| Summary: | [NH<sub>3</sub>(CH<sub>2</sub>)<sub>5</sub>NH<sub>3</sub>]MnCl<sub>4</sub> crystals are grown via slow evaporation, and the crystal undergoes a phase transition at 298 K (T<sub>C</sub>) according to differential scanning calorimetry, and the structures determined via X-ray diffraction at 173 and 333 K are orthorhombic systems in the space group Imma. These results differed slightly from those previously reported, and the reasons for this are analyzed. The thermal stability is relatively high, with a thermal decomposition temperature of approximately 570 K. The <sup>1</sup>H spin-lattice relaxation times t<sub>1ρ</sub> exhibited very large variations, as indicated by the large thermal displacement around the <sup>1</sup>H atoms, suggesting energy transfer at ~T<sub>C</sub>, even if no structural changes occurred. The influences of the chemical shifts of <sup>1</sup>H of NH<sub>3</sub> and short t<sub>1ρ</sub> of C1 adjacent to NH<sub>3</sub> in cation are insignificant, indicating a minor change in the N−H⋯Cl hydrogen bond related to the coordination geometry of the MnCl<sub>6</sub> octahedron. These properties will be make it a potential application for eco-friendly solar cells.
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