Solvothermal synthesis of a new 3-D mixed-metal sulfide framework, (H1.33tren)[In2.67Sb1.33S8]∙tren

Lampkin, J. D., Powell, A. V. and Chippindale, A. M. ORCID: https://orcid.org/0000-0002-5918-8701 (2016) Solvothermal synthesis of a new 3-D mixed-metal sulfide framework, (H1.33tren)[In2.67Sb1.33S8]∙tren. Journal of Solid State Chemistry, 243. pp. 44-49. ISSN 0022-4596 doi: 10.1016/j.jssc.2016.08.007

Abstract/Summary

A new indium(III) antimony(V) sulfide, (H1.33tren)[In2.67Sb1.33S8]∙tren, has been prepared solvothermally at 433 K. The compound crystallises in the tetragonal space group I-42d (lattice parameters, a = 12.6248(5) and c = 19.4387(18) Å at 150 K) and contains adamantane-like T2 supertetrahedral units comprised of corner-sharing InS45- and SbS43- tetrahedra. The adamantane-like units are then linked through sulfur vertices to generate an open, 3-D framework structure containing large pores in which neutral, protonated tren (tris(2-aminoethylene)amine) molecules reside. The presence of the organic components was confirmed by solid-state 13C NMR (10 kHz), combustion and thermogravimetric analysis. The band gap, obtained from UV-vis diffuse reflectance measurements, is 2.7(2) eV. Stirring with either water or alkali-metal salt solution leads to removal of the neutral tren molecules and an ~9 % reduction in unit-cell volume on formation of (H1.33tren)[In2.67Sb1.33S8]∙(H2O)4.