The Smallest Polyoxotungstate Retained by TRIS-Stabilization

A polycondensation reaction of the orthotungstate anion WO4 2–, buffered at pH 7.5 in a TRIS-HCl (0.15 M) solution, results in the first example of a discrete polyoxotungstate anion, with just two W ions stabilized with TRIS ligands. It was isolated and characterized as Na2[WVI 2O6(C4O3NH10)2]·6H2O...

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Bibliographic Details
Published in:Inorganic chemistry 2021-09, Vol.60 (17), p.12671-12675
Main Authors: Gumerova, Nadiia I, Prado-Roller, Alexander, Rambaran, Mark A, Ohlin, C. André, Rompel, Annette
Format: Article
Language:English
Subjects:
Communication
Inorganic Chemistry
oorganisk kemi
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Summary:A polycondensation reaction of the orthotungstate anion WO4 2–, buffered at pH 7.5 in a TRIS-HCl (0.15 M) solution, results in the first example of a discrete polyoxotungstate anion, with just two W ions stabilized with TRIS ligands. It was isolated and characterized as Na2[WVI 2O6(C4O3NH10)2]·6H2O by single-crystal and powder X-ray diffraction, FT-IR spectroscopy, thermogravimetrical analysis (TGA), and elemental analysis in solid state and by electro-spray ionization mass spectrometry (ESI-MS), 13C, and 183W NMR, as well as Raman spectroscopy in solution. This synthesis demonstrates the crucial and new role of the added tris-alkoxy ligand in the development of a new hybrid TRIS-isopolytungstate with the lowest known nuclearity (so far) and the terminal oxygens substituted with two nitrogen atoms arising from amines of the TRIS ligands.
ISSN:0020-1669
1520-510X
1520-510X
DOI:10.1021/acs.inorgchem.1c01188