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_8000050
_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            'C28 H38 N2 O2 Si W'
_chemical_formula_weight         646.54
_space_group_IT_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                93.026(3)
_cell_angle_beta                 93.875(2)
_cell_angle_gamma                113.821(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1870(2)
_cell_length_b                   9.70270(10)
_cell_length_c                   16.6719(5)
_cell_measurement_temperature    150(2)
_cell_volume                     1351.17(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12568
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    4.346
_exptl_absorpt_correction_T_max  0.6704
_exptl_absorpt_correction_T_min  0.3555
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.291
_refine_diff_density_min         -3.908
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.378
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         6129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.378
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+28.9400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                6001
_reflns_number_total             6129
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               8000050