Abstract
The preparation of [AlW12O40]5– and of [AlMo6O21]3– has been monitored by 27Al n.m.r. spectroscopy. It is possible to distinguish between aluminium in octahedral and tetrahedral environments. The preparation of [AlW12O40]5– gives rise to four species containing aluminium of which one is the desired product, one is probably a protonated form of it, and one may be the 2 : 18 (Al : W) anion.

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