Single crystals of a new cyclohexaphosphate, are synthesised and investigated by X-ray diffraction. This compound crystallizes in the triclinic system with the space group P-1 and cell parameters a = 7.773(4), b = 9.238(3), c = 18.532 (7) Å, α = 88.57(3), β = 88.10(4), γ = 67.35(4) • , Z = 1 and V = 1227(1) Å 3 . The three-dimensional network is built up from parallel (0 0 1) layers of [CdP 6 O 18 (H 2 O) 6 ] 4− between which the organic molecules are inserted. The Cd atoms, in 1(a) sites, adopt an octahedral coordination. The 3,4-xylidinium cations exercise an electrostatic interaction on the inorganic anion and establish strong H-bonds with their oxygen atoms.