Ruthenium-Catalyzed Hydrogenation of Nitriles: Insights into the Mechanism
Rebeca Reguillo; Mary Grellier; Nicolas Vautravers; Laure Vendier; Sylviane Sabo-Etienne; Journal of the American Chemical Society 132 (2010) 7854–7855; doi:10.1021/ja102759z

data_4102525
_publ_contact_author
;
Sylviane Sabo-Etienne and Mary Grellier
;
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
205 Route de Narbonne
31077 Toulouse Cedex 04
;
_publ_contact_author_email
'sabo@lcc-toulouse.fr, grellier@lcc-toulouse.fr'
_publ_section_title
;
 Ruthenium-Catalyzed Hydrogenation of Nitriles: Insights into the
 Mechanism
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7854
_journal_page_last               7855
_journal_paper_doi               10.1021/ja102759z
_journal_volume                  132
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C34 H62 N2 P2 Ru'
_chemical_formula_sum            'C34 H62 N2 P2 Ru'
_chemical_formula_weight         661.87
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 95.596(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5860(6)
_cell_length_b                   16.4840(7)
_cell_length_c                   21.6790(10)
_cell_measurement_reflns_used    9000
_cell_measurement_temperature    110
_cell_measurement_theta_max      32.1051
_cell_measurement_theta_min      2.8265
_cell_measurement_wavelength     0.71073
_cell_volume                     3409.3(3)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       \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  0.0326
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23177
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.23
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  4
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_T_max  0.8882
_exptl_absorpt_correction_T_min  0.7327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2125
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.66
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         6944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+7.7753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0748
_reflns_number_gt                6440
_reflns_number_total             6944
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja102759z_si_001.cif
_cod_data_source_block           global
_cod_database_code               4102525