Synthesis, reactivity and catalytic activity in transfer hydrogenation of ketones of ruthenium(II) and ruthenium(IV) complexes containing the novel N-thiophosphorylated iminophosphorane-phosphine ligands Ph2PCH2P{NP(S)(OR)2}Ph2(R = Et, Ph)
Victorio Cadierno; Pascale Crochet; Josefina Díez; Joaquín García-Álvarez; Sergio E. García-Garrido; Santiago García-Granda; José Gimeno; Miguel A. Rodríguez; Dalton Trans.  (2003) 3240–3249; doi:10.1039/b305520e

data_7013201
_publ_section_title
;
 Synthesis, reactivity and catalytic activity in transfer hydrogenation
 of ketones of ruthenium(II) and ruthenium(IV) complexes containing the
 novel N-thiophosphorylated iminophosphorane-phosphine ligands
 Ph2PCH2P{NP(S)(OR)2}Ph2(R = Et, Ph)
;
_journal_issue                   16
_journal_name_full               'Dalton Trans.'
_journal_page_first              3240
_journal_page_last               3249
_journal_paper_doi               10.1039/b305520e
_journal_year                    2003
_chemical_compound_source        synthesis
_chemical_formula_moiety
'C39 H48 Cl N O2 P3 Ru S, C5 H12, 2(C H2 Cl2), B F4'
_chemical_formula_sum            'C46 H64 B Cl5 F4 N O2 P3 Ru S'
_chemical_formula_weight         1153.08
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 125.00(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1739(6)
_cell_length_b                   23.8656(9)
_cell_length_c                   21.1320(8)
_cell_measurement_reflns_used    8421
_cell_measurement_temperature    120(2)
_cell_volume                     5029(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowki & Minor 1997)'
_computing_data_collection       'Collet (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens, 1996)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       '95 mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f and \w scan'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            66067
_diffrn_reflns_theta_full        69.64
_diffrn_reflns_theta_max         69.64
_diffrn_reflns_theta_min         3.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.705
_exptl_absorpt_correction_T_max  0.309
_exptl_absorpt_correction_T_min  0.212
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XABS (Parkin, Moezzi & Hope, 1995)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.040
_refine_diff_density_min         -1.315
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         9349
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.520
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0708
_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^)+(0.1503P)^2^+16.5632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2102
_refine_ls_wR_factor_ref         0.2525
_reflns_number_gt                7795
_reflns_number_total             9349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305520e.txt
_cod_data_source_block           6a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7013201