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The reaction between [Os,(CO), ,(MeCN),] and q2-Fe[C,H,(C2SiMe3)l,)l 1 and the decarbonylated product of this complex, [OS,(CO)~(~~-~~-F~[C,H,(C~S~M~~)]~}] 2, the structure of which has been shown by X-ray crystallography to incorporate a triosmium cluster linked oia a metallobutadienyl ligand to a ferrocene unit; the cyclic voltammogram of 2 shows a reversible one-electron oxidation of the ferrocene unit and an irreversible two-electron [Fe( c 5H,(C2SiMed) 21 yielded Los, ( c o ) 1 0 { p 3reduction for the triosmium unit.Recent reports have indicated that organic complexes and polymers which contain ferrocene or metal-alkyne units exhibit novel physical properties which may have applications in the electronicsWe have been undertaking a series of studies which involve the incorporation of both ferrocene and metal-alkyne units into the same heterobimetallic complex. These systems exhibit 'donor-acceptor' characteristics and show potential for non-linear optical b e h a ~i o u r . ~. ~In this communication we describe a novel extension of this work to include diyne systems and report the linkage of a ferrocene derivative to a triosmium cluster unit via a co-ordinated diyne.The reaction of the activated cluster [OS,(CO),,(M~CN)~]~ with the bis(trimethylsilylalkyny1)-substituted ferrocene derivative [Fe{q 5-C,H,(C2SiMe,)} 2] at room temperature, in dichloromethane, led to an instantaneous change from orange to deep red, and after 0.5 h the IR spectrum of the reaction mixture shows that none of the starting material remains. Separation and purification of the reaction mixture by TLC afforded two red bands. The first, characterised as