Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_cambridge 222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Mario Bakardjiev' 'Josef Holub' 'Michael J. Carr' 'John D. Kennedy' 'Bohumil Stibr' _publ_contact_author_name 'Prof Bohumil Stibr' _publ_contact_author_address ; Academy of Sciences of the Czech Republic 250 68 Rez CZECH REPUBLIC ; _publ_contact_author_email STIBR@IIC.CAS.CZ _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Diphosphacarborane Analogues of Ferrocene: The Synthesis of two Isomeric Twelve-Vertex closo-[(h5-C5H5)FeP2CB8H9] Complexes ; data_mgsl2942s _database_code_depnum_ccdc_archive 'CCDC 238383' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H14 B8 Fe P2' _chemical_formula_sum 'C6 H14 B8 Fe P2' _chemical_formula_weight 290.44 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' Fe Fe 0.3463 0.8444 '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 P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.4441(3) _cell_length_b 10.3911(6) _cell_length_c 8.8386(4) _cell_angle_alpha 90.00 _cell_angle_beta 113.950(3) _cell_angle_gamma 90.00 _cell_volume 624.82(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour Red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 292 _exptl_absorpt_coefficient_mu 1.421 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8479 _exptl_absorpt_correction_T_max 0.9721 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; Bruker-Nonius FR591 rotating-anode ; _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type ; Bruker-Nonius 95mm CCD camera on \k-goniostat ; _diffrn_measurement_method '\p & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7825 _diffrn_reflns_av_R_equivalents 0.0598 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 4.63 _diffrn_reflns_theta_max 27.60 _reflns_number_total 1514 _reflns_number_gt 1272 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; COLLECT (Hooft, 1999) ; _computing_cell_refinement ; DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1999) #Although determined using DirAx, the cell is refined in the HKL package during data reduction ; _computing_data_reduction ; DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1999) ; _computing_structure_solution ; SHELXS-97 (Sheldrick, 1986) ; _computing_structure_refinement ; SHELXS-97 (Sheldrick, 1986) ; _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material ; enCIFer (CCDC, 2002) ; _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 'w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+1.4767P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1514 _refine_ls_number_parameters 85 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1516 _refine_ls_wR_factor_gt 0.1439 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 0.77934(9) 0.7500 0.07416(8) 0.0239(3) Uani 1 2 d S . . P2 P 0.4535(2) 0.7500 -0.08641(18) 0.0351(4) Uani 1 2 d S . . P3 P 0.6425(2) 0.91926(18) -0.0908(2) 0.0337(4) Uani 0.50 1 d P . . C13 C 0.7586(6) 0.8182(4) 0.2871(4) 0.0308(8) Uani 1 1 d . . . H13 H 0.6570 0.8718 0.2906 0.037 Uiso 1 1 calc R . . B5 B 0.4418(6) 0.8366(4) -0.2982(5) 0.0259(8) Uani 1 1 d . . . H5 H 0.3029 0.8917 -0.3666 0.031 Uiso 1 1 calc R . . B12 B 0.5557(8) 0.7500 -0.4059(7) 0.0298(13) Uani 1 2 d S . . H12 H 0.4898 0.7500 -0.5446 0.036 Uiso 1 2 calc SR . . B6 B 0.6744(6) 0.8877(5) -0.2928(5) 0.0357(10) Uani 1 1 d . . . H6 H 0.6859 0.9775 -0.3585 0.043 Uiso 1 1 calc R . . C14 C 0.9339(7) 0.8605(5) 0.2810(5) 0.0486(12) Uani 1 1 d . . . H14 H 0.9724 0.9475 0.2795 0.058 Uiso 1 1 calc R . . B7 B 0.8137(9) 0.7500 -0.2888(7) 0.0385(16) Uani 1 2 d S . . H7 H 0.9168 0.7500 -0.3523 0.046 Uiso 1 2 calc SR . . C15 C 1.0435(9) 0.7500 0.2775(7) 0.065(3) Uani 1 2 d S . . H15 H 1.1691 0.7500 0.2734 0.078 Uiso 1 2 calc SR . . B3 B 0.6425(2) 0.91926(18) -0.0908(2) 0.0337(4) Uani 0.50 1 d P . . H3 H 0.5986 0.9993 -0.0279 0.040 Uiso 0.50 1 calc PR . . C4 C 0.8767(7) 0.8334(4) -0.0987(4) 0.0343(10) Uani 0.50 1 d P . . B4 B 0.8767(7) 0.8334(4) -0.0987(4) 0.0343(10) Uani 0.50 1 d P . . H4 H 0.9857 0.9026 -0.0124 0.041 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 0.0198(4) 0.0328(4) 0.0175(4) 0.000 0.0059(3) 0.000 P2 0.0286(7) 0.0428(9) 0.0321(7) 0.000 0.0104(6) 0.000 P3 0.0251(8) 0.0421(10) 0.0288(8) 0.0006(7) 0.0056(6) 0.0008(7) C13 0.041(2) 0.0306(19) 0.0219(16) -0.0018(15) 0.0143(15) -0.0024(16) B5 0.0210(18) 0.0282(19) 0.0245(18) 0.0026(15) 0.0052(15) -0.0002(15) B12 0.022(3) 0.044(4) 0.021(3) 0.000 0.007(2) 0.000 B6 0.029(2) 0.041(2) 0.030(2) 0.0117(19) 0.0045(17) -0.0088(19) C14 0.050(3) 0.069(3) 0.0220(18) -0.012(2) 0.0097(18) -0.031(2) B7 0.023(3) 0.072(5) 0.019(3) 0.000 0.008(2) 0.000 C15 0.024(3) 0.142(8) 0.020(3) 0.000 -0.002(2) 0.000 B3 0.0251(8) 0.0421(10) 0.0288(8) 0.0006(7) 0.0056(6) 0.0008(7) C4 0.065(3) 0.0254(19) 0.0113(15) 0.0045(14) 0.0144(17) 0.0053(18) B4 0.065(3) 0.0254(19) 0.0113(15) 0.0045(14) 0.0144(17) 0.0053(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 C15 2.056(6) . ? Fe1 C14 2.068(4) . ? Fe1 C14 2.068(4) 4_575 ? Fe1 C13 2.075(4) 4_575 ? Fe1 C13 2.075(4) . ? Fe1 C4 2.124(4) 4_575 ? Fe1 C4 2.124(4) . ? Fe1 B3 2.2473(18) 4_575 ? Fe1 P2 2.2592(16) . ? P2 B5 2.047(4) 4_575 ? P2 B5 2.047(4) . ? P2 P3 2.263(2) . ? P2 P3 2.263(2) 4_575 ? C13 C14 1.398(6) . ? C13 C13 1.418(7) 4_575 ? C13 H13 0.9500 . ? B5 B12 1.758(6) . ? B5 B6 1.793(6) . ? B5 B5 1.800(8) 4_575 ? B5 H5 1.1200 . ? B12 B5 1.758(6) 4_575 ? B12 B6 1.764(6) . ? B12 B6 1.764(6) 4_575 ? B12 B7 1.774(8) . ? B12 H12 1.1200 . ? B6 B7 1.759(6) . ? B6 H6 1.1200 . ? C14 C15 1.416(7) . ? C14 H14 0.9500 . ? B7 B6 1.759(6) 4_575 ? B7 B4 1.776(6) 4_575 ? B7 H7 1.1200 . ? C15 C14 1.416(7) 4_575 ? C15 H15 0.9500 . ? 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 Fe1 C14 40.17(18) . . ? C15 Fe1 C14 40.17(18) . 4_575 ? C14 Fe1 C14 67.4(3) . 4_575 ? C15 Fe1 C13 66.7(2) . 4_575 ? C14 Fe1 C13 66.87(16) . 4_575 ? C14 Fe1 C13 39.45(16) 4_575 4_575 ? C15 Fe1 C13 66.7(2) . . ? C14 Fe1 C13 39.45(16) . . ? C14 Fe1 C13 66.87(16) 4_575 . ? C13 Fe1 C13 40.0(2) 4_575 . ? C15 Fe1 C4 98.3(2) . 4_575 ? C14 Fe1 C4 129.25(19) . 4_575 ? C14 Fe1 C4 100.34(17) 4_575 4_575 ? C13 Fe1 C4 133.31(15) 4_575 4_575 ? C13 Fe1 C4 164.76(17) . 4_575 ? C15 Fe1 C4 98.3(2) . . ? C14 Fe1 C4 100.34(17) . . ? C14 Fe1 C4 129.25(19) 4_575 . ? C13 Fe1 C4 164.76(17) 4_575 . ? C13 Fe1 C4 133.31(15) . . ? C4 Fe1 C4 48.2(2) 4_575 . ? C15 Fe1 B3 126.00(7) . 4_575 ? C14 Fe1 B3 161.98(16) . 4_575 ? C14 Fe1 B3 94.70(16) 4_575 4_575 ? C13 Fe1 B3 98.05(11) 4_575 4_575 ? C13 Fe1 B3 132.45(12) . 4_575 ? C4 Fe1 B3 53.92(13) 4_575 4_575 ? C4 Fe1 B3 92.87(12) . 4_575 ? C15 Fe1 P2 162.0(2) . . ? C14 Fe1 P2 128.72(15) . . ? C14 Fe1 P2 128.72(16) 4_575 . ? C13 Fe1 P2 96.52(12) 4_575 . ? C13 Fe1 P2 96.52(12) . . ? C4 Fe1 P2 98.12(13) 4_575 . ? C4 Fe1 P2 98.12(13) . . ? B3 Fe1 P2 60.28(5) 4_575 . ? B5 P2 B5 52.2(2) 4_575 . ? B5 P2 Fe1 102.15(12) 4_575 . ? B5 P2 Fe1 102.15(12) . . ? B5 P2 P3 97.01(14) 4_575 . ? B5 P2 P3 55.83(12) . . ? Fe1 P2 P3 59.60(5) . . ? B5 P2 P3 55.83(12) 4_575 4_575 ? B5 P2 P3 97.01(14) . 4_575 ? Fe1 P2 P3 59.60(5) . 4_575 ? P3 P2 P3 102.03(11) . 4_575 ? C14 C13 C13 108.3(3) . 4_575 ? C14 C13 Fe1 70.0(2) . . ? C13 C13 Fe1 70.02(10) 4_575 . ? C14 C13 H13 125.8 . . ? C13 C13 H13 125.8 4_575 . ? Fe1 C13 H13 125.7 . . ? B12 B5 B6 59.6(3) . . ? B12 B5 B5 59.21(16) . 4_575 ? B6 B5 B5 107.2(2) . 4_575 ? B12 B5 P2 114.8(2) . . ? B6 B5 P2 115.1(2) . . ? B5 B5 P2 63.91(12) 4_575 . ? B12 B5 H5 120.7 . . ? B6 B5 H5 122.2 . . ? B5 B5 H5 120.7 4_575 . ? P2 B5 H5 113.9 . . ? B5 B12 B5 61.6(3) 4_575 . ? B5 B12 B6 110.4(4) 4_575 . ? B5 B12 B6 61.2(2) . . ? B5 B12 B6 61.2(2) 4_575 4_575 ? B5 B12 B6 110.4(4) . 4_575 ? B6 B12 B6 108.4(4) . 4_575 ? B5 B12 B7 109.2(3) 4_575 . ? B5 B12 B7 109.2(3) . . ? B6 B12 B7 59.6(2) . . ? B6 B12 B7 59.6(2) 4_575 . ? B5 B12 H12 120.0 4_575 . ? B5 B12 H12 120.0 . . ? B6 B12 H12 121.1 . . ? B6 B12 H12 121.1 4_575 . ? B7 B12 H12 121.9 . . ? B7 B6 B12 60.4(3) . . ? B7 B6 B5 108.3(3) . . ? B12 B6 B5 59.2(3) . . ? B7 B6 H6 121.3 . . ? B12 B6 H6 120.5 . . ? B5 B6 H6 120.6 . . ? C13 C14 C15 107.5(5) . . ? C13 C14 Fe1 70.5(2) . . ? C15 C14 Fe1 69.5(3) . . ? C13 C14 H14 126.2 . . ? C15 C14 H14 126.2 . . ? Fe1 C14 H14 125.4 . . ? B6 B7 B6 108.9(4) 4_575 . ? B6 B7 B12 59.9(2) 4_575 . ? B6 B7 B12 59.9(2) . . ? B6 B7 B4 63.2(2) 4_575 4_575 ? B6 B7 B4 110.1(4) . 4_575 ? B12 B7 B4 111.1(4) . 4_575 ? B6 B7 H7 120.5 4_575 . ? B6 B7 H7 120.5 . . ? B12 B7 H7 120.5 . . ? B4 B7 H7 120.2 4_575 . ? C14 C15 C14 108.3(6) 4_575 . ? C14 C15 Fe1 70.4(3) 4_575 . ? C14 C15 Fe1 70.4(3) . . ? C14 C15 H15 125.8 4_575 . ? C14 C15 H15 125.8 . . ? Fe1 C15 H15 125.0 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.761 _refine_diff_density_min -0.882 _refine_diff_density_rms 0.109 data_mgsl2942 _database_code_depnum_ccdc_archive 'CCDC 238384' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H14 B8 Fe P2' _chemical_formula_sum 'C6 H14 B8 Fe P2' _chemical_formula_weight 290.44 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' P P 0.1023 0.0942 '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 C2/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' '-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 26.8072(15) _cell_length_b 6.9641(6) _cell_length_c 16.3096(11) _cell_angle_alpha 90.00 _cell_angle_beta 124.336(4) _cell_angle_gamma 90.00 _cell_volume 2514.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour Red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 1.413 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7370 _exptl_absorpt_correction_T_max 0.9327 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _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_collimation miracol _diffrn_radiation_polarisn_norm ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_detector 'CCD plate' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4632 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_sigmaI/netI 0.0837 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 26.01 _reflns_number_total 2191 _reflns_number_gt 1787 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_data_reduction ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SHELXS-97 (Sheldrick, 1986) ; _computing_structure_refinement ; SHELXS-97 (Sheldrick, 1986) ; _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material ; 'enCIFer (CCDC, 2002)' ; _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 'w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+18.3102P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2191 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1643 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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 0.10974(4) 0.27556(11) 0.16680(5) 0.0299(3) Uani 1 1 d . . . P2 P 0.12450(8) -0.0132(2) 0.12029(11) 0.0383(4) Uani 1 1 d . . . P3 P 0.04429(7) 0.1837(2) 0.00698(10) 0.0342(4) Uani 1 1 d . . . C5 C 0.1638(3) 0.4117(9) 0.1328(5) 0.0392(14) Uani 1 1 d . . . H5 H 0.1857 0.5371 0.1842 0.047 Uiso 1 1 calc R . . C13 C 0.0784(3) 0.1610(10) 0.2482(5) 0.0473(16) Uani 1 1 d . . . H13 H 0.0640 0.0339 0.2432 0.057 Uiso 1 1 calc R . . C14 C 0.0429(3) 0.3220(10) 0.1926(4) 0.0420(14) Uani 1 1 d . . . H14 H 0.0006 0.3215 0.1433 0.050 Uiso 1 1 calc R . . C15 C 0.0816(3) 0.4835(10) 0.2238(4) 0.0421(14) Uani 1 1 d . . . H15 H 0.0697 0.6108 0.1993 0.050 Uiso 1 1 calc R . . C16 C 0.1404(3) 0.4233(11) 0.2971(5) 0.0502(17) Uani 1 1 d . . . H16 H 0.1754 0.5024 0.3309 0.060 Uiso 1 1 calc R . . C17 C 0.1385(4) 0.2221(11) 0.3118(5) 0.0550(19) Uani 1 1 d . . . H17 H 0.1721 0.1434 0.3568 0.066 Uiso 1 1 calc R . . B4 B 0.0904(3) 0.4373(10) 0.0426(5) 0.0340(14) Uani 1 1 d . . . H4 H 0.0643 0.5715 0.0318 0.041 Uiso 1 1 calc R . . B6 B 0.1901(3) 0.1927(11) 0.1829(5) 0.0408(15) Uani 1 1 d . . . H6 H 0.2282 0.1705 0.2625 0.049 Uiso 1 1 calc R . . B7 B 0.1026(3) 0.0471(11) -0.0231(5) 0.0391(15) Uani 1 1 d . . . H7 H 0.0826 -0.0747 -0.0774 0.047 Uiso 1 1 calc R . . B8 B 0.0813(4) 0.2951(10) -0.0620(5) 0.0396(16) Uani 1 1 d . . . H8 H 0.0474 0.3318 -0.1420 0.048 Uiso 1 1 calc R . . B9 B 0.1453(4) 0.4391(11) 0.0147(6) 0.0457(18) Uani 1 1 d . . . H9 H 0.1526 0.5733 -0.0150 0.055 Uiso 1 1 calc R . . B10 B 0.2061(4) 0.2920(12) 0.0998(7) 0.0501(19) Uani 1 1 d . . . H10 H 0.2536 0.3289 0.1262 0.060 Uiso 1 1 calc R . . B11 B 0.1820(3) 0.0510(11) 0.0805(6) 0.0426(16) Uani 1 1 d . . . H11 H 0.2132 -0.0696 0.0932 0.051 Uiso 1 1 calc R . . B12 B 0.1538(4) 0.2087(11) -0.0209(6) 0.0436(17) Uani 1 1 d . . . H12 H 0.1667 0.1885 -0.0748 0.052 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 0.0290(5) 0.0307(5) 0.0319(5) 0.0005(3) 0.0183(4) 0.0009(3) P2 0.0484(10) 0.0270(8) 0.0437(8) 0.0020(6) 0.0285(8) 0.0026(6) P3 0.0277(8) 0.0399(9) 0.0360(7) -0.0036(6) 0.0185(6) -0.0027(6) C5 0.037(3) 0.036(3) 0.053(3) -0.012(3) 0.031(3) -0.011(3) C13 0.071(5) 0.041(4) 0.053(4) 0.003(3) 0.049(4) -0.004(3) C14 0.038(3) 0.057(4) 0.040(3) -0.002(3) 0.027(3) 0.001(3) C15 0.052(4) 0.040(4) 0.047(3) 0.001(3) 0.035(3) 0.008(3) C16 0.050(4) 0.064(5) 0.040(3) -0.014(3) 0.028(3) -0.012(3) C17 0.065(5) 0.068(5) 0.035(3) 0.010(3) 0.030(3) 0.019(4) B4 0.039(4) 0.029(3) 0.042(3) 0.001(3) 0.029(3) 0.003(3) B6 0.029(4) 0.041(4) 0.048(4) -0.007(3) 0.020(3) 0.002(3) B7 0.039(4) 0.042(4) 0.044(3) -0.009(3) 0.028(3) -0.002(3) B8 0.053(5) 0.033(4) 0.040(3) 0.002(3) 0.030(3) 0.001(3) B9 0.071(5) 0.032(4) 0.062(4) -0.004(3) 0.055(4) -0.005(3) B10 0.040(4) 0.056(5) 0.072(5) -0.018(4) 0.042(4) -0.008(4) B11 0.034(4) 0.039(4) 0.058(4) -0.008(3) 0.027(3) 0.004(3) B12 0.052(5) 0.040(4) 0.061(4) -0.006(3) 0.045(4) -0.005(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 C5 2.053(6) . ? Fe1 C17 2.066(6) . ? Fe1 C16 2.068(6) . ? Fe1 C15 2.080(6) . ? Fe1 C14 2.086(6) . ? Fe1 C13 2.089(6) . ? Fe1 B6 2.099(7) . ? Fe1 B4 2.111(6) . ? Fe1 P2 2.2616(17) . ? Fe1 P3 2.2633(16) . ? P2 B11 2.031(8) . ? P2 B6 2.042(8) . ? P2 B7 2.107(7) . ? P2 P3 2.332(2) . ? P3 B8 2.028(7) . ? P3 B4 2.043(7) . ? P3 B7 2.110(7) . ? C5 B4 1.675(9) . ? C5 B6 1.685(10) . ? C5 B9 1.707(9) . ? C5 B10 1.721(9) . ? C5 H5 1.1200 . ? C13 C17 1.403(11) . ? C13 C14 1.419(10) . ? C13 H13 0.9500 . ? C14 C15 1.416(10) . ? C14 H14 0.9500 . ? C15 C16 1.403(10) . ? C15 H15 0.9500 . ? C16 C17 1.427(11) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? B4 B9 1.767(9) . ? B4 B8 1.866(9) . ? B4 H4 1.1200 . ? B6 B10 1.777(11) . ? B6 B11 1.844(10) . ? B6 H6 1.1200 . ? B7 B12 1.761(10) . ? B7 B8 1.817(10) . ? B7 B11 1.825(10) . ? B7 H7 1.1200 . ? B8 B9 1.759(11) . ? B8 B12 1.767(11) . ? B8 H8 1.1200 . ? B9 B10 1.755(12) . ? B9 B12 1.765(10) . ? B9 H9 1.1200 . ? B10 B12 1.750(11) . ? B10 B11 1.762(11) . ? B10 H10 1.1200 . ? B11 B12 1.761(11) . ? B11 H11 1.1200 . ? B12 H12 1.1200 . ? 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 C5 Fe1 C17 121.8(3) . . ? C5 Fe1 C16 96.6(3) . . ? C17 Fe1 C16 40.4(3) . . ? C5 Fe1 C15 106.8(3) . . ? C17 Fe1 C15 67.0(3) . . ? C16 Fe1 C15 39.5(3) . . ? C5 Fe1 C14 143.3(3) . . ? C17 Fe1 C14 66.7(3) . . ? C16 Fe1 C14 66.7(3) . . ? C15 Fe1 C14 39.7(3) . . ? C5 Fe1 C13 161.1(3) . . ? C17 Fe1 C13 39.5(3) . . ? C16 Fe1 C13 66.8(3) . . ? C15 Fe1 C13 66.7(3) . . ? C14 Fe1 C13 39.7(3) . . ? C5 Fe1 B6 47.9(3) . . ? C17 Fe1 B6 96.5(3) . . ? C16 Fe1 B6 102.9(3) . . ? C15 Fe1 B6 137.9(3) . . ? C14 Fe1 B6 163.0(3) . . ? C13 Fe1 B6 124.6(3) . . ? C5 Fe1 B4 47.4(3) . . ? C17 Fe1 B4 157.8(3) . . ? C16 Fe1 B4 117.4(3) . . ? C15 Fe1 B4 95.9(2) . . ? C14 Fe1 B4 109.7(3) . . ? C13 Fe1 B4 147.6(3) . . ? B6 Fe1 B4 86.9(3) . . ? C5 Fe1 P2 92.08(18) . . ? C17 Fe1 P2 101.6(2) . . ? C16 Fe1 P2 138.0(2) . . ? C15 Fe1 P2 161.00(19) . . ? C14 Fe1 P2 122.6(2) . . ? C13 Fe1 P2 94.7(2) . . ? B6 Fe1 P2 55.7(2) . . ? B4 Fe1 P2 98.48(18) . . ? C5 Fe1 P3 91.52(18) . . ? C17 Fe1 P3 144.5(2) . . ? C16 Fe1 P3 157.6(2) . . ? C15 Fe1 P3 118.06(19) . . ? C14 Fe1 P3 94.59(18) . . ? C13 Fe1 P3 107.2(2) . . ? B6 Fe1 P3 98.1(2) . . ? B4 Fe1 P3 55.55(19) . . ? P2 Fe1 P3 62.04(6) . . ? B11 P2 B6 53.8(3) . . ? B11 P2 B7 52.3(3) . . ? B6 P2 B7 92.1(3) . . ? B11 P2 Fe1 102.7(2) . . ? B6 P2 Fe1 58.1(2) . . ? B7 P2 Fe1 101.7(2) . . ? B11 P2 P3 98.3(2) . . ? B6 P2 P3 97.6(2) . . ? B7 P2 P3 56.5(2) . . ? Fe1 P2 P3 59.02(6) . . ? B8 P3 B4 54.6(3) . . ? B8 P3 B7 52.1(3) . . ? B4 P3 B7 92.7(3) . . ? B8 P3 Fe1 103.1(2) . . ? B4 P3 Fe1 58.45(18) . . ? B7 P3 Fe1 101.6(2) . . ? B8 P3 P2 98.3(2) . . ? B4 P3 P2 98.3(2) . . ? B7 P3 P2 56.4(2) . . ? Fe1 P3 P2 58.94(6) . . ? B4 C5 B6 119.0(5) . . ? B4 C5 B9 63.0(4) . . ? B6 C5 B9 115.1(5) . . ? B4 C5 B10 115.6(5) . . ? B6 C5 B10 62.9(4) . . ? B9 C5 B10 61.6(4) . . ? B4 C5 Fe1 68.1(3) . . ? B6 C5 Fe1 67.5(3) . . ? B9 C5 Fe1 123.7(4) . . ? B10 C5 Fe1 123.5(4) . . ? B4 C5 H5 115.7 . . ? B6 C5 H5 116.3 . . ? B9 C5 H5 117.0 . . ? B10 C5 H5 116.9 . . ? Fe1 C5 H5 108.0 . . ? C17 C13 C14 108.1(6) . . ? C17 C13 Fe1 69.4(4) . . ? C14 C13 Fe1 70.0(3) . . ? C17 C13 H13 126.0 . . ? C14 C13 H13 126.0 . . ? Fe1 C13 H13 126.2 . . ? C15 C14 C13 107.8(6) . . ? C15 C14 Fe1 69.9(3) . . ? C13 C14 Fe1 70.3(4) . . ? C15 C14 H14 126.1 . . ? C13 C14 H14 126.1 . . ? Fe1 C14 H14 125.3 . . ? C16 C15 C14 108.2(6) . . ? C16 C15 Fe1 69.8(4) . . ? C14 C15 Fe1 70.3(3) . . ? C16 C15 H15 125.9 . . ? C14 C15 H15 125.9 . . ? Fe1 C15 H15 125.6 . . ? C15 C16 C17 107.9(6) . . ? C15 C16 Fe1 70.7(3) . . ? C17 C16 Fe1 69.7(4) . . ? C15 C16 H16 126.1 . . ? C17 C16 H16 126.1 . . ? Fe1 C16 H16 125.1 . . ? C13 C17 C16 108.0(6) . . ? C13 C17 Fe1 71.1(4) . . ? C16 C17 Fe1 69.9(4) . . ? C13 C17 H17 126.0 . . ? C16 C17 H17 126.0 . . ? Fe1 C17 H17 124.6 . . ? C5 B4 B9 59.4(4) . . ? C5 B4 B8 103.3(5) . . ? B9 B4 B8 57.8(4) . . ? C5 B4 P3 112.4(4) . . ? B9 B4 P3 113.0(4) . . ? B8 B4 P3 62.3(3) . . ? C5 B4 Fe1 64.5(3) . . ? B9 B4 Fe1 117.4(4) . . ? B8 B4 Fe1 115.4(4) . . ? P3 B4 Fe1 66.0(2) . . ? C5 B4 H4 123.2 . . ? B9 B4 H4 119.3 . . ? B8 B4 H4 123.4 . . ? P3 B4 H4 116.9 . . ? Fe1 B4 H4 113.0 . . ? C5 B6 B10 59.5(4) . . ? C5 B6 B11 104.0(5) . . ? B10 B6 B11 58.2(4) . . ? C5 B6 P2 112.7(4) . . ? B10 B6 P2 113.7(5) . . ? B11 B6 P2 62.8(3) . . ? C5 B6 Fe1 64.6(3) . . ? B10 B6 Fe1 118.1(5) . . ? B11 B6 Fe1 116.4(4) . . ? P2 B6 Fe1 66.2(2) . . ? C5 B6 H6 123.0 . . ? B10 B6 H6 119.0 . . ? B11 B6 H6 122.7 . . ? P2 B6 H6 116.5 . . ? Fe1 B6 H6 112.5 . . ? B12 B7 B8 59.2(4) . . ? B12 B7 B11 58.8(4) . . ? B8 B7 B11 106.4(5) . . ? B12 B7 P2 112.3(4) . . ? B8 B7 P2 114.4(4) . . ? B11 B7 P2 61.7(3) . . ? B12 B7 P3 112.2(4) . . ? B8 B7 P3 61.6(3) . . ? B11 B7 P3 114.1(4) . . ? P2 B7 P3 67.1(2) . . ? B12 B7 H7 121.3 . . ? B8 B7 H7 121.8 . . ? B11 B7 H7 122.1 . . ? P2 B7 H7 115.9 . . ? P3 B7 H7 116.0 . . ? B9 B8 B12 60.1(4) . . ? B9 B8 B7 107.8(5) . . ? B12 B8 B7 58.8(4) . . ? B9 B8 B4 58.3(4) . . ? B12 B8 B4 106.6(5) . . ? B7 B8 B4 109.4(4) . . ? B9 B8 P3 114.1(4) . . ? B12 B8 P3 115.9(4) . . ? B7 B8 P3 66.3(3) . . ? B4 B8 P3 63.1(3) . . ? B9 B8 H8 121.6 . . ? B12 B8 H8 121.2 . . ? B7 B8 H8 120.9 . . ? B4 B8 H8 123.0 . . ? P3 B8 H8 113.8 . . ? C5 B9 B10 59.6(4) . . ? C5 B9 B8 106.6(5) . . ? B10 B9 B8 109.2(5) . . ? C5 B9 B12 105.1(5) . . ? B10 B9 B12 59.6(5) . . ? B8 B9 B12 60.2(4) . . ? C5 B9 B4 57.6(3) . . ? B10 B9 B4 109.3(5) . . ? B8 B9 B4 63.9(4) . . ? B12 B9 B4 111.1(5) . . ? C5 B9 H9 124.9 . . ? B10 B9 H9 121.2 . . ? B8 B9 H9 120.4 . . ? B12 B9 H9 121.9 . . ? B4 B9 H9 119.4 . . ? C5 B10 B12 105.2(5) . . ? C5 B10 B9 58.8(4) . . ? B12 B10 B9 60.5(5) . . ? C5 B10 B11 106.1(5) . . ? B12 B10 B11 60.2(4) . . ? B9 B10 B11 109.3(6) . . ? C5 B10 B6 57.6(4) . . ? B12 B10 B6 110.1(5) . . ? B9 B10 B6 108.2(5) . . ? B11 B10 B6 62.8(4) . . ? C5 B10 H10 125.1 . . ? B12 B10 H10 121.7 . . ? B9 B10 H10 121.2 . . ? B11 B10 H10 120.7 . . ? B6 B10 H10 120.4 . . ? B12 B11 B10 59.6(5) . . ? B12 B11 B7 58.8(4) . . ? B10 B11 B7 107.4(5) . . ? B12 B11 B6 106.6(5) . . ? B10 B11 B6 59.0(4) . . ? B7 B11 B6 109.1(5) . . ? B12 B11 P2 115.9(4) . . ? B10 B11 P2 114.9(4) . . ? B7 B11 P2 66.0(3) . . ? B6 B11 P2 63.4(3) . . ? B12 B11 H11 121.4 . . ? B10 B11 H11 121.4 . . ? B7 B11 H11 121.3 . . ? B6 B11 H11 122.7 . . ? P2 B11 H11 113.5 . . ? B10 B12 B7 110.9(5) . . ? B10 B12 B11 60.2(5) . . ? B7 B12 B11 62.4(4) . . ? B10 B12 B9 59.9(5) . . ? B7 B12 B9 110.1(5) . . ? B11 B12 B9 108.9(5) . . ? B10 B12 B8 109.1(5) . . ? B7 B12 B8 62.0(4) . . ? B11 B12 B8 111.5(5) . . ? B9 B12 B8 59.7(4) . . ? B10 B12 H12 121.2 . . ? B7 B12 H12 119.1 . . ? B11 B12 H12 120.0 . . ? B9 B12 H12 121.8 . . ? B8 B12 H12 120.3 . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.889 _refine_diff_density_max 1.185 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.117