Abstract Phenylethynyl itterbium derivative (PhC≡ C) 2 Yb (THF) 2 reacts with tetraphenylantimony halides in tetrahydrofuran (THF) at room temperature to form triphenylantimony, phenylacetylene, benzene, and phenylethynylitterbium PhC≡ CYbX (THF) 4 and itterbium YbX 2 (THF) 4 halides; X= Cl, Br, I. The reduction of the antimony derivative is accompanied with the generation of phenyl and phenylethynyl radicals