Abstract
The storage of metastable compounds and modifications of elements are of great interest for synthesis and other, e.g., semiconductor, applications. Whereas white phosphorus is a metastable modification that can be stored under certain conditions, storage of the extremely (light- and air-)sensitive form of arsenic, yellow arsenic, is a challenge rarely tackled so far. Herein, we report on the facile storage and release of these tetrahedral E4 molecules (E = P, As) using activated carbon as a porous storage material. These loaded materials are air- and light-stable and have been comprehensively characterized by solid-state 31P{1H} MAS NMR spectroscopy, powder X-ray diffraction analysis, nitrogen adsorption measurements, and thermogravimetric analysis. Additionally, we show that these materials can be used as a suitable E4 source for releasing intact white phosphorus or yellow arsenic, enabling subsequent reactions in solution. Because the uptake and release of E4 are reversible, these materials are excellent carriers of these highly reactive modifications.
Highlights
The storage of metastable compounds and modifications of elements are of great interest for synthesis and other, e.g., semiconductor, applications
While activation of the P4 tetrahedron is of great interest in academic research[2,3,4,5], industry is especially interested in the production of organophosphorus compounds and the synthesis of highly pure phosphoric acid starting from white phosphorus
The loaded materials E4@C (E = P, As) can be prepared by adsorbing E4 (E = P, As) from a freshly prepared solution in tetrahydrofuran (THF) by an activated carbon material (C) with a defined pore size distribution resulting in an air- and light-stable black solid of E4@C after work-up (Supplementary Figs. 1 and 2)
Summary
The storage of metastable compounds and modifications of elements are of great interest for synthesis and other, e.g., semiconductor, applications. We report on the facile storage and release of these tetrahedral E4 molecules (E = P, As) using activated carbon as a porous storage material. These loaded materials are air- and light-stable and have been comprehensively characterized by solid-state 31P{1H} MAS NMR spectroscopy, powder X-ray diffraction analysis, nitrogen adsorption measurements, and thermogravimetric analysis. Succeeded in storing P4 and, interestingly, As4 within tetrahedrally shaped cage complexes in solution[7, 8] In all these cases, no subsequent reactions with the host–guest complexes were examined due to the resulting multi-component mixtures of the overall systems (occurrence of side reactions).
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