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_4086762
_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         '(C11 H21 N2), (C18 H B F15)'
_chemical_formula_sum            'C29 H22 B F15 N2'
_chemical_formula_weight         694.30
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.9836(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3068(3)
_cell_length_b                   11.0982(5)
_cell_length_c                   28.5353(10)
_cell_measurement_reflns_used    35395
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.44
_cell_volume                     2936.23(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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0839
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            42296
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_T_max  0.9921
_exptl_absorpt_correction_T_min  0.9689
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.268
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         6725
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.268
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0937
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+4.5050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2076
_reflns_number_gt                5266
_reflns_number_total             6725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00670_si_002.cif
_cod_data_source_block           '[HMeIiPr][HS(C6F5)3]'
_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               4086762