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Hydroxylammonium fluorometalate: synthesis and characterisation of a new fluorozincate

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Abstract

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.

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Acknowledgments

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

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Authors and Affiliations

  1. Faculty of Chemistry and Chemical Engineering, University of Maribor, Smetanova 17, 2000, Maribor, Slovenia

    Brina Dojer, Matjaž Kristl & Miha Drofenik

  2. Faculty of Chemistry and Chemical Technology, University of Ljubljana, Aškerčeva 5, 1000, Ljubljana, Slovenia

    Amalija Golobič

  3. Institute of Mathematics, Physics and Mechanics, Jadranska 19, 1000, Ljubljana, Slovenia

    Zvonko Jagličić

  4. Faculty of Civil and Geodetic Engineering, Jamova 2, 1000, Ljubljana, Slovenia

    Zvonko Jagličić

  5. Jozef Stefan Institute, Jamova 39, 1000, Ljubljana, Slovenia

    Miha Drofenik

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  1. Brina Dojer
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  2. Amalija Golobič
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  3. Zvonko Jagličić
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  4. Matjaž Kristl
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  5. Miha Drofenik
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Correspondence to Brina Dojer.

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Dojer, B., Golobič, A., Jagličić, Z. et al. Hydroxylammonium fluorometalate: synthesis and characterisation of a new fluorozincate. Monatsh Chem 143, 175–180 (2012). https://doi.org/10.1007/s00706-011-0667-3

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  • DOI: https://doi.org/10.1007/s00706-011-0667-3

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