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Black Cu2Bi2S3(AlCl4)2 and orange Ag2Bi2S3(AlCl4)2 were synthesized by solvent‐free reaction (polycrystalline powders) as well as in Lewis‐acidic ionic liquids (crystals) at temperatures of 200 °C or lower. X‐ray diffraction on single‐crystals of Cu2Bi2S3(AlCl4)2 revealed two centrosymmetric polytypes: a rhombohedral one, space group R$\bar{3}$c [a = 658.02(3) pm, c = 6794.3(3) pm], with six formula...
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