 
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 H16 Fe N2 O4 W' 
_chemical_formula_weight          636.09 
_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' 
 'N'  'N'   0.0061   0.0033 
 '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' 
 'W'  'W'  -0.8490   6.8722 
 '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 

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                    11.732(3) 
_cell_length_b                    16.0425(15) 
_cell_length_c                    12.2877(13) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  113.566(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      2119.7(6) 
_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           0.2
_exptl_crystal_size_mid           0.18
_exptl_crystal_size_min           0.11 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.993 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1224 
_exptl_absorpt_coefficient_mu     6.141 
_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             7046 
_diffrn_reflns_av_R_equivalents   0.0549 
_diffrn_reflns_av_sigmaI/netI     0.0632 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -18 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          2.03 
_diffrn_reflns_theta_max          25.03 
_reflns_number_total              3211 
_reflns_number_observed           2698 
_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 1 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^)+(0.0438P)^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          3210 
_refine_ls_number_parameters      289 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0439 
_refine_ls_R_factor_obs           0.0354 
_refine_ls_wR_factor_all          0.0852 
_refine_ls_wR_factor_obs          0.0833 
_refine_ls_goodness_of_fit_all    1.023 
_refine_ls_goodness_of_fit_obs    1.106 
_refine_ls_restrained_S_all       1.029 
_refine_ls_restrained_S_obs       1.106 
_refine_ls_shift/esd_max          0.002 
_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 
W1 W 0.15177(2) 0.87274(2) 0.89096(2) 0.01942(12) Uani 1 d . . 
Fe1 Fe 0.21410(9) 0.85290(6) 1.35616(9) 0.0289(3) Uani 1 d . . 
N1 N 0.2791(5) 0.9396(3) 1.0595(5) 0.0202(13) Uani 1 d . . 
N2 N 0.2029(5) 0.9955(3) 0.8361(5) 0.0228(13) Uani 1 d . . 
O1 O 0.3882(4) 0.7865(3) 0.8748(5) 0.0389(14) Uani 1 d . . 
O2 O 0.1197(5) 0.6979(3) 0.9889(5) 0.0373(13) Uani 1 d . . 
O3 O -0.1110(5) 0.9238(3) 0.8909(5) 0.0447(15) Uani 1 d . . 
O4 O -0.0088(5) 0.8085(3) 0.6358(4) 0.0405(13) Uani 1 d . . 
C1 C 0.3029(7) 0.9558(5) 1.4509(7) 0.041(2) Uani 1 d . . 
H1 H 0.3456(7) 0.9967(5) 1.4286(7) 0.050 Uiso 1 calc R . 
C2 C 0.3547(8) 0.8801(5) 1.5142(7) 0.043(2) Uani 1 d . . 
H2 H 0.4364(8) 0.8618(5) 1.5386(7) 0.052 Uiso 1 calc R . 
C3 C 0.2574(8) 0.8393(6) 1.5320(7) 0.047(2) Uani 1 d . . 
H3 H 0.2648(8) 0.7892(6) 1.5723(7) 0.056 Uiso 1 calc R . 
C4 C 0.1477(9) 0.8858(5) 1.4796(8) 0.051(2) Uani 1 d . . 
H4 H 0.0705(9) 0.8719(5) 1.4790(8) 0.061 Uiso 1 calc R . 
C5 C 0.1748(8) 0.9563(6) 1.4288(8) 0.050(2) Uani 1 d . . 
H5 H 0.1180(8) 0.9973(6) 1.3871(8) 0.060 Uiso 1 calc R . 
C6 C 0.2828(7) 0.7727(4) 1.2681(6) 0.032(2) Uani 1 d . . 
H6 H 0.3634(7) 0.7517(4) 1.2966(6) 0.039 Uiso 1 calc R . 
C7 C 0.1801(7) 0.7361(5) 1.2822(7) 0.039(2) Uani 1 d . . 
H7 H 0.1809(7) 0.6861(5) 1.3209(7) 0.047 Uiso 1 calc R . 
C8 C 0.0744(7) 0.7892(4) 1.2266(7) 0.038(2) Uani 1 d . . 
H8 H -0.0049(7) 0.7802(4) 1.2241(7) 0.046 Uiso 1 calc R . 
C9 C 0.1111(7) 0.8570(4) 1.1766(6) 0.028(2) Uani 1 d . . 
H9 H 0.0601(7) 0.9005(4) 1.1344(6) 0.033 Uiso 1 calc R . 
C10 C 0.2401(6) 0.8481(4) 1.2017(6) 0.024(2) Uani 1 d . . 
C11 C 0.3173(6) 0.9078(4) 1.1692(6) 0.0170(14) Uani 1 d . . 
C12 C 0.4333(6) 0.9334(4) 1.2590(6) 0.029(2) Uani 1 d . . 
H12 H 0.4645(6) 0.9065(4) 1.3321(6) 0.035 Uiso 1 calc R . 
C13 C 0.4990(6) 0.9975(4) 1.2379(6) 0.032(2) Uani 1 d . . 
H13 H 0.5751(6) 1.0142(4) 1.2957(6) 0.039 Uiso 1 calc R . 
C14 C 0.4500(6) 1.0369(4) 1.1288(6) 0.026(2) Uani 1 d . . 
H14 H 0.4891(6) 1.0835(4) 1.1146(6) 0.031 Uiso 1 calc R . 
C15 C 0.3416(6) 1.0062(4) 1.0405(6) 0.0203(15) Uani 1 d . . 
C16 C 0.2910(6) 1.0417(4) 0.9207(6) 0.025(2) Uani 1 d . . 
C17 C 0.3338(6) 1.1154(4) 0.8914(7) 0.030(2) Uani 1 d . . 
H17 H 0.3925(6) 1.1474(4) 0.9504(7) 0.036 Uiso 1 calc R . 
C18 C 0.2893(7) 1.1412(5) 0.7752(8) 0.045(2) Uani 1 d . . 
H18 H 0.3183(7) 1.1904(5) 0.7553(8) 0.054 Uiso 1 calc R . 
C19 C 0.2014(7) 1.0936(5) 0.6881(7) 0.038(2) Uani 1 d . . 
H19 H 0.1707(7) 1.1099(5) 0.6088(7) 0.046 Uiso 1 calc R . 
C20 C 0.1603(7) 1.0213(4) 0.7217(7) 0.039(2) Uani 1 d . . 
H20 H 0.1011(7) 0.9890(4) 0.6635(7) 0.047 Uiso 1 calc R . 
C21 C 0.3047(6) 0.8214(4) 0.8808(6) 0.025(2) Uani 1 d . . 
C22 C 0.1302(6) 0.7638(5) 0.9550(6) 0.026(2) Uani 1 d . . 
C23 C -0.0140(7) 0.9102(4) 0.8939(6) 0.030(2) Uani 1 d . . 
C24 C 0.0517(6) 0.8310(4) 0.7309(6) 0.025(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 
W1 C24 1.962(7) . ? 
W1 C22 1.974(8) . ? 
W1 C21 2.023(7) . ? 
W1 C23 2.050(8) . ? 
W1 N2 2.239(5) . ? 
W1 N1 2.280(5) . ? 
Fe1 C3 2.024(8) . ? 
Fe1 C5 2.023(9) . ? 
Fe1 C2 2.031(8) . ? 
Fe1 C4 2.033(8) . ? 
Fe1 C10 2.041(7) . ? 
Fe1 C6 2.043(7) . ? 
Fe1 C8 2.044(7) . ? 
Fe1 C9 2.049(7) . ? 
Fe1 C1 2.049(7) . ? 
Fe1 C7 2.051(8) . ? 
N1 C11 1.340(8) . ? 
N1 C15 1.368(8) . ? 
N2 C16 1.357(8) . ? 
N2 C20 1.355(9) . ? 
O1 C21 1.157(8) . ? 
O2 C22 1.160(8) . ? 
O3 C23 1.145(9) . ? 
O4 C24 1.156(8) . ? 
C1 C5 1.417(11) . ? 
C1 C2 1.439(11) . ? 
C2 C3 1.406(12) . ? 
C3 C4 1.402(12) . ? 
C4 C5 1.389(12) . ? 
C6 C7 1.412(10) . ? 
C6 C10 1.433(9) . ? 
C7 C8 1.433(10) . ? 
C8 C9 1.399(10) . ? 
C9 C10 1.426(10) . ? 
C10 C11 1.477(9) . ? 
C11 C12 1.428(9) . ? 
C12 C13 1.371(10) . ? 
C13 C14 1.381(10) . ? 
C14 C15 1.390(9) . ? 
C15 C16 1.465(9) . ? 
C16 C17 1.387(9) . ? 
C17 C18 1.373(11) . ? 
C18 C19 1.381(12) . ? 
C19 C20 1.382(10) . ? 
 
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 
C24 W1 C22 88.7(3) . . ? 
C24 W1 C21 89.4(3) . . ? 
C22 W1 C21 85.6(3) . . ? 
C24 W1 C23 85.8(3) . . ? 
C22 W1 C23 88.8(3) . . ? 
C21 W1 C23 172.6(2) . . ? 
C24 W1 N2 97.1(2) . . ? 
C22 W1 N2 172.3(2) . . ? 
C21 W1 N2 89.3(2) . . ? 
C23 W1 N2 96.7(2) . . ? 
C24 W1 N1 169.6(2) . . ? 
C22 W1 N1 101.3(2) . . ? 
C21 W1 N1 88.4(2) . . ? 
C23 W1 N1 97.4(2) . . ? 
N2 W1 N1 72.7(2) . . ? 
C3 Fe1 C5 67.7(4) . . ? 
C3 Fe1 C2 40.6(3) . . ? 
C5 Fe1 C2 69.1(3) . . ? 
C3 Fe1 C4 40.4(4) . . ? 
C5 Fe1 C4 40.1(3) . . ? 
C2 Fe1 C4 68.7(4) . . ? 
C3 Fe1 C10 157.2(3) . . ? 
C5 Fe1 C10 125.9(3) . . ? 
C2 Fe1 C10 122.1(3) . . ? 
C4 Fe1 C10 161.5(3) . . ? 
C3 Fe1 C6 120.9(3) . . ? 
C5 Fe1 C6 163.4(3) . . ? 
C2 Fe1 C6 107.5(3) . . ? 
C4 Fe1 C6 155.4(3) . . ? 
C10 Fe1 C6 41.1(3) . . ? 
C3 Fe1 C8 124.0(3) . . ? 
C5 Fe1 C8 120.0(3) . . ? 
C2 Fe1 C8 160.8(3) . . ? 
C4 Fe1 C8 106.5(4) . . ? 
C10 Fe1 C8 68.2(3) . . ? 
C6 Fe1 C8 68.6(3) . . ? 
C3 Fe1 C9 160.2(3) . . ? 
C5 Fe1 C9 108.0(3) . . ? 
C2 Fe1 C9 157.9(3) . . ? 
C4 Fe1 C9 123.9(3) . . ? 
C10 Fe1 C9 40.8(3) . . ? 
C6 Fe1 C9 68.8(3) . . ? 
C8 Fe1 C9 40.0(3) . . ? 
C3 Fe1 C1 68.1(3) . . ? 
C5 Fe1 C1 40.7(3) . . ? 
C2 Fe1 C1 41.3(3) . . ? 
C4 Fe1 C1 68.1(4) . . ? 
C10 Fe1 C1 109.1(3) . . ? 
C6 Fe1 C1 126.1(3) . . ? 
C8 Fe1 C1 155.9(3) . . ? 
C9 Fe1 C1 122.2(3) . . ? 
C3 Fe1 C7 107.2(3) . . ? 
C5 Fe1 C7 155.1(3) . . ? 
C2 Fe1 C7 124.1(3) . . ? 
C4 Fe1 C7 120.2(3) . . ? 
C10 Fe1 C7 68.2(3) . . ? 
C6 Fe1 C7 40.4(3) . . ? 
C8 Fe1 C7 41.0(3) . . ? 
C9 Fe1 C7 68.0(3) . . ? 
C1 Fe1 C7 162.3(3) . . ? 
C11 N1 C15 118.9(5) . . ? 
C11 N1 W1 124.7(4) . . ? 
C15 N1 W1 114.4(4) . . ? 
C16 N2 C20 118.7(6) . . ? 
C16 N2 W1 117.6(4) . . ? 
C20 N2 W1 123.3(4) . . ? 
C5 C1 C2 107.1(8) . . ? 
C5 C1 Fe1 68.7(5) . . ? 
C2 C1 Fe1 68.7(4) . . ? 
C3 C2 C1 106.5(7) . . ? 
C3 C2 Fe1 69.4(5) . . ? 
C1 C2 Fe1 70.0(4) . . ? 
C4 C3 C2 109.6(8) . . ? 
C4 C3 Fe1 70.1(5) . . ? 
C2 C3 Fe1 70.0(5) . . ? 
C5 C4 C3 107.8(8) . . ? 
C5 C4 Fe1 69.6(5) . . ? 
C3 C4 Fe1 69.4(5) . . ? 
C4 C5 C1 109.0(8) . . ? 
C4 C5 Fe1 70.4(5) . . ? 
C1 C5 Fe1 70.6(5) . . ? 
C7 C6 C10 107.5(6) . . ? 
C7 C6 Fe1 70.1(4) . . ? 
C10 C6 Fe1 69.4(4) . . ? 
C6 C7 C8 108.2(6) . . ? 
C6 C7 Fe1 69.5(4) . . ? 
C8 C7 Fe1 69.2(4) . . ? 
C9 C8 C7 108.2(7) . . ? 
C9 C8 Fe1 70.2(4) . . ? 
C7 C8 Fe1 69.8(4) . . ? 
C8 C9 C10 108.3(6) . . ? 
C8 C9 Fe1 69.8(4) . . ? 
C10 C9 Fe1 69.3(4) . . ? 
C9 C10 C6 107.9(6) . . ? 
C9 C10 C11 126.1(6) . . ? 
C6 C10 C11 126.0(6) . . ? 
C9 C10 Fe1 69.9(4) . . ? 
C6 C10 Fe1 69.5(4) . . ? 
C11 C10 Fe1 124.2(4) . . ? 
N1 C11 C12 119.9(6) . . ? 
N1 C11 C10 121.6(5) . . ? 
C12 C11 C10 118.4(6) . . ? 
C13 C12 C11 120.3(7) . . ? 
C12 C13 C14 118.6(6) . . ? 
C13 C14 C15 119.5(6) . . ? 
N1 C15 C14 121.9(6) . . ? 
N1 C15 C16 116.5(5) . . ? 
C14 C15 C16 121.6(6) . . ? 
N2 C16 C17 120.7(7) . . ? 
N2 C16 C15 115.8(6) . . ? 
C17 C16 C15 123.3(6) . . ? 
C18 C17 C16 120.0(7) . . ? 
C17 C18 C19 119.7(7) . . ? 
C18 C19 C20 118.2(7) . . ? 
N2 C20 C19 122.6(7) . . ? 
O1 C21 W1 175.0(5) . . ? 
O2 C22 W1 176.6(6) . . ? 
O3 C23 W1 173.4(6) . . ? 
O4 C24 W1 178.1(6) . . ? 
 
_refine_diff_density_max    3.068 
_refine_diff_density_min   -0.958 
_refine_diff_density_rms    0.189 
