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_4313616
_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         'C49 H46 N3 O5 P3 Ru, C H2 Cl2'
_chemical_formula_sum            'C50 H48 Cl2 N3 O5 P3 Ru'
_chemical_formula_weight         1035.79
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.3059(3)
_cell_length_b                   9.1822(1)
_cell_length_c                   22.6599(4)
_cell_measurement_reflns_used    4937
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      69.77
_cell_measurement_theta_min      3.79
_cell_volume                     4849.21(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & 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, 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      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.081
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            63933
_diffrn_reflns_theta_full        69.77
_diffrn_reflns_theta_max         69.77
_diffrn_reflns_theta_min         3.79
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.965
_exptl_absorpt_correction_T_max  0.605
_exptl_absorpt_correction_T_min  0.250
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XABS2 (Parkin, Moezzi& Hope, 1995)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.012
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.487(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         8644
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0755P)^2^+2.5453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1354
_reflns_number_gt                8272
_reflns_number_total             8644
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020702k_2.cif
_cod_data_source_block           12b
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' 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_database_code               4313616