Citation: ZHENG Xiao-Yuan, LIU Yang, LIU Yi, QIN Liu-Lei, WANG Le, LIU Zun-Qi. Synthesis, Phase Transition and Dielectric Properties of Ferrate Cyanogen(Ⅲ) Hydrogen-Bonding Supramolecular Crystal[J]. Chinese Journal of Inorganic Chemistry, ;2020, 36(3): 406-414. doi: 10.11862/CJIC.2020.049 shu

Synthesis, Phase Transition and Dielectric Properties of Ferrate Cyanogen(Ⅲ) Hydrogen-Bonding Supramolecular Crystal

Chemical Engineering College, Xinjiang Agricultural University, Urumqi 830052, China

Corresponding author: LIU Yang, liuyangxj85@163.com LIU Zun-Qi, zunqi85@163.com
Received Date: 15 July 2019
Revised Date: 15 November 2019

Figures(10)

Synthesis of novel ferric cyanide hydrogen-bonding cage-like supramolecular crystal material (C₃H₅N₂)₃[Fe(CN)₆]·2(18-crown-6)·2H₂O (1) by solvent evaporation in methanol solution with imidazole, 18-crown-6 and ferric cyanide. The structure, thermal energy and electrical properties of the crystal were characterized by variable temperature X-ray diffraction single crystal diffraction, infrared spectroscopy, elemental analysis, thermogravimetric analysis (TG), differential scanning calorimetry (DSC) and dielectric constant test. The space group of the crystal is P2₁/c, which belongs to the monoclinic system at low temperatures. The crystal structure shows that the cyano-iron complex, the water molecule and the imidazolium cation form a three-dimensional cage structure with iron atoms as the apex in the form of hydrogen bonds. This resulted in phase transition at around 250 K and stepped reversible dielectric anomalies in a range of 220~260 K. Temperature variation triggers the cage structure abrupt change, and at the same time causes dynamic oscillation of supramolecules within the framework of[Fe(CN)₆]^3-, thus induces the phase transition of crystal structure. The phase transition temperature interval of the crystal structure was accompanied with step-like change in dielectric physical properties. The dielectric constant was reversible and changed from 38 to 43 with temperature increasing from 220 to 280 K. Above 270 K, the sudden jump in dielectric is caused by water vapor.
- metal-organic framework,
- crystal structure,
- hydrogen bond,
- dielectric properties
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