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“Inverse Sodium Hydride”: A Crystalline Salt that Contains H + and Na -

2002; American Chemical Society; Volume: 124; Issue: 21 Linguagem: Inglês

10.1021/ja025655+

1943-2984

Mikhail Y. Redko, Mircea Vlassa, James E. Jackson, A.W. Misiolek, Rui Huang, James L. Dye,

Covalent Organic Framework Applications

A crystalline salt has been synthesized that contains H(+) and Na(-) rather than the usual hydride oxidation states of H(-) and Na(+). The key is irreversible encapsulation of H(+) within the cage of 3(6)adamanzane (Adz). The internal proton is kinetically inert to reduction by Na(-) in solution in NH(3)-MeNH(2) mixtures. Synthesis of the sodide is accomplished by a metathesis reaction between Na and AdzH(+)X(-) in which X(-) is a sacrificial anion such as glycolate, isethionate, or nitrate. Reduction or deprotonation of the sacrificial anion forms insoluble byproducts and AdzH(+)Na(-) in solution. After solvent removal, the sodide is dissolved in dimethyl ether and transferred through a frit into a separate chamber for crystallization. The compound was characterized as the sodide by analysis, NMR spectra, and optical absorption spectroscopy.