 
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 Cr Fe N2 O4' 
_chemical_formula_weight          504.24 
_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' 
 'Cr'  'Cr'   0.3209   0.6236 
 '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                    12.779(3) 
_cell_length_b                    13.0204(15) 
_cell_length_c                    12.8041(13) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  94.119(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      2125.0(6) 
_cell_formula_units_Z             4 
_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           0.24 
_exptl_crystal_size_mid           0.18
_exptl_crystal_size_min           0.11
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.576 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1024 
_exptl_absorpt_coefficient_mu     1.228 
_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             7164 
_diffrn_reflns_av_R_equivalents   0.0507 
_diffrn_reflns_av_sigmaI/netI     0.0639 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          2.17 
_diffrn_reflns_theta_max          25.04 
_reflns_number_total              3223 
_reflns_number_observed           2676 
_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 0 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^)+(0.0480P)^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          3223 
_refine_ls_number_parameters      289 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0475 
_refine_ls_R_factor_obs           0.0396 
_refine_ls_wR_factor_all          0.0956 
_refine_ls_wR_factor_obs          0.0943 
_refine_ls_goodness_of_fit_all    1.016 
_refine_ls_goodness_of_fit_obs    1.110 
_refine_ls_restrained_S_all       1.015 
_refine_ls_restrained_S_obs       1.110 
_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 
Cr1 Cr 0.28432(4) 0.17716(3) 1.01530(4) 0.0209(2) Uani 1 d . . 
Fe1 Fe 0.21695(3) 0.58506(3) 0.95958(4) 0.0226(2) Uani 1 d . . 
N1 N 0.2012(2) 0.2898(2) 1.1027(2) 0.0173(6) Uani 1 d . . 
N2 N 0.1682(2) 0.0904(2) 1.0831(2) 0.0198(6) Uani 1 d . . 
O1 O 0.1624(2) 0.2025(2) 0.8035(2) 0.0387(6) Uani 1 d . . 
O2 O 0.4540(2) 0.3036(2) 0.9278(2) 0.0355(6) Uani 1 d . . 
O3 O 0.4488(2) 0.1617(2) 1.1989(2) 0.0482(7) Uani 1 d . . 
O4 O 0.3891(2) -0.0015(2) 0.9169(2) 0.0555(8) Uani 1 d . . 
C1 C 0.2077(3) 0.7417(3) 0.9483(4) 0.0535(12) Uani 1 d . . 
H1 H 0.2623(3) 0.7858(3) 0.9347(4) 0.064 Uiso 1 calc R . 
C2 C 0.1802(3) 0.7085(3) 1.0482(4) 0.0509(12) Uani 1 d . . 
H2 H 0.2141(3) 0.7273(3) 1.1121(4) 0.061 Uiso 1 calc R . 
C3 C 0.0940(3) 0.6430(2) 1.0350(3) 0.0351(9) Uani 1 d . . 
H3 H 0.0608(3) 0.6110(2) 1.0885(3) 0.042 Uiso 1 calc R . 
C4 C 0.0656(3) 0.6334(3) 0.9272(3) 0.0359(9) Uani 1 d . . 
H4 H 0.0107(3) 0.5941(3) 0.8970(3) 0.043 Uiso 1 calc R . 
C5 C 0.1357(3) 0.6945(3) 0.8729(3) 0.0451(10) Uani 1 d . . 
H5 H 0.1349(3) 0.7024(3) 0.8006(3) 0.054 Uiso 1 calc R . 
C6 C 0.3496(2) 0.5151(2) 1.0239(2) 0.0237(7) Uani 1 d . . 
H6 H 0.3889(2) 0.5362(2) 1.0840(2) 0.028 Uiso 1 calc R . 
C7 C 0.3643(3) 0.5472(2) 0.9204(3) 0.0270(8) Uani 1 d . . 
H7 H 0.4153(3) 0.5928(2) 0.9006(3) 0.032 Uiso 1 calc R . 
C8 C 0.2874(3) 0.4977(2) 0.8521(3) 0.0280(8) Uani 1 d . . 
H8 H 0.2798(3) 0.5051(2) 0.7797(3) 0.034 Uiso 1 calc R . 
C9 C 0.2244(3) 0.4351(2) 0.9133(2) 0.0230(7) Uani 1 d . . 
H9 H 0.1676(3) 0.3951(2) 0.8885(2) 0.028 Uiso 1 calc R . 
C10 C 0.2641(2) 0.4448(2) 1.0198(2) 0.0192(7) Uani 1 d . . 
C11 C 0.2206(2) 0.3926(2) 1.1103(2) 0.0196(7) Uani 1 d . . 
C12 C 0.1975(2) 0.4477(2) 1.1992(2) 0.0231(7) Uani 1 d . . 
H12 H 0.2162(2) 0.5166(2) 1.2053(2) 0.028 Uiso 1 calc R . 
C13 C 0.1474(2) 0.4008(2) 1.2779(2) 0.0232(7) Uani 1 d . . 
H13 H 0.1338(2) 0.4368(2) 1.3382(2) 0.028 Uiso 1 calc R . 
C14 C 0.1174(2) 0.2992(2) 1.2658(2) 0.0217(7) Uani 1 d . . 
H14 H 0.0799(2) 0.2667(2) 1.3159(2) 0.026 Uiso 1 calc R . 
C15 C 0.1445(2) 0.2467(2) 1.1772(2) 0.0185(7) Uani 1 d . . 
C16 C 0.1151(2) 0.1381(2) 1.1576(2) 0.0197(7) Uani 1 d . . 
C17 C 0.0367(2) 0.0883(2) 1.2084(2) 0.0228(7) Uani 1 d . . 
H17 H 0.0004(2) 0.1226(2) 1.2583(2) 0.027 Uiso 1 calc R . 
C18 C 0.0140(3) -0.0126(2) 1.1834(3) 0.0294(8) Uani 1 d . . 
H18 H -0.0373(3) -0.0474(2) 1.2173(3) 0.035 Uiso 1 calc R . 
C19 C 0.0670(3) -0.0616(2) 1.1083(3) 0.0259(7) Uani 1 d . . 
H19 H 0.0518(3) -0.1295(2) 1.0904(3) 0.031 Uiso 1 calc R . 
C20 C 0.1430(2) -0.0087(2) 1.0602(2) 0.0242(7) Uani 1 d . . 
H20 H 0.1789(2) -0.0423(2) 1.0096(2) 0.029 Uiso 1 calc R . 
C21 C 0.2035(3) 0.1936(2) 0.8864(3) 0.0258(8) Uani 1 d . . 
C22 C 0.3846(3) 0.2588(2) 0.9614(3) 0.0267(8) Uani 1 d . . 
C23 C 0.3832(3) 0.1658(2) 1.1343(3) 0.0263(8) Uani 1 d . . 
C24 C 0.3484(3) 0.0668(2) 0.9563(3) 0.0341(8) 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 
Cr1 C22 1.837(3) . ? 
Cr1 C24 1.842(3) . ? 
Cr1 C21 1.895(4) . ? 
Cr1 C23 1.914(4) . ? 
Cr1 N2 2.101(2) . ? 
Cr1 N1 2.169(2) . ? 
Fe1 C2 2.042(3) . ? 
Fe1 C7 2.043(3) . ? 
Fe1 C5 2.043(4) . ? 
Fe1 C8 2.044(3) . ? 
Fe1 C6 2.045(3) . ? 
Fe1 C9 2.045(3) . ? 
Fe1 C3 2.047(3) . ? 
Fe1 C1 2.047(3) . ? 
Fe1 C4 2.048(3) . ? 
Fe1 C10 2.056(3) . ? 
N1 C15 1.360(4) . ? 
N1 C11 1.363(4) . ? 
N2 C20 1.357(4) . ? 
N2 C16 1.360(4) . ? 
O1 C21 1.156(4) . ? 
O2 C22 1.169(4) . ? 
O3 C23 1.136(4) . ? 
O4 C24 1.163(4) . ? 
C1 C2 1.419(6) . ? 
C1 C5 1.424(6) . ? 
C2 C3 1.393(5) . ? 
C3 C4 1.408(5) . ? 
C4 C5 1.418(5) . ? 
C6 C7 1.415(4) . ? 
C6 C10 1.424(4) . ? 
C7 C8 1.422(5) . ? 
C8 C9 1.422(4) . ? 
C9 C10 1.426(4) . ? 
C10 C11 1.485(4) . ? 
C11 C12 1.395(4) . ? 
C12 C13 1.376(4) . ? 
C13 C14 1.383(4) . ? 
C14 C15 1.389(4) . ? 
C15 C16 1.481(4) . ? 
C16 C17 1.392(4) . ? 
C17 C18 1.379(4) . ? 
C18 C19 1.373(4) . ? 
C19 C20 1.372(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 
C22 Cr1 C24 87.37(14) . . ? 
C22 Cr1 C21 87.63(14) . . ? 
C24 Cr1 C21 87.77(15) . . ? 
C22 Cr1 C23 84.57(14) . . ? 
C24 Cr1 C23 88.78(15) . . ? 
C21 Cr1 C23 171.61(13) . . ? 
C22 Cr1 N2 176.78(11) . . ? 
C24 Cr1 N2 95.63(12) . . ? 
C21 Cr1 N2 93.65(12) . . ? 
C23 Cr1 N2 94.30(12) . . ? 
C22 Cr1 N1 100.57(11) . . ? 
C24 Cr1 N1 171.01(12) . . ? 
C21 Cr1 N1 96.69(11) . . ? 
C23 Cr1 N1 87.80(11) . . ? 
N2 Cr1 N1 76.35(9) . . ? 
C2 Fe1 C7 125.40(15) . . ? 
C2 Fe1 C5 68.0(2) . . ? 
C7 Fe1 C5 118.42(14) . . ? 
C2 Fe1 C8 160.5(2) . . ? 
C7 Fe1 C8 40.72(13) . . ? 
C5 Fe1 C8 104.69(15) . . ? 
C2 Fe1 C6 110.12(15) . . ? 
C7 Fe1 C6 40.49(12) . . ? 
C5 Fe1 C6 154.63(14) . . ? 
C8 Fe1 C6 68.33(13) . . ? 
C2 Fe1 C9 158.4(2) . . ? 
C7 Fe1 C9 68.65(13) . . ? 
C5 Fe1 C9 122.8(2) . . ? 
C8 Fe1 C9 40.70(12) . . ? 
C6 Fe1 C9 68.71(13) . . ? 
C2 Fe1 C3 39.84(15) . . ? 
C7 Fe1 C3 163.10(15) . . ? 
C5 Fe1 C3 67.80(14) . . ? 
C8 Fe1 C3 155.98(15) . . ? 
C6 Fe1 C3 128.04(13) . . ? 
C9 Fe1 C3 122.81(13) . . ? 
C2 Fe1 C1 40.6(2) . . ? 
C7 Fe1 C1 105.81(14) . . ? 
C5 Fe1 C1 40.7(2) . . ? 
C8 Fe1 C1 122.2(2) . . ? 
C6 Fe1 C1 120.9(2) . . ? 
C9 Fe1 C1 159.2(2) . . ? 
C3 Fe1 C1 67.90(14) . . ? 
C2 Fe1 C4 67.58(15) . . ? 
C7 Fe1 C4 153.91(14) . . ? 
C5 Fe1 C4 40.55(14) . . ? 
C8 Fe1 C4 119.37(14) . . ? 
C6 Fe1 C4 164.17(13) . . ? 
C9 Fe1 C4 107.33(14) . . ? 
C3 Fe1 C4 40.21(14) . . ? 
C1 Fe1 C4 68.32(15) . . ? 
C2 Fe1 C10 124.3(2) . . ? 
C7 Fe1 C10 68.12(12) . . ? 
C5 Fe1 C10 161.3(2) . . ? 
C8 Fe1 C10 68.10(12) . . ? 
C6 Fe1 C10 40.63(11) . . ? 
C9 Fe1 C10 40.70(12) . . ? 
C3 Fe1 C10 111.38(12) . . ? 
C1 Fe1 C10 157.7(2) . . ? 
C4 Fe1 C10 126.60(13) . . ? 
C15 N1 C11 117.3(2) . . ? 
C15 N1 Cr1 112.8(2) . . ? 
C11 N1 Cr1 127.4(2) . . ? 
C20 N2 C16 117.6(2) . . ? 
C20 N2 Cr1 125.9(2) . . ? 
C16 N2 Cr1 116.6(2) . . ? 
C2 C1 C5 106.9(3) . . ? 
C2 C1 Fe1 69.5(2) . . ? 
C5 C1 Fe1 69.5(2) . . ? 
C3 C2 C1 108.8(4) . . ? 
C3 C2 Fe1 70.3(2) . . ? 
C1 C2 Fe1 69.9(2) . . ? 
C2 C3 C4 108.6(3) . . ? 
C2 C3 Fe1 69.9(2) . . ? 
C4 C3 Fe1 69.9(2) . . ? 
C3 C4 C5 107.7(3) . . ? 
C3 C4 Fe1 69.8(2) . . ? 
C5 C4 Fe1 69.6(2) . . ? 
C4 C5 C1 108.0(4) . . ? 
C4 C5 Fe1 69.9(2) . . ? 
C1 C5 Fe1 69.8(2) . . ? 
C7 C6 C10 108.0(3) . . ? 
C7 C6 Fe1 69.7(2) . . ? 
C10 C6 Fe1 70.1(2) . . ? 
C6 C7 C8 108.1(3) . . ? 
C6 C7 Fe1 69.8(2) . . ? 
C8 C7 Fe1 69.7(2) . . ? 
C9 C8 C7 108.3(3) . . ? 
C9 C8 Fe1 69.7(2) . . ? 
C7 C8 Fe1 69.6(2) . . ? 
C8 C9 C10 107.4(3) . . ? 
C8 C9 Fe1 69.6(2) . . ? 
C10 C9 Fe1 70.1(2) . . ? 
C6 C10 C9 108.2(3) . . ? 
C6 C10 C11 126.5(3) . . ? 
C9 C10 C11 125.3(3) . . ? 
C6 C10 Fe1 69.3(2) . . ? 
C9 C10 Fe1 69.2(2) . . ? 
C11 C10 Fe1 125.7(2) . . ? 
N1 C11 C12 121.0(3) . . ? 
N1 C11 C10 118.0(2) . . ? 
C12 C11 C10 120.9(3) . . ? 
C13 C12 C11 120.4(3) . . ? 
C12 C13 C14 118.8(3) . . ? 
C13 C14 C15 118.6(3) . . ? 
N1 C15 C14 123.1(3) . . ? 
N1 C15 C16 114.6(2) . . ? 
C14 C15 C16 122.2(3) . . ? 
N2 C16 C17 121.8(3) . . ? 
N2 C16 C15 114.9(2) . . ? 
C17 C16 C15 123.2(3) . . ? 
C18 C17 C16 118.8(3) . . ? 
C19 C18 C17 120.0(3) . . ? 
C20 C19 C18 118.8(3) . . ? 
N2 C20 C19 123.1(3) . . ? 
O1 C21 Cr1 173.9(3) . . ? 
O2 C22 Cr1 174.3(3) . . ? 
O3 C23 Cr1 173.6(3) . . ? 
O4 C24 Cr1 178.4(3) . . ? 
 
_refine_diff_density_max    0.910 
_refine_diff_density_min   -0.446 
_refine_diff_density_rms    0.089 
