Syntheses, Crystal Structures, Spectroscopic Characterization, and Electrochemical Studies of the Ditungsten(III) Complexes Cl~3~W(μ-L)~3~WCl~3~ and [Cl~3~W(μ-L)~2~(μ-Cl)WCl~3~]^-^ (L = 1,4-Dithiane, 1,4-Thioxane, pms = Pentamethylene Sulfide). C-S Bond Cleavage of the Bridging Thioether(s) in Cl~3~W(μ-L)~3~WCl~3~
P. Michael Boorman; Naomi L. Langdon; Vivian J. Mozol; Masood Parvez; Glenn P. A. Yap; Inorganic Chemistry 37 (1998) 6023–6029; doi:10.1021/ic971542t

data_4323149
_publ_contact_author
;
    Masood Parvez
    Department of Chemistry
    University of Calgary
    2500 University Drive N.W.
    Calgary, Alberta, Canada T2N 1N4
;
_publ_contact_author_email       ' parvez@acs.ucalgary.ca '
_publ_contact_author_fax         ' (403)289-9488 '
_publ_contact_author_phone       ' (403)220-5348 '
_publ_section_title
;
 Syntheses, Crystal Structures, Spectroscopic Characterization, and
 Electrochemical Studies of the Ditungsten(III) Complexes
 Cl~3~W(\m-L)~3~WCl~3~ and [Cl~3~W(\m-L)~2~(\m-Cl)WCl~3~]^-^ (L =
 1,4-Dithiane, 1,4-Thioxane, pms = Pentamethylene Sulfide). C-S Bond
 Cleavage of the Bridging Thioether(s) in Cl~3~W(\m-L)~3~WCl~3~
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6023
_journal_page_last               6029
_journal_paper_doi               10.1021/ic971542t
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C13.5 H27 Cl6 O3.5 S3 W2'
_chemical_formula_weight         921.93
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   25.7603(3)
_cell_length_b                   25.7603(3)
_cell_length_c                   18.6771(2)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      1.47
_cell_volume                     12394.0(2)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL XPREP'
_computing_molecular_graphics    'Siemens SHELXTL XP'
_computing_publication_material  'Siemens SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       'hemisphere scans'
_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  0.0889
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23722
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         1.12
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    8.152
_exptl_absorpt_correction_T_max  0.3200
_exptl_absorpt_correction_T_min  0.2022
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6944
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.218
_refine_ls_goodness_of_fit_obs   1.234
_refine_ls_hydrogen_treatment    idealized
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.220
_refine_ls_restrained_S_obs      1.234
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_obs          0.0763
_refine_ls_shift/esd_max         -0.006
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+477.4664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1348
_refine_ls_wR_factor_obs         0.1309
_reflns_number_observed          3092
_reflns_number_total             3334
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971542t_3.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+477.4664P] 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^)+(0.0256P)^2^+477.4664P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_original_formula_sum        'C13.50 H27 Cl6 O3.50 S3 W2'
_cod_database_code               4323149