Polymorphism of In 5 S 5 Cl – X‐ray and HRTEM‐Investigations

• Published in: Zeitschrift für anorganische und allgemeine Chemie (1950) Vol. 636; no. 1; pp. 79 - 84
• Main Authors: Nickel, Vera, Deiseroth, Hans‐Jörg, Kienle, Lorenz, Duppel, Viola, Reiner, Christof
• Format: Journal Article
• Language: English
• Published: 01.01.2010
• ISSN: 0044-2313; 1521-3749
• DOI: 10.1002/zaac.200900414

Abstract In 5 S 5 Cl belongs to the group of mixed valence indium compounds with indium occurring simultaneously in three oxidation states (In 5 S 5 Cl = In + (In 2 ) 4+ 2In 3+ 5S 2– Cl – ). It was shown in an earlier work that In 5 S 5 Cl obtained from InCl 3 , indium and sulfur at 550 °C, crystallises in a monoclinic structure type in contrast to the orthorhombic bromide, In 5 S 5 Br. The main difference of both structure types is an ordered mutual exchange of In + and (In 2 ) 4+ in specific crystallographic positions. This exchange is possible due to the almost identical coordination pattern of both ions. A closer inspection of the real structure of monoclinic In 5 S 5 Cl by High Resolution Transmission Microscopy (HRTEM) already showed the presence of small orthorhombic domains in the real structure of this compound. Now we also obtained macroscopic quantities of orthorhombic In 5 S 5 Cl by the reaction of InCl 3 , indium and sulfur at reaction temperatures below 500 °C ( Pmn 2 1 , a = 3.907(1) Å, b = 9.021(2) Å, c = 14.866(3) Å, Z = 2). The new polymorph is analysed by X‐ray single crystal and X‐ray powder diffraction and HRTEM investigations.