Unexpected Formation of NHC-Stabilized Hydrosilylyne Complexes via Alkane Elimination from NHC-Stabilized Hydrido(alkylsilylene) Complexes.
Fukuda, Tetsuya; Hashimoto, Hisako; Tobita, Hiromi; Journal of the American Chemical Society 137 (2015) 10906–10909; doi:10.1021/jacs.5b06366

data_4124369
_publ_section_title
;
 Unexpected Formation of NHC-Stabilized Hydrosilylyne Complexes via Alkane
 Elimination from NHC-Stabilized Hydrido(alkylsilylene) Complexes.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10906
_journal_page_last               10909
_journal_paper_doi               10.1021/jacs.5b06366
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C27 H42 N4 O2 Si W'
_chemical_formula_sum            'C27 H42 N4 O2 Si W'
_chemical_formula_weight         666.59
_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                 103.81(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.01(3)
_cell_length_b                   14.11(3)
_cell_length_c                   15.26(3)
_cell_measurement_reflns_used    652
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      6.90
_cell_volume                     2720(10)
_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  0.0630
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25397
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    4.322
_exptl_absorpt_correction_T_max  0.8129
_exptl_absorpt_correction_T_min  0.4639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.046
_refine_diff_density_min         -1.569
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         6230
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0225P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0650
_reflns_number_gt                5168
_reflns_number_total             6230
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b06366_si_004.cif
_cod_data_source_block           ex20
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4124369