The crystal structures of [NH3(CH2)5NH3]CdCl4 are determined by X‐ray diffraction at 293 K (phase I) and 353 K (phase II) in order to obtain a structural description of the second‐order phase transition occurring at 337 K. This continuous transition is mainly of order‐disorder type and can be associated to the reorientational dynamics of the alkylenediammonium chains, with all trans conformation between two distinct positions. A model of “twisted” chains, coexisting with the trans ones is proposed in the high temperature phase to account for the observed electron density distribution due to the carbon atoms.
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