Highly Selective Asymmetric Hydrogenation Using a Three Hindered Quadrant Bisphosphine Rhodium Catalyst
Garrett Hoge; He-Ping Wu; William S. Kissel; Derek A. Pflum; Derek J. Greene; Jian Bao; Journal of the American Chemical Society 126 (2004) 5966–5967; doi:10.1021/ja048496y

data_4112559
_publ_section_title
;
 Highly Selective Asymmetric Hydrogenation Using a Three Hindered Quadrant
 Bisphosphine Rhodium Catalyst
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5966
_journal_page_last               5967
_journal_paper_doi               10.1021/ja048496y
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C22 H44 B F4 P2 Rh'
_chemical_formula_weight         560.23
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 93.1200(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4395(4)
_cell_length_b                   16.8558(7)
_cell_length_c                   18.3565(8)
_cell_measurement_temperature    223(2)
_cell_volume                     2607.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23133
_diffrn_reflns_theta_full        26.45
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.814
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_F_000             1168
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(3)
_refine_ls_extinction_coef       0.00000(17)
_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_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         10615
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          6.484
_refine_ls_shift/su_mean         0.057
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.3590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1181
_reflns_number_gt                9034
_reflns_number_total             10615
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048496ysi20040405_022619.cif
_cod_data_source_block           aa02
_cod_database_code               4112559