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Attempts to prepare the compound [Ni(H2O)2(15‐crown‐5)](X)2 were eventually successful with X = NO provided that a synthetic route aimed at restricting water was followed. Application of this method was extended to make the analogous compound with X = HSO, for which three symmetry‐related phases were isolated between 295 and 110 K: a room‐temperature phase with Z′ = ½ [phase (I)], an intermediate‐temperature...
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