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(NEt 4 ) 2 S 5  was prepared from NEt 4 Cl and Na 2 S 4  in ethanol. Its reaction with boiling acetonitrile yielded tetraethylammonium tetrathiooxalate. (NEt 4 ) 2 [C 2 S4] was also obtained by heating (NEt 4 ) 2 S 5  with tetraethylammonium dithioacetate in ethanol. Benzyltriethylammonium tetrathiooxalate, (NEt 3 Bz) 2 [C 2 S 4 ]· 2 toluene, crystallized after NEt 3 BzCl and Na 2 S 4  were heated in acetonitrile on subsequent addition of toluene. The crystal structure of (NEt 4 ) 2 [C 2 S 4 ] 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 P4 2 /nmc, Z = 2. The [C 2 S 4]2-  ion has point symmetry 4m2 (D 2d ), i.e. the dihedral angle between the two CS 2  groups is 90°. The ethyl groups of the NEt 4  +  ions are disordered in two orientations.

zeitschrift für naturforschung b

Ein neuer Zugang zu Tetrathiooxalaten. Die Kristallstruktur von (NEt4) 2 [C 2 S 4 ] / A Novel Access to Tetrathiooxalates. Crystal Structure of (NEt 4 ) 2 [C 2 S 4 ]