Tris[(alkylthio)methyl]silanes: Syntheses and Structures of Chromium, Molybdenum, and Tungsten Complexes with a Tripodal Thioether Ligand
Hing W. Yim; Linh M. Tran; Ebern D. Dobbin; Daniel Rabinovich; Louise M. Liable-Sands; Christopher D. Incarvito; Kin-Chung Lam; Arnold L. Rheingold; Inorganic Chemistry 38 (1999) 2211–2215; doi:10.1021/ic981001j

data_4321947
_publ_contact_author
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     Dr. Daniel Rabinovich
     Department of Chemistry
     University of North Carolina at Charlotte
     9201 University City Blvd.
     Charlotte, NC  28223
     USA
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_publ_contact_author_email       DRabinov@email.uncc.edu
_publ_contact_author_fax         '+704 547 3151'
_publ_contact_author_phone       '+704 547 4442'
_publ_section_title
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 Tris[(alkylthio)methyl]silanes: Syntheses and Structures of Chromium,
 Molybdenum, and Tungsten Complexes with a Tripodal Thioether Ligand
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2211
_journal_page_last               2215
_journal_paper_doi               10.1021/ic981001j
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C10 H18 Mo O3 S3 Si'
_chemical_formula_weight         406.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.8987(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.34630(6)
_cell_length_b                   15.2747(2)
_cell_length_c                   27.1865(4)
_cell_measurement_reflns_used    7801
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3465.51(7)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      198(2)
_diffrn_measurement_device       'Siemens P4/CCD'
_diffrn_measurement_method       'phi, omega'
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19659
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    1.184
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       rod
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.064
_refine_ls_goodness_of_fit_obs   1.103
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         7789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_restrained_S_obs      1.103
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_obs          0.0260
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0634
_refine_ls_wR_factor_obs         0.0603
_reflns_number_observed          6722
_reflns_number_total             7793
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981001j_2.cif
_cod_data_source_block           drab03
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0300P)^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^)+(0.0300P)^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        3465.44(10)
_cod_database_code               4321947