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Issue 1, 2010
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Trilacunary A-β-Keggin tungstogermanates and -silicates functionalized with phenyltin(iv) electrophiles

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Abstract

The first organic derivative of a β-Keggin tungstogermanate, the monomeric Keggin anion [{(C6H5)Sn(OH)}3(A-β-GeW9O34)]4− (1), was the only species isolated from the reaction of (C6H5)SnCl3 with Na10[A-β-GeW9O34] in water, whereas the Si-analogue [{(C6H5)Sn(OH)}3(A-β-SiW9O34)]4− (2) and two dimeric tungstosilicates, the unprecedented species [{(C6H5)Sn(A-β-H3SiW9Sn2O37)}2O2]8− (3) and the known sandwich-type polyanion [{(C6H5)Sn(OH)}3(A-β-H3SiW9O34)2]8− (4), were isolated starting from [A-β-SiW9O34]10−. The novel polyanion 3 can be described as the product of a double Sn–C hydrolysis followed by condensation of two subunits of 2 through double Sn–O–Sn bridge formation. Solid-state characterization has been carried out by infrared spectroscopy, thermogravimetry and single-crystal X-ray diffraction, representing the first structural analysis for 4. A full solution multinuclear NMR (1H, 13C, 117Sn, and 183W) and solid-state 117Sn CP-MAS NMR study enabled full characterization of 1. A weak 1-dimensional polyanion association through (Sn)O–H⋯Ot hydrogen contacts involving one of the protonated bridging O atoms of the (C6H5)3Sn3O12 corner-shared triad is observed for 1 by X-ray diffraction, resulting in a local Cs pseudosymmetry for the Sn centers detected by solid-state 117Sn NMR spectroscopy.

Graphical abstract: Trilacunary A-β-Keggin tungstogermanates and -silicates functionalized with phenyltin(iv) electrophiles

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Supplementary files

Article information


Submitted
03 Jun 2009
Accepted
12 Oct 2009
First published
11 Nov 2009

Dalton Trans., 2010,39, 248-255
Article type
Paper

Trilacunary A-β-Keggin tungstogermanates and -silicates functionalized with phenyltin(IV) electrophiles

S. Reinoso, L. F. Piedra-Garza, M. H. Dickman, A. Praetorius, M. Biesemans, R. Willem and U. Kortz, Dalton Trans., 2010, 39, 248
DOI: 10.1039/B910889K

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