By the reaction of AuI with alkali metal hydrogen acetylides MIC2H (MI = Li–Cs) in liquid ammonia and subsequent heating of the remaining residue in refluxing pyridine (MI = Li, Na, K) or as a solid phase at about 110 °C in vacuum (MI = Rb, Cs) ternary alkali metal gold acetylides MIAuC2 were obtained. Their crystal structures were investigated by the means of X‐ray powder diffraction. $^1_\infty$[Au(C2)2/2–] chains are the characteristic structural motif which are packed in a hexagonal (LiAgC2) and tetragonal arrangement (NaAuC2–CsAuC2), respectively. Simple calculations based on the close packing of rods and spheres can explain these different arrangements. The existence of C–C triple bonds in the title compounds is confirmed by Raman spectroscopic investigations.

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