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_4086760
_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         'C57 H88 N2 O2 Si W'
_chemical_formula_sum            'C57 H88 N2 O2 Si W'
_chemical_formula_weight         1045.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.2122(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8192(3)
_cell_length_b                   27.4879(4)
_cell_length_c                   16.5417(3)
_cell_measurement_reflns_used    81718
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      1.48
_cell_volume                     5372.95(18)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0731
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            78479
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    2.213
_exptl_absorpt_correction_T_max  0.6659
_exptl_absorpt_correction_T_min  0.6301
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.235
_refine_diff_density_min         -2.846
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.340
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         12230
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.340
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0316P)^2^+15.0529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                10870
_reflns_number_total             12230
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00670_si_002.cif
_cod_data_source_block           '_anionic_silylene_complex_(Eind)/4_C6H6'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 4624 2016-04-14 12:54:50Z antanas 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4086760