Ein neuer Zugang zu Tetrathiooxalaten. Die Kristallstruktur von (NEt4)2[C2S4] / A Novel Access to Tetrathiooxalates. Crystal Structure of (NEt4)2[C2S4]
(NEt4)2S5 was prepared from NEt4Cl and Na2S4 in ethanol. Its reaction with boiling acetonitrile yielded tetraethylammonium tetrathiooxalate. (NEt4)2[C2S4] was also obtained by heating (NEt4)2S5 with tetraethylammonium dithioacetate in ethanol. Benzyltriethylammonium tetrathiooxalate, (NEt3Bz)2[C2S4]· 2 toluene, crystallized after NEt3BzCl and Na2S4 were heated in acetonitrile on subsequent addition of toluene. The crystal structure of (NEt4)2[C2S4] was determined by X-ray diffraction (454 independent observed reflexions, R = 0.047). Crystal data: tetragonal, a = 871.2(1) pm, c = 1566.0(3) pm, space group P42/nmc, Z = 2. The [C2S4]2- ion has point symmetry 4m2 (D2d), i.e. the dihedral angle between the two CS2 groups is 90°. The ethyl groups of the NEt4+ ions are disordered in two orientations.