B(C6F5)3-catalyzed formation of B‒P bonds by dehydrocoupling of phosphine‒boranes
Denis, Jean-Marc; Forintos, Henrietta; Szelke, Helga; Toupet, Loic; Pham, Thi-Nhàn; Madec, Pierre-Jean; Gaumont, Annie-Claude; Chemical Communications (Cambridge, United Kingdom)  (2003) 54–55; doi:10.1039/b206559b

data_7113889
_publ_section_title
;
 B(C6F5)3-catalyzed formation of B--P bonds by dehydrocoupling of
 phosphine--boranes
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   1
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              54
_journal_page_last               55
_journal_paper_doi               10.1039/b206559b
_journal_year                    2003
_chemical_formula_sum            'C24 H7 B F15 P'
_chemical_formula_weight         622.08
_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                86.66(9)
_cell_angle_beta                 77.22(7)
_cell_angle_gamma                87.560(8)
_cell_formula_units_Z            2
_cell_length_a                   8.070(5)
_cell_length_b                   11.337(9)
_cell_length_c                   12.992(9)
_cell_measurement_temperature    293(2)
_cell_volume                     1156.7(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4389
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.254
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.0043(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         4070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0327P)^2^+0.2136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0918
_reflns_number_gt                2495
_reflns_number_total             4070
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103617
_cod_data_source_file            b206559b.txt
_cod_data_source_block           ph
_cod_original_cell_volume        1156.7(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7113889