Journal
ORGANOMETALLICS
Volume 31, Issue 15, Pages 5541-5545Publisher
AMER CHEMICAL SOC
DOI: 10.1021/om300507z
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Funding
- National Science Foundation Award [CHE-1212441]
- University at Albany
- Direct For Mathematical & Physical Scien
- Division Of Chemistry [1212441] Funding Source: National Science Foundation
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The reduction of corannulene (C20H10) with excess lithium metal in a strong chelating O-donor solvent, diglyme, leads to the formation of the highly reduced C20H104- anion. However, in contrast to the formation of the sandwich-type supramolecular aggregate [Li-5(C20H104-)(2)](3-) observed in THF, corannulene tetraanions and lithium counterions in diglyme form only contact ion pairs according to Li-7 NMR spectroscopy. Furthermore, the slow dissociation of the premade sandwich [Li-5(C20H104-)(2)](3-) in neat diglyme has been demonstrated by multinuclear NMR spectroscopy. In contrast, the [Li-5(C20H104-)(2)](3-) sandwich can be crystallized from the THF/diglyme mixture as the new crystalline product [Li(THF)(2)(diglyme)(+)[Li-2(THF)-(diglyme)//Li-5(C20H104-)(2)](-), showing a complex ID hybrid architecture according to the single-crystal X-ray diffraction study.
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