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_4086443
_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         '(C40 H43 B F15 O2 Si4 W)(C11 H21 N2)'
_chemical_formula_sum            'C51 H64 B F15 N2 O2 Si4 W'
_chemical_formula_weight         1329.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.128(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0977(19)
_cell_length_b                   28.123(4)
_cell_length_c                   15.752(2)
_cell_measurement_reflns_used    43999
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.70
_cell_measurement_theta_min      3.00
_cell_volume                     5787.1(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1017
_diffrn_reflns_av_sigmaI/netI    0.0896
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            56270
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    2.167
_exptl_absorpt_correction_T_max  0.7810
_exptl_absorpt_correction_T_min  0.6711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.782
_refine_diff_density_min         -2.964
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.267
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         13242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.267
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0862
_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^)+(0.0178P)^2^+79.8872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1861
_refine_ls_wR_factor_ref         0.1939
_reflns_number_gt                10284
_reflns_number_total             13242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00095_si_002.cif
_cod_data_source_block           ex14
_cod_depositor_comments
'Adding full bibliography for 4086443--4086444.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4086443