DecacurbonyZ-l-(~-cyelo~exa-1,3-diene)-triangulo-triosnziunz, [Os,(CO) ,,(C,H,>] (1) .-The compound [Os3(CO),,H,] (500 mg) was added to distilled refluxing n-hexane containing an excess of cyclohexa-1,3-diene or -1,4-diene under nitrogen. After 4 h, the solvent and excess diene were removed in vacuo and the 4 residue was chromatographed on silica plates using hexanediethyl ether (19 : 1) as eluant. The required compound was removed from the plates as an intense orange band and was recrystallized from hexane at -25 "C, yield 60% (Found: C, 20.7; H, 0.9. C,,H,0,,0s3 requires C, 20.5; H I 0.85%). diertyZ)-triangulo-triosnziunzTetrufluoroborate, [Os,(CO),,-(C,H,)] [BFa], (2) .-Compound (1) (30 mg) dissolved in dry dichloromethane (5 cm3) was added to [CPh,][BF,] (100 mg)

Edge-bridging hydrides in [RHOs,(CO),,] ( R = H or vinyl) have been located by an integrated X-rayneutron diffraction study, which also finds precise positions for the other light atoms.

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