 
data_s92 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C17 H11 Br Fe Mo O6' 
_chemical_formula_weight          542.96 
_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' 
 'O'  'O'   0.0106   0.0060 
 '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' 
 'Br'  'Br'  -0.2901   2.4595 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Mo'  'Mo'  -1.6832   0.6857 
 '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                    10.655(4) 
_cell_length_b                    12.3456(6) 
_cell_length_c                    14.319(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  103.142(11) 
_cell_angle_gamma                 90.00 
_cell_volume                      1834.1(7) 
_cell_formula_units_Z             4 
_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           0.31 
_exptl_crystal_size_mid           0.18 
_exptl_crystal_size_min           0.11 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.966 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1056 
_exptl_absorpt_coefficient_mu     3.683 
_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             7104 
_diffrn_reflns_av_R_equivalents   0.0586 
_diffrn_reflns_av_sigmaI/netI     0.0677 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -16 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          1.96 
_diffrn_reflns_theta_max          24.94 
_reflns_number_total              2654 
_reflns_number_observed           2039 
_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 8 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^)+(0.0899P)^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          2646 
_refine_ls_number_parameters      236 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0586 
_refine_ls_R_factor_obs           0.0448 
_refine_ls_wR_factor_all          0.1471 
_refine_ls_wR_factor_obs          0.1230 
_refine_ls_goodness_of_fit_all    0.912 
_refine_ls_goodness_of_fit_obs    1.023 
_refine_ls_restrained_S_all       1.063 
_refine_ls_restrained_S_obs       1.023 
_refine_ls_shift/esd_max          -0.434 
_refine_ls_shift/esd_mean         0.009 
 
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 
Mo1 Mo 0.05233(5) 0.69154(5) 0.16456(4) 0.0289(2) Uani 1 d . . 
Br1 Br 0.65855(10) 0.60836(9) 0.54439(7) 0.0766(4) Uani 1 d . . 
Fe1 Fe 0.46754(9) 0.74458(8) 0.34828(7) 0.0338(3) Uani 1 d . . 
O1 O 0.2534(4) 0.8837(4) 0.1538(3) 0.0385(12) Uani 1 d . . 
O2 O 0.1376(5) 0.5854(5) 0.3702(4) 0.058(2) Uani 1 d . . 
O3 O -0.0902(7) 0.8706(5) 0.2631(5) 0.077(2) Uani 1 d . . 
O4 O -0.1997(6) 0.5518(5) 0.1496(4) 0.074(2) Uani 1 d . . 
O5 O -0.0748(6) 0.7737(5) -0.0478(4) 0.072(2) Uani 1 d . . 
O6 O 0.1738(6) 0.4990(5) 0.0667(4) 0.073(2) Uani 1 d . . 
C1 C 0.5437(8) 0.7192(7) 0.4902(5) 0.047(2) Uani 1 d . . 
C2 C 0.5771(9) 0.8242(7) 0.4630(6) 0.060(2) Uani 1 d . . 
H2 H 0.6600(9) 0.8505(7) 0.4672(6) 0.072 Uiso 1 calc R . 
C3 C 0.4633(11) 0.8799(7) 0.4291(6) 0.068(3) Uani 1 d . . 
H3 H 0.4578(11) 0.9509(7) 0.4068(6) 0.081 Uiso 1 calc R . 
C4 C 0.3585(9) 0.8150(7) 0.4330(6) 0.059(2) Uani 1 d . . 
H4 H 0.2720(9) 0.8339(7) 0.4135(6) 0.071 Uiso 1 calc R . 
C5 C 0.4081(8) 0.7144(7) 0.4724(5) 0.052(2) Uani 1 d . . 
H5 H 0.3598(8) 0.6555(7) 0.4845(5) 0.063 Uiso 1 calc R . 
C6 C 0.3988(7) 0.6288(5) 0.2477(5) 0.036(2) Uani 1 d . . 
H6 H 0.3412(7) 0.5736(5) 0.2525(5) 0.043 Uiso 1 calc R . 
C7 C 0.5338(7) 0.6219(6) 0.2767(5) 0.043(2) Uani 1 d . . 
H7 H 0.5802(7) 0.5620(6) 0.3051(5) 0.051 Uiso 1 calc R . 
C8 C 0.5858(7) 0.7185(7) 0.2559(6) 0.054(2) Uani 1 d . . 
H8 H 0.6734(7) 0.7332(7) 0.2657(6) 0.065 Uiso 1 calc R . 
C9 C 0.4852(7) 0.7920(6) 0.2174(5) 0.045(2) Uani 1 d . . 
H9 H 0.4947(7) 0.8637(6) 0.2002(5) 0.054 Uiso 1 calc R . 
C10 C 0.3647(6) 0.7343(6) 0.2100(4) 0.034(2) Uani 1 d . . 
C11 C 0.2362(6) 0.7819(5) 0.1784(4) 0.031(2) Uani 1 d . . 
C12 C 0.1459(7) 0.9550(6) 0.1183(6) 0.045(2) Uani 1 d . . 
H12A H 0.1037(29) 0.9340(25) 0.0543(14) 0.067 Uiso 1 calc R . 
H12B H 0.1765(9) 1.0281(8) 0.1177(34) 0.067 Uiso 1 calc R . 
H12C H 0.0861(24) 0.9504(30) 0.1591(21) 0.067 Uiso 1 calc R . 
C13 C 0.1125(6) 0.6255(6) 0.2978(5) 0.038(2) Uani 1 d . . 
C14 C -0.0364(8) 0.8107(6) 0.2266(6) 0.046(2) Uani 1 d . . 
C15 C -0.1105(8) 0.6033(6) 0.1527(5) 0.044(2) Uani 1 d . . 
C16 C -0.0267(8) 0.7488(6) 0.0281(6) 0.049(2) Uani 1 d . . 
C17 C 0.1327(7) 0.5689(6) 0.1025(5) 0.043(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 
Mo1 C15 2.022(8) . ? 
Mo1 C17 2.040(8) . ? 
Mo1 C13 2.039(8) . ? 
Mo1 C16 2.069(9) . ? 
Mo1 C14 2.057(9) . ? 
Mo1 C11 2.224(7) . ? 
Br1 C1 1.882(8) . ? 
Fe1 C9 2.012(7) . ? 
Fe1 C1 2.033(7) . ? 
Fe1 C2 2.038(8) . ? 
Fe1 C10 2.037(6) . ? 
Fe1 C3 2.038(8) . ? 
Fe1 C6 2.043(7) . ? 
Fe1 C7 2.043(7) . ? 
Fe1 C5 2.052(8) . ? 
Fe1 C8 2.049(8) . ? 
Fe1 C4 2.054(8) . ? 
O1 C11 1.329(8) . ? 
O1 C12 1.442(8) . ? 
O2 C13 1.126(8) . ? 
O3 C14 1.133(9) . ? 
O4 C15 1.137(8) . ? 
O5 C16 1.133(9) . ? 
O6 C17 1.140(9) . ? 
C1 C5 1.409(11) . ? 
C1 C2 1.422(11) . ? 
C2 C3 1.383(12) . ? 
C3 C4 1.386(13) . ? 
C4 C5 1.416(11) . ? 
C6 C7 1.405(10) . ? 
C6 C10 1.426(9) . ? 
C7 C8 1.375(11) . ? 
C8 C9 1.417(10) . ? 
C9 C10 1.451(10) . ? 
C10 C11 1.463(9) . ? 
 
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 Mo1 C17 90.0(3) . . ? 
C15 Mo1 C13 86.9(3) . . ? 
C17 Mo1 C13 92.1(3) . . ? 
C15 Mo1 C16 87.0(3) . . ? 
C17 Mo1 C16 87.9(3) . . ? 
C13 Mo1 C16 173.8(3) . . ? 
C15 Mo1 C14 87.2(3) . . ? 
C17 Mo1 C14 177.3(3) . . ? 
C13 Mo1 C14 87.7(3) . . ? 
C16 Mo1 C14 92.0(3) . . ? 
C15 Mo1 C11 177.5(3) . . ? 
C17 Mo1 C11 87.9(3) . . ? 
C13 Mo1 C11 91.9(3) . . ? 
C16 Mo1 C11 94.2(3) . . ? 
C14 Mo1 C11 94.9(3) . . ? 
C9 Fe1 C1 151.0(3) . . ? 
C9 Fe1 C2 116.9(4) . . ? 
C1 Fe1 C2 40.9(3) . . ? 
C9 Fe1 C10 42.0(3) . . ? 
C1 Fe1 C10 164.9(3) . . ? 
C2 Fe1 C10 153.6(3) . . ? 
C9 Fe1 C3 108.0(4) . . ? 
C1 Fe1 C3 67.3(3) . . ? 
C2 Fe1 C3 39.7(3) . . ? 
C10 Fe1 C3 121.7(3) . . ? 
C9 Fe1 C6 69.0(3) . . ? 
C1 Fe1 C6 126.4(3) . . ? 
C2 Fe1 C6 162.4(3) . . ? 
C10 Fe1 C6 40.9(3) . . ? 
C3 Fe1 C6 157.3(4) . . ? 
C9 Fe1 C7 68.4(3) . . ? 
C1 Fe1 C7 106.4(3) . . ? 
C2 Fe1 C7 124.2(3) . . ? 
C10 Fe1 C7 68.7(3) . . ? 
C3 Fe1 C7 161.3(4) . . ? 
C6 Fe1 C7 40.2(3) . . ? 
C9 Fe1 C5 166.4(3) . . ? 
C1 Fe1 C5 40.4(3) . . ? 
C2 Fe1 C5 67.8(4) . . ? 
C10 Fe1 C5 128.8(3) . . ? 
C3 Fe1 C5 66.8(4) . . ? 
C6 Fe1 C5 110.6(3) . . ? 
C7 Fe1 C5 120.7(3) . . ? 
C9 Fe1 C8 40.8(3) . . ? 
C1 Fe1 C8 117.2(3) . . ? 
C2 Fe1 C8 105.8(4) . . ? 
C10 Fe1 C8 68.7(3) . . ? 
C3 Fe1 C8 126.3(4) . . ? 
C6 Fe1 C8 67.0(3) . . ? 
C7 Fe1 C8 39.3(3) . . ? 
C5 Fe1 C8 152.4(3) . . ? 
C9 Fe1 C4 127.8(3) . . ? 
C1 Fe1 C4 68.0(3) . . ? 
C2 Fe1 C4 67.5(4) . . ? 
C10 Fe1 C4 110.4(3) . . ? 
C3 Fe1 C4 39.6(4) . . ? 
C6 Fe1 C4 123.5(3) . . ? 
C7 Fe1 C4 156.4(4) . . ? 
C5 Fe1 C4 40.3(3) . . ? 
C8 Fe1 C4 164.0(4) . . ? 
C11 O1 C12 121.6(5) . . ? 
C5 C1 C2 107.4(7) . . ? 
C5 C1 Br1 126.0(6) . . ? 
C2 C1 Br1 126.6(6) . . ? 
C5 C1 Fe1 70.6(4) . . ? 
C2 C1 Fe1 69.7(4) . . ? 
Br1 C1 Fe1 126.8(4) . . ? 
C3 C2 C1 107.2(8) . . ? 
C3 C2 Fe1 70.2(5) . . ? 
C1 C2 Fe1 69.4(4) . . ? 
C2 C3 C4 110.4(8) . . ? 
C2 C3 Fe1 70.2(5) . . ? 
C4 C3 Fe1 70.8(5) . . ? 
C3 C4 C5 107.0(8) . . ? 
C3 C4 Fe1 69.6(5) . . ? 
C5 C4 Fe1 69.8(4) . . ? 
C1 C5 C4 108.0(8) . . ? 
C1 C5 Fe1 69.1(4) . . ? 
C4 C5 Fe1 69.9(5) . . ? 
C7 C6 C10 108.8(6) . . ? 
C7 C6 Fe1 69.9(4) . . ? 
C10 C6 Fe1 69.3(4) . . ? 
C8 C7 C6 108.6(7) . . ? 
C8 C7 Fe1 70.6(4) . . ? 
C6 C7 Fe1 69.9(4) . . ? 
C7 C8 C9 109.5(7) . . ? 
C7 C8 Fe1 70.1(5) . . ? 
C9 C8 Fe1 68.2(4) . . ? 
C8 C9 C10 107.0(7) . . ? 
C8 C9 Fe1 71.0(4) . . ? 
C10 C9 Fe1 69.9(4) . . ? 
C6 C10 C9 106.0(6) . . ? 
C6 C10 C11 128.6(6) . . ? 
C9 C10 C11 125.1(6) . . ? 
C6 C10 Fe1 69.7(4) . . ? 
C9 C10 Fe1 68.1(4) . . ? 
C11 C10 Fe1 122.3(5) . . ? 
O1 C11 C10 106.6(6) . . ? 
O1 C11 Mo1 128.5(5) . . ? 
C10 C11 Mo1 124.7(5) . . ? 
O2 C13 Mo1 175.1(6) . . ? 
O3 C14 Mo1 175.0(7) . . ? 
O4 C15 Mo1 177.1(6) . . ? 
O5 C16 Mo1 175.2(7) . . ? 
O6 C17 Mo1 177.8(7) . . ? 
 
_refine_diff_density_max    0.703 
_refine_diff_density_min   -1.265 
_refine_diff_density_rms    0.132 
