Reactions of (Silyl)(silylene)tungsten and -molybdenum Complexes with Sulfur Reagents
Muraoka, Takako; Nakamura, Tomoko; Nakamura, Atsushi; Ueno, Keiji; Organometallics 29 (2010) 6624–; doi:10.1021/om100875h

data_4067172
_publ_section_title
;
 Reactions of (Silyl)(silylene)tungsten and -molybdenum Complexes with
 Sulfur Reagents
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6624
_journal_paper_doi               10.1021/om100875h
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         '(C36 H53 O2 S2 Si2 W1) (C5 C12)0.25'
_chemical_formula_sum            'C34.25 H49 O2 S2 Si2 W'
_chemical_formula_weight         796.88
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.64(4)
_cell_angle_beta                 83.42(5)
_cell_angle_gamma                63.19(4)
_cell_formula_units_Z            2
_cell_length_a                   11.566(3)
_cell_length_b                   11.7367(11)
_cell_length_c                   16.033(3)
_cell_measurement_reflns_used    336
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.0307
_cell_measurement_theta_min      1.3387
_cell_volume                     1842.6(10)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.724
_diffrn_measured_fraction_theta_max 0.724
_diffrn_measurement_device_type  'RIGAKU RAXIS-IV Imaging Plate'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20675
_diffrn_reflns_theta_full        32.27
_diffrn_reflns_theta_max         32.27
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    3.340
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.8669
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             809
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.398
_refine_diff_density_min         -1.704
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         9473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.341
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.433
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0186P)^2^+6.8249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                9356
_reflns_number_total             9473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100875h_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1842.7(6)
_cod_database_code               4067172