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_4103060
_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_formula_sum            'C39 H58 N3 P Si'
_chemical_formula_weight         627.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                84.5520(10)
_cell_angle_beta                 89.2500(10)
_cell_angle_gamma                67.9810(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2808(2)
_cell_length_b                   11.0503(2)
_cell_length_c                   17.9965(4)
_cell_measurement_reflns_used    6597
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.31
_cell_volume                     1886.26(7)
_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      193(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0398
_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       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18499
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         5.15
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  0.9867
_exptl_absorpt_correction_T_min  0.9239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         7564
_refine_ls_number_restraints     354
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0578P)^2^+0.5827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1236
_reflns_number_gt                5868
_reflns_number_total             7564
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1054912_si_001.cif
_cod_data_source_block           2a
_cod_database_code               4103060