Single crystals of GdClSO4 are obtained from the reaction of Gd-2(SO4)(3) a
nd GdCl3 in silica ampoules. In the monoclinic compound (P2(1)/c, Z = 4, a
= 943.7(1), 657.59(8), 680.05(9) pm, beta = 104.87(2)degrees, R-all = 0.035
2) Gd3+ is surrounded by five sulfate groups and three chloride ligands. On
e of the sulfate groups acts as a bidentate ligand so that the coordination
number of Gd3+ is nine. The reaction of Gd-2(SO4)(3) with LiF in sealed go
ld ampoules yields colorless transparent single crystals of GdFSO4. The com
pound crystallizes orthorhombic (Pnma, Z = 4, a = 843.6(1), b = 701.76(8),
c = 643.38(7) pm, R-all = 0.0207) and contains eight-coordinate Gd3+ ions.
The ligands are six oxygen atoms of five sulfate groups and two fluoride io
ns.