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_4079491
_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         'C36 H44 N2 O2 Si2 W '
_chemical_formula_sum            'C36 H44 N2 O2 Si2 W'
_chemical_formula_weight         776.78
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                92.190(6)
_cell_angle_beta                 95.119(4)
_cell_angle_gamma                91.953(5)
_cell_formula_units_Z            2
_cell_length_a                   9.675(3)
_cell_length_b                   11.977(4)
_cell_length_c                   15.321(5)
_cell_measurement_reflns_used    5489
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      5.1
_cell_volume                     1765.7(10)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      173.00
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25319
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_exptl_absorpt_coefficient_mu    3.375
_exptl_absorpt_correction_T_max  0.509
_exptl_absorpt_correction_T_min  0.336
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             784.00
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.82
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     432
_refine_ls_number_reflns         8021
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0005Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0672
_reflns_number_gt                7584
_reflns_number_total             8021
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om300772c_si_001.cif
_cod_data_source_block           6a
_cod_original_cell_volume        1765.8(10)
_cod_original_formula_sum        'C36 H44 N2 O2 Si2 W '
_cod_database_code               4079491