Solvothermal synthesis and selected properties of {[Ni(dien)2]3[V6As8O26]}2+·2 Cl– featuring the small [V6IVAs8IIIO26]4– cluster anion

Maren Rasmussen; Christian Näther; Wolfgang Bensch

doi:10.1515/znb-2023-0074

Published by De Gruyter April 5, 2024

Solvothermal synthesis and selected properties of {[Ni(dien)₂]₃[V₆As₈O₂₆]}²⁺·2 Cl^– featuring the small [V₆^IVAs₈^IIIO₂₆]^4– cluster anion

Maren Rasmussen , Christian Näther and Wolfgang Bensch

From the journal Zeitschrift für Naturforschung B

https://doi.org/10.1515/znb-2023-0074

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Abstract

A new arsenato-polyoxovanadate with the composition {[Ni(dien)₂]₃[V₆As₈O₂₆]}²⁺·2 Cl^– has been crystallized under solvothermal conditions as turquoise block-like crystals. The central structural feature is the [V₆^IVAs₈^IIIO₂₆]^4– cluster anion, which is composed of two trinuclear {V₃O₁₁} groups consisting of three edge-sharing VO₅ polyhedra. Pairs of pyramidal AsO₃ moieties share a common corner forming As₂O₅ units, which interconnect the {V₃O₁₁} groups. One of the [Ni(dien)₂]²⁺ complexes adopts the s-fac (Ni1) and the second complex the mer configuration (Ni2). The Cl⁻ anion is involved in strong hydrogen bonding interactions and links the [Ni(dien)₂]²⁺ complexes to form twelve-membered rings which host the [V₆As₈O₂₆]^4– cluster anions. The Hirshfeld surface analysis yields a detailed picture of the intermolecular interactions revealing clear differences for the two unique [Ni(dien)₂]²⁺ complexes. Intermolecular contacts also include As⋯H, O⋯H and H⋯H interactions. In the electronic spectrum the bands of d–d transitions of the vanadyl group and of the Ni²⁺ cations overlap, preventing a detailed analysis.

Keywords: arsenato-polyoxovanadate; solvothermal synthesis; crystal structure; Hirshfeld surface analysis; spectroscopic properties

Dedicated to Professor Thomas Bredow of the University of Bonn on the occasion of his 60th birthday.

Corresponding author: Wolfgang Bensch, Institute of Inorganic Chemistry, Christian-Albrechts-University of Kiel, Max-Eyth-Straße 2, 24118 Kiel, Germany, E-mail: wbensch@ac.uni-kiel.de

5 Supporting information

Experimental and calculated X-ray powder patterns, further structural drawings, the IR spectrum, a table with selected structural data and refinement results, and tables of interatomic distances and angles are given as supplementary material available online (https://doi.org/10.1515/znb-2023-0074).

Acknowledgments

The authors thank the State of Schleswig-Holstein for financial support.

Research ethics: Not applicable.
Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.
Competing interests: The authors declare no conflict of interest regarding this article.
Research funding: None declared.
Data availability: The raw data can be obtained on request from the corresponding author.

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Supplementary Material

This article contains supplementary material (https://doi.org/10.1515/znb-2023-0074s).

Received: 2023-09-07

Accepted: 2023-10-20

Published Online: 2024-04-05

Published in Print: 2024-04-25