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_4076774
_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            'C27 H27 O6 Ru3 Si'
_chemical_formula_weight         778.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.816(12)
_cell_angle_beta                 112.652(6)
_cell_angle_gamma                77.36(2)
_cell_formula_units_Z            2
_cell_length_a                   10.990(3)
_cell_length_b                   14.709(5)
_cell_length_c                   9.685(3)
_cell_measurement_reflns_used    7674
_cell_measurement_temperature    183
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.2
_cell_volume                     1409.5(8)
_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_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF94 PATTY (Beurskens, 1994)'
_diffrn_ambient_temperature      183
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.720
_diffrn_measurement_device       'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       oscillation
_diffrn_orient_matrix_UB_11      -0.00812
_diffrn_orient_matrix_UB_12      -0.06494
_diffrn_orient_matrix_UB_13      0.01343
_diffrn_orient_matrix_UB_21      -0.09496
_diffrn_orient_matrix_UB_22      0.01371
_diffrn_orient_matrix_UB_23      -0.07485
_diffrn_orient_matrix_UB_31      0.03294
_diffrn_orient_matrix_UB_32      -0.02125
_diffrn_orient_matrix_UB_33      -0.08209
_diffrn_radiation_detector       'Imaging Plate'
_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    0.0516
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4960
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.668
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.600
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             766
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.054
_refine_diff_density_min         -1.594
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         4660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0676
_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^)+(0.0995P)^2^+11.1059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1791
_reflns_number_gt                3609
_reflns_number_total             4960
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0200050.cif
_cod_data_source_block           6
_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 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1409.6(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4076774