利用有机含氮杂环小分子吡咯烷与氯化锌、盐酸反应,制备得到1例新颖的金属有机相变化合物——四氯合锌酸二吡咯烷.通过差热扫描量热(DSC)测试,在升温(339.5 K)和降温(320.5 K)过程中出现可逆的热力学相变峰和较大的的热滞(19 K),表明该化合物发生了可逆的一级相变.对其变温介电常数进行分析,室温下低介电态到高温下高介电态的转变进一步证实了化合物发生结构相变.通过变温X射线单晶衍射,研究了晶体在150和353 K晶体结构,揭示了其相变机理,表明锌离子的相对位移是该化合物相变的主要原因.
A new metal-organic hybrid compound(1) with stuctural phase transition above room temprature has been synthesized. Differential scanning calorimetry(DSC) measurement shows a pair of reversible thermodynamics peaks at 320.5 K(cooling) and 339.5 K(heating) with a large heat hysteresis about 19 K, indicating the compound undergoes a reversible structural phase transition. Dielectric measurement with a step-like dielectric anomaly further confirms the phase transition. The crystal structures of 1, determined at 150 K and 353 K, are both monoclinic in P21/c, suggesting the phase transition is isosymmetric. Temperature-dependent single crystal analyses of 1 reveal that the displacement of zinc atom is mainly responsible for the reversible structural phase transition.