Hydrogenation of Benzonitrile to Benzylamine Catalyzed by Ruthenium Hydride Complexes with P−NH−NH−P Tetradentate Ligands: Evidence for a Hydridic−Protonic Outer Sphere Mechanism
Li, Tianshu; Bergner, Ines; Haque, F. Nipa; Zimmer-De Iuliis, Marco; Song, Datong; Morris, Robert H.; Organometallics 26 (2007) 5940–; doi:10.1021/om700783e

data_4073981
_publ_section_title
;
 Hydrogenation of Benzonitrile to Benzylamine Catalyzed by Ruthenium
 Hydride Complexes with P&#x2212;NH&#x2212;NH&#x2212;P Tetradentate
 Ligands:&#x00A0; Evidence for a Hydridic&#x2212;Protonic Outer Sphere
 Mechanism
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5940
_journal_paper_doi               10.1021/om700783e
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C40 H43 B N2 P2 Ru'
_chemical_formula_weight         725.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                99.54(3)
_cell_angle_beta                 98.42(3)
_cell_angle_gamma                104.56(3)
_cell_formula_units_Z            4
_cell_length_a                   10.163(2)
_cell_length_b                   15.129(3)
_cell_length_c                   24.273(5)
_cell_measurement_temperature    150(2)
_cell_volume                     3492.5(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0985
_diffrn_reflns_av_sigmaI/netI    0.1746
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            36954
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     869
_refine_ls_number_reflns         15771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1808
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+7.3295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1328
_reflns_number_gt                7941
_reflns_number_total             15771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700783e-file003.cif
_cod_data_source_block           Complex7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3492.6(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4073981