Ru-catalyzed hydrogenation of 3,5-diketo amides: simultaneous control of chemo- and enantioselectivity
Wanfang Li; Weizheng Fan; Xin Ma; Xiaoming Tao; Xiaoming Li; Xiaomin Xie; Zhaoguo Zhang; Chemical Communications 48 (2012) 8976–; doi:10.1039/c2cc33695b

data_7108240
_publ_section_title
;
 Ru-catalyzed hydrogenation of 3,5-diketo amides: simultaneous control of
 chemo- and enantioselectivity
;
_journal_name_full               'Chemical Communications'
_journal_page_first              8976
_journal_paper_doi               10.1039/c2cc33695b
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C13 H19 N O4'
_chemical_formula_weight         253.29
_space_group_IT_number           19
_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                   7.7341(4)
_cell_length_b                   8.4900(5)
_cell_length_c                   20.9282(11)
_cell_measurement_temperature    173(2)
_cell_volume                     1374.20(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7946
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         68.33
_diffrn_reflns_theta_min         4.22
_exptl_absorpt_coefficient_mu    0.748
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2426
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0692P)^2^+0.1776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1142
_refine_ls_wR_factor_ref         0.1150
_reflns_number_gt                2376
_reflns_number_total             2426
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc33695b.txt
_cod_data_source_block           (S)-4s
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               7108240