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.

A single crystal X-ray diffraction study on [Os,(CO) 161 reveals a trigonal bipyramidal (D3J metal unit which is slightly distorted towards a capped butterfly arrangement (C,,). THE pink-red pentanuclear cluster [Os,(CO) 161 was first discovered by us as a product of the pyrolysis of [Os,(CO),,] in small amounts (ca. 7%) using extensive t.1.c.l The molecular formula [0s5(c0),,], like those of [os,(c0)1,] and 7 Reprints not available.[OS,(CO),,],~~~ was primarily deduced on the basis of mass spectrometry. We report here an X-ray structure determination of [Os,(CO),,] which supports our initial view that the carbonyl groups are iE an unusual arrangement around a distorted trigonal bipyramid of metal atoms.Crystal data: C,,O,,Os,, M 1399.2, trigonal, space group P3,21, a = b = 9-204(2), G = 24-818(4) A, 2 = 3, D, = 3.83 g ~m -~. Data were collected on an automated Stoe two-circle diffractometer using graphite monochromated

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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