Acycliccatena-Diphosphinodiphosphonium Dications [R3P-PR'-PR'-PR3]2+ or Bisphosphine-Diphosphenium Complexes [R3P→PR'-PR'←PR3]2+: Synthesis by Reductive P-P Coupling of [R3P-PR'Cl]+ and Phosphine Ligand Exchange
C. Adam Dyker; Neil Burford; Michael D. Lumsden; Andreas Decken; Journal of the American Chemical Society 128 (2006) 9632–9633; doi:10.1021/ja062972y

data_4110777
_publ_contact_author_address
;Department of Chemistry
University of New Brunswick
Fredericton, NB
E3B 6E2
Canada
;
_publ_contact_author_email       adecken@unb.ca
_publ_contact_author_fax         '(506) 453-4981'
_publ_contact_author_name        'Andreas Decken'
_publ_contact_author_phone       '(506) 453-4875'
_publ_section_title
;
 Acycliccatena-Diphosphinodiphosphonium Dications [R3P-PR'-PR'-PR3]2+ or
 Bisphosphine-Diphosphenium Complexes
 [R3P\\rightarrowPR'-PR'\\leftarrowPR3]2+: Synthesis by Reductive P-P
 Coupling of [R3P-PR'Cl]+ and Phosphine Ligand Exchange
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9632
_journal_page_last               9633
_journal_paper_doi               10.1021/ja062972y
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C25 H20 Cl F3 O3 P2 S'
_chemical_formula_weight         554.86
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      7
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.192(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0707(16)
_cell_length_b                   8.8891(15)
_cell_length_c                   14.166(2)
_cell_measurement_reflns_used    4133
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      28.06
_cell_measurement_theta_min      2.28
_cell_volume                     1229.4(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8149
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.24
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker AXS SMART1000/P4'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997b)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       Plate
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         4027
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0349P)^2^+0.0883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0630
_reflns_number_gt                3720
_reflns_number_total             4027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja062972ysi20060428_101942.cif
_cod_data_source_block           nb060137
_cod_original_cell_volume        1229.5(3)
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               4110777