Metalation of Trimethylphosphine−Borane. Unexpected Reactivity of a Simple Phosphine−Borane-Stabilized Carbanion toward Siloxanes
Izod, Keith; Wills, Corinne; Clegg, William; Harrington, Ross W.; Organometallics 26 (2007) 2861–; doi:10.1021/om070150j

data_4073186
_publ_section_title
;
 Metalation of Trimethylphosphine&#x2212;Borane. Unexpected Reactivity of
 a Simple Phosphine&#x2212;Borane-Stabilized Carbanion toward Siloxanes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2861
_journal_paper_doi               10.1021/om070150j
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C7 H19 B Na O P'
_chemical_formula_sum            'C7 H19 B Na O P'
_chemical_formula_weight         183.99
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.279(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.534(2)
_cell_length_b                   14.6996(12)
_cell_length_c                   13.079(3)
_cell_measurement_reflns_used    115
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.
_cell_measurement_theta_min      2.50
_cell_volume                     2354.6(7)
_computing_cell_refinement       EvalCCD
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11758
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         4.45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+1.6530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                2061
_reflns_number_total             2626
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om070150jsi20070219_080003.cif
_cod_data_source_block           ki234_compound_5a
_cod_original_cell_volume        2354.5(7)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4073186