Ionothermal Synthesis of Sulfidobismuth spiro-Dicubane Cations

ChemistryOpen. 2022 Feb;11(2):e202100145. doi: 10.1002/open.202100145. Epub 2021 Aug 13.

Abstract

Bi2 S3 was dissolved in the presence of NaCl in the ionic liquid [BMIm]Cl ⋅ 4AlCl3 (BMIm=1-n-butyl-3-methylimidazolium) through annealing the mixture at 180 °C. Upon cooling to room temperature, orange, air-sensitive crystals of Na(Bi7 S8 )[S(AlCl3 )3 ]2 [AlCl4 ]2 (1) precipitated. X-ray diffraction on single-crystals of 1 revealed a triclinic crystal structure that contains (Bi7 S8 )5+ spiro-dicubanes, [S(AlCl3 )3 ]2- tetrahedra triples, isolated [AlCl4 ]- tetrahedra, and sodium cations.

Keywords: bismuth; heterocubanes; ionic liquids; ionothermal synthesis; spirocubanes.