Synthesis of Ruthenium Complexes with a NonspectatorSi,O,P-Chelate Ligand: Interconversion between a Hydrido(η2-silane) Complex and a Silyl Complex Leading to Catalytic Alkene Hydrogenation
Komuro, Takashi; Arai, Takafumi; Kikuchi, Kei; Tobita, Hiromi; Organometallics 34 (2015) 1211–; doi:10.1021/om5011885

data_1518895
_publ_section_title
;
 Synthesis of Ruthenium Complexes with a NonspectatorSi,O,P-Chelate
 Ligand: Interconversion between a Hydrido(\h2-silane) Complex and a Silyl
 Complex Leading to Catalytic Alkene Hydrogenation
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1211
_journal_paper_doi               10.1021/om5011885
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C55 H61 Cl O P2 Ru Si, 0.5(C5 H12)'
_chemical_formula_sum            'C57.5 H67 Cl O P2 Ru Si'
_chemical_formula_weight         1000.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.5022(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6569(4)
_cell_length_b                   18.1443(5)
_cell_length_c                   26.9876(8)
_cell_measurement_reflns_used    89679
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      0.8
_cell_volume                     5213.4(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver.1.11'
_computing_molecular_graphics
;
'ORTEP-3', 'Yadokari-XG 2009 (Wakita, Nemoto, et al., 2009)'
;
_computing_publication_material
;
'Yadokari-XG 2009 (Wakita, Nemoto, et al., 2009)'
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-2008 (PATTY)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            73214
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_T_max  0.954560
_exptl_absorpt_correction_T_min  0.932705
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
HIGASHI, T. (1999). Shape - Program to obtain Crystal Shape using CCD camera.
Rigaku Corporation, Tokyo, Japan. 
HIGASHI, T. (1999). Numabs - Numerical Absorption Correction,
Rigaku Corporation, Tokyo, Japan. 
;
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.343
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.246
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         11914
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.246
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0857
_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^)+(0.0766P)^2^+19.3415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1915
_refine_ls_wR_factor_ref         0.2047
_reflns_number_gt                9957
_reflns_number_total             11914
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om5011885_si_002.cif
_cod_data_source_block           complex-2
_cod_depositor_comments
'Adding full bibliography for 1518895--1518896.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C57.50 H67 Cl O P2 Ru Si'
_cod_database_code               1518895