Reactions of Tungsten Acetylide‒Silylene Complexes with Pyridines: Direct Observation of Silylene/Silyl Migration in Tungsten Acetylide and Carbyne/Vinylidene Frameworks
Sakaba, Hiroyuki; Oike, Hiroyuki; Arai, Yasuhiro; Kwon, Eunsang; Organometallics 31 (2012) 8172–; doi:10.1021/om300772c

data_4079490
_publ_section_title
;
 Reactions of Tungsten Acetylide--Silylene Complexes with Pyridines:
 Direct Observation of Silylene/Silyl Migration in Tungsten Acetylide and
 Carbyne/Vinylidene Frameworks
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              8172
_journal_paper_doi               10.1021/om300772c
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C40 H51 N2 O2 Si W'
_chemical_formula_sum            'C40 H51 N2 O2 Si W'
_chemical_formula_weight         803.79
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 107.810(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   35.081(7)
_cell_length_b                   11.577(2)
_cell_length_c                   19.643(4)
_cell_measurement_reflns_used    10694
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.12
_cell_volume                     7595(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            53484
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.111
_exptl_absorpt_correction_T_max  0.537
_exptl_absorpt_correction_T_min  0.457
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3272.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.210
_refine_diff_density_max         2.930
_refine_diff_density_min         -0.740
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     415
_refine_ls_number_reflns         8585
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0275P)^2^+18.1017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0587
_reflns_number_gt                8055
_reflns_number_total             8585
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om300772c_si_001.cif
_cod_data_source_block           cis4_0.5hexane
_cod_original_cell_volume        7596(3)
_cod_database_code               4079490