Microcrystalline diffraction techniques employing synchrotron radiation are used to obtain detailed structural information on two zeotype aluminophosphates. For DAF-1 a much improved description of the framework structure, especially relating to the Al-O, P-O bond alternation, has been obtained. A detailed in situ study of the structural changes occurring during the calcination of the template in the material CoAPSO-44 is reported. In situ FTIR spectroscopy yields a correlation between the decomposition of the template and the creation of framework Bronsted acid sites.
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