# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2006


data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'S. Aldridge'
'A. Al-Fawaz'
'William Clegg'
'Ross W. Harrington'
'Peter N. Horton'
'Michael B. Hursthouse'
'Kevin M. Jones'
'Deborah L. Kays'

_publ_contact_author_name        'Simon Aldridge'
_publ_contact_author_address     
;
School of Chemistry
Cardiff University
Main Building
Park Place
Cardiff
CF10 3AT
UNITED KINGDOM
;

_publ_contact_author_email       ALDRIDGES@CARDIFF.AC.UK

_publ_requested_journal          'Chemical Communications'

_publ_section_title              
;
Migratory insertion of [B(C6F5)2]- into C-H bonds: CO
promoted boryl anion transfer
;

# Attachment 'Combined.cif'

data_2
_database_code_depnum_ccdc_archive 'CCDC 602510'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H5 B F10 Fe O3'
_chemical_formula_weight         549.90

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'
B B 0.0013 0.0007 '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'
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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.4491(3)
_cell_length_b                   8.4985(4)
_cell_length_c                   15.6646(5)
_cell_angle_alpha                103.233(2)
_cell_angle_beta                 90.730(2)
_cell_angle_gamma                92.815(2)
_cell_volume                     963.88(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    4322
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      27.485

_exptl_crystal_description       Plate
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             540
_exptl_absorpt_coefficient_mu    0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_T_max  0.965
_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  '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19675
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.48
_reflns_number_total             4417
_reflns_number_gt                3837
_reflns_threshold_expression     I>2\s(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 F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0272P)^2^+0.6274P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4417
_refine_ls_number_parameters     320
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.0761
_refine_ls_wR_factor_gt          0.0726
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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 0.6275(2) 0.6246(2) 0.30383(12) 0.0206(4) Uani 1 1 d . . .
C2 C 0.6112(2) 0.5270(2) 0.36749(11) 0.0224(4) Uani 1 1 d . . .
H2 H 0.7082 0.5028 0.4015 0.027 Uiso 1 1 calc R . .
C3 C 0.4300(3) 0.4723(2) 0.37227(12) 0.0255(4) Uani 1 1 d . . .
H3 H 0.3847 0.4063 0.4094 0.031 Uiso 1 1 calc R . .
C4 C 0.3281(2) 0.5344(2) 0.31121(13) 0.0261(4) Uani 1 1 d . . .
H4 H 0.2022 0.5170 0.2998 0.031 Uiso 1 1 calc R . .
C5 C 0.4488(2) 0.6270(2) 0.27032(13) 0.0239(4) Uani 1 1 d . . .
H5 H 0.4154 0.6826 0.2269 0.029 Uiso 1 1 calc R . .
C6 C 0.8465(2) 0.8924(2) 0.35319(11) 0.0195(3) Uani 1 1 d . . .
C7 C 1.0206(2) 0.9608(2) 0.37079(12) 0.0213(4) Uani 1 1 d . . .
C8 C 1.0612(2) 1.1122(2) 0.42292(12) 0.0237(4) Uani 1 1 d . . .
C9 C 0.9246(3) 1.2048(2) 0.46167(12) 0.0238(4) Uani 1 1 d . . .
C10 C 0.7497(2) 1.1440(2) 0.44663(12) 0.0229(4) Uani 1 1 d . . .
C11 C 0.7143(2) 0.9909(2) 0.39357(12) 0.0214(4) Uani 1 1 d . . .
C12 C 0.8393(2) 0.7392(2) 0.18621(12) 0.0216(4) Uani 1 1 d . . .
C13 C 0.7383(3) 0.8441(2) 0.15233(12) 0.0254(4) Uani 1 1 d . . .
C14 C 0.7646(3) 0.8821(2) 0.07227(14) 0.0327(4) Uani 1 1 d . . .
C15 C 0.9008(3) 0.8118(3) 0.02070(13) 0.0340(5) Uani 1 1 d . . .
C16 C 1.0075(3) 0.7084(2) 0.05096(13) 0.0317(4) Uani 1 1 d . . .
C17 C 0.9745(3) 0.6734(2) 0.13125(12) 0.0254(4) Uani 1 1 d . . .
C21 C 0.5042(3) 0.3852(2) 0.13025(14) 0.0292(4) Uani 1 1 d . . .
C22 C 0.7339(3) 0.2902(2) 0.23653(12) 0.0267(4) Uani 1 1 d . . .
C23 C 0.3762(2) 0.2033(2) 0.23259(12) 0.0250(4) Uani 1 1 d . . .
B1 B 0.8158(3) 0.7129(2) 0.28609(13) 0.0201(4) Uani 1 1 d . . .
O21 O 0.4892(2) 0.3863(2) 0.05832(10) 0.0436(4) Uani 1 1 d . . .
O22 O 0.87004(19) 0.23504(18) 0.23339(10) 0.0372(3) Uani 1 1 d . . .
O23 O 0.27842(19) 0.09475(17) 0.22494(10) 0.0355(3) Uani 1 1 d . . .
F7 F 1.16080(13) 0.87553(13) 0.33549(7) 0.0285(2) Uani 1 1 d . . .
F8 F 1.23326(14) 1.17104(14) 0.43820(8) 0.0329(3) Uani 1 1 d . . .
F9 F 0.96089(16) 1.35253(13) 0.51346(8) 0.0338(3) Uani 1 1 d . . .
F10 F 0.61530(15) 1.23469(13) 0.48305(7) 0.0310(3) Uani 1 1 d . . .
F11 F 0.53916(14) 0.94104(13) 0.38209(7) 0.0294(3) Uani 1 1 d . . .
F13 F 0.60352(15) 0.91940(13) 0.20054(8) 0.0318(3) Uani 1 1 d . . .
F14 F 0.66167(19) 0.98642(17) 0.04443(9) 0.0475(3) Uani 1 1 d . . .
F15 F 0.9278(2) 0.84384(17) -0.05848(8) 0.0493(4) Uani 1 1 d . . .
F16 F 1.14305(18) 0.64107(16) 0.00168(8) 0.0442(3) Uani 1 1 d . . .
F17 F 1.08464(15) 0.56735(14) 0.15512(7) 0.0333(3) Uani 1 1 d . . .
Fe1 Fe 0.52152(3) 0.38559(3) 0.244963(16) 0.01989(8) Uani 1 1 d . . .
H1B H 0.927(3) 0.632(2) 0.3024(13) 0.022(5) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0209(8) 0.0157(8) 0.0238(9) 0.0006(7) 0.0018(7) 0.0039(7)
C2 0.0249(9) 0.0204(9) 0.0203(9) 0.0012(7) 0.0015(7) 0.0026(7)
C3 0.0285(10) 0.0206(9) 0.0254(9) 0.0005(7) 0.0098(8) 0.0008(7)
C4 0.0192(9) 0.0213(9) 0.0358(11) 0.0019(8) 0.0049(8) 0.0033(7)
C5 0.0230(9) 0.0160(8) 0.0323(10) 0.0041(7) 0.0003(7) 0.0039(7)
C6 0.0199(8) 0.0193(8) 0.0199(8) 0.0057(7) 0.0005(7) 0.0003(7)
C7 0.0205(8) 0.0224(9) 0.0233(9) 0.0093(7) 0.0029(7) 0.0026(7)
C8 0.0213(9) 0.0248(9) 0.0268(9) 0.0114(7) -0.0023(7) -0.0061(7)
C9 0.0333(10) 0.0166(8) 0.0213(9) 0.0051(7) -0.0027(7) -0.0030(7)
C10 0.0264(9) 0.0200(9) 0.0227(9) 0.0050(7) 0.0026(7) 0.0049(7)
C11 0.0174(8) 0.0233(9) 0.0232(9) 0.0051(7) -0.0002(7) -0.0010(7)
C12 0.0214(9) 0.0183(8) 0.0237(9) 0.0021(7) -0.0011(7) -0.0007(7)
C13 0.0256(9) 0.0221(9) 0.0276(10) 0.0038(7) 0.0005(7) 0.0019(7)
C14 0.0391(11) 0.0275(10) 0.0334(11) 0.0117(9) -0.0085(9) 0.0004(9)
C15 0.0470(13) 0.0318(11) 0.0230(10) 0.0077(8) 0.0002(9) -0.0079(9)
C16 0.0349(11) 0.0301(10) 0.0258(10) -0.0020(8) 0.0074(8) -0.0027(8)
C17 0.0257(9) 0.0232(9) 0.0260(9) 0.0029(7) 0.0008(7) 0.0012(7)
C21 0.0286(10) 0.0261(10) 0.0326(11) 0.0066(8) 0.0013(8) -0.0004(8)
C22 0.0303(10) 0.0218(9) 0.0260(10) 0.0010(7) 0.0019(8) 0.0029(8)
C23 0.0259(9) 0.0218(9) 0.0269(10) 0.0037(7) 0.0020(8) 0.0051(8)
B1 0.0187(9) 0.0181(9) 0.0234(10) 0.0040(8) 0.0013(8) 0.0032(7)
O21 0.0510(10) 0.0537(10) 0.0270(8) 0.0128(7) -0.0021(7) -0.0025(8)
O22 0.0290(8) 0.0382(8) 0.0440(9) 0.0063(7) 0.0048(6) 0.0130(7)
O23 0.0335(8) 0.0254(7) 0.0460(9) 0.0061(6) 0.0021(7) -0.0037(6)
F7 0.0174(5) 0.0286(6) 0.0394(6) 0.0074(5) 0.0047(5) 0.0023(4)
F8 0.0232(6) 0.0311(6) 0.0436(7) 0.0098(5) -0.0033(5) -0.0098(5)
F9 0.0435(7) 0.0187(5) 0.0353(6) 0.0002(5) -0.0041(5) -0.0057(5)
F10 0.0315(6) 0.0249(6) 0.0332(6) -0.0017(5) 0.0039(5) 0.0079(5)
F11 0.0170(5) 0.0271(6) 0.0394(6) -0.0022(5) 0.0020(4) 0.0017(4)
F13 0.0294(6) 0.0297(6) 0.0388(7) 0.0112(5) 0.0031(5) 0.0111(5)
F14 0.0576(9) 0.0467(8) 0.0459(8) 0.0256(6) -0.0082(6) 0.0096(7)
F15 0.0741(10) 0.0512(8) 0.0245(6) 0.0143(6) 0.0042(6) -0.0060(7)
F16 0.0476(8) 0.0475(8) 0.0339(7) 0.0005(6) 0.0188(6) 0.0032(6)
F17 0.0311(6) 0.0367(7) 0.0325(6) 0.0057(5) 0.0055(5) 0.0142(5)
Fe1 0.01969(13) 0.01719(13) 0.02232(14) 0.00325(10) 0.00171(10) 0.00218(9)

_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 1.428(3) . ?
C1 C2 1.438(2) . ?
C1 B1 1.615(3) . ?
C1 Fe1 2.1369(17) . ?
C2 C3 1.415(3) . ?
C2 Fe1 2.0993(18) . ?
C2 H2 0.950 . ?
C3 C4 1.421(3) . ?
C3 Fe1 2.0968(18) . ?
C3 H3 0.950 . ?
C4 C5 1.419(3) . ?
C4 Fe1 2.0900(18) . ?
C4 H4 0.950 . ?
C5 Fe1 2.0980(17) . ?
C5 H5 0.950 . ?
C6 C11 1.388(2) . ?
C6 C7 1.392(2) . ?
C6 B1 1.646(3) . ?
C7 F7 1.352(2) . ?
C7 C8 1.374(3) . ?
C8 F8 1.351(2) . ?
C8 C9 1.378(3) . ?
C9 F9 1.343(2) . ?
C9 C10 1.374(3) . ?
C10 F10 1.346(2) . ?
C10 C11 1.385(2) . ?
C11 F11 1.348(2) . ?
C12 C13 1.384(3) . ?
C12 C17 1.388(3) . ?
C12 B1 1.641(3) . ?
C13 F13 1.360(2) . ?
C13 C14 1.379(3) . ?
C14 F14 1.342(2) . ?
C14 C15 1.378(3) . ?
C15 F15 1.345(2) . ?
C15 C16 1.370(3) . ?
C16 F16 1.348(2) . ?
C16 C17 1.379(3) . ?
C17 F17 1.358(2) . ?
C21 O21 1.133(2) . ?
C21 Fe1 1.799(2) . ?
C22 O22 1.135(2) . ?
C22 Fe1 1.805(2) . ?
C23 O23 1.130(2) . ?
C23 Fe1 1.8175(19) . ?
B1 H1B 1.16(2) . ?

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 104.68(15) . . ?
C5 C1 B1 132.64(16) . . ?
C2 C1 B1 122.58(16) . . ?
C5 C1 Fe1 68.83(10) . . ?
C2 C1 Fe1 68.75(10) . . ?
B1 C1 Fe1 128.82(12) . . ?
C3 C2 C1 110.25(16) . . ?
C3 C2 Fe1 70.20(10) . . ?
C1 C2 Fe1 71.57(10) . . ?
C3 C2 H2 124.9 . . ?
C1 C2 H2 124.9 . . ?
Fe1 C2 H2 124.9 . . ?
C2 C3 C4 107.33(16) . . ?
C2 C3 Fe1 70.40(10) . . ?
C4 C3 Fe1 69.90(10) . . ?
C2 C3 H3 126.3 . . ?
C4 C3 H3 126.3 . . ?
Fe1 C3 H3 125.0 . . ?
C5 C4 C3 107.48(16) . . ?
C5 C4 Fe1 70.50(10) . . ?
C3 C4 Fe1 70.41(10) . . ?
C5 C4 H4 126.3 . . ?
C3 C4 H4 126.3 . . ?
Fe1 C4 H4 124.5 . . ?
C4 C5 C1 110.26(17) . . ?
C4 C5 Fe1 69.89(10) . . ?
C1 C5 Fe1 71.77(10) . . ?
C4 C5 H5 124.9 . . ?
C1 C5 H5 124.9 . . ?
Fe1 C5 H5 125.0 . . ?
C11 C6 C7 114.01(16) . . ?
C11 C6 B1 126.82(15) . . ?
C7 C6 B1 119.12(15) . . ?
F7 C7 C8 116.65(16) . . ?
F7 C7 C6 119.34(16) . . ?
C8 C7 C6 124.01(16) . . ?
F8 C8 C7 121.16(17) . . ?
F8 C8 C9 119.24(16) . . ?
C7 C8 C9 119.59(16) . . ?
F9 C9 C10 120.17(17) . . ?
F9 C9 C8 120.72(17) . . ?
C10 C9 C8 119.10(17) . . ?
F10 C10 C9 119.49(16) . . ?
F10 C10 C11 120.94(16) . . ?
C9 C10 C11 119.57(17) . . ?
F11 C11 C10 115.62(15) . . ?
F11 C11 C6 120.66(15) . . ?
C10 C11 C6 123.71(16) . . ?
C13 C12 C17 113.25(17) . . ?
C13 C12 B1 122.84(16) . . ?
C17 C12 B1 123.54(16) . . ?
F13 C13 C14 115.87(17) . . ?
F13 C13 C12 119.16(16) . . ?
C14 C13 C12 124.96(18) . . ?
F14 C14 C15 119.84(19) . . ?
F14 C14 C13 121.33(19) . . ?
C15 C14 C13 118.82(19) . . ?
F15 C15 C16 120.57(19) . . ?
F15 C15 C14 120.3(2) . . ?
C16 C15 C14 119.14(18) . . ?
F16 C16 C15 119.64(18) . . ?
F16 C16 C17 120.64(19) . . ?
C15 C16 C17 119.72(18) . . ?
F17 C17 C16 115.64(16) . . ?
F17 C17 C12 120.27(16) . . ?
C16 C17 C12 124.08(18) . . ?
O21 C21 Fe1 178.29(19) . . ?
O22 C22 Fe1 177.50(18) . . ?
O23 C23 Fe1 176.45(17) . . ?
C1 B1 C12 115.43(15) . . ?
C1 B1 C6 111.15(14) . . ?
C12 B1 C6 106.87(14) . . ?
C1 B1 H1B 105.5(10) . . ?
C12 B1 H1B 110.1(10) . . ?
C6 B1 H1B 107.6(10) . . ?
C21 Fe1 C22 94.70(9) . . ?
C21 Fe1 C23 93.14(9) . . ?
C22 Fe1 C23 97.62(8) . . ?
C21 Fe1 C4 108.39(8) . . ?
C22 Fe1 C4 153.94(8) . . ?
C23 Fe1 C4 93.13(8) . . ?
C21 Fe1 C3 148.06(8) . . ?
C22 Fe1 C3 116.23(8) . . ?
C23 Fe1 C3 90.56(8) . . ?
C4 Fe1 C3 39.69(8) . . ?
C21 Fe1 C5 87.05(8) . . ?
C22 Fe1 C5 133.91(8) . . ?
C23 Fe1 C5 128.33(8) . . ?
C4 Fe1 C5 39.61(7) . . ?
C3 Fe1 C5 66.19(7) . . ?
C21 Fe1 C2 143.03(8) . . ?
C22 Fe1 C2 88.23(8) . . ?
C23 Fe1 C2 123.04(8) . . ?
C4 Fe1 C2 66.09(7) . . ?
C3 Fe1 C2 39.40(7) . . ?
C5 Fe1 C2 65.45(7) . . ?
C21 Fe1 C1 103.50(8) . . ?
C22 Fe1 C1 96.40(8) . . ?
C23 Fe1 C1 157.23(8) . . ?
C4 Fe1 C1 67.08(7) . . ?
C3 Fe1 C1 67.12(7) . . ?
C5 Fe1 C1 39.40(7) . . ?
C2 Fe1 C1 39.69(7) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.062

#===END

data_3
_database_code_depnum_ccdc_archive 'CCDC 602511'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H4 B F11 Fe O3'
_chemical_formula_sum            'C20 H4 B F11 Fe O3'
_chemical_formula_weight         567.89

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'
B B 0.0013 0.0007 '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'
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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.5733(4)
_cell_length_b                   8.4751(4)
_cell_length_c                   15.5751(7)
_cell_angle_alpha                103.050(2)
_cell_angle_beta                 90.431(2)
_cell_angle_gamma                92.131(2)
_cell_volume                     973.06(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    6323
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      28.82

_exptl_crystal_description       block
_exptl_crystal_colour            'pale brown'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             556
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.6751
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX2 CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        5
_diffrn_reflns_number            10183
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         28.81
_reflns_number_total             5501
_reflns_number_gt                5117
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0606P)^2^+0.3416P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5501
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.1011
_refine_ls_wR_factor_gt          0.0992
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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
Fe Fe 0.97835(2) 0.61772(2) 0.255636(12) 0.01775(8) Uani 1 1 d . . .
C1 C 0.7702(2) 0.71843(17) 0.26447(10) 0.0242(3) Uani 1 1 d . . .
O1 O 0.63868(16) 0.77891(15) 0.26901(9) 0.0336(3) Uani 1 1 d . . .
C2 C 1.1211(2) 0.79922(17) 0.26836(10) 0.0244(3) Uani 1 1 d . . .
O2 O 1.21694(17) 0.90673(15) 0.27655(9) 0.0348(3) Uani 1 1 d . . .
C3 C 0.9936(2) 0.61750(19) 0.37125(11) 0.0276(3) Uani 1 1 d . . .
O3 O 1.0080(2) 0.61614(19) 0.44317(9) 0.0431(3) Uani 1 1 d . . .
C4 C 1.05330(18) 0.37535(16) 0.22970(11) 0.0235(3) Uani 1 1 d . . .
H4 H 1.0867 0.3184 0.2729 0.028 Uiso 1 1 calc R . .
C5 C 1.17123(18) 0.46869(17) 0.18821(11) 0.0255(3) Uani 1 1 d . . .
H5 H 1.2948 0.4857 0.1991 0.031 Uiso 1 1 calc R . .
C6 C 1.06935(19) 0.53196(17) 0.12723(10) 0.0242(3) Uani 1 1 d . . .
H6 H 1.1131 0.5983 0.0898 0.029 Uiso 1 1 calc R . .
C7 C 0.89133(18) 0.47815(16) 0.13244(9) 0.0206(2) Uani 1 1 d . . .
H7 H 0.7957 0.5031 0.0986 0.025 Uiso 1 1 calc R . .
C8 C 0.87670(17) 0.37989(15) 0.19671(9) 0.0188(2) Uani 1 1 d . . .
B B 0.68887(18) 0.29576(17) 0.21425(10) 0.0181(2) Uani 1 1 d . . .
F1 F 0.56122(12) 0.40171(12) 0.19309(7) 0.0286(2) Uani 1 1 d . . .
C9 C 0.65828(17) 0.11521(16) 0.14751(9) 0.0188(2) Uani 1 1 d . . .
C10 C 0.78924(18) 0.01536(16) 0.10643(9) 0.0208(2) Uani 1 1 d . . .
F10 F 0.96092(11) 0.06559(11) 0.11552(7) 0.02811(19) Uani 1 1 d . . .
C11 C 0.7558(2) -0.13956(17) 0.05529(9) 0.0238(3) Uani 1 1 d . . .
F11 F 0.88860(14) -0.23084(11) 0.01849(7) 0.0327(2) Uani 1 1 d . . .
C12 C 0.5840(2) -0.20108(17) 0.04294(10) 0.0257(3) Uani 1 1 d . . .
F12 F 0.54995(16) -0.35069(12) -0.00588(7) 0.0376(2) Uani 1 1 d . . .
C13 C 0.4487(2) -0.10729(18) 0.08209(10) 0.0247(3) Uani 1 1 d . . .
F13 F 0.28111(13) -0.16650(13) 0.06986(8) 0.0351(2) Uani 1 1 d . . .
C14 C 0.48762(18) 0.04656(17) 0.13282(9) 0.0208(2) Uani 1 1 d . . .
F14 F 0.34940(11) 0.13072(11) 0.17017(7) 0.02835(19) Uani 1 1 d . . .
C15 C 0.66070(18) 0.26925(16) 0.31471(9) 0.0204(2) Uani 1 1 d . . .
C16 C 0.7635(2) 0.16373(17) 0.34822(10) 0.0242(3) Uani 1 1 d . . .
F16 F 0.89839(13) 0.09161(12) 0.29921(7) 0.0303(2) Uani 1 1 d . . .
C17 C 0.7377(2) 0.1223(2) 0.42807(11) 0.0316(3) Uani 1 1 d . . .
F17 F 0.84259(18) 0.01785(15) 0.45476(8) 0.0469(3) Uani 1 1 d . . .
C18 C 0.6009(3) 0.1885(2) 0.48002(11) 0.0347(4) Uani 1 1 d . . .
F18 F 0.5738(2) 0.15236(16) 0.55850(7) 0.0501(3) Uani 1 1 d . . .
C19 C 0.4923(2) 0.2920(2) 0.45018(11) 0.0315(3) Uani 1 1 d . . .
F19 F 0.35613(17) 0.35553(15) 0.49972(8) 0.0450(3) Uani 1 1 d . . .
C20 C 0.5243(2) 0.33176(18) 0.36985(10) 0.0248(3) Uani 1 1 d . . .
F20 F 0.41251(13) 0.43643(13) 0.34753(7) 0.0331(2) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe 0.01603(11) 0.01526(11) 0.02198(11) 0.00411(7) 0.00146(7) 0.00140(7)
C1 0.0257(6) 0.0209(6) 0.0254(6) 0.0034(5) 0.0021(5) 0.0035(5)
O1 0.0269(5) 0.0329(6) 0.0403(6) 0.0048(5) 0.0046(5) 0.0121(4)
C2 0.0258(7) 0.0204(6) 0.0266(7) 0.0045(5) 0.0022(5) 0.0018(5)
O2 0.0337(6) 0.0255(5) 0.0445(7) 0.0081(5) 0.0019(5) -0.0072(4)
C3 0.0283(7) 0.0260(7) 0.0294(7) 0.0083(6) -0.0001(5) -0.0002(5)
O3 0.0491(8) 0.0520(8) 0.0307(6) 0.0155(6) -0.0025(5) -0.0027(6)
C4 0.0177(6) 0.0169(6) 0.0357(7) 0.0051(5) -0.0017(5) 0.0029(4)
C5 0.0158(6) 0.0200(6) 0.0390(8) 0.0025(5) 0.0053(5) 0.0024(4)
C6 0.0229(6) 0.0206(6) 0.0271(7) 0.0013(5) 0.0090(5) 0.0002(5)
C7 0.0207(6) 0.0186(6) 0.0214(6) 0.0022(5) 0.0034(4) 0.0018(4)
C8 0.0168(5) 0.0139(5) 0.0250(6) 0.0025(4) 0.0007(4) 0.0022(4)
B 0.0149(6) 0.0166(6) 0.0232(6) 0.0054(5) 0.0012(5) 0.0015(4)
F1 0.0219(4) 0.0295(5) 0.0369(5) 0.0119(4) 0.0016(3) 0.0048(3)
C9 0.0174(5) 0.0185(6) 0.0213(6) 0.0063(4) 0.0008(4) 0.0002(4)
C10 0.0201(6) 0.0192(6) 0.0229(6) 0.0047(5) 0.0011(4) -0.0006(4)
F10 0.0175(4) 0.0245(4) 0.0387(5) -0.0008(4) 0.0042(3) 0.0015(3)
C11 0.0301(7) 0.0182(6) 0.0232(6) 0.0045(5) 0.0036(5) 0.0033(5)
F11 0.0393(5) 0.0223(4) 0.0338(5) -0.0004(4) 0.0080(4) 0.0083(4)
C12 0.0382(8) 0.0165(6) 0.0223(6) 0.0054(5) -0.0032(5) -0.0052(5)
F12 0.0557(7) 0.0187(4) 0.0352(5) 0.0009(4) -0.0052(5) -0.0092(4)
C13 0.0256(7) 0.0235(6) 0.0266(7) 0.0110(5) -0.0040(5) -0.0085(5)
F13 0.0287(5) 0.0324(5) 0.0442(6) 0.0116(4) -0.0067(4) -0.0155(4)
C14 0.0189(6) 0.0209(6) 0.0241(6) 0.0087(5) 0.0002(4) -0.0007(4)
F14 0.0167(4) 0.0277(4) 0.0412(5) 0.0091(4) 0.0044(3) -0.0001(3)
C15 0.0203(6) 0.0178(6) 0.0225(6) 0.0037(5) -0.0005(4) 0.0002(4)
C16 0.0256(7) 0.0209(6) 0.0263(7) 0.0055(5) -0.0017(5) 0.0016(5)
F16 0.0282(5) 0.0272(4) 0.0381(5) 0.0115(4) 0.0013(4) 0.0097(3)
C17 0.0400(9) 0.0268(7) 0.0299(7) 0.0108(6) -0.0070(6) -0.0011(6)
F17 0.0611(8) 0.0421(6) 0.0451(6) 0.0251(5) -0.0109(5) 0.0081(5)
C18 0.0518(10) 0.0308(8) 0.0213(7) 0.0071(6) -0.0005(6) -0.0078(7)
F18 0.0789(9) 0.0494(7) 0.0243(5) 0.0143(5) 0.0048(5) -0.0067(6)
C19 0.0376(8) 0.0300(8) 0.0238(7) 0.0000(6) 0.0085(6) -0.0032(6)
F19 0.0498(7) 0.0487(7) 0.0325(5) 0.0002(5) 0.0199(5) 0.0018(5)
C20 0.0252(6) 0.0234(6) 0.0242(6) 0.0022(5) 0.0022(5) 0.0015(5)
F20 0.0286(5) 0.0381(5) 0.0330(5) 0.0067(4) 0.0072(4) 0.0140(4)

_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
Fe C1 1.8118(15) . ?
Fe C2 1.8193(15) . ?
Fe C3 1.8040(16) . ?
Fe C4 2.1024(13) . ?
Fe C5 2.0961(14) . ?
Fe C6 2.0987(14) . ?
Fe C7 2.1008(14) . ?
Fe C8 2.1298(13) . ?
C1 O1 1.1325(19) . ?
C2 O2 1.1270(19) . ?
C3 O3 1.127(2) . ?
C4 H4 0.950 . ?
C4 C5 1.424(2) . ?
C4 C8 1.4341(18) . ?
C5 H5 0.950 . ?
C5 C6 1.426(2) . ?
C6 H6 0.950 . ?
C6 C7 1.4159(19) . ?
C7 H7 0.950 . ?
C7 C8 1.4419(19) . ?
C8 B 1.6201(19) . ?
B F1 1.4293(16) . ?
B C9 1.651(2) . ?
B C15 1.645(2) . ?
C9 C10 1.3917(19) . ?
C9 C14 1.3931(18) . ?
C10 F10 1.3493(16) . ?
C10 C11 1.3865(19) . ?
C11 F11 1.3435(17) . ?
C11 C12 1.379(2) . ?
C12 F12 1.3378(16) . ?
C12 C13 1.380(2) . ?
C13 F13 1.3437(16) . ?
C13 C14 1.383(2) . ?
C14 F14 1.3491(16) . ?
C15 C16 1.3907(19) . ?
C15 C20 1.3904(19) . ?
C16 F16 1.3594(17) . ?
C16 C17 1.380(2) . ?
C17 F17 1.3423(19) . ?
C17 C18 1.376(3) . ?
C18 F18 1.3410(19) . ?
C18 C19 1.375(3) . ?
C19 F19 1.3473(19) . ?
C19 C20 1.388(2) . ?
C20 F20 1.3475(18) . ?

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
C1 Fe C2 96.85(7) . . ?
C1 Fe C3 94.66(7) . . ?
C1 Fe C4 135.26(6) . . ?
C1 Fe C5 154.16(7) . . ?
C1 Fe C6 115.93(6) . . ?
C1 Fe C7 88.48(6) . . ?
C1 Fe C8 97.41(6) . . ?
C2 Fe C3 92.93(7) . . ?
C2 Fe C4 127.74(6) . . ?
C2 Fe C5 92.65(6) . . ?
C2 Fe C6 90.55(6) . . ?
C2 Fe C7 123.17(6) . . ?
C2 Fe C8 157.20(6) . . ?
C3 Fe C4 87.30(7) . . ?
C3 Fe C5 108.82(7) . . ?
C3 Fe C6 148.55(7) . . ?
C3 Fe C7 143.17(6) . . ?
C3 Fe C8 103.53(6) . . ?
C4 Fe C5 39.66(6) . . ?
C4 Fe C6 66.25(6) . . ?
C4 Fe C7 65.75(6) . . ?
C4 Fe C8 39.61(5) . . ?
C5 Fe C6 39.76(6) . . ?
C5 Fe C7 66.33(6) . . ?
C5 Fe C8 67.30(5) . . ?
C6 Fe C7 39.41(5) . . ?
C6 Fe C8 67.19(5) . . ?
C7 Fe C8 39.85(5) . . ?
Fe C1 O1 178.74(15) . . ?
Fe C2 O2 176.35(14) . . ?
Fe C3 O3 178.05(16) . . ?
Fe C4 H4 125.4 . . ?
Fe C4 C5 69.93(8) . . ?
Fe C4 C8 71.23(7) . . ?
H4 C4 C5 125.0 . . ?
H4 C4 C8 125.0 . . ?
C5 C4 C8 110.03(13) . . ?
Fe C5 C4 70.41(8) . . ?
Fe C5 H5 124.6 . . ?
Fe C5 C6 70.22(8) . . ?
C4 C5 H5 126.3 . . ?
C4 C5 C6 107.30(12) . . ?
H5 C5 C6 126.3 . . ?
Fe C6 C5 70.02(8) . . ?
Fe C6 H6 125.1 . . ?
Fe C6 C7 70.38(8) . . ?
C5 C6 H6 126.1 . . ?
C5 C6 C7 107.75(12) . . ?
H6 C6 C7 126.1 . . ?
Fe C7 C6 70.22(8) . . ?
Fe C7 H7 125.2 . . ?
Fe C7 C8 71.16(8) . . ?
C6 C7 H7 125.0 . . ?
C6 C7 C8 109.91(12) . . ?
H7 C7 C8 125.0 . . ?
Fe C8 C4 69.17(7) . . ?
Fe C8 C7 68.99(7) . . ?
Fe C8 B 127.96(9) . . ?
C4 C8 C7 105.00(12) . . ?
C4 C8 B 133.98(12) . . ?
C7 C8 B 120.95(11) . . ?
C8 B F1 103.91(10) . . ?
C8 B C9 111.16(11) . . ?
C8 B C15 115.73(11) . . ?
F1 B C9 108.94(11) . . ?
F1 B C15 110.81(11) . . ?
C9 B C15 106.21(10) . . ?
B C9 C10 126.48(11) . . ?
B C9 C14 119.21(12) . . ?
C10 C9 C14 114.20(12) . . ?
C9 C10 F10 120.67(12) . . ?
C9 C10 C11 123.77(13) . . ?
F10 C10 C11 115.56(12) . . ?
C10 C11 F11 120.84(13) . . ?
C10 C11 C12 119.44(13) . . ?
F11 C11 C12 119.71(13) . . ?
C11 C12 F12 120.04(15) . . ?
C11 C12 C13 119.27(13) . . ?
F12 C12 C13 120.69(14) . . ?
C12 C13 F13 119.43(13) . . ?
C12 C13 C14 119.54(13) . . ?
F13 C13 C14 121.03(14) . . ?
C9 C14 C13 123.78(13) . . ?
C9 C14 F14 119.78(12) . . ?
C13 C14 F14 116.43(12) . . ?
B C15 C16 121.21(12) . . ?
B C15 C20 124.97(12) . . ?
C16 C15 C20 113.43(13) . . ?
C15 C16 F16 118.89(13) . . ?
C15 C16 C17 125.00(15) . . ?
F16 C16 C17 116.10(13) . . ?
C16 C17 F17 120.91(16) . . ?
C16 C17 C18 118.98(15) . . ?
F17 C17 C18 120.11(15) . . ?
C17 C18 F18 120.41(17) . . ?
C17 C18 C19 119.02(15) . . ?
F18 C18 C19 120.57(17) . . ?
C18 C19 F19 119.64(15) . . ?
C18 C19 C20 120.07(15) . . ?
F19 C19 C20 120.29(16) . . ?
C15 C20 C19 123.48(14) . . ?
C15 C20 F20 121.15(13) . . ?
C19 C20 F20 115.37(14) . . ?

_diffrn_measured_fraction_theta_max 0.928
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.944
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.061

#===END