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Reaction of [PflC^CCF^dppm)], dppm = Ph2PCH2PPh2, with CO in aqueous methanol gives the cluster complex [Pt3(/u3-CO) (ju-dppm)3] [CF3C02] 2 (1) which may be converted to the [PFe]" salt 2. The complexes 1 and 2 are the first complexes reported to contain the Pt3U3-CO) group and are significant as models for CO chemisorbed at a threefold site on a Pt surface. Complexes 1 and 2 were characterized by elemental analysis, IR, and , 31P, and 196Pt NMR and by X-ray crystallography (for 2, as the acetone solvate). Crystals of 2-C3H60 are triclinic, space group PI, with Z = 2, a = 14.090 (2) A, b = 22.711 (4) A, c = 13.637 (4) A, a = 103.43°, ß = 99.52 (2)°, and y = 106.72 (1)°. The structure was solved by the heavy-atom method and refined by full-matrix least-squares calculations with anisotropic thermal parameters for the non-phenyl and non-solvate atoms. At convergence, R = 0.035 for 6234 reflections with I > 3 ( ). The crystal structure contains discrete cations, anions, and acetone solvate molecules. The Pt atoms of the cation form a triangle with Pt-Pt = 2.613-2.650 (1) A. The carbonyl ligand occupies a triply bridging site with Pt-C = 2.080-2.095 (9) A. The atoms of the Pt3P6 moiety are only approximately coplanar; the Pt-P distances are in the range 2.262-2.304 (2) A. The three Pt2P2C five-membered rings adopt envelope conformations with the CH2 moiety at the flap.

Reaction of Pd(OAc), with Ph2PCH2PPh2 under CO in a solvent containing excess of CF3C02H yields the first example of a dicationic cluster of palladium, [Pd3(p3-CO) (p-Ph2PCH2PPh2) J 2 +, the structure of which has been established by X-ray crystallography.

7) Giickel, G.; Schweitzer, D.; Collman, J. P.; Bencosme, S.; Evitt, E.; (8) Darwent, J. R.; Douglas, P.; Harriman, A,; Porter, G.; Richoux, M.-C. (9) Burgner, R. P.; Ponte Goncalves, A. M.

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