Diastereoselective Synthesis of Bulky, Strongly Nucleophilic, and Configurationally Stable P-Stereogenic Tricyclic Phosphines
David Gau; Ricardo Rodriguez; Tsuyoshi Kato; Nathalie Saffon-Merceron; Antoine Baceiredo; Journal of the American Chemical Society 132 (2010) 12841–12843; doi:10.1021/ja1054912

data_4103063
_publ_section_title
;
 Diastereoselective Synthesis of Bulky, Strongly Nucleophilic, and
 Configurationally Stable P-Stereogenic Tricyclic Phosphines
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12841
_journal_page_last               12843
_journal_paper_doi               10.1021/ja1054912
_journal_volume                  132
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C47 H70 Cl N3 P Rh Si, C H2 Cl2'
_chemical_formula_sum            'C48 H72 Cl3 N3 P Rh Si'
_chemical_formula_weight         959.41
_chemical_name_systematic
;
 ?
;
_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
_cell_angle_alpha                108.789(1)
_cell_angle_beta                 100.115(1)
_cell_angle_gamma                92.699(1)
_cell_formula_units_Z            2
_cell_length_a                   10.2915(2)
_cell_length_b                   14.4688(2)
_cell_length_c                   17.2543(3)
_cell_measurement_reflns_used    5277
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24.42
_cell_measurement_theta_min      2.16
_cell_measurement_wavelength     0.71073
_cell_volume                     2379.69(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34326
_diffrn_reflns_theta_full        28.94
_diffrn_reflns_theta_max         28.94
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         12555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1067
_reflns_number_gt                8818
_reflns_number_total             12555
_reflns_threshold_expression     >2/sigma(I)
_cod_data_source_file            ja1054912_si_004.cif
_cod_data_source_block           global
_cod_database_code               4103063