Single crystals of Sr-2(VO)V2O8 have been prepared by quenching melts from higher temperatures. This compound represents a new structure type and crystallizes with monoclinic symmetry, space group C-2h(6)-I2/a = 6.929, b = 16.246, c = 7.260 Angstrom, beta = 115.82 degrees, Z = 4. The point positions occupied by V5+ show tetrahedral coordination. The refinement of the V4+ position led to split positions with acentric orientations of V4+ in the octahedral O2- surrounding. It results in a square pyramidal coordination with one short V-O distance typically for vanadyl groups.
