Synthesis and Kr NMR spectroscopy of Kr@C

Synthesis of Kr@C 60 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 60 using 'molecular surgery' and Kr@C 60 is prepared with >99.4% incorporation of the endohe...

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Published inChemical communications (Cambridge, England) Vol. 58; no. 8; pp. 11284 - 11287
Main Authors Hoffman, Gabriela, Bacanu, George R, Marsden, Elizabeth S, Walkey, Mark C, Sabba, Mohamed, Bloodworth, Sally, Tizzard, Graham J, Levitt, Malcolm H, Whitby, Richard J
Format Journal Article
Published 06.10.2022
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Summary:Synthesis of Kr@C 60 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 60 using 'molecular surgery' and Kr@C 60 is prepared with >99.4% incorporation of the endohedral atom, in ca. 4% yield from C 60 . Encapsulation in C 60 causes a shift of the 83 Kr resonance by −39.5 ppm with respect to free 83 Kr in solution. The 83 Kr spin-lattice relaxation time T 1 is approximately 36 times longer for Kr encapsulated in C 60 than for free Kr in solution. This is the first characterisation of a stable Kr compound by 83 Kr NMR. Synthesis of Kr@C 60 is achieved by a synthetic route that involves quantitative encapsulation of krypton by an open-cage derivative of C 60 . Fine structure is observed in the 13 C NMR spectrum, and 83 Kr NMR characterisation is carried out.
Bibliography:Electronic supplementary information (ESI) available. CCDC
For ESI and crystallographic data in CIF or other electronic format see DOI
2141931
https://doi.org/10.1039/d2cc03398d
ISSN:1359-7345
1364-548X
DOI:10.1039/d2cc03398d