C13 Fe2 C21 161.21(9) . . ? C18 Fe2 C21 68.59(12) . . ? C19 Fe2 C21 68.44(11) . . ? C22 Fe2 C21 40.61(11) . . ? C14 Fe2 C21 157.41(10) . . ? C20 Fe2 C21 40.62(10) . . ? C16 Fe2 C21 109.55(11) . . ? C15 Fe2 C21 123.42(11) . . ? C16 C12 C13 108.77(19) . . ? C16 C12 C17 122.6(2) . . ? C13 C12 C17 128.5(2) . . ? C16 C12 Fe2 70.48(13) . . ? C13 C12 Fe2 69.41(13) . . ? C17 C12 Fe2 122.73(16) . . ? C14 C13 C12 106.6(2) . . ? C14 C13 Fe2 70.05(14) . . ? C12 C13 Fe2 69.16(13) . . ? C14 C13 H13 126.7 . . ? C12 C13 H13 126.7 . . ? Fe2 C13 H13 126.7 . . ? C15 C14 C13 108.7(2) . . ? C15 C14 Fe2 70.38(14) . . ? C13 C14 Fe2 68.98(13) . . ? C15 C14 H14 125.6 . . ? C13 C14 H14 125.6 . . ? Fe2 C14 H14 125.6 . . ? C14 C15 C16 108.7(2) . . ? C14 C15 Fe2 69.25(14) . . ? C16 C15 Fe2 69.61(13) . . ? C14 C15 H15 125.6 . . ? C16 C15 H15 125.6 . . ? Fe2 C15 H15 125.6 . . ? C15 C16 C12 107.2(2) . . ? C15 C16 Fe2 70.09(14) . . ? C12 C16 Fe2 68.51(13) . . ? C15 C16 H16 126.4 . . ? C12 C16 H16 126.4 . . ? Fe2 C16 H16 126.4 . . ? O2 C17 N2 123.5(2) . . ? O2 C17 C12 116.8(2) . . ? N2 C17 C12 119.7(2) . . ? C17 O2 Cu1 139.05(17) . . ? C17 N2 H2A 120.0 . . ? C17 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C19 C18 C22 107.7(3) . . ? C19 C18 Fe2 69.58(15) . . ? C22 C18 Fe2 69.66(15) . . ? C19 C18 H18 126.2 . . ? C22 C18 H18 126.2 . . ? Fe2 C18 H18 126.2 . . ? C20 C19 C18 108.2(2) . . ? C20 C19 Fe2 70.20(15) . . ? C18 C19 Fe2 69.52(14) . . ? C20 C19 H19 125.9 . . ? C18 C19 H19 125.9 . . ? Fe2 C19 H19 125.9 . . ? C19 C20 C21 108.4(2) . . ? C19 C20 Fe2 69.26(15) . . ? C21 C20 Fe2 70.34(14) . . ? C19 C20 H20 125.8 . . ? C21 C20 H20 125.8 . . ? Fe2 C20 H20 125.8 . . ? C22 C21 C20 107.2(3) . . ? C22 C21 Fe2 68.65(15) . . ? C20 C21 Fe2 69.04(14) . . ? C22 C21 H21 126.4 . . ? C20 C21 H21 126.4 . . ? Fe2 C21 H21 126.4 . . ? C18 C22 C21 108.5(2) . . ? C18 C22 Fe2 69.46(14) . . ? C21 C22 Fe2 70.74(14) . . ? C18 C22 H22 125.7 . . ? C21 C22 H22 125.7 . . ? Fe2 C22 H22 125.7 . . ? O6 C24 C25 106.4(3) . . ? O6 C24 H24A 110.4 . . ? C25 C24 H24A 110.4 . . ? O6 C24 H24B 110.4 . . ? C25 C24 H24B 110.4 . . ? H24A C24 H24B 108.6 . . ? C24 C25 C26 106.1(3) . . ? C24 C25 H25A 110.5 . . ? C26 C25 H25A 110.5 . . ? C24 C25 H25B 110.5 . . ? C26 C25 H25B 110.5 . . ? H25A C25 H25B 108.7 . . ? C25 C26 C27 102.2(3) . . ? C25 C26 H26A 111.3 . . ? C27 C26 H26A 111.3 . . ? C25 C26 H26B 111.3 . . ? C27 C26 H26B 111.3 . . ? H26A C26 H26B 109.2 . . ? O6 C27 C26 105.5(3) . . ? O6 C27 H27A 110.6 . . ? C26 C27 H27A 110.6 . . ? O6 C27 H27B 110.6 . . ? C26 C27 H27B 110.6 . . ? H27A C27 H27B 108.8 . . ? C27 O6 C24 105.2(2) . . ? O4 S1 O5 115.74(12) . . ? O4 S1 O3 116.37(12) . . ? O5 S1 O3 112.85(11) . . ? O4 S1 C23 104.15(11) . . ? O5 S1 C23 104.12(12) . . ? O3 S1 C23 101.13(11) . . ? S1 O3 Cu1 139.21(10) . . ? F1 C23 F3 107.9(2) . . ? F1 C23 F2 107.6(2) . . ? F3 C23 F2 106.9(2) . . ? F1 C23 S1 111.74(17) . . ? F3 C23 S1 112.06(18) . . ? F2 C23 S1 110.45(19) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.09 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.692 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.086