Synthesis, Structure, and Fluxional Behavior of Donor-Stabilized Bis(silylene)tungsten Complexes
Ueno, Keiji; Masuko, Akira; Ogino, Hiroshi; Organometallics 16 (1997) 5023–; doi:10.1021/om970609h

data_4078388
_publ_section_title
;
 Synthesis, Structure, and Fluxional Behavior of Donor-Stabilized
 Bis(silylene)tungsten Complexes
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5023
_journal_paper_doi               10.1021/om970609h
_journal_volume                  16
_journal_year                    1997
_chemical_formula_sum            'C6 H10 O1.5 Si W0.5'
_chemical_formula_weight         226.15
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2ab'
_symmetry_space_group_name_H-M   'P b m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.771(6)
_cell_length_b                   14.478(6)
_cell_length_c                   8.755(4)
_cell_measurement_reflns_used    86
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      25
_cell_volume                     1618.8(13)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC-6A'
_diffrn_measurement_method       omega/2theta
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
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_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2212
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.33
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.282
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.36
_refine_diff_density_max         3.650
_refine_diff_density_min         -3.678
_refine_diff_density_rms         0.318
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.960
_refine_ls_goodness_of_fit_obs   1.035
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         2212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
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_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_obs          0.0617
_refine_ls_shift/esd_max         -0.034
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1494
_refine_ls_wR_factor_obs         0.1380
_reflns_number_observed          1640
_reflns_number_total             2212
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om970609h.cif
_cod_data_source_block           CpW(CO)2{(SiMe2)2...OMe}
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'orthorohmbic' was replaced with
'orthorhombic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1618.8(12)
_cod_original_sg_symbol_H-M      Pbma
_cod_original_formula_sum        'C6 H10 O1.50 Si W0.50'
_cod_database_code               4078388