 
data_s92 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C23 H29 Br2 Fe2 P' 
_chemical_formula_weight          607.95 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
 
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' 
 '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' 
 
_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                    7.6828(10) 
_cell_length_b                    9.4950(14) 
_cell_length_c                    14.6420(13) 
_cell_angle_alpha                 99.180(9) 
_cell_angle_beta                  93.392(5) 
_cell_angle_gamma                 90.311(9) 
_cell_volume                      1052.5(2) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.18 
_exptl_crystal_size_mid           0.11 
_exptl_crystal_size_min           0.11
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.918 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              608 
_exptl_absorpt_coefficient_mu     5.259 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71069 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        ? 
_diffrn_measurement_method        ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             4038 
_diffrn_reflns_av_R_equivalents   0.0807 
_diffrn_reflns_av_sigmaI/netI     0.0729 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -8 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          2.17 
_diffrn_reflns_theta_max          25.06 
_reflns_number_total              2900 
_reflns_number_observed           2349 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-92 (Sheldrick, 1993)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement on F² for ALL reflections except for 4 with very negative F² 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses of fit S are based on F², conventional R-factors R 
 are based on F, with F set to zero for negative F². The observed criterion 
 of F² > 2sigma(F²) is used only for calculating _R_factor_obs etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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^)+(0.1333P)^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     ? 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          2896 
_refine_ls_number_parameters      249 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0799 
_refine_ls_R_factor_obs           0.0687 
_refine_ls_wR_factor_all          0.1962 
_refine_ls_wR_factor_obs          0.1805 
_refine_ls_goodness_of_fit_all    1.043 
_refine_ls_goodness_of_fit_obs    1.131 
_refine_ls_restrained_S_all       1.098 
_refine_ls_restrained_S_obs       1.131 
_refine_ls_shift/esd_max          0.004 
_refine_ls_shift/esd_mean         0.001 
 
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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Fe1 Fe 0.67855(15) -0.21819(12) -0.26532(8) 0.0170(4) Uani 1 d . . 
Fe2 Fe 0.27063(14) 0.29834(12) -0.30467(8) 0.0158(4) Uani 1 d . . 
Br1 Br 0.17202(12) 0.34163(10) 0.05923(7) 0.0328(3) Uani 1 d . . 
Br2 Br -0.11639(12) 0.24474(11) -0.44666(7) 0.0385(4) Uani 1 d . . 
P1 P 0.6150(3) 0.1542(2) -0.18595(14) 0.0153(5) Uani 1 d . . 
C1 C 0.7924(11) -0.4120(9) -0.2614(6) 0.022(2) Uani 1 d . . 
H1 H 0.7363(11) -0.4987(9) -0.2604(6) 0.027 Uiso 1 calc R . 
C2 C 0.8390(12) -0.3548(10) -0.3403(7) 0.031(2) Uani 1 d . . 
H2 H 0.8167(12) -0.3973(10) -0.4017(7) 0.037 Uiso 1 calc R . 
C3 C 0.9247(11) -0.2227(10) -0.3101(7) 0.031(2) Uani 1 d . . 
H3 H 0.9688(11) -0.1632(10) -0.3482(7) 0.037 Uiso 1 calc R . 
C4 C 0.9324(11) -0.1960(9) -0.2131(6) 0.024(2) Uani 1 d . . 
H4 H 0.9838(11) -0.1171(9) -0.1751(6) 0.029 Uiso 1 calc R . 
C5 C 0.8490(11) -0.3096(9) -0.1848(6) 0.021(2) Uani 1 d . . 
H5 H 0.8325(11) -0.3173(9) -0.1234(6) 0.025 Uiso 1 calc R . 
C6 C 0.4710(10) -0.1364(9) -0.1932(6) 0.018(2) Uani 1 d . . 
H6 H 0.4594(10) -0.1324(9) -0.1299(6) 0.021 Uiso 1 calc R . 
C7 C 0.4161(11) -0.2518(9) -0.2633(6) 0.022(2) Uani 1 d . . 
H7 H 0.3622(11) -0.3359(9) -0.2541(6) 0.027 Uiso 1 calc R . 
C8 C 0.4580(11) -0.2158(9) -0.3495(6) 0.0209(14) Uani 1 d . . 
H8 H 0.4355(11) -0.2715(9) -0.4073(6) 0.025 Uiso 1 calc R . 
C9 C 0.5407(11) -0.0794(9) -0.3319(6) 0.0209(14) Uani 1 d . . 
H9 H 0.5841(11) -0.0316(9) -0.3766(6) 0.025 Uiso 1 calc R . 
C10 C 0.5468(10) -0.0275(8) -0.2358(6) 0.016(2) Uani 1 d . . 
C11 C 0.6329(11) 0.1516(9) -0.0591(6) 0.018(2) Uani 1 d . . 
H11 H 0.5244(11) 0.1119(9) -0.0411(6) 0.021 Uiso 1 calc R . 
C12 C 0.6573(12) 0.3048(9) -0.0079(6) 0.025(2) Uani 1 d . . 
H12A H 0.5541(31) 0.3580(19) -0.0182(33) 0.038 Uiso 1 calc R . 
H12B H 0.7552(48) 0.3488(22) -0.0306(29) 0.038 Uiso 1 calc R . 
H12C H 0.6779(76) 0.3036(10) 0.0573(8) 0.038 Uiso 1 calc R . 
C13 C 0.7842(11) 0.0607(9) -0.0320(6) 0.023(2) Uani 1 d . . 
H13A H 0.7726(39) -0.0332(19) -0.0678(26) 0.035 Uiso 1 calc R . 
H13B H 0.7831(41) 0.0543(46) 0.0327(10) 0.035 Uiso 1 calc R . 
H13C H 0.8922(12) 0.1036(31) -0.0440(34) 0.035 Uiso 1 calc R . 
C14 C 0.4023(10) 0.2368(8) -0.1918(5) 0.016(2) Uani 1 d . . 
C15 C 0.3726(11) 0.3876(9) -0.1774(6) 0.020(2) Uani 1 d . . 
H15 H 0.4595(11) 0.4578(9) -0.1655(6) 0.024 Uiso 1 calc R . 
C16 C 0.1938(12) 0.4131(9) -0.1838(6) 0.023(2) Uani 1 d . . 
H16 H 0.1425(12) 0.5024(9) -0.1766(6) 0.028 Uiso 1 calc R . 
C17 C 0.1037(11) 0.2801(10) -0.2032(6) 0.023(2) Uani 1 d . . 
H17 H -0.0166(11) 0.2665(10) -0.2113(6) 0.028 Uiso 1 calc R . 
C18 C 0.2308(10) 0.1708(10) -0.2079(5) 0.019(2) Uani 1 d . . 
H18 H 0.2073(10) 0.0731(10) -0.2195(5) 0.022 Uiso 1 calc R . 
C19 C 0.2076(11) 0.4146(9) -0.4077(5) 0.018(2) Uani 1 d . . 
H19 H 0.1526(11) 0.5023(9) -0.4014(5) 0.022 Uiso 1 calc R . 
C20 C 0.3910(11) 0.3903(10) -0.4014(6) 0.025(2) Uani 1 d . . 
H20 H 0.4785(11) 0.4599(10) -0.3893(6) 0.030 Uiso 1 calc R . 
C21 C 0.4154(11) 0.2411(9) -0.4169(6) 0.020(2) Uani 1 d . . 
H21 H 0.5224(11) 0.1958(9) -0.4170(6) 0.024 Uiso 1 calc R . 
C22 C 0.2534(12) 0.1732(10) -0.4321(6) 0.024(2) Uani 1 d . . 
H22 H 0.2331(12) 0.0751(10) -0.4444(6) 0.028 Uiso 1 calc R . 
C23 C 0.1267(11) 0.2777(10) -0.4255(6) 0.022(2) Uani 1 d . . 
 
 
_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 2.003(8) . ? 
Fe1 C9 2.028(8) . ? 
Fe1 C2 2.032(9) . ? 
Fe1 C8 2.038(8) . ? 
Fe1 C3 2.036(9) . ? 
Fe1 C7 2.043(8) . ? 
Fe1 C4 2.050(9) . ? 
Fe1 C1 2.049(8) . ? 
Fe1 C6 2.053(8) . ? 
Fe1 C10 2.076(8) . ? 
Fe2 C23 2.011(8) . ? 
Fe2 C15 2.030(8) . ? 
Fe2 C19 2.044(8) . ? 
Fe2 C18 2.040(8) . ? 
Fe2 C22 2.042(8) . ? 
Fe2 C21 2.043(8) . ? 
Fe2 C16 2.045(8) . ? 
Fe2 C20 2.041(8) . ? 
Fe2 C17 2.047(8) . ? 
Fe2 C14 2.053(8) . ? 
Br1 C5 1.927(9) 2_655 ? 
Br2 C23 1.891(8) . ? 
P1 C14 1.820(8) . ? 
P1 C10 1.824(8) . ? 
P1 C11 1.859(8) . ? 
C1 C5 1.408(12) . ? 
C1 C2 1.415(13) . ? 
C2 C3 1.408(13) . ? 
C3 C4 1.400(13) . ? 
C4 C5 1.383(12) . ? 
C5 Br1 1.927(9) 2_655 ? 
C6 C7 1.420(12) . ? 
C6 C10 1.428(12) . ? 
C7 C8 1.414(13) . ? 
C8 C9 1.419(12) . ? 
C9 C10 1.414(12) . ? 
C11 C13 1.523(12) . ? 
C11 C12 1.531(12) . ? 
C14 C15 1.435(12) . ? 
C14 C18 1.446(11) . ? 
C15 C16 1.396(12) . ? 
C16 C17 1.417(12) . ? 
C17 C18 1.425(12) . ? 
C19 C23 1.417(12) . ? 
C19 C20 1.429(12) . ? 
C20 C21 1.414(12) . ? 
C21 C22 1.388(12) . ? 
C22 C23 1.390(13) . ? 
 
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 C9 165.2(3) . . ? 
C5 Fe1 C2 67.6(4) . . ? 
C9 Fe1 C2 117.9(4) . . ? 
C5 Fe1 C8 153.7(3) . . ? 
C9 Fe1 C8 40.9(3) . . ? 
C2 Fe1 C8 104.6(4) . . ? 
C5 Fe1 C3 67.1(4) . . ? 
C9 Fe1 C3 107.4(4) . . ? 
C2 Fe1 C3 40.5(4) . . ? 
C8 Fe1 C3 124.2(4) . . ? 
C5 Fe1 C7 121.4(4) . . ? 
C9 Fe1 C7 68.3(4) . . ? 
C2 Fe1 C7 123.6(4) . . ? 
C8 Fe1 C7 40.5(4) . . ? 
C3 Fe1 C7 160.9(4) . . ? 
C5 Fe1 C4 39.9(4) . . ? 
C9 Fe1 C4 127.2(3) . . ? 
C2 Fe1 C4 67.9(4) . . ? 
C8 Fe1 C4 162.5(4) . . ? 
C3 Fe1 C4 40.1(4) . . ? 
C7 Fe1 C4 156.8(4) . . ? 
C5 Fe1 C1 40.6(3) . . ? 
C9 Fe1 C1 152.0(3) . . ? 
C2 Fe1 C1 40.6(4) . . ? 
C8 Fe1 C1 117.1(3) . . ? 
C3 Fe1 C1 68.2(4) . . ? 
C7 Fe1 C1 106.3(3) . . ? 
C4 Fe1 C1 68.3(3) . . ? 
C5 Fe1 C6 111.4(3) . . ? 
C9 Fe1 C6 67.8(3) . . ? 
C2 Fe1 C6 162.3(4) . . ? 
C8 Fe1 C6 68.1(3) . . ? 
C3 Fe1 C6 156.8(4) . . ? 
C7 Fe1 C6 40.6(3) . . ? 
C4 Fe1 C6 123.6(3) . . ? 
C1 Fe1 C6 127.0(3) . . ? 
C5 Fe1 C10 129.5(3) . . ? 
C9 Fe1 C10 40.3(3) . . ? 
C2 Fe1 C10 153.7(4) . . ? 
C8 Fe1 C10 68.3(3) . . ? 
C3 Fe1 C10 121.2(3) . . ? 
C7 Fe1 C10 68.4(3) . . ? 
C4 Fe1 C10 110.9(3) . . ? 
C1 Fe1 C10 165.5(3) . . ? 
C6 Fe1 C10 40.5(3) . . ? 
C23 Fe2 C15 159.4(4) . . ? 
C23 Fe2 C19 40.9(3) . . ? 
C15 Fe2 C19 123.0(3) . . ? 
C23 Fe2 C18 122.0(3) . . ? 
C15 Fe2 C18 68.5(3) . . ? 
C19 Fe2 C18 157.6(3) . . ? 
C23 Fe2 C22 40.1(4) . . ? 
C15 Fe2 C22 159.2(4) . . ? 
C19 Fe2 C22 68.3(4) . . ? 
C18 Fe2 C22 107.9(4) . . ? 
C23 Fe2 C21 67.3(3) . . ? 
C15 Fe2 C21 124.0(3) . . ? 
C19 Fe2 C21 68.3(3) . . ? 
C18 Fe2 C21 123.9(3) . . ? 
C22 Fe2 C21 39.7(3) . . ? 
C23 Fe2 C16 123.5(4) . . ? 
C15 Fe2 C16 40.1(3) . . ? 
C19 Fe2 C16 107.0(3) . . ? 
C18 Fe2 C16 68.3(3) . . ? 
C22 Fe2 C16 159.5(4) . . ? 
C21 Fe2 C16 159.0(3) . . ? 
C23 Fe2 C20 68.2(3) . . ? 
C15 Fe2 C20 108.1(4) . . ? 
C19 Fe2 C20 41.0(3) . . ? 
C18 Fe2 C20 160.0(4) . . ? 
C22 Fe2 C20 67.9(3) . . ? 
C21 Fe2 C20 40.5(3) . . ? 
C16 Fe2 C20 122.6(3) . . ? 
C23 Fe2 C17 107.2(3) . . ? 
C15 Fe2 C17 68.1(4) . . ? 
C19 Fe2 C17 121.4(4) . . ? 
C18 Fe2 C17 40.8(3) . . ? 
C22 Fe2 C17 123.5(3) . . ? 
C21 Fe2 C17 159.5(3) . . ? 
C16 Fe2 C17 40.5(3) . . ? 
C20 Fe2 C17 157.9(4) . . ? 
C23 Fe2 C14 158.1(3) . . ? 
C15 Fe2 C14 41.1(3) . . ? 
C19 Fe2 C14 159.5(3) . . ? 
C18 Fe2 C14 41.4(3) . . ? 
C22 Fe2 C14 122.5(3) . . ? 
C21 Fe2 C14 107.9(3) . . ? 
C16 Fe2 C14 68.9(3) . . ? 
C20 Fe2 C14 123.1(3) . . ? 
C17 Fe2 C14 69.4(3) . . ? 
C14 P1 C10 97.9(4) . . ? 
C14 P1 C11 97.7(4) . . ? 
C10 P1 C11 103.8(4) . . ? 
C5 C1 C2 105.3(8) . . ? 
C5 C1 Fe1 67.9(5) . . ? 
C2 C1 Fe1 69.1(5) . . ? 
C3 C2 C1 108.4(8) . . ? 
C3 C2 Fe1 69.9(5) . . ? 
C1 C2 Fe1 70.4(5) . . ? 
C4 C3 C2 108.5(8) . . ? 
C4 C3 Fe1 70.5(5) . . ? 
C2 C3 Fe1 69.6(5) . . ? 
C5 C4 C3 106.8(8) . . ? 
C5 C4 Fe1 68.3(5) . . ? 
C3 C4 Fe1 69.5(5) . . ? 
C4 C5 C1 110.9(8) . . ? 
C4 C5 Br1 127.0(7) . 2_655 ? 
C1 C5 Br1 121.8(7) . 2_655 ? 
C4 C5 Fe1 71.9(5) . . ? 
C1 C5 Fe1 71.4(5) . . ? 
Br1 C5 Fe1 128.5(4) 2_655 . ? 
C7 C6 C10 108.8(8) . . ? 
C7 C6 Fe1 69.3(5) . . ? 
C10 C6 Fe1 70.7(4) . . ? 
C6 C7 C8 107.8(8) . . ? 
C6 C7 Fe1 70.1(5) . . ? 
C8 C7 Fe1 69.6(5) . . ? 
C9 C8 C7 107.6(7) . . ? 
C9 C8 Fe1 69.2(5) . . ? 
C7 C8 Fe1 69.9(5) . . ? 
C8 C9 C10 109.3(8) . . ? 
C8 C9 Fe1 70.0(5) . . ? 
C10 C9 Fe1 71.7(5) . . ? 
C9 C10 C6 106.5(7) . . ? 
C9 C10 P1 123.1(6) . . ? 
C6 C10 P1 129.9(6) . . ? 
C9 C10 Fe1 68.0(4) . . ? 
C6 C10 Fe1 68.9(4) . . ? 
P1 C10 Fe1 133.7(4) . . ? 
C13 C11 C12 109.9(7) . . ? 
C13 C11 P1 111.6(6) . . ? 
C12 C11 P1 109.0(6) . . ? 
C15 C14 C18 105.3(7) . . ? 
C15 C14 P1 125.2(6) . . ? 
C18 C14 P1 129.5(6) . . ? 
C15 C14 Fe2 68.6(5) . . ? 
C18 C14 Fe2 68.8(5) . . ? 
P1 C14 Fe2 128.2(4) . . ? 
C16 C15 C14 109.9(7) . . ? 
C16 C15 Fe2 70.5(5) . . ? 
C14 C15 Fe2 70.3(4) . . ? 
C15 C16 C17 108.5(7) . . ? 
C15 C16 Fe2 69.4(5) . . ? 
C17 C16 Fe2 69.8(5) . . ? 
C18 C17 C16 107.6(7) . . ? 
C18 C17 Fe2 69.3(5) . . ? 
C16 C17 Fe2 69.7(5) . . ? 
C17 C18 C14 108.7(8) . . ? 
C17 C18 Fe2 69.8(5) . . ? 
C14 C18 Fe2 69.8(4) . . ? 
C23 C19 C20 105.9(7) . . ? 
C23 C19 Fe2 68.3(5) . . ? 
C20 C19 Fe2 69.4(5) . . ? 
C21 C20 C19 107.6(7) . . ? 
C21 C20 Fe2 69.8(5) . . ? 
C19 C20 Fe2 69.7(5) . . ? 
C22 C21 C20 108.8(8) . . ? 
C22 C21 Fe2 70.1(5) . . ? 
C20 C21 Fe2 69.7(5) . . ? 
C23 C22 C21 107.9(8) . . ? 
C23 C22 Fe2 68.8(5) . . ? 
C21 C22 Fe2 70.1(5) . . ? 
C22 C23 C19 109.7(7) . . ? 
C22 C23 Br2 125.6(7) . . ? 
C19 C23 Br2 124.5(6) . . ? 
C22 C23 Fe2 71.1(5) . . ? 
C19 C23 Fe2 70.8(5) . . ? 
Br2 C23 Fe2 128.3(4) . . ? 
 
_refine_diff_density_max    2.242 
_refine_diff_density_min   -1.038 
_refine_diff_density_rms    0.266 
