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_4106483
_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         'C15 H42 B Cl Ir N P3, C24 H12 B Cl8'
_chemical_formula_sum            'C39 H54 B2 Cl9 Ir N P3'
_chemical_formula_weight         1162.70
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             11-05-26
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.47060(10)
_cell_length_b                   17.23380(10)
_cell_length_c                   17.53330(10)
_cell_measurement_reflns_used    6222
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4976.85(5)
_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 0.992
_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  0.018
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54087
_diffrn_reflns_theta_full        26.924
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         5.128
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.291
_exptl_absorpt_correction_T_max  0.59
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.05
_refine_diff_density_min         -1.25
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9275
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5845
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.0042217
_refine_ls_shift/su_mean         0.0001155
_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: 
 13.6 20.6 10.4 2.81 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0676
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0676
_reflns_limit_h_max              21
_reflns_limit_h_min              0
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                5082
_reflns_number_total             5845
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.53
_oxford_diffrn_Wilson_scale      84.63
_oxford_refine_ls_r_factor_ref   0.0313
_oxford_refine_ls_scale          0.11339(2)
_oxford_reflns_number_all        5845
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '5231505 005monp11'
_cod_data_source_file            ja2050748_si_002_1.cif
_cod_data_source_block           4a.BAr(Cl)4
_cod_original_sg_symbol_H-M      'P n m a '
_cod_original_formula_sum        'C39 H54 B2 Cl9 Ir1 N1 P3'
_cod_database_code               4106483
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S  H(11,X'S) 
REM RIDE IR  (   1,X'S) H   (  11,X'S) 
RIDE C   (   4,X'S) H   (  42,X'S) H   (  41,X'S) H   (  43,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) H   (  53,X'S) H   (  52,X'S) 
RIDE C   (   6,X'S) H   (  62,X'S) H   (  61,X'S) H   (  63,X'S) 
RIDE C   (   8,X'S) H   (  82,X'S) H   (  83,X'S) H   (  81,X'S) 
RIDE C   (   9,X)   H   (  91,X)   H   (  92,X) 
RIDE C   (   9,Z)   H   (  91,Z)   H   (  92,Z) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) H   ( 133,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
DIST 0.95, 0.001 = C(12) TO H(121) 
DIST 0.95, 0.001 = C(14) TO H(141) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;