Phosphine Coordination Complexes of the Diphenylphosphenium Cation: A Versatile Synthetic Methodology for P-P Bond Formation
Neil Burford; Paul J. Ragogna; Robert McDonald; Michael J. Ferguson; Journal of the American Chemical Society 125 (2003) 14404–14410; doi:10.1021/ja036649w

data_4114378
_publ_contact_author_address
;Department of Chemistry
Dalhousie University
Halifax, NS
B3H 4J6, CANADA
;
_publ_contact_author_email       Neil.Burford@dal.ca
_publ_contact_author_fax         +1-902-494-1310
_publ_contact_author_name        'Neil Burford'
_publ_contact_author_phone       +1-902-494-1390
_publ_section_title
;
 Phosphine Coordination Complexes of the Diphenylphosphenium Cation: A
 Versatile Synthetic Methodology for P-P Bond Formation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14404
_journal_page_last               14410
_journal_paper_doi               10.1021/ja036649w
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C27 H32 F3 O3 P3 S'
_chemical_formula_sum            'C27 H32 F3 O3 P3 S'
_chemical_formula_weight         586.50
_chemical_melting_point          437
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                102.753(3)
_cell_angle_beta                 107.407(3)
_cell_angle_gamma                100.374(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0399(15)
_cell_length_b                   10.6383(16)
_cell_length_c                   14.648(2)
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.316
_cell_measurement_theta_min      2.204
_cell_volume                     1404.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8007
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.52
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_T_max  0.9706
_exptl_absorpt_correction_T_min  0.9036
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       needle
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0598P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1179
_reflns_number_gt                4000
_reflns_number_total             5620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja036649wsi20030616_040239.cif
_cod_data_source_block           dal0310
_cod_database_code               4114378