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_4323148
_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            'C18 H36 Cl6 O2 S6 W2'
_chemical_formula_weight         1057.26
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           'by teXsan v1.7'
_cell_angle_alpha                90
_cell_angle_beta                 93.34(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.518(3)
_cell_length_b                   9.475(2)
_cell_length_c                   27.408(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    170
_cell_measurement_theta_max      10.8
_cell_measurement_theta_min      9.2
_cell_volume                     3245.3(11)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'teXsan (MSC, 1995)'
_computing_structure_solution    'Direct methods'
_diffrn_ambient_temperature      170
_diffrn_measurement_device       'Rigaku AFC6S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.01210
_diffrn_orient_matrix_UB_12      0.10230
_diffrn_orient_matrix_UB_13      -0.00675
_diffrn_orient_matrix_UB_21      0.02874
_diffrn_orient_matrix_UB_22      -0.02496
_diffrn_orient_matrix_UB_23      -0.03218
_diffrn_orient_matrix_UB_31      -0.07369
_diffrn_orient_matrix_UB_32      0.00706
_diffrn_orient_matrix_UB_33      -0.01596
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_av_sigmaI/netI    0.110
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            6431
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        1.93
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.125
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    2.164
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2024.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         '1.71 (between W-atoms)'
_refine_diff_density_min         -1.77
_refine_ls_extinction_coef       0.000000108(7)
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   1.896
_refine_ls_goodness_of_fit_obs   1.896
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_obs          0.0463
_refine_ls_shift/esd_max         0.0013
_refine_ls_shift/esd_mean        0.0001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0478
_refine_ls_wR_factor_obs         0.0478
_reflns_number_observed          3316
_reflns_number_total             6132
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ic971542t_2.cif
_cod_data_source_block           Compound_1
_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 'w = 1/[\s^2^(Fo) +
0.00002|Fo|^2^]' 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) + 0.00002|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3245(1)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C18 H36 Cl6 O2 S6 W2 '
_cod_database_code               4323148