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Metal Assisted Synthesis of Cationic Sulfidobismuth Cubanes in Ionic Liquids

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Ruck,  Michael
Michael Ruck, Max Planck Fellow, Max Planck Institute for Chemical Physics of Solids, Max Planck Society;

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Citation

Knies, M., Groh, M. F., Pietsch, T., Lê Anh, M., & Ruck, M. (2021). Metal Assisted Synthesis of Cationic Sulfidobismuth Cubanes in Ionic Liquids. ChemistryOpen, 10(2), 110-116. doi:10.1002/open.202000246.


Cite as: https://hdl.handle.net/21.11116/0000-0007-5D5C-B
Abstract
Bi2S3 was dissolved in the presence of either AuCl/PtCl2 or AgCl in the ionic liquids [BMIm]Cl ⋅ xAlCl3 (BMIm=1-n-butyl-3-methylimidazolium; x=4–4.3) through annealing the mixtures at 180 or 200 °C. Upon cooling to room temperature, orange, air-sensitive crystals of [BMIm](Bi4S4)[AlCl4]5 (1) or Ag(Bi7S8)[S(AlCl3)3]2[AlCl4]2 (2) precipitated, respectively. 1 did not form in the absence of AuCl/PtCl2, suggesting an essential role of the metal cations. X-ray diffraction on single-crystals of 1 revealed a monoclinic crystal structure that contains (Bi4S4)4+ heterocubanes and [AlCl4]− tetrahedra as well as [BMIm]+ cations. The intercalation of the ionic liquid was confirmed via solid state NMR spectroscopy, revealing unusual coupling behavior. The crystal structure of 2 consists of (Bi7S8)5+ spiro-dicubanes, [S(AlCl3)3]2− tetrahedra triples, isolated [AlCl4]− tetrahedra, and heavily disordered silver(I) cations. No cation ordering took place in 2 upon slow cooling to 100 K. © 2020 The Authors. Published by Wiley-VCH GmbH