Abstract: | Caesium aluminium dizirconium tetrakisphosphate(V)], CsAlZr2(PO4)4, has been synthesized by high‐temperature reaction and studied by single‐crystal X‐ray diffraction at room temperature. This represents the first detailed structural analysis of an anhydrous phosphate containing both zirconium and aluminium. The structure features a complicated three‐dimensional framework of AlZr2(PO4)4] constructed by PO4, AlO4 and ZrO6 polyhedra interconnected via corner‐sharing O atoms, and one‐dimensional Cs chains which are located in the infinite tunnels within the AlZr2(PO4)4] framework, which run along the c axis. The Cs, Al, one P and two O atoms lie on a mirror plane, while a second P atom lies on a twofold axis. |