Synthesis and Reactivity of the Phosphinoboranes R2PB(C6F5)2
Stephen J. Geier; Thomas M. Gilbert; Douglas W. Stephan; Inorganic Chemistry 50 (2011) 336–344; doi:10.1021/ic102003x

data_4324164
_publ_section_title
;
 Synthesis and Reactivity of the Phosphinoboranes R2PB(C6F5)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              336
_journal_page_last               344
_journal_paper_doi               10.1021/ic102003x
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C24 H12 B F10 P'
_chemical_formula_weight         532.12
_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                106.381(3)
_cell_angle_beta                 94.690(3)
_cell_angle_gamma                96.226(3)
_cell_formula_units_Z            2
_cell_length_a                   8.9820(6)
_cell_length_b                   10.3690(6)
_cell_length_c                   12.4150(6)
_cell_measurement_reflns_used    4947
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.70
_cell_volume                     1095.11(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0657
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9937
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    0.222
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         4947
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0543
_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^+0.6725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1600
_reflns_number_gt                3199
_reflns_number_total             4947
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102003x_si_002_6.cif
_cod_data_source_block           (Ph2PH)(BH(C6F5)2)
_cod_database_code               4324164