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A novel layered zincophosphate (ZnPO-MPA) was prepared by hydrothermal crystallization using 3-methylaminopropylamine (MPA) as a structure-directing agent. The structure consists of macroanion [Zn₂P₃O ₈(OH)₃]^2- layers which are built up of 4-membered ring channels. The channels (of about 3.7 A diameter) arise through the connection of the neighbouring rings by two oxygen bridges. The negative charge of the layers is compensated by diprotonated MPA molecules which are stacked parallel to the ring channels. ZnPO-MPA is stable up to 300°C. At higher temperatures MPA decomposition begins followed by a dehydration, which occurs through condensation of the framework hydroxyl groups. The activation energy of the MPA decomposition is high due to the fact that the layers and MPA cations are held together by strong hydrogen bonds.