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Synthesis and structure of hydroxylammonium fluoroaluminate

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Abstract

Hydroxylammonium fluoroaluminate with the formula (NH3OH)2AlF5 was synthesized by the reaction of solid NH3OHF and an aqueous solution of aluminum in HF, and its structure was determined by single-crystal X-ray diffraction. The structure consists of NH3OH+ cations and centrosymmetrical AlF6 octahedra, which are formed by sharing two opposite corners connected in polymeric (AlF5) 2−n anions. Oxygen and nitrogen atoms of hydroxylammonium cations are donors of hydrogen bonds to terminal fluorine atoms of fluoroaluminate chains. The compound crystallizes monoclinic P2/c, with cell parameters a = 10.8675(3) Å, b = 7.3098(2) Å, c = 7.2071(2) Å, and β = 91.080(2)°. The thermal decomposition of the compound was studied by TG, DSC, and X-ray powder diffraction. By controlled heating of (NH3OH)2AlF5, a new compound with the formula (NH3OH)AlF4 was obtained, and the final product of the decomposition is γ-AlF3.

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Acknowledgments

The authors appreciate the financial support of the Ministry of Higher Education, Science, and Technology of the Republic of Slovenia.

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Correspondence to Matjaž Kristl.

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Kristl, M., Golobič, A., Dojer, B. et al. Synthesis and structure of hydroxylammonium fluoroaluminate. Monatsh Chem 142, 755–762 (2011). https://doi.org/10.1007/s00706-011-0508-4

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