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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Kristl M, Golič L, Volavšek B (1994) Monatsh Chem 125:1207
Kristl M, Volavšek B, Golič L (1996) Monatsh Chem 127:581
Kristl M, Drofenik M, Golič L (2002) Acta Chim Slov 49:243
Kristl M, Drofenik M, Golič L, Golobič A (2003) Acta Chim Slov 50:431
Kristl M, Dojer B, Kasunič M, Golobič A, Jagličić Z, Drofenik M (2010) J Fluorine Chem 131:907
Ban I, Golič L, Milićev S, Volavšek B (1995) Monatsh Chem 126:1279
Ban I, Kristl M, Volavšek B, Golič L (1999) Monatsh Chem 130:401
Pintarič M, Milićev S, Volavšek B (1990) Monatsh Chem 121:357
Bukovec P, Šiftar J (1971) Therm Anal, Proc Int Conf, 3rd 321
Bentrup U, Kolditz L (1988) J Therm Anal 33:827
Menz DH, Bentrupp U (1989) Z Anorg Allg Chem 576:186
Pugh W, Hotz MCB (1953) J Chem Soc 2493. doi:10.1039/JR9530002493
Šiftar J, Bukovec P (1970) Monatsh Chem 101:1184
Bukovec P, Šiftar J (1971) Monatsh Chem 102:94
Milićev S, Rahten A (1991) Eur J Solid State Inorg Chem 28:557
Rahten A, Benkič P, Jesih A (1999) Acta Chim Slov 46:339
Herron N, Thorn DL, Harlow RL, Jones GA, Parise JB, Fernandez-Baca JA, Vogt T (1995) Chem Mater 7:75
Bulou A, Leble A, Hewat AW, Fourquet JL (1982) Mat Res Bull 17:391
Udovenko AA, Laptash NM, Maslennikova IG (2003) J Fluorine Chem 124:5
Parnham ER, Slawin AMZ, Morris RE (2007) J Solid State Chem 180:49
Adil K, Goreshnik E, Courant S, Leblanc M, Maisinneuve V (2004) Solid State Sci 6:1229
Chamayou AC, Neelakantan MA, Thalamuthu S, Janiak C (2011) Inorg Chim Acta 365:447
Zhuge FY, Wu BA, Dong LH, Yang J, Janiak C, Tang N, Yang XJ (2010) Aust J Chem 63:1358
Gil-Hernandez B, Hoppe HA, Vieth JK, Sanchiz J, Janiak C (2010) Chem Commun 46:8270
Habib HA, Gil-Hernandez B, Abu-Shandi K, Sanchiz J, Janiak C (2010) Polyhedron 29:2537
Gilli G, Gilli P (2009) The Nature of the Hydrogen Bond. Oxford University Press, Oxford, p 31
Hydrofluoric acid, MSDS No. 47590, Sigma-Aldrich, Steinheim, Germany; http://www.sigmaaldrich.com, accessed 17 Mar 2011
Furman NH (1962) Standard methods of chemical analysis. Van Nostrand, Princeton, p 196 vol 1, 6th edn
DIFFRACplus (1997) Search/match, Version 3.0
Otwinowski Z, Minor W (1997) Methods Enzym 276:307
Altomare A, Burla MC, Camalli M, Cascarano G, Giacovazzo C, Guagliardi A, Moliterni AGG, Polidori G, Spagna R (1999) J Appl Cryst 32:115
Hall SR, Du Boulay DJ, Olthof–Hazekamp R (1999) Xtal3.6 System. University of Western Australia, Lamb, Perth
Farrugia LJ (1997) J Appl Cryst 30:568
Dowty E (2005) ATOMS, Version 6.2. Shape Software, Kingsport
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The authors appreciate the financial support of the Ministry of Higher Education, Science, and Technology of the Republic of Slovenia.
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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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DOI: https://doi.org/10.1007/s00706-011-0508-4