Gd(HSO4)3 is obtained on treatment of Gd2(SO4)3 in conc. H2SO4 in closed vessels at 200 °C. The extremely moisture-sensitive crystals belong to the orthorhombic space group Pbca. Lattice constants are a = 12.080(8), b = 9.574(8), c = 16.513(8)Å and Z = 8. Gadolinium is coordinated by eight oxygen atoms of the hydrogensulfate ligands forming a distorted square antiprism. There are three different HSO4- anions within the structure. One of them is coordinated with two Gd atom s while two HSO4- anions bridge three Gd atoms. The Gd-O bond lengths vary in the range of 2.334(6)-2.423(5)Å .

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