Issue 41, 2012
From the journal:

Dalton Transactions

Convenient synthesis of fluoride-alkoxides of Nb(v) and Ta(v): a spectroscopic, crystallographic and computational study†

Marco Bortoluzzi,a   Nicola Guazzelli,b   Fabio Marchetti,*b   Guido Pampalonib  and  Stefano Zacchinic  

* Corresponding authors

a University of Venezia, Dipartimento di Scienze Molecolari e Nanosistemi, Dorsoduro 2137, I-30123 Venezia, Italy

b University of Pisa, Dipartimento di Chimica e Chimica Industriale, Via Risorgimento 35, I-56126 Pisa, Italy
E-mail: fabmar@dcci.unipi.it
Fax: +39 050 2219246
Tel: +39 050 2219245

c University of Bologna, Dipartimento di Chimica Fisica e Inorganica, Viale Risorgimento 4, I-40136 Bologna, Italy

Abstract

The synthesis and the spectroscopic characterization of fluoride-alkoxides of niobium and tantalum in the highest oxidation state are reported. Suspensions of MF5 (M = Nb, Ta) in a chlorinated solvent reacted with up to three equivalents of ROSiMe3 (R = Me, Et, Ph) to afford polynuclear derivatives and variable amounts of FSiMe3. Thus MF4(OR) (R = Et, Ph) and MF3(OR)2 were obtained by selective 1 : 1 and 1 : 2 reactions almost exclusively as single isomeric products; otherwise mixtures of MF4(OMe) species were afforded from the equimolar reactions of MF5 with MeOSiMe3. The 1 : 3 reaction of TaF5 with MeOSiMe3 led to different forms of TaF2(OMe)3. The synthesis of TaF(OPh)4 was forced by high temperature conditions or the use of a large excess of PhOSiMe3. DFT studies were carried out in order to predict, in the distinct cases, the most stable structures of the metal products. The molecular structures of [NbF2(OPh)2(μ-F)]3 and [TaF(OPh)3(μ-OPh)]2 were ascertained by X-ray diffraction.

Graphical abstract: Convenient synthesis of fluoride-alkoxides of Nb(v) and Ta(v): a spectroscopic, crystallographic and computational study

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Article information

DOI
https://doi.org/10.1039/C2DT31453C
Article type
Paper
Submitted
11 Apr 2012
Accepted
28 Aug 2012
First published
18 Sep 2012

Dalton Trans., 2012,41, 12898-12906

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Convenient synthesis of fluoride-alkoxides of Nb(V) and Ta(V): a spectroscopic, crystallographic and computational study

M. Bortoluzzi, N. Guazzelli, F. Marchetti, G. Pampaloni and S. Zacchini, Dalton Trans., 2012, 41, 12898 DOI: 10.1039/C2DT31453C

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