Synthesis of a Tungsten‒Silylyne Complex via Stepwise Proton and Hydride Abstraction from a Hydrido Hydrosilylene Complex
Fukuda, Tetsuya; Yoshimoto, Takashi; Hashimoto, Hisako; Tobita, Hiromi; Organometallics 35 (2016) 921–; doi:10.1021/acs.organomet.6b00095

data_4086444
_publ_section_title
;
 Synthesis of a Tungsten--Silylyne Complex via Stepwise Proton and Hydride
 Abstraction from a Hydrido Hydrosilylene Complex
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              921
_journal_paper_doi               10.1021/acs.organomet.6b00095
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C22 H42 O2 Si4 W'
_chemical_formula_sum            'C22 H42 O2 Si4 W'
_chemical_formula_weight         634.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                68.987(6)
_cell_angle_beta                 89.604(4)
_cell_angle_gamma                79.879(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2590(11)
_cell_length_b                   12.6926(10)
_cell_length_c                   13.2925(15)
_cell_measurement_reflns_used    8464
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.64
_cell_volume                     1432.9(3)
_computing_data_collection       'teXsan Ver. 1.11'
_computing_molecular_graphics    'Yadokari-XG 2009(Wakita,Nemoto et al.,2009)'
_computing_publication_material  'Yadokari-XG 2009(Wakita,Nemoto et al.,2009)'
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotation-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13385
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    4.213
_exptl_absorpt_correction_T_max  0.3646
_exptl_absorpt_correction_T_min  0.2586
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   NUMABS(Higashi,1999),ABSCOR(Higashi,1995)
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.417
_refine_diff_density_min         -1.454
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         6428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.2708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                6177
_reflns_number_total             6428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00095_si_003.cif
_cod_data_source_block           tf141
_cod_depositor_comments
'Adding full bibliography for 4086443--4086444.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4086444