The quaternary thioaluminogermanates Na(AlS2)(GeS2) (1) and K(AlS2)(GeS2) (2) crystallize in the tetragonal space group I4/mcm (no. 140) with unit cell parameters a = 7.4274(11) Å, c = 5.8560(12) Å for Na(AlS2)(GeS2) and a = 7.8826(2) Å, c = 5.8642(4) Å for K(AlS2)(GeS2). The crystal structure comprises of one‐dimensional [(AlS2)(GeS2)]– anionic chains with Al and Ge sharing the tetrahedral site. The alkali metal cations fill the square antiprismatic voids between chains. Both 1 and 2 are semiconductors with bandgap of around 3.6 eV and 3.5 eV, respectively.

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The title compounds are prepared from stoichiometric mixtures of M2S (M: Na, K) and elemental Al, Ge, and S (fused silica ampules, 850 °C, 4 d).

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