The rhodacarbaborane salts (I) and (IV) are used to prepare the mixed‐metal complexes (III), (V), (VII), and (VIII).

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Treatment of [PtCI(H) (PEt,),] with [NEt,] [Rh(CO) (PPh,) (q5-7,9-C,B,Hll)] in thf (tetrahydrofuran) in the presence of TIBF, affords [RhPt(p-H) (p-CO) (PEt,),( PPh,) (q5-7,9-C,B,H,,)], the structure of which has been established by X-ray diffraction. On heating at reflux in thf for several days the compound yields [ RhPt(p-ts:q 5-7,9-C,B,Hl,) (CO) (PEt,),( PPh,)], a product in which the rhodium-platinum bond is spanned by an exopolyhedral cage B-Pt linkage. Reactions between the platinum compounds [PtCI(R)L,] (R = M e or Ph; L = PEt,, PPh, or PMe,Ph) and [NEt,][Rh(CO)(PPh3)(q5-7,n-C,BgH,,)] (n = 8 or 9) afford several dimetal complexes in which the Rh-Pt bonds are bridged by exopolyhedral cage B-H -Pt or B-Pt bridge bonds. The latter are formed from the former by loss of RH molecules, and this process is favoured for Rh(q5-7,9-C,BgHll) versus Rh(q5-7,8-C,B,Hll), and in the order L = PPh, < PMe,Ph < PEt, for the ligands on platinum. The NMR data (lH, 13C-{lH}, llB-{lH} and "P-('H}) are reported and discussed in relation t o the structures of the products.

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