#------------------------------------------------------------------------------
#$Date: 2016-03-21 16:59:14 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178763 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/17/4101760.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_4101760
loop_
_publ_author_name
'Zhang, Jian'
'Deng, Liang'
'Chan, Hoi-Shan'
'Xie, Zuowei'
_publ_section_title
;
 Role of c,c'-linkage in the formation and stabilization of
 supercarboranes. Synthesis and structure of carbon-atoms-apart 13-vertex
 carborane and 14-vertex metallacarborane.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18
_journal_page_last               19
_journal_paper_doi               10.1021/ja067129e
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C4 H17 B11'
_chemical_formula_weight         184.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 115.576(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.0551(9)
_cell_length_b                   11.6875(14)
_cell_length_c                   8.0262(10)
_cell_measurement_temperature    293(2)
_cell_volume                     596.96(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'BRUKER SMART CCD DIFFRACOMETER'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3274
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    0.043
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9829
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.024
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             192
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0724
_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)+(0.1487P)²+0.1601P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2121
_refine_ls_wR_factor_ref         0.2415
_reflns_number_gt                817
_reflns_number_total             1109
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja067129esi20061005_033852.cif
_cod_data_source_block           3a
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               4101760
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
B3 B 0.9816(5) 0.2500 0.0878(5) 0.0495(9) Uani 1 2 d S . .
B4 B 0.8454(4) 0.1103(2) 0.1102(4) 0.0536(8) Uani 1 1 d . . .
B5 B 0.5972(4) 0.1671(2) 0.0929(4) 0.0489(7) Uani 1 1 d . . .
B6 B 1.0444(4) 0.1753(3) 0.3072(4) 0.0563(8) Uani 1 1 d . . .
B7 B 0.8079(5) 0.1259(3) 0.3097(4) 0.0614(9) Uani 1 1 d . . .
B8 B 0.6555(6) 0.2500 0.2911(5) 0.0571(11) Uani 1 2 d S . .
B9 B 0.9311(7) 0.2500 0.4331(5) 0.0655(12) Uani 1 2 d S . .
C1 C 0.7137(4) 0.1892(2) -0.0647(3) 0.0562(8) Uani 1 1 d . . .
C11 C 0.6373(6) 0.1257(3) -0.2475(4) 0.0964(13) Uani 1 1 d . . .
H11A H 0.4918 0.1062 -0.2893 0.145 Uiso 1 1 calc R . .
H11B H 0.7183 0.0571 -0.2310 0.145 Uiso 1 1 calc R . .
H11C H 0.6537 0.1737 -0.3375 0.145 Uiso 1 1 calc R . .
H3 H 1.076(6) 0.2500 0.020(5) 0.063(10) Uiso 1 2 d S . .
H5 H 0.454(4) 0.123(2) 0.028(4) 0.066(7) Uiso 1 1 d . . .
H8 H 0.544(7) 0.2500 0.337(6) 0.086(13) Uiso 1 2 d S . .
H6 H 1.194(4) 0.129(3) 0.364(4) 0.078(8) Uiso 1 1 d . . .
H9 H 0.994(6) 0.2500 0.595(6) 0.088(13) Uiso 1 2 d S . .
H4 H 0.871(5) 0.023(3) 0.070(4) 0.085(9) Uiso 1 1 d . . .
H7 H 0.806(5) 0.045(3) 0.387(5) 0.091(9) Uiso 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'
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
B6 B3 B6 56.6(2) 4_565 . ?
B6 B3 C1 123.9(2) 4_565 . ?
B6 B3 C1 101.62(17) . . ?
B6 B3 C1 101.62(17) 4_565 4_565 ?
B6 B3 C1 123.9(2) . 4_565 ?
C1 B3 C1 44.11(18) . 4_565 ?
B6 B3 B4 103.6(2) 4_565 . ?
B6 B3 B4 55.72(14) . . ?
C1 B3 B4 49.30(13) . . ?
C1 B3 B4 88.82(18) 4_565 . ?
B6 B3 B4 55.72(14) 4_565 4_565 ?
B6 B3 B4 103.6(2) . 4_565 ?
C1 B3 B4 88.82(18) . 4_565 ?
C1 B3 B4 49.30(13) 4_565 4_565 ?
B4 B3 B4 114.4(2) . 4_565 ?
C1 B4 B7 119.0(2) . . ?
C1 B4 B6 118.2(2) . . ?
B7 B4 B6 60.69(16) . . ?
C1 B4 B5 63.09(15) . . ?
B7 B4 B5 60.60(16) . . ?
B6 B4 B5 106.10(19) . . ?
C1 B4 B3 63.69(16) . . ?
B7 B4 B3 105.9(2) . . ?
B6 B4 B3 59.21(16) . . ?
B5 B4 B3 100.60(18) . . ?
B8 B5 B7 59.86(16) . . ?
B8 B5 C1 123.98(19) . . ?
B7 B5 C1 106.31(17) . . ?
B8 B5 B4 106.92(19) . . ?
B7 B5 B4 57.51(16) . . ?
C1 B5 B4 52.43(14) . . ?
B8 B5 B5 56.46(11) . 4_565 ?
B7 B5 B5 105.53(14) . 4_565 ?
C1 B5 B5 81.76(12) . 4_565 ?
B4 B5 B5 111.41(12) . 4_565 ?
B6 B6 B9 60.39(12) 4_565 . ?
B6 B6 B4 115.44(13) 4_565 . ?
B9 B6 B4 110.0(2) . . ?
B6 B6 B7 108.99(14) 4_565 . ?
B9 B6 B7 59.58(18) . . ?
B4 B6 B7 58.88(16) . . ?
B6 B6 B3 61.68(11) 4_565 . ?
B9 B6 B3 109.37(19) . . ?
B4 B6 B3 65.07(15) . . ?
B7 B6 B3 109.05(18) . . ?
B4 B7 B9 111.7(2) . . ?
B4 B7 B8 109.6(2) . . ?
B9 B7 B8 60.49(19) . . ?
B4 B7 B6 60.43(16) . . ?
B9 B7 B6 60.0(2) . . ?
B8 B7 B6 105.8(2) . . ?
B4 B7 B5 61.89(15) . . ?
B9 B7 B5 108.9(2) . . ?
B8 B7 B5 58.76(17) . . ?
B6 B7 B5 106.87(18) . . ?
B5 B8 B5 67.1(2) . 4_565 ?
B5 B8 B7 115.2(2) . 4_565 ?
B5 B8 B7 61.38(15) 4_565 4_565 ?
B5 B8 B7 61.38(15) . . ?
B5 B8 B7 115.2(2) 4_565 . ?
B7 B8 B7 109.8(3) 4_565 . ?
B5 B8 B9 110.2(2) . . ?
B5 B8 B9 110.2(2) 4_565 . ?
B7 B8 B9 59.39(15) 4_565 . ?
B7 B8 B9 59.39(15) . . ?
B7 B9 B7 111.0(3) . 4_565 ?
B7 B9 B6 60.42(16) . . ?
B7 B9 B6 108.7(2) 4_565 . ?
B7 B9 B6 108.7(2) . 4_565 ?
B7 B9 B6 60.42(16) 4_565 4_565 ?
B6 B9 B6 59.2(2) . 4_565 ?
B7 B9 B8 60.12(16) . . ?
B7 B9 B8 60.12(16) 4_565 . ?
B6 B9 B8 105.8(2) . . ?
B6 B9 B8 105.8(2) 4_565 . ?
C1 C1 C11 119.23(17) 4_565 . ?
C1 C1 B4 125.23(13) 4_565 . ?
C11 C1 B4 113.2(2) . . ?
C1 C1 B5 98.24(12) 4_565 . ?
C11 C1 B5 121.9(2) . . ?
B4 C1 B5 64.48(15) . . ?
C1 C1 B3 67.95(9) 4_565 . ?
C11 C1 B3 130.3(2) . . ?
B4 C1 B3 67.00(14) . . ?
B5 C1 B3 103.37(17) . . ?
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
B3 B6 1.840(4) 4_565 ?
B3 B6 1.840(4) . ?
B3 C1 1.892(4) . ?
B3 C1 1.892(4) 4_565 ?
B3 B4 1.942(3) . ?
B3 B4 1.942(3) 4_565 ?
B4 C1 1.600(4) . ?
B4 B7 1.742(4) . ?
B4 B6 1.770(4) . ?
B4 B5 1.822(4) . ?
B5 B8 1.752(4) . ?
B5 B7 1.799(4) . ?
B5 C1 1.800(3) . ?
B5 B5 1.937(5) 4_565 ?
B6 B6 1.746(6) 4_565 ?
B6 B9 1.767(5) . ?
B6 B7 1.774(4) . ?
B7 B9 1.759(4) . ?
B7 B8 1.773(4) . ?
B8 B5 1.752(4) 4_565 ?
B8 B7 1.773(4) 4_565 ?
B8 B9 1.779(5) . ?
B9 B7 1.759(4) 4_565 ?
B9 B6 1.767(5) 4_565 ?
C1 C1 1.421(5) 4_565 ?
C1 C11 1.520(3) . ?
