data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Brian Mann' _publ_contact_author_email b.mann@sheffield.ac.uk loop_ _publ_author_name L.Hewison S.Crook T.R.Johnson B.E.Mann H.Adams P.Sawle ; R.Motterlini ; # Attachment 'ime114.cif' data_ime114 _database_code_depnum_ccdc_archive 'CCDC 640144' #TrackingRef 'ime114.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H7 Cl4 Fe2 O5' _chemical_formula_weight 460.66 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.0283(6) _cell_length_b 23.800(2) _cell_length_c 9.6737(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.931(4) _cell_angle_gamma 90.00 _cell_volume 1617.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7004 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.85 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.891 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 2.466 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5891 _exptl_absorpt_correction_T_max 0.7086 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 31667 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0115 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.85 _reflns_number_total 3830 _reflns_number_gt 3667 _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^)+(0.0295P)^2^+0.7489P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3830 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0203 _refine_ls_R_factor_gt 0.0192 _refine_ls_wR_factor_ref 0.0534 _refine_ls_wR_factor_gt 0.0528 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.70696(2) 0.155788(7) 0.785738(18) 0.01464(6) Uani 1 1 d . . . Fe2 Fe 0.29351(3) 0.118218(8) 0.23533(2) 0.01961(6) Uani 1 1 d . . . Cl1 Cl 0.36144(5) 0.047680(14) 0.37184(4) 0.02830(8) Uani 1 1 d . . . Cl3 Cl 0.16169(6) 0.089848(19) 0.04157(4) 0.03675(10) Uani 1 1 d . . . Cl2 Cl 0.09832(6) 0.174543(17) 0.34291(4) 0.03740(10) Uani 1 1 d . . . Cl4 Cl 0.55375(6) 0.166616(19) 0.19455(4) 0.03760(10) Uani 1 1 d . . . O1 O 0.34062(14) 0.20705(4) 0.85777(11) 0.0268(2) Uani 1 1 d . . . O2 O 0.6444(2) 0.05089(5) 0.94072(13) 0.0396(3) Uani 1 1 d . . . O3 O 0.90748(16) 0.21773(5) 1.00598(12) 0.0350(3) Uani 1 1 d . . . O4 O 1.23601(14) 0.10436(4) 0.69505(11) 0.0246(2) Uani 1 1 d . . . O5 O 1.01974(14) 0.03446(4) 0.69369(12) 0.0291(2) Uani 1 1 d . . . C1 C 0.47980(19) 0.18650(5) 0.83220(14) 0.0193(2) Uani 1 1 d . . . C2 C 0.6685(2) 0.09135(6) 0.88350(15) 0.0242(3) Uani 1 1 d . . . C3 C 0.83121(19) 0.19253(6) 0.92370(14) 0.0222(3) Uani 1 1 d . . . C4 C 0.72335(19) 0.10849(6) 0.60317(14) 0.0206(3) Uani 1 1 d . . . H4A H 0.6764 0.0692 0.5896 0.025 Uiso 1 1 calc R . . C5 C 0.91063(18) 0.12461(5) 0.64999(13) 0.0180(2) Uani 1 1 d . . . C6 C 0.91913(18) 0.18422(6) 0.65069(13) 0.0189(2) Uani 1 1 d . . . H6A H 1.0326 0.2074 0.6774 0.023 Uiso 1 1 calc R . . C7 C 0.73867(19) 0.20530(6) 0.60837(14) 0.0215(3) Uani 1 1 d . . . H7A H 0.7030 0.2458 0.5986 0.026 Uiso 1 1 calc R . . C8 C 0.6190(2) 0.15815(6) 0.57686(14) 0.0219(3) Uani 1 1 d . . . H8A H 0.4843 0.1601 0.5422 0.026 Uiso 1 1 calc R . . C9 C 1.07561(19) 0.08725(6) 0.68284(13) 0.0192(2) Uani 1 1 d . . . C10 C 1.1696(2) -0.00613(7) 0.7215(2) 0.0359(4) Uani 1 1 d . . . H10A H 1.1142 -0.0438 0.7276 0.054 Uiso 1 1 calc R . . H10B H 1.2340 0.0032 0.8091 0.054 Uiso 1 1 calc R . . H10C H 1.2616 -0.0052 0.6465 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01309(9) 0.01639(9) 0.01444(9) -0.00034(6) 0.00017(7) -0.00119(6) Fe2 0.02273(10) 0.01954(10) 0.01663(10) 0.00056(7) 0.00266(7) 0.00140(7) Cl1 0.03243(18) 0.02132(16) 0.03092(18) 0.00470(13) -0.00662(14) 0.00094(13) Cl3 0.0425(2) 0.0454(2) 0.02203(17) -0.00318(15) -0.00694(15) 0.00063(17) Cl2 0.0491(2) 0.03045(19) 0.0332(2) 0.00339(15) 0.01830(18) 0.01478(16) Cl4 0.0349(2) 0.0412(2) 0.0369(2) 0.00252(17) 0.00861(16) -0.01290(16) O1 0.0193(5) 0.0279(5) 0.0335(6) -0.0068(4) 0.0028(4) 0.0021(4) O2 0.0521(7) 0.0261(6) 0.0410(7) 0.0109(5) 0.0131(6) 0.0011(5) O3 0.0299(5) 0.0461(7) 0.0287(6) -0.0073(5) -0.0062(5) -0.0122(5) O4 0.0174(4) 0.0272(5) 0.0292(5) -0.0033(4) 0.0004(4) -0.0013(4) O5 0.0204(5) 0.0192(5) 0.0479(7) 0.0023(5) 0.0040(5) 0.0009(4) C1 0.0199(6) 0.0199(6) 0.0182(6) -0.0022(5) -0.0006(5) -0.0041(5) C2 0.0249(7) 0.0244(7) 0.0233(7) -0.0003(5) 0.0046(5) 0.0018(5) C3 0.0171(6) 0.0278(7) 0.0219(6) 0.0010(5) 0.0007(5) -0.0027(5) C4 0.0203(6) 0.0246(6) 0.0169(6) -0.0049(5) 0.0006(5) -0.0028(5) C5 0.0175(6) 0.0207(6) 0.0159(6) -0.0015(5) 0.0031(5) -0.0010(5) C6 0.0178(6) 0.0210(6) 0.0181(6) 0.0022(5) 0.0042(5) -0.0022(5) C7 0.0235(6) 0.0240(6) 0.0171(6) 0.0048(5) 0.0014(5) 0.0006(5) C8 0.0199(6) 0.0313(7) 0.0144(6) -0.0001(5) -0.0016(5) 0.0001(5) C9 0.0188(6) 0.0209(6) 0.0179(6) -0.0024(5) 0.0041(5) 0.0000(5) C10 0.0296(8) 0.0245(7) 0.0538(10) 0.0056(7) 0.0057(7) 0.0090(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C3 1.8085(14) . ? Fe1 C1 1.8189(14) . ? Fe1 C2 1.8242(15) . ? Fe1 C5 2.0941(13) . ? Fe1 C7 2.0963(13) . ? Fe1 C4 2.0991(13) . ? Fe1 C8 2.1042(13) . ? Fe1 C6 2.1099(13) . ? Fe2 Cl1 2.1839(4) . ? Fe2 Cl3 2.1843(4) . ? Fe2 Cl2 2.1928(4) . ? Fe2 Cl4 2.2026(4) . ? O1 C1 1.1249(17) . ? O2 C2 1.1248(19) . ? O3 C3 1.1255(18) . ? O4 C9 1.2026(17) . ? O5 C9 1.3212(17) . ? O5 C10 1.4508(18) . ? C4 C8 1.412(2) . ? C4 C5 1.4372(18) . ? C4 H4A 1.0000 . ? C5 C6 1.4201(18) . ? C5 C9 1.4913(18) . ? C6 C7 1.4181(19) . ? C6 H6A 1.0000 . ? C7 C8 1.432(2) . ? C7 H7A 1.0000 . ? C8 H8A 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Fe1 C1 92.21(6) . . ? C3 Fe1 C2 95.61(7) . . ? C1 Fe1 C2 94.10(6) . . ? C3 Fe1 C5 107.90(6) . . ? C1 Fe1 C5 155.37(6) . . ? C2 Fe1 C5 97.81(6) . . ? C3 Fe1 C7 106.01(6) . . ? C1 Fe1 C7 94.69(6) . . ? C2 Fe1 C7 156.28(6) . . ? C5 Fe1 C7 66.62(5) . . ? C3 Fe1 C4 147.97(6) . . ? C1 Fe1 C4 118.93(6) . . ? C2 Fe1 C4 89.77(6) . . ? C5 Fe1 C4 40.09(5) . . ? C7 Fe1 C4 66.72(6) . . ? C3 Fe1 C8 145.75(6) . . ? C1 Fe1 C8 88.92(6) . . ? C2 Fe1 C8 118.46(6) . . ? C5 Fe1 C8 66.45(5) . . ? C7 Fe1 C8 39.87(5) . . ? C4 Fe1 C8 39.25(5) . . ? C3 Fe1 C6 87.95(6) . . ? C1 Fe1 C6 131.01(6) . . ? C2 Fe1 C6 134.66(6) . . ? C5 Fe1 C6 39.48(5) . . ? C7 Fe1 C6 39.40(5) . . ? C4 Fe1 C6 66.55(5) . . ? C8 Fe1 C6 66.20(5) . . ? Cl1 Fe2 Cl3 111.516(18) . . ? Cl1 Fe2 Cl2 108.378(18) . . ? Cl3 Fe2 Cl2 109.65(2) . . ? Cl1 Fe2 Cl4 109.651(18) . . ? Cl3 Fe2 Cl4 110.478(19) . . ? Cl2 Fe2 Cl4 107.04(2) . . ? C9 O5 C10 115.61(12) . . ? O1 C1 Fe1 177.49(13) . . ? O2 C2 Fe1 178.25(14) . . ? O3 C3 Fe1 176.64(14) . . ? C8 C4 C5 107.68(12) . . ? C8 C4 Fe1 70.57(8) . . ? C5 C4 Fe1 69.77(7) . . ? C8 C4 H4A 126.2 . . ? C5 C4 H4A 126.2 . . ? Fe1 C4 H4A 126.2 . . ? C6 C5 C4 107.85(12) . . ? C6 C5 C9 124.20(12) . . ? C4 C5 C9 127.80(12) . . ? C6 C5 Fe1 70.86(7) . . ? C4 C5 Fe1 70.14(7) . . ? C9 C5 Fe1 127.93(9) . . ? C7 C6 C5 108.34(12) . . ? C7 C6 Fe1 69.78(7) . . ? C5 C6 Fe1 69.66(7) . . ? C7 C6 H6A 125.8 . . ? C5 C6 H6A 125.8 . . ? Fe1 C6 H6A 125.8 . . ? C6 C7 C8 107.68(12) . . ? C6 C7 Fe1 70.82(7) . . ? C8 C7 Fe1 70.36(8) . . ? C6 C7 H7A 126.1 . . ? C8 C7 H7A 126.1 . . ? Fe1 C7 H7A 126.1 . . ? C4 C8 C7 108.42(12) . . ? C4 C8 Fe1 70.18(8) . . ? C7 C8 Fe1 69.77(8) . . ? C4 C8 H8A 125.8 . . ? C7 C8 H8A 125.8 . . ? Fe1 C8 H8A 125.8 . . ? O4 C9 O5 126.41(13) . . ? O4 C9 C5 122.92(12) . . ? O5 C9 C5 110.66(11) . . ? O5 C10 H10A 109.5 . . ? O5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.548 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.080 # Attachment 'ime148.cif' data_ime148 _database_code_depnum_ccdc_archive 'CCDC 766622' #TrackingRef 'ime148.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H10 B F4 Fe N O2' _chemical_formula_weight 354.88 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6851(8) _cell_length_b 18.7238(16) _cell_length_c 7.7446(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.239(4) _cell_angle_gamma 90.00 _cell_volume 1398.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9804 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 36.12 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 1.128 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6427 _exptl_absorpt_correction_T_max 0.8059 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number ? _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 47413 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 36.42 _reflns_number_total 6726 _reflns_number_gt 5968 _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^)+(0.0268P)^2^+0.9580P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6726 _refine_ls_number_parameters 210 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_restrained_S_all 1.167 _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 Fe1 Fe 0.189620(17) 0.433164(9) 0.32314(2) 0.01658(4) Uani 1 1 d . . . O1 O 0.17852(13) 0.32879(7) 0.03770(15) 0.0341(2) Uani 1 1 d . . . O2 O -0.04209(10) 0.52233(6) 0.18250(14) 0.02534(19) Uani 1 1 d . . . N1 N 0.07617(11) 0.37752(6) 0.46415(14) 0.02050(19) Uani 1 1 d . . . C1 C 0.17978(13) 0.36850(8) 0.14858(17) 0.0230(2) Uani 1 1 d . . . C2 C 0.04605(13) 0.48608(7) 0.23360(16) 0.0198(2) Uani 1 1 d . . . C3 C 0.40660(12) 0.41492(7) 0.40689(16) 0.0201(2) Uani 1 1 d . . . C4 C 0.38517(13) 0.46405(8) 0.26278(17) 0.0228(2) Uani 1 1 d . . . H4A H 0.4227 0.4587 0.1474 0.027 Uiso 1 1 calc R . . C5 C 0.31181(13) 0.52393(7) 0.31911(17) 0.0223(2) Uani 1 1 d . . . H5A H 0.2883 0.5679 0.2493 0.027 Uiso 1 1 calc R . . C6 C 0.27845(13) 0.51165(7) 0.49259(16) 0.0197(2) Uani 1 1 d . . . H6A H 0.2273 0.5451 0.5648 0.024 Uiso 1 1 calc R . . C7 C 0.34230(12) 0.44553(6) 0.54919(16) 0.01797(19) Uani 1 1 d . . . C8 C 0.34627(13) 0.40887(7) 0.71051(17) 0.0217(2) Uani 1 1 d . . . H8A H 0.3022 0.4280 0.8049 0.026 Uiso 1 1 calc R . . C9 C 0.41549(15) 0.34518(8) 0.7256(2) 0.0274(3) Uani 1 1 d . . . H9A H 0.4195 0.3201 0.8326 0.033 Uiso 1 1 calc R . . C10 C 0.48190(15) 0.31527(8) 0.5851(2) 0.0299(3) Uani 1 1 d . . . H10A H 0.5300 0.2712 0.6015 0.036 Uiso 1 1 calc R . . C11 C 0.47789(14) 0.34835(8) 0.4283(2) 0.0264(3) Uani 1 1 d . . . H11A H 0.5215 0.3276 0.3353 0.032 Uiso 1 1 calc R . . C12 C 0.00771(13) 0.34293(7) 0.54221(16) 0.0211(2) Uani 1 1 d . . . C13 C -0.08363(16) 0.29909(8) 0.6384(2) 0.0298(3) Uani 1 1 d . . . H13A H -0.1754 0.2963 0.5739 0.045 Uiso 1 1 calc R . . H13B H -0.0922 0.3206 0.7523 0.045 Uiso 1 1 calc R . . H13C H -0.0447 0.2510 0.6535 0.045 Uiso 1 1 calc R . . B1 B 0.74735(15) 0.37218(8) 0.08928(18) 0.0209(2) Uani 1 1 d D . . F1 F 0.6753(8) 0.3201(2) -0.0083(15) 0.0463(14) Uani 0.71(4) 1 d PDU A 1 F1' F 0.646(2) 0.3232(10) 0.034(3) 0.050(2) Uani 0.29(4) 1 d PDU A 2 F2 F 0.86758(11) 0.38055(6) 0.00837(16) 0.0408(2) Uani 1 1 d . A . F3 F 0.67624(11) 0.43657(6) 0.08755(14) 0.0370(2) Uani 1 1 d . A . F4 F 0.78309(14) 0.35075(7) 0.25879(13) 0.0501(3) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01438(7) 0.02018(8) 0.01527(7) -0.00016(6) 0.00190(5) -0.00438(5) O1 0.0350(6) 0.0374(6) 0.0306(5) -0.0128(5) 0.0067(4) -0.0041(5) O2 0.0214(4) 0.0286(5) 0.0258(5) 0.0007(4) 0.0005(3) 0.0009(3) N1 0.0187(4) 0.0233(5) 0.0195(4) -0.0003(4) 0.0017(3) -0.0040(3) C1 0.0189(5) 0.0276(6) 0.0227(5) -0.0019(4) 0.0037(4) -0.0046(4) C2 0.0188(5) 0.0234(5) 0.0177(5) -0.0014(4) 0.0032(4) -0.0046(4) C3 0.0139(4) 0.0245(5) 0.0222(5) -0.0019(4) 0.0027(4) -0.0042(4) C4 0.0177(5) 0.0305(6) 0.0207(5) 0.0010(4) 0.0037(4) -0.0084(4) C5 0.0204(5) 0.0236(5) 0.0224(5) 0.0038(4) -0.0008(4) -0.0083(4) C6 0.0196(5) 0.0194(5) 0.0195(5) -0.0005(4) -0.0018(4) -0.0034(4) C7 0.0145(4) 0.0197(5) 0.0194(5) -0.0002(4) -0.0002(3) -0.0028(3) C8 0.0194(5) 0.0250(6) 0.0201(5) 0.0037(4) -0.0008(4) -0.0009(4) C9 0.0232(6) 0.0265(6) 0.0317(7) 0.0081(5) -0.0016(5) 0.0000(5) C10 0.0227(6) 0.0231(6) 0.0438(8) 0.0021(5) 0.0018(5) 0.0026(5) C11 0.0181(5) 0.0256(6) 0.0361(7) -0.0053(5) 0.0056(5) -0.0011(4) C12 0.0214(5) 0.0216(5) 0.0207(5) -0.0003(4) 0.0044(4) -0.0027(4) C13 0.0317(7) 0.0264(6) 0.0330(7) 0.0044(5) 0.0126(6) -0.0065(5) B1 0.0193(5) 0.0241(6) 0.0193(5) 0.0028(5) 0.0021(4) -0.0014(4) F1 0.0274(15) 0.0350(10) 0.073(3) -0.0021(12) -0.0147(16) -0.0103(8) F1' 0.036(4) 0.043(3) 0.069(4) 0.012(2) -0.010(3) -0.027(3) F2 0.0361(5) 0.0369(5) 0.0534(6) 0.0009(5) 0.0262(5) -0.0009(4) F3 0.0397(5) 0.0384(5) 0.0338(5) 0.0036(4) 0.0077(4) 0.0182(4) F4 0.0600(7) 0.0698(8) 0.0212(4) 0.0106(5) 0.0072(4) 0.0357(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C2 1.7944(13) . ? Fe1 C1 1.8109(14) . ? Fe1 N1 1.9247(11) . ? Fe1 C5 2.0728(12) . ? Fe1 C4 2.0740(12) . ? Fe1 C6 2.1013(12) . ? Fe1 C3 2.1690(12) . ? Fe1 C7 2.1983(12) . ? O1 C1 1.1350(17) . ? O2 C2 1.1332(16) . ? N1 C12 1.1393(16) . ? C3 C11 1.427(2) . ? C3 C7 1.4338(17) . ? C3 C4 1.4466(19) . ? C4 C5 1.417(2) . ? C4 H4A 1.0000 . ? C5 C6 1.4289(18) . ? C5 H5A 1.0000 . ? C6 C7 1.4345(18) . ? C6 H6A 1.0000 . ? C7 C8 1.4230(17) . ? C8 C9 1.368(2) . ? C8 H8A 0.9500 . ? C9 C10 1.428(2) . ? C9 H9A 0.9500 . ? C10 C11 1.361(2) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C13 1.4600(18) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? B1 F1' 1.380(3) . ? B1 F2 1.3808(17) . ? B1 F1 1.383(2) . ? B1 F4 1.3861(17) . ? B1 F3 1.3879(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe1 C1 95.43(6) . . ? C2 Fe1 N1 93.20(5) . . ? C1 Fe1 N1 93.89(5) . . ? C2 Fe1 C5 87.98(5) . . ? C1 Fe1 C5 121.88(6) . . ? N1 Fe1 C5 143.96(5) . . ? C2 Fe1 C4 116.76(6) . . ? C1 Fe1 C4 90.29(6) . . ? N1 Fe1 C4 149.23(5) . . ? C5 Fe1 C4 39.97(6) . . ? C2 Fe1 C6 96.53(5) . . ? C1 Fe1 C6 157.59(5) . . ? N1 Fe1 C6 104.27(5) . . ? C5 Fe1 C6 40.03(5) . . ? C4 Fe1 C6 67.39(5) . . ? C2 Fe1 C3 153.89(5) . . ? C1 Fe1 C3 95.82(5) . . ? N1 Fe1 C3 109.44(5) . . ? C5 Fe1 C3 66.09(5) . . ? C4 Fe1 C3 39.79(5) . . ? C6 Fe1 C3 65.99(5) . . ? C2 Fe1 C7 133.69(5) . . ? C1 Fe1 C7 130.59(6) . . ? N1 Fe1 C7 89.00(5) . . ? C5 Fe1 C7 65.30(5) . . ? C4 Fe1 C7 65.70(5) . . ? C6 Fe1 C7 38.90(5) . . ? C3 Fe1 C7 38.33(5) . . ? C12 N1 Fe1 177.34(11) . . ? O1 C1 Fe1 177.36(12) . . ? O2 C2 Fe1 176.43(12) . . ? C11 C3 C7 119.96(12) . . ? C11 C3 C4 132.74(12) . . ? C7 C3 C4 107.28(11) . . ? C11 C3 Fe1 128.13(9) . . ? C7 C3 Fe1 71.94(7) . . ? C4 C3 Fe1 66.57(7) . . ? C5 C4 C3 107.83(11) . . ? C5 C4 Fe1 69.97(7) . . ? C3 C4 Fe1 73.64(7) . . ? C5 C4 H4A 126.0 . . ? C3 C4 H4A 126.0 . . ? Fe1 C4 H4A 126.0 . . ? C4 C5 C6 108.96(11) . . ? C4 C5 Fe1 70.06(7) . . ? C6 C5 Fe1 71.06(7) . . ? C4 C5 H5A 125.5 . . ? C6 C5 H5A 125.5 . . ? Fe1 C5 H5A 125.5 . . ? C5 C6 C7 107.34(11) . . ? C5 C6 Fe1 68.91(7) . . ? C7 C6 Fe1 74.20(7) . . ? C5 C6 H6A 126.2 . . ? C7 C6 H6A 126.2 . . ? Fe1 C6 H6A 126.2 . . ? C8 C7 C3 120.21(12) . . ? C8 C7 C6 131.37(12) . . ? C3 C7 C6 108.39(11) . . ? C8 C7 Fe1 127.64(9) . . ? C3 C7 Fe1 69.73(7) . . ? C6 C7 Fe1 66.90(7) . . ? C9 C8 C7 117.98(13) . . ? C9 C8 H8A 121.0 . . ? C7 C8 H8A 121.0 . . ? C8 C9 C10 121.89(13) . . ? C8 C9 H9A 119.1 . . ? C10 C9 H9A 119.1 . . ? C11 C10 C9 121.57(13) . . ? C11 C10 H10A 119.2 . . ? C9 C10 H10A 119.2 . . ? C10 C11 C3 118.37(13) . . ? C10 C11 H11A 120.8 . . ? C3 C11 H11A 120.8 . . ? N1 C12 C13 178.24(15) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? F1' B1 F2 122.5(13) . . ? F1' B1 F1 18.9(8) . . ? F2 B1 F1 103.7(5) . . ? F1' B1 F4 102.1(6) . . ? F2 B1 F4 108.34(12) . . ? F1 B1 F4 112.5(5) . . ? F1' B1 F3 103.8(11) . . ? F2 B1 F3 109.59(12) . . ? F1 B1 F3 112.5(2) . . ? F4 B1 F3 109.97(12) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 36.42 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.795 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.071 # Attachment '[(Ind)Fe(CO)2(PPh3)][BF4]CHCl3.cif' data_ch1tj2 _database_code_depnum_ccdc_archive 'CCDC 766623' #TrackingRef '[(Ind)Fe(CO)2(PPh3)][BF4]CHCl3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H23 B Cl3 F4 Fe O2 P' _chemical_formula_weight 695.46 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.4217(5) _cell_length_b 11.0573(5) _cell_length_c 28.4413(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2963.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1923 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 27.48 _exptl_crystal_description NEEDLE _exptl_crystal_colour 'clear pale orange' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.887 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8288 _exptl_absorpt_correction_T_max 0.8638 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 58444 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6787 _reflns_number_gt 6489 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0351P)^2^+0.7977P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(9) _refine_ls_number_reflns 6787 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0621 _refine_ls_wR_factor_gt 0.0611 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.77991(3) 0.03484(2) 0.087948(8) 0.01487(6) Uani 1 1 d . . . C1 C 0.7552(2) -0.10920(16) 0.11572(6) 0.0214(4) Uani 1 1 d . . . O1 O 0.73478(18) -0.20001(13) 0.13260(5) 0.0351(3) Uani 1 1 d . . . C2 C 0.6633(2) 0.11390(17) 0.12709(6) 0.0207(4) Uani 1 1 d . . . O2 O 0.58322(15) 0.16292(14) 0.15055(5) 0.0306(3) Uani 1 1 d . . . C3 C 0.84147(19) -0.03469(18) 0.02233(6) 0.0199(3) Uani 1 1 d . . . H3 H 0.8953 -0.1048 0.0194 0.024 Uiso 1 1 calc R . . C4 C 0.89514(19) 0.08401(18) 0.02832(6) 0.0204(4) Uani 1 1 d . . . H4 H 0.9905 0.1056 0.0280 0.025 Uiso 1 1 calc R . . C5 C 0.7793(2) 0.16488(16) 0.03486(6) 0.0196(3) Uani 1 1 d . . . H5 H 0.7857 0.2470 0.0417 0.024 Uiso 1 1 calc R . . C6 C 0.65023(19) 0.09627(16) 0.02893(6) 0.0174(3) Uani 1 1 d . . . C7 C 0.5042(2) 0.12999(16) 0.02928(6) 0.0198(4) Uani 1 1 d . . . H7 H 0.4769 0.2094 0.0352 0.024 Uiso 1 1 calc R . . C8 C 0.40596(19) 0.04274(18) 0.02069(6) 0.0219(4) Uani 1 1 d . . . H8 H 0.3105 0.0640 0.0200 0.026 Uiso 1 1 calc R . . C9 C 0.4446(2) -0.08037(17) 0.01274(6) 0.0221(4) Uani 1 1 d . . . H9 H 0.3740 -0.1368 0.0064 0.027 Uiso 1 1 calc R . . C10 C 0.5826(2) -0.11710(16) 0.01424(6) 0.0203(4) Uani 1 1 d . . . H10 H 0.6066 -0.1981 0.0106 0.024 Uiso 1 1 calc R . . C11 C 0.68872(18) -0.02781(17) 0.02158(6) 0.0177(3) Uani 1 1 d . . . P1 P 0.96844(4) 0.07771(4) 0.132660(15) 0.01506(9) Uani 1 1 d . . . C12 C 1.0513(2) 0.22265(15) 0.11813(6) 0.0172(3) Uani 1 1 d . . . C13 C 1.19701(19) 0.23155(16) 0.10974(6) 0.0203(4) Uani 1 1 d . . . H13 H 1.2539 0.1629 0.1114 0.024 Uiso 1 1 calc R . . C14 C 1.2573(2) 0.34344(17) 0.09882(7) 0.0236(4) Uani 1 1 d . . . H14 H 1.3544 0.3494 0.0935 0.028 Uiso 1 1 calc R . . C15 C 1.1730(2) 0.44528(16) 0.09598(6) 0.0232(4) Uani 1 1 d . . . H15 H 1.2138 0.5197 0.0889 0.028 Uiso 1 1 calc R . . C16 C 1.0279(2) 0.43755(16) 0.10360(6) 0.0225(4) Uani 1 1 d . . . H16 H 0.9715 0.5064 0.1015 0.027 Uiso 1 1 calc R . . C17 C 0.9670(2) 0.32635(16) 0.11437(6) 0.0196(3) Uani 1 1 d . . . H17 H 0.8695 0.3209 0.1191 0.024 Uiso 1 1 calc R . . C18 C 1.11479(17) -0.03035(16) 0.13269(6) 0.0168(3) Uani 1 1 d . . . C19 C 1.1235(2) -0.12390(16) 0.09987(6) 0.0200(4) Uani 1 1 d . . . H19 H 1.0509 -0.1352 0.0781 0.024 Uiso 1 1 calc R . . C20 C 1.2407(2) -0.20024(16) 0.09971(6) 0.0235(4) Uani 1 1 d . . . H20 H 1.2459 -0.2628 0.0779 0.028 Uiso 1 1 calc R . . C21 C 1.3500(2) -0.18396(17) 0.13169(7) 0.0239(4) Uani 1 1 d . . . H21 H 1.4287 -0.2346 0.1310 0.029 Uiso 1 1 calc R . . C22 C 1.3415(2) -0.09170(18) 0.16479(7) 0.0231(4) Uani 1 1 d . . . H22 H 1.4146 -0.0809 0.1864 0.028 Uiso 1 1 calc R . . C23 C 1.2242(2) -0.01568(15) 0.16567(6) 0.0202(3) Uani 1 1 d . . . H23 H 1.2181 0.0451 0.1882 0.024 Uiso 1 1 calc R . . C24 C 0.91897(18) 0.08529(16) 0.19467(6) 0.0178(3) Uani 1 1 d . . . C25 C 0.9005(2) 0.19450(17) 0.21814(7) 0.0221(4) Uani 1 1 d . . . H25 H 0.9218 0.2669 0.2031 0.027 Uiso 1 1 calc R . . C26 C 0.8504(2) 0.19565(19) 0.26403(7) 0.0269(4) Uani 1 1 d . . . H26 H 0.8379 0.2690 0.2795 0.032 Uiso 1 1 calc R . . C27 C 0.8190(2) 0.0886(2) 0.28694(7) 0.0281(4) Uani 1 1 d . . . H27 H 0.7844 0.0901 0.3176 0.034 Uiso 1 1 calc R . . C28 C 0.8393(2) -0.02168(19) 0.26407(7) 0.0255(4) Uani 1 1 d . . . H28 H 0.8200 -0.0939 0.2796 0.031 Uiso 1 1 calc R . . C29 C 0.8886(2) -0.02311(17) 0.21808(6) 0.0219(4) Uani 1 1 d . . . H29 H 0.9016 -0.0965 0.2027 0.026 Uiso 1 1 calc R . . B1 B 1.1117(2) -0.0317(2) -0.06245(7) 0.0204(4) Uani 1 1 d . . . F1 F 1.10491(13) 0.09370(10) -0.05633(4) 0.0291(3) Uani 1 1 d . . . F2 F 1.12754(11) -0.08633(10) -0.01818(4) 0.0250(2) Uani 1 1 d . . . F3 F 0.98745(12) -0.07263(11) -0.08342(4) 0.0316(3) Uani 1 1 d . . . F4 F 1.22720(13) -0.06039(12) -0.09042(4) 0.0362(3) Uani 1 1 d . . . C30 C 1.3607(2) 0.06918(17) 0.30523(7) 0.0235(4) Uani 1 1 d . . . H30 H 1.3745 0.1002 0.3372 0.028 Uiso 1 1 calc R . . Cl1 Cl 1.17794(5) 0.05715(6) 0.294559(19) 0.04187(15) Uani 1 1 d . . . Cl2 Cl 1.43905(6) 0.17103(6) 0.26534(2) 0.04189(14) Uani 1 1 d . . . Cl3 Cl 1.44219(9) -0.07328(6) 0.30111(2) 0.05446(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01651(11) 0.01384(11) 0.01427(11) 0.00050(9) 0.00122(9) -0.00044(9) C1 0.0244(10) 0.0215(9) 0.0184(8) -0.0016(7) -0.0019(7) -0.0031(7) O1 0.0496(9) 0.0217(7) 0.0340(8) 0.0084(6) -0.0069(7) -0.0104(7) C2 0.0203(8) 0.0236(9) 0.0183(8) 0.0011(7) -0.0023(7) -0.0027(7) O2 0.0249(7) 0.0385(8) 0.0284(7) -0.0069(6) 0.0059(6) 0.0047(6) C3 0.0218(8) 0.0218(8) 0.0163(8) -0.0007(7) 0.0019(7) 0.0024(8) C4 0.0197(8) 0.0269(9) 0.0147(8) 0.0021(7) 0.0032(7) -0.0025(8) C5 0.0252(9) 0.0190(8) 0.0146(8) 0.0041(6) 0.0002(7) -0.0025(8) C6 0.0236(9) 0.0163(8) 0.0122(8) 0.0035(6) -0.0003(7) -0.0003(7) C7 0.0247(9) 0.0170(8) 0.0179(8) 0.0007(7) -0.0013(7) 0.0029(7) C8 0.0200(8) 0.0255(9) 0.0201(8) 0.0027(7) -0.0019(7) 0.0031(7) C9 0.0241(9) 0.0225(9) 0.0198(8) 0.0002(7) -0.0025(7) -0.0058(8) C10 0.0268(9) 0.0163(8) 0.0178(8) -0.0007(7) 0.0002(7) -0.0007(7) C11 0.0217(8) 0.0196(8) 0.0119(7) 0.0000(7) 0.0003(6) 0.0009(7) P1 0.0165(2) 0.01322(19) 0.01544(19) -0.00002(16) 0.00100(16) 0.00034(16) C12 0.0216(8) 0.0154(8) 0.0146(8) -0.0010(6) 0.0001(7) -0.0016(7) C13 0.0215(9) 0.0169(8) 0.0224(9) 0.0003(7) 0.0025(7) 0.0006(7) C14 0.0222(9) 0.0247(9) 0.0238(9) -0.0015(7) 0.0046(7) -0.0046(7) C15 0.0338(10) 0.0166(9) 0.0192(8) 0.0005(7) 0.0014(7) -0.0060(7) C16 0.0315(10) 0.0154(9) 0.0206(8) -0.0015(7) -0.0018(7) 0.0018(7) C17 0.0215(9) 0.0182(8) 0.0191(8) -0.0002(7) -0.0005(7) 0.0002(7) C18 0.0175(8) 0.0146(8) 0.0182(8) 0.0034(7) 0.0032(6) 0.0006(7) C19 0.0258(9) 0.0176(8) 0.0166(8) 0.0004(6) -0.0001(7) 0.0000(7) C20 0.0305(10) 0.0187(8) 0.0212(9) 0.0004(7) 0.0042(7) 0.0042(8) C21 0.0230(9) 0.0210(9) 0.0276(10) 0.0072(8) 0.0066(8) 0.0060(7) C22 0.0191(9) 0.0265(10) 0.0238(9) 0.0051(8) 0.0003(7) 0.0010(8) C23 0.0220(8) 0.0193(8) 0.0194(8) 0.0009(7) 0.0025(7) 0.0016(8) C24 0.0159(8) 0.0226(8) 0.0150(8) 0.0003(7) -0.0011(6) 0.0021(7) C25 0.0234(9) 0.0212(9) 0.0216(9) -0.0006(7) 0.0005(7) 0.0008(7) C26 0.0281(10) 0.0293(10) 0.0232(9) -0.0063(8) 0.0008(8) 0.0073(8) C27 0.0266(10) 0.0397(11) 0.0180(9) -0.0004(8) 0.0036(7) 0.0053(9) C28 0.0241(9) 0.0297(10) 0.0228(9) 0.0070(8) 0.0026(7) -0.0005(8) C29 0.0235(9) 0.0212(9) 0.0209(9) 0.0001(7) -0.0001(7) 0.0018(8) B1 0.0229(10) 0.0187(9) 0.0195(9) -0.0027(8) 0.0004(7) -0.0016(8) F1 0.0377(7) 0.0171(5) 0.0326(6) -0.0011(5) -0.0015(5) -0.0031(5) F2 0.0226(5) 0.0252(5) 0.0271(6) 0.0040(5) 0.0000(4) 0.0001(5) F3 0.0274(6) 0.0290(6) 0.0383(7) -0.0047(5) -0.0113(5) -0.0031(5) F4 0.0308(6) 0.0487(7) 0.0292(6) -0.0116(5) 0.0081(5) 0.0016(6) C30 0.0235(9) 0.0250(10) 0.0221(9) -0.0001(7) -0.0004(7) -0.0026(7) Cl1 0.0250(2) 0.0733(4) 0.0274(2) 0.0014(3) -0.00246(19) -0.0127(2) Cl2 0.0410(3) 0.0502(3) 0.0345(3) 0.0122(2) 0.0001(2) -0.0183(3) Cl3 0.0772(5) 0.0315(3) 0.0547(4) -0.0090(3) -0.0038(3) 0.0179(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 Fe1 C2 1.7920(19) . ? Fe1 C1 1.7930(18) . ? Fe1 C5 2.0850(17) . ? Fe1 C4 2.0857(17) . ? Fe1 C3 2.1001(18) . ? Fe1 C6 2.1844(17) . ? Fe1 C11 2.1866(17) . ? Fe1 P1 2.2355(5) . ? C1 O1 1.129(2) . ? C2 O2 1.144(2) . ? C3 C4 1.417(3) . ? C3 C11 1.441(2) . ? C3 H3 0.9300 . ? C4 C5 1.423(3) . ? C4 H4 0.9300 . ? C5 C6 1.443(3) . ? C5 H5 0.9300 . ? C6 C7 1.426(3) . ? C6 C11 1.434(2) . ? C7 C8 1.359(3) . ? C7 H7 0.9300 . ? C8 C9 1.427(3) . ? C8 H8 0.9300 . ? C9 C10 1.363(3) . ? C9 H9 0.9300 . ? C10 C11 1.421(3) . ? C10 H10 0.9300 . ? P1 C18 1.8245(17) . ? P1 C24 1.8260(17) . ? P1 C12 1.8301(17) . ? C12 C13 1.396(3) . ? C12 C17 1.399(2) . ? C13 C14 1.396(3) . ? C13 H13 0.9300 . ? C14 C15 1.381(3) . ? C14 H14 0.9300 . ? C15 C16 1.387(3) . ? C15 H15 0.9300 . ? C16 C17 1.391(2) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.396(2) . ? C18 C23 1.403(2) . ? C19 C20 1.390(3) . ? C19 H19 0.9300 . ? C20 C21 1.385(3) . ? C20 H20 0.9300 . ? C21 C22 1.390(3) . ? C21 H21 0.9300 . ? C22 C23 1.389(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.391(3) . ? C24 C29 1.401(3) . ? C25 C26 1.388(3) . ? C25 H25 0.9300 . ? C26 C27 1.383(3) . ? C26 H26 0.9300 . ? C27 C28 1.395(3) . ? C27 H27 0.9300 . ? C28 C29 1.388(3) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? B1 F4 1.385(2) . ? B1 F3 1.390(2) . ? B1 F1 1.399(2) . ? B1 F2 1.404(2) . ? C30 Cl1 1.7532(19) . ? C30 Cl3 1.756(2) . ? C30 Cl2 1.7609(19) . ? C30 H30 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe1 C1 94.59(8) . . ? C2 Fe1 C5 96.42(8) . . ? C1 Fe1 C5 158.63(7) . . ? C2 Fe1 C4 134.20(8) . . ? C1 Fe1 C4 131.10(8) . . ? C5 Fe1 C4 39.90(7) . . ? C2 Fe1 C3 154.17(8) . . ? C1 Fe1 C3 95.86(8) . . ? C5 Fe1 C3 67.03(7) . . ? C4 Fe1 C3 39.57(7) . . ? C2 Fe1 C6 89.01(7) . . ? C1 Fe1 C6 122.83(7) . . ? C5 Fe1 C6 39.43(7) . . ? C4 Fe1 C6 65.50(7) . . ? C3 Fe1 C6 65.51(7) . . ? C2 Fe1 C11 116.74(7) . . ? C1 Fe1 C11 92.74(7) . . ? C5 Fe1 C11 65.94(7) . . ? C4 Fe1 C11 65.49(7) . . ? C3 Fe1 C11 39.23(7) . . ? C6 Fe1 C11 38.31(6) . . ? C2 Fe1 P1 91.74(6) . . ? C1 Fe1 P1 92.35(6) . . ? C5 Fe1 P1 105.53(5) . . ? C4 Fe1 P1 89.63(5) . . ? C3 Fe1 P1 111.33(5) . . ? C6 Fe1 P1 144.65(5) . . ? C11 Fe1 P1 150.52(5) . . ? O1 C1 Fe1 177.53(18) . . ? O2 C2 Fe1 176.48(17) . . ? C4 C3 C11 108.01(17) . . ? C4 C3 Fe1 69.67(10) . . ? C11 C3 Fe1 73.62(10) . . ? C4 C3 H3 126.0 . . ? C11 C3 H3 126.0 . . ? Fe1 C3 H3 122.4 . . ? C3 C4 C5 108.92(16) . . ? C3 C4 Fe1 70.77(10) . . ? C5 C4 Fe1 70.03(10) . . ? C3 C4 H4 125.5 . . ? C5 C4 H4 125.5 . . ? Fe1 C4 H4 125.3 . . ? C4 C5 C6 107.49(15) . . ? C4 C5 Fe1 70.08(10) . . ? C6 C5 Fe1 74.00(10) . . ? C4 C5 H5 126.3 . . ? C6 C5 H5 126.3 . . ? Fe1 C5 H5 121.4 . . ? C7 C6 C11 119.68(16) . . ? C7 C6 C5 132.45(17) . . ? C11 C6 C5 107.86(15) . . ? C7 C6 Fe1 128.01(13) . . ? C11 C6 Fe1 70.92(10) . . ? C5 C6 Fe1 66.57(9) . . ? C8 C7 C6 118.06(17) . . ? C8 C7 H7 121.0 . . ? C6 C7 H7 121.0 . . ? C7 C8 C9 122.14(17) . . ? C7 C8 H8 118.9 . . ? C9 C8 H8 118.9 . . ? C10 C9 C8 121.50(17) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 117.97(17) . . ? C9 C10 H10 121.0 . . ? C11 C10 H10 121.0 . . ? C10 C11 C6 120.54(16) . . ? C10 C11 C3 131.94(18) . . ? C6 C11 C3 107.50(17) . . ? C10 C11 Fe1 128.57(12) . . ? C6 C11 Fe1 70.76(10) . . ? C3 C11 Fe1 67.15(10) . . ? C18 P1 C24 102.86(8) . . ? C18 P1 C12 104.54(8) . . ? C24 P1 C12 106.67(8) . . ? C18 P1 Fe1 117.51(6) . . ? C24 P1 Fe1 110.87(6) . . ? C12 P1 Fe1 113.36(6) . . ? C13 C12 C17 119.17(16) . . ? C13 C12 P1 121.32(14) . . ? C17 C12 P1 119.50(14) . . ? C14 C13 C12 120.01(17) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 120.11(17) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.52(17) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C17 119.70(17) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C12 120.46(17) . . ? C16 C17 H17 119.8 . . ? C12 C17 H17 119.8 . . ? C19 C18 C23 119.32(16) . . ? C19 C18 P1 121.97(13) . . ? C23 C18 P1 118.67(13) . . ? C20 C19 C18 119.92(17) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 120.62(17) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 119.83(17) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 120.12(17) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C18 120.17(17) . . ? C22 C23 H23 119.9 . . ? C18 C23 H23 119.9 . . ? C25 C24 C29 119.30(15) . . ? C25 C24 P1 122.36(14) . . ? C29 C24 P1 118.16(13) . . ? C26 C25 C24 120.12(18) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C25 120.53(18) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C28 119.91(17) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 119.69(18) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C24 120.43(18) . . ? C28 C29 H29 119.8 . . ? C24 C29 H29 119.8 . . ? F4 B1 F3 109.94(15) . . ? F4 B1 F1 109.54(16) . . ? F3 B1 F1 109.72(16) . . ? F4 B1 F2 109.46(16) . . ? F3 B1 F2 109.52(16) . . ? F1 B1 F2 108.64(15) . . ? Cl1 C30 Cl3 110.47(11) . . ? Cl1 C30 Cl2 110.41(11) . . ? Cl3 C30 Cl2 110.32(11) . . ? Cl1 C30 H30 108.5 . . ? Cl3 C30 H30 108.5 . . ? Cl2 C30 H30 108.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.633 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.051 # Attachment '[(ind)Fe(CO)2{P(OPh)3}][BF4].cif' data_chtj4m _database_code_depnum_ccdc_archive 'CCDC 766624' #TrackingRef '[(ind)Fe(CO)2{P(OPh)3}][BF4].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H22 B1 F4 Fe1 O5 P1' _chemical_formula_sum 'C29 H22 B F4 Fe O5 P' _chemical_formula_weight 624.10 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 13.092(12) _cell_length_b 20.322(12) _cell_length_c 21.77(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.458(17) _cell_angle_gamma 90.00 _cell_volume 5525(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1290 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 23.54 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 0.669 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8143 _exptl_absorpt_correction_T_max 0.9240 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Smart Apex II Bruker' _diffrn_measurement_method 'w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 31374 _diffrn_reflns_av_R_equivalents 0.0967 _diffrn_reflns_av_sigmaI/netI 0.0978 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.67 _reflns_number_total 12567 _reflns_number_gt 8434 _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^)+(0.1040P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.512(19) _refine_ls_number_reflns 12567 _refine_ls_number_parameters 740 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1050 _refine_ls_R_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.1794 _refine_ls_wR_factor_gt 0.1600 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.99920(6) 0.04530(4) -0.00018(4) 0.03019(19) Uani 1 1 d . . . P1 P 0.89590(11) 0.04333(7) 0.05997(7) 0.0305(3) Uani 1 1 d . . . O1 O 0.8972(5) -0.0643(3) -0.0835(3) 0.0756(18) Uani 1 1 d . . . O2 O 0.8897(4) 0.1561(3) -0.0768(3) 0.0646(15) Uani 1 1 d . . . O3 O 0.9256(3) 0.08768(19) 0.12270(18) 0.0340(8) Uani 1 1 d . . . O4 O 0.8921(3) -0.0270(2) 0.0913(2) 0.0384(9) Uani 1 1 d . . . O5 O 0.7738(3) 0.0651(2) 0.03017(18) 0.0351(9) Uani 1 1 d . . . C1 C 0.9339(5) -0.0209(4) -0.0500(3) 0.0460(16) Uani 1 1 d . . . C2 C 0.9300(5) 0.1125(3) -0.0467(3) 0.0400(14) Uani 1 1 d . . . C3 C 1.1480(4) 0.0141(3) -0.0157(3) 0.0343(12) Uani 1 1 d . . . C4 C 1.1337(5) -0.0123(3) 0.0425(3) 0.0386(14) Uani 1 1 d . . . H4 H 1.1283 -0.0576 0.0519 0.046 Uiso 1 1 calc R . . C5 C 1.1289(5) 0.0409(3) 0.0833(3) 0.0405(14) Uani 1 1 d . . . H5 H 1.1251 0.0370 0.1260 0.049 Uiso 1 1 calc R . . C6 C 1.1307(4) 0.1008(3) 0.0506(3) 0.0370(13) Uani 1 1 d . . . H6 H 1.1225 0.1437 0.0659 0.044 Uiso 1 1 calc R . . C7 C 1.1473(4) 0.0848(3) -0.0101(3) 0.0343(12) Uani 1 1 d . . . C8 C 1.1597(5) 0.1244(3) -0.0610(3) 0.0383(13) Uani 1 1 d . . . H8 H 1.1577 0.1710 -0.0585 0.046 Uiso 1 1 calc R . . C9 C 1.1742(5) 0.0948(3) -0.1128(3) 0.0435(15) Uani 1 1 d . . . H9 H 1.1853 0.1210 -0.1464 0.052 Uiso 1 1 calc R . . C10 C 1.1734(5) 0.0250(3) -0.1186(3) 0.0433(15) Uani 1 1 d . . . H10 H 1.1819 0.0055 -0.1565 0.052 Uiso 1 1 calc R . . C11 C 1.1608(5) -0.0137(3) -0.0715(3) 0.0410(14) Uani 1 1 d . . . H11 H 1.1606 -0.0602 -0.0761 0.049 Uiso 1 1 calc R . . C12 C 0.9517(4) 0.1553(3) 0.1266(3) 0.0319(12) Uani 1 1 d . . . C13 C 1.0301(5) 0.1742(3) 0.1812(3) 0.0407(14) Uani 1 1 d . . . H13 H 1.0678 0.1428 0.2120 0.049 Uiso 1 1 calc R . . C14 C 1.0527(5) 0.2412(4) 0.1899(4) 0.0498(17) Uani 1 1 d . . . H14 H 1.1044 0.2561 0.2280 0.060 Uiso 1 1 calc R . . C15 C 1.0010(6) 0.2857(3) 0.1439(4) 0.0491(15) Uani 1 1 d . . . H15 H 1.0196 0.3310 0.1497 0.059 Uiso 1 1 calc R . . C16 C 0.9232(5) 0.2663(3) 0.0898(3) 0.0417(14) Uani 1 1 d . . . H16 H 0.8871 0.2980 0.0588 0.050 Uiso 1 1 calc R . . C17 C 0.8966(4) 0.2000(3) 0.0800(3) 0.0347(12) Uani 1 1 d . . . H17 H 0.8425 0.1858 0.0426 0.042 Uiso 1 1 calc R . . C18 C 0.8514(5) -0.0372(3) 0.1436(3) 0.0363(13) Uani 1 1 d . . . C19 C 0.7431(5) -0.0412(3) 0.1341(3) 0.0403(14) Uani 1 1 d . . . H19 H 0.6939 -0.0372 0.0921 0.048 Uiso 1 1 calc R . . C20 C 0.7075(5) -0.0512(3) 0.1866(3) 0.0429(15) Uani 1 1 d . . . H20 H 0.6326 -0.0538 0.1804 0.052 Uiso 1 1 calc R . . C21 C 0.7763(6) -0.0573(3) 0.2474(4) 0.0485(16) Uani 1 1 d . . . H21 H 0.7498 -0.0640 0.2830 0.058 Uiso 1 1 calc R . . C22 C 0.8857(5) -0.0537(3) 0.2562(3) 0.0454(16) Uani 1 1 d . . . H22 H 0.9344 -0.0584 0.2982 0.055 Uiso 1 1 calc R . . C23 C 0.9245(5) -0.0434(3) 0.2041(3) 0.0426(14) Uani 1 1 d . . . H23 H 0.9993 -0.0406 0.2100 0.051 Uiso 1 1 calc R . . C24 C 0.7085(5) 0.0519(3) -0.0323(3) 0.0339(12) Uani 1 1 d . . . C25 C 0.6581(5) 0.1058(3) -0.0688(3) 0.0401(14) Uani 1 1 d . . . H25 H 0.6716 0.1492 -0.0522 0.048 Uiso 1 1 calc R . . C26 C 0.5885(5) 0.0947(3) -0.1291(3) 0.0464(15) Uani 1 1 d . . . H26 H 0.5519 0.1307 -0.1540 0.056 Uiso 1 1 calc R . . C27 C 0.5710(5) 0.0316(3) -0.1541(3) 0.0464(16) Uani 1 1 d . . . H27 H 0.5243 0.0248 -0.1964 0.056 Uiso 1 1 calc R . . C28 C 0.6208(5) -0.0206(3) -0.1182(3) 0.0415(14) Uani 1 1 d . . . H28 H 0.6082 -0.0638 -0.1355 0.050 Uiso 1 1 calc R . . C29 C 0.6909(5) -0.0110(3) -0.0554(3) 0.0373(13) Uani 1 1 d . . . H29 H 0.7249 -0.0472 -0.0298 0.045 Uiso 1 1 calc R . . Fe2 Fe 1.08501(6) 0.70471(4) 0.17125(4) 0.03035(19) Uani 1 1 d . . . P2 P 0.92162(11) 0.70660(7) 0.11145(7) 0.0299(3) Uani 1 1 d . . . O101 O 1.0671(4) 0.8141(3) 0.2548(3) 0.0729(17) Uani 1 1 d . . . O102 O 1.0523(4) 0.5939(3) 0.2481(3) 0.0666(15) Uani 1 1 d . . . O103 O 0.8884(3) 0.66230(19) 0.04894(18) 0.0351(9) Uani 1 1 d . . . O104 O 0.8866(3) 0.7772(2) 0.0801(2) 0.0382(9) Uani 1 1 d . . . O105 O 0.8292(3) 0.6847(2) 0.14149(19) 0.0367(9) Uani 1 1 d . . . C101 C 1.0704(5) 0.7720(4) 0.2221(3) 0.0490(17) Uani 1 1 d . . . C102 C 1.0622(5) 0.6369(4) 0.2185(3) 0.0435(15) Uani 1 1 d . . . C103 C 1.2491(4) 0.7357(3) 0.1871(3) 0.0322(12) Uani 1 1 d . . . C104 C 1.1770(5) 0.7619(3) 0.1293(3) 0.0388(14) Uani 1 1 d . . . H104 H 1.1630 0.8072 0.1201 0.047 Uiso 1 1 calc R . . C105 C 1.1302(5) 0.7092(3) 0.0881(3) 0.0393(14) Uani 1 1 d . . . H105 H 1.0832 0.7132 0.0456 0.047 Uiso 1 1 calc R . . C106 C 1.1657(5) 0.6493(3) 0.1214(3) 0.0363(13) Uani 1 1 d . . . H106 H 1.1423 0.6064 0.1061 0.044 Uiso 1 1 calc R . . C107 C 1.2429(4) 0.6646(3) 0.1822(3) 0.0344(12) Uani 1 1 d . . . C108 C 1.3060(5) 0.6249(3) 0.2323(3) 0.0387(13) Uani 1 1 d . . . H108 H 1.3021 0.5782 0.2297 0.046 Uiso 1 1 calc R . . C109 C 1.3724(5) 0.6554(3) 0.2843(3) 0.0424(14) Uani 1 1 d . . . H109 H 1.4167 0.6292 0.3180 0.051 Uiso 1 1 calc R . . C110 C 1.3786(5) 0.7252(4) 0.2908(3) 0.0443(15) Uani 1 1 d . . . H110 H 1.4257 0.7442 0.3286 0.053 Uiso 1 1 calc R . . C111 C 1.3179(5) 0.7649(3) 0.2434(3) 0.0398(14) Uani 1 1 d . . . H111 H 1.3217 0.8114 0.2481 0.048 Uiso 1 1 calc R . . C112 C 0.9102(4) 0.5946(3) 0.0451(3) 0.0307(12) Uani 1 1 d . . . C113 C 0.9335(5) 0.5753(3) -0.0095(3) 0.0402(14) Uani 1 1 d . . . H113 H 0.9390 0.6066 -0.0408 0.048 Uiso 1 1 calc R . . C114 C 0.9490(5) 0.5085(4) -0.0179(4) 0.0516(17) Uani 1 1 d . . . H114 H 0.9636 0.4935 -0.0557 0.062 Uiso 1 1 calc R . . C115 C 0.9434(6) 0.4648(3) 0.0281(4) 0.0483(15) Uani 1 1 d . . . H115 H 0.9564 0.4195 0.0226 0.058 Uiso 1 1 calc R . . C116 C 0.9197(5) 0.4840(3) 0.0817(3) 0.0457(15) Uani 1 1 d . . . H116 H 0.9147 0.4525 0.1129 0.055 Uiso 1 1 calc R . . C117 C 0.9027(4) 0.5499(3) 0.0908(3) 0.0360(13) Uani 1 1 d . . . H117 H 0.8860 0.5641 0.1282 0.043 Uiso 1 1 calc R . . C118 C 0.7935(4) 0.7870(3) 0.0274(3) 0.0330(12) Uani 1 1 d . . . C119 C 0.6947(5) 0.7912(3) 0.0379(3) 0.0409(14) Uani 1 1 d . . . H119 H 0.6878 0.7873 0.0800 0.049 Uiso 1 1 calc R . . C120 C 0.6063(5) 0.8011(3) -0.0151(3) 0.0462(16) Uani 1 1 d . . . H120 H 0.5374 0.8035 -0.0093 0.055 Uiso 1 1 calc R . . C121 C 0.6157(5) 0.8077(3) -0.0759(4) 0.0510(17) Uani 1 1 d . . . H121 H 0.5539 0.8148 -0.1116 0.061 Uiso 1 1 calc R . . C122 C 0.7155(6) 0.8040(3) -0.0847(3) 0.0483(17) Uani 1 1 d . . . H122 H 0.7225 0.8085 -0.1267 0.058 Uiso 1 1 calc R . . C123 C 0.8059(5) 0.7939(3) -0.0326(3) 0.0428(14) Uani 1 1 d . . . H123 H 0.8749 0.7918 -0.0384 0.051 Uiso 1 1 calc R . . C124 C 0.8274(4) 0.6980(3) 0.2041(3) 0.0335(12) Uani 1 1 d . . . C125 C 0.8128(5) 0.6446(3) 0.2401(3) 0.0389(13) Uani 1 1 d . . . H125 H 0.8096 0.6012 0.2234 0.047 Uiso 1 1 calc R . . C126 C 0.8029(5) 0.6555(3) 0.3002(3) 0.0450(15) Uani 1 1 d . . . H126 H 0.7909 0.6194 0.3249 0.054 Uiso 1 1 calc R . . C127 C 0.8102(5) 0.7187(4) 0.3254(3) 0.0473(16) Uani 1 1 d . . . H127 H 0.8051 0.7257 0.3675 0.057 Uiso 1 1 calc R . . C128 C 0.8247(5) 0.7704(3) 0.2893(3) 0.0410(14) Uani 1 1 d . . . H128 H 0.8300 0.8136 0.3067 0.049 Uiso 1 1 calc R . . C129 C 0.8319(5) 0.7613(3) 0.2274(3) 0.0374(13) Uani 1 1 d . . . H129 H 0.8397 0.7977 0.2019 0.045 Uiso 1 1 calc R . . B1 B 0.7605(6) 0.4535(4) 0.2261(3) 0.0408(16) Uani 1 1 d . . . F1 F 0.8410(4) 0.4840(2) 0.2077(2) 0.0617(11) Uani 1 1 d . . . F2 F 0.8044(3) 0.4202(2) 0.28319(18) 0.0515(9) Uani 1 1 d . . . F3 F 0.6890(3) 0.5012(2) 0.23277(18) 0.0516(9) Uani 1 1 d . . . F4 F 0.7067(5) 0.4100(2) 0.1780(2) 0.0826(16) Uani 1 1 d . . . B2 B 0.1211(6) 0.2029(4) 0.4448(3) 0.0410(16) Uani 1 1 d . . . F5 F 0.2193(3) 0.2338(2) 0.4644(2) 0.0637(12) Uani 1 1 d . . . F6 F 0.1136(5) 0.1599(2) 0.4935(2) 0.0800(16) Uani 1 1 d . . . F7 F 0.0417(3) 0.2515(2) 0.43893(18) 0.0522(10) Uani 1 1 d . . . F8 F 0.1071(3) 0.1704(2) 0.38842(18) 0.0516(9) 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 Fe1 0.0251(4) 0.0327(4) 0.0318(4) -0.0002(3) 0.0069(3) 0.0001(3) P1 0.0286(7) 0.0288(7) 0.0343(7) -0.0007(6) 0.0096(6) -0.0001(6) O1 0.055(3) 0.082(4) 0.099(4) -0.055(4) 0.039(3) -0.026(3) O2 0.052(3) 0.083(4) 0.063(3) 0.036(3) 0.022(3) 0.023(3) O3 0.034(2) 0.031(2) 0.037(2) 0.0034(17) 0.0114(16) 0.0001(17) O4 0.037(2) 0.033(2) 0.050(2) -0.0004(18) 0.0191(19) 0.0031(17) O5 0.027(2) 0.037(2) 0.038(2) -0.0085(18) 0.0054(16) -0.0006(17) C1 0.035(3) 0.057(4) 0.050(4) -0.015(3) 0.019(3) -0.003(3) C2 0.029(3) 0.057(4) 0.035(3) 0.014(3) 0.011(2) 0.007(3) C3 0.027(3) 0.033(3) 0.043(3) 0.003(2) 0.012(2) 0.004(2) C4 0.030(3) 0.040(4) 0.043(3) 0.010(3) 0.007(2) 0.007(3) C5 0.024(3) 0.051(4) 0.042(3) 0.000(3) 0.004(2) 0.005(3) C6 0.026(3) 0.036(3) 0.045(3) -0.005(3) 0.004(2) -0.001(2) C7 0.021(3) 0.034(3) 0.045(3) 0.003(3) 0.007(2) 0.001(2) C8 0.030(3) 0.034(3) 0.050(4) 0.010(3) 0.012(3) -0.004(2) C9 0.034(3) 0.054(4) 0.042(3) 0.016(3) 0.010(3) 0.002(3) C10 0.032(3) 0.060(4) 0.038(3) -0.003(3) 0.009(3) 0.008(3) C11 0.037(3) 0.037(3) 0.052(4) 0.005(3) 0.017(3) 0.006(3) C12 0.028(3) 0.039(3) 0.032(3) 0.000(2) 0.014(2) -0.002(2) C13 0.030(3) 0.046(4) 0.043(3) 0.000(3) 0.007(2) 0.000(3) C14 0.038(4) 0.049(4) 0.059(4) -0.015(3) 0.010(3) -0.014(3) C15 0.047(4) 0.038(3) 0.066(4) -0.010(3) 0.024(3) -0.011(3) C16 0.036(3) 0.034(3) 0.059(4) 0.001(3) 0.021(3) -0.002(3) C17 0.028(3) 0.040(3) 0.036(3) 0.001(3) 0.010(2) -0.001(2) C18 0.040(3) 0.028(3) 0.045(3) 0.002(2) 0.019(3) -0.004(2) C19 0.034(3) 0.031(3) 0.054(4) 0.000(3) 0.011(3) -0.002(2) C20 0.034(3) 0.040(4) 0.058(4) 0.002(3) 0.018(3) -0.003(3) C21 0.052(4) 0.037(4) 0.066(4) 0.014(3) 0.031(3) 0.003(3) C22 0.044(4) 0.042(4) 0.049(4) 0.012(3) 0.013(3) 0.010(3) C23 0.031(3) 0.043(4) 0.053(4) 0.012(3) 0.010(3) 0.003(3) C24 0.033(3) 0.033(3) 0.036(3) -0.005(2) 0.012(2) 0.000(2) C25 0.033(3) 0.036(3) 0.050(4) -0.001(3) 0.011(3) 0.003(3) C26 0.038(4) 0.046(4) 0.049(4) 0.003(3) 0.005(3) 0.012(3) C27 0.034(3) 0.058(4) 0.045(4) -0.009(3) 0.008(3) 0.002(3) C28 0.045(4) 0.041(3) 0.040(3) -0.008(3) 0.014(3) -0.003(3) C29 0.035(3) 0.040(3) 0.039(3) 0.004(3) 0.012(2) 0.003(3) Fe2 0.0264(4) 0.0328(4) 0.0318(4) -0.0006(3) 0.0086(3) -0.0002(3) P2 0.0274(7) 0.0284(7) 0.0328(7) -0.0010(6) 0.0074(6) -0.0002(6) O101 0.038(3) 0.086(4) 0.091(4) -0.058(4) 0.013(3) -0.009(3) O102 0.044(3) 0.085(4) 0.067(3) 0.038(3) 0.011(2) -0.004(3) O103 0.035(2) 0.032(2) 0.037(2) 0.0023(17) 0.0075(16) 0.0039(17) O104 0.029(2) 0.031(2) 0.051(2) 0.0002(18) 0.0056(18) 0.0004(16) O105 0.030(2) 0.036(2) 0.046(2) -0.0061(18) 0.0142(18) -0.0040(17) C101 0.025(3) 0.068(5) 0.051(4) -0.017(4) 0.007(3) -0.003(3) C102 0.029(3) 0.062(4) 0.037(3) 0.014(3) 0.006(2) 0.000(3) C103 0.027(3) 0.037(3) 0.035(3) 0.005(2) 0.011(2) 0.000(2) C104 0.041(3) 0.041(4) 0.035(3) 0.009(3) 0.013(3) 0.002(3) C105 0.043(3) 0.047(4) 0.031(3) 0.000(3) 0.016(3) -0.002(3) C106 0.039(3) 0.037(3) 0.035(3) -0.006(2) 0.014(2) -0.001(3) C107 0.029(3) 0.038(3) 0.037(3) 0.001(3) 0.011(2) 0.003(2) C108 0.029(3) 0.032(3) 0.055(4) 0.009(3) 0.012(3) 0.004(2) C109 0.032(3) 0.053(4) 0.039(3) 0.007(3) 0.006(3) 0.006(3) C110 0.031(3) 0.059(4) 0.041(3) 0.001(3) 0.008(3) -0.009(3) C111 0.030(3) 0.039(3) 0.048(4) 0.001(3) 0.009(3) -0.002(3) C112 0.023(3) 0.037(3) 0.029(3) -0.001(2) 0.002(2) 0.001(2) C113 0.027(3) 0.050(4) 0.043(3) 0.003(3) 0.009(2) 0.000(3) C114 0.036(4) 0.060(5) 0.062(4) -0.020(4) 0.020(3) 0.001(3) C115 0.042(3) 0.036(3) 0.064(4) -0.009(3) 0.012(3) 0.003(3) C116 0.032(3) 0.037(3) 0.062(4) 0.002(3) 0.006(3) 0.005(3) C117 0.026(3) 0.042(3) 0.038(3) -0.003(3) 0.005(2) 0.004(2) C118 0.026(3) 0.028(3) 0.041(3) 0.000(2) 0.003(2) 0.000(2) C119 0.038(3) 0.033(3) 0.053(4) 0.000(3) 0.015(3) 0.004(3) C120 0.029(3) 0.046(4) 0.063(4) 0.002(3) 0.012(3) 0.004(3) C121 0.035(3) 0.039(4) 0.073(5) 0.011(3) 0.008(3) 0.005(3) C122 0.050(4) 0.046(4) 0.047(4) 0.009(3) 0.011(3) -0.004(3) C123 0.031(3) 0.041(4) 0.055(4) 0.012(3) 0.011(3) 0.003(3) C124 0.024(3) 0.039(3) 0.036(3) 0.000(2) 0.008(2) 0.000(2) C125 0.037(3) 0.033(3) 0.048(3) -0.002(3) 0.016(3) -0.008(3) C126 0.040(3) 0.048(4) 0.050(4) 0.008(3) 0.017(3) -0.007(3) C127 0.039(4) 0.063(5) 0.042(3) -0.010(3) 0.016(3) -0.007(3) C128 0.033(3) 0.033(3) 0.055(4) -0.003(3) 0.011(3) 0.001(3) C129 0.033(3) 0.038(3) 0.041(3) 0.003(3) 0.011(2) 0.002(3) B1 0.049(4) 0.032(4) 0.040(4) 0.002(3) 0.012(3) -0.006(3) F1 0.059(3) 0.060(3) 0.077(3) 0.017(2) 0.038(2) 0.005(2) F2 0.061(2) 0.050(2) 0.044(2) 0.0098(17) 0.0155(17) 0.0033(19) F3 0.046(2) 0.060(3) 0.050(2) 0.0071(18) 0.0158(17) 0.0054(18) F4 0.128(5) 0.039(2) 0.057(3) -0.006(2) -0.008(3) -0.010(3) B2 0.044(4) 0.039(4) 0.039(4) -0.001(3) 0.010(3) -0.003(3) F5 0.034(2) 0.061(3) 0.084(3) -0.016(2) 0.001(2) -0.0071(19) F6 0.145(5) 0.042(3) 0.058(3) 0.006(2) 0.039(3) -0.010(3) F7 0.040(2) 0.063(3) 0.049(2) -0.0114(18) 0.0062(16) 0.0006(18) F8 0.053(2) 0.054(2) 0.042(2) -0.0097(17) 0.0062(17) -0.0001(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 1.778(7) . ? Fe1 C2 1.779(6) . ? Fe1 C6 2.078(6) . ? Fe1 C5 2.083(6) . ? Fe1 C4 2.086(6) . ? Fe1 P1 2.147(2) . ? Fe1 C7 2.168(6) . ? Fe1 C3 2.169(6) . ? P1 O3 1.584(4) . ? P1 O4 1.590(4) . ? P1 O5 1.596(4) . ? O1 C1 1.153(8) . ? O2 C2 1.132(8) . ? O3 C12 1.413(7) . ? O4 C18 1.409(7) . ? O5 C24 1.399(7) . ? C3 C11 1.395(9) . ? C3 C4 1.439(8) . ? C3 C7 1.442(8) . ? C4 C5 1.411(9) . ? C4 H4 0.9500 . ? C5 C6 1.414(9) . ? C5 H5 0.9500 . ? C6 C7 1.438(9) . ? C6 H6 0.9500 . ? C7 C8 1.419(8) . ? C8 C9 1.340(9) . ? C8 H8 0.9500 . ? C9 C10 1.425(10) . ? C9 H9 0.9500 . ? C10 C11 1.342(9) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.372(8) . ? C12 C17 1.391(8) . ? C13 C14 1.393(10) . ? C13 H13 0.9500 . ? C14 C15 1.368(11) . ? C14 H14 0.9500 . ? C15 C16 1.364(10) . ? C15 H15 0.9500 . ? C16 C17 1.390(8) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.373(9) . ? C18 C23 1.383(9) . ? C19 C20 1.372(9) . ? C19 H19 0.9500 . ? C20 C21 1.365(10) . ? C20 H20 0.9500 . ? C21 C22 1.388(10) . ? C21 H21 0.9500 . ? C22 C23 1.390(9) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C29 1.366(8) . ? C24 C25 1.397(9) . ? C25 C26 1.374(9) . ? C25 H25 0.9500 . ? C26 C27 1.383(10) . ? C26 H26 0.9500 . ? C27 C28 1.363(9) . ? C27 H27 0.9500 . ? C28 C29 1.415(9) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? Fe2 C102 1.797(7) . ? Fe2 C101 1.804(7) . ? Fe2 C106 2.061(6) . ? Fe2 C105 2.068(6) . ? Fe2 C104 2.073(6) . ? Fe2 P2 2.145(2) . ? Fe2 C103 2.165(6) . ? Fe2 C107 2.168(6) . ? P2 O103 1.580(4) . ? P2 O104 1.596(4) . ? P2 O105 1.601(4) . ? O101 C101 1.123(8) . ? O102 C102 1.116(8) . ? O103 C112 1.412(7) . ? O104 C118 1.415(7) . ? O105 C124 1.397(7) . ? C103 C111 1.415(8) . ? C103 C104 1.430(8) . ? C103 C107 1.450(8) . ? C104 C105 1.412(9) . ? C104 H104 0.9500 . ? C105 C106 1.422(9) . ? C105 H105 0.9500 . ? C106 C107 1.438(8) . ? C106 H106 0.9500 . ? C107 C108 1.409(8) . ? C108 C109 1.353(9) . ? C108 H108 0.9500 . ? C109 C110 1.425(10) . ? C109 H109 0.9500 . ? C110 C111 1.362(9) . ? C110 H110 0.9500 . ? C111 H111 0.9500 . ? C112 C113 1.370(8) . ? C112 C117 1.373(8) . ? C113 C114 1.393(10) . ? C113 H113 0.9500 . ? C114 C115 1.358(11) . ? C114 H114 0.9500 . ? C115 C116 1.351(10) . ? C115 H115 0.9500 . ? C116 C117 1.381(9) . ? C116 H116 0.9500 . ? C117 H117 0.9500 . ? C118 C123 1.369(9) . ? C118 C119 1.383(9) . ? C119 C120 1.382(10) . ? C119 H119 0.9500 . ? C120 C121 1.372(10) . ? C120 H120 0.9500 . ? C121 C122 1.379(10) . ? C121 H121 0.9500 . ? C122 C123 1.387(10) . ? C122 H122 0.9500 . ? C123 H123 0.9500 . ? C124 C129 1.378(8) . ? C124 C125 1.384(8) . ? C125 C126 1.370(9) . ? C125 H125 0.9500 . ? C126 C127 1.388(10) . ? C126 H126 0.9500 . ? C127 C128 1.359(9) . ? C127 H127 0.9500 . ? C128 C129 1.392(9) . ? C128 H128 0.9500 . ? C129 H129 0.9500 . ? B1 F2 1.379(8) . ? B1 F1 1.383(8) . ? B1 F3 1.387(9) . ? B1 F4 1.389(8) . ? B2 F8 1.357(8) . ? B2 F5 1.378(9) . ? B2 F6 1.399(8) . ? B2 F7 1.411(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C2 99.4(3) . . ? C1 Fe1 C6 154.9(3) . . ? C2 Fe1 C6 94.9(3) . . ? C1 Fe1 C5 128.1(3) . . ? C2 Fe1 C5 132.3(3) . . ? C6 Fe1 C5 39.7(2) . . ? C1 Fe1 C4 92.0(3) . . ? C2 Fe1 C4 154.5(3) . . ? C6 Fe1 C4 67.3(3) . . ? C5 Fe1 C4 39.6(2) . . ? C1 Fe1 P1 94.7(2) . . ? C2 Fe1 P1 93.2(2) . . ? C6 Fe1 P1 104.99(19) . . ? C5 Fe1 P1 88.0(2) . . ? C4 Fe1 P1 108.63(18) . . ? C1 Fe1 C7 120.0(3) . . ? C2 Fe1 C7 88.7(3) . . ? C6 Fe1 C7 39.5(2) . . ? C5 Fe1 C7 65.4(2) . . ? C4 Fe1 C7 65.9(2) . . ? P1 Fe1 C7 144.41(17) . . ? C1 Fe1 C3 88.5(3) . . ? C2 Fe1 C3 117.6(2) . . ? C6 Fe1 C3 66.5(2) . . ? C5 Fe1 C3 65.7(2) . . ? C4 Fe1 C3 39.5(2) . . ? P1 Fe1 C3 148.11(16) . . ? C7 Fe1 C3 38.9(2) . . ? O3 P1 O4 99.9(2) . . ? O3 P1 O5 98.6(2) . . ? O4 P1 O5 105.5(2) . . ? O3 P1 Fe1 118.60(17) . . ? O4 P1 Fe1 112.65(16) . . ? O5 P1 Fe1 118.95(17) . . ? C12 O3 P1 126.7(3) . . ? C18 O4 P1 123.2(4) . . ? C24 O5 P1 126.0(4) . . ? O1 C1 Fe1 175.7(6) . . ? O2 C2 Fe1 177.2(6) . . ? C11 C3 C4 134.2(6) . . ? C11 C3 C7 118.9(5) . . ? C4 C3 C7 106.9(5) . . ? C11 C3 Fe1 127.0(4) . . ? C4 C3 Fe1 67.1(3) . . ? C7 C3 Fe1 70.5(3) . . ? C5 C4 C3 108.0(6) . . ? C5 C4 Fe1 70.1(3) . . ? C3 C4 Fe1 73.4(3) . . ? C5 C4 H4 126.0 . . ? C3 C4 H4 126.0 . . ? Fe1 C4 H4 122.2 . . ? C4 C5 C6 109.5(6) . . ? C4 C5 Fe1 70.3(3) . . ? C6 C5 Fe1 69.9(3) . . ? C4 C5 H5 125.3 . . ? C6 C5 H5 125.3 . . ? Fe1 C5 H5 126.1 . . ? C5 C6 C7 107.3(5) . . ? C5 C6 Fe1 70.3(3) . . ? C7 C6 Fe1 73.6(3) . . ? C5 C6 H6 126.4 . . ? C7 C6 H6 126.4 . . ? Fe1 C6 H6 121.4 . . ? C8 C7 C6 132.4(6) . . ? C8 C7 C3 119.6(5) . . ? C6 C7 C3 108.0(5) . . ? C8 C7 Fe1 127.1(4) . . ? C6 C7 Fe1 66.9(3) . . ? C3 C7 Fe1 70.6(3) . . ? C9 C8 C7 118.8(6) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C8 C9 C10 121.5(6) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C11 C10 C9 121.0(6) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C3 120.2(6) . . ? C10 C11 H11 119.9 . . ? C3 C11 H11 119.9 . . ? C13 C12 C17 122.5(6) . . ? C13 C12 O3 115.4(5) . . ? C17 C12 O3 121.9(5) . . ? C12 C13 C14 117.7(6) . . ? C12 C13 H13 121.2 . . ? C14 C13 H13 121.2 . . ? C15 C14 C13 120.6(6) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C16 C15 C14 121.1(6) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 120.0(6) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C12 118.0(6) . . ? C16 C17 H17 121.0 . . ? C12 C17 H17 121.0 . . ? C19 C18 C23 121.7(6) . . ? C19 C18 O4 120.7(6) . . ? C23 C18 O4 117.5(5) . . ? C20 C19 C18 118.5(6) . . ? C20 C19 H19 120.8 . . ? C18 C19 H19 120.8 . . ? C21 C20 C19 122.0(6) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C20 C21 C22 118.9(6) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C21 C22 C23 120.6(6) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C18 C23 C22 118.3(6) . . ? C18 C23 H23 120.9 . . ? C22 C23 H23 120.9 . . ? C29 C24 C25 121.7(6) . . ? C29 C24 O5 121.6(5) . . ? C25 C24 O5 116.7(5) . . ? C26 C25 C24 118.7(6) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C25 C26 C27 120.8(6) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C28 C27 C26 120.2(6) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 120.4(6) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C24 C29 C28 118.3(6) . . ? C24 C29 H29 120.8 . . ? C28 C29 H29 120.8 . . ? C102 Fe2 C101 99.4(3) . . ? C102 Fe2 C106 94.7(3) . . ? C101 Fe2 C106 154.4(3) . . ? C102 Fe2 C105 132.5(3) . . ? C101 Fe2 C105 127.9(3) . . ? C106 Fe2 C105 40.3(2) . . ? C102 Fe2 C104 154.2(3) . . ? C101 Fe2 C104 91.6(3) . . ? C106 Fe2 C104 67.5(3) . . ? C105 Fe2 C104 39.9(2) . . ? C102 Fe2 P2 93.1(2) . . ? C101 Fe2 P2 95.1(2) . . ? C106 Fe2 P2 105.39(19) . . ? C105 Fe2 P2 87.9(2) . . ? C104 Fe2 P2 109.15(18) . . ? C102 Fe2 C103 117.3(2) . . ? C101 Fe2 C103 88.0(3) . . ? C106 Fe2 C103 66.6(2) . . ? C105 Fe2 C103 66.2(2) . . ? C104 Fe2 C103 39.4(2) . . ? P2 Fe2 C103 148.53(16) . . ? C102 Fe2 C107 88.0(3) . . ? C101 Fe2 C107 119.4(3) . . ? C106 Fe2 C107 39.6(2) . . ? C105 Fe2 C107 66.3(2) . . ? C104 Fe2 C107 66.3(2) . . ? P2 Fe2 C107 144.87(17) . . ? C103 Fe2 C107 39.1(2) . . ? O103 P2 O104 100.0(2) . . ? O103 P2 O105 98.5(2) . . ? O104 P2 O105 105.6(2) . . ? O103 P2 Fe2 118.63(17) . . ? O104 P2 Fe2 112.45(17) . . ? O105 P2 Fe2 119.02(18) . . ? C112 O103 P2 126.7(4) . . ? C118 O104 P2 122.7(4) . . ? C124 O105 P2 125.5(4) . . ? O101 C101 Fe2 176.3(6) . . ? O102 C102 Fe2 177.1(6) . . ? C111 C103 C104 133.4(6) . . ? C111 C103 C107 119.3(5) . . ? C104 C103 C107 107.3(5) . . ? C111 C103 Fe2 127.1(4) . . ? C104 C103 Fe2 66.8(3) . . ? C107 C103 Fe2 70.6(3) . . ? C105 C104 C103 108.9(6) . . ? C105 C104 Fe2 69.9(3) . . ? C103 C104 Fe2 73.8(3) . . ? C105 C104 H104 125.6 . . ? C103 C104 H104 125.6 . . ? Fe2 C104 H104 122.4 . . ? C104 C105 C106 108.2(5) . . ? C104 C105 Fe2 70.3(3) . . ? C106 C105 Fe2 69.6(3) . . ? C104 C105 H105 125.9 . . ? C106 C105 H105 125.9 . . ? Fe2 C105 H105 125.8 . . ? C105 C106 C107 108.4(5) . . ? C105 C106 Fe2 70.1(3) . . ? C107 C106 Fe2 74.2(3) . . ? C105 C106 H106 125.8 . . ? C107 C106 H106 125.8 . . ? Fe2 C106 H106 121.6 . . ? C108 C107 C106 132.5(6) . . ? C108 C107 C103 120.5(5) . . ? C106 C107 C103 107.0(5) . . ? C108 C107 Fe2 128.2(4) . . ? C106 C107 Fe2 66.2(3) . . ? C103 C107 Fe2 70.4(3) . . ? C109 C108 C107 117.7(6) . . ? C109 C108 H108 121.1 . . ? C107 C108 H108 121.1 . . ? C108 C109 C110 122.8(6) . . ? C108 C109 H109 118.6 . . ? C110 C109 H109 118.6 . . ? C111 C110 C109 120.8(6) . . ? C111 C110 H110 119.6 . . ? C109 C110 H110 119.6 . . ? C110 C111 C103 118.8(6) . . ? C110 C111 H111 120.6 . . ? C103 C111 H111 120.6 . . ? C113 C112 C117 121.5(6) . . ? C113 C112 O103 115.6(5) . . ? C117 C112 O103 122.8(5) . . ? C112 C113 C114 118.1(6) . . ? C112 C113 H113 121.0 . . ? C114 C113 H113 121.0 . . ? C115 C114 C113 120.0(6) . . ? C115 C114 H114 120.0 . . ? C113 C114 H114 120.0 . . ? C116 C115 C114 121.6(6) . . ? C116 C115 H115 119.2 . . ? C114 C115 H115 119.2 . . ? C115 C116 C117 119.6(6) . . ? C115 C116 H116 120.2 . . ? C117 C116 H116 120.2 . . ? C112 C117 C116 119.2(6) . . ? C112 C117 H117 120.4 . . ? C116 C117 H117 120.4 . . ? C123 C118 C119 122.4(6) . . ? C123 C118 O104 117.9(5) . . ? C119 C118 O104 119.6(5) . . ? C120 C119 C118 117.5(6) . . ? C120 C119 H119 121.3 . . ? C118 C119 H119 121.3 . . ? C121 C120 C119 121.7(6) . . ? C121 C120 H120 119.2 . . ? C119 C120 H120 119.2 . . ? C120 C121 C122 119.4(6) . . ? C120 C121 H121 120.3 . . ? C122 C121 H121 120.3 . . ? C121 C122 C123 120.4(7) . . ? C121 C122 H122 119.8 . . ? C123 C122 H122 119.8 . . ? C118 C123 C122 118.6(6) . . ? C118 C123 H123 120.7 . . ? C122 C123 H123 120.7 . . ? C129 C124 C125 121.4(5) . . ? C129 C124 O105 121.9(5) . . ? C125 C124 O105 116.6(5) . . ? C126 C125 C124 118.9(6) . . ? C126 C125 H125 120.6 . . ? C124 C125 H125 120.6 . . ? C125 C126 C127 120.8(6) . . ? C125 C126 H126 119.6 . . ? C127 C126 H126 119.6 . . ? C128 C127 C126 119.5(6) . . ? C128 C127 H127 120.3 . . ? C126 C127 H127 120.3 . . ? C127 C128 C129 121.2(6) . . ? C127 C128 H128 119.4 . . ? C129 C128 H128 119.4 . . ? C124 C129 C128 118.2(6) . . ? C124 C129 H129 120.9 . . ? C128 C129 H129 120.9 . . ? F2 B1 F1 109.5(6) . . ? F2 B1 F3 111.1(5) . . ? F1 B1 F3 108.2(5) . . ? F2 B1 F4 110.4(6) . . ? F1 B1 F4 109.0(6) . . ? F3 B1 F4 108.6(6) . . ? F8 B2 F5 111.2(6) . . ? F8 B2 F6 111.1(6) . . ? F5 B2 F6 108.7(6) . . ? F8 B2 F7 111.2(6) . . ? F5 B2 F7 107.6(6) . . ? F6 B2 F7 106.8(6) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.67 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.681 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.111 # Attachment '[(ind)Fe(CO)2(MeC3N2H3)]{BF4].cif' data_mann1 _database_code_depnum_ccdc_archive 'CCDC 766625' #TrackingRef '[(ind)Fe(CO)2(MeC3N2H3)]{BF4].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H13 Fe N2 O2, B F4' _chemical_formula_sum 'C15 H13 B F4 Fe N2 O2' _chemical_formula_weight 395.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3460 0.8440 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.0213(5) _cell_length_b 10.6698(8) _cell_length_c 11.1259(8) _cell_angle_alpha 78.540(3) _cell_angle_beta 83.572(3) _cell_angle_gamma 81.108(3) _cell_volume 804.23(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9759 _cell_measurement_theta_min 4.906 _cell_measurement_theta_max 71.435 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 0.992 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7552 _exptl_absorpt_correction_T_max 0.9614 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker smart4000' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 21878 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 36.17 _reflns_number_total 7270 _reflns_number_gt 6036 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _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^)+(0.0562P)^2^+0.5342P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7270 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1172 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Fe Fe 0.25880(3) 0.319090(19) 0.333596(18) 0.01389(6) Uani 1 1 d . . . N1 N 0.22842(17) 0.15219(12) 0.29210(11) 0.0159(2) Uani 1 1 d . . . N2 N 0.2443(2) -0.00566(13) 0.18956(14) 0.0227(3) Uani 1 1 d . . . O1 O 0.1336(2) 0.47905(13) 0.10152(12) 0.0294(3) Uani 1 1 d . . . O2 O -0.11742(17) 0.34853(13) 0.47251(12) 0.0269(2) Uani 1 1 d . . . B1 B 0.2058(3) 0.2530(2) 0.79302(19) 0.0278(4) Uani 1 1 d . . . C1 C 0.5625(2) 0.24296(14) 0.36051(13) 0.0170(2) Uani 1 1 d . . . C2 C 0.4435(2) 0.24887(15) 0.47367(13) 0.0187(2) Uani 1 1 d . . . H2 H 0.4190 0.1777 0.5369 0.022 Uiso 1 1 calc R . . C3 C 0.3691(2) 0.38071(16) 0.47372(14) 0.0199(3) Uani 1 1 d . . . H3 H 0.2941 0.4132 0.5402 0.024 Uiso 1 1 calc R . . C4 C 0.4249(2) 0.45611(15) 0.35836(14) 0.0189(2) Uani 1 1 d . . . H4 H 0.3862 0.5459 0.3320 0.023 Uiso 1 1 calc R . . C5 C 0.5514(2) 0.37089(14) 0.28854(13) 0.0170(2) Uani 1 1 d . . . C6 C 0.6559(2) 0.39401(16) 0.17054(14) 0.0211(3) Uani 1 1 d . . . H6 H 0.6506 0.4786 0.1226 0.025 Uiso 1 1 calc R . . C7 C 0.7639(2) 0.29104(17) 0.12832(15) 0.0233(3) Uani 1 1 d . . . H7 H 0.8368 0.3050 0.0507 0.028 Uiso 1 1 calc R . . C8 C 0.7696(2) 0.16356(16) 0.19800(16) 0.0220(3) Uani 1 1 d . . . H8 H 0.8442 0.0942 0.1649 0.026 Uiso 1 1 calc R . . C9 C 0.6708(2) 0.13817(15) 0.31110(15) 0.0198(3) Uani 1 1 d . . . H9 H 0.6745 0.0523 0.3558 0.024 Uiso 1 1 calc R . . C10 C 0.2599(2) 0.11961(15) 0.18135(14) 0.0190(3) Uani 1 1 d . . . H10 H 0.2892 0.1770 0.1069 0.023 Uiso 1 1 calc R . . C11 C 0.1911(2) 0.04129(15) 0.37376(15) 0.0210(3) Uani 1 1 d . . . H11 H 0.1631 0.0347 0.4602 0.025 Uiso 1 1 calc R . . C12 C 0.2007(3) -0.05680(16) 0.31103(17) 0.0260(3) Uani 1 1 d . . . H12 H 0.1811 -0.1434 0.3445 0.031 Uiso 1 1 calc R . . C13 C 0.2686(3) -0.0754(2) 0.0868(2) 0.0360(4) Uani 1 1 d . . . H13A H 0.1574 -0.1217 0.0900 0.054 Uiso 1 1 calc R . . H13B H 0.3874 -0.1372 0.0928 0.054 Uiso 1 1 calc R . . H13C H 0.2771 -0.0139 0.0089 0.054 Uiso 1 1 calc R . . C14 C 0.1770(2) 0.41587(15) 0.19129(14) 0.0193(3) Uani 1 1 d . . . C15 C 0.0280(2) 0.33613(15) 0.41624(14) 0.0194(3) Uani 1 1 d . . . F2 F 0.1371(2) 0.22834(16) 0.91503(12) 0.0498(4) Uani 1 1 d . A . F3 F 0.3790(3) 0.2997(2) 0.77693(18) 0.0748(6) Uani 1 1 d . A . F4 F 0.2334(4) 0.14157(18) 0.74748(19) 0.0870(8) Uani 1 1 d . A . F1 F 0.1044(5) 0.3665(4) 0.7302(3) 0.0387(11) Uiso 0.457(8) 1 d P A 1 F1' F 0.0579(5) 0.3200(4) 0.7235(3) 0.0483(10) Uiso 0.543(8) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.01255(9) 0.01679(10) 0.01261(9) -0.00211(6) -0.00095(6) -0.00373(6) N1 0.0150(5) 0.0174(5) 0.0153(5) -0.0012(4) -0.0023(4) -0.0038(4) N2 0.0242(6) 0.0190(6) 0.0261(6) -0.0068(5) -0.0033(5) -0.0026(5) O1 0.0327(7) 0.0296(6) 0.0236(6) 0.0049(5) -0.0085(5) -0.0054(5) O2 0.0171(5) 0.0369(7) 0.0278(6) -0.0105(5) 0.0033(4) -0.0050(4) B1 0.0311(9) 0.0249(8) 0.0258(8) -0.0057(7) 0.0049(7) -0.0027(7) C1 0.0135(5) 0.0212(6) 0.0168(6) -0.0024(5) -0.0032(4) -0.0045(4) C2 0.0177(6) 0.0254(7) 0.0138(5) -0.0022(5) -0.0032(4) -0.0062(5) C3 0.0188(6) 0.0276(7) 0.0159(6) -0.0074(5) -0.0007(5) -0.0072(5) C4 0.0188(6) 0.0202(6) 0.0199(6) -0.0064(5) -0.0003(5) -0.0070(5) C5 0.0142(5) 0.0198(6) 0.0179(6) -0.0036(5) -0.0001(4) -0.0063(4) C6 0.0196(6) 0.0233(7) 0.0204(6) -0.0032(5) 0.0030(5) -0.0076(5) C7 0.0187(6) 0.0292(8) 0.0224(7) -0.0066(6) 0.0044(5) -0.0066(5) C8 0.0160(6) 0.0257(7) 0.0253(7) -0.0087(6) -0.0008(5) -0.0012(5) C9 0.0156(6) 0.0206(6) 0.0228(6) -0.0025(5) -0.0047(5) -0.0016(5) C10 0.0193(6) 0.0196(6) 0.0191(6) -0.0048(5) -0.0010(5) -0.0044(5) C11 0.0217(7) 0.0207(6) 0.0197(6) 0.0020(5) -0.0032(5) -0.0067(5) C12 0.0293(8) 0.0180(7) 0.0297(8) 0.0011(6) -0.0059(6) -0.0050(6) C13 0.0456(11) 0.0295(9) 0.0380(10) -0.0191(8) -0.0023(8) -0.0045(8) C14 0.0180(6) 0.0205(6) 0.0197(6) -0.0026(5) -0.0024(5) -0.0046(5) C15 0.0175(6) 0.0226(7) 0.0195(6) -0.0054(5) -0.0020(5) -0.0046(5) F2 0.0554(9) 0.0633(9) 0.0215(5) -0.0003(6) 0.0060(5) 0.0036(7) F3 0.0742(13) 0.0940(14) 0.0649(11) 0.0011(10) -0.0034(9) -0.0603(11) F4 0.141(2) 0.0506(10) 0.0772(13) -0.0413(10) 0.0543(13) -0.0449(12) _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 Fe C15 1.7736(15) . ? Fe C14 1.8093(15) . ? Fe N1 1.9739(12) . ? Fe C3 2.0730(15) . ? Fe C4 2.0813(14) . ? Fe C2 2.0880(14) . ? Fe C5 2.1878(14) . ? Fe C1 2.1923(14) . ? N1 C10 1.3317(19) . ? N1 C11 1.3819(19) . ? N2 C10 1.342(2) . ? N2 C12 1.373(2) . ? N2 C13 1.464(2) . ? O1 C14 1.132(2) . ? O2 C15 1.1403(19) . ? B1 F4 1.361(3) . ? B1 F3 1.365(3) . ? B1 F2 1.377(2) . ? B1 F1' 1.386(4) . ? B1 F1 1.404(4) . ? C1 C9 1.421(2) . ? C1 C5 1.434(2) . ? C1 C2 1.438(2) . ? C2 C3 1.423(2) . ? C2 H2 0.9500 . ? C3 C4 1.422(2) . ? C3 H3 0.9500 . ? C4 C5 1.448(2) . ? C4 H4 0.9500 . ? C5 C6 1.426(2) . ? C6 C7 1.368(2) . ? C6 H6 0.9500 . ? C7 C8 1.423(2) . ? C7 H7 0.9500 . ? C8 C9 1.366(2) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.358(2) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 Fe C14 94.51(7) . . ? C15 Fe N1 93.98(6) . . ? C14 Fe N1 95.27(6) . . ? C15 Fe C3 87.99(6) . . ? C14 Fe C3 127.70(7) . . ? N1 Fe C3 136.74(6) . . ? C15 Fe C4 111.56(6) . . ? C14 Fe C4 92.56(6) . . ? N1 Fe C4 152.59(6) . . ? C3 Fe C4 40.04(6) . . ? C15 Fe C2 102.64(6) . . ? C14 Fe C2 157.38(6) . . ? N1 Fe C2 98.11(6) . . ? C3 Fe C2 39.99(6) . . ? C4 Fe C2 67.56(6) . . ? C15 Fe C5 150.71(6) . . ? C14 Fe C5 92.11(6) . . ? N1 Fe C5 113.79(5) . . ? C3 Fe C5 65.68(6) . . ? C4 Fe C5 39.55(6) . . ? C2 Fe C5 65.80(6) . . ? C15 Fe C1 141.34(6) . . ? C14 Fe C1 123.78(6) . . ? N1 Fe C1 88.09(5) . . ? C3 Fe C1 65.44(6) . . ? C4 Fe C1 65.89(6) . . ? C2 Fe C1 39.15(6) . . ? C5 Fe C1 38.23(5) . . ? C10 N1 C11 105.99(13) . . ? C10 N1 Fe 126.87(10) . . ? C11 N1 Fe 126.79(10) . . ? C10 N2 C12 108.03(13) . . ? C10 N2 C13 125.98(15) . . ? C12 N2 C13 125.99(15) . . ? F4 B1 F3 107.4(2) . . ? F4 B1 F2 109.49(18) . . ? F3 B1 F2 112.17(19) . . ? F4 B1 F1' 99.0(3) . . ? F3 B1 F1' 118.4(2) . . ? F2 B1 F1' 109.3(2) . . ? F4 B1 F1 121.1(3) . . ? F3 B1 F1 94.7(2) . . ? F2 B1 F1 111.0(2) . . ? F1' B1 F1 27.13(15) . . ? C9 C1 C5 119.58(13) . . ? C9 C1 C2 132.29(14) . . ? C5 C1 C2 108.04(13) . . ? C9 C1 Fe 125.72(10) . . ? C5 C1 Fe 70.72(8) . . ? C2 C1 Fe 66.51(8) . . ? C3 C2 C1 107.56(13) . . ? C3 C2 Fe 69.43(8) . . ? C1 C2 Fe 74.34(8) . . ? C3 C2 H2 126.2 . . ? C1 C2 H2 126.2 . . ? Fe C2 H2 121.7 . . ? C4 C3 C2 109.12(13) . . ? C4 C3 Fe 70.29(8) . . ? C2 C3 Fe 70.57(8) . . ? C4 C3 H3 125.4 . . ? C2 C3 H3 125.4 . . ? Fe C3 H3 125.3 . . ? C3 C4 C5 107.37(13) . . ? C3 C4 Fe 69.67(8) . . ? C5 C4 Fe 74.20(8) . . ? C3 C4 H4 126.3 . . ? C5 C4 H4 126.3 . . ? Fe C4 H4 121.6 . . ? C6 C5 C1 120.33(14) . . ? C6 C5 C4 132.04(14) . . ? C1 C5 C4 107.63(12) . . ? C6 C5 Fe 128.23(11) . . ? C1 C5 Fe 71.05(8) . . ? C4 C5 Fe 66.26(8) . . ? C7 C6 C5 118.14(14) . . ? C7 C6 H6 120.9 . . ? C5 C6 H6 120.9 . . ? C6 C7 C8 121.47(14) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C9 C8 C7 121.81(15) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C8 C9 C1 118.59(14) . . ? C8 C9 H9 120.7 . . ? C1 C9 H9 120.7 . . ? N1 C10 N2 110.52(14) . . ? N1 C10 H10 124.7 . . ? N2 C10 H10 124.7 . . ? C12 C11 N1 109.26(14) . . ? C12 C11 H11 125.4 . . ? N1 C11 H11 125.4 . . ? C11 C12 N2 106.20(14) . . ? C11 C12 H12 126.9 . . ? N2 C12 H12 126.9 . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O1 C14 Fe 176.73(14) . . ? O2 C15 Fe 177.56(14) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.266 _refine_diff_density_min -0.974 _refine_diff_density_rms 0.092 data_mann2 _database_code_depnum_ccdc_archive 'CCDC 766626' #TrackingRef 'MANN2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H12 B F4 Fe N O2' _chemical_formula_weight 392.93 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9950(16) _cell_length_b 9.5420(19) _cell_length_c 10.832(2) _cell_angle_alpha 89.32(3) _cell_angle_beta 78.41(3) _cell_angle_gamma 82.82(3) _cell_volume 803.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2376 _cell_measurement_theta_min 1.92 _cell_measurement_theta_max 27.53 _exptl_crystal_description BLOCK _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 0.991 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7898 _exptl_absorpt_correction_T_max 0.8903 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18344 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.53 _reflns_number_total 3675 _reflns_number_gt 3203 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _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^)+(0.0435P)^2^+0.2310P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3675 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0824 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _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 Fe1 Fe 1.11663(3) 0.67694(2) 0.12948(2) 0.01249(9) Uani 1 1 d . . . N1 N 1.20485(19) 0.66149(15) 0.29162(13) 0.0139(3) Uani 1 1 d . . . O1 O 1.34403(16) 0.43317(13) -0.00145(12) 0.0200(3) Uani 1 1 d . . . O2 O 0.83738(16) 0.49958(13) 0.21512(12) 0.0197(3) Uani 1 1 d . . . C1 C 0.9243(2) 0.85663(18) 0.10610(17) 0.0185(4) Uani 1 1 d . . . C2 C 1.0073(2) 0.78554(19) -0.01207(17) 0.0192(4) Uani 1 1 d . . . H2A H 0.9490 0.7437 -0.0713 0.023 Uiso 1 1 calc R . . C3 C 1.1870(2) 0.79905(19) -0.03219(17) 0.0199(4) Uani 1 1 d . . . H3A H 1.2729 0.7672 -0.1077 0.024 Uiso 1 1 calc R . . C4 C 1.2207(2) 0.86691(19) 0.07527(17) 0.0189(4) Uani 1 1 d . . . H4A H 1.3330 0.8900 0.0861 0.023 Uiso 1 1 calc R . . C5 C 1.0568(2) 0.90641(18) 0.16124(17) 0.0178(4) Uani 1 1 d . . . C6 C 1.0118(3) 0.97585(19) 0.28246(18) 0.0275(5) Uani 1 1 d . . . H6A H 1.0954 1.0082 0.3194 0.033 Uiso 1 1 calc R . . C7 C 0.8417(3) 0.9931(2) 0.3423(2) 0.0367(6) Uani 1 1 d . . . H7A H 0.8115 1.0357 0.4218 0.044 Uiso 1 1 calc R . . C8 C 0.7097(3) 0.9478(2) 0.2867(2) 0.0379(6) Uani 1 1 d . . . H8A H 0.5959 0.9640 0.3297 0.045 Uiso 1 1 calc R . . C9 C 0.7472(3) 0.8807(2) 0.1711(2) 0.0291(5) Uani 1 1 d . . . H9A H 0.6604 0.8516 0.1357 0.035 Uiso 1 1 calc R . . C10 C 1.3754(2) 0.65347(18) 0.29271(16) 0.0161(4) Uani 1 1 d . . . H10A H 1.4536 0.6461 0.2162 0.019 Uiso 1 1 calc R . . C11 C 1.4383(2) 0.65582(19) 0.40378(17) 0.0187(4) Uani 1 1 d . . . H11A H 1.5559 0.6522 0.4006 0.022 Uiso 1 1 calc R . . C12 C 1.3233(2) 0.66371(19) 0.51959(17) 0.0194(4) Uani 1 1 d . . . H12A H 1.3623 0.6653 0.5948 0.023 Uiso 1 1 calc R . . C13 C 1.1476(2) 0.66923(19) 0.51957(17) 0.0190(4) Uani 1 1 d . . . H13A H 1.0678 0.6730 0.5953 0.023 Uiso 1 1 calc R . . C14 C 1.0932(2) 0.66897(18) 0.40557(16) 0.0163(4) Uani 1 1 d . . . H14A H 0.9759 0.6741 0.4068 0.020 Uiso 1 1 calc R . . C15 C 0.9480(2) 0.56665(18) 0.18260(15) 0.0144(4) Uani 1 1 d . . . C16 C 1.2597(2) 0.52839(19) 0.05261(16) 0.0152(4) Uani 1 1 d . . . B1 B 0.3384(3) 1.2367(2) 0.2588(2) 0.0233(5) Uani 1 1 d . . . F1 F 0.18241(14) 1.31588(12) 0.24490(10) 0.0254(3) Uani 1 1 d . . . F2 F 0.46963(14) 1.32451(12) 0.24274(10) 0.0269(3) Uani 1 1 d . . . F3 F 0.38330(18) 1.13161(14) 0.16268(15) 0.0489(4) Uani 1 1 d . . . F4 F 0.31871(18) 1.17585(18) 0.37697(14) 0.0539(4) 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 Fe1 0.01220(15) 0.01339(14) 0.01197(14) 0.00152(9) -0.00236(10) -0.00217(10) N1 0.0141(8) 0.0136(7) 0.0136(7) 0.0009(5) -0.0024(6) -0.0014(6) O1 0.0190(7) 0.0211(7) 0.0184(7) -0.0019(5) -0.0015(5) -0.0008(6) O2 0.0174(7) 0.0237(7) 0.0200(7) 0.0041(5) -0.0053(5) -0.0073(6) C1 0.0180(10) 0.0128(8) 0.0243(10) 0.0068(7) -0.0044(8) -0.0013(7) C2 0.0256(10) 0.0172(9) 0.0178(9) 0.0058(7) -0.0114(8) -0.0034(8) C3 0.0231(10) 0.0180(9) 0.0164(9) 0.0077(7) -0.0004(7) -0.0008(8) C4 0.0180(10) 0.0179(9) 0.0222(9) 0.0067(7) -0.0048(7) -0.0067(7) C5 0.0236(10) 0.0106(8) 0.0191(9) 0.0041(7) -0.0048(7) -0.0021(7) C6 0.0470(14) 0.0133(9) 0.0218(10) 0.0013(7) -0.0057(9) -0.0046(9) C7 0.0600(17) 0.0148(10) 0.0252(11) 0.0013(8) 0.0106(11) 0.0035(10) C8 0.0318(13) 0.0197(10) 0.0479(14) 0.0096(10) 0.0181(11) 0.0081(9) C9 0.0173(10) 0.0191(10) 0.0480(13) 0.0119(9) -0.0022(9) 0.0001(8) C10 0.0143(9) 0.0176(9) 0.0155(9) -0.0009(7) -0.0011(7) -0.0013(7) C11 0.0161(9) 0.0190(9) 0.0221(9) 0.0003(7) -0.0069(7) -0.0011(7) C12 0.0253(10) 0.0182(9) 0.0158(9) -0.0008(7) -0.0084(8) -0.0003(8) C13 0.0220(10) 0.0193(9) 0.0136(9) 0.0010(7) 0.0002(7) -0.0011(8) C14 0.0129(9) 0.0179(9) 0.0170(9) 0.0014(7) -0.0005(7) -0.0018(7) C15 0.0165(9) 0.0149(8) 0.0113(8) -0.0007(6) -0.0050(7) 0.0032(7) C16 0.0144(9) 0.0202(9) 0.0128(8) 0.0044(7) -0.0045(7) -0.0061(7) B1 0.0175(11) 0.0219(11) 0.0325(12) 0.0032(9) -0.0097(9) -0.0021(9) F1 0.0154(6) 0.0337(6) 0.0257(6) 0.0074(5) -0.0033(5) 0.0007(5) F2 0.0207(6) 0.0335(6) 0.0286(6) -0.0031(5) -0.0069(5) -0.0077(5) F3 0.0357(8) 0.0364(8) 0.0742(11) -0.0257(7) -0.0093(7) -0.0033(6) F4 0.0365(8) 0.0759(11) 0.0515(9) 0.0406(8) -0.0147(7) -0.0097(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C16 1.803(2) . ? Fe1 C15 1.8122(19) . ? Fe1 N1 2.0173(15) . ? Fe1 C3 2.1120(18) . ? Fe1 C2 2.1128(18) . ? Fe1 C4 2.1161(18) . ? Fe1 C5 2.1981(18) . ? Fe1 C1 2.2033(19) . ? N1 C10 1.358(2) . ? N1 C14 1.367(2) . ? O1 C16 1.150(2) . ? O2 C15 1.152(2) . ? C1 C9 1.441(3) . ? C1 C5 1.446(3) . ? C1 C2 1.451(3) . ? C2 C3 1.431(3) . ? C2 H2A 0.9800 . ? C3 C4 1.426(3) . ? C3 H3A 0.9800 . ? C4 C5 1.456(3) . ? C4 H4A 0.9800 . ? C5 C6 1.437(3) . ? C6 C7 1.374(3) . ? C6 H6A 0.9300 . ? C7 C8 1.428(4) . ? C7 H7A 0.9300 . ? C8 C9 1.373(3) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 C11 1.396(3) . ? C10 H10A 0.9300 . ? C11 C12 1.395(3) . ? C11 H11A 0.9300 . ? C12 C13 1.399(3) . ? C12 H12A 0.9300 . ? C13 C14 1.389(3) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? B1 F4 1.387(3) . ? B1 F1 1.409(3) . ? B1 F2 1.406(2) . ? B1 F3 1.415(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 C16 Fe1 C15 91.45(8) . . ? C16 Fe1 N1 95.28(7) . . ? C15 Fe1 N1 94.24(7) . . ? C16 Fe1 C3 89.42(8) . . ? C15 Fe1 C3 134.72(8) . . ? N1 Fe1 C3 130.75(7) . . ? C16 Fe1 C2 106.47(8) . . ? C15 Fe1 C2 97.70(8) . . ? N1 Fe1 C2 154.80(7) . . ? C3 Fe1 C2 39.61(7) . . ? C16 Fe1 C4 109.90(8) . . ? C15 Fe1 C4 156.12(8) . . ? N1 Fe1 C4 94.28(7) . . ? C3 Fe1 C4 39.43(7) . . ? C2 Fe1 C4 66.71(7) . . ? C16 Fe1 C5 149.30(7) . . ? C15 Fe1 C5 118.57(8) . . ? N1 Fe1 C5 89.09(7) . . ? C3 Fe1 C5 65.43(7) . . ? C2 Fe1 C5 65.71(7) . . ? C4 Fe1 C5 39.40(7) . . ? C16 Fe1 C1 145.51(7) . . ? C15 Fe1 C1 90.84(7) . . ? N1 Fe1 C1 118.85(7) . . ? C3 Fe1 C1 65.27(8) . . ? C2 Fe1 C1 39.22(7) . . ? C4 Fe1 C1 65.55(7) . . ? C5 Fe1 C1 38.35(7) . . ? C10 N1 C14 117.34(15) . . ? C10 N1 Fe1 121.77(12) . . ? C14 N1 Fe1 120.73(12) . . ? C9 C1 C5 119.87(18) . . ? C9 C1 C2 132.36(18) . . ? C5 C1 C2 107.77(16) . . ? C9 C1 Fe1 127.06(13) . . ? C5 C1 Fe1 70.63(10) . . ? C2 C1 Fe1 67.02(10) . . ? C3 C2 C1 107.78(16) . . ? C3 C2 Fe1 70.17(10) . . ? C1 C2 Fe1 73.76(10) . . ? C3 C2 H2A 126.0 . . ? C1 C2 H2A 126.0 . . ? Fe1 C2 H2A 126.0 . . ? C4 C3 C2 108.91(16) . . ? C4 C3 Fe1 70.44(10) . . ? C2 C3 Fe1 70.23(10) . . ? C4 C3 H3A 125.5 . . ? C2 C3 H3A 125.5 . . ? Fe1 C3 H3A 125.5 . . ? C3 C4 C5 107.89(17) . . ? C3 C4 Fe1 70.13(10) . . ? C5 C4 Fe1 73.34(10) . . ? C3 C4 H4A 126.0 . . ? C5 C4 H4A 126.0 . . ? Fe1 C4 H4A 126.0 . . ? C6 C5 C1 119.82(18) . . ? C6 C5 C4 132.69(19) . . ? C1 C5 C4 107.45(16) . . ? C6 C5 Fe1 125.25(12) . . ? C1 C5 Fe1 71.02(10) . . ? C4 C5 Fe1 67.26(10) . . ? C7 C6 C5 118.1(2) . . ? C7 C6 H6A 120.9 . . ? C5 C6 H6A 120.9 . . ? C6 C7 C8 122.3(2) . . ? C6 C7 H7A 118.9 . . ? C8 C7 H7A 118.9 . . ? C9 C8 C7 121.4(2) . . ? C9 C8 H8A 119.3 . . ? C7 C8 H8A 119.3 . . ? C8 C9 C1 118.4(2) . . ? C8 C9 H9A 120.8 . . ? C1 C9 H9A 120.8 . . ? N1 C10 C11 122.79(16) . . ? N1 C10 H10A 118.6 . . ? C11 C10 H10A 118.6 . . ? C12 C11 C10 119.43(17) . . ? C12 C11 H11A 120.3 . . ? C10 C11 H11A 120.3 . . ? C11 C12 C13 118.22(17) . . ? C11 C12 H12A 120.9 . . ? C13 C12 H12A 120.9 . . ? C14 C13 C12 119.47(16) . . ? C14 C13 H13A 120.3 . . ? C12 C13 H13A 120.3 . . ? N1 C14 C13 122.73(17) . . ? N1 C14 H14A 118.6 . . ? C13 C14 H14A 118.6 . . ? O2 C15 Fe1 177.93(15) . . ? O1 C16 Fe1 175.72(15) . . ? F4 B1 F1 109.81(18) . . ? F4 B1 F2 110.33(17) . . ? F1 B1 F2 109.83(16) . . ? F4 B1 F3 110.76(18) . . ? F1 B1 F3 107.99(17) . . ? F2 B1 F3 108.06(17) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.882 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.071