Abstract

Yellow–orange single crystals of CuSbF 6, were prepared by reacting Cu wire (∼10 mmol) with SbF 5 (∼3 mmol) in liquid anhydrous hydrogen fluoride (aHF) and by reduction of Cu(SbF 6) 2 with Cu metal in aHF. CuSbF 6 crystallizes rhombohedral at 296 K with the LiSbF 6 structure type, with a = 530.4(4) pm, c = 1453(1) pm and Z = 3, space group R 3 ¯ (no. 148). The structure is dominated by isolated layers of regular [SbF 6] − octahedra and Cu + cations. An attempt to prepare CuF by reaction between CuSbF 6 and CsF in aHF at ∼190 K failed. Instead of CuF, a mixture of Cu and CuF 2 was obtained.

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