Synthesis and Structure of Ruthenium-Silylene Complexes: Activation of Si-Cl Bonds in N-Heterocyclic Silanes
Hyojong Yoo; Patrick J. Carroll; Donald H. Berry; Journal of the American Chemical Society 128 (2006) 6038–6039; doi:10.1021/ja0580744

data_4110580
_publ_section_title
;
 Synthesis and Structure of Ruthenium-Silylene Complexes: Activation of
 Si-Cl Bonds in N-Heterocyclic Silanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6038
_journal_page_last               6039
_journal_paper_doi               10.1021/ja0580744
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C43 H58 Cl N5 Ru Si'
_chemical_formula_weight         809.55
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                62.065(3)
_cell_angle_beta                 80.408(4)
_cell_angle_gamma                80.262(4)
_cell_formula_units_Z            4
_cell_length_a                   13.1359(5)
_cell_length_b                   18.6998(5)
_cell_length_c                   19.8721(5)
_cell_measurement_temperature    143(1)
_cell_volume                     4229.0(3)
_computing_data_collection       'CrystalClear (Rigaku, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       'phi and omega rotations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37358
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7298
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         18587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+3.4612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1051
_reflns_number_gt                15141
_reflns_number_total             18587
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0580744si20051128_020434.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        4229.0(2)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4110580