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Issue 12, 2011
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Alpha and beta isomers of tetrahafnium(iv) containing decatungstosilicates, [Hf4(OH)6(CH3COO)2(x-SiW10O37)2]12 (x = α, β)

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Abstract

The two dimeric, Hf-containing tungstosilicates [Hf4(OH)6(CH3COO)2(α-SiW10O37)2]12 (1) and [Hf4(OH)6(CH3COO)2(β-SiW10O37)2]12 (2) have been synthesized by reacting HfCl4 with [γ-SiW10O36]8 in potassium acetate solutions at pH = 3.6 and 4.8, respectively. Polyanions 1 and 2 comprise a tetrahafnium(IV) assembly {Hf4(OH)6(CH3COO)2} sandwiched between two dilacunary [α-SiW10O36]8 (in 1) or {β-SiW10} (in 2) Keggin type decatungstosilicates. This implies that the starting precursor {γ-SiW10} isomerizes in situ to [β-SiW10O37]10 and then to [α-SiW10O37]10 by controlled variation of pH and temperature. The hydrated potassium salts of 1 and 2 were investigated in the solid state by single-crystal XRD, FT-IR, thermogravimetric and elemental analyses, and in solution by UV-Vis and 183W NMR spectroscopy, and electrochemistry.

Graphical abstract: Alpha and beta isomers of tetrahafnium(iv) containing decatungstosilicates, [Hf4(OH)6(CH3COO)2(x-SiW10O37)2]12− (x = α, β)

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Supplementary files

Article information


Submitted
06 Nov 2010
Accepted
07 Jan 2011
First published
11 Feb 2011

Dalton Trans., 2011,40, 2920-2925
Article type
Paper

Alpha and beta isomers of tetrahafnium(IV) containing decatungstosilicates, [Hf4(OH)6(CH3COO)2(x-SiW10O37)2]12 (x = α, β)

A. S. Assran, S. S. Mal, N. V. Izarova, A. Banerjee, A. Suchopar, M. Sadakane and U. Kortz, Dalton Trans., 2011, 40, 2920 DOI: 10.1039/C0DT01543A

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