Synthesis and Properties of a Silyl(silylene)ruthenium Complex: Activation Barrier of the Ru═Si Bond Rotation and Facile Replacement of the Methyl Groups with Alkoxy Groups of a Silyl Ligand
Hashimoto, Hisako; Sato, Jun; Tobita, Hiromi; Organometallics 28 (2009) 3963–; doi:10.1021/om900177z

data_4069405
_publ_section_title
;
 Synthesis and Properties of a Silyl(silylene)ruthenium Complex:
 Activation Barrier of the Ru&#x2550;Si Bond Rotation and Facile
 Replacement of the Methyl Groups with Alkoxy Groups of a Silyl Ligand
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3963
_journal_paper_doi               10.1021/om900177z
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C32 H46 O Ru Si2 '
_chemical_formula_sum            'C32 H46 O Ru Si2'
_chemical_formula_weight         603.96
_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                 95.1401(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5565(3)
_cell_length_b                   18.7387(7)
_cell_length_c                   15.7809(6)
_cell_measurement_reflns_used    21702
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      1.7
_cell_volume                     3109.15(19)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26763
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  0.8589
_exptl_absorpt_correction_T_min  0.8541
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         6879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+2.4185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.1004
_reflns_number_gt                6166
_reflns_number_total             6879
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900177z_si_002.cif
_cod_data_source_block           jun1
_cod_original_formula_sum        'C32 H46 O Ru Si2 '
_cod_database_code               4069405