An experiment is described that produces multiple-quantum magicangle spinning (MQMAS) NMR spectrumof 27Al via 1H cross polarization (CP).An application of this new technique to the study of a fullyhydrated AlPO4-11 aluminophosphate is presented. It is shown that a combination ofMQMAS and CPMQMAS provides new insightinto the structure of this sample. While MQMAS alone can be usedto obtain high-resolution spectra and quantitativeinformation on the distribution of Al sites, CPMQMAS allows one toestablish the positions of water moleculeswithin the AlPO4-11 framework.