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An unprecedented alkyne–nitrile metathesis takes place when the highvalent ironnitrido dication FeLN2+, with L=2,6bis2methyl1,3diaminopropan2ylpyridine, is reacted with alkynes in the gas phase under thermal conditions. While the detailed role of the alkyne substrate with respect to relative rates, regioselectivities, and branching ratios remains to be elucidated, the very existence of this novel metathesis reaction provides additional experimental evidence of a genuine, longlived, formal ironVnitrido dication. [ABSTRACT FROM AUTHOR]