Interplay between Hydrido/Dihydrogen and Amine/Amido Ligands in Ruthenium-Catalyzed Transfer Hydrogenation of Ketones
Alexandre Picot; Hellen Dyer; Antoine Buchard; Audrey Auffrant; Laure Vendier; Pascal Le Floch; Sylviane Sabo-Etienne; Inorganic Chemistry 49 (2010) 1310–1312; doi:10.1021/ic902339j

data_4314903
_publ_contact_author
;
Sylviane Sabo-Etienne
;
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
205 Route de Narbonne
31077 Toulouse Cedex 04
;
_publ_contact_author_email       sylviane.sabo@lcc-toulouse.fr
_publ_section_title
;
 Interplay between Hydrido/Dihydrogen and Amine/Amido Ligands in
 Ruthenium-Catalyzed Transfer Hydrogenation of Ketones
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1310
_journal_page_last               1312
_journal_paper_doi               10.1021/ic902339j
_journal_volume                  49
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'C49 H63 Cl N2 P3 Ru, C32 H12 B F24, 2(C7 H8)'
_chemical_formula_sum            'C95 H91 B Cl F24 N2 P3 Ru'
_chemical_formula_weight         1956.94
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 104.6080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2098(4)
_cell_length_b                   33.3099(9)
_cell_length_c                   20.1020(5)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      32.09
_cell_measurement_theta_min      2.18
_cell_measurement_wavelength     0.71073
_cell_volume                     9207.2(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       \w-\f
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            155148
_diffrn_reflns_theta_full        32.47
_diffrn_reflns_theta_max         32.47
_diffrn_reflns_theta_min         1.7
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             4008
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.225
_refine_diff_density_min         -1.688
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1146
_refine_ls_number_reflns         32511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.082
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0909P)^2^+10.4083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.1774
_reflns_number_gt                24678
_reflns_number_total             32511
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic902339j_si_001_2.cif
_cod_data_source_block           hdo110609
_cod_database_code               4314903