Chiral Ruthenabicyclic Complexes: Precatalysts for Rapid, Enantioselective, and Wide-Scope Hydrogenation of Ketones
Kazuhiko Matsumura; Noriyoshi Arai; Kiyoto Hori; Takao Saito; Noboru Sayo; Takeshi Ohkuma; Journal of the American Chemical Society 133 (2011) 10696–10699; doi:10.1021/ja202296w

data_4106403
_publ_section_title
;
 Chiral Ruthenabicyclic Complexes: Precatalysts for Rapid,
 Enantioselective, and Wide-Scope Hydrogenation of Ketones
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10696
_journal_page_last               10699
_journal_paper_doi               10.1021/ja202296w
_journal_volume                  133
_journal_year                    2011
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C65 H69 Cl N2 O6 P2 Ru, C6 H6'
_chemical_formula_sum            'C71 H75 Cl N2 O6 P2 Ru'
_chemical_formula_weight         1250.85
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 103.648(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   13.7017(8)
_cell_length_b                   12.6570(6)
_cell_length_c                   20.2986(15)
_cell_measurement_reflns_used    25887
_cell_measurement_temperature    223
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.06
_cell_volume                     3420.8(4)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      223
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32832
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       prism
_exptl_crystal_F_000             1308.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.510
_refine_diff_density_min         -0.600
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  6175 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     761
_refine_ls_number_reflns         14339
_refine_ls_number_restraints     1
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1217P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1917
_reflns_number_gt                11693
_reflns_number_total             14339
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja202296w_si_002.cif
_cod_data_source_block           sc0779
_cod_database_code               4106403