Reaction of Diphenylphosphanylacetylene with RB(C6F5)2 Reagents: Evidence for a Remarkable Sequence of Synergistic Frustrated Lewis Pair Addition Reactions
Jiangang Yu; Gerald Kehr; Constantin G. Daniliuc; Gerhard Erker; Inorganic Chemistry 52 (2013) 11661–11668; doi:10.1021/ic402139g

data_4336386
_publ_section_title
;
 Reaction of Diphenylphosphanylacetylene with RB(C6F5)2 Reagents: Evidence
 for a Remarkable Sequence of Synergistic Frustrated Lewis Pair Addition
 Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11661
_journal_page_last               11668
_journal_paper_doi               10.1021/ic402139g
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C34 H15 B F15 P'
_chemical_formula_weight         750.24
_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                71.570(6)
_cell_angle_beta                 83.088(8)
_cell_angle_gamma                74.813(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9861(12)
_cell_length_b                   12.7129(19)
_cell_length_c                   14.7045(10)
_cell_measurement_reflns_used    4737
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     1536.7(3)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20191
_diffrn_reflns_theta_full        66.88
_diffrn_reflns_theta_max         66.88
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    1.882
_exptl_absorpt_correction_T_max  0.8640
_exptl_absorpt_correction_T_min  0.7047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       prism
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         5217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0701P)^2^+0.9605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1426
_reflns_number_gt                4206
_reflns_number_total             5217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402139g_si_002_3.cif
_cod_data_source_block           erk6831
_cod_database_code               4336386