Trisaquatris(tetraoxorhenate(VII)) gadolinium(III), Gd(ReO4)3(H2O) 3, was prepared by the reaction of Gd2O3 with HReO4 at room temperature. The colorless compound crystallizes in the orthorhombic space group Pna21 (No. 33) with four formula units per unit cell (a = 1470.9 pm , b = 843.6 pm, c = 1146.1 pm ). The main feature of the crystal structure is the formation of a non-centric 3D network. This arrangement shows distorted tricapped trigonal prisms of Gd(H2O)3(ReO4) 6/2 interconected via the ReO4- ligands. The compound is paramagnetic and follows the Curie-Weiss law with a magnetic moment of 7.6 BM. It decomposes above 1170 K with evolution of volatile rhenium oxides and formation of Gd3ReO8