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An iron(III) calix[4]pyrrolidine complex undergoes a slow phase transformation at ca 173 K from monoclinic space group P21/n to the maximal non-isomorphic subgroup, triclinic space group P\overline{1}, which is accompanied by nonmerohedral twinning. The NH H atoms are directed below the planes of the macrocycles and are hydrogen bonded to the coordinated Cl ions. There are also intra­molecular C—H...Cl hydrogen bonds present in both forms.
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