Borylated Methylenephosphonium Salts: Precursors of Elusive Boryl(phosphino)carbenes
Florie Lavigne; Eddy Maerten; Gilles Alcaraz; Nathalie Saffon-Merceron; Carles Acosta-Silva; Vicenç Branchadell; Antoine Baceiredo; Journal of the American Chemical Society 132 (2010) 8864–8865; doi:10.1021/ja103422b

data_4102629
_publ_section_title
;
 Borylated Methylenephosphonium Salts: Precursors of Elusive
 Boryl(phosphino)carbenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8864
_journal_page_last               8865
_journal_paper_doi               10.1021/ja103422b
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C31 H50 B N2 P'
_chemical_formula_weight         492.51
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.917(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1594(4)
_cell_length_b                   9.2248(4)
_cell_length_c                   30.9493(12)
_cell_measurement_reflns_used    1377
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      16.68
_cell_measurement_theta_min      2.31
_cell_volume                     3147.5(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1498
_diffrn_reflns_av_sigmaI/netI    0.1261
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            31633
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         5.16
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.9979
_exptl_absorpt_correction_T_min  0.9768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.039
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         5298
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1721
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+0.0978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1403
_refine_ls_wR_factor_ref         0.1787
_reflns_number_gt                2467
_reflns_number_total             5298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja103422b_si_002.cif
_cod_data_source_block           5
_cod_database_code               4102629