Crystal Structures of Hydrazinium(II) Salts of [SbF 6 ] – and [Sb 2 F 11 ] –

N 2 H 6 (Sb 2 F 11 ) 2 was synthesized by the reaction of N 2 H 6 F 2 with excess of SbF 5 in anhydrous hydrogen fluoride (aHF). It crystallizes in the triclinic space group P $\bar{1}$ (No. 2) with a = 6.6467(3) Å, b = 8.3039(4) Å, c = 8.3600(5) Å, α = 76.394(5) o , β = 70.161(5) o , γ = 70.797(5) o , V = 405.90(4) Å 3 at 150 K, Z = 2. When it is redissolved in aHF, it solvolysis with the release of SbF 5 yielding N 2 H 6 (SbF 6 ) 2 which crystallizes in the monoclinic C 2/ c space group (No. 15) with a = 7.3805(3) Å, b = 12.3248(5) Å, c = 10.4992(4) Å, β = 92.218(4) o , V = 954.33(7) Å 3 at 150 K, and Z = 8. No other phases were observed in crystallization products when different molar ratios of N 2 H 6 F 2 /SbF 5 (1:1,2:3,1:3) in aHF were used as starting materials.