A new layered aluminum phosphate with P:Al ratio 4:3 has been prepared under nonaqueous conditions in the presence of 1,5-diaminopentane and the structure has been determined by single-crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P2(1)/c (Z = 4), with lattice parameters a = 9.801(2), b = 14.837(2), c = 17.815(3) angstrom, beta = 105.65(1)degrees, and V = 2494.7 angstrom3 (R = 0.042 and R(w) = 0.058). The structure consists of AlO4 and PO4 tetrahedra linked to form layers. Two organic cations, diprotonated 1,5-diaminopentane and protonated piperidine derived from cyclization of the starting amine, lie between the inorganic layers and are hydrogen bonded to the layers through NH3+ and NH2+ groups, respectively. The two organic cations are located in two crystallographically distinct eight-membered windows within the layers, the piperidinium cations being associated with circular cavities approximately 6.9 angstrom in diameter, and the 1,5-diaminopentane cations with elliptical cavities (of axes approximately 5.9 and 8.0 angstrom). (C) 1994 Academic Press, Inc.