The synthesis and crystal structure determination of d,l-Co(en)(3) . Ga3P4O16. xH(2)O (Pnna, a = 8.6502(9) b = 21.528(3), c = 13.717(2) Angstrom) is described. This nb:vel layered material contains Ga3P4O163- macroanions. The preparation and preliminary catalytic testing of a vanadium doped aluminophosphate that is isostructural with the gallophosphate is also discussed.