Boron-Boron σ-Bond Formation by Two-Electron Reduction of a H-Bridged Dimer of Monoborane
Yoshiaki Shoji; Tsukasa Matsuo; Daisuke Hashizume; Matthias J. Gutmann; Hiroyuki Fueno; Kazuyoshi Tanaka; Kohei Tamao; Journal of the American Chemical Society 133 (2011) 11058–11061; doi:10.1021/ja203333j

data_4106454
_publ_section_title
;
 Boron-Boron \s-Bond Formation by Two-Electron Reduction of a H-Bridged
 Dimer of Monoborane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11058
_journal_page_last               11061
_journal_paper_doi               10.1021/ja203333j
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C56 H90 B2 D2'
_chemical_formula_sum            'C56 H90 B2 D2'
_chemical_formula_weight         789.36
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 91.610(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.668(4)
_cell_length_b                   10.302(2)
_cell_length_c                   22.374(5)
_cell_measurement_reflns_used    1100
_cell_measurement_temperature    40
_cell_volume                     4992.4(17)
_computing_cell_refinement       'SXD-2001 (Gutmann, 2005)'
_computing_data_collection       'SXD-2001 (Gutmann, 2005)'
_computing_data_reduction        'SXD-2001 (Gutmann, 2005)'
_computing_molecular_graphics    'ORTEP-3 for Windows'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'previously reported'
_diffrn_ambient_temperature      40
_diffrn_measurement_device_type  SXD
_diffrn_measurement_method       'time-of-flight LAUE diffraction'
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ISIS spallation source'
_diffrn_radiation_type           white-beam
_diffrn_radiation_wavelength     0.48-8.8
_diffrn_reflns_av_R_equivalents  0.1120
_diffrn_reflns_av_sigmaI/netI    0.2084
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            11439
_diffrn_reflns_resolution_full   82.55
_diffrn_reflns_theta_max         82.49
_diffrn_reflns_theta_min         7.75
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.002
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_description       plate
_exptl_crystal_F_000             249
_exptl_crystal_size_max          7.00
_exptl_crystal_size_mid          4.00
_exptl_crystal_size_min          1.00
_refine_diff_density_max         1.687
_refine_diff_density_min         -1.451
_refine_diff_density_rms         0.331
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         5470
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0651
_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^)+(0.0322P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1320
_reflns_number_gt                4603
_reflns_number_total             5470
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja203333j_si_004.cif
_cod_data_source_block           Diborane4-neutron
_cod_original_cell_volume        4992.7(18)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4106454
_diffrn_reflns_sin(theta)/lambda_min 0.03
_diffrn_reflns_sin(theta)/lambda_max 2.11