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A systematic approach to the formation of endohedrally filled atom clusters by a high‐temperature route instead of the more frequent multistep syntheses in solution is presented. Zintl phases Na12Ni1−xSn17 and K13−xCo1−xSn17, containing endohedrally filled intermetalloid clusters [Ni@Sn9]4− or [Co@Sn9]5− beside [Sn4]4−, are obtained from high‐temperature reactions. The arrangement of [Ni@Sn9]4− or...
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