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Stoichiometric reduction of carbon monoxide in metal carbonyl complexes: the search for metal nuclearity effects

Thesis/Dissertation ·
OSTI ID:5622836
This research explores the dependence of metal cluster nuclearity on the homogeneous and heterogeneous reactions of transition metal carbonyl complexes. The effects of metal nuclearity on the proton-induced reduction of CO to CH/sub 4/ in metal carbonyls are described. A survey of the reaction of metal carbonyl complexes in neat super acid at room temperature revealed that a minimum number of 4 metals is required for the production of CH/sub 4/. Cases in which trace amounts of CH/sub 4/ were detected for 2- and 3-metal systems are thought to proceed through the initial formation of 4-metal (or larger) clusters. An important intermediate in the proton-induced reduction of CO to CH/sub 4/ in (Fe/sub 4/(CO)/sub 13/)/sup 2 -/, namely HFe/sub 4/(CH)(CO)/sub 12/, is investigated. Spectroscopic studies indicate the cluster undergoes protonation in neat HSO/sub 3/CF/sub 3/ to yield the dihydride cluster (H/sub 2/Fe/sub 4/(CH)(CO)/sub 12/)/sup +/. The reaction of HFe/sub 4/(CH)(CO)/sub 12/ with neat HSO/sub 3/CF/sub 3/ at room temperature exhibits an induction period of about 1 week, after which 1 mole of CH/sub 4/ per mole of cluster is produced over the next 50 days. Adding reducing agents to the reaction eliminates the induction period but does not significantly increase the rate of CH/sub 4/ evolution.
OSTI ID:
5622836
Country of Publication:
United States
Language:
English