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_4089053
_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         'C53 H70 O3 Si W'
_chemical_formula_sum            'C53 H70 O3 Si W'
_chemical_formula_weight         967.03
_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                99.1384(19)
_cell_angle_beta                 105.6093(17)
_cell_angle_gamma                100.000(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2995(5)
_cell_length_b                   13.3593(6)
_cell_length_c                   17.9891(9)
_cell_measurement_reflns_used    32276
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.11
_cell_volume                     2291.90(19)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1325
_diffrn_reflns_av_sigmaI/netI    0.0961
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37104
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    2.588
_exptl_absorpt_correction_T_max  0.8602
_exptl_absorpt_correction_T_min  0.6674
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.163
_refine_diff_density_min         -3.340
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         10504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0746
_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^)+(0.0523P)^2^+27.3012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1667
_reflns_number_gt                8896
_reflns_number_total             10504
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4086764
_cod_data_source_file            om6b00670_si_002.cif
_cod_data_source_block           benzophenone_adduct_6
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4089053