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_4106485
_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 B Ir N P3, C24 H12 B Cl8'
_chemical_formula_sum            'C45 H63 B2 Cl8 Ir N P3'
_chemical_formula_weight         1208.39
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             11-05-26
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                107.9175(5)
_cell_angle_beta                 93.8315(5)
_cell_angle_gamma                100.1645(5)
_cell_formula_units_Z            2
_cell_length_a                   12.10780(10)
_cell_length_b                   15.4482(2)
_cell_length_c                   15.9503(2)
_cell_measurement_reflns_used    11297
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2770.69(6)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            47975
_diffrn_reflns_theta_full        26.635
_diffrn_reflns_theta_max         27.459
_diffrn_reflns_theta_min         5.116
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.912
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_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         1.58
_refine_diff_density_min         -1.38
_refine_ls_extinction_coef       69(4)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9632
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         12563
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.0018274
_refine_ls_shift/su_mean         0.0000305
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 4.06 3.82 1.08 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0715
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0715
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              19
_reflns_limit_k_min              -20
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                10420
_reflns_number_total             12563
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.84
_oxford_diffrn_Wilson_scale      53.87
_oxford_refine_ls_r_factor_ref   0.0495
_oxford_refine_ls_scale          0.13879(3)
_oxford_reflns_number_all        12563
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '5071126 012monp11'
_cod_data_source_file            ja2050748_si_002_3.cif
_cod_data_source_block           3b.B(ArCl)4
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C45 H63 B2 Cl8 Ir1 N1 P3'
_cod_database_code               4106485