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_4114380
_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         902-494-1310
_publ_contact_author_name        'Neil Burford'
_publ_contact_author_phone       902-494-3190
_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_sum            'C24 H20 Cl5 Ga P2'
_chemical_formula_weight         617.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.482(6)
_cell_length_b                   27.662(8)
_cell_length_c                   10.744(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.8
_cell_measurement_theta_min      20.8
_cell_volume                     5493(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction
;
teXsan for Windows version 1.06 (MSC, 1997-1999)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.00840
_diffrn_orient_matrix_UB_12      -0.03525
_diffrn_orient_matrix_UB_13      -0.01476
_diffrn_orient_matrix_UB_21      -0.03013
_diffrn_orient_matrix_UB_22      0.00167
_diffrn_orient_matrix_UB_23      -0.07719
_diffrn_orient_matrix_UB_31      0.04415
_diffrn_orient_matrix_UB_32      0.00784
_diffrn_orient_matrix_UB_33      -0.04987
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.212
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5044
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        63.59
_diffrn_reflns_theta_max         63.59
_diffrn_reflns_theta_min         2.88
_diffrn_standards_decay_%        0.19
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.038
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North,Phillips & Matthews, 1968
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.00037(7)
_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_all   0.971
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4499
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.2658
_refine_ls_R_factor_obs          0.0512
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2082
_refine_ls_wR_factor_obs         0.1329
_reflns_number_gt                1279
_reflns_number_total             4499
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja036649wsi20030616_040605.cif
_cod_data_source_block           paul6
_cod_original_sg_symbol_H-M      'P b c a '
_cod_original_formula_sum        'C24 H20 Cl5 Ga1 P2'
_cod_database_code               4114380