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Issue 19, 1998
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Synthesis and characterisation of tungsten siloxides including the crystal structure of [WO{O(Ph2SiO)3}2(thf )]

Brian J. Brisdon,  Mary F. Mahon  and  Christopher C. Rainford 

Abstract

Reactions of WOCl4 with NaOSiPh3 and Na2O2SiPh2 gave respectively [WO(Cl)(OSiPh3)3] and [{WO2[(OSiPh2)2O]}2]. Under similar conditions NaOSiPh3 reacted with [WO2Cl2(OSC4H8)2] to yield [WO2(OSiPh3)2(OSC4H8)2]. The novel spirocyclic tungstasiloxane [WO{O(Ph2SiO)3}2(thf )] was prepared from the reaction between equimolar quantities of (Ph2SiO)3 and WOCl4 in tetrahydrofuran. A crystal structure determination on this product revealed a distorted octahedral geometry about the central tungsten atom with the axially co-ordinated ether ligand trans to the oxo group, and puckered eight-membered siloxane rings oriented on opposite sides of the equatorial plane defined by the four co-ordinated siloxide O atoms. The W–O (Si) separations ranged from 1.851(7) to 1.896(8) Å and the W[double bond, length half m-dash]O bond length was 1.675(13) Å. In dichloromethane WCl6 reacted with (Ph2SiO)3 to afford good yields of WOCl4, whereas in tetrahydrofuran the same reactants caused solvent polymerisation.

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Article type: Paper
DOI: 10.1039/A803830I
Citation: J. Chem. Soc., Dalton Trans., 1998,0, 3295-3300
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    Synthesis and characterisation of tungsten siloxides including the crystal structure of [WO{O(Ph2SiO)3}2(thf )]

    B. J. Brisdon, M. F. Mahon and C. C. Rainford, J. Chem. Soc., Dalton Trans., 1998, 0, 3295
    DOI: 10.1039/A803830I

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