Abstract
Iron(II)oxalate dihydrate FeC2O4 × 2 H2O—humboldtine is not only an important synthetic intermediate, but also a key building block for the preparation of various advanced materials. Interestingly, FeC2O4 × 2 H2O can be transformed readily into phase-pure siderite FeCO3. The importance of siderite for earth sciences, in particular for the understanding of the deep carbon cycle of our planet, is paramount. The availability of high-quality single crystals of FeC2O4 × 2 H2O is crucial for diffraction or spectroscopic studies at high pressure. The present article describes a versatile synthetic approach to single crystals of FeC2O4 × 2 H2O and its deuterated analogue starting from metallic iron together with a complete characterization of the products obtained. The same protocol has been employed successfully for the preparation of 57FeC2O4 × 2 H2O, as required for Möβbauer spectroscopy. In addition, the pressure-dependence of the crystal and molecular structure of the title compound was investigated up to p ≥ 20 GPa.
Highlights
Iron(II)oxalate dihydrate FeC2 O4 × 2 H2 O—humboldtine is an important synthetic intermediate, and a key building block for the preparation of various advanced materials
FeC2 O4 × 2 H2 O has emerged as an important building block for the preparation of new, functional advanced materials
The pressure dependence of the crystal and molecular structure of the title compound is reported for applied hydrostatic pressures up to p ≥ 20 GPa
Summary
Iron(II)oxalate dihydrate FeC2 O4 × 2 H2 O is the ferrous salt of ethandicarboxylic acid (oxalic acid). FeC2 O4 × 2 H2 O has emerged as an important building block for the preparation of new, functional advanced materials In this context, high, thermally activated proton conductivity of synthetic humboldtine has been reported [8]. While an impressive body of information is available on the thermal, spectroscopic, magnetic, and structural properties of iron(II)oxalate dihydrate at ambient conditions, little if anything is known about the pressure-dependence of the molecular and crystal structure [3,4,5,6,7,8,9,10,11,12,13,14,15,16,17,18,19]. The pressure dependence of the crystal and molecular structure of the title compound is reported for applied hydrostatic pressures up to p ≥ 20 GPa
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