Monatshefte für Chemie - Chemical Monthly

, Volume 143, Issue 2, pp 175–180 | Cite as

Hydroxylammonium fluorometalate: synthesis and characterisation of a new fluorozincate

  • Brina Dojer
  • Amalija Golobič
  • Zvonko Jagličić
  • Matjaž Kristl
  • Miha Drofenik
Original Paper


A new coordination compound of zinc fluoride and hydroxylammonium, (NH3OH)2ZnF4, was obtained after dissolving zinc powder in hydrofluoric acid (40%) and adding solid hydroxylammonium fluoride. The colourless crystals were characterised chemically, magnetically, structurally by single-crystal X-ray diffraction analysis, and thermogravimetrically by TGA and DSC analysis. The structure consists of NH3OH+ cations and ZnF6 octahedra in which the metal ion lies on the inversion centre. Each of the ZnF6 octahedra shares four of its vertices in a way that each vertex is shared between two octahedra. Oxygen and nitrogen atoms of hydroxylammonium cations are donors of hydrogen bonds. Hydroxylamonium fluorozincate crystallizes monoclinic, P21/c, with cell parameters a = 8.1604(4) Å, b = 5.8406(3) Å, c = 5.6586(2) Å and β = 94.745(3)°. The compound decomposes above 373 K in four steps, obtaining ZnO as the final residue. Magnetic properties of the compound were studied between 2 and 300 K, giving the prevailing diamagnetic behaviour with room temperature susceptibility of −9 × 10−5 emu mol−1.

Graphical Abstract


Hydroxylammonium fluorozincate Crystal structure Hydrogen bonds X-ray structure determination Thermochemistry 



The authors thank the Ministry of Higher Education, Science and Technology of the Republic of Slovenia for their support.


  1. 1.
    Kristl M, Dojer B, Kasunič M, Golobič A, Jagličić Z, Drofenik M (2010) J Fluorine Chem 131:907CrossRefGoogle Scholar
  2. 2.
    Slivnik J, Rahten A, Maček J, Sedej B (1979) Documenta Chemica Yugoslavica 26:19Google Scholar
  3. 3.
    Slivnik J, Maček J, Rahten A, Sedej B (1980) Thermochim Acta 39:21CrossRefGoogle Scholar
  4. 4.
    Milićev S, Maček J (1985) Spectrochim Acta A 41:651CrossRefGoogle Scholar
  5. 5.
    Chaudhuri MK, Ghosh SK, Hiese Z (1984) J Chem Soc Dalton Trans 8:1763Google Scholar
  6. 6.
    Bartolome J, Navarro R, Gonzalez D, de Jongh LJ (1977) Chem Phys Lett 48:536CrossRefGoogle Scholar
  7. 7.
    Bartolome J, Navarro R, Gonzalez D, de Jongh LJ (1977) Physica B C 92:23CrossRefGoogle Scholar
  8. 8.
    Steenbergen C, Degraaf LA, Bevaart L, Bartolome J, de Jongh LJ (1979) J Chem Phys 70:1450CrossRefGoogle Scholar
  9. 9.
    Bartolome J, Palacio F, Calleja JM, Rueda FA, Cardona M, Migoni R (1985) J Phys C Solid State Phys 18:6083CrossRefGoogle Scholar
  10. 10.
    Agullo de Rueda F, Calleja JM, Bartolome J (1988) J Phys C Solid State Phys 21:1287CrossRefGoogle Scholar
  11. 11.
    Plaza I, Rubin J, Laguna MA, Bartolome J (1996) Spectrochim Acta A 52:57CrossRefGoogle Scholar
  12. 12.
    Aleksandrov KS, Bartolome J, Gorev MV, Flerov IN (2000) Phys Status Solidi B 217:785CrossRefGoogle Scholar
  13. 13.
    Kristl M, Golič L, Volavšek B (1994) Monatsh Chem 125:1207CrossRefGoogle Scholar
  14. 14.
    Dojer B, Kristl M, Jagličić Z, Drofenik M, Meden A (2008) Acta Chim Slov 55:834Google Scholar
  15. 15.
    Gilli G, Gilli P (2009) The nature of the hydrogen bond, IUCr monographs on crystallography - 23. Oxford University Press, UK, p 31Google Scholar
  16. 16.
    Kristl M, Volavšek B, Golič L (1996) Monatsh Chem 127:581CrossRefGoogle Scholar
  17. 17.
    Kristl M, Drofenik M, Golič L, Golobič A (2003) Acta Chim Slov 50:431Google Scholar
  18. 18.
    Kristl M, Golobič A, Dojer B, Drofenik M (2011) Monatsh Chem 142:755CrossRefGoogle Scholar
  19. 19.
    Otwinowski Z, Minor W (1997) Methods Enzym 276:307CrossRefGoogle Scholar
  20. 20.
    Kahn O (1993) Molecular magnetism. VCH, Weinheim, p 3Google Scholar
  21. 21.
    Ashcroft NW, Mermin ND (1976) Solid state physics. Saunders College Publishing, USAGoogle Scholar
  22. 22.
    Furman NH (1962) Standard methods of chemical analysis, vol 1, 6th edn. Van Nostrand, Princeton, p 196Google Scholar
  23. 23.
    Altomare A, Burla MC, Camalli M, Cascarano G, Giacovazzo C, Guagliardi A, Moliterni AGG, Polidori G, Spagna R (1999) J Appl Cryst 32:115CrossRefGoogle Scholar
  24. 24.
    Hall SR, Du Boulay DJ, Olthof-Hazekamp R (1999) Xtal 3.6 System. University of Western Australia, LambGoogle Scholar
  25. 25.
    Macrae CF, Edgington PR, McCabe P, Pidcock E, Shields GP, Taylor R, Towler M, van de Streek J (2006) J Appl Cryst 39:453CrossRefGoogle Scholar
  26. 26.
    Dowty E (2005) ATOMS, Version 6.2. Shape Software, KingsportGoogle Scholar

Copyright information

© Springer-Verlag 2011

Authors and Affiliations

  • Brina Dojer
    • 1
  • Amalija Golobič
    • 2
  • Zvonko Jagličić
    • 3
    • 4
  • Matjaž Kristl
    • 1
  • Miha Drofenik
    • 1
    • 5
  1. 1.Faculty of Chemistry and Chemical EngineeringUniversity of MariborMariborSlovenia
  2. 2.Faculty of Chemistry and Chemical TechnologyUniversity of LjubljanaLjubljanaSlovenia
  3. 3.Institute of Mathematics, Physics and MechanicsLjubljanaSlovenia
  4. 4.Faculty of Civil and Geodetic EngineeringLjubljanaSlovenia
  5. 5.Jozef Stefan InstituteLjubljanaSlovenia

Personalised recommendations