Hydrogenation of amides catalyzed by a combined catalytic system of a Ru complex with a zinc salt
Yusuke Kita; Takafumi Higuchi; Kazushi Mashima; Chem.Commun. 50 (2014) 11211–; doi:10.1039/C4cc04481A

data_7115639
_publ_section_title
;
 Hydrogenation of amides catalyzed by a combined catalytic system of a Ru
 complex with a zinc salt
;
_journal_name_full               Chem.Commun.
_journal_page_first              11211
_journal_paper_doi               10.1039/C4cc04481A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C32 H32 F6 N2 O4 P2 Ru'
_chemical_formula_sum            'C32 H32 F6 N2 O4 P2 Ru'
_chemical_formula_weight         785.61
_chemical_melting_point          140
_chemical_name_common            4
_chemical_name_systematic        4
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                119.5260(10)
_cell_angle_beta                 92.516(15)
_cell_angle_gamma                115.846(8)
_cell_formula_units_Z            2
_cell_length_a                   12.660(18)
_cell_length_b                   13.268(19)
_cell_length_c                   13.386(18)
_cell_measurement_reflns_used    4224
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      3.04
_cell_volume                     1662(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0989
_diffrn_reflns_av_sigmaI/netI    0.1327
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12279
_diffrn_reflns_theta_full        24.15
_diffrn_reflns_theta_max         24.15
_diffrn_reflns_theta_min         3.04
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_T_max  0.9626
_exptl_absorpt_correction_T_min  0.9156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.303
_refine_diff_density_min         -1.181
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.1648
_refine_ls_R_factor_gt           0.1234
_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^)+(0.1517P)^2^+13.4829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3060
_refine_ls_wR_factor_ref         0.3475
_reflns_number_gt                3417
_reflns_number_total             5272
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc04481a2.cif
_cod_data_source_block           shelxl
_cod_database_code               7115639