Аннотация:Samarium hydrogen iodate Sm(IO3)3HIO3 was successfully synthesized by the unconven-tional low-temperature solution-melt method, its structure was determined by X-ray dif-fraction analysis of single crystals. This compound crystallizes in the monoclinic space group P21/c with lattice parameters: a = 10.4637(6) Å, b = 7.4629(5) Å, c = 14.0174(13) Å, β = 110.53(0), Z = 6. In the studied structure, samarium atoms are surrounded by 8 ox-ygen atoms in a polyhedron in the form of a distorted square antiprism. The iodate groups are linked through common oxygen atoms of the SmO8 antiprism into a three-dimensional framework. The compound was characterized by X-ray diffraction, IR and NQR spectros-copy and EDX analysis.