Reversible 1,2-Migration of Aryl Groups on Silyl Ligands: Formation and Properties of Silylenetungsten Complexes Stabilized by an External Base
Eiji Suzuki; Masaaki Okazaki; Hiromi Tobita; Chemistry Letters 34 (2005) 1026–; doi:10.1246/cl.2005.1026

data_8000049
_publ_section_title
;
 Reversible 1,2-Migration of Aryl Groups on Silyl Ligands: Formation
 and Properties of Silylenetungsten Complexes Stabilized by an External
 Base
;
_journal_issue                   7
_journal_name_full               'Chemistry Letters'
_journal_page_first              1026
_journal_paper_doi               10.1246/cl.2005.1026
_journal_volume                  34
_journal_year                    2005
_chemical_formula_sum            'C27 H36 N2 O2 Si W'
_chemical_formula_weight         632.52
_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                84.401(2)
_cell_angle_beta                 79.749(4)
_cell_angle_gamma                72.982(3)
_cell_formula_units_Z            4
_cell_length_a                   9.3757(5)
_cell_length_b                   14.2704(12)
_cell_length_c                   21.0280(10)
_cell_measurement_reflns_used    10441
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      54.84
_cell_measurement_theta_min      2.99
_cell_volume                     2644.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ' '
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0857
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21775
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         0.99
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    4.439
_exptl_absorpt_correction_T_max  0.8085
_exptl_absorpt_correction_T_min  0.4705
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Higashit, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.151
_refine_diff_density_min         -4.045
_refine_diff_density_rms         0.349
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         10873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.1278
_refine_ls_R_factor_gt           0.1034
_refine_ls_shift/su_max          2.247
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+237.4687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2395
_refine_ls_wR_factor_ref         0.2528
_reflns_number_gt                8581
_reflns_number_total             10873
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               8000049