Borane to Boryl Hydride to Borylene Dihydride: Explicit Demonstration of Boron-to-Metal α-Hydride Migration in Aminoborane Activation
Michael O'Neill; David A. Addy; Ian Riddlestone; Michael Kelly; Nicholas Phillips; Simon Aldridge; Journal of the American Chemical Society 133 (2011) 11500–11503; doi:10.1021/ja2050748

data_4106484
_publ_contact_author             'Simon Aldridge'
_publ_contact_author_email       simon.aldridge@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 272690'
_publ_section_title
;
 Borane to Boryl Hydride to Borylene Dihydride: Explicit Demonstration of
 Boron-to-Metal \a-Hydride Migration in Aminoborane Activation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11500
_journal_page_last               11503
_journal_paper_doi               10.1021/ja2050748
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C21 H51 B1 Cl1 Ir1 N1 P3'
_chemical_formula_sum            'C21 H51 B Cl Ir N P3'
_chemical_formula_weight         649.05
_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
_audit_creation_date             11-05-24
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90
_cell_angle_beta                 109.749(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3710(4)
_cell_length_b                   14.3825(2)
_cell_length_c                   15.8506(4)
_cell_measurement_reflns_used    16277
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.2926
_cell_measurement_theta_min      2.5275
_cell_volume                     3512.60(15)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            38213
_diffrn_reflns_theta_full        27.629
_diffrn_reflns_theta_max         30.361
_diffrn_reflns_theta_min         2.601
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.021
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       needle
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.530
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_platon_squeeze_details
;The discrete Fourier transform of the void region 
were treated as contributions to the A and B parts 
of the calculated structure factors.
;
_refine_diff_density_max         4.62
_refine_diff_density_min         -2.84
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.8669
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         9535
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.0008575
_refine_ls_shift/su_mean         0.0000251
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ +11.40P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0909
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0908
_reflns_limit_h_max              21
_reflns_limit_h_min              -23
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                7468
_reflns_number_total             9563
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.39
_oxford_diffrn_Wilson_scale      2.97
_oxford_refine_ls_r_factor_ref   0.0504
_oxford_refine_ls_scale          0.8424(14)
_oxford_reflns_number_all        9536
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 0303MOMK11
_cod_data_source_file            ja2050748_si_002_2.cif
_cod_data_source_block           2b
_cod_original_cell_volume        3512.58(14)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C21 H51 B1 Cl1 Ir1 N1 P3'
_cod_database_code               4106484