Abstract
The monoclinic α-polymorph of (VIVO)(PO3)2 is obtained reproducibly by reaction of V2O5 and H3PO4 (85%) (Au crucible, 380 °C, 4 d). Its crystal structure was refined from X-ray single-crystal data [C2/c, Z = 4, a = 15.1038(7) Å, b = 4.193(2) Å, c = 9.573(9) Å, β = 126.45(3), R1 = 0.052, wR2 = 0.189 for 976 unique reflections with Fo > 4σ(Fo), 48 variables]. A single-phase powder of the β-polymorph is obtained by the reaction of V2O5, H3PO4 (85%) and oxalic acid, evaporating the mixture, and subsequent annealing (porcelain crucible, 800 °C in air, 2 d). Single crystals of β-(VIVO)(PO3)2 were grown in a sealed silica ampoule with chlorine as mineralizer. The crystal structure of the orthorhombic (pseudo-tetragonal) β-polymorph was refined from X-ray single-crystal data [pseudo-merohedral twin, Fdd2, Z = 8, a = 15.536(2) Å, b = 15.586(2) Å, c = 4.2611(5) Å, R1 = 0.032, wR2 = 0.068 for 1072 unique reflections with Fo > 4σ(Fo), 50 variables]. Earlier reports on a tetragonal polymorph with unusual geometric structure of the [(V≡O)O5] polyhedron are corrected.
Dedicated to Professor Dr. Ulrich Müller on the occasion of his 80th birthday.
Acknowledgments
We thank Dr. Gregor Schnakenburg and Charlotte Rödde for the collection of the single crystal X-ray data and Dominik Offermanns (all University of Bonn) for the XRPD data of α- and β-VO(PO3)2.
Author contribution: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.
Research funding: None declared.
Conflict of interest statement: The authors declare no conflicts of interest regarding this article.
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Supplementary Material
The online version of this article offers supplementary material (https://doi.org/10.1515/zkri-2020-0037).
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