Isolated zirconium centres captured from aqueous solution: the structure of zirconium mandelate revealed from NMR crystallography

Zirconium tetramandelate (2-hydroxy-2-phenylacetate) has been used for selective gravimetric analysis of zirconium for over 70 years. Herein its crystal structure is reported from synchrotron powder X-ray diffraction and 13 C solid-state NMR. The complex is a rare example of isolated zirconium catio...

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Bibliographic Details
Published in:Chemical communications (Cambridge, England) England), 2020-09, Vol.56 (7), p.1159-1162
Main Authors: Crosland, James M, Corlett, Emily K, Scapens, Dave, Guillou, Nathalie, Brown, Steven P, Walton, Richard I
Format: Article
Language:English
Subjects:
Aqueous solutions
Chemical Sciences
Crystal structure
Crystallography
Crystals
Gravimetric analysis
NMR
Nuclear magnetic resonance
Physics
Synchrotrons
X ray powder diffraction
Zirconium
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Summary:Zirconium tetramandelate (2-hydroxy-2-phenylacetate) has been used for selective gravimetric analysis of zirconium for over 70 years. Herein its crystal structure is reported from synchrotron powder X-ray diffraction and 13 C solid-state NMR. The complex is a rare example of isolated zirconium cations, rather than the clusters prevalent in aqueous solutions. Zirconium tetramandelate forms from aqueous solution and unusually contains isolated cations; its structure is determined ab initio from a polycrystalline sample using a combined synchrotron X-ray powder diffraction and solid-state NMR approach.
ISSN:1359-7345
1364-548X
DOI:10.1039/d0cc03647a