The title compounds have been prepared by the reactions of a potassium diselenide solution in DMF with excess selenium in the presence of tetraethyl and tetrapropyl ammonium chloride, respectively. They were characterized by X-ray crystal structure determinations.
(NEt4+)2[Se52-·1 /2 Se6 · Se7]: Space group PĪ, Z = 2, 2514 observed unique reflections, R = 0.085. Lattice dimensions at —40 °C: a = 957.7(4), b = 1384.2(4), c = 1545.3(7) pm, α = 107.32(3)°, β = 97.27(4)°, γ = 105.94(3)°. The compound has an ionic structure of NEt4+ ions and chains of pentaselenide ions, which are associated with Se6 and Se7, ring molecules, forming layers parallel to (110).
(NPr4)2Se11: Space group C2/c, Ζ = 4, 2198 observed unique reflections, R = 0.082. Lattice dimensions at —40 °C: a = 2364.7(5), b = 1206.8(2), c = 1609.6(3) pm, β = 118.74(3)°. The compound consists of cations (N(C3H7)4+ and spirocyclic anions Se112-, in which two Se6 rings having chair conformation are linked by a common Se atom with planar coordination. There are no short contacts between the S112- ions.
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