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

Abstract 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-ra...

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Autores principales: S. F. Mayer, J. E. Rodrigues, I. Sobrados, J. Gainza, M. T. Fernández-Díaz, C. Marini, M. C. Asensio, J. A. Alonso
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Publicado: Nature Portfolio 2021
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Acceso en línea:https://doaj.org/article/ad2eafc632cf43178e0d0d61ee42b701
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spelling oai:doaj.org-article:ad2eafc632cf43178e0d0d61ee42b7012021-12-02T19:13:48ZSynergy of diffraction and spectroscopic techniques to unveil the crystal structure of antimonic acid10.1038/s41598-021-97147-02045-2322https://doaj.org/article/ad2eafc632cf43178e0d0d61ee42b7012021-09-01T00:00:00Zhttps://doi.org/10.1038/s41598-021-97147-0https://doaj.org/toc/2045-2322Abstract 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 (H3O)1.20(7)H0.77(9)Sb2O6. Some protons belong to heavily delocalized H3O+ 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 Sb5+ 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.S. F. MayerJ. E. RodriguesI. SobradosJ. GainzaM. T. Fernández-DíazC. MariniM. C. AsensioJ. A. AlonsoNature PortfolioarticleMedicineRScienceQENScientific Reports, Vol 11, Iss 1, Pp 1-13 (2021)
institution DOAJ
collection DOAJ
language EN
topic Medicine
R
Science
Q
spellingShingle Medicine
R
Science
Q
S. F. Mayer
J. E. Rodrigues
I. Sobrados
J. Gainza
M. T. Fernández-Díaz
C. Marini
M. C. Asensio
J. A. Alonso
Synergy of diffraction and spectroscopic techniques to unveil the crystal structure of antimonic acid
description Abstract 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 (H3O)1.20(7)H0.77(9)Sb2O6. Some protons belong to heavily delocalized H3O+ 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 Sb5+ 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.
format article
author S. F. Mayer
J. E. Rodrigues
I. Sobrados
J. Gainza
M. T. Fernández-Díaz
C. Marini
M. C. Asensio
J. A. Alonso
author_facet S. F. Mayer
J. E. Rodrigues
I. Sobrados
J. Gainza
M. T. Fernández-Díaz
C. Marini
M. C. Asensio
J. A. Alonso
author_sort S. F. Mayer
title Synergy of diffraction and spectroscopic techniques to unveil the crystal structure of antimonic acid
title_short Synergy of diffraction and spectroscopic techniques to unveil the crystal structure of antimonic acid
title_full Synergy of diffraction and spectroscopic techniques to unveil the crystal structure of antimonic acid
title_fullStr Synergy of diffraction and spectroscopic techniques to unveil the crystal structure of antimonic acid
title_full_unstemmed Synergy of diffraction and spectroscopic techniques to unveil the crystal structure of antimonic acid
title_sort synergy of diffraction and spectroscopic techniques to unveil the crystal structure of antimonic acid
publisher Nature Portfolio
publishDate 2021
url https://doaj.org/article/ad2eafc632cf43178e0d0d61ee42b701
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