#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:54:20 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180114 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/12/7101222.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7101222
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_section_title
;
Migratory insertion of [B(C6F5)2]- into C-H bonds: CO
promoted boryl anion transfer
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/B604141H
_journal_year                    2006
_chemical_formula_moiety         'C20 H4 B F11 Fe O3'
_chemical_formula_sum            'C20 H4 B F11 Fe O3'
_chemical_formula_weight         567.89
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.050(2)
_cell_angle_beta                 90.431(2)
_cell_angle_gamma                92.131(2)
_cell_formula_units_Z            2
_cell_length_a                   7.5733(4)
_cell_length_b                   8.4751(4)
_cell_length_c                   15.5751(7)
_cell_measurement_reflns_used    6323
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.82
_cell_measurement_theta_min      2.34
_cell_volume                     973.06(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Bruker APEX2 CCD diffractometer'
_diffrn_measurement_method       'thin-slice ω scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6751
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10183
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.81
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0606P)²+0.3416P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1011
_reflns_number_gt                5117
_reflns_number_total             5501
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            B604141H.txt
_cod_database_code               7101222
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
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_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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
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)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
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)
