 
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 Mo N2 O4' 
_chemical_formula_weight          548.18 
_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' 
 'N'  'N'   0.0061   0.0033 
 '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' 
 '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)/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                    12.839(4) 
_cell_length_b                    12.9785(10) 
_cell_length_c                    12.9803(15) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  95.693(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      2152.2(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           0.2 
_exptl_crystal_size_mid           0.14
_exptl_crystal_size_min           0.06 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.692 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1096 
_exptl_absorpt_coefficient_mu     1.291 
_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             8753 
_diffrn_reflns_av_R_equivalents   0.0766 
_diffrn_reflns_av_sigmaI/netI     0.1964 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          2.13 
_diffrn_reflns_theta_max          25.04 
_reflns_number_total              3221 
_reflns_number_observed           2076 
_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 6 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^)+(0.0096P)^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          3215 
_refine_ls_number_parameters      289 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0751 
_refine_ls_R_factor_obs           0.0409 
_refine_ls_wR_factor_all          0.0872 
_refine_ls_wR_factor_obs          0.0772 
_refine_ls_goodness_of_fit_all    0.760 
_refine_ls_goodness_of_fit_obs    0.924 
_refine_ls_restrained_S_all       0.844 
_refine_ls_restrained_S_obs       0.924 
_refine_ls_shift/esd_max          0.003 
_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 
Mo1 Mo -0.01212(4) 0.32904(4) 0.71349(4) 0.0213(2) Uani 1 d . . 
Fe1 Fe 0.04116(7) 0.91756(6) 0.78484(7) 0.0230(2) Uani 1 d . . 
N1 N -0.0852(3) 0.4147(3) 0.8382(3) 0.0200(11) Uani 1 d . . 
N2 N -0.1027(3) 0.2113(3) 0.8020(4) 0.0181(11) Uani 1 d . . 
O1 O -0.2092(4) 0.3413(3) 0.5464(4) 0.0503(13) Uani 1 d . . 
O2 O 0.0805(4) 0.5209(3) 0.6109(4) 0.058(2) Uani 1 d . . 
O3 O 0.0740(3) 0.1965(3) 0.5414(3) 0.0376(12) Uani 1 d . . 
O4 O 0.2094(4) 0.2977(3) 0.8370(4) 0.0386(12) Uani 1 d . . 
C1 C 0.0856(4) 1.0682(4) 0.7770(5) 0.0242(15) Uani 1 d . . 
H1 H 0.1111(4) 1.1089(4) 0.8328(5) 0.029 Uiso 1 calc R . 
C2 C 0.1464(5) 1.0065(4) 0.7159(5) 0.0254(15) Uani 1 d . . 
H2 H 0.2188(5) 0.9992(4) 0.7240(5) 0.030 Uiso 1 calc R . 
C3 C 0.0752(5) 0.9571(4) 0.6391(5) 0.026(2) Uani 1 d . . 
H3 H 0.0942(5) 0.9131(4) 0.5876(5) 0.031 Uiso 1 calc R . 
C4 C -0.0270(4) 0.9857(4) 0.6538(5) 0.0234(15) Uani 1 d . . 
H4 H -0.0875(4) 0.9624(4) 0.6156(5) 0.028 Uiso 1 calc R . 
C5 C -0.0224(4) 1.0568(4) 0.7376(4) 0.0208(15) Uani 1 d . . 
C6 C -0.0427(6) 0.7926(5) 0.8220(6) 0.048(2) Uani 1 d . . 
H6 H -0.1068(6) 0.7722(5) 0.7885(6) 0.057 Uiso 1 calc R . 
C7 C 0.0549(6) 0.7596(4) 0.7948(5) 0.044(2) Uani 1 d . . 
H7 H 0.0676(6) 0.7147(4) 0.7416(5) 0.052 Uiso 1 calc R . 
C8 C 0.1315(6) 0.8101(5) 0.8667(5) 0.044(2) Uani 1 d . . 
H8 H 0.2038(6) 0.8039(5) 0.8680(5) 0.052 Uiso 1 calc R . 
C9 C 0.0777(5) 0.8704(4) 0.9345(5) 0.033(2) Uani 1 d . . 
H9 H 0.1086(5) 0.9102(4) 0.9888(5) 0.039 Uiso 1 calc R . 
C10 C -0.0310(5) 0.8602(4) 0.9063(5) 0.034(2) Uani 1 d . . 
H10 H -0.0844(5) 0.8922(4) 0.9377(5) 0.041 Uiso 1 calc R . 
C11 C -0.0643(4) 0.5140(4) 0.8650(4) 0.0212(15) Uani 1 d . . 
H11 H -0.0150(4) 0.5497(4) 0.8311(4) 0.025 Uiso 1 calc R . 
C12 C -0.1126(4) 0.5638(4) 0.9398(4) 0.0241(15) Uani 1 d . . 
H12 H -0.0966(4) 0.6322(4) 0.9560(4) 0.029 Uiso 1 calc R . 
C13 C -0.1861(5) 0.5111(4) 0.9917(5) 0.029(2) Uani 1 d . . 
H13 H -0.2202(5) 0.5438(4) 1.0425(5) 0.035 Uiso 1 calc R . 
C14 C -0.2074(4) 0.4096(4) 0.9665(4) 0.0234(15) Uani 1 d . . 
H14 H -0.2547(4) 0.3721(4) 1.0014(4) 0.028 Uiso 1 calc R . 
C15 C -0.1573(4) 0.3646(4) 0.8885(5) 0.0199(14) Uani 1 d . . 
C16 C -0.1768(4) 0.2552(4) 0.8567(4) 0.0192(14) Uani 1 d . . 
C17 C -0.2657(4) 0.2031(4) 0.8812(4) 0.0212(14) Uani 1 d . . 
H17 H -0.3151(4) 0.2352(4) 0.9181(4) 0.025 Uiso 1 calc R . 
C18 C -0.2787(4) 0.1001(4) 0.8483(4) 0.0245(15) Uani 1 d . . 
H18 H -0.3399(4) 0.0646(4) 0.8580(4) 0.029 Uiso 1 calc R . 
C19 C -0.1998(4) 0.0527(4) 0.8016(4) 0.0216(14) Uani 1 d . . 
H19 H -0.2055(4) -0.0166(4) 0.7837(4) 0.026 Uiso 1 calc R . 
C20 C -0.1117(4) 0.1085(4) 0.7813(4) 0.0202(14) Uani 1 d . . 
C21 C -0.1430(5) 0.3393(4) 0.6091(5) 0.0240(14) Uani 1 d . . 
C22 C 0.0460(5) 0.4485(5) 0.6460(5) 0.029(2) Uani 1 d . . 
C23 C 0.0427(4) 0.2441(4) 0.6069(5) 0.0241(15) Uani 1 d . . 
C24 C 0.1271(5) 0.3108(4) 0.7994(5) 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 
Mo1 C23 1.954(6) . ? 
Mo1 C22 1.964(6) . ? 
Mo1 C24 2.025(6) . ? 
Mo1 C21 2.056(7) . ? 
Mo1 N1 2.244(4) . ? 
Mo1 N2 2.295(4) . ? 
Fe1 C6 2.031(6) . ? 
Fe1 C4 2.036(6) . ? 
Fe1 C8 2.043(6) . ? 
Fe1 C1 2.042(5) . ? 
Fe1 C9 2.047(6) . ? 
Fe1 C10 2.047(6) . ? 
Fe1 C3 2.049(6) . ? 
Fe1 C2 2.049(5) . ? 
Fe1 C5 2.052(5) . ? 
Fe1 C7 2.060(6) . ? 
N1 C15 1.352(6) . ? 
N1 C11 1.354(6) . ? 
N2 C20 1.364(6) . ? 
N2 C16 1.367(6) . ? 
O1 C21 1.116(7) . ? 
O2 C22 1.153(6) . ? 
O3 C23 1.155(6) . ? 
O4 C24 1.131(6) . ? 
C1 C2 1.416(7) . ? 
C1 C5 1.437(8) . ? 
C2 C3 1.435(8) . ? 
C3 C4 1.395(7) . ? 
C4 C5 1.423(7) . ? 
C5 C20 1.488(7) 1_565 ? 
C6 C10 1.399(9) . ? 
C6 C7 1.402(9) . ? 
C7 C8 1.444(9) . ? 
C8 C9 1.409(8) . ? 
C9 C10 1.413(8) . ? 
C11 C12 1.366(7) . ? 
C12 C13 1.391(7) . ? 
C13 C14 1.378(7) . ? 
C14 C15 1.382(7) . ? 
C15 C16 1.492(7) . ? 
C16 C17 1.391(7) . ? 
C17 C18 1.407(7) . ? 
C18 C19 1.376(7) . ? 
C19 C20 1.391(7) . ? 
C20 C5 1.488(7) 1_545 ? 
 
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 
C23 Mo1 C22 87.1(2) . . ? 
C23 Mo1 C24 87.9(2) . . ? 
C22 Mo1 C24 89.1(2) . . ? 
C23 Mo1 C21 84.1(2) . . ? 
C22 Mo1 C21 88.7(2) . . ? 
C24 Mo1 C21 171.8(2) . . ? 
C23 Mo1 N1 174.8(2) . . ? 
C22 Mo1 N1 97.7(2) . . ? 
C24 Mo1 N1 94.0(2) . . ? 
C21 Mo1 N1 94.0(2) . . ? 
C23 Mo1 N2 102.4(2) . . ? 
C22 Mo1 N2 169.1(2) . . ? 
C24 Mo1 N2 96.3(2) . . ? 
C21 Mo1 N2 87.2(2) . . ? 
N1 Mo1 N2 72.6(2) . . ? 
C6 Fe1 C4 110.6(3) . . ? 
C6 Fe1 C8 67.6(3) . . ? 
C4 Fe1 C8 154.9(2) . . ? 
C6 Fe1 C1 159.0(3) . . ? 
C4 Fe1 C1 69.0(2) . . ? 
C8 Fe1 C1 122.2(3) . . ? 
C6 Fe1 C9 67.2(3) . . ? 
C4 Fe1 C9 164.2(2) . . ? 
C8 Fe1 C9 40.3(2) . . ? 
C1 Fe1 C9 107.2(2) . . ? 
C6 Fe1 C10 40.1(2) . . ? 
C4 Fe1 C10 127.7(2) . . ? 
C8 Fe1 C10 68.2(3) . . ? 
C1 Fe1 C10 122.5(2) . . ? 
C9 Fe1 C10 40.4(2) . . ? 
C6 Fe1 C3 125.9(3) . . ? 
C4 Fe1 C3 39.9(2) . . ? 
C8 Fe1 C3 119.3(2) . . ? 
C1 Fe1 C3 68.1(2) . . ? 
C9 Fe1 C3 154.4(3) . . ? 
C10 Fe1 C3 163.1(3) . . ? 
C6 Fe1 C2 160.3(3) . . ? 
C4 Fe1 C2 68.8(2) . . ? 
C8 Fe1 C2 104.3(3) . . ? 
C1 Fe1 C2 40.5(2) . . ? 
C9 Fe1 C2 119.0(3) . . ? 
C10 Fe1 C2 155.5(3) . . ? 
C3 Fe1 C2 41.0(2) . . ? 
C6 Fe1 C5 124.7(3) . . ? 
C4 Fe1 C5 40.7(2) . . ? 
C8 Fe1 C5 161.0(3) . . ? 
C1 Fe1 C5 41.1(2) . . ? 
C9 Fe1 C5 126.5(2) . . ? 
C10 Fe1 C5 110.7(2) . . ? 
C3 Fe1 C5 67.5(2) . . ? 
C2 Fe1 C5 68.5(2) . . ? 
C6 Fe1 C7 40.1(2) . . ? 
C4 Fe1 C7 120.8(3) . . ? 
C8 Fe1 C7 41.2(2) . . ? 
C1 Fe1 C7 158.9(3) . . ? 
C9 Fe1 C7 68.5(2) . . ? 
C10 Fe1 C7 68.4(2) . . ? 
C3 Fe1 C7 106.4(2) . . ? 
C2 Fe1 C7 122.1(3) . . ? 
C5 Fe1 C7 157.5(3) . . ? 
C15 N1 C11 117.5(5) . . ? 
C15 N1 Mo1 117.7(3) . . ? 
C11 N1 Mo1 124.8(4) . . ? 
C20 N2 C16 117.4(5) . . ? 
C20 N2 Mo1 126.2(4) . . ? 
C16 N2 Mo1 113.3(3) . . ? 
C2 C1 C5 108.0(5) . . ? 
C2 C1 Fe1 70.0(3) . . ? 
C5 C1 Fe1 69.8(3) . . ? 
C1 C2 C3 107.1(5) . . ? 
C1 C2 Fe1 69.5(3) . . ? 
C3 C2 Fe1 69.5(3) . . ? 
C4 C3 C2 109.2(5) . . ? 
C4 C3 Fe1 69.5(3) . . ? 
C2 C3 Fe1 69.5(3) . . ? 
C3 C4 C5 108.0(5) . . ? 
C3 C4 Fe1 70.5(3) . . ? 
C5 C4 Fe1 70.2(3) . . ? 
C4 C5 C1 107.7(5) . . ? 
C4 C5 C20 127.5(5) . 1_565 ? 
C1 C5 C20 124.8(5) . 1_565 ? 
C4 C5 Fe1 69.1(3) . . ? 
C1 C5 Fe1 69.1(3) . . ? 
C20 C5 Fe1 125.6(4) 1_565 . ? 
C10 C6 C7 111.1(7) . . ? 
C10 C6 Fe1 70.5(3) . . ? 
C7 C6 Fe1 71.1(4) . . ? 
C6 C7 C8 105.5(6) . . ? 
C6 C7 Fe1 68.9(3) . . ? 
C8 C7 Fe1 68.8(3) . . ? 
C9 C8 C7 108.1(6) . . ? 
C9 C8 Fe1 70.0(3) . . ? 
C7 C8 Fe1 70.0(4) . . ? 
C8 C9 C10 108.6(6) . . ? 
C8 C9 Fe1 69.7(4) . . ? 
C10 C9 Fe1 69.8(4) . . ? 
C6 C10 C9 106.7(6) . . ? 
C6 C10 Fe1 69.3(4) . . ? 
C9 C10 Fe1 69.8(3) . . ? 
N1 C11 C12 122.7(5) . . ? 
C11 C12 C13 119.3(5) . . ? 
C14 C13 C12 118.9(5) . . ? 
C13 C14 C15 118.8(5) . . ? 
N1 C15 C14 122.8(5) . . ? 
N1 C15 C16 115.4(5) . . ? 
C14 C15 C16 121.8(5) . . ? 
N2 C16 C17 123.1(5) . . ? 
N2 C16 C15 115.7(5) . . ? 
C17 C16 C15 121.3(5) . . ? 
C16 C17 C18 117.9(5) . . ? 
C19 C18 C17 119.2(5) . . ? 
C18 C19 C20 120.0(5) . . ? 
N2 C20 C19 121.8(5) . . ? 
N2 C20 C5 117.6(5) . 1_545 ? 
C19 C20 C5 120.7(5) . 1_545 ? 
O1 C21 Mo1 174.1(5) . . ? 
O2 C22 Mo1 176.8(6) . . ? 
O3 C23 Mo1 177.7(5) . . ? 
O4 C24 Mo1 172.1(6) . . ? 
 
_refine_diff_density_max    0.778 
_refine_diff_density_min   -0.412 
_refine_diff_density_rms    0.109 
