data_s93
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. I. R. Butler
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C21 H12 Br F6 Fe N'
_chemical_formula_weight          528.08
 
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'
 'F'  'F'   0.0171   0.0103
 '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            orthorhombic
_symmetry_space_group_name_H-M    Pna2(1)
_symmetry_space_group_name_hall   'P 2c -2n'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, z+1/2'
 'x+1/2, -y+1/2, z'
 '-x+1/2, y+1/2, z+1/2'
 
_cell_length_a                    14.7387(12)
_cell_length_b                    10.7713(9)
_cell_length_c                    23.365(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      3709.4(6)
_cell_formula_units_Z             8
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     4552
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Plate
_exptl_crystal_colour             Red
_exptl_crystal_size_max           0.56
_exptl_crystal_size_mid           0.36
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.891
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              2080
_exptl_absorpt_coefficient_mu     3.034
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.2814
_exptl_absorpt_correction_T_max   0.8631
_exptl_absorpt_process_details       'SADABS V2.10 (Sheldrick, G.M., 2003)'

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    'graphite'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             25849
_diffrn_reflns_av_R_equivalents   0.0468
_diffrn_reflns_av_sigmaI/netI     0.0556
_diffrn_reflns_limit_h_min        -19
_diffrn_reflns_limit_h_max        18
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -28
_diffrn_reflns_limit_l_max        30
_diffrn_reflns_theta_min          3.35
_diffrn_reflns_theta_max          27.48
_reflns_number_total              8235
_reflns_number_gt                 6449
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_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)+(0.0801P)²+4.5403P] 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      none
_refine_ls_extinction_coef        ?
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.425(13)
_refine_ls_number_reflns          8235
_refine_ls_number_parameters      542
_refine_ls_number_restraints      669
_refine_ls_R_factor_all           0.0745
_refine_ls_R_factor_gt            0.0523
_refine_ls_wR_factor_ref          0.1409
_refine_ls_wR_factor_gt           0.1296
_refine_ls_goodness_of_fit_ref    1.040
_refine_ls_restrained_S_all       1.001
_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 0.7488(5) 0.3448(6) 0.5685(3) 0.0209(13) Uani 1 1 d U . .
C2 C 0.7026(5) 0.2580(6) 0.5292(4) 0.0140(15) Uani 1 1 d U . .
H2 H 0.6597 0.2778 0.5002 0.017 Uiso 1 1 calc R . .
C3 C 0.7368(4) 0.1365(7) 0.5442(3) 0.0229(14) Uani 1 1 d U . .
H3 H 0.7202 0.0606 0.5263 0.027 Uiso 1 1 calc R . .
C4 C 0.7982(5) 0.1487(7) 0.5894(3) 0.0278(14) Uani 1 1 d U . .
H4 H 0.8304 0.0816 0.6062 0.033 Uiso 1 1 calc R . .
C5 C 0.8061(6) 0.2730(9) 0.6065(4) 0.0284(16) Uani 1 1 d U . .
H5 H 0.8419 0.3041 0.6371 0.034 Uiso 1 1 calc R . .
C6 C 0.8773(4) 0.2976(7) 0.4390(3) 0.0164(12) Uani 1 1 d U . .
C7 C 0.9164(4) 0.3827(6) 0.4798(3) 0.0189(11) Uani 1 1 d U . .
H7 H 0.9052 0.4693 0.4830 0.023 Uiso 1 1 calc R . .
C8 C 0.9757(4) 0.3089(8) 0.5144(3) 0.0252(16) Uani 1 1 d U . .
H8 H 1.0134 0.3400 0.5441 0.030 Uiso 1 1 calc R . .
C9 C 0.9703(4) 0.1891(8) 0.4987(3) 0.0233(16) Uani 1 1 d U . .
H9 H 1.0021 0.1222 0.5160 0.028 Uiso 1 1 calc R . .
C10 C 0.9087(4) 0.1787(6) 0.4517(3) 0.0160(12) Uani 1 1 d U . .
H10 H 0.8922 0.1043 0.4326 0.019 Uiso 1 1 calc R . .
C11 C 0.8101(3) 0.3367(5) 0.3951(2) 0.0127(11) Uani 1 1 d U . .
C12 C 0.7466(4) 0.4252(6) 0.4078(2) 0.0140(12) Uani 1 1 d U . .
H12 H 0.7459 0.4649 0.4441 0.017 Uiso 1 1 calc R . .
C13 C 0.6821(4) 0.4555(5) 0.3654(3) 0.0148(12) Uani 1 1 d U . .
C14 C 0.7406(4) 0.3231(6) 0.3005(2) 0.0137(11) Uani 1 1 d U . .
C15 C 0.7378(5) 0.2694(6) 0.2445(4) 0.0135(14) Uani 1 1 d U . .
C16 C 0.8026(4) 0.1870(6) 0.2271(3) 0.0197(13) Uani 1 1 d U . .
H16 H 0.8001 0.1519 0.1899 0.024 Uiso 1 1 calc R . .
C17 C 0.8731(4) 0.1547(6) 0.2648(3) 0.0245(14) Uani 1 1 d U . .
H17 H 0.9188 0.0987 0.2523 0.029 Uiso 1 1 calc R . .
C18 C 0.8775(4) 0.2015(6) 0.3184(3) 0.0192(12) Uani 1 1 d U . .
H18 H 0.9261 0.1776 0.3427 0.023 Uiso 1 1 calc R . .
C19 C 0.8108(4) 0.2857(7) 0.3394(3) 0.0151(11) Uani 1 1 d U . .
C20 C 0.6088(4) 0.5516(6) 0.3807(3) 0.0192(13) Uani 1 1 d U . .
C21 C 0.6668(4) 0.3104(6) 0.2026(3) 0.0258(13) Uani 1 1 d U . .
N1 N 0.6750(3) 0.4076(5) 0.3152(2) 0.0124(10) Uani 1 1 d U . .
F1 F 0.5919(3) 0.5529(5) 0.4364(2) 0.0424(13) Uani 1 1 d U . .
F2 F 0.6343(3) 0.6641(4) 0.3664(2) 0.0469(12) Uani 1 1 d U . .
F3 F 0.5308(3) 0.5305(5) 0.3556(2) 0.0466(14) Uani 1 1 d U . .
F4 F 0.5831(3) 0.2885(5) 0.22146(19) 0.0346(10) Uani 1 1 d U . .
F5 F 0.6712(3) 0.4327(4) 0.19136(17) 0.0353(9) Uani 1 1 d U . .
F6 F 0.6756(4) 0.2526(4) 0.1529(3) 0.0405(17) Uani 1 1 d U . .
Fe1 Fe 0.84402(8) 0.25170(7) 0.52178(5) 0.0139(3) Uani 1 1 d U . .
Br1 Br 0.72936(6) 0.51461(6) 0.57053(4) 0.03923(19) Uani 1 1 d U . .
C31 C 0.9987(5) -0.3424(6) 0.1982(3) 0.0227(13) Uani 1 1 d U . .
C32 C 1.0408(6) -0.2562(6) 0.2321(5) 0.0225(19) Uani 1 1 d U . .
H32 H 1.0842 -0.2754 0.2608 0.027 Uiso 1 1 calc R . .
C33 C 1.0125(5) -0.1395(8) 0.2191(3) 0.0264(15) Uani 1 1 d U . .
H33 H 1.0315 -0.0650 0.2373 0.032 Uiso 1 1 calc R . .
C34 C 0.9482(4) -0.1493(8) 0.1728(3) 0.0275(14) Uani 1 1 d U . .
H34 H 0.9180 -0.0833 0.1537 0.033 Uiso 1 1 calc R . .
C35 C 0.9397(5) -0.2778(9) 0.1617(3) 0.0256(13) Uani 1 1 d U . .
H35 H 0.9006 -0.3143 0.1341 0.031 Uiso 1 1 calc R . .
C36 C 0.8754(4) -0.2955(7) 0.3263(3) 0.0136(11) Uani 1 1 d U . .
C37 C 0.8452(4) -0.1702(7) 0.3131(3) 0.0185(13) Uani 1 1 d U . .
H37 H 0.8636 -0.0966 0.3322 0.022 Uiso 1 1 calc R . .
C38 C 0.7823(4) -0.1773(7) 0.2658(3) 0.0177(14) Uani 1 1 d U . .
H38 H 0.7516 -0.1103 0.2479 0.021 Uiso 1 1 calc R . .
C39 C 0.7757(4) -0.3111(7) 0.2511(3) 0.0175(14) Uani 1 1 d U . .
H39 H 0.7384 -0.3455 0.2219 0.021 Uiso 1 1 calc R . .
C40 C 0.8326(4) -0.3771(6) 0.2868(3) 0.0189(11) Uani 1 1 d U . .
H40 H 0.8417 -0.4644 0.2853 0.023 Uiso 1 1 calc R . .
C41 C 0.9414(3) -0.3339(5) 0.3706(2) 0.0136(11) Uani 1 1 d U . .
C42 C 1.0052(4) -0.4225(6) 0.3578(3) 0.0151(12) Uani 1 1 d U . .
H42 H 1.0048 -0.4616 0.3214 0.018 Uiso 1 1 calc R . .
C43 C 1.0697(4) -0.4550(5) 0.3977(3) 0.0128(11) Uani 1 1 d U . .
C44 C 1.0129(3) -0.3223(5) 0.4644(2) 0.0116(11) Uani 1 1 d U . .
C45 C 1.0165(6) -0.2732(7) 0.5214(4) 0.0198(14) Uani 1 1 d U . .
C46 C 0.9504(4) -0.1895(6) 0.5385(3) 0.0231(13) Uani 1 1 d U . .
H46 H 0.9534 -0.1552 0.5759 0.028 Uiso 1 1 calc R . .
C47 C 0.8797(4) -0.1541(6) 0.5024(3) 0.0240(14) Uani 1 1 d U . .
H47 H 0.8346 -0.0982 0.5158 0.029 Uiso 1 1 calc R . .
C48 C 0.8749(4) -0.2003(6) 0.4469(3) 0.0198(13) Uani 1 1 d U . .
H48 H 0.8266 -0.1761 0.4224 0.024 Uiso 1 1 calc R . .
C49 C 0.9422(4) -0.2834(7) 0.4273(3) 0.0137(11) Uani 1 1 d U . .
C50 C 1.1395(4) -0.5518(6) 0.3840(3) 0.0188(13) Uani 1 1 d U . .
C51 C 1.0889(4) -0.3131(6) 0.5616(3) 0.0256(14) Uani 1 1 d U . .
N31 N 1.0767(3) -0.4072(5) 0.4501(2) 0.0157(11) Uani 1 1 d U . .
F31 F 1.1561(3) -0.5582(4) 0.3280(2) 0.0362(12) Uani 1 1 d U . .
F32 F 1.1139(3) -0.6631(4) 0.4004(2) 0.0486(13) Uani 1 1 d U . .
F33 F 1.2198(3) -0.5299(5) 0.4084(2) 0.0434(13) Uani 1 1 d U . .
F34 F 1.1737(3) -0.2904(5) 0.5414(2) 0.0356(9) Uani 1 1 d U . .
F35 F 1.0854(3) -0.4348(4) 0.57286(17) 0.0326(9) Uani 1 1 d U . .
F36 F 1.0839(4) -0.2533(3) 0.6124(3) 0.0308(15) Uani 1 1 d U . .
Fe31 Fe 0.90706(8) -0.24877(7) 0.24374(5) 0.0131(3) Uani 1 1 d U . .
Br31 Br 1.02227(6) -0.51253(7) 0.19742(5) 0.0435(2) Uani 1 1 d U . .
 
 
_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 1.448(11) . ?
C1 C2 1.478(10) . ?
C1 Br1 1.852(7) . ?
C1 Fe1 2.041(7) . ?
C2 C3 1.446(9) . ?
C2 Fe1 2.093(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.396(10) . ?
C3 Fe1 2.077(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.403(11) . ?
C4 Fe1 2.045(6) . ?
C4 H4 0.9500 . ?
C5 Fe1 2.071(9) . ?
C5 H5 0.9500 . ?
C6 C10 1.393(10) . ?
C6 C7 1.443(9) . ?
C6 C11 1.487(8) . ?
C6 Fe1 2.056(6) . ?
C7 C8 1.433(9) . ?
C7 Fe1 2.023(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.344(14) . ?
C8 Fe1 2.044(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.429(10) . ?
C9 Fe1 2.051(7) . ?
C9 H9 0.9500 . ?
C10 Fe1 2.051(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.368(8) . ?
C11 C19 1.413(8) . ?
C12 C13 1.413(8) . ?
C12 H12 0.9500 . ?
C13 N1 1.284(8) . ?
C13 C20 1.539(9) . ?
C14 N1 1.372(8) . ?
C14 C15 1.430(10) . ?
C14 C19 1.435(8) . ?
C15 C16 1.366(9) . ?
C15 C21 1.500(10) . ?
C16 C17 1.406(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.352(9) . ?
C17 H17 0.9500 . ?
C18 C19 1.424(9) . ?
C18 H18 0.9500 . ?
C20 F3 1.310(7) . ?
C20 F2 1.312(8) . ?
C20 F1 1.325(8) . ?
C21 F6 1.325(9) . ?
C21 F4 1.331(8) . ?
C21 F5 1.345(8) . ?
C31 C32 1.369(10) . ?
C31 C35 1.403(11) . ?
C31 Br31 1.865(7) . ?
C31 Fe31 1.993(7) . ?
C32 C33 1.358(10) . ?
C32 Fe31 1.992(8) . ?
C32 H32 0.9500 . ?
C33 C34 1.442(9) . ?
C33 Fe31 2.032(7) . ?
C33 H33 0.9500 . ?
C34 C35 1.414(11) . ?
C34 Fe31 2.065(7) . ?
C34 H34 0.9500 . ?
C35 Fe31 2.001(8) . ?
C35 H35 0.9500 . ?
C36 C40 1.423(9) . ?
C36 C37 1.454(9) . ?
C36 C41 1.479(8) . ?
C36 Fe31 2.048(6) . ?
C37 C38 1.443(10) . ?
C37 Fe31 2.043(7) . ?
C37 H37 0.9500 . ?
C38 C39 1.485(12) . ?
C38 Fe31 2.059(6) . ?
C38 H38 0.9500 . ?
C39 C40 1.381(9) . ?
C39 Fe31 2.057(7) . ?
C39 H39 0.9500 . ?
C40 Fe31 2.033(6) . ?
C40 H40 0.9500 . ?
C41 C42 1.373(8) . ?
C41 C49 1.432(9) . ?
C42 C43 1.377(9) . ?
C42 H42 0.9500 . ?
C43 N31 1.331(8) . ?
C43 C50 1.499(9) . ?
C44 N31 1.353(8) . ?
C44 C49 1.420(8) . ?
C44 C45 1.433(10) . ?
C45 C46 1.387(10) . ?
C45 C51 1.485(11) . ?
C46 C47 1.393(9) . ?
C46 H46 0.9500 . ?
C47 C48 1.391(9) . ?
C47 H47 0.9500 . ?
C48 C49 1.413(9) . ?
C48 H48 0.9500 . ?
C50 F32 1.314(8) . ?
C50 F31 1.333(8) . ?
C50 F33 1.334(7) . ?
C51 F35 1.337(8) . ?
C51 F36 1.353(9) . ?
C51 F34 1.359(7) . ?
 
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 108.2(6) . . ?
C5 C1 Br1 127.0(6) . . ?
C2 C1 Br1 124.7(5) . . ?
C5 C1 Fe1 70.5(4) . . ?
C2 C1 Fe1 70.9(4) . . ?
Br1 C1 Fe1 127.2(4) . . ?
C3 C2 C1 105.1(6) . . ?
C3 C2 Fe1 69.1(4) . . ?
C1 C2 Fe1 67.2(4) . . ?
C3 C2 H2 127.5 . . ?
C1 C2 H2 127.5 . . ?
Fe1 C2 H2 127.7 . . ?
C4 C3 C2 108.9(7) . . ?
C4 C3 Fe1 69.0(4) . . ?
C2 C3 Fe1 70.3(4) . . ?
C4 C3 H3 125.5 . . ?
C2 C3 H3 125.5 . . ?
Fe1 C3 H3 126.8 . . ?
C3 C4 C5 111.1(7) . . ?
C3 C4 Fe1 71.4(4) . . ?
C5 C4 Fe1 71.1(4) . . ?
C3 C4 H4 124.5 . . ?
C5 C4 H4 124.5 . . ?
Fe1 C4 H4 124.6 . . ?
C4 C5 C1 106.6(7) . . ?
C4 C5 Fe1 69.1(4) . . ?
C1 C5 Fe1 68.3(4) . . ?
C4 C5 H5 126.7 . . ?
C1 C5 H5 126.7 . . ?
Fe1 C5 H5 127.5 . . ?
C10 C6 C7 108.1(6) . . ?
C10 C6 C11 129.0(7) . . ?
C7 C6 C11 122.8(6) . . ?
C10 C6 Fe1 70.0(3) . . ?
C7 C6 Fe1 68.1(3) . . ?
C11 C6 Fe1 123.9(4) . . ?
C8 C7 C6 105.3(6) . . ?
C8 C7 Fe1 70.1(4) . . ?
C6 C7 Fe1 70.5(4) . . ?
C8 C7 H7 127.3 . . ?
C6 C7 H7 127.3 . . ?
Fe1 C7 H7 123.7 . . ?
C9 C8 C7 110.0(6) . . ?
C9 C8 Fe1 71.1(4) . . ?
C7 C8 Fe1 68.6(3) . . ?
C9 C8 H8 125.0 . . ?
C7 C8 H8 125.0 . . ?
Fe1 C8 H8 126.9 . . ?
C8 C9 C10 108.8(6) . . ?
C8 C9 Fe1 70.5(4) . . ?
C10 C9 Fe1 69.6(3) . . ?
C8 C9 H9 125.6 . . ?
C10 C9 H9 125.6 . . ?
Fe1 C9 H9 125.8 . . ?
C6 C10 C9 107.7(6) . . ?
C6 C10 Fe1 70.4(3) . . ?
C9 C10 Fe1 69.6(4) . . ?
C6 C10 H10 126.2 . . ?
C9 C10 H10 126.2 . . ?
Fe1 C10 H10 125.4 . . ?
C12 C11 C19 118.4(5) . . ?
C12 C11 C6 120.2(5) . . ?
C19 C11 C6 121.3(5) . . ?
C11 C12 C13 118.0(5) . . ?
C11 C12 H12 121.0 . . ?
C13 C12 H12 121.0 . . ?
N1 C13 C12 127.0(6) . . ?
N1 C13 C20 115.2(5) . . ?
C12 C13 C20 117.7(5) . . ?
N1 C14 C15 118.6(5) . . ?
N1 C14 C19 122.3(5) . . ?
C15 C14 C19 119.1(6) . . ?
C16 C15 C14 121.0(7) . . ?
C16 C15 C21 119.0(7) . . ?
C14 C15 C21 119.9(6) . . ?
C15 C16 C17 119.4(6) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C18 C17 C16 121.6(6) . . ?
C18 C17 H17 119.2 . . ?
C16 C17 H17 119.2 . . ?
C17 C18 C19 121.5(6) . . ?
C17 C18 H18 119.2 . . ?
C19 C18 H18 119.2 . . ?
C11 C19 C18 124.7(6) . . ?
C11 C19 C14 118.0(5) . . ?
C18 C19 C14 117.3(6) . . ?
F3 C20 F2 107.4(5) . . ?
F3 C20 F1 106.1(6) . . ?
F2 C20 F1 107.1(6) . . ?
F3 C20 C13 113.3(5) . . ?
F2 C20 C13 111.1(6) . . ?
F1 C20 C13 111.6(5) . . ?
F6 C21 F4 107.4(6) . . ?
F6 C21 F5 106.5(5) . . ?
F4 C21 F5 106.4(5) . . ?
F6 C21 C15 111.5(6) . . ?
F4 C21 C15 112.2(6) . . ?
F5 C21 C15 112.5(5) . . ?
C13 N1 C14 116.1(5) . . ?
C7 Fe1 C1 106.2(3) . . ?
C7 Fe1 C8 41.3(3) . . ?
C1 Fe1 C8 123.4(3) . . ?
C7 Fe1 C4 158.0(3) . . ?
C1 Fe1 C4 68.0(3) . . ?
C8 Fe1 C4 122.8(3) . . ?
C7 Fe1 C10 68.6(3) . . ?
C1 Fe1 C10 159.2(3) . . ?
C8 Fe1 C10 66.8(3) . . ?
C4 Fe1 C10 124.2(3) . . ?
C7 Fe1 C9 67.9(3) . . ?
C1 Fe1 C9 157.8(3) . . ?
C8 Fe1 C9 38.3(4) . . ?
C4 Fe1 C9 108.9(3) . . ?
C10 Fe1 C9 40.8(3) . . ?
C7 Fe1 C6 41.4(3) . . ?
C1 Fe1 C6 123.3(3) . . ?
C8 Fe1 C6 67.8(3) . . ?
C4 Fe1 C6 159.4(3) . . ?
C10 Fe1 C6 39.6(3) . . ?
C9 Fe1 C6 67.4(3) . . ?
C7 Fe1 C5 122.0(3) . . ?
C1 Fe1 C5 41.2(3) . . ?
C8 Fe1 C5 107.7(3) . . ?
C4 Fe1 C5 39.8(3) . . ?
C10 Fe1 C5 158.7(3) . . ?
C9 Fe1 C5 122.2(3) . . ?
C6 Fe1 C5 159.7(3) . . ?
C7 Fe1 C3 160.1(3) . . ?
C1 Fe1 C3 68.6(3) . . ?
C8 Fe1 C3 157.5(3) . . ?
C4 Fe1 C3 39.6(3) . . ?
C10 Fe1 C3 109.0(3) . . ?
C9 Fe1 C3 124.1(3) . . ?
C6 Fe1 C3 124.2(3) . . ?
C5 Fe1 C3 67.6(3) . . ?
C7 Fe1 C2 122.8(3) . . ?
C1 Fe1 C2 41.9(3) . . ?
C8 Fe1 C2 160.6(3) . . ?
C4 Fe1 C2 68.0(3) . . ?
C10 Fe1 C2 122.8(3) . . ?
C9 Fe1 C2 159.4(3) . . ?
C6 Fe1 C2 107.9(3) . . ?
C5 Fe1 C2 69.4(4) . . ?
C3 Fe1 C2 40.6(3) . . ?
C32 C31 C35 107.2(7) . . ?
C32 C31 Br31 126.0(6) . . ?
C35 C31 Br31 126.6(6) . . ?
C32 C31 Fe31 69.9(5) . . ?
C35 C31 Fe31 69.7(4) . . ?
Br31 C31 Fe31 128.9(4) . . ?
C33 C32 C31 111.1(8) . . ?
C33 C32 Fe31 71.9(4) . . ?
C31 C32 Fe31 70.0(4) . . ?
C33 C32 H32 124.5 . . ?
C31 C32 H32 124.5 . . ?
Fe31 C32 H32 125.3 . . ?
C32 C33 C34 107.6(7) . . ?
C32 C33 Fe31 68.7(5) . . ?
C34 C33 Fe31 70.6(4) . . ?
C32 C33 H33 126.2 . . ?
C34 C33 H33 126.2 . . ?
Fe31 C33 H33 126.0 . . ?
C35 C34 C33 105.5(7) . . ?
C35 C34 Fe31 67.2(4) . . ?
C33 C34 Fe31 68.2(4) . . ?
C35 C34 H34 127.2 . . ?
C33 C34 H34 127.2 . . ?
Fe31 C34 H34 128.8 . . ?
C31 C35 C34 108.6(7) . . ?
C31 C35 Fe31 69.2(4) . . ?
C34 C35 Fe31 72.1(4) . . ?
C31 C35 H35 125.7 . . ?
C34 C35 H35 125.7 . . ?
Fe31 C35 H35 124.6 . . ?
C40 C36 C37 107.4(5) . . ?
C40 C36 C41 124.9(6) . . ?
C37 C36 C41 127.6(6) . . ?
C40 C36 Fe31 69.0(3) . . ?
C37 C36 Fe31 69.0(3) . . ?
C41 C36 Fe31 125.3(4) . . ?
C38 C37 C36 108.1(6) . . ?
C38 C37 Fe31 70.0(4) . . ?
C36 C37 Fe31 69.4(3) . . ?
C38 C37 H37 126.0 . . ?
C36 C37 H37 126.0 . . ?
Fe31 C37 H37 126.2 . . ?
C37 C38 C39 105.7(6) . . ?
C37 C38 Fe31 68.8(4) . . ?
C39 C38 Fe31 68.8(3) . . ?
C37 C38 H38 127.1 . . ?
C39 C38 H38 127.1 . . ?
Fe31 C38 H38 126.8 . . ?
C40 C39 C38 108.6(6) . . ?
C40 C39 Fe31 69.3(3) . . ?
C38 C39 Fe31 68.9(3) . . ?
C40 C39 H39 125.7 . . ?
C38 C39 H39 125.7 . . ?
Fe31 C39 H39 127.7 . . ?
C39 C40 C36 110.1(6) . . ?
C39 C40 Fe31 71.2(4) . . ?
C36 C40 Fe31 70.2(4) . . ?
C39 C40 H40 125.0 . . ?
C36 C40 H40 125.0 . . ?
Fe31 C40 H40 125.2 . . ?
C42 C41 C49 117.3(5) . . ?
C42 C41 C36 119.6(5) . . ?
C49 C41 C36 123.1(5) . . ?
C41 C42 C43 120.2(5) . . ?
C41 C42 H42 119.9 . . ?
C43 C42 H42 119.9 . . ?
N31 C43 C42 125.3(6) . . ?
N31 C43 C50 114.3(5) . . ?
C42 C43 C50 120.4(5) . . ?
N31 C44 C49 124.0(5) . . ?
N31 C44 C45 116.9(6) . . ?
C49 C44 C45 119.1(6) . . ?
C46 C45 C44 118.9(7) . . ?
C46 C45 C51 120.6(7) . . ?
C44 C45 C51 120.5(6) . . ?
C45 C46 C47 121.9(7) . . ?
C45 C46 H46 119.1 . . ?
C47 C46 H46 119.1 . . ?
C48 C47 C46 120.3(6) . . ?
C48 C47 H47 119.8 . . ?
C46 C47 H47 119.8 . . ?
C47 C48 C49 119.6(6) . . ?
C47 C48 H48 120.2 . . ?
C49 C48 H48 120.2 . . ?
C48 C49 C44 120.3(6) . . ?
C48 C49 C41 122.4(5) . . ?
C44 C49 C41 117.3(5) . . ?
F32 C50 F31 106.9(6) . . ?
F32 C50 F33 107.0(5) . . ?
F31 C50 F33 105.4(5) . . ?
F32 C50 C43 112.0(6) . . ?
F31 C50 C43 111.8(5) . . ?
F33 C50 C43 113.3(5) . . ?
F35 C51 F36 107.0(5) . . ?
F35 C51 F34 106.2(5) . . ?
F36 C51 F34 105.6(5) . . ?
F35 C51 C45 112.4(6) . . ?
F36 C51 C45 112.3(6) . . ?
F34 C51 C45 112.9(6) . . ?
C43 N31 C44 115.8(5) . . ?
C32 Fe31 C31 40.2(3) . . ?
C32 Fe31 C35 67.9(4) . . ?
C31 Fe31 C35 41.1(3) . . ?
C32 Fe31 C33 39.4(3) . . ?
C31 Fe31 C33 67.9(3) . . ?
C35 Fe31 C33 68.6(3) . . ?
C32 Fe31 C40 125.1(3) . . ?
C31 Fe31 C40 106.6(3) . . ?
C35 Fe31 C40 119.9(3) . . ?
C33 Fe31 C40 161.3(3) . . ?
C32 Fe31 C37 124.5(3) . . ?
C31 Fe31 C37 159.3(3) . . ?
C35 Fe31 C37 158.8(3) . . ?
C33 Fe31 C37 109.0(3) . . ?
C40 Fe31 C37 69.4(3) . . ?
C32 Fe31 C36 110.2(3) . . ?
C31 Fe31 C36 122.2(3) . . ?
C35 Fe31 C36 156.8(3) . . ?
C33 Fe31 C36 125.7(3) . . ?
C40 Fe31 C36 40.8(3) . . ?
C37 Fe31 C36 41.6(3) . . ?
C32 Fe31 C39 158.5(3) . . ?
C31 Fe31 C39 121.2(3) . . ?
C35 Fe31 C39 104.8(3) . . ?
C33 Fe31 C39 158.8(3) . . ?
C40 Fe31 C39 39.5(3) . . ?
C37 Fe31 C39 69.4(3) . . ?
C36 Fe31 C39 68.1(3) . . ?
C32 Fe31 C38 158.9(3) . . ?
C31 Fe31 C38 158.1(3) . . ?
C35 Fe31 C38 120.9(3) . . ?
C33 Fe31 C38 122.5(3) . . ?
C40 Fe31 C38 69.4(3) . . ?
C37 Fe31 C38 41.2(3) . . ?
C36 Fe31 C38 69.6(3) . . ?
C39 Fe31 C38 42.3(3) . . ?
C32 Fe31 C34 67.7(3) . . ?
C31 Fe31 C34 68.6(3) . . ?
C35 Fe31 C34 40.7(3) . . ?
C33 Fe31 C34 41.2(3) . . ?
C40 Fe31 C34 155.4(3) . . ?
C37 Fe31 C34 123.6(3) . . ?
C36 Fe31 C34 161.9(3) . . ?
C39 Fe31 C34 120.9(3) . . ?
C38 Fe31 C34 105.7(3) . . ?
 
_diffrn_measured_fraction_theta_max    0.989
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.989
_refine_diff_density_max    1.827
_refine_diff_density_min   -1.241
_refine_diff_density_rms    0.131
