#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:39:08 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178661 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/72/4077264.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_4077264
loop_
_publ_author_name
'Franken, Andreas'
'Du, Shaowu'
'Jelliss, Paul A.'
'Kautz, Jason A.'
'Stone, F. Gordon A.'
_publ_section_title
;
 Cage Substitution Reactions of Monocarbollide Carbonyl Complexes of
 Iron:  Generation of Iminium Groups at a Boron Vertex†
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1597
_journal_paper_doi               10.1021/om001057x
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C7 H17 B10 Fe N O3'
_chemical_formula_weight         327.17
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.755(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2967(13)
_cell_length_b                   8.978(3)
_cell_length_c                   13.820(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      24
_cell_volume                     1552.7(6)
_computing_cell_refinement       'Enraf-Nonius CAD4 (1989)'
_computing_data_collection       'Enraf-Nonius CAD4 (1989)'
_computing_data_reduction        'XCAD4 Siemens Software (Harms, 1993)'
_computing_molecular_graphics    'XP in SHELXTL-PC (Bruker, 1995)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       w-2/3q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0119
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2795
_diffrn_reflns_theta_full        24.81
_diffrn_reflns_theta_max         24.81
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        5.42
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_T_max  0.8140
_exptl_absorpt_correction_T_min  0.6086
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Applied with SHELXTL/PC v 5.03'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         2671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0336P)²+1.8087P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0936
_reflns_number_gt                2437
_reflns_number_total             2671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om001057x.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Numerical'
changed to 'numerical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4077264
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.36043(3) 0.14007(4) 0.21897(3) 0.02300(14) Uani 1 1 d . A .
C1 C 0.2791(2) 0.3347(3) 0.1397(2) 0.0303(7) Uani 1 1 d . A .
H1 H 0.3177 0.3697 0.0844 0.036 Uiso 1 1 calc R . .
B2 B 0.1980(2) 0.1776(4) 0.1134(2) 0.0228(7) Uani 1 1 d . A .
H2 H 0.1818 0.1088 0.0439 0.027 Uiso 1 1 calc R . .
B3 B 0.2057(2) 0.1012(3) 0.2399(2) 0.0229(7) Uani 1 1 d . . .
B4 B 0.2977(3) 0.2183(4) 0.3373(3) 0.0284(7) Uani 1 1 d . A .
H4 H 0.3457 0.1761 0.4137 0.034 Uiso 1 1 calc R . .
B5 B 0.3405(3) 0.3604(4) 0.2696(2) 0.0259(7) Uani 1 1 d . . .
H5 H 0.4199 0.4119 0.3024 0.031 Uiso 1 1 calc R A .
B6 B 0.1420(3) 0.3606(4) 0.1051(3) 0.0288(7) Uani 1 1 d . . .
H6 H 0.0919 0.4074 0.0309 0.035 Uiso 1 1 calc R A .
B7 B 0.0956(2) 0.2163(4) 0.1675(2) 0.0242(7) Uani 1 1 d . A .
H7 H 0.0152 0.1685 0.1331 0.029 Uiso 1 1 calc R . .
B8 B 0.1558(3) 0.2420(4) 0.3035(2) 0.0265(7) Uani 1 1 d . A .
H8 H 0.1141 0.2119 0.3573 0.032 Uiso 1 1 calc R . .
B9 B 0.2419(3) 0.4016(4) 0.3235(3) 0.0333(8) Uani 1 1 d . A .
H9 H 0.2572 0.4750 0.3907 0.040 Uiso 1 1 calc R . .
B10 B 0.2320(3) 0.4732(4) 0.2012(3) 0.0316(8) Uani 1 1 d . A .
H10 H 0.2408 0.5929 0.1889 0.038 Uiso 1 1 calc R . .
B11 B 0.1160(3) 0.3999(4) 0.2212(3) 0.0280(7) Uani 1 1 d . A .
H11 H 0.0491 0.4710 0.2223 0.034 Uiso 1 1 calc R . .
C2 C 0.4591(2) 0.1913(3) 0.1609(2) 0.0331(7) Uani 1 1 d . . .
O2 O 0.52193(19) 0.2229(3) 0.1250(2) 0.0514(7) Uani 1 1 d . A .
C3 C 0.4650(2) 0.0873(3) 0.3356(3) 0.0341(7) Uani 1 1 d . . .
O3 O 0.53255(18) 0.0579(3) 0.40977(18) 0.0495(6) Uani 1 1 d . A .
C4 C 0.3442(2) -0.0395(4) 0.1595(2) 0.0309(7) Uani 1 1 d . . .
O4 O 0.33394(19) -0.1542(3) 0.1211(2) 0.0472(6) Uani 1 1 d . A .
N1A N 0.1543(10) -0.0703(17) 0.2248(12) 0.018(3) Uani 0.270(13) 1 d P A 1
C5A C 0.1660(9) -0.1567(16) 0.2989(10) 0.029(5) Uani 0.270(13) 1 d P A 1
H5B H 0.1371 -0.2517 0.2834 0.035 Uiso 0.270(13) 1 calc PR A 1
C7A C 0.071(3) -0.128(4) 0.119(3) 0.030(7) Uani 0.270(13) 1 d P A 1
H7D H 0.0485 -0.2272 0.1283 0.046 Uiso 0.270(13) 1 calc PR A 1
H7E H 0.1050 -0.1300 0.0676 0.046 Uiso 0.270(13) 1 calc PR A 1
H7F H 0.0106 -0.0632 0.0976 0.046 Uiso 0.270(13) 1 calc PR A 1
C6A C 0.221(3) -0.123(4) 0.407(3) 0.043(7) Uani 0.270(13) 1 d P A 1
H6D H 0.2536 -0.0264 0.4132 0.065 Uiso 0.270(13) 1 calc PR A 1
H6E H 0.2743 -0.1966 0.4368 0.065 Uiso 0.270(13) 1 calc PR A 1
H6F H 0.1698 -0.1225 0.4427 0.065 Uiso 0.270(13) 1 calc PR A 1
N N 0.1849(4) -0.0583(6) 0.2741(4) 0.0189(13) Uani 0.730(13) 1 d P A 2
C5 C 0.1261(4) -0.1604(7) 0.2147(4) 0.0225(16) Uani 0.730(13) 1 d P A 2
H5A H 0.1137 -0.2462 0.2466 0.027 Uiso 0.730(13) 1 calc PR A 2
C6 C 0.0778(9) -0.1538(15) 0.1030(11) 0.032(3) Uani 0.730(13) 1 d P A 2
H6A H 0.0898 -0.0572 0.0793 0.048 Uiso 0.730(13) 1 calc PR A 2
H6B H 0.0024 -0.1716 0.0836 0.048 Uiso 0.730(13) 1 calc PR A 2
H6C H 0.1094 -0.2284 0.0726 0.048 Uiso 0.730(13) 1 calc PR A 2
C7 C 0.2326(10) -0.0985(12) 0.3861(9) 0.030(2) Uani 0.730(13) 1 d P A 2
H7A H 0.2052 -0.1932 0.3978 0.045 Uiso 0.730(13) 1 calc PR A 2
H7B H 0.2141 -0.0238 0.4269 0.045 Uiso 0.730(13) 1 calc PR A 2
H7C H 0.3089 -0.1041 0.4051 0.045 Uiso 0.730(13) 1 calc PR A 2
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'
N N 0.0061 0.0033 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
C4 Fe C3 96.35(14) y
C4 Fe C2 91.04(14) y
C3 Fe C2 90.46(14) y
C4 Fe B5 166.46(12) y
C3 Fe B5 95.38(13) y
C2 Fe B5 95.61(13) y
C4 Fe C1 122.44(13) y
C3 Fe C1 140.68(13) y
C2 Fe C1 83.27(12) y
B5 Fe C1 47.19(12) ?
C4 Fe B2 83.91(12) y
C3 Fe B2 158.14(13) y
C2 Fe B2 111.40(13) y
B5 Fe B2 82.69(12) ?
C1 Fe B2 47.24(11) ?
C4 Fe B4 128.00(13) y
C3 Fe B4 77.82(13) y
C2 Fe B4 139.90(14) y
B5 Fe B4 48.66(12) ?
C1 Fe B4 82.35(12) ?
B2 Fe B4 84.80(12) ?
C4 Fe B3 86.84(12) y
C3 Fe B3 108.28(13) y
C2 Fe B3 161.26(13) y
B5 Fe B3 83.07(12) ?
C1 Fe B3 82.20(11) ?
B2 Fe B3 49.86(11) ?
B4 Fe B3 48.92(12) ?
B5 C1 B6 110.7(2) ?
B5 C1 B2 111.7(2) ?
B6 C1 B2 62.11(18) ?
B5 C1 B10 61.02(19) ?
B6 C1 B10 61.37(19) ?
B2 C1 B10 112.5(2) ?
B5 C1 Fe 66.21(15) ?
B6 C1 Fe 123.32(19) ?
B2 C1 Fe 67.42(14) ?
B10 C1 Fe 122.3(2) ?
C1 B2 B6 58.94(17) ?
C1 B2 B7 105.1(2) ?
B6 B2 B7 59.43(17) ?
C1 B2 B3 105.8(2) ?
B6 B2 B3 106.8(2) ?
B7 B2 B3 59.01(16) ?
C1 B2 Fe 65.33(14) ?
B6 B2 Fe 118.68(19) ?
B7 B2 Fe 117.98(19) ?
B3 B2 Fe 65.48(14) ?
N B3 N1A 23.8(4) ?
N B3 B8 111.4(3) y
N1A B3 B8 120.5(4) y
N B3 B7 120.1(3) y
N1A B3 B7 103.8(5) y
B8 B3 B7 59.96(17) ?
N B3 B4 116.7(3) y
N1A B3 B4 140.5(6) y
B8 B3 B4 59.75(18) ?
B7 B3 B4 107.3(2) ?
N B3 B2 131.9(3) y
N1A B3 B2 109.6(6) y
B8 B3 B2 107.0(2) ?
B7 B3 B2 59.02(16) ?
B4 B3 B2 107.1(2) ?
N B3 Fe 117.1(2) y
N1A B3 Fe 119.5(4) y
B8 B3 Fe 118.12(19) ?
B7 B3 Fe 117.28(18) ?
B4 B3 Fe 65.20(14) ?
B2 B3 Fe 64.66(13) ?
B5 B4 B9 58.71(19) ?
B5 B4 B8 105.8(2) ?
B9 B4 B8 60.16(19) ?
B5 B4 B3 106.2(2) ?
B9 B4 B3 107.6(2) ?
B8 B4 B3 59.41(17) ?
B5 B4 Fe 64.40(15) ?
B9 B4 Fe 117.7(2) ?
B8 B4 Fe 118.4(2) ?
B3 B4 Fe 65.89(14) ?
C1 B5 B9 108.2(2) ?
C1 B5 B10 60.03(18) ?
B9 B5 B10 60.7(2) ?
C1 B5 B4 109.2(2) ?
B9 B5 B4 60.74(19) ?
B10 B5 B4 110.2(2) ?
C1 B5 Fe 66.60(14) ?
B9 B5 Fe 121.8(2) ?
B10 B5 Fe 121.8(2) ?
B4 B5 Fe 66.94(15) ?
C1 B6 B10 59.34(18) ?
C1 B6 B7 105.8(2) ?
B10 B6 B7 108.0(2) ?
C1 B6 B11 106.4(2) ?
B10 B6 B11 60.09(19) ?
B7 B6 B11 60.30(18) ?
C1 B6 B2 58.96(17) ?
B10 B6 B2 108.3(2) ?
B7 B6 B2 60.36(17) ?
B11 B6 B2 109.0(2) ?
B6 B7 B11 60.06(18) ?
B6 B7 B8 108.1(2) ?
B11 B7 B8 59.70(18) ?
B6 B7 B3 109.8(2) ?
B11 B7 B3 108.6(2) ?
B8 B7 B3 59.90(18) ?
B6 B7 B2 60.21(17) ?
B11 B7 B2 108.7(2) ?
B8 B7 B2 109.2(2) ?
B3 B7 B2 61.97(17) ?
B11 B8 B3 109.1(2) ?
B11 B8 B7 60.11(18) ?
B3 B8 B7 60.13(17) ?
B11 B8 B4 108.6(2) ?
B3 B8 B4 60.84(18) ?
B7 B8 B4 108.3(2) ?
B11 B8 B9 59.99(19) ?
B3 B8 B9 108.4(2) ?
B7 B8 B9 107.4(2) ?
B4 B8 B9 59.69(19) ?
B5 B9 B10 59.75(19) ?
B5 B9 B4 60.55(18) ?
B10 B9 B4 109.3(2) ?
B5 B9 B11 107.3(2) ?
B10 B9 B11 60.06(19) ?
B4 B9 B11 108.6(2) ?
B5 B9 B8 107.2(2) ?
B10 B9 B8 107.8(2) ?
B4 B9 B8 60.14(19) ?
B11 B9 B8 59.61(19) ?
C1 B10 B5 58.95(18) ?
C1 B10 B9 106.5(2) ?
B5 B10 B9 59.58(19) ?
C1 B10 B6 59.29(18) ?
B5 B10 B6 107.4(2) ?
B9 B10 B6 108.7(2) ?
C1 B10 B11 106.5(2) ?
B5 B10 B11 107.5(2) ?
B9 B10 B11 60.5(2) ?
B6 B10 B11 60.31(19) ?
B10 B11 B8 107.9(2) ?
B10 B11 B6 59.60(19) ?
B8 B11 B6 108.1(2) ?
B10 B11 B9 59.46(19) ?
B8 B11 B9 60.41(19) ?
B6 B11 B9 107.4(2) ?
B10 B11 B7 107.1(2) ?
B8 B11 B7 60.19(18) ?
B6 B11 B7 59.64(18) ?
B9 B11 B7 107.8(2) ?
O2 C2 Fe 179.4(3) y
O3 C3 Fe 178.0(3) y
O4 C4 Fe 179.7(3) y
C5A N1A C7A 113.8(18) y
C5A N1A B3 122.5(14) y
C7A N1A B3 123.0(15) y
N1A C5A C6A 126.2(19) y
C5 N C7 115.8(6) y
C5 N B3 125.8(5) y
C7 N B3 118.4(6) y
N C5 C6 126.5(7) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Fe C4 1.790(3) y
Fe C3 1.800(3) y
Fe C2 1.813(3) y
Fe B5 2.144(3) y
Fe C1 2.150(3) y
Fe B2 2.185(3) y
Fe B4 2.188(3) y
Fe B3 2.199(3) y
C1 B5 1.719(4) ?
C1 B6 1.737(4) ?
C1 B2 1.737(4) ?
C1 B10 1.738(4) ?
B2 B6 1.792(4) ?
B2 B7 1.795(4) ?
B2 B3 1.848(4) ?
B3 N 1.562(6) y
B3 N1A 1.669(16) y
B3 B8 1.791(4) ?
B3 B7 1.795(4) ?
B3 B4 1.816(5) ?
B4 B5 1.785(5) ?
B4 B9 1.789(5) ?
B4 B8 1.797(4) ?
B5 B9 1.752(5) ?
B5 B10 1.755(5) ?
B6 B10 1.773(5) ?
B6 B7 1.778(4) ?
B6 B11 1.786(5) ?
B7 B11 1.790(5) ?
B7 B8 1.792(4) ?
B8 B11 1.783(5) ?
B8 B9 1.797(5) ?
B9 B10 1.771(5) ?
B9 B11 1.790(5) ?
B10 B11 1.782(4) ?
C2 O2 1.142(4) y
C3 O3 1.142(4) y
C4 O4 1.145(4) y
N1A C5A 1.25(3) y
N1A C7A 1.59(4) y
C5A C6A 1.46(4) y
N C5 1.301(10) y
N C7 1.504(12) y
C5 C6 1.459(15) y
