ABSTRACTThe use of A2 Q/Q melts (A - alkali metal, Q - S or Se) for the synthesis of new one-dimensional solid-state materials is found to be of general utility and is illustrated here for the synthesis of K4 Ti3 SI4. Reaction of Ti metal with a K2 S/S melt at 375°C for 50 h affords K4 Ti3 SI4. The structure possesses one-dimensional chains of seven and eightcoordinate Ti atoms with each chain isolated from all others by surrounding K atoms. There are six S-S pairs (dave - 2.069(3) Å) so that the compound is one of TiIV and may be described as K4 [Ti3 (S)2 (S2)6]. Electrical conductivity measurements indicate that this material is a semiconductor.