Synthesis and Characterization of DMAP-Stabilized Aryl(silylene) Complexes and (Arylsilyl)(DMAP) Complexes of Tungsten: Mechanistic Study on the Interconversion between These Complexes via 1,2-Aryl Migration
Suzuki, Eiji; Komuro, Takashi; Okazaki, Masaaki; Tobita, Hiromi; Organometallics 28 (2009) 1791–; doi:10.1021/om801140d

data_4068873
_publ_section_title
;
 Synthesis and Characterization of DMAP-Stabilized Aryl(silylene)
 Complexes and (Arylsilyl)(DMAP) Complexes of Tungsten: Mechanistic Study
 on the Interconversion between These Complexes via 1,2-Aryl Migration
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1791
_journal_paper_doi               10.1021/om801140d
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C37.5 H46 N2 O2 Si W'
_chemical_formula_weight         768.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.067(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.348(7)
_cell_length_b                   9.7497(16)
_cell_length_c                   24.761(4)
_cell_measurement_reflns_used    29149
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.3
_cell_volume                     6954(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1124
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            17256
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    3.391
_exptl_absorpt_correction_T_max  0.7279
_exptl_absorpt_correction_T_min  0.4397
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
HIGASHI, T. (1999). Shape - Program to obtain Crystal Shape using CCD camera.
Rigaku Corporation, Tokyo, Japan. 
HIGASHI, T. (1999). Numabs - Numerical Absorption Correction,
Rigaku Corporation, Tokyo, Japan. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.271
_refine_diff_density_min         -2.521
_refine_diff_density_rms         0.294
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         7167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0788
_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^)+(0.0837P)^2^+243.5877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1988
_refine_ls_wR_factor_ref         0.2432
_reflns_number_gt                5177
_reflns_number_total             7167
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om801140d_si_001.cif
_cod_data_source_block           complex1c
_cod_original_formula_sum        'C37.50 H46 N2 O2 Si W'
_cod_database_code               4068873