Аннотация:New cesium cerium (IV) iodate Cs2Ce(IO3)6 was successfully prepared by hydrothermal technique from starting reagents CsF, CeO2,H5IO6 and HIO3 at 230°C. Cs2Ce(IO3)6 were analyzed by single crystal and powder XRD, EDX, IR spectroscopy and thermal analysis. New compound crystallizes in the monoclinic space group C2/c with a = 14.0652 (3) Å, b = 8.1890 (2) Å, c = 17.7211 (4) Å, β = 103.601 (2)o, V = 1983.99(8) Å3, Z = 4. Crystal structure of Cs2Ce(IO3)6 consists from CeO8 square antiprisms which sharing their apexes and edges with trigonal pyramidal IO3— groups to form layers [Ce(IO3)6]2— parallel to ab plane. These layers are furher stabilised by 12-vertex polyhedra, CsO12, situated in their voids. The IR spectrum of Cs2Ce(IO3)6 possess iodate groups bands. According to DTA analysis cesium cerium (IV) iodate shows high thermal stability on air up to 414°C.