氪内嵌富勒烯（Kr@C）的合成与氪核磁共振光谱分析

Synthesis and Kr NMR spectroscopy of Kr@C.

作者信息

Hoffman Gabriela, Bacanu George R, Marsden Elizabeth S, Walkey Mark C, Sabba Mohamed, Bloodworth Sally, Tizzard Graham J, Levitt Malcolm H, Whitby Richard J

机构信息

Chemistry, Faculty of Engineering and Physical Sciences, University of Southampton, Southampton, SO17 1BJ, UK.

出版信息

Chem Commun (Camb). 2022 Oct 6;58(80):11284-11287. doi: 10.1039/d2cc03398d.

DOI:10.1039/d2cc03398d

PMID:36124877

Abstract

Synthesis of Kr@C is achieved by quantitative high-pressure encapsulation of the noble gas into an open-fullerene, and subsequent cage closure. Krypton is the largest noble gas entrapped in C using 'molecular surgery' and Kr@C is prepared with >99.4% incorporation of the endohedral atom, in 4% yield from C. Encapsulation in C causes a shift of the Kr resonance by -39.5 ppm with respect to free Kr in solution. The Kr spin-lattice relaxation time is approximately 36 times longer for Kr encapsulated in C than for free Kr in solution. This is the first characterisation of a stable Kr compound by Kr NMR.

摘要

通过将稀有气体定量高压封装到开放的富勒烯中并随后进行笼闭来实现Kr@C的合成。氪是使用“分子手术”被困在C中的最大稀有气体，制备的Kr@C中内包原子的掺入率>99.4%，相对于C的产率为4%。封装在C中会使Kr共振相对于溶液中的游离Kr发生-39.5 ppm的位移。封装在C中的Kr的自旋晶格弛豫时间比溶液中的游离Kr长约36倍。这是通过Kr NMR对稳定的Kr化合物进行的首次表征。