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lb-e) are generated from R e 2 0 t and either ZnX2, (noxides in good yields. These synthetic routes have the advan-C4H9)3SnX, [(n-C,H&N]X, or [ (CAHS)4P]X in clean reactions. tage to proceed under very mild conditions. The adducts of Compounds la-f form with stable six-coordinate adducts 2,2'-bipyridine with halorhenium(VI1) oxides show characte-XRe03.L (2a-f, 3a, 4a, 5a: L = N,N'-ligand) upon addition ristic thermogravimetric (TG) behavior that reflects the volaof the free ligand L, e.g. 2,2'-bipyridine. l a is readily alky-tility of the uncoordinated complexes X-Re03. CI

Molecular Structure of frans-Bis(acetonftrile)tris(tri-ferf-buty~e~oxy)ne~ymiumThe first lanthanide complex 3a is obtained from the sterically Under the same conditions D Y [ N { S~( C H~)~)~]~ (2b) yields the demanding silanol (tC,H9)3SiOH (silox", la) and Nd-homoleptic ditox derivative 6. The new complexes are all very p{Si(CH3)3)d3 (2a). Similarly, the bulky alcohols hitox-H', soluble in aliphatic hydrocarbons. They show a very different tri-tert-butylmethanol (1 b), and "ditox-H", di-tert-butylme-thermal stability as, for example, expressed in their sublimathan01 (lc), react with 2a to give the corresponding alkoxide tion behaviour.

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