Facile B-H Bond Activation of Borane by Stable Carbenoid Species
Hadrien Heuclin; Samuel Y.-F. Ho; Xavier F. Le Goff; Cheuk-Wai So; Nicolas Mézailles; Journal of the American Chemical Society 135 (2013) 8774–8777; doi:10.1021/ja401763c

data_4119941
_publ_contact_author_address
;Laboratoire DCPH
Ecole Polytechnique
Route de Saclay
F91128 Palaiseau
France
;
_publ_contact_author_email       mezailles@chimie.ups-tlse.fr
_publ_contact_author_fax         +33(0)561558204
_publ_contact_author_name        'Nicolas Mezailles'
_publ_contact_author_phone       +33(0)561556292
_publ_section_title
;
 Facile B-H Bond Activation of Borane by Stable Carbenoid Species
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8774
_journal_page_last               8777
_journal_paper_doi               10.1021/ja401763c
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C50 H46 B2 P4 S2'
_chemical_formula_sum            'C50 H46 B2 P4 S2'
_chemical_formula_weight         856.49
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   29.053(1)
_cell_length_b                   29.053(1)
_cell_length_c                   9.752(1)
_cell_measurement_reflns_used    3609
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      0.998
_cell_volume                     7128.6(8)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        'DENZO & COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  KappaCCD
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0829
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14886
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.280
_exptl_absorpt_correction_T_max  0.9672
_exptl_absorpt_correction_T_min  0.9462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       Block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         8264
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1240
_refine_ls_R_factor_gt           0.0885
_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^)+(0.0914P)^2^+19.4249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2147
_refine_ls_wR_factor_ref         0.2357
_reflns_number_gt                5760
_reflns_number_total             8264
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja401763c_si_002_2.cif
_cod_data_source_block           hh937_bateau
_cod_database_code               4119941