Silyl-migrations in frustrated Lewis pair chemistry: reactions of (CH3)3Si)3P and B(C6F4H)3 with H2 and CO2
Katsuhiko Takeuchi; Douglas W. Stephan; Chem.Commun. 48 (2012) 11304–; doi:10.1039/c2cc36470k

data_7108588
_publ_section_title
;
 Silyl-migrations in frustrated Lewis pair chemistry: reactions of
 (CH3)3Si)3P and B(C6F4H)3 with H2 and CO2
;
_journal_name_full               Chem.Commun.
_journal_page_first              11304
_journal_paper_doi               10.1039/c2cc36470k
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C29 H30 B F12 O4 P Si3'
_chemical_formula_weight         796.58
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.657(2)
_cell_angle_beta                 87.6520(10)
_cell_angle_gamma                85.639(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8454(4)
_cell_length_b                   11.2438(4)
_cell_length_c                   15.4120(6)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.461
_cell_measurement_theta_min      2.650
_cell_volume                     1864.72(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32663
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_T_max  0.9494
_exptl_absorpt_correction_T_min  0.9494
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         8451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0410P)^2^+1.1322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                6312
_reflns_number_total             8451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc36470k.txt
_cod_data_source_block           kt004_0m
_cod_database_code               7108588