A Silylyne Tungsten Complex Having an Eind Group on Silicon: Its Dimer–Monomer Equilibrium and Cycloaddition Reactions with Carbodiimide and Diaryl Ketones
Yoshimoto, Takashi; Hashimoto, Hisako; Hayakawa, Naoki; Matsuo, Tsukasa; Tobita, Hiromi; Organometallics 35 (2016) 3444–3447; doi:10.1021/acs.organomet.6b00670

data_4089050
_publ_section_title
;
 A Silylyne Tungsten Complex Having an Eind Group on Silicon: Its
 Dimer--Monomer Equilibrium and Cycloaddition Reactions with Carbodiimide
 and Diaryl Ketones
;
_journal_coden_ASTM              ORGND7
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              3444
_journal_page_last               3447
_journal_paper_doi               10.1021/acs.organomet.6b00670
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C83 H127 O4 Si2 W2'
_chemical_formula_sum            'C83 H127 O4 Si2 W2'
_chemical_formula_weight         1612.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.3105(15)
_cell_angle_beta                 88.5806(19)
_cell_angle_gamma                76.323(3)
_cell_formula_units_Z            2
_cell_length_a                   13.7165(8)
_cell_length_b                   14.2405(6)
_cell_length_c                   20.9850(15)
_cell_measurement_reflns_used    22177
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      1.95
_cell_volume                     3955.6(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        '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 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37542
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         0.98
_exptl_absorpt_coefficient_mu    2.982
_exptl_absorpt_correction_T_max  0.7547
_exptl_absorpt_correction_T_min  0.5471
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1666
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.907
_refine_diff_density_min         -1.401
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         17722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0568P)^2^+9.0280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                14805
_reflns_number_total             17722
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4086761
_cod_data_source_file            om6b00670_si_002.cif
_cod_data_source_block           silylyne_complex_dimer_2_0.5_C6H14
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4089050