Layered transition metal dichalcogenides have been extensively studied in recent years but very few data are available for transition metal trichalcogenides. This is due to the difficulty in growing large size, good quality single crystals of transition metal trichalcogenides. The chemical bonding processes in transition metal trichalcogenides are of great interest because of opposing nature to those in the dichalcogenides. They may involve either single chalcogen atom or legands. In this book, author described in details about chemical vapour transport technique for growing large size layered single crystals, structural, electrical as well as optical properties of zirconium sulphoselenide single crystals. Author also nicely presented variation of all above mentioned properties with variation sulphur content. This book is useful for researcher who works with crystal growth and its characterizations.