METHYLTRIOXORHENIUM - AIR-STABLE COMPOUND CONTAINING A CARBON-RHENIUM BOND

During the preparation of trimethyldioxorhenium (using literature methods1), we observed the growth of needle crystals in tubes containing residues and which had been left open to the atmosphere. Purification of the product by sublimation in vacuo resulted in the isolation of a colorless crystalline material which melted sharply. Elemental analysis suggested the compound to be methyltrioxorhenium. The compound could be synthesized by exposure of either tetramethyloxorhenium2 or trimethyldioxorhenium1 to dry air in a closed system. The mass spectrum showed parention peaks CH3ReO3+ at 250 and 248 mass units corresponding to species containing 187 Re and 185 Re, respectively. The two peaks did not have the expected intensity ratio based on the relative isotopic abundances, due to the overlap of the lower mass unit peak with that of the species CH187ReO3+. © 1979, American Chemical Society. All rights reserved.