Abstract: | The reactions of the Zintl phase K2Cs2Sn9 with elemental tellurium and selenium in ethylenediamine have been investigated. From the reaction of K2Cs2Sn9 with elemental tellurium [K‐(2,2,2‐crypt)]4Te6Te4 ( 2 ) and [K‐(2,2,2‐crypt)]2Sn2Te3 ( 3 ) were obtained, whereas the reaction of K2Cs2Sn9 with elemental selenium led to the formation of [K‐(2,2,2‐crypt)]2Sn(Se4)3 ( 4 ) and [K‐(2,2,2‐crypt)]2Cs2Sn2Se6·2en ( 5 )1). Compounds 2 , 4 , 5 have been characterized by single crystal X‐ray structure determination. |