Asymmetric Hydrogenation of Ketones with Ruthenium Complexes ofrac- and Enantiopure (S,S)-1,2-Bis((diphenylphosphino)methyl)cyclohexane: A Comparative Study withrac- and (R)-BINAP
Doherty, Simon; Knight, Julian G.; Bell, Adam L.; Harrington, Ross W.; Clegg, William; Organometallics 26 (2007) 2465–; doi:10.1021/om070129i

data_4073166
_publ_section_title
;
 Asymmetric Hydrogenation of Ketones with Ruthenium Complexes ofrac- and
 Enantiopure (S,S)-1,2-Bis((diphenylphosphino)methyl)cyclohexane:&#x00A0;
 A Comparative Study withrac- and (R)-BINAP
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2465
_journal_paper_doi               10.1021/om070129i
_journal_volume                  26
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C46 H50 Cl2 N2 P2 Ru, 2 C7 H8'
_chemical_formula_sum            'C58 H66 Cl2 N2 P2 Ru'
_chemical_formula_weight         1025.04
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.390(3)
_cell_length_b                   16.690(5)
_cell_length_c                   21.375(7)
_cell_measurement_reflns_used    201
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.50
_cell_volume                     5490(3)
_computing_cell_refinement       EvalCCD
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            91483
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         4.04
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         12570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+0.6104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1132
_reflns_number_gt                11072
_reflns_number_total             12570
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om070129isi20070209_122746.cif
_cod_data_source_block           sd204
_cod_database_code               4073166