Synergy of diffraction and spectroscopic techniques to unveil the crystal structure of antimonic acid

The elusive crystal structure of the so-called ‘antimonic acid’ has been investigated by means of robust and state-of-the-art techniques. The synergic results of solid-state magic-angle spinning nuclear magnetic resonance spectroscopy and a combined Rietveld refinement from synchrotron X-ray and neu...

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Bibliographic Details
Published in:Scientific reports 2021-09, Vol.11 (1), p.17763-17763, Article 17763
Main Authors: Mayer, S. F., Rodrigues, J. E., Sobrados, I., Gainza, J., Fernández-Díaz, M. T., Marini, C., Asensio, M. C., Alonso, J. A.
Format: Article
Language:English
Subjects:
639/301
639/301/299
Absorption spectroscopy
Calorimetry
Crystal structure
Differential scanning calorimetry
Diffraction
Humanities and Social Sciences
Magnetic resonance spectroscopy
multidisciplinary
NMR
Nuclear magnetic resonance
Physics
Protons
Science
Science (multidisciplinary)
Spectrum analysis
Thermal analysis
Water content
X-ray absorption spectroscopy
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Summary:The elusive crystal structure of the so-called ‘antimonic acid’ has been investigated by means of robust and state-of-the-art techniques. The synergic results of solid-state magic-angle spinning nuclear magnetic resonance spectroscopy and a combined Rietveld refinement from synchrotron X-ray and neutron powder diffraction data reveal that this compound contains two types of protons, in a pyrochlore-type structure of stoichiometric formula (H 3 O) 1.20(7) H 0.77(9) Sb 2 O 6 . Some protons belong to heavily delocalized H 3 O + subunits, while some H + are directly bonded to the oxygen atoms of the covalent framework of the pyrochlore structure, with O–H distances close to 1 Å. A proton diffusion mechanism is proposed relying on percolation pathways determined by bond-valence energy landscape analysis. X-ray absorption spectroscopy results corroborate the structural data around Sb 5+ ions at short-range order. Thermogravimetric analysis and differential scanning calorimetry endorsed the conclusions on the water content within antimonic acid. Additional 0.7 water molecules per formula were assessed as moisture water by thermal analysis.
ISSN:2045-2322
2045-2322
DOI:10.1038/s41598-021-97147-0