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

Hamid Choujaa; Andrew L. Johnson; Gabriele Kociok-Köhn; Kieran C. Molloy

doi:10.1039/c2dt30966a

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

Hamid Choujaa, Andrew L. Johnson, Gabriele Kociok-Köhn, Kieran C. Molloy

Research output: Contribution to journal › Article › peer-review

7 Citations (SciVal)

Abstract

The tungsten aminoalkoxides W(O)(OPrⁱ)₃L [L = dmae, OCH₂CH₂NMe₂ (1); bdmap, OCH(CH ₂NMe₂)₂ (2); tdmap, OC(CH₂NMe ₂)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), W ₆O₆(μ-O)₉(tdmap)₆ (6), W ₄O₄(μ-O)₆(tdmap)₄ (7), W ₄O₄(μ-O)₆(tdmap)₄·4H ₂O (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 WO_x needles and carbon spherules.

Original language	English
Pages (from-to)	11393-11401
Number of pages	9
Journal	Dalton Transactions
Volume	41
Issue number	37
Early online date	16 Jul 2012
DOIs	https://doi.org/10.1039/c2dt30966a
Publication status	Published - 1 Dec 2012

ASJC Scopus subject areas

Inorganic Chemistry

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title = "The synthesis of W-O-W μ-oxo clusters by hydrolysis of tungsten aminoalkoxides and their structural characterisation",

abstract = "The tungsten aminoalkoxides W(O)(OPri)3L [L = dmae, OCH2CH2NMe2 (1); bdmap, OCH(CH 2NMe2)2 (2); tdmap, OC(CH2NMe 2)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), W 6O6(μ-O)9(tdmap)6 (6), W 4O4(μ-O)6(tdmap)4 (7), W 4O4(μ-O)6(tdmap)4·4H 2O (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.",

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AU - Molloy, Kieran C.

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N2 - The tungsten aminoalkoxides W(O)(OPri)3L [L = dmae, OCH2CH2NMe2 (1); bdmap, OCH(CH 2NMe2)2 (2); tdmap, OC(CH2NMe 2)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), W 6O6(μ-O)9(tdmap)6 (6), W 4O4(μ-O)6(tdmap)4 (7), W 4O4(μ-O)6(tdmap)4·4H 2O (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.

AB - The tungsten aminoalkoxides W(O)(OPri)3L [L = dmae, OCH2CH2NMe2 (1); bdmap, OCH(CH 2NMe2)2 (2); tdmap, OC(CH2NMe 2)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), W 6O6(μ-O)9(tdmap)6 (6), W 4O4(μ-O)6(tdmap)4 (7), W 4O4(μ-O)6(tdmap)4·4H 2O (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.

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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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