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.
Zhang, Jian; Deng, Liang; Chan, Hoi-Shan; Xie, Zuowei; Journal of the American Chemical Society 129 (2007) 18–19; doi:10.1021/ja067129e

data_4101760
_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/[\s^2^(Fo^2^)+(0.1487P)^2^+0.1601P] where P=(Fo^2^+2Fc^2^)/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