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Issue 37, 2012
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The synthesis of W–O–W μ-oxo clusters by hydrolysis of tungsten aminoalkoxides and their structural characterisation

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Abstract

The tungsten aminoalkoxides W(O)(OPri)3L [L = dmae, OCH2CH2NMe2 (1); bdmap, OCH(CH2NMe2)2 (2); tdmap, OC(CH2NMe2)3 (3)] have been synthesised. Controlled hydrolysis of 1–3 has allowed isolation of W4O4(μ-O)6(dmae)4 (4), W4O4(μ-O)4(OPri)4(bdmap)4 (5), W6O6(μ-O)9(tdmap)6 (6), W4O4(μ-O)6(tdmap)4 (7), W4O4(μ-O)6(tdmap)4·4H2O (7a), all of which have been characterised by X-ray crystallography. 4, 7, 7a each embody a W4O6 core with adamantane structure, 5 incorporates a folded W4O4 square and 6 has a trigonal prismatic W6O9 at its heart. 7 decomposes in air at to give orthorhombic WO3, while 1–3 decomposed under an autogenerated pressure (Reaction under Autogenic Pressure at Elevated Temperatures, RAPET) to form mixtures of carbon-coated WOx needles and carbon spherules.

Graphical abstract: The synthesis of W–O–W μ-oxo clusters by hydrolysis of tungsten aminoalkoxides and their structural characterisation

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Publication details

The article was received on 03 May 2012, accepted on 16 Jul 2012 and first published on 16 Jul 2012


Article type: Paper
DOI: 10.1039/C2DT30966A
Citation: Dalton Trans., 2012,41, 11393-11401
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    The synthesis of W–O–W μ-oxo clusters by hydrolysis of tungsten aminoalkoxides and their structural characterisation

    H. Choujaa, A. L. Johnson, G. Kociok-Köhn and K. C. Molloy, Dalton Trans., 2012, 41, 11393
    DOI: 10.1039/C2DT30966A

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