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The reaction of selenium and NbCl5 with arsenic in the Lewis‐acidic ionic liquid BMImCl·4.8AlCl3 at 100 °C yielded dark‐red block‐shaped crystals of Nb2Se4(AlCl4)4, which immediately decompose when exposed to humid air. Arsenic takes the part of the reducing agent for niobium as well as selenium. The crystal structure was described in the monoclinic space group P21/n (no. 14) with a = 898.0(1) pm,...
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