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According to the crystal structure determination by Edstrand & Blomqvist [Ark. Kemi (1955), 8, 245–256], intercalate NH4Cl·As2O3·0.5H2O () is not isostructural with compound KCl·As2O3·0.5H2O. This is very unlikely because both NH4Br·2As2O3 and KBr·2As2O3 as well as NH4I·2As2O3 and KI·2As2O3 are isostructural. Hence, intercalate has been studied using single‐crystal X‐ray diffraction in addition...