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1.
Synthesis, crystal structure and magnetic properties of a new hydroxylammonium fluoroferrate
Brina Dojer, Matjaž Kristl, Zvonko Jagličić, Amalija Golobič, Marta Kasunič, Mihael Drofenik, 2012, original scientific article

Abstract: This paper reports on the synthesis of a new hydroxylammonium fluoroferrate, with the formula $(NH_3OH)_3FeF_6$, obtained after dissolving iron powder in hydrofluoric acid and adding solid $NH_3OHF$. This new compound has been characterized by chemical and thermal analysis, single-crystal X-ray diffraction, and magnetic measurements. The title compound crystallizes trigonal, R3c, with cell parameters a = 11.4154(2) Å, c = 11.5720(2) Å, Z = 6. The structure consists of $NH_3OH^+$ cations and isolated $FeF_6^{3–}$ octahedra in which the central ion lies on a threefold axis. The oxygen and nitrogen atoms of the hydroxylammonium cations are donors of hydrogen bonds to fluoride anions, resulting in a network of hydrogen bonds between counterions. The effective magnetic moment $µ_{eff}$ = 5.8 BM was calculated and perfectly matches the expected value of high-spin Fe(III) ions. The thermal decomposition of the compound was studied by TG, DSC, and X-ray powder diffraction.
Keywords: inorganic chemistry, crystallography, coordination compounds, synthesis, crystal structure, characterization of compounds, determination of the structure of compounds, X-ray diffraction, magnetic measurements, thermal analysis, TG, DSC, hydrogen bond, metal complexes, hydroxylammonium fluoromethalatehydroxylammonium, fluoroferrate
Published in DKUM: 25.08.2017; Views: 1356; Downloads: 56
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2.
Ammoniumbis(hydroxylammonium) pentafluoridooxidovanadate(IV) : synthesis and characterisation of a new fluorovanadate
Brina Dojer, Matjaž Kristl, Zvonko Jagličić, Mihael Drofenik, Anton Meden, 2008, original scientific article

Abstract: Turquoise crystals of a new hydroxylammonium compound with the formula $NH_4(NH_3OH)_2[VOF_5]$ have been synthesized by the reaction of solid $NH_3OHF$ and the aqueous solution of vanadium in HF. The compound crystallizes monoclinic, $P2_1/n$, with cell parameters: a = 10.5658(2) Å, b = 6.6143(1) Å, c = 11.6618(2) Å, β = 96.282(1). Magnetic susceptibility was measured using a SQUID device over a temperature range 2–300 K at magnetic field $10^3 Oe$ giving the result $µ_{eff}$ = 1.65 BM. The thermal decomposition was studied by TG and DSC analysis. $NH_4(NH_3OH)_2[OF_5V]$ decomposes above 354 K in three steps, obtaining $NH_4VOF_3$ after the first step and $V_2O_5$ as the final residue.
Keywords: hydroxylammonium fluorovanadates, x-ray powder diffraction, x-ray structure determination, thermal analysis
Published in DKUM: 17.08.2017; Views: 1099; Downloads: 77
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