data_s94
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. I. Butler
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C24 H14 Br2 Fe O2'
_chemical_formula_weight          550.02
 
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'
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    Pc
_symmetry_space_group_name_hall   'P 2yc'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 'x, -y, z+1/2'
 
_cell_length_a                    15.9575(4)
_cell_length_b                    8.8522(2)
_cell_length_c                    13.7492(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  101.9050(10)
_cell_angle_gamma                 90.00
_cell_volume                      1900.42(8)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     4486
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Plate
_exptl_crystal_colour             'Dark Grey'
_exptl_crystal_size_max           0.26
_exptl_crystal_size_mid           0.12
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.922
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1080
_exptl_absorpt_coefficient_mu     5.018
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.3553
_exptl_absorpt_correction_T_max   0.9515
_exptl_absorpt_process_details    'SORTAV Blessing (1997)'
_exptl_special_details
;
 PLEASE NOTE cell_measurement_ fields are not relevant to area detector data,
 the entire data set is used to refine the cell, which is indexed from all
 observed reflections in a 10 degree phi range.
;
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'φ and ω scans to fill Ewald Sphere'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             24120
_diffrn_reflns_av_R_equivalents   0.0935
_diffrn_reflns_av_sigmaI/netI     0.0774
_diffrn_reflns_limit_h_min        -20
_diffrn_reflns_limit_h_max        19
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          2.91
_diffrn_reflns_theta_max          27.48
_reflns_number_total              7305
_reflns_number_gt                 6547
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection
' DENZO (Otwinowski and Minor, 1997)'
_computing_cell_refinement        
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_reduction         
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'PLATON (Spek, 1990)'
_computing_publication_material   ? 
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) 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
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0369P)²+3.5410P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0017(3)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    -0.014(11)
_refine_ls_number_reflns          7305
_refine_ls_number_parameters      524
_refine_ls_number_restraints      2
_refine_ls_R_factor_all           0.0538
_refine_ls_R_factor_gt            0.0445
_refine_ls_wR_factor_ref          0.1057
_refine_ls_wR_factor_gt           0.0999
_refine_ls_goodness_of_fit_ref    1.033
_refine_ls_restrained_S_all       1.033
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_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_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.9993(5) 0.0864(7) 0.0434(5) 0.0229(14) Uani 1 1 d . . .
C2 C 1.0584(4) -0.0042(7) 0.0004(5) 0.0199(14) Uani 1 1 d . . .
H2 H 1.1192 0.0012 0.0154 0.024 Uiso 1 1 calc R . .
C3 C 1.0062(5) -0.1034(7) -0.0693(5) 0.0237(15) Uani 1 1 d . . .
H3 H 1.0267 -0.1753 -0.1101 0.028 Uiso 1 1 calc R . .
C4 C 0.9182(5) -0.0766(8) -0.0674(5) 0.0257(15) Uani 1 1 d . . .
H4 H 0.8706 -0.1284 -0.1059 0.031 Uiso 1 1 calc R . .
C5 C 0.9143(4) 0.0420(7) 0.0024(5) 0.0219(14) Uani 1 1 d . . .
H5 H 0.8638 0.0832 0.0183 0.026 Uiso 1 1 calc R . .
C6 C 0.9103(4) -0.2431(7) 0.1558(4) 0.0172(13) Uani 1 1 d . . .
C7 C 0.9767(4) -0.1536(7) 0.2176(5) 0.0202(14) Uani 1 1 d . . .
H7 H 0.9681 -0.0736 0.2606 0.024 Uiso 1 1 calc R . .
C8 C 1.0560(4) -0.2060(8) 0.2028(5) 0.0222(14) Uani 1 1 d . . .
H8 H 1.1103 -0.1665 0.2337 0.027 Uiso 1 1 calc R . .
C9 C 1.0420(5) -0.3263(8) 0.1349(5) 0.0220(14) Uani 1 1 d . . .
H9 H 1.0855 -0.3817 0.1127 0.026 Uiso 1 1 calc R . .
C10 C 0.9537(5) -0.3516(7) 0.1051(5) 0.0201(14) Uani 1 1 d . . .
H10 H 0.9272 -0.4268 0.0596 0.024 Uiso 1 1 calc R . .
C11 C 0.8173(4) -0.2236(7) 0.1415(4) 0.0172(13) Uani 1 1 d . . .
C12 C 0.7805(4) -0.1305(7) 0.2046(5) 0.0211(14) Uani 1 1 d . . .
H12 H 0.8167 -0.0772 0.2569 0.025 Uiso 1 1 calc R . .
C13 C 0.6937(4) -0.1156(7) 0.1918(5) 0.0186(13) Uani 1 1 d . . .
C14 C 0.6569(4) -0.0172(7) 0.2611(5) 0.0204(14) Uani 1 1 d . . .
C15 C 0.5622(4) -0.0065(7) 0.2481(5) 0.0195(14) Uani 1 1 d . . .
C16 C 0.5268(5) 0.0831(8) 0.3120(5) 0.0228(14) Uani 1 1 d . . .
H16 H 0.5631 0.1364 0.3643 0.027 Uiso 1 1 calc R . .
C17 C 0.4381(4) 0.0948(7) 0.2996(5) 0.0221(14) Uani 1 1 d . . .
H17 H 0.4138 0.1572 0.3428 0.026 Uiso 1 1 calc R . .
C18 C 0.3850(5) 0.0144(7) 0.2232(5) 0.0191(14) Uani 1 1 d . . .
C19 C 0.4199(5) -0.0767(8) 0.1592(5) 0.0228(14) Uani 1 1 d . . .
H19 H 0.3836 -0.1310 0.1075 0.027 Uiso 1 1 calc R . .
C20 C 0.5077(4) -0.0874(7) 0.1716(4) 0.0182(13) Uani 1 1 d . . .
C21 C 0.5447(4) -0.1812(8) 0.0999(5) 0.0210(14) Uani 1 1 d . . .
C22 C 0.6377(4) -0.1945(7) 0.1145(5) 0.0189(13) Uani 1 1 d . . .
C23 C 0.6739(4) -0.2873(7) 0.0517(5) 0.0192(14) Uani 1 1 d . . .
H23 H 0.6379 -0.3425 0.0002 0.023 Uiso 1 1 calc R . .
C24 C 0.7618(4) -0.2988(7) 0.0645(5) 0.0178(13) Uani 1 1 d . . .
H24 H 0.7853 -0.3595 0.0198 0.021 Uiso 1 1 calc R . .
O1 O 0.7043(4) 0.0553(7) 0.3266(4) 0.0403(14) Uani 1 1 d . . .
O2 O 0.4963(3) -0.2408(6) 0.0290(4) 0.0297(12) Uani 1 1 d . . .
Fe1 Fe 0.98376(6) -0.13528(10) 0.07172(6) 0.0166(2) Uani 1 1 d . . .
Br1 Br 1.03531(5) 0.23609(8) 0.14040(5) 0.03125(19) Uani 1 1 d . . .
Br2 Br 0.26510(4) 0.03441(8) 0.20592(5) 0.02508(17) Uani 1 1 d . . .
C31 C 0.2802(5) -0.4097(8) -0.1323(5) 0.0240(15) Uani 1 1 d . . .
C32 C 0.2237(4) -0.5008(7) -0.2038(5) 0.0195(13) Uani 1 1 d . . .
H32 H 0.1630 -0.4945 -0.2209 0.023 Uiso 1 1 calc R . .
C33 C 0.2772(5) -0.6028(8) -0.2442(5) 0.0249(15) Uani 1 1 d . . .
H33 H 0.2578 -0.6781 -0.2929 0.030 Uiso 1 1 calc R . .
C34 C 0.3640(5) -0.5727(8) -0.1994(5) 0.0263(15) Uani 1 1 d . . .
H34 H 0.4124 -0.6229 -0.2142 0.032 Uiso 1 1 calc R . .
C35 C 0.3664(4) -0.4538(7) -0.1279(5) 0.0242(14) Uani 1 1 d . . .
H35 H 0.4160 -0.4128 -0.0858 0.029 Uiso 1 1 calc R . .
C36 C 0.3710(4) -0.7389(7) 0.0261(4) 0.0158(12) Uani 1 1 d . . .
C37 C 0.3052(5) -0.6481(8) 0.0568(5) 0.0229(15) Uani 1 1 d . . .
H37 H 0.3149 -0.5673 0.1033 0.027 Uiso 1 1 calc R . .
C38 C 0.2249(4) -0.6996(8) 0.0064(5) 0.0214(14) Uani 1 1 d . . .
H38 H 0.1710 -0.6601 0.0132 0.026 Uiso 1 1 calc R . .
C39 C 0.2374(5) -0.8191(8) -0.0558(5) 0.0229(14) Uani 1 1 d . . .
H39 H 0.1932 -0.8728 -0.0990 0.028 Uiso 1 1 calc R . .
C40 C 0.3269(4) -0.8473(7) -0.0440(5) 0.0199(14) Uani 1 1 d . . .
H40 H 0.3527 -0.9238 -0.0765 0.024 Uiso 1 1 calc R . .
C41 C 0.4635(4) -0.7203(7) 0.0560(4) 0.0181(13) Uani 1 1 d . . .
C42 C 0.5004(4) -0.6294(7) 0.1370(4) 0.0176(13) Uani 1 1 d . . .
H42 H 0.4640 -0.5767 0.1721 0.021 Uiso 1 1 calc R . .
C43 C 0.5881(4) -0.6141(7) 0.1673(4) 0.0196(13) Uani 1 1 d . . .
C44 C 0.6248(5) -0.5146(7) 0.2531(5) 0.0214(14) Uani 1 1 d . . .
C45 C 0.7187(4) -0.5067(8) 0.2855(5) 0.0191(14) Uani 1 1 d . . .
C46 C 0.7556(4) -0.4163(8) 0.3665(5) 0.0223(14) Uani 1 1 d . . .
H46 H 0.7195 -0.3614 0.4008 0.027 Uiso 1 1 calc R . .
C47 C 0.8442(4) -0.4053(7) 0.3979(5) 0.0201(14) Uani 1 1 d . . .
H47 H 0.8687 -0.3432 0.4527 0.024 Uiso 1 1 calc R . .
C48 C 0.8964(5) -0.4883(7) 0.3463(5) 0.0202(15) Uani 1 1 d . . .
C49 C 0.8613(4) -0.5770(8) 0.2663(5) 0.0206(14) Uani 1 1 d . . .
H49 H 0.8976 -0.6318 0.2322 0.025 Uiso 1 1 calc R . .
C50 C 0.7730(4) -0.5870(7) 0.2351(4) 0.0178(13) Uani 1 1 d . . .
C51 C 0.7364(5) -0.6821(8) 0.1459(5) 0.0235(14) Uani 1 1 d . . .
C52 C 0.6429(4) -0.6934(7) 0.1167(5) 0.0186(13) Uani 1 1 d . . .
C53 C 0.6071(5) -0.7853(8) 0.0361(5) 0.0208(14) Uani 1 1 d . . .
H53 H 0.6437 -0.8394 0.0020 0.025 Uiso 1 1 calc R . .
C54 C 0.5188(5) -0.7990(8) 0.0051(5) 0.0232(15) Uani 1 1 d . . .
H54 H 0.4955 -0.8612 -0.0502 0.028 Uiso 1 1 calc R . .
O31 O 0.5777(3) -0.4414(7) 0.2948(4) 0.0380(14) Uani 1 1 d . . .
O32 O 0.7843(3) -0.7436(6) 0.0989(4) 0.0302(12) Uani 1 1 d . . .
Fe31 Fe 0.29660(6) -0.63078(10) -0.09322(6) 0.0175(2) Uani 1 1 d . . .
Br31 Br 0.24097(5) -0.25949(8) -0.05499(6) 0.03266(19) Uani 1 1 d . . .
Br32 Br 1.01607(4) -0.47106(8) 0.38638(5) 0.02391(16) Uani 1 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
C1 C5 1.413(10) . ?
C1 C2 1.453(9) . ?
C1 Br1 1.884(7) . ?
C1 Fe1 2.026(7) . ?
C2 C3 1.434(10) . ?
C2 Fe1 2.052(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.429(10) . ?
C3 Fe1 2.063(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.433(10) . ?
C4 Fe1 2.049(7) . ?
C4 H4 0.9500 . ?
C5 Fe1 2.041(6) . ?
C5 H5 0.9500 . ?
C6 C10 1.445(9) . ?
C6 C7 1.451(9) . ?
C6 C11 1.466(9) . ?
C6 Fe1 2.044(6) . ?
C7 C8 1.401(10) . ?
C7 Fe1 2.039(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.404(10) . ?
C8 Fe1 2.028(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.403(10) . ?
C9 Fe1 2.036(7) . ?
C9 H9 0.9500 . ?
C10 Fe1 2.049(6) . ?
C10 H10 0.9500 . ?
C11 C24 1.401(9) . ?
C11 C12 1.409(9) . ?
C12 C13 1.367(10) . ?
C12 H12 0.9500 . ?
C13 C22 1.422(9) . ?
C13 C14 1.498(9) . ?
C14 O1 1.230(9) . ?
C14 C15 1.486(9) . ?
C15 C16 1.388(9) . ?
C15 C20 1.414(9) . ?
C16 C17 1.394(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.401(10) . ?
C17 H17 0.9500 . ?
C18 C19 1.392(9) . ?
C18 Br2 1.887(7) . ?
C19 C20 1.379(10) . ?
C19 H19 0.9500 . ?
C20 C21 1.500(9) . ?
C21 O2 1.232(8) . ?
C21 C22 1.460(9) . ?
C22 C23 1.399(9) . ?
C23 C24 1.381(9) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C31 C35 1.419(10) . ?
C31 C32 1.436(10) . ?
C31 Br31 1.888(7) . ?
C31 Fe31 2.032(7) . ?
C32 C33 1.431(10) . ?
C32 Fe31 2.064(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.421(10) . ?
C33 Fe31 2.050(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.435(10) . ?
C34 Fe31 2.049(7) . ?
C34 H34 0.9500 . ?
C35 Fe31 2.035(7) . ?
C35 H35 0.9500 . ?
C36 C40 1.437(9) . ?
C36 C37 1.452(9) . ?
C36 C41 1.457(9) . ?
C36 Fe31 2.053(6) . ?
C37 C38 1.401(10) . ?
C37 Fe31 2.045(6) . ?
C37 H37 0.9500 . ?
C38 C39 1.399(10) . ?
C38 Fe31 2.050(6) . ?
C38 H38 0.9500 . ?
C39 C40 1.427(10) . ?
C39 Fe31 2.034(7) . ?
C39 H39 0.9500 . ?
C40 Fe31 2.057(6) . ?
C40 H40 0.9500 . ?
C41 C42 1.402(9) . ?
C41 C54 1.417(9) . ?
C42 C43 1.383(9) . ?
C42 H42 0.9500 . ?
C43 C52 1.411(9) . ?
C43 C44 1.492(8) . ?
C44 O31 1.222(8) . ?
C44 C45 1.474(9) . ?
C45 C46 1.399(9) . ?
C45 C50 1.408(9) . ?
C46 C47 1.394(10) . ?
C46 H46 0.9500 . ?
C47 C48 1.408(9) . ?
C47 H47 0.9500 . ?
C48 C49 1.373(10) . ?
C48 Br32 1.881(7) . ?
C49 C50 1.388(9) . ?
C49 H49 0.9500 . ?
C50 C51 1.503(9) . ?
C51 O32 1.225(8) . ?
C51 C52 1.467(10) . ?
C52 C53 1.398(9) . ?
C53 C54 1.391(10) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
 
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
C5 C1 C2 109.6(6) . . ?
C5 C1 Br1 127.2(5) . . ?
C2 C1 Br1 123.2(5) . . ?
C5 C1 Fe1 70.2(4) . . ?
C2 C1 Fe1 70.1(4) . . ?
Br1 C1 Fe1 125.2(3) . . ?
C3 C2 C1 105.9(6) . . ?
C3 C2 Fe1 70.0(4) . . ?
C1 C2 Fe1 68.2(3) . . ?
C3 C2 H2 127.1 . . ?
C1 C2 H2 127.1 . . ?
Fe1 C2 H2 126.3 . . ?
C4 C3 C2 108.9(6) . . ?
C4 C3 Fe1 69.1(4) . . ?
C2 C3 Fe1 69.2(3) . . ?
C4 C3 H3 125.6 . . ?
C2 C3 H3 125.6 . . ?
Fe1 C3 H3 127.7 . . ?
C3 C4 C5 108.3(6) . . ?
C3 C4 Fe1 70.2(4) . . ?
C5 C4 Fe1 69.2(4) . . ?
C3 C4 H4 125.9 . . ?
C5 C4 H4 125.9 . . ?
Fe1 C4 H4 126.3 . . ?
C1 C5 C4 107.4(6) . . ?
C1 C5 Fe1 69.1(4) . . ?
C4 C5 Fe1 69.8(4) . . ?
C1 C5 H5 126.3 . . ?
C4 C5 H5 126.3 . . ?
Fe1 C5 H5 126.4 . . ?
C10 C6 C7 106.3(6) . . ?
C10 C6 C11 125.9(6) . . ?
C7 C6 C11 127.7(6) . . ?
C10 C6 Fe1 69.5(3) . . ?
C7 C6 Fe1 69.0(3) . . ?
C11 C6 Fe1 123.5(4) . . ?
C8 C7 C6 107.9(6) . . ?
C8 C7 Fe1 69.4(4) . . ?
C6 C7 Fe1 69.4(3) . . ?
C8 C7 H7 126.1 . . ?
C6 C7 H7 126.1 . . ?
Fe1 C7 H7 126.7 . . ?
C7 C8 C9 108.9(6) . . ?
C7 C8 Fe1 70.3(4) . . ?
C9 C8 Fe1 70.1(4) . . ?
C7 C8 H8 125.5 . . ?
C9 C8 H8 125.5 . . ?
Fe1 C8 H8 125.7 . . ?
C10 C9 C8 109.1(6) . . ?
C10 C9 Fe1 70.4(4) . . ?
C8 C9 Fe1 69.5(4) . . ?
C10 C9 H9 125.4 . . ?
C8 C9 H9 125.4 . . ?
Fe1 C9 H9 126.3 . . ?
C9 C10 C6 107.8(6) . . ?
C9 C10 Fe1 69.4(4) . . ?
C6 C10 Fe1 69.1(3) . . ?
C9 C10 H10 126.1 . . ?
C6 C10 H10 126.1 . . ?
Fe1 C10 H10 126.9 . . ?
C24 C11 C12 117.7(6) . . ?
C24 C11 C6 120.7(6) . . ?
C12 C11 C6 121.7(6) . . ?
C13 C12 C11 121.2(6) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C12 C13 C22 120.8(6) . . ?
C12 C13 C14 119.7(6) . . ?
C22 C13 C14 119.5(6) . . ?
O1 C14 C15 120.8(6) . . ?
O1 C14 C13 120.4(6) . . ?
C15 C14 C13 118.8(6) . . ?
C16 C15 C20 119.5(6) . . ?
C16 C15 C14 119.7(6) . . ?
C20 C15 C14 120.8(6) . . ?
C15 C16 C17 120.0(6) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C18 119.7(6) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C19 C18 C17 120.6(7) . . ?
C19 C18 Br2 120.2(5) . . ?
C17 C18 Br2 119.2(5) . . ?
C20 C19 C18 119.4(6) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C19 C20 C15 120.7(6) . . ?
C19 C20 C21 119.0(6) . . ?
C15 C20 C21 120.2(6) . . ?
O2 C21 C22 121.9(6) . . ?
O2 C21 C20 119.3(6) . . ?
C22 C21 C20 118.8(6) . . ?
C23 C22 C13 118.3(6) . . ?
C23 C22 C21 120.0(6) . . ?
C13 C22 C21 121.8(6) . . ?
C24 C23 C22 120.1(6) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C11 121.9(6) . . ?
C23 C24 H24 119.0 . . ?
C11 C24 H24 119.0 . . ?
C1 Fe1 C8 113.6(3) . . ?
C1 Fe1 C9 145.4(3) . . ?
C8 Fe1 C9 40.4(3) . . ?
C1 Fe1 C7 107.5(3) . . ?
C8 Fe1 C7 40.3(3) . . ?
C9 Fe1 C7 68.1(3) . . ?
C1 Fe1 C5 40.7(3) . . ?
C8 Fe1 C5 143.8(3) . . ?
C9 Fe1 C5 173.9(3) . . ?
C7 Fe1 C5 112.7(3) . . ?
C1 Fe1 C6 131.9(3) . . ?
C8 Fe1 C6 68.9(3) . . ?
C9 Fe1 C6 68.6(3) . . ?
C7 Fe1 C6 41.6(3) . . ?
C5 Fe1 C6 107.7(3) . . ?
C1 Fe1 C4 68.5(3) . . ?
C8 Fe1 C4 174.4(3) . . ?
C9 Fe1 C4 135.2(3) . . ?
C7 Fe1 C4 144.9(3) . . ?
C5 Fe1 C4 41.0(3) . . ?
C6 Fe1 C4 113.9(3) . . ?
C1 Fe1 C10 172.8(3) . . ?
C8 Fe1 C10 68.2(3) . . ?
C9 Fe1 C10 40.2(3) . . ?
C7 Fe1 C10 69.1(3) . . ?
C5 Fe1 C10 133.9(3) . . ?
C6 Fe1 C10 41.4(2) . . ?
C4 Fe1 C10 110.4(3) . . ?
C1 Fe1 C2 41.7(3) . . ?
C8 Fe1 C2 108.7(3) . . ?
C9 Fe1 C2 114.5(3) . . ?
C7 Fe1 C2 132.1(3) . . ?
C5 Fe1 C2 69.8(3) . . ?
C6 Fe1 C2 172.5(2) . . ?
C4 Fe1 C2 69.2(3) . . ?
C10 Fe1 C2 145.2(2) . . ?
C1 Fe1 C3 68.6(3) . . ?
C8 Fe1 C3 134.5(3) . . ?
C9 Fe1 C3 111.2(3) . . ?
C7 Fe1 C3 172.5(3) . . ?
C5 Fe1 C3 68.8(3) . . ?
C6 Fe1 C3 145.7(3) . . ?
C4 Fe1 C3 40.7(3) . . ?
C10 Fe1 C3 115.6(3) . . ?
C2 Fe1 C3 40.8(3) . . ?
C35 C31 C32 109.9(6) . . ?
C35 C31 Br31 126.9(6) . . ?
C32 C31 Br31 123.1(5) . . ?
C35 C31 Fe31 69.7(4) . . ?
C32 C31 Fe31 70.7(4) . . ?
Br31 C31 Fe31 124.6(3) . . ?
C33 C32 C31 106.3(6) . . ?
C33 C32 Fe31 69.1(4) . . ?
C31 C32 Fe31 68.3(4) . . ?
C33 C32 H32 126.9 . . ?
C31 C32 H32 126.9 . . ?
Fe31 C32 H32 127.2 . . ?
C34 C33 C32 108.6(6) . . ?
C34 C33 Fe31 69.7(4) . . ?
C32 C33 Fe31 70.2(4) . . ?
C34 C33 H33 125.7 . . ?
C32 C33 H33 125.7 . . ?
Fe31 C33 H33 126.0 . . ?
C33 C34 C35 108.7(6) . . ?
C33 C34 Fe31 69.8(4) . . ?
C35 C34 Fe31 68.9(4) . . ?
C33 C34 H34 125.6 . . ?
C35 C34 H34 125.6 . . ?
Fe31 C34 H34 127.3 . . ?
C31 C35 C34 106.4(6) . . ?
C31 C35 Fe31 69.5(4) . . ?
C34 C35 Fe31 69.9(4) . . ?
C31 C35 H35 126.8 . . ?
C34 C35 H35 126.8 . . ?
Fe31 C35 H35 125.4 . . ?
C40 C36 C37 106.3(6) . . ?
C40 C36 C41 126.2(5) . . ?
C37 C36 C41 127.4(6) . . ?
C40 C36 Fe31 69.7(4) . . ?
C37 C36 Fe31 68.9(4) . . ?
C41 C36 Fe31 123.9(4) . . ?
C38 C37 C36 108.6(6) . . ?
C38 C37 Fe31 70.2(4) . . ?
C36 C37 Fe31 69.5(3) . . ?
C38 C37 H37 125.7 . . ?
C36 C37 H37 125.7 . . ?
Fe31 C37 H37 126.1 . . ?
C39 C38 C37 108.5(6) . . ?
C39 C38 Fe31 69.3(4) . . ?
C37 C38 Fe31 69.8(4) . . ?
C39 C38 H38 125.8 . . ?
C37 C38 H38 125.8 . . ?
Fe31 C38 H38 126.7 . . ?
C38 C39 C40 109.2(6) . . ?
C38 C39 Fe31 70.6(4) . . ?
C40 C39 Fe31 70.5(4) . . ?
C38 C39 H39 125.4 . . ?
C40 C39 H39 125.4 . . ?
Fe31 C39 H39 125.1 . . ?
C39 C40 C36 107.4(6) . . ?
C39 C40 Fe31 68.7(4) . . ?
C36 C40 Fe31 69.4(4) . . ?
C39 C40 H40 126.3 . . ?
C36 C40 H40 126.3 . . ?
Fe31 C40 H40 127.2 . . ?
C42 C41 C54 118.2(6) . . ?
C42 C41 C36 121.6(6) . . ?
C54 C41 C36 120.2(6) . . ?
C43 C42 C41 121.9(6) . . ?
C43 C42 H42 119.0 . . ?
C41 C42 H42 119.0 . . ?
C42 C43 C52 119.6(6) . . ?
C42 C43 C44 120.3(6) . . ?
C52 C43 C44 120.1(6) . . ?
O31 C44 C45 121.3(6) . . ?
O31 C44 C43 120.3(6) . . ?
C45 C44 C43 118.4(6) . . ?
C46 C45 C50 118.7(6) . . ?
C46 C45 C44 120.1(6) . . ?
C50 C45 C44 121.2(6) . . ?
C47 C46 C45 121.3(6) . . ?
C47 C46 H46 119.4 . . ?
C45 C46 H46 119.4 . . ?
C46 C47 C48 118.4(6) . . ?
C46 C47 H47 120.8 . . ?
C48 C47 H47 120.8 . . ?
C49 C48 C47 121.0(7) . . ?
C49 C48 Br32 120.2(5) . . ?
C47 C48 Br32 118.8(5) . . ?
C48 C49 C50 120.3(6) . . ?
C48 C49 H49 119.8 . . ?
C50 C49 H49 119.8 . . ?
C49 C50 C45 120.2(6) . . ?
C49 C50 C51 119.1(6) . . ?
C45 C50 C51 120.6(6) . . ?
O32 C51 C52 122.4(6) . . ?
O32 C51 C50 120.0(6) . . ?
C52 C51 C50 117.6(6) . . ?
C53 C52 C43 119.2(6) . . ?
C53 C52 C51 118.9(6) . . ?
C43 C52 C51 122.0(6) . . ?
C54 C53 C52 121.1(6) . . ?
C54 C53 H53 119.5 . . ?
C52 C53 H53 119.5 . . ?
C53 C54 C41 120.1(6) . . ?
C53 C54 H54 120.0 . . ?
C41 C54 H54 120.0 . . ?
C31 Fe31 C39 144.6(3) . . ?
C31 Fe31 C35 40.8(3) . . ?
C39 Fe31 C35 174.5(3) . . ?
C31 Fe31 C37 108.5(3) . . ?
C39 Fe31 C37 67.7(3) . . ?
C35 Fe31 C37 111.6(3) . . ?
C31 Fe31 C34 68.1(3) . . ?
C39 Fe31 C34 136.5(3) . . ?
C35 Fe31 C34 41.1(3) . . ?
C37 Fe31 C34 143.3(3) . . ?
C31 Fe31 C38 113.8(3) . . ?
C39 Fe31 C38 40.1(3) . . ?
C35 Fe31 C38 142.5(3) . . ?
C37 Fe31 C38 40.0(3) . . ?
C34 Fe31 C38 176.1(3) . . ?
C31 Fe31 C33 68.4(3) . . ?
C39 Fe31 C33 112.0(3) . . ?
C35 Fe31 C33 69.3(3) . . ?
C37 Fe31 C33 174.5(3) . . ?
C34 Fe31 C33 40.6(3) . . ?
C38 Fe31 C33 136.4(3) . . ?
C31 Fe31 C36 133.0(3) . . ?
C39 Fe31 C36 68.8(3) . . ?
C35 Fe31 C36 107.0(3) . . ?
C37 Fe31 C36 41.5(3) . . ?
C34 Fe31 C36 112.6(3) . . ?
C38 Fe31 C36 68.8(2) . . ?
C33 Fe31 C36 143.9(3) . . ?
C31 Fe31 C40 173.3(3) . . ?
C39 Fe31 C40 40.8(3) . . ?
C35 Fe31 C40 133.7(3) . . ?
C37 Fe31 C40 68.6(3) . . ?
C34 Fe31 C40 110.2(3) . . ?
C38 Fe31 C40 68.2(3) . . ?
C33 Fe31 C40 115.0(3) . . ?
C36 Fe31 C40 40.9(2) . . ?
C31 Fe31 C32 41.0(3) . . ?
C39 Fe31 C32 115.0(3) . . ?
C35 Fe31 C32 69.6(3) . . ?
C37 Fe31 C32 134.1(3) . . ?
C34 Fe31 C32 68.5(3) . . ?
C38 Fe31 C32 110.5(3) . . ?
C33 Fe31 C32 40.7(3) . . ?
C36 Fe31 C32 173.7(3) . . ?
C40 Fe31 C32 145.2(3) . . ?
 
_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    0.886
_refine_diff_density_min   -0.606
_refine_diff_density_rms    0.128
