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_4106486
_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_absolute_configuration ad
_chemical_formula_moiety         '    C21 H49 B Ir N P3, C32 H12 B F24'
_chemical_formula_sum            'C53 H61 B2 F24 Ir N P3'
_chemical_formula_weight         1474.79
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             11-05-25
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.13813(9)
_cell_length_b                   21.35767(18)
_cell_length_c                   25.9754(2)
_cell_measurement_reflns_used    39708
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     7288.69(10)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15214
_diffrn_reflns_theta_full        76.350
_diffrn_reflns_theta_max         76.350
_diffrn_reflns_theta_min         3.403
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.997
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       block
_exptl_crystal_F_000             2936.000
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_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         4.03
_refine_diff_density_min         -1.38
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.430(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9868
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1092
_refine_ls_number_reflns         15152
_refine_ls_number_restraints     1856
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.0257659
_refine_ls_shift/su_mean         0.0013786
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.15P)^2^ +20.20P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1997
_refine_ls_wR_factor_gt          0.1954
_refine_ls_wR_factor_ref         0.1997
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                14465
_reflns_number_total             15214
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.58
_oxford_diffrn_Wilson_scale      0.52
_oxford_refine_ls_r_factor_ref   0.0715
_oxford_refine_ls_scale          1.553(9)
_oxford_reflns_number_all        15153
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '0343MOMK11 in P2(1)2(1)2(1)'
_cod_data_source_file            ja2050748_si_002_4.cif
_cod_data_source_block           3b.B(ArF)4
_cod_original_cell_volume        7288.70(10)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C53 H61 B2 F24 Ir1 N1 P3'
_cod_database_code               4106486