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The crystal structure of HSbCl 6  · 4½H 2 O has been determined from three-dimensional X-ray data collected with a diffractometer at 180(± 5) K and refined to  R  = 0.023 (Mo Kα , radiation, 2169 reflexions). The correct space group is  I 112/b with  a  = 12.42(1),  b  = 16.65(1),  c  = 11.93(1) Å and  γ  = 92.44(5)° observed at 180 K. Pairs of asymmetrically coordinated H 5 O 2  +  ions [O – H⋯O 2.413(3) Å] are bridged by water molecules [O – H⋯O 2.682(2), 2.737(3) Å] to give centrosymmetric six-membered rings H 14 O 6  2+ . With the remaining water molecules attached to these rings [O – H⋯O 2.707(2), 2.791(3) Å] infinite chains along [010] are formed. The SbCl 6  −  ions build up a pseudocubic subcell with  Z  = 2. To accommodate the protonated water chain the anions are shifted apart and rotated with regard to one of the ‘cubic’ diagonals, thus explaining the observed reduction of symmetry and a unit cell with  Z  = 8.

Hydrate der Hexachloroantimon(V)säure: Die Kristallstruktur von HSbCl 6 · 4½H 2 O