Hydrothermal synthesis of chabazite-like AlPO4 in a fluoride medium, using piperidine as the structure directing agent, is also successful in the preparation of transition-metal-modified AlPO products. The transition metal (Co, Mn, and Ni) has no influence on the triclinic deformation of the chabazite framework, formed by an interaction of fluoride ions with the AlPO framework. Upon calcination, successive destruction of piperidine and fluoride bridges occurs. The calcined chabazite-like products exhibit a particular sensitivity for humidity resulting in a new triclinic deformation of the chabazite framework The deformation is completely reversible and can be removed by dehydration. The transition-metal incorporation exerts an influence on the dehydration process.