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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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Synthesis and characterisation of hydroxylammonium fluorochromate
Matjaž Kristl, Mihael Drofenik, Ljubo Golič, Amalija Golobič, 2003, original scientific article

Abstract: Reactions in the system $Cr – NH_3OHF – HF – H_2O$ were investigated. Green crystals of a new compound with the formula $(NH_3OH)_3CrF_6$ have been isolated from the water solution and characterized by chemical analysis. The compound crystallizes as triclinic, P-1, with cell parameters: a = 6.5461(2) Å, b = 6.9347(2) Å, c = 9.4072(3) Å, α = 86.772(1)°, β = 83.804(1)°, γ = 70.283(1)°. The effective magnetic moment, $µ_{eff}$ = 3.82 BM, was calculated from magnetic susceptibility measurements in the temperature range 80-290 K. The thermal decomposition of the compound was studied by TG and DSC analysis. $(NH_3OH)_3CrF_6$ decomposes above 125 °C in three steps and the residue has been identified by X-ray powder diffraction as $α – Cr_2O_3$.
Keywords: inorganic chemistry, structural chemistry, crystalline structure, coordination compounds, synthesis, inorganic reactions, thermal decomposition, characterization of compounds, TG, DSC, X-ray diffraction, chromium complexes, hydroxylammonium fluoro chromates, crystals
Published in DKUM: 25.08.2017; Views: 1152; Downloads: 94
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Crystal-structure and Mössbauer studies of Li[sub]1.746]Nd[sub]4.494FeO9[sub]9.493
Mihael Drofenik, Irena Ban, Darko Makovec, Darko Hanžel, Amalija Golobič, Ljubo Golič, 2007, original scientific article

Abstract: The ▫$Li_1.746Nd_4.494FeO_9.493$▫ (LNF) ternary phase, located in the ▫$Li_2O$▫-rich part of the ▫$Li_2O-Nd_2O_3-Fe_2O_3$▫ system, crystallizes with a cubic unit cell of dimension and the space group Im3m. Refinement on F resulted in R=1.9%. The structure is comprised of a network of corners, edges and faces sharing the coordination polyhedra of neodymium. In between this skeleton the regular octahedra of oxygen-coordinated iron and trigonal prisms of lithium are located. The Mössbauer spectra revealed the presence of ▫$Fe^3+$▫, ▫$Fe^4+$▫ and ▫$Fe^5+$▫ ions distributed on two symmetry-independent lattice positions.
Keywords: crystal structure, ternary compounds, single-crystal X-ray diffraction, Mössbauer spectroscopy, iron oxidation state, kristalna struktura, ternarne spojine, rentgenska difrakcija, Mössbauerjeva spektroskopija, rentgenska strukturna analiza
Published in DKUM: 01.06.2012; Views: 1948; Downloads: 40
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