 
data_s92 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C24 H18 Fe' 
_chemical_formula_weight          362.23 
_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' 
 'Fe'  'Fe'   0.3463   0.8444 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Orthorhombic 
_symmetry_space_group_name_H-M    Pbca 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 '-x, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, -z' 
 '-x, -y, -z' 
 'x-1/2, y, -z-1/2' 
 'x, -y-1/2, z-1/2' 
 '-x-1/2, y-1/2, z' 
 
_cell_length_a                    10.7966(8) 
_cell_length_b                    17.6155(6) 
_cell_length_c                    17.888(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      3402.1(9) 
_cell_formula_units_Z             8 
_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           0.14 
_exptl_crystal_size_mid           0.07 
_exptl_crystal_size_min           0.02 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.414 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1504 
_exptl_absorpt_coefficient_mu     0.888 
_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             12511 
_diffrn_reflns_av_R_equivalents   0.0965 
_diffrn_reflns_av_sigmaI/netI     0.2053 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -19 
_diffrn_reflns_limit_k_max        19 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          2.28 
_diffrn_reflns_theta_max          24.98 
_reflns_number_total              2675 
_reflns_number_observed           1090 
_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 7 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^)+(0.0000P)^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          2668 
_refine_ls_number_parameters      226 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1210 
_refine_ls_R_factor_obs           0.0330 
_refine_ls_wR_factor_all          0.0662 
_refine_ls_wR_factor_obs          0.0501 
_refine_ls_goodness_of_fit_all    0.562 
_refine_ls_goodness_of_fit_obs    0.781 
_refine_ls_restrained_S_all       0.639 
_refine_ls_restrained_S_obs       0.781 
_refine_ls_shift/esd_max          -0.001 
_refine_ls_shift/esd_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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Fe1 Fe 0.52550(4) 0.13377(3) 0.58754(3) 0.0356(2) Uani 1 d . . 
C1 C 0.7035(3) 0.1035(3) 0.5644(3) 0.054(2) Uani 1 d . . 
H1 H 0.7312(3) 0.0808(3) 0.5205(3) 0.065 Uiso 1 calc R . 
C2 C 0.6621(3) 0.0654(3) 0.6279(3) 0.0568(14) Uani 1 d . . 
H2 H 0.6574(3) 0.0131(3) 0.6339(3) 0.068 Uiso 1 calc R . 
C3 C 0.6287(3) 0.1206(3) 0.6817(2) 0.0528(13) Uani 1 d . . 
H3 H 0.5980(3) 0.1107(3) 0.7293(2) 0.063 Uiso 1 calc R . 
C4 C 0.6498(3) 0.1925(3) 0.6510(3) 0.0482(13) Uani 1 d . . 
H4 H 0.6359(3) 0.2389(3) 0.6744(3) 0.058 Uiso 1 calc R . 
C5 C 0.6962(3) 0.1814(3) 0.5776(3) 0.0499(13) Uani 1 d . . 
H5 H 0.7181(3) 0.2195(3) 0.5441(3) 0.060 Uiso 1 calc R . 
C6 C 0.3448(3) 0.1225(3) 0.6165(2) 0.0413(12) Uani 1 d . . 
H6 H 0.3161(3) 0.1154(3) 0.6650(2) 0.050 Uiso 1 calc R . 
C7 C 0.3805(3) 0.0645(3) 0.5675(3) 0.0497(13) Uani 1 d . . 
H7 H 0.3785(3) 0.0128(3) 0.5777(3) 0.060 Uiso 1 calc R . 
C8 C 0.4197(3) 0.0978(3) 0.5008(3) 0.0446(12) Uani 1 d . . 
H8 H 0.4486(3) 0.0722(3) 0.4588(3) 0.053 Uiso 1 calc R . 
C9 C 0.4077(3) 0.1767(3) 0.5081(2) 0.0374(11) Uani 1 d . . 
H9 H 0.4281(3) 0.2123(3) 0.4717(2) 0.045 Uiso 1 calc R . 
C10 C 0.3592(3) 0.1938(2) 0.5806(2) 0.0283(10) Uani 1 d . . 
C11 C 0.3134(3) 0.2682(2) 0.6094(2) 0.0308(11) Uani 1 d . . 
C12 C 0.1917(3) 0.2705(2) 0.6394(2) 0.0289(10) Uani 1 d . . 
C13 C 0.1055(3) 0.2089(2) 0.6328(2) 0.0370(11) Uani 1 d . . 
H13 H 0.1295(3) 0.1647(2) 0.6082(2) 0.044 Uiso 1 calc R . 
C14 C -0.0102(3) 0.2138(2) 0.6618(2) 0.0451(12) Uani 1 d . . 
H14 H -0.0643(3) 0.1730(2) 0.6565(2) 0.054 Uiso 1 calc R . 
C15 C -0.0499(3) 0.2792(3) 0.6995(2) 0.0514(13) Uani 1 d . . 
H15 H -0.1290(3) 0.2812(3) 0.7200(2) 0.062 Uiso 1 calc R . 
C16 C 0.0273(3) 0.3391(2) 0.7058(2) 0.0474(12) Uani 1 d . . 
H16 H 0.0007(3) 0.3820(2) 0.7317(2) 0.057 Uiso 1 calc R . 
C17 C 0.1488(3) 0.3386(3) 0.6739(2) 0.0403(12) Uani 1 d . . 
C18 C 0.2229(3) 0.4021(2) 0.6771(2) 0.0443(12) Uani 1 d . . 
H18 H 0.1964(3) 0.4448(2) 0.7032(2) 0.053 Uiso 1 calc R . 
C19 C 0.3375(4) 0.4025(2) 0.6413(2) 0.0369(11) Uani 1 d . . 
C20 C 0.4097(4) 0.4711(2) 0.6393(2) 0.0539(13) Uani 1 d . . 
H20 H 0.3804(4) 0.5146(2) 0.6627(2) 0.065 Uiso 1 calc R . 
C21 C 0.5201(4) 0.4725(2) 0.6034(3) 0.0672(15) Uani 1 d . . 
H21 H 0.5651(4) 0.5175(2) 0.6011(3) 0.081 Uiso 1 calc R . 
C22 C 0.5672(3) 0.4064(3) 0.5695(3) 0.061(2) Uani 1 d . . 
H22 H 0.6435(3) 0.4079(3) 0.5455(3) 0.073 Uiso 1 calc R . 
C23 C 0.5032(3) 0.3411(2) 0.5715(2) 0.0464(12) Uani 1 d . . 
H23 H 0.5365(3) 0.2981(2) 0.5490(2) 0.056 Uiso 1 calc R . 
C24 C 0.3848(3) 0.3359(2) 0.6074(2) 0.0296(11) 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 C7 2.017(4) . ? 
Fe1 C6 2.028(3) . ? 
Fe1 C8 2.029(4) . ? 
Fe1 C5 2.033(4) . ? 
Fe1 C3 2.033(4) . ? 
Fe1 C2 2.037(4) . ? 
Fe1 C1 2.037(4) . ? 
Fe1 C4 2.040(4) . ? 
Fe1 C9 2.051(4) . ? 
Fe1 C10 2.088(3) . ? 
C1 C2 1.393(5) . ? 
C1 C5 1.395(5) . ? 
C2 C3 1.414(5) . ? 
C3 C4 1.399(5) . ? 
C4 C5 1.419(5) . ? 
C6 C7 1.399(5) . ? 
C6 C10 1.419(5) . ? 
C7 C8 1.396(5) . ? 
C8 C9 1.402(5) . ? 
C9 C10 1.430(5) . ? 
C10 C11 1.492(5) . ? 
C11 C12 1.420(4) . ? 
C11 C24 1.420(5) . ? 
C12 C17 1.426(5) . ? 
C12 C13 1.435(5) . ? 
C13 C14 1.355(4) . ? 
C14 C15 1.402(5) . ? 
C15 C16 1.350(5) . ? 
C16 C17 1.432(4) . ? 
C17 C18 1.376(5) . ? 
C18 C19 1.393(5) . ? 
C19 C24 1.417(5) . ? 
C19 C20 1.437(5) . ? 
C20 C21 1.354(5) . ? 
C21 C22 1.409(5) . ? 
C22 C23 1.342(4) . ? 
C23 C24 1.433(4) . ? 
 
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 
C7 Fe1 C6 40.47(14) . . ? 
C7 Fe1 C8 40.4(2) . . ? 
C6 Fe1 C8 67.84(15) . . ? 
C7 Fe1 C5 159.7(2) . . ? 
C6 Fe1 C5 159.2(2) . . ? 
C8 Fe1 C5 124.9(2) . . ? 
C7 Fe1 C3 120.2(2) . . ? 
C6 Fe1 C3 107.7(2) . . ? 
C8 Fe1 C3 155.1(2) . . ? 
C5 Fe1 C3 67.8(2) . . ? 
C7 Fe1 C2 105.5(2) . . ? 
C6 Fe1 C2 123.3(2) . . ? 
C8 Fe1 C2 119.7(2) . . ? 
C5 Fe1 C2 67.5(2) . . ? 
C3 Fe1 C2 40.66(15) . . ? 
C7 Fe1 C1 122.5(2) . . ? 
C6 Fe1 C1 159.0(2) . . ? 
C8 Fe1 C1 107.1(2) . . ? 
C5 Fe1 C1 40.10(14) . . ? 
C3 Fe1 C1 67.8(2) . . ? 
C2 Fe1 C1 40.0(2) . . ? 
C7 Fe1 C4 156.4(2) . . ? 
C6 Fe1 C4 122.7(2) . . ? 
C8 Fe1 C4 162.7(2) . . ? 
C5 Fe1 C4 40.78(15) . . ? 
C3 Fe1 C4 40.19(15) . . ? 
C2 Fe1 C4 68.0(2) . . ? 
C1 Fe1 C4 68.0(2) . . ? 
C7 Fe1 C9 67.6(2) . . ? 
C6 Fe1 C9 67.45(15) . . ? 
C8 Fe1 C9 40.20(13) . . ? 
C5 Fe1 C9 110.5(2) . . ? 
C3 Fe1 C9 162.9(2) . . ? 
C2 Fe1 C9 155.9(2) . . ? 
C1 Fe1 C9 122.7(2) . . ? 
C4 Fe1 C9 127.3(2) . . ? 
C7 Fe1 C10 68.17(14) . . ? 
C6 Fe1 C10 40.31(13) . . ? 
C8 Fe1 C10 68.2(2) . . ? 
C5 Fe1 C10 124.4(2) . . ? 
C3 Fe1 C10 125.4(2) . . ? 
C2 Fe1 C10 160.7(2) . . ? 
C1 Fe1 C10 158.8(2) . . ? 
C4 Fe1 C10 110.0(2) . . ? 
C9 Fe1 C10 40.41(13) . . ? 
C2 C1 C5 108.4(5) . . ? 
C2 C1 Fe1 70.0(2) . . ? 
C5 C1 Fe1 69.8(2) . . ? 
C1 C2 C3 107.9(4) . . ? 
C1 C2 Fe1 70.0(3) . . ? 
C3 C2 Fe1 69.5(2) . . ? 
C4 C3 C2 108.3(4) . . ? 
C4 C3 Fe1 70.2(2) . . ? 
C2 C3 Fe1 69.8(2) . . ? 
C3 C4 C5 107.2(4) . . ? 
C3 C4 Fe1 69.7(2) . . ? 
C5 C4 Fe1 69.4(2) . . ? 
C1 C5 C4 108.2(5) . . ? 
C1 C5 Fe1 70.1(2) . . ? 
C4 C5 Fe1 69.9(2) . . ? 
C7 C6 C10 109.4(3) . . ? 
C7 C6 Fe1 69.3(2) . . ? 
C10 C6 Fe1 72.1(2) . . ? 
C8 C7 C6 108.2(4) . . ? 
C8 C7 Fe1 70.3(2) . . ? 
C6 C7 Fe1 70.2(2) . . ? 
C7 C8 C9 108.0(4) . . ? 
C7 C8 Fe1 69.4(2) . . ? 
C9 C8 Fe1 70.8(3) . . ? 
C8 C9 C10 109.1(4) . . ? 
C8 C9 Fe1 69.0(3) . . ? 
C10 C9 Fe1 71.2(2) . . ? 
C6 C10 C9 105.3(4) . . ? 
C6 C10 C11 125.8(4) . . ? 
C9 C10 C11 128.2(4) . . ? 
C6 C10 Fe1 67.6(2) . . ? 
C9 C10 Fe1 68.4(2) . . ? 
C11 C10 Fe1 135.2(3) . . ? 
C12 C11 C24 119.2(4) . . ? 
C12 C11 C10 117.5(3) . . ? 
C24 C11 C10 123.3(3) . . ? 
C11 C12 C17 119.2(4) . . ? 
C11 C12 C13 123.2(4) . . ? 
C17 C12 C13 117.5(3) . . ? 
C14 C13 C12 121.2(4) . . ? 
C13 C14 C15 121.2(4) . . ? 
C16 C15 C14 119.7(4) . . ? 
C15 C16 C17 121.8(4) . . ? 
C18 C17 C12 120.9(4) . . ? 
C18 C17 C16 120.7(4) . . ? 
C12 C17 C16 118.4(4) . . ? 
C17 C18 C19 120.1(4) . . ? 
C18 C19 C24 120.8(4) . . ? 
C18 C19 C20 119.9(4) . . ? 
C24 C19 C20 119.3(4) . . ? 
C21 C20 C19 120.4(4) . . ? 
C20 C21 C22 120.4(4) . . ? 
C23 C22 C21 120.8(4) . . ? 
C22 C23 C24 121.7(4) . . ? 
C19 C24 C11 119.3(3) . . ? 
C19 C24 C23 117.4(3) . . ? 
C11 C24 C23 123.3(4) . . ? 
 
_refine_diff_density_max    0.405 
_refine_diff_density_min   -0.176 
_refine_diff_density_rms    0.047 
