Tridentate and Tetradentate Iminophosphorane-Based Ruthenium Complexes in Catalytic Transfer Hydrogenation of Ketones
Dyer, Hellen; Picot, Alexandre; Vendier, Laure; Auffrant, Audrey; Le Floch, Pascal; Sabo-Etienne, Sylviane; Organometallics 30 (2011) 1478–; doi:10.1021/om101058m

data_4063949
_publ_section_title
;
 Tridentate and Tetradentate Iminophosphorane-Based Ruthenium Complexes in
 Catalytic Transfer Hydrogenation of Ketones
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1478
_journal_paper_doi               10.1021/om101058m
_journal_volume                  30
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C60 H68 Cl N2 P4 Ru, C32 H12 B'
_chemical_formula_sum            'C92 H80 B Cl F24 N2 P4 Ru'
_chemical_formula_weight         1940.79
_chemical_name_systematic
;
 ?
;
_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
_cell_angle_alpha                90.634(15)
_cell_angle_beta                 99.270(16)
_cell_angle_gamma                102.486(14)
_cell_formula_units_Z            2
_cell_length_a                   11.515(2)
_cell_length_b                   17.723(4)
_cell_length_c                   22.221(5)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_measurement_wavelength     0.71073
_cell_volume                     4364.8(16)
_computing_cell_refinement       'Bruker Kappa APEX II'
_computing_data_collection       'Bruker Kappa APEX II'
_computing_data_reduction        'Bruker Kappa APEX II'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.08
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            73011
_diffrn_reflns_theta_full        21.46
_diffrn_reflns_theta_max         21.46
_diffrn_reflns_theta_min         0.93
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.382
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1139
_refine_ls_number_reflns         9922
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.043
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+15.8087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                7339
_reflns_number_total             9922
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101058m_si_002.cif
_cod_data_source_block           complex7
_cod_original_cell_volume        4364.8(15)
_cod_database_code               4063949