Oxidative Addition of H−SiR3to Di- and Triruthenium Carbonyl Complexes Bearing a Bridging Azulene Ligand: Isolation of New Silylruthenium Complexes and Catalytic Hydrosilylation of Ketones
Matsubara, Kouki; Ryu, Kazuhiro; Maki, Tomoyuki; Iura, Takafumi; Nagashima, Hideo; Organometallics 21 (2002) 3023–; doi:10.1021/om0200050

data_4076775
_publ_section_title
;
 Oxidative Addition of H&#x2212;SiR3to Di- and Triruthenium Carbonyl
 Complexes Bearing a Bridging Azulene Ligand:&#x00A0; Isolation of New
 Silylruthenium Complexes and Catalytic Hydrosilylation of Ketones
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3023
_journal_paper_doi               10.1021/om0200050
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C33 H38 O4 Ru2 Si2'
_chemical_formula_weight         756.95
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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                   16.701(4)
_cell_length_b                   20.811(15)
_cell_length_c                   9.5303(19)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     3312(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction
;
teXsan for Windows version 1.06 (MSC, 1997-1999)
;
_computing_molecular_graphics    'ORTEP III (Farrujia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      296.2
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.137
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5391
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        -6.51
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.12(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1329
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0294P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1152
_reflns_number_gt                3188
_reflns_number_total             5360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0200050.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               4076775