Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_requested_category FM _publ_contact_author_name 'Rudolf Pirtschnig' _publ_contact_author_address ; Institute of Chemistry, Karl-Franzens University Graz, Schubertstr. 1, A-8010 Graz, Austria ; _publ_contact_author_email rudolf.pietschnig@uni-graz.at _publ_contact_author_fax 43(316)3809835 _publ_contact_author_phone 43(316)3805287 _publ_section_title ; The Homologous Series of 1,1'-Ferrocenylenebisdihalophosphanes (C5H4PX2)2Fe (X = F, Cl, Br, I): Precursors for the First Metallocene Bridged Bisphosphaalkene ; loop_ _publ_author_name _publ_author_address 'Rudolf Pietschnig' ; Institute of Chemistry, Karl-Franzens University Graz, Schubertstr. 1, A-8010 Graz, Austria ; 'Ferdinand Belaj' ; ; 'Carmen Moser' ; ; 'Martin Nieger' ; ; #============================================================================== data_rp104a_compound_3b. _database_code_depnum_ccdc_archive 'CCDC 102240' _audit_creation_method 'manual edited SHELXL-97 .cif file' _chemical_name_systematic ; 1,1'-bis(dichlorophosphano)ferrocene ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H8 Cl4 Fe P2' _chemical_formula_sum 'C10 H8 Cl4 Fe P2' _chemical_formula_weight 387.75 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' 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' 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 #(no.14) 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 6.7838(1) _cell_length_b 11.2938(3) _cell_length_c 17.8651(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.105(2) _cell_angle_gamma 90.00 _cell_volume 1358.22(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 13.943 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rods _exptl_crystal_colour brownish _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 2.103 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.56135 _exptl_absorpt_correction_T_max 0.71894 _exptl_special_details ; dx = 34.945(2) mm, mos.= 0.481(1) 2 x 45 sec., 1 deg., 591 frames ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22012 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 28.37 _reflns_number_total 3339 _reflns_number_gt 2817 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0343P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3339 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0297 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0612 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.18489(3) 0.200877(18) 0.585470(11) 0.01338(8) Uani 1 d . . . Cl1 Cl 0.24681(6) 0.39468(4) 0.76201(2) 0.02814(11) Uani 1 d . . . Cl2 Cl -0.20653(5) 0.46187(3) 0.73249(2) 0.02317(10) Uani 1 d . . . Cl3 Cl 0.57324(6) 0.35317(4) 0.38913(2) 0.02966(12) Uani 1 d . . . Cl4 Cl 0.13433(6) 0.25394(3) 0.36886(2) 0.02573(11) Uani 1 d . . . P1 P 0.03526(6) 0.43776(4) 0.67291(2) 0.01832(10) Uani 1 d . . . P2 P 0.31610(6) 0.35974(3) 0.44155(2) 0.01745(10) Uani 1 d . . . C1 C -0.0214(2) 0.29405(13) 0.63397(8) 0.0161(3) Uani 1 d . . . C2 C 0.0007(2) 0.17863(13) 0.66704(9) 0.0172(3) Uani 1 d . . . H2 H 0.0403 0.1614 0.7188 0.021 Uiso 1 calc R . . C3 C -0.0472(2) 0.09456(14) 0.60842(9) 0.0199(3) Uani 1 d . . . H3 H -0.0451 0.0110 0.6144 0.024 Uiso 1 calc R . . C4 C -0.0990(2) 0.15618(14) 0.53945(9) 0.0200(3) Uani 1 d . . . H4 H -0.1372 0.1209 0.4916 0.024 Uiso 1 calc R . . C5 C -0.0838(2) 0.27961(14) 0.55442(9) 0.0184(3) Uani 1 d . . . H5 H -0.1101 0.3414 0.5185 0.022 Uiso 1 calc R . . C6 C 0.3829(2) 0.25715(13) 0.51670(8) 0.0155(3) Uani 1 d . . . C7 C 0.4426(2) 0.29606(13) 0.59288(8) 0.0169(3) Uani 1 d . . . H7 H 0.4593 0.3759 0.6091 0.020 Uiso 1 calc R . . C8 C 0.4718(2) 0.19449(14) 0.63922(9) 0.0182(3) Uani 1 d . . . H8 H 0.5120 0.1944 0.6921 0.022 Uiso 1 calc R . . C9 C 0.4311(2) 0.09293(14) 0.59352(9) 0.0185(3) Uani 1 d . . . H9 H 0.4391 0.0132 0.6105 0.022 Uiso 1 calc R . . C10 C 0.3761(2) 0.13063(13) 0.51775(8) 0.0167(3) Uani 1 d . . . H10 H 0.3411 0.0806 0.4754 0.020 Uiso 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 0.01098(13) 0.01686(13) 0.01214(13) -0.00051(8) 0.00078(9) 0.00044(8) Cl1 0.0209(2) 0.0371(3) 0.0243(2) -0.01151(18) -0.00570(16) 0.00369(18) Cl2 0.0193(2) 0.0283(2) 0.0226(2) -0.00573(16) 0.00537(16) 0.00321(16) Cl3 0.0215(2) 0.0478(3) 0.0204(2) 0.01014(18) 0.00526(16) 0.00024(19) Cl4 0.0295(2) 0.0255(2) 0.0195(2) 0.00092(16) -0.00746(17) -0.00529(17) P1 0.0164(2) 0.0198(2) 0.0189(2) -0.00190(16) 0.00302(16) 0.00043(16) P2 0.0177(2) 0.0182(2) 0.0160(2) 0.00077(16) 0.00034(15) -0.00103(16) C1 0.0115(7) 0.0219(8) 0.0149(8) -0.0017(6) 0.0020(6) 0.0012(6) C2 0.0134(7) 0.0227(8) 0.0160(8) -0.0008(6) 0.0042(6) -0.0016(6) C3 0.0155(8) 0.0202(8) 0.0248(9) -0.0027(7) 0.0058(6) -0.0039(6) C4 0.0130(8) 0.0285(9) 0.0177(8) -0.0066(7) -0.0009(6) -0.0024(7) C5 0.0120(7) 0.0258(8) 0.0167(8) 0.0001(6) -0.0010(6) 0.0028(6) C6 0.0107(7) 0.0206(8) 0.0152(8) 0.0000(6) 0.0020(6) -0.0005(6) C7 0.0106(7) 0.0231(8) 0.0166(8) -0.0016(6) 0.0003(6) -0.0011(6) C8 0.0107(8) 0.0298(9) 0.0137(8) 0.0008(6) -0.0007(6) 0.0022(6) C9 0.0142(8) 0.0220(8) 0.0198(8) 0.0040(6) 0.0037(6) 0.0056(6) C10 0.0136(7) 0.0202(8) 0.0166(8) -0.0020(6) 0.0032(6) 0.0021(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 C1 2.0290(14) . ? Fe1 C6 2.0313(14) . ? Fe1 C10 2.0407(14) . ? Fe1 C5 2.0425(14) . ? Fe1 C7 2.0424(14) . ? Fe1 C2 2.0489(14) . ? Fe1 C9 2.0585(14) . ? Fe1 C4 2.0611(14) . ? Fe1 C3 2.0615(15) . ? Fe1 C8 2.0625(14) . ? Cl1 P1 2.0651(6) . ? Cl2 P1 2.0806(5) . ? Cl3 P2 2.0808(6) . ? Cl4 P2 2.0588(5) . ? P1 C1 1.7888(15) . ? P2 C6 1.7888(15) . ? C1 C2 1.431(2) . ? C1 C5 1.441(2) . ? C2 C3 1.421(2) . ? C3 C4 1.421(2) . ? C4 C5 1.421(2) . ? C6 C10 1.430(2) . ? C6 C7 1.440(2) . ? C7 C8 1.414(2) . ? C8 C9 1.415(2) . ? C9 C10 1.424(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C6 129.70(6) . . ? C1 Fe1 C10 167.81(6) . . ? C6 Fe1 C10 41.11(6) . . ? C1 Fe1 C5 41.45(6) . . ? C6 Fe1 C5 109.54(6) . . ? C10 Fe1 C5 128.30(6) . . ? C1 Fe1 C7 109.23(6) . . ? C6 Fe1 C7 41.39(6) . . ? C10 Fe1 C7 68.98(6) . . ? C5 Fe1 C7 121.10(6) . . ? C1 Fe1 C2 41.09(6) . . ? C6 Fe1 C2 167.31(6) . . ? C10 Fe1 C2 149.57(6) . . ? C5 Fe1 C2 69.16(6) . . ? C7 Fe1 C2 127.64(6) . . ? C1 Fe1 C9 150.92(6) . . ? C6 Fe1 C9 68.65(6) . . ? C10 Fe1 C9 40.65(6) . . ? C5 Fe1 C9 165.03(6) . . ? C7 Fe1 C9 68.08(6) . . ? C2 Fe1 C9 116.01(6) . . ? C1 Fe1 C4 68.75(6) . . ? C6 Fe1 C4 119.38(6) . . ? C10 Fe1 C4 107.42(6) . . ? C5 Fe1 C4 40.51(6) . . ? C7 Fe1 C4 154.79(6) . . ? C2 Fe1 C4 68.40(6) . . ? C9 Fe1 C4 126.36(6) . . ? C1 Fe1 C3 68.46(6) . . ? C6 Fe1 C3 151.78(6) . . ? C10 Fe1 C3 116.66(6) . . ? C5 Fe1 C3 68.25(6) . . ? C7 Fe1 C3 164.24(6) . . ? C2 Fe1 C3 40.46(6) . . ? C9 Fe1 C3 105.92(6) . . ? C4 Fe1 C3 40.32(6) . . ? C1 Fe1 C8 118.72(6) . . ? C6 Fe1 C8 68.64(6) . . ? C10 Fe1 C8 68.28(6) . . ? C5 Fe1 C8 154.28(6) . . ? C7 Fe1 C8 40.30(6) . . ? C2 Fe1 C8 106.73(6) . . ? C9 Fe1 C8 40.17(6) . . ? C4 Fe1 C8 163.46(6) . . ? C3 Fe1 C8 125.96(6) . . ? C1 P1 Cl1 100.45(5) . . ? C1 P1 Cl2 99.94(5) . . ? Cl1 P1 Cl2 98.81(2) . . ? C6 P2 Cl4 100.01(5) . . ? C6 P2 Cl3 99.55(5) . . ? Cl4 P2 Cl3 99.52(2) . . ? C2 C1 C5 107.89(13) . . ? C2 C1 P1 131.24(12) . . ? C5 C1 P1 120.60(12) . . ? C2 C1 Fe1 70.20(8) . . ? C5 C1 Fe1 69.77(8) . . ? P1 C1 Fe1 120.68(7) . . ? C3 C2 C1 107.55(14) . . ? C3 C2 Fe1 70.25(8) . . ? C1 C2 Fe1 68.71(8) . . ? C4 C3 C2 108.74(14) . . ? C4 C3 Fe1 69.83(9) . . ? C2 C3 Fe1 69.29(8) . . ? C5 C4 C3 108.23(13) . . ? C5 C4 Fe1 69.04(8) . . ? C3 C4 Fe1 69.85(8) . . ? C4 C5 C1 107.60(14) . . ? C4 C5 Fe1 70.45(8) . . ? C1 C5 Fe1 68.77(8) . . ? C10 C6 C7 107.37(13) . . ? C10 C6 P2 130.66(11) . . ? C7 C6 P2 121.82(11) . . ? C10 C6 Fe1 69.79(8) . . ? C7 C6 Fe1 69.72(8) . . ? P2 C6 Fe1 122.10(7) . . ? C8 C7 C6 107.97(13) . . ? C8 C7 Fe1 70.61(8) . . ? C6 C7 Fe1 68.89(8) . . ? C7 C8 C9 108.45(13) . . ? C7 C8 Fe1 69.08(8) . . ? C9 C8 Fe1 69.76(8) . . ? C8 C9 C10 108.40(14) . . ? C8 C9 Fe1 70.07(8) . . ? C10 C9 Fe1 69.00(8) . . ? C9 C10 C6 107.82(13) . . ? C9 C10 Fe1 70.34(8) . . ? C6 C10 Fe1 69.09(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 P1 C1 C2 23.18(14) . . . . ? Cl2 P1 C1 C2 -77.80(14) . . . . ? Cl1 P1 C1 C5 -149.92(11) . . . . ? Cl2 P1 C1 C5 109.09(11) . . . . ? Cl1 P1 C1 Fe1 -66.60(8) . . . . ? Cl2 P1 C1 Fe1 -167.58(7) . . . . ? C6 Fe1 C1 C2 -167.74(8) . . . . ? C10 Fe1 C1 C2 154.9(3) . . . . ? C5 Fe1 C1 C2 118.72(13) . . . . ? C7 Fe1 C1 C2 -125.73(9) . . . . ? C9 Fe1 C1 C2 -46.46(16) . . . . ? C4 Fe1 C1 C2 81.08(9) . . . . ? C3 Fe1 C1 C2 37.63(9) . . . . ? C8 Fe1 C1 C2 -82.61(10) . . . . ? C6 Fe1 C1 C5 73.54(11) . . . . ? C10 Fe1 C1 C5 36.1(3) . . . . ? C7 Fe1 C1 C5 115.55(9) . . . . ? C2 Fe1 C1 C5 -118.72(13) . . . . ? C9 Fe1 C1 C5 -165.18(11) . . . . ? C4 Fe1 C1 C5 -37.64(9) . . . . ? C3 Fe1 C1 C5 -81.09(10) . . . . ? C8 Fe1 C1 C5 158.67(9) . . . . ? C6 Fe1 C1 P1 -40.80(12) . . . . ? C10 Fe1 C1 P1 -78.2(3) . . . . ? C5 Fe1 C1 P1 -114.34(13) . . . . ? C7 Fe1 C1 P1 1.21(11) . . . . ? C2 Fe1 C1 P1 126.94(13) . . . . ? C9 Fe1 C1 P1 80.48(15) . . . . ? C4 Fe1 C1 P1 -151.98(11) . . . . ? C3 Fe1 C1 P1 164.57(11) . . . . ? C8 Fe1 C1 P1 44.33(11) . . . . ? C5 C1 C2 C3 0.08(16) . . . . ? P1 C1 C2 C3 -173.68(11) . . . . ? Fe1 C1 C2 C3 -59.76(10) . . . . ? C5 C1 C2 Fe1 59.85(10) . . . . ? P1 C1 C2 Fe1 -113.92(13) . . . . ? C1 Fe1 C2 C3 118.93(13) . . . . ? C6 Fe1 C2 C3 167.0(2) . . . . ? C10 Fe1 C2 C3 -50.88(16) . . . . ? C5 Fe1 C2 C3 80.52(10) . . . . ? C7 Fe1 C2 C3 -165.63(9) . . . . ? C9 Fe1 C2 C3 -84.16(10) . . . . ? C4 Fe1 C2 C3 36.93(9) . . . . ? C8 Fe1 C2 C3 -126.33(10) . . . . ? C6 Fe1 C2 C1 48.1(3) . . . . ? C10 Fe1 C2 C1 -169.80(11) . . . . ? C5 Fe1 C2 C1 -38.40(9) . . . . ? C7 Fe1 C2 C1 75.44(11) . . . . ? C9 Fe1 C2 C1 156.92(8) . . . . ? C4 Fe1 C2 C1 -82.00(9) . . . . ? C3 Fe1 C2 C1 -118.93(13) . . . . ? C8 Fe1 C2 C1 114.74(9) . . . . ? C1 C2 C3 C4 -0.04(17) . . . . ? Fe1 C2 C3 C4 -58.83(10) . . . . ? C1 C2 C3 Fe1 58.79(10) . . . . ? C1 Fe1 C3 C4 82.11(10) . . . . ? C6 Fe1 C3 C4 -53.68(16) . . . . ? C10 Fe1 C3 C4 -85.77(10) . . . . ? C5 Fe1 C3 C4 37.35(9) . . . . ? C7 Fe1 C3 C4 166.7(2) . . . . ? C2 Fe1 C3 C4 120.32(13) . . . . ? C9 Fe1 C3 C4 -128.07(9) . . . . ? C8 Fe1 C3 C4 -167.29(9) . . . . ? C1 Fe1 C3 C2 -38.20(9) . . . . ? C6 Fe1 C3 C2 -174.00(11) . . . . ? C10 Fe1 C3 C2 153.92(9) . . . . ? C5 Fe1 C3 C2 -82.97(10) . . . . ? C7 Fe1 C3 C2 46.4(3) . . . . ? C9 Fe1 C3 C2 111.61(10) . . . . ? C4 Fe1 C3 C2 -120.32(13) . . . . ? C8 Fe1 C3 C2 72.39(11) . . . . ? C2 C3 C4 C5 -0.02(17) . . . . ? Fe1 C3 C4 C5 -58.53(10) . . . . ? C2 C3 C4 Fe1 58.51(10) . . . . ? C1 Fe1 C4 C5 38.49(9) . . . . ? C6 Fe1 C4 C5 -86.09(10) . . . . ? C10 Fe1 C4 C5 -129.25(9) . . . . ? C7 Fe1 C4 C5 -51.72(18) . . . . ? C2 Fe1 C4 C5 82.79(9) . . . . ? C9 Fe1 C4 C5 -170.10(9) . . . . ? C3 Fe1 C4 C5 119.83(13) . . . . ? C8 Fe1 C4 C5 158.57(19) . . . . ? C1 Fe1 C4 C3 -81.35(9) . . . . ? C6 Fe1 C4 C3 154.07(9) . . . . ? C10 Fe1 C4 C3 110.92(9) . . . . ? C5 Fe1 C4 C3 -119.83(13) . . . . ? C7 Fe1 C4 C3 -171.55(13) . . . . ? C2 Fe1 C4 C3 -37.05(9) . . . . ? C9 Fe1 C4 C3 70.06(11) . . . . ? C8 Fe1 C4 C3 38.7(2) . . . . ? C3 C4 C5 C1 0.08(16) . . . . ? Fe1 C4 C5 C1 -58.96(10) . . . . ? C3 C4 C5 Fe1 59.03(10) . . . . ? C2 C1 C5 C4 -0.10(16) . . . . ? P1 C1 C5 C4 174.46(10) . . . . ? Fe1 C1 C5 C4 60.01(10) . . . . ? C2 C1 C5 Fe1 -60.11(10) . . . . ? P1 C1 C5 Fe1 114.44(10) . . . . ? C1 Fe1 C5 C4 -118.82(13) . . . . ? C6 Fe1 C5 C4 112.71(9) . . . . ? C10 Fe1 C5 C4 70.31(11) . . . . ? C7 Fe1 C5 C4 157.02(9) . . . . ? C2 Fe1 C5 C4 -80.74(9) . . . . ? C9 Fe1 C5 C4 32.4(3) . . . . ? C3 Fe1 C5 C4 -37.18(9) . . . . ? C8 Fe1 C5 C4 -166.13(13) . . . . ? C6 Fe1 C5 C1 -128.47(9) . . . . ? C10 Fe1 C5 C1 -170.87(8) . . . . ? C7 Fe1 C5 C1 -84.16(10) . . . . ? C2 Fe1 C5 C1 38.08(9) . . . . ? C9 Fe1 C5 C1 151.2(2) . . . . ? C4 Fe1 C5 C1 118.82(13) . . . . ? C3 Fe1 C5 C1 81.64(9) . . . . ? C8 Fe1 C5 C1 -47.31(18) . . . . ? Cl4 P2 C6 C10 19.81(14) . . . . ? Cl3 P2 C6 C10 -81.73(13) . . . . ? Cl4 P2 C6 C7 -154.96(11) . . . . ? Cl3 P2 C6 C7 103.50(11) . . . . ? Cl4 P2 C6 Fe1 -70.26(9) . . . . ? Cl3 P2 C6 Fe1 -171.80(7) . . . . ? C1 Fe1 C6 C10 -168.76(9) . . . . ? C5 Fe1 C6 C10 -126.41(8) . . . . ? C7 Fe1 C6 C10 118.37(12) . . . . ? C2 Fe1 C6 C10 151.8(2) . . . . ? C9 Fe1 C6 C10 37.73(8) . . . . ? C4 Fe1 C6 C10 -82.96(10) . . . . ? C3 Fe1 C6 C10 -46.21(16) . . . . ? C8 Fe1 C6 C10 81.01(9) . . . . ? C1 Fe1 C6 C7 72.88(11) . . . . ? C10 Fe1 C6 C7 -118.37(12) . . . . ? C5 Fe1 C6 C7 115.23(9) . . . . ? C2 Fe1 C6 C7 33.4(3) . . . . ? C9 Fe1 C6 C7 -80.64(9) . . . . ? C4 Fe1 C6 C7 158.67(9) . . . . ? C3 Fe1 C6 C7 -164.58(12) . . . . ? C8 Fe1 C6 C7 -37.36(9) . . . . ? C1 Fe1 C6 P2 -42.70(12) . . . . ? C10 Fe1 C6 P2 126.06(13) . . . . ? C5 Fe1 C6 P2 -0.35(11) . . . . ? C7 Fe1 C6 P2 -115.57(13) . . . . ? C2 Fe1 C6 P2 -82.2(3) . . . . ? C9 Fe1 C6 P2 163.79(11) . . . . ? C4 Fe1 C6 P2 43.10(11) . . . . ? C3 Fe1 C6 P2 79.85(15) . . . . ? C8 Fe1 C6 P2 -152.93(11) . . . . ? C10 C6 C7 C8 0.15(16) . . . . ? P2 C6 C7 C8 175.99(10) . . . . ? Fe1 C6 C7 C8 60.05(10) . . . . ? C10 C6 C7 Fe1 -59.91(9) . . . . ? P2 C6 C7 Fe1 115.94(10) . . . . ? C1 Fe1 C7 C8 112.05(9) . . . . ? C6 Fe1 C7 C8 -119.10(12) . . . . ? C10 Fe1 C7 C8 -80.80(9) . . . . ? C5 Fe1 C7 C8 156.27(9) . . . . ? C2 Fe1 C7 C8 69.69(11) . . . . ? C9 Fe1 C7 C8 -36.97(9) . . . . ? C4 Fe1 C7 C8 -167.18(13) . . . . ? C3 Fe1 C7 C8 33.3(3) . . . . ? C1 Fe1 C7 C6 -128.85(9) . . . . ? C10 Fe1 C7 C6 38.30(8) . . . . ? C5 Fe1 C7 C6 -84.63(10) . . . . ? C2 Fe1 C7 C6 -171.21(8) . . . . ? C9 Fe1 C7 C6 82.13(9) . . . . ? C4 Fe1 C7 C6 -48.08(18) . . . . ? C3 Fe1 C7 C6 152.4(2) . . . . ? C8 Fe1 C7 C6 119.10(12) . . . . ? C6 C7 C8 C9 -0.16(16) . . . . ? Fe1 C7 C8 C9 58.81(10) . . . . ? C6 C7 C8 Fe1 -58.97(10) . . . . ? C1 Fe1 C8 C7 -86.26(10) . . . . ? C6 Fe1 C8 C7 38.34(9) . . . . ? C10 Fe1 C8 C7 82.69(9) . . . . ? C5 Fe1 C8 C7 -52.56(18) . . . . ? C2 Fe1 C8 C7 -129.15(9) . . . . ? C9 Fe1 C8 C7 120.13(13) . . . . ? C4 Fe1 C8 C7 160.60(19) . . . . ? C3 Fe1 C8 C7 -169.38(9) . . . . ? C1 Fe1 C8 C9 153.61(9) . . . . ? C6 Fe1 C8 C9 -81.79(9) . . . . ? C10 Fe1 C8 C9 -37.43(9) . . . . ? C5 Fe1 C8 C9 -172.69(13) . . . . ? C7 Fe1 C8 C9 -120.13(13) . . . . ? C2 Fe1 C8 C9 110.72(9) . . . . ? C4 Fe1 C8 C9 40.5(2) . . . . ? C3 Fe1 C8 C9 70.49(11) . . . . ? C7 C8 C9 C10 0.12(16) . . . . ? Fe1 C8 C9 C10 58.51(10) . . . . ? C7 C8 C9 Fe1 -58.40(10) . . . . ? C1 Fe1 C9 C8 -53.31(16) . . . . ? C6 Fe1 C9 C8 81.77(9) . . . . ? C10 Fe1 C9 C8 119.92(13) . . . . ? C5 Fe1 C9 C8 167.6(2) . . . . ? C7 Fe1 C9 C8 37.09(9) . . . . ? C2 Fe1 C9 C8 -85.33(10) . . . . ? C4 Fe1 C9 C8 -166.74(9) . . . . ? C3 Fe1 C9 C8 -127.50(9) . . . . ? C1 Fe1 C9 C10 -173.23(11) . . . . ? C6 Fe1 C9 C10 -38.14(9) . . . . ? C5 Fe1 C9 C10 47.7(3) . . . . ? C7 Fe1 C9 C10 -82.83(9) . . . . ? C2 Fe1 C9 C10 154.75(9) . . . . ? C4 Fe1 C9 C10 73.34(11) . . . . ? C3 Fe1 C9 C10 112.58(9) . . . . ? C8 Fe1 C9 C10 -119.92(13) . . . . ? C8 C9 C10 C6 -0.03(16) . . . . ? Fe1 C9 C10 C6 59.14(9) . . . . ? C8 C9 C10 Fe1 -59.17(10) . . . . ? C7 C6 C10 C9 -0.07(16) . . . . ? P2 C6 C10 C9 -175.42(11) . . . . ? Fe1 C6 C10 C9 -59.93(10) . . . . ? C7 C6 C10 Fe1 59.86(10) . . . . ? P2 C6 C10 Fe1 -115.49(12) . . . . ? C1 Fe1 C10 C9 164.3(3) . . . . ? C6 Fe1 C10 C9 118.97(12) . . . . ? C5 Fe1 C10 C9 -165.91(9) . . . . ? C7 Fe1 C10 C9 80.42(10) . . . . ? C2 Fe1 C10 C9 -49.20(15) . . . . ? C4 Fe1 C10 C9 -126.04(9) . . . . ? C3 Fe1 C10 C9 -83.48(10) . . . . ? C8 Fe1 C10 C9 37.00(9) . . . . ? C1 Fe1 C10 C6 45.3(3) . . . . ? C5 Fe1 C10 C6 75.12(10) . . . . ? C7 Fe1 C10 C6 -38.55(8) . . . . ? C2 Fe1 C10 C6 -168.17(11) . . . . ? C9 Fe1 C10 C6 -118.97(12) . . . . ? C4 Fe1 C10 C6 114.99(9) . . . . ? C3 Fe1 C10 C6 157.55(8) . . . . ? C8 Fe1 C10 C6 -81.97(9) . . . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 0.565 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.095 # Attachment 'pietschnig_compound_3c.cif' data_rp104a_compound_3c _database_code_depnum_ccdc_archive 'CCDC 294451' _audit_creation_method 'manual edited SHELXL-97 .cif file' _chemical_name_systematic ; 1,1'-bis(dibromophosphano)ferrocene ; _chemical_name_common 1,1'-bis(dibromophosphano)ferrocene _chemical_melting_point ? _chemical_formula_moiety 'C10 H8 Br4 Fe P2' _chemical_formula_sum 'C10 H8 Br4 Fe P2' _chemical_formula_weight 565.59 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' Br Br -0.2901 2.4595 '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 'P 2/n' _symmetry_space_group_name_Hall '-P 2yac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 13.647(4) _cell_length_b 8.992(2) _cell_length_c 13.668(3) _cell_angle_alpha 90.00 _cell_angle_beta 119.010(18) _cell_angle_gamma 90.00 _cell_volume 1466.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 15.38 _cell_measurement_theta_max 21.35 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 12.116 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2849 _exptl_absorpt_correction_T_max 0.3795 _exptl_absorpt_process_details 'Parkin, S., Moezzi, B. and Hope H. (1995) J. Appl. Cryst. 28, 53-56' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type Stoe _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.2 _diffrn_reflns_number 6511 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2882 _reflns_number_gt 2709 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'local software' _computing_cell_refinement 'local software' _computing_data_reduction 'local software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1965)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The non-hydrogen atoms were refined with anisotropic displacement parameters without any constraints. The H atoms of the cyclopentadienyl rings were put at the external bisector of the C-C-C angle at a C-H distance of 0.95 \%A and one common isotropic displacement parameter was refined for the H atoms of the same ring (AFIX 43 of SHELXL-97). ; _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^)+(0.0680P)^2^+4.5809P] 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 2882 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1177 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.7500 0.95335(18) 0.2500 0.0134(4) Uani 1 2 d S . . P1 P 0.6774(2) 0.8672(2) 0.4487(2) 0.0183(5) Uani 1 1 d . . . Br11 Br 0.54704(9) 1.04291(11) 0.37424(9) 0.0310(3) Uani 1 1 d . . . Br12 Br 0.76407(8) 0.94765(10) 0.62656(8) 0.0245(2) Uani 1 1 d . . . C11 C 0.7774(7) 0.9287(9) 0.4095(7) 0.0175(18) Uani 1 1 d . . . C12 C 0.8463(7) 0.8258(10) 0.3883(7) 0.0175(18) Uani 1 1 d . . . H12 H 0.8447 0.7205 0.3931 0.021(13) Uiso 1 1 calc R . . C13 C 0.9169(8) 0.9088(12) 0.3589(8) 0.024(2) Uani 1 1 d . . . H13 H 0.9699 0.8683 0.3401 0.021(13) Uiso 1 1 calc R . . C14 C 0.8950(8) 1.0609(11) 0.3625(8) 0.023(2) Uani 1 1 d . . . H14 H 0.9314 1.1405 0.3474 0.021(13) Uiso 1 1 calc R . . C15 C 0.8084(8) 1.0759(10) 0.3928(8) 0.0197(19) Uani 1 1 d . . . H15 H 0.7772 1.1666 0.4005 0.021(13) Uiso 1 1 calc R . . Fe2 Fe 0.2500 0.53529(18) 0.2500 0.0129(4) Uani 1 2 d S . . P2 P 0.44274(18) 0.4149(2) 0.1805(2) 0.0181(5) Uani 1 1 d . . . Br21 Br 0.38856(9) 0.58915(12) 0.05008(9) 0.0318(3) Uani 1 1 d . . . Br22 Br 0.62908(8) 0.46026(10) 0.26939(9) 0.0250(3) Uani 1 1 d . . . C21 C 0.4086(6) 0.4977(10) 0.2794(7) 0.0147(16) Uani 1 1 d . . . C22 C 0.3838(7) 0.4030(10) 0.3492(7) 0.0177(19) Uani 1 1 d . . . H22 H 0.3843 0.2973 0.3500 0.022(14) Uiso 1 1 calc R . . C23 C 0.3583(7) 0.4984(13) 0.4170(9) 0.023(2) Uani 1 1 d . . . H23 H 0.3396 0.4666 0.4721 0.022(14) Uiso 1 1 calc R . . C24 C 0.3655(8) 0.6493(12) 0.3889(8) 0.027(2) Uani 1 1 d . . . H24 H 0.3513 0.7347 0.4210 0.022(14) Uiso 1 1 calc R . . C25 C 0.3973(7) 0.6495(10) 0.3048(8) 0.0168(17) Uani 1 1 d . . . H25 H 0.4092 0.7350 0.2711 0.022(14) 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 0.0115(8) 0.0125(8) 0.0133(9) 0.000 0.0038(7) 0.000 P1 0.0204(11) 0.0152(10) 0.0234(12) -0.0044(9) 0.0139(10) -0.0023(9) Br11 0.0206(5) 0.0424(6) 0.0267(6) -0.0037(4) 0.0089(4) 0.0098(4) Br12 0.0278(6) 0.0281(5) 0.0183(5) 0.0018(3) 0.0116(4) 0.0054(4) C11 0.016(4) 0.014(4) 0.018(4) 0.000(3) 0.005(3) -0.006(3) C12 0.017(4) 0.023(4) 0.014(4) 0.000(3) 0.009(4) 0.000(4) C13 0.013(5) 0.032(5) 0.019(5) 0.011(4) 0.001(4) 0.002(4) C14 0.014(4) 0.032(5) 0.012(4) 0.006(4) -0.004(4) -0.010(4) C15 0.022(5) 0.009(4) 0.021(5) -0.001(3) 0.005(4) -0.005(4) Fe2 0.0060(8) 0.0125(8) 0.0182(9) 0.000 0.0043(7) 0.000 P2 0.0139(11) 0.0157(10) 0.0276(13) -0.0016(9) 0.0124(10) -0.0028(9) Br21 0.0233(5) 0.0401(5) 0.0294(6) 0.0111(4) 0.0107(4) 0.0008(4) Br22 0.0130(5) 0.0311(5) 0.0324(6) 0.0047(4) 0.0122(4) 0.0017(3) C21 0.005(3) 0.016(4) 0.021(5) 0.003(4) 0.004(3) 0.000(3) C22 0.012(4) 0.018(4) 0.017(4) 0.004(4) 0.001(4) 0.004(3) C23 0.010(4) 0.031(5) 0.029(6) 0.005(4) 0.010(4) 0.007(4) C24 0.014(4) 0.034(5) 0.026(5) -0.005(4) 0.004(4) 0.001(4) C25 0.007(4) 0.016(4) 0.024(5) 0.000(3) 0.004(3) -0.003(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 C11 2.038(9) . yes Fe1 C12 2.051(9) . yes Fe1 C13 2.067(9) . yes Fe1 C14 2.065(9) . yes Fe1 C15 2.037(9) . yes P1 C11 1.779(9) . yes P1 Br11 2.223(3) . yes P1 Br12 2.246(3) . yes C11 C15 1.441(11) . ? C11 C12 1.445(12) . ? C12 C13 1.421(13) . ? C12 H12 0.95 . ? C13 C14 1.406(14) . ? C13 H13 0.95 . ? C14 C15 1.435(14) . ? C14 H14 0.95 . ? C15 H15 0.95 . ? Fe2 C21 2.028(8) . yes Fe2 C22 2.046(8) . yes Fe2 C23 2.057(10) . yes Fe2 C24 2.058(10) . yes Fe2 C25 2.049(8) . yes P2 C21 1.792(9) . yes P2 Br21 2.213(3) . yes P2 Br22 2.261(3) . yes C21 C25 1.436(12) . ? C21 C22 1.436(13) . ? C22 C23 1.424(14) . ? C22 H22 0.95 . ? C23 C24 1.427(16) . ? C23 H23 0.95 . ? C24 C25 1.411(14) . ? C24 H24 0.95 . ? C25 H25 0.95 . ? 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 C15 114.5(5) . 2_655 ? C15 Fe1 C11 41.4(3) . . ? C15 Fe1 C11 150.2(4) . 2_655 ? C11 Fe1 C11 167.5(5) . 2_655 ? C15 Fe1 C12 164.5(4) . 2_655 ? C11 Fe1 C12 128.9(3) . 2_655 ? C15 Fe1 C12 69.0(4) . . ? C11 Fe1 C12 41.4(3) . . ? C12 Fe1 C12 112.0(5) . 2_655 ? C15 Fe1 C14 41.0(4) . . ? C11 Fe1 C14 69.0(4) . . ? C12 Fe1 C14 67.7(4) . . ? C15 Fe1 C14 104.4(4) . 2_655 ? C11 Fe1 C14 117.4(4) . 2_655 ? C12 Fe1 C14 154.5(4) . 2_655 ? C14 Fe1 C14 124.1(5) . 2_655 ? C15 Fe1 C13 125.3(4) . 2_655 ? C11 Fe1 C13 108.4(4) . 2_655 ? C12 Fe1 C13 123.0(4) . 2_655 ? C14 Fe1 C13 161.8(4) . 2_655 ? C15 Fe1 C13 68.4(4) . . ? C11 Fe1 C13 69.0(4) . . ? C12 Fe1 C13 40.4(4) . . ? C14 Fe1 C13 39.8(4) . . ? C13 Fe1 C13 157.6(6) . 2_655 ? C11 P1 Br11 101.6(3) . . yes C11 P1 Br12 98.5(3) . . yes Br11 P1 Br12 98.67(9) . . yes C15 C11 C12 106.6(8) . . yes C15 C11 P1 131.3(7) . . yes C12 C11 P1 122.0(6) . . yes C15 C11 Fe1 69.3(5) . . ? C12 C11 Fe1 69.8(5) . . ? P1 C11 Fe1 125.9(5) . . ? C13 C12 C11 108.5(8) . . ? C13 C12 Fe1 70.5(5) . . ? C11 C12 Fe1 68.8(5) . . ? C13 C12 H12 125.8 . . ? C11 C12 H12 125.8 . . ? Fe1 C12 H12 126.5 . . ? C14 C13 C12 108.5(9) . . ? C14 C13 Fe1 70.0(5) . . ? C12 C13 Fe1 69.2(5) . . ? C14 C13 H13 125.8 . . ? C12 C13 H13 125.8 . . ? Fe1 C13 H13 126.6 . . ? C13 C14 C15 108.7(8) . . ? C13 C14 Fe1 70.2(5) . . ? C15 C14 Fe1 68.5(5) . . ? C13 C14 H14 125.7 . . ? C15 C14 H14 125.7 . . ? Fe1 C14 H14 127.2 . . ? C14 C15 C11 107.8(8) . . ? C14 C15 Fe1 70.6(5) . . ? C11 C15 Fe1 69.3(5) . . ? C14 C15 H15 126.1 . . ? C11 C15 H15 126.1 . . ? Fe1 C15 H15 125.6 . . ? C21 Fe2 C21 160.8(5) . 2 ? C21 Fe2 C22 123.9(4) . 2 ? C21 Fe2 C22 41.3(4) . . ? C22 Fe2 C22 108.9(5) . 2 ? C21 Fe2 C25 41.2(3) . . ? C22 Fe2 C25 69.3(3) . . ? C21 Fe2 C25 156.8(4) . 2 ? C22 Fe2 C25 159.4(4) . 2 ? C25 Fe2 C25 119.8(5) . 2 ? C21 Fe2 C23 108.4(4) . 2 ? C22 Fe2 C23 124.9(4) . 2 ? C25 Fe2 C23 122.4(4) . 2 ? C21 Fe2 C23 68.3(4) . . ? C22 Fe2 C23 40.6(4) . . ? C25 Fe2 C23 68.0(4) . . ? C23 Fe2 C23 161.4(6) . 2 ? C21 Fe2 C24 68.5(4) . . ? C22 Fe2 C24 68.9(4) . . ? C25 Fe2 C24 40.2(4) . . ? C23 Fe2 C24 40.6(4) . . ? C21 Fe2 C24 122.1(4) . 2 ? C22 Fe2 C24 159.9(4) . 2 ? C25 Fe2 C24 105.3(4) . 2 ? C23 Fe2 C24 157.0(4) . 2 ? C24 Fe2 C24 120.2(6) . 2 ? C21 P2 Br21 101.9(3) . . yes C21 P2 Br22 99.0(3) . . yes Br21 P2 Br22 98.90(9) . . yes C25 C21 C22 108.4(8) . . yes C25 C21 P2 132.5(7) . . yes C22 C21 P2 119.1(7) . . yes C25 C21 Fe2 70.2(5) . . ? C22 C21 Fe2 70.0(5) . . ? P2 C21 Fe2 124.3(4) . . ? C23 C22 C21 106.6(9) . . ? C23 C22 Fe2 70.1(5) . . ? C21 C22 Fe2 68.7(5) . . ? C23 C22 H22 126.7 . . ? C21 C22 H22 126.7 . . ? Fe2 C22 H22 126.0 . . ? C22 C23 C24 109.1(9) . . ? C22 C23 Fe2 69.3(6) . . ? C24 C23 Fe2 69.7(6) . . ? C22 C23 H23 125.4 . . ? C24 C23 H23 125.4 . . ? Fe2 C23 H23 127.1 . . ? C25 C24 C23 108.0(9) . . ? C25 C24 Fe2 69.6(5) . . ? C23 C24 Fe2 69.7(6) . . ? C25 C24 H24 126.0 . . ? C23 C24 H24 126.0 . . ? Fe2 C24 H24 126.3 . . ? C24 C25 C21 107.9(8) . . ? C24 C25 Fe2 70.3(5) . . ? C21 C25 Fe2 68.6(4) . . ? C24 C25 H25 126.1 . . ? C21 C25 H25 126.1 . . ? Fe2 C25 H25 126.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag #C11 Fe1 C11 C15 161.2(5) 2_655 . . . ? #C11 Fe1 C11 C12 43.4(4) 2_655 . . . ? #C11 Fe1 C11 P1 -72.1(5) 2_655 . . . ? #C13 Fe1 C13 C12 -49.6(5) 2_655 . . . ? #C21 Fe2 C21 C22 -45.5(5) 2 . . . ? #C21 Fe2 C21 P2 66.8(5) 2 . . . ? #C23 Fe2 C23 C22 44.4(5) 2 . . . ? #C23 Fe2 C23 C24 165.2(6) 2 . . . ? Br11 P1 C11 C15 31.4(9) . . . . yes Br12 P1 C11 C15 -69.3(9) . . . . yes Br11 P1 C11 C12 -148.8(7) . . . . yes Br12 P1 C11 C12 110.5(7) . . . . yes Br11 P1 C11 Fe1 -61.7(6) . . . . ? Br12 P1 C11 Fe1 -162.4(5) . . . . ? C15 Fe1 C11 C15 -44.3(12) 2_655 . . . ? C12 Fe1 C11 C15 -163.1(5) 2_655 . . . ? C12 Fe1 C11 C15 117.7(7) . . . . ? C14 Fe1 C11 C15 38.0(6) . . . . ? C14 Fe1 C11 C15 -80.6(6) 2_655 . . . ? C13 Fe1 C11 C15 -122.8(6) 2_655 . . . ? C13 Fe1 C11 C15 80.8(6) . . . . ? C15 Fe1 C11 C12 -117.7(7) . . . . ? C15 Fe1 C11 C12 -162.0(7) 2_655 . . . ? C12 Fe1 C11 C12 79.2(8) 2_655 . . . ? C14 Fe1 C11 C12 -79.7(6) . . . . ? C14 Fe1 C11 C12 161.7(5) 2_655 . . . ? C13 Fe1 C11 C12 119.4(5) 2_655 . . . ? C13 Fe1 C11 C12 -37.0(5) . . . . ? C15 Fe1 C11 P1 126.7(9) . . . . ? C15 Fe1 C11 P1 82.4(9) 2_655 . . . ? C12 Fe1 C11 P1 -36.4(8) 2_655 . . . ? C12 Fe1 C11 P1 -115.5(8) . . . . ? C14 Fe1 C11 P1 164.7(7) . . . . ? C14 Fe1 C11 P1 46.2(7) 2_655 . . . ? C13 Fe1 C11 P1 3.9(7) 2_655 . . . ? C13 Fe1 C11 P1 -152.5(7) . . . . ? C15 C11 C12 C13 -0.3(10) . . . . ? P1 C11 C12 C13 179.9(7) . . . . yes Fe1 C11 C12 C13 59.5(6) . . . . ? C15 C11 C12 Fe1 -59.8(6) . . . . ? P1 C11 C12 Fe1 120.4(6) . . . . ? C15 Fe1 C12 C13 -81.0(6) . . . . ? C15 Fe1 C12 C13 25.1(16) 2_655 . . . ? C11 Fe1 C12 C13 -119.9(8) . . . . ? C11 Fe1 C12 C13 71.2(7) 2_655 . . . ? C12 Fe1 C12 C13 115.6(6) 2_655 . . . ? C14 Fe1 C12 C13 -36.8(6) . . . . ? C14 Fe1 C12 C13 -160.2(9) 2_655 . . . ? C13 Fe1 C12 C13 159.8(6) 2_655 . . . ? C15 Fe1 C12 C11 38.9(5) . . . . ? C15 Fe1 C12 C11 145.0(13) 2_655 . . . ? C11 Fe1 C12 C11 -169.0(4) 2_655 . . . ? C12 Fe1 C12 C11 -124.5(5) 2_655 . . . ? C14 Fe1 C12 C11 83.0(6) . . . . ? C14 Fe1 C12 C11 -40.4(10) 2_655 . . . ? C13 Fe1 C12 C11 -80.4(6) 2_655 . . . ? C13 Fe1 C12 C11 119.9(8) . . . . ? C11 C12 C13 C14 0.7(10) . . . . ? Fe1 C12 C13 C14 59.2(6) . . . . ? C11 C12 C13 Fe1 -58.5(6) . . . . ? C15 Fe1 C13 C14 -37.4(6) . . . . ? C15 Fe1 C13 C14 68.1(8) 2_655 . . . ? C11 Fe1 C13 C14 -82.0(6) . . . . ? C11 Fe1 C13 C14 111.0(6) 2_655 . . . ? C12 Fe1 C13 C14 154.4(6) 2_655 . . . ? C12 Fe1 C13 C14 -119.9(9) . . . . ? C14 Fe1 C13 C14 32.3(19) 2_655 . . . ? C13 Fe1 C13 C14 -169.5(6) 2_655 . . . ? C15 Fe1 C13 C12 82.5(6) . . . . ? C15 Fe1 C13 C12 -172.0(5) 2_655 . . . ? C11 Fe1 C13 C12 37.9(5) . . . . ? C11 Fe1 C13 C12 -129.1(6) 2_655 . . . ? C12 Fe1 C13 C12 -85.7(8) 2_655 . . . ? C14 Fe1 C13 C12 119.9(9) . . . . ? C14 Fe1 C13 C12 152.2(12) 2_655 . . . ? C12 C13 C14 C15 -0.8(10) . . . . ? Fe1 C13 C14 C15 57.8(6) . . . . ? C12 C13 C14 Fe1 -58.7(6) . . . . ? C15 Fe1 C14 C13 120.5(8) . . . . ? C15 Fe1 C14 C13 -128.6(6) 2_655 . . . ? C11 Fe1 C14 C13 82.0(6) . . . . ? C11 Fe1 C14 C13 -86.2(6) 2_655 . . . ? C12 Fe1 C14 C13 -57.3(10) 2_655 . . . ? C12 Fe1 C14 C13 37.3(6) . . . . ? C14 Fe1 C14 C13 -168.4(7) 2_655 . . . ? C13 Fe1 C14 C13 167.2(9) 2_655 . . . ? C15 Fe1 C14 C15 111.0(7) 2_655 . . . ? C11 Fe1 C14 C15 -38.4(5) . . . . ? C11 Fe1 C14 C15 153.3(5) 2_655 . . . ? C12 Fe1 C14 C15 -177.8(7) 2_655 . . . ? C12 Fe1 C14 C15 -83.1(6) . . . . ? C14 Fe1 C14 C15 71.1(5) 2_655 . . . ? C13 Fe1 C14 C15 46.8(15) 2_655 . . . ? C13 Fe1 C14 C15 -120.5(8) . . . . ? C13 C14 C15 C11 0.7(10) . . . . ? Fe1 C14 C15 C11 59.5(6) . . . . ? C13 C14 C15 Fe1 -58.9(6) . . . . ? C12 C11 C15 C14 -0.2(10) . . . . ? P1 C11 C15 C14 179.5(7) . . . . ? Fe1 C11 C15 C14 -60.3(6) . . . . ? C12 C11 C15 Fe1 60.1(6) . . . . ? P1 C11 C15 Fe1 -120.1(8) . . . . ? C15 Fe1 C15 C14 -83.8(5) 2_655 . . . ? C11 Fe1 C15 C14 118.7(8) . . . . ? C11 Fe1 C15 C14 -53.2(10) 2_655 . . . ? C12 Fe1 C15 C14 176.5(12) 2_655 . . . ? C12 Fe1 C15 C14 79.8(6) . . . . ? C14 Fe1 C15 C14 -126.0(7) 2_655 . . . ? C13 Fe1 C15 C14 -163.8(6) 2_655 . . . ? C13 Fe1 C15 C14 36.4(5) . . . . ? C15 Fe1 C15 C11 157.6(6) 2_655 . . . ? C11 Fe1 C15 C11 -171.9(4) 2_655 . . . ? C12 Fe1 C15 C11 57.8(15) 2_655 . . . ? C12 Fe1 C15 C11 -38.8(5) . . . . ? C14 Fe1 C15 C11 -118.7(8) . . . . ? C14 Fe1 C15 C11 115.3(6) 2_655 . . . ? C13 Fe1 C15 C11 77.5(7) 2_655 . . . ? C13 Fe1 C15 C11 -82.3(6) . . . . ? Br21 P2 C21 C25 -25.7(8) . . . . yes Br22 P2 C21 C25 75.5(8) . . . . yes Br21 P2 C21 C22 152.8(6) . . . . yes Br22 P2 C21 C22 -106.1(6) . . . . yes Br21 P2 C21 Fe2 68.1(5) . . . . ? Br22 P2 C21 Fe2 169.3(5) . . . . ? C21 Fe2 C21 C25 -164.7(5) 2 . . . ? C22 Fe2 C21 C25 160.8(5) 2 . . . ? C22 Fe2 C21 C25 -119.2(8) . . . . ? C25 Fe2 C21 C25 41.5(13) 2 . . . ? C23 Fe2 C21 C25 118.5(6) 2 . . . ? C23 Fe2 C21 C25 -80.9(6) . . . . ? C24 Fe2 C21 C25 -37.2(6) . . . . ? C24 Fe2 C21 C25 75.9(6) 2 . . . ? C22 Fe2 C21 C22 -80.0(8) 2 . . . ? C25 Fe2 C21 C22 119.2(8) . . . . ? C25 Fe2 C21 C22 160.7(8) 2 . . . ? C23 Fe2 C21 C22 -122.2(6) 2 . . . ? C23 Fe2 C21 C22 38.3(6) . . . . ? C24 Fe2 C21 C22 82.1(6) . . . . ? C24 Fe2 C21 C22 -164.8(6) 2 . . . ? C22 Fe2 C21 P2 32.3(7) 2 . . . ? C22 Fe2 C21 P2 112.2(8) . . . . ? C25 Fe2 C21 P2 -128.5(8) . . . . ? C25 Fe2 C21 P2 -87.0(11) 2 . . . ? C23 Fe2 C21 P2 -10.0(7) 2 . . . ? C23 Fe2 C21 P2 150.5(7) . . . . ? C24 Fe2 C21 P2 -165.7(7) . . . . ? C24 Fe2 C21 P2 -52.6(7) 2 . . . ? C25 C21 C22 C23 -0.3(9) . . . . ? P2 C21 C22 C23 -179.1(6) . . . . yes Fe2 C21 C22 C23 -60.2(6) . . . . ? C25 C21 C22 Fe2 59.9(5) . . . . ? P2 C21 C22 Fe2 -118.9(6) . . . . ? C21 Fe2 C22 C23 -78.6(7) 2 . . . ? C21 Fe2 C22 C23 117.8(8) . . . . ? C22 Fe2 C22 C23 -121.9(6) 2 . . . ? C25 Fe2 C22 C23 79.9(6) . . . . ? C25 Fe2 C22 C23 -40.6(13) 2 . . . ? C23 Fe2 C22 C23 -164.3(6) 2 . . . ? C24 Fe2 C22 C23 36.7(6) . . . . ? C24 Fe2 C22 C23 157.9(11) 2 . . . ? C21 Fe2 C22 C21 163.6(5) 2 . . . ? C22 Fe2 C22 C21 120.2(6) 2 . . . ? C25 Fe2 C22 C21 -37.9(5) . . . . ? C25 Fe2 C22 C21 -158.4(9) 2 . . . ? C23 Fe2 C22 C21 77.9(7) 2 . . . ? C23 Fe2 C22 C21 -117.8(8) . . . . ? C24 Fe2 C22 C21 -81.1(6) . . . . ? C24 Fe2 C22 C21 40.1(14) 2 . . . ? C21 C22 C23 C24 0.8(9) . . . . ? Fe2 C22 C23 C24 -58.5(6) . . . . ? C21 C22 C23 Fe2 59.3(6) . . . . ? C21 Fe2 C23 C22 120.9(6) 2 . . . ? C21 Fe2 C23 C22 -38.9(6) . . . . ? C22 Fe2 C23 C22 78.1(8) 2 . . . ? C25 Fe2 C23 C22 -83.5(6) . . . . ? C25 Fe2 C23 C22 164.3(5) 2 . . . ? C24 Fe2 C23 C22 -120.9(8) . . . . ? C24 Fe2 C23 C22 -160.7(9) 2 . . . ? C21 Fe2 C23 C24 -118.2(6) 2 . . . ? C21 Fe2 C23 C24 81.9(6) . . . . ? C22 Fe2 C23 C24 -161.0(5) 2 . . . ? C22 Fe2 C23 C24 120.9(8) . . . . ? C25 Fe2 C23 C24 37.4(6) . . . . ? C25 Fe2 C23 C24 -74.9(6) 2 . . . ? C24 Fe2 C23 C24 -39.8(14) 2 . . . ? C22 C23 C24 C25 -1.0(10) . . . . ? Fe2 C23 C24 C25 -59.2(6) . . . . ? C22 C23 C24 Fe2 58.2(6) . . . . ? C21 Fe2 C24 C25 -159.8(5) 2 . . . ? C21 Fe2 C24 C25 38.1(5) . . . . ? C22 Fe2 C24 C25 170.1(10) 2 . . . ? C22 Fe2 C24 C25 82.5(6) . . . . ? C25 Fe2 C24 C25 -118.3(6) 2 . . . ? C23 Fe2 C24 C25 -48.7(12) 2 . . . ? C23 Fe2 C24 C25 119.3(8) . . . . ? C24 Fe2 C24 C25 -77.5(5) 2 . . . ? C21 Fe2 C24 C23 80.8(7) 2 . . . ? C21 Fe2 C24 C23 -81.2(6) . . . . ? C22 Fe2 C24 C23 50.7(14) 2 . . . ? C22 Fe2 C24 C23 -36.8(6) . . . . ? C25 Fe2 C24 C23 -119.3(8) . . . . ? C25 Fe2 C24 C23 122.4(6) 2 . . . ? C23 Fe2 C24 C23 -168.0(6) 2 . . . ? C24 Fe2 C24 C23 163.1(6) 2 . . . ? C23 C24 C25 C21 0.8(10) . . . . ? Fe2 C24 C25 C21 -58.5(6) . . . . ? C23 C24 C25 Fe2 59.3(6) . . . . ? C22 C21 C25 C24 -0.3(10) . . . . ? P2 C21 C25 C24 178.2(7) . . . . ? Fe2 C21 C25 C24 59.5(6) . . . . ? C22 C21 C25 Fe2 -59.8(5) . . . . ? P2 C21 C25 Fe2 118.7(7) . . . . ? C21 Fe2 C25 C24 47.9(12) 2 . . . ? C21 Fe2 C25 C24 -119.4(8) . . . . ? C22 Fe2 C25 C24 -170.3(10) 2 . . . ? C22 Fe2 C25 C24 -81.4(6) . . . . ? C25 Fe2 C25 C24 78.1(6) 2 . . . ? C23 Fe2 C25 C24 159.6(6) 2 . . . ? C23 Fe2 C25 C24 -37.7(6) . . . . ? C24 Fe2 C25 C24 119.0(7) 2 . . . ? C21 Fe2 C25 C21 167.3(6) 2 . . . ? C22 Fe2 C25 C21 -50.9(12) 2 . . . ? C22 Fe2 C25 C21 38.0(5) . . . . ? C25 Fe2 C25 C21 -162.5(6) 2 . . . ? C23 Fe2 C25 C21 -81.0(6) 2 . . . ? C23 Fe2 C25 C21 81.7(6) . . . . ? C24 Fe2 C25 C21 119.4(8) . . . . ? C24 Fe2 C25 C21 -121.6(6) 2 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.511 _refine_diff_density_min -1.483 _refine_diff_density_rms 0.217