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On heating the hydrated complexes 18-Crown[6]·M[H2PO4]·xH2O (x= 2 for M = K, Rb; x= 1.5 for M = Cs), quantitatively prepared by mechanical mixing of crystalline 18-Crown[6] and M[H2PO4], to ca. 60 °C, water loss takes place, accompanied by the extrusion of the crown ether from the crystalline complex and followed by reconstruction of the inorganic phase M[H2PO4](M = K, Rb, Cs); the resulting solid mixture reverts to 18-Crown[6]·M[H2PO4]·xH2O (x= 2 for M = K, Rb; x= 1.5 for M = Cs) upon grinding in air. [ABSTRACT FROM AUTHOR]