Facile synthesis of highly congested 1,2-diphosphinobenzenes from bis(phosphine)boronium salts.
Yamamoto, Yoshikazu; Koizumi, Toru; Katagiri, Kosuke; Furuya, Yui; Danjo, Hiroshi; Imamoto, Tsuneo; Yamaguchi, Kentaro; Organic letters 8 (2006) 6103–6106; doi:10.1021/ol062717i

data_1506324
_publ_section_title
;
 Facile synthesis of highly congested 1,2-diphosphinobenzenes from
 bis(phosphine)boronium salts.
;
_journal_issue                   26
_journal_name_full               'Organic letters'
_journal_page_first              6103
_journal_page_last               6106
_journal_paper_doi               10.1021/ol062717i
_journal_volume                  8
_journal_year                    2006
_chemical_formula_moiety         'C29 H48 P2 Rh 1+, F6 P 1-, C4 H8 O'
_chemical_formula_sum            'C33 H56 F6 O P3 Rh'
_chemical_formula_weight         778.60
_chemical_name_common            '[Rh(dtbpb)(nbd)]PF6'
_chemical_name_systematic
'[Bis(di-tert-butylphosphino-\k2,P,P)benzene](norbornadiene)rhodium(I) PF6'
_space_group_IT_number           145
_symmetry_cell_setting           rhombohedral
_symmetry_Int_Tables_number      145
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.1077(6)
_cell_length_b                   11.1077(6)
_cell_length_c                   24.942(3)
_cell_measurement_reflns_used    3812
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.82
_cell_measurement_theta_min      2.27
_cell_volume                     2665.1(4)
_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, 1990)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Bruker APEX II 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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            14766
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.12
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX II'
_exptl_absorpt_coefficient_mu    0.673
_exptl_absorpt_correction_T_max  0.9358
_exptl_absorpt_correction_T_min  0.7700
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1218
_exptl_crystal_recrystallization_method 'from tetrahydrofuran'
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.185
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         7854
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0540P)^2^+1.3602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                6832
_reflns_number_total             7854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol062717isi20061110_015747.cif
_cod_data_source_block           a0605122dan
_cod_database_code               1506324