Ruthenium(II) and Ruthenium(IV) Complexes Containing κ1-P-, κ2-P,O-, and κ3-P,N,O-Iminophosphorane-Phosphine Ligands Ph2PCH2P{NP(O)(OR)2}Ph2 (R = Et, Ph): Synthesis, Reactivity, Theoretical Studies, and Catalytic Activity in Transfer Hydrogenation of Cyclohexanone
Victorio Cadierno; Pascale Crochet; Josefina Díez; Joaquín García-Álvarez; Sergio E. García-Garrido; José Gimeno; Santiago García-Granda; Miguel A. Rodríguez; Inorganic Chemistry 42 (2003) 3293–3307; doi:10.1021/ic020702k

data_4313615
_publ_contact_author
;
      Santiago Garc\'ia-Granda
      Departamento de Qu\'imica F\'isica y Anal\'itica
      Facultad de Qu\'imica
      Universidad de Oviedo
      Avda. Juli\'an Claver\'ia, 8
      33071 Oviedo
      Spain
;
_publ_contact_author_email       sgg@sauron.quimica.uniovi.es
_publ_contact_author_fax         '0034 98 5103125'
_publ_contact_author_phone       '0034 98 5103477'
_publ_section_title
;
 Ruthenium(II) and Ruthenium(IV) Complexes Containing \k1-P-, \k2-P,O-,
 and \k3-P,N,O-Iminophosphorane-Phosphine Ligands Ph2PCH2P{NP(O)(OR)2}Ph2
 (R = Et, Ph): Synthesis, Reactivity, Theoretical Studies, and Catalytic
 Activity in Transfer Hydrogenation of Cyclohexanone
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3293
_journal_page_last               3307
_journal_paper_doi               10.1021/ic020702k
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C47 H46 Cl N O3 P3 Ru, P F6'
_chemical_formula_sum            'C47 H46 Cl F6 N O3 P4 Ru'
_chemical_formula_weight         1047.25
_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                 95.640(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2905(9)
_cell_length_b                   21.584(2)
_cell_length_c                   22.062(2)
_cell_measurement_reflns_used    884
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      42.528
_cell_measurement_theta_min      4.402
_cell_volume                     4876.5(8)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SHELXTL'
_computing_molecular_graphics    'PLATON-2000 (Spek, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens, 1996)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scan'
_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  0.097
_diffrn_reflns_av_sigmaI/netI    0.2290
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            18222
_diffrn_reflns_theta_full        30.58
_diffrn_reflns_theta_max         30.58
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.577
_refine_diff_density_min         -1.229
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         14493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.2272
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0936P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1517
_refine_ls_wR_factor_ref         0.2073
_reflns_number_gt                5458
_reflns_number_total             14493
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020702k_1.cif
_cod_data_source_block           3b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4876.3(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4313615