NDLI: Self-assembly of tetrareduced corannulene with mixed Li–Rb clusters: dynamic transformations, unique structures and record <sup>7</sup>Li NMR shifts

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Self-assembly of tetrareduced corannulene with mixed Li–Rb clusters: dynamic transformations, unique structures and record ⁷Li NMR shifts

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Chemical Science Vol - 6 Issue - 2

Chemical Science Vol -5

Chemical Science Vol -4

Chemical Science Vol -3

Chemical Science Vol -2

Chemical Science Vol -1

Self-assembly of tetrareduced corannulene with mixed Li–Rb clusters: dynamic transformations, unique structures and record ⁷Li NMR shifts

Content Provider	Royal Society of Chemistry (RSC)
Author	Rogachev, Andrey Yu. Zabula, Alexander V. Spisak, Sarah N. Petrukhina, Marina A. McNeely, James Filatov, Alexander S.
Copyright Year	2015
Abstract	Self-assembly processes of the highly reduced bowl-shaped corannulene generated by the chemical reduction with a binary combination of alkali metals, namely Li–Rb, have been investigated by variable-temperature 1H and 7Li NMR spectroscopy. The formation of several unique mixed metal sandwich products based on tetrareduced corannulene, C20H104− (14−), has been revealed followed by investigation of their dynamic transformations in solutions. Analysis of NMR data allowed to propose the mechanism of stepwise alkali metal substitution as well as to identify experimental conditions for the isolation of intermediate and final supramolecular products. As a result, two new triple-decker aggregates with a mixed Li–Rb core, [{Rb(THF)2}2]//[Li3Rb2(C20H10)2{Li+(THF)}] (2) and [{Rb(diglyme)}2]//[Li3Rb3(C20H10)2(diglyme)2]·0.5THF (3·0.5THF), have been crystallized and structurally characterized. The Li3Rb2-product has an open coordination site at the sandwich periphery and thus is considered transient on the way to the Li3Rb3-sandwich having the maximized intercalated alkali metal content. Next, the formation of the LiRb5 self-assembly with 14− has been identified by 7Li NMR as the final step in a series of dynamic transformations in this system. This product was also isolated and crystallographically characterized to confirm the LiRb5 core. Notably, all sandwiches have their central cavities, located in between the hub-sites of two C20H104− decks, occupied by an internal Li+ ion which exhibits the record high negative shift (ranging from −21 to −25 ppm) in 7Li NMR spectra. The isolation of three novel aggregates having different Li–Rb core compositions allowed us to look into the origin of the unusual 7Li NMR shifts at the molecular level. The discussion of formation mechanisms, dynamic transformations as well as unique electronic structures of these remarkable mixed alkali metal organometallic self-assemblies is provided and supported by DFT calculations.
Starting Page	1959
Ending Page	1966
Page Count	8
File Format	HTM / HTML PDF
ISSN	20416520
Volume Number	6
Issue Number	3
Journal	Chemical Science
DOI	10.1039/c4sc03485f
Language	English
Publisher	Royal Society of Chemistry
Access Restriction	Subscribed
Subject Keyword	Three-decker (house) Self-assembly Sandwich compound Diglyme Organometallic chemistry Nuclear magnetic resonance spectroscopy Ion Alkali metal Li
Content Type	Text
Resource Type	Article
Subject	Chemistry

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Self-assembly of tetrareduced corannulene with mixed Li–Rb clusters: dynamic transformations, unique structures and record ⁷Li NMR shifts