Abstract
Bi2S3 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(Bi7S8)[S(AlCl3)3]2[AlCl4]2 (1) precipitated. X‐ray diffraction on single‐crystals of 1 revealed a triclinic crystal structure that contains (Bi7S8)5+ spiro‐dicubanes, [S(AlCl3)3]2− tetrahedra triples, isolated [AlCl4]− tetrahedra, and sodium cations.
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