Oxorz OX1 1 OQX) c = 9.832 A, /3 = 92.66', 2 = 12, I / o ( I ) 2 3-0, range 3-15', present R-value = 0-23 (Ru only) for 1480 reflections.

Treatment of [Os,(CO),,] with KOH in MeOH gives the anion [Os,H(CO),,]-; low-temperature 13C n.m.r. spectroscopy reveals that the structure of this hydrido-cluster is the same as that established for [Fe,H(CO),,]-in the solid state ; a t higher temperatures, fluxional behaviour similar to that previously observed for [Fe,H(CO),,]occurs. The [Os,H(CO),,]-anion reacts with [ O S ~( C O ) ~~] to produce the Os, anion [(OC),,,HOs,(~-CO,)-0s6(CO),,]-which contains an Os, and Os, unit linked by a CO, group. Carbon-73 n.m.r. spectroscopic studies reveal that the C atom of the C 0 2 linkage arises from the [OS,(CO)~~].

Improved Syntheses of the Hexanuclear Clusters [ Ru6(C0)18]~-, [HRus-Polynuclear Carbonyl containing an Interstitial Hydrogen Ligand (co)l8]-, and H2RUs( co)18. The X -Ray Analysis O f [ H Rug( CO)is]-,t a

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