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Synthesis and structural characterization of a 3-D lithium based metal-organic framework showing dynamic structural behavior

机译：具有动态结构行为的3-D锂基金属-有机骨架的合成和结构表征

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摘要

A 3-D lithium based metal organic framework Li_2(C _7H_3NO_4)(C_3H_7NO) [Li _2(2,5-PDC)(DMF), 1; ULMOF-5, UL= ultralight, PDC = pyridinedicarboxylate, space group Pbcn, a = 15.800(3) ?, b = 8.5958(17) ?, c = 18.460(4) ?, V = 2507.1(9) ?~3] was synthesized using the solvothermal method and characterized by single crystal and powder X-ray diffraction techniques. Compound 1 contains tetrameric edge and corner sharing lithium polyhedral clusters connected by organic linkers, forming channels along the [001] direction, with coordinated DMF molecules pointing toward each other in these channels. Thermogravimetric analysis shows compound 1 is stable up to 280 °C under N_2 atmosphere followed by removal of the coordinated DMF molecules, as evident from the associated weight loss. BET (25.06 m~2/g) surface area measurement showed loss of porosity after solvent removal because of a structure change. Solid-state ~6Li NMR on the desolvated compound showed the absence of tricoordinated lithium centers, indicating rearrangement of bonds around the lithium center after DMF removal. The desolvated form reverts to the original form upon exposure to DMF, showing dynamic structural behavior.
机译：3-D锂基金属有机骨架Li_2（C _7H_3NO_4）（C_3H_7NO）[Li _2（2,5-PDC）（DMF），1; ULMOF-5，UL =超轻，PDC =吡啶二甲酸吡啶酯，空间基团Pbcn，a = 15.800（3），b = 8.5958（17），c = 18.460（4），V = 2507.1（9）〜3]用溶剂热法合成了，通过单晶和粉末X射线衍射技术表征。化合物1包含通过有机连接基连接的四聚体边和角共享的锂多面体簇，沿着[001]方向形成通道，配位的DMF分子在这些通道中彼此指向。热重分析表明，化合物1在N_2气氛下，在高达280°C的温度下稳定，随后除去配位的DMF分子，这从相关的重量损失中可以明显看出。 BET（25.06 m〜2 / g）表面积测量显示，由于结构变化，去除溶剂后孔隙度损失。在去溶剂化的化合物上的固态〜6Li NMR显示不存在三配位的锂中心，表明在去除DMF后锂中心周围的键重排。暴露于DMF后，去溶剂化形式恢复为原始形式，显示出动态的结构行为。

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