 
data_s92 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C34 H28 Fe P2' 
_chemical_formula_weight          554.35 
_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' 
 'Fe'  'Fe'   0.3463   0.8444 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/c
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    8.6164(4) 
_cell_length_b                    18.419(2) 
_cell_length_c                    8.7071(7) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  101.283(11) 
_cell_angle_gamma                 90.00 
_cell_volume                      1355.1(2) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.21 
_exptl_crystal_size_mid           0.21
_exptl_crystal_size_min           0.14
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.359 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              576 
_exptl_absorpt_coefficient_mu     0.696 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       150(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             5442 
_diffrn_reflns_av_R_equivalents   0.1434 
_diffrn_reflns_av_sigmaI/netI     0.1489 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -19 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        -10 
_diffrn_reflns_limit_l_max        9 
_diffrn_reflns_theta_min          2.21 
_diffrn_reflns_theta_max          25.02 
_reflns_number_total              1969 
_reflns_number_observed           1398 
_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^)+(0.0255P)^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          1962 
_refine_ls_number_parameters      169 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0706 
_refine_ls_R_factor_obs           0.0457 
_refine_ls_wR_factor_all          0.1176 
_refine_ls_wR_factor_obs          0.0992 
_refine_ls_goodness_of_fit_all    0.909 
_refine_ls_goodness_of_fit_obs    1.058 
_refine_ls_restrained_S_all       1.059 
_refine_ls_restrained_S_obs       1.058 
_refine_ls_shift/esd_max          0.000 
_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 0.5000 0.5000 0.0000 0.0277(3) Uani 1 d S . 
P1 P 0.61421(11) 0.36397(6) 0.27242(12) 0.0273(3) Uani 1 d . . 
C1 C 0.5182(4) 0.5178(2) 0.2323(4) 0.0281(10) Uani 1 d . . 
H1 H 0.4344(4) 0.5167(2) 0.2852(4) 0.034 Uiso 1 calc R . 
C2 C 0.5707(5) 0.5793(2) 0.1642(5) 0.0408(11) Uani 1 d . . 
H2 H 0.5295(5) 0.6259(2) 0.1657(5) 0.049 Uiso 1 calc R . 
C3 C 0.6962(5) 0.5588(3) 0.0931(4) 0.0411(12) Uani 1 d . . 
H3 H 0.7519(5) 0.5892(3) 0.0380(4) 0.049 Uiso 1 calc R . 
C4 C 0.7236(4) 0.4848(3) 0.1191(4) 0.0353(11) Uani 1 d . . 
H4 H 0.8010(4) 0.4576(3) 0.0844(4) 0.042 Uiso 1 calc R . 
C5 C 0.6121(4) 0.4572(2) 0.2086(4) 0.0268(9) Uani 1 d . . 
C6 C 0.8100(4) 0.4342(2) 0.5298(4) 0.0259(9) Uani 1 d . . 
H6 H 0.8181(4) 0.4719(2) 0.4607(4) 0.031 Uiso 1 calc R . 
C7 C 0.8938(4) 0.4378(2) 0.6832(4) 0.0317(10) Uani 1 d . . 
H7 H 0.9567(4) 0.4780(2) 0.7161(4) 0.038 Uiso 1 calc R . 
C8 C 0.8844(4) 0.3824(2) 0.7865(5) 0.0328(10) Uani 1 d . . 
H8 H 0.9404(4) 0.3849(2) 0.8891(5) 0.039 Uiso 1 calc R . 
C9 C 0.7902(4) 0.3225(2) 0.7356(5) 0.0361(10) Uani 1 d . . 
H9 H 0.7824(4) 0.2849(2) 0.8050(5) 0.043 Uiso 1 calc R . 
C10 C 0.7082(4) 0.3185(2) 0.5834(4) 0.0336(10) Uani 1 d . . 
H10 H 0.6480(4) 0.2774(2) 0.5504(4) 0.040 Uiso 1 calc R . 
C11 C 0.7139(4) 0.3746(2) 0.4786(4) 0.0236(9) Uani 1 d . . 
C12 C 0.4102(4) 0.3474(2) 0.2939(4) 0.0236(9) Uani 1 d . . 
C13 C 0.3411(4) 0.3807(2) 0.4086(4) 0.0284(10) Uani 1 d . . 
H13 H 0.4009(4) 0.4121(2) 0.4806(4) 0.034 Uiso 1 calc R . 
C14 C 0.1856(4) 0.3675(2) 0.4159(5) 0.0358(11) Uani 1 d . . 
H14 H 0.1409(4) 0.3899(2) 0.4927(5) 0.043 Uiso 1 calc R . 
C15 C 0.0955(4) 0.3211(2) 0.3092(5) 0.0389(11) Uani 1 d . . 
H15 H -0.0102(4) 0.3131(2) 0.3132(5) 0.047 Uiso 1 calc R . 
C16 C 0.1611(4) 0.2867(2) 0.1978(5) 0.0439(12) Uani 1 d . . 
H16 H 0.1007(4) 0.2549(2) 0.1272(5) 0.053 Uiso 1 calc R . 
C17 C 0.3180(4) 0.2996(2) 0.1912(5) 0.0348(10) Uani 1 d . . 
H17 H 0.3626(4) 0.2756(2) 0.1163(5) 0.042 Uiso 1 calc R . 
 
 
_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 C4 2.021(3) 3_665 ? 
Fe1 C4 2.021(3) . ? 
Fe1 C1 2.024(4) . ? 
Fe1 C1 2.024(4) 3_665 ? 
Fe1 C3 2.037(4) . ? 
Fe1 C3 2.037(4) 3_665 ? 
Fe1 C5 2.041(3) 3_665 ? 
Fe1 C5 2.041(3) . ? 
Fe1 C2 2.052(4) . ? 
Fe1 C2 2.052(4) 3_665 ? 
P1 C5 1.804(4) . ? 
P1 C12 1.829(4) . ? 
P1 C11 1.843(4) . ? 
C1 C2 1.395(5) . ? 
C1 C5 1.417(5) . ? 
C2 C3 1.399(6) . ? 
C3 C4 1.394(6) . ? 
C4 C5 1.442(5) . ? 
C6 C7 1.390(5) . ? 
C6 C11 1.395(5) . ? 
C7 C8 1.373(5) . ? 
C8 C9 1.389(5) . ? 
C9 C10 1.377(5) . ? 
C10 C11 1.386(5) . ? 
C12 C17 1.389(5) . ? 
C12 C13 1.401(5) . ? 
C13 C14 1.375(5) . ? 
C14 C15 1.384(5) . ? 
C15 C16 1.370(5) . ? 
C16 C17 1.385(5) . ? 
 
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 
C4 Fe1 C4 180.0 3_665 . ? 
C4 Fe1 C1 111.71(14) 3_665 . ? 
C4 Fe1 C1 68.29(14) . . ? 
C4 Fe1 C1 68.29(14) 3_665 3_665 ? 
C4 Fe1 C1 111.71(14) . 3_665 ? 
C1 Fe1 C1 180.0 . 3_665 ? 
C4 Fe1 C3 139.8(2) 3_665 . ? 
C4 Fe1 C3 40.2(2) . . ? 
C1 Fe1 C3 67.7(2) . . ? 
C1 Fe1 C3 112.3(2) 3_665 . ? 
C4 Fe1 C3 40.2(2) 3_665 3_665 ? 
C4 Fe1 C3 139.8(2) . 3_665 ? 
C1 Fe1 C3 112.3(2) . 3_665 ? 
C1 Fe1 C3 67.7(2) 3_665 3_665 ? 
C3 Fe1 C3 180.0 . 3_665 ? 
C4 Fe1 C5 41.59(14) 3_665 3_665 ? 
C4 Fe1 C5 138.41(14) . 3_665 ? 
C1 Fe1 C5 139.20(14) . 3_665 ? 
C1 Fe1 C5 40.80(14) 3_665 3_665 ? 
C3 Fe1 C5 111.1(2) . 3_665 ? 
C3 Fe1 C5 68.9(2) 3_665 3_665 ? 
C4 Fe1 C5 138.41(14) 3_665 . ? 
C4 Fe1 C5 41.59(14) . . ? 
C1 Fe1 C5 40.80(14) . . ? 
C1 Fe1 C5 139.20(14) 3_665 . ? 
C3 Fe1 C5 68.9(2) . . ? 
C3 Fe1 C5 111.1(2) 3_665 . ? 
C5 Fe1 C5 180.0 3_665 . ? 
C4 Fe1 C2 112.5(2) 3_665 . ? 
C4 Fe1 C2 67.5(2) . . ? 
C1 Fe1 C2 40.01(15) . . ? 
C1 Fe1 C2 139.99(15) 3_665 . ? 
C3 Fe1 C2 40.0(2) . . ? 
C3 Fe1 C2 140.0(2) 3_665 . ? 
C5 Fe1 C2 111.7(2) 3_665 . ? 
C5 Fe1 C2 68.3(2) . . ? 
C4 Fe1 C2 67.5(2) 3_665 3_665 ? 
C4 Fe1 C2 112.5(2) . 3_665 ? 
C1 Fe1 C2 139.99(15) . 3_665 ? 
C1 Fe1 C2 40.01(15) 3_665 3_665 ? 
C3 Fe1 C2 140.0(2) . 3_665 ? 
C3 Fe1 C2 40.0(2) 3_665 3_665 ? 
C5 Fe1 C2 68.3(2) 3_665 3_665 ? 
C5 Fe1 C2 111.7(2) . 3_665 ? 
C2 Fe1 C2 180.0 . 3_665 ? 
C5 P1 C12 103.8(2) . . ? 
C5 P1 C11 100.0(2) . . ? 
C12 P1 C11 101.1(2) . . ? 
C2 C1 C5 109.6(4) . . ? 
C2 C1 Fe1 71.1(2) . . ? 
C5 C1 Fe1 70.2(2) . . ? 
C1 C2 C3 108.1(4) . . ? 
C1 C2 Fe1 68.9(2) . . ? 
C3 C2 Fe1 69.4(2) . . ? 
C4 C3 C2 108.3(4) . . ? 
C4 C3 Fe1 69.3(2) . . ? 
C2 C3 Fe1 70.5(2) . . ? 
C3 C4 C5 108.8(4) . . ? 
C3 C4 Fe1 70.5(2) . . ? 
C5 C4 Fe1 69.9(2) . . ? 
C1 C5 C4 105.1(4) . . ? 
C1 C5 P1 132.6(3) . . ? 
C4 C5 P1 122.3(3) . . ? 
C1 C5 Fe1 69.0(2) . . ? 
C4 C5 Fe1 68.5(2) . . ? 
P1 C5 Fe1 128.0(2) . . ? 
C7 C6 C11 120.6(4) . . ? 
C8 C7 C6 120.6(4) . . ? 
C7 C8 C9 119.1(4) . . ? 
C10 C9 C8 120.5(4) . . ? 
C9 C10 C11 121.0(4) . . ? 
C10 C11 C6 118.2(3) . . ? 
C10 C11 P1 119.5(3) . . ? 
C6 C11 P1 121.9(3) . . ? 
C17 C12 C13 117.9(3) . . ? 
C17 C12 P1 118.7(3) . . ? 
C13 C12 P1 123.4(3) . . ? 
C14 C13 C12 120.6(4) . . ? 
C13 C14 C15 120.1(4) . . ? 
C16 C15 C14 120.4(4) . . ? 
C15 C16 C17 119.4(4) . . ? 
C16 C17 C12 121.5(4) . . ? 
 
_refine_diff_density_max    0.518 
_refine_diff_density_min   -0.402 
_refine_diff_density_rms    0.080 
