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Issue 9, 2014
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Synthesis, properties and structures of NbOF3 complexes and comparisons with NbOCl3 analogues

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Abstract

The first series of complexes of niobium(V) oxide trifluoride, [NbOF3(OPR3)2] (R = Me or Ph), [NbOF3(dppmO2)] (dppmO2 = Ph2P(O)CH2P(O)Ph2), [NbOF3(dmso)2], [NbOF3(tmeda)] (tmeda = Me2N(CH2)2NMe2) and [NbOF3(diimine)] (diimine = 2,2′-bipy, 1,10-phen) have been prepared, either by reaction of the corresponding complexes of NbF5 and hexamethyldisiloxane (HMDSO) in CH2Cl2–MeCN solution, or directly from NbF5, ligand and HMDSO. They were characterised by IR, 1H, 31P{1H} and 19F{1H} NMR spectroscopy, and X-ray crystal structures are reported for [NbOF3(OPR3)2] (R = Me or Ph) and [NbOF3(dppmO2)]. Complexes of NbOCl3, [NbOCl3(OPPh3)2], [NbOCl3(dppmO2)], [NbOCl3(dppeO2)] (dppeO2 = Ph2P(O)(CH2)2P(O)Ph2), [NbOCl3(tmeda)] and [NbOCl3(diimine)] were made from NbCl5 and HMDSO in MeCN (which forms [NbOCl3(MeCN)2] in situ), followed by addition of the neutral ligand. Their properties are compared with the oxide fluoride analogues. X-ray structures are reported for [NbOCl3(dppmO2)], [NbOCl3(dppeO2)], [NbOCl3(tmeda)] and [NbOCl3(2,2′-bipy)]. The synthesis and spectroscopic characterisation of [MF5L] (M = Nb or Ta; L = OPR3, OAsPh3) and [MF4(diimine)2][MF6] are also described, and the key properties of the four series of complexes compared.

Graphical abstract: Synthesis, properties and structures of NbOF3 complexes and comparisons with NbOCl3 analogues

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Publication details

The article was received on 25 Nov 2013, accepted on 23 Dec 2013 and first published on 03 Jan 2014


Article type: Paper
DOI: 10.1039/C3DT53322K
Citation: Dalton Trans., 2014,43, 3649-3659
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    Synthesis, properties and structures of NbOF3 complexes and comparisons with NbOCl3 analogues

    W. Levason, G. Reid, J. Trayer and W. Zhang, Dalton Trans., 2014, 43, 3649
    DOI: 10.1039/C3DT53322K

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