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Synthesis of two mercaptide-substituted hexanuclear molybdenum halide clusters. [((Mo/sub 6/Cl/sub 8/)(SCH/sub 2/CH/sub 3/)/sub 4/(C/sub 5/H/sub 5/N)/sub 2/) and Na/sub 2/((Mo/sub 6/Cl/sub 8/)(SCH/sub 2/CH/sub 3/)/sub 6/) x 3(C/sub 5/H/sub 5/N)]

Technical Report ·
DOI:https://doi.org/10.2172/7313701· OSTI ID:7313701

Two new derivatives of the ((Mo/sub 6/Cl/sub 8/)Cl/sub 4/) cluster have been prepared. Na/sub 2/((Mo/sub 6/Cl/sub 8/)(SC/sub 2/H/sub 5/)/sub 6/) . 3(C/sub 5/H/sub 5/N) was made by first reacting molybdenum dichloride with sodium ethyl mercaptide (1:6 mole ratio) in refluxing methanol. The orange product was recovered in pure crystalline form by extraction of the solid residue with pyridine. This compound was characterized by its X-ray powder pattern, elemental analysis, and infrared and electronic spectra. It dissolves in most polar solvents, yielding reddish-orange solutions. Treatment of alcohol solutions with hydrochloric acid causes rapid conversion to ((Mo/sub 6/Cl/sub 8/)Cl/sub 6/)/sup 2 -/, accompanied by the evolution of ethyl mercaptan. ((Mo/sub 6/Cl/sub 8/)(SC/sub 2/H/sub 5/)/sub 4/(C/sub 5/H/sub 5/N)/sub 2/) was prepared using the same procedure, starting with a 1:4 mole ratio of molybdenum dichloride and sodium ethyl mercaptide. This material was isolated as a red, amorphous solid. It was characterized by elemental analysis and infrared and electronic spectra. It is soluble in pyridine, DMSO, and DMF; other polar solvents must be acidified before it will dissolve. Treatment of this compound with a solution of concentrated hydrochloric acid in methanol again yielded ((Mo/sub 6/Cl/sub 8/)Cl/sub 6/)/sup 2 -/. Its amorphism and insolubility in most polar solvents suggest this compound might be polymeric. Individual cluster units are probably linked in a random way by intercluster mercaptide bridges. More extensive characterization of this compound in its solid state is required to confirm this.

Research Organization:
Ames Lab., IA (USA)
DOE Contract Number:
W-7405-ENG-82
OSTI ID:
7313701
Report Number(s):
IS-T-746
Country of Publication:
United States
Language:
English

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Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400201 -- Chemical & Physicochemical Properties
400301* -- Organic Chemistry-- Chemical & Physicochemical Properties-- (-1987)
AZINES
CHEMICAL ANALYSIS
CHEMICAL PREPARATION
CHEMICAL REACTIONS
CHLORIDES
CHLORINE COMPOUNDS
COHERENT SCATTERING
COMPLEXES
DECOMPOSITION
DIFFRACTION
DMSO
ELECTRONIC STRUCTURE
EXTRACTION
HALIDES
HALOGEN COMPOUNDS
HETEROCYCLIC COMPOUNDS
HYDROCHLORIC ACID
HYDROGEN COMPOUNDS
INORGANIC ACIDS
MOLYBDENUM CHLORIDES
MOLYBDENUM COMPLEXES
MOLYBDENUM COMPOUNDS
ORGANIC COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
ORGANIC SULFUR COMPOUNDS
ORGANOMETALLIC COMPOUNDS
PYRIDINE
PYRIDINES
SCATTERING
SEPARATION PROCESSES
SOLUBILITY
SOLVENT EXTRACTION
SULFOXIDES
SYNTHESIS
THIOLS
TRANSITION ELEMENT COMPLEXES
TRANSITION ELEMENT COMPOUNDS
X-RAY DIFFRACTION