Low-temperature synthetic pathways can result in crystallization of metastable materials. These methods have been widely explored for the preparation of metal oxides. Adaptation of nonhydrolytic sol-gel chemistry to non-oxide systems offers an elegant route to transition-metal sulfides. The method can be exploited for the facile and reproducible synthesis of iron sulfide crystallizing in the troilite structure. This phase is only found in meteorites: and planets and has previously been obtained by high-temperature or high-energy ball-milling methods. "Nonhydrolytic" sol-gel processing results in direct crystallization of troilite with no need for further calcination.