Synthesis of Self-Stabilized and Donor-Free Silyl(silylene)tungsten Complexes
Ueno, Keiji; Asami, Satsuki; Watanabe, Nobuhiko; Ogino, Hiroshi; Organometallics 21 (2002) 1326–; doi:10.1021/om020023h

data_4076783
_publ_section_title
;
 Synthesis of Self-Stabilized and Donor-Free Silyl(silylene)tungsten
 Complexes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1326
_journal_paper_doi               10.1021/om020023h
_journal_volume                  21
_journal_year                    2002
_chemical_formula_moiety
;
 '(C5 (C H3)4 (C2 H5) W (C O)2 Si(C H3)2 Si(C H3)3'
;
_chemical_formula_sum            'C18 H32 O2 Si2 W'
_chemical_formula_weight         520.47
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 112.43(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.184(3)
_cell_length_b                   26.208(9)
_cell_length_c                   9.354(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      22.41
_cell_measurement_theta_min      22.09
_cell_volume                     2081.1(12)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        TeXsan
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6397
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        0.629
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.672
_exptl_absorpt_correction_T_max  0.9994
_exptl_absorpt_correction_T_min  0.5700
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         5.693
_refine_diff_density_min         -9.356
_refine_diff_density_rms         0.374
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         6073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.070
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1278P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1669
_reflns_number_gt                4826
_reflns_number_total             6073
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020023h.cif
_cod_data_source_block           2b
_cod_original_cell_volume        2081.2(11)
_cod_database_code               4076783