Ca-3(P5O14)(2) was prepared by the solid-state reaction of CaBPO5 and (NH4)(2)HPO4 as small single crystals. The cell dimensions were calculated in the monoclinic system using its powder diffraction pattern and were found to be a=8.695(5), b=8.999(6), c=12.940(1) Angstrom, beta=91.89(5)degrees, and the space group is probably P2(1)/m (No. 11) or P2(1) (No. 4) with Z=4. The compound was characterized by SEM, IR spectroscopy, and EDX analysis of the single crystals. (C) 1997 Academic Press.