Synthesis and characterization of reduced tungsten sulfide cluster complexes

Technical Report · Thu Jun 27 04:00:00 EDT 1991

OSTI ID:5487981

Zhang, Xiang

Reduction of tungsten(IV) chloride with metals was studied in order to find a high-yield and convenient preparation of {alpha}-tungsten (II) chloride. The reduction of tungsten(IV) chloride with iron metal proved to be the most convenient and reliable synthesis, with a good yield of 60%. The reactions between {alpha}-tungsten(II) chloride and sodium hydrosulfide were investigated. Complete substitution of sulfide for chloride in W{sub 6}Cl{sub 8}{sup 4+} was achieved in the presence of sodium n-butoxide in pyridine solution. Single crystals were grown at elevated temperature (200{degrees}C) in pyridine, and the structure of W{sub 6}S{sub 8}(py){sub 6} was determined by single crystal x-ray techniques. The triethylphosphine (PEt{sub 3}) and tetrahydrothiophene (THT) complexes of W{sub 6}S{sub 8} were established by ligand displacement of pyridine in W{sub 6}S{sub 8}(py){sub 6}. Structures for both W{sub 6}S{sub 8}(PEt{sub 3}){sub 6}. 1.44CH{sub 2}Cl{sub 2} and W{sub 6}S{sub 8}(THT){sub 6} were determined by single crystal x-ray diffraction. These molecular complexes of the W{sub 6}S{sub 8} cluster were also characterized by infrared spectroscopy. 86 refs., 19 figs., 22 tabs.

• Research Organization: Ames Lab., IA (United States)
• Sponsoring Organization: DOE; USDOE, Washington, DC (United States)
• DOE Contract Number: W-7405-ENG-82
• OSTI ID: 5487981
• Report Number(s): IS-T-1534; ON: DE91014916
• Country of Publication: United States
• Language: English

Related Subjects

36 MATERIALS SCIENCE
360602* -- Other Materials-- Structure & Phase Studies
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400201 -- Chemical & Physicochemical Properties
AZINES
CHALCOGENIDES
CHEMICAL PREPARATION
CHEMICAL REACTIONS
CHLORIDES
CHLORINE COMPOUNDS
COHERENT SCATTERING
COMPLEXES
DIFFRACTION
ELECTRIC CONDUCTIVITY
ELECTRICAL PROPERTIES
HALIDES
HALOGEN COMPOUNDS
HETEROCYCLIC COMPOUNDS
INFRARED SPECTRA
LIGANDS
ORGANIC COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
PHYSICAL PROPERTIES
PYRIDINE
PYRIDINES
REDUCTION
REFRACTORY METAL COMPOUNDS
SCATTERING
SOLID CLUSTERS
SPECTRA
STRUCTURAL CHEMICAL ANALYSIS
SULFIDES
SULFUR COMPOUNDS
SUPERCONDUCTIVITY
SYNTHESIS
TRANSITION ELEMENT COMPLEXES
TRANSITION ELEMENT COMPOUNDS
TUNGSTEN CHLORIDES
TUNGSTEN COMPLEXES
TUNGSTEN COMPOUNDS
TUNGSTEN SULFIDES
X-RAY DIFFRACTION