The first heterometallic borole complexes of Fe and Au have been prepa
red by reaction of [HFe{eta(5)-(1-phenylborole)}(CO)(2)](-) (1) with [
AuCl(PPh3)] in CH2Cl2, and the crystal structure of [(OC)(2){eta(5)-(1
-phenylborole)}Fe{Au(PPh3)}(2)] (2) reveals an interesting orientation
of the borole ligand. This complex reacts with [AuCl(PPh3)]/TIPF6 in
CH2Cl2 to give the new cationic FeAu3 cluster OC)(2){eta(5)-(1-phenylb
orole)}Fe{Au(PPh3)}(3)]PF6 (4) which has a tetrahedral metal core, as
established by a wide angle X-ray scattering study.