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A synthesis and puri®cation route has been developed for base-free trialkylgallium compounds which avoids the use of traditional ether solvents. The R 3 Ga compound (R~Et, Pr i ) is synthesised in triethylamine, NEt 3 , which leads to the adducts R 3 Ga(NEt 3 ). The NEt 3 ligand can be readily displaced by the addition of low volatility bidentate, tetradentate or hexadentate tertiary amines to give adducts of the type (R 3 Ga) x L (x~2, 4, 6), from which base-free R 3 Ga compounds are obtained by mild thermal dissociation. The synthesis and characterisation of these adducts are described and crystal structures reported for the adducts between R 3 Ga (R~Et, Pr i ) and the multidentate macrocyclic amines 1

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