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Syntheses, structures and multinuclear NMR (Sc-45, Y-89, P-31) studies of Ph3PO, Ph2MePO and Me3PO complexes of scandium and yttrium nitrates

Record type: Article

The reactions of the tertiary phosphine oxides Ph3PO, Ph2MePO or Me3PO with hydrated yttrium(III) nitrate in ethanol gave the complexes [Y(R3PO)(2)(EtOH)(NO3)(3)] (R3PO=Ph3PO or Ph2MePO), [Y(Me3PO)(2)(H2O)(NO3)(3)], [Y(R3PO)(3)(NO3)(3)] (R3PO=Ph3PO, Ph2MePO or Me3PO), and [Y(Ph3PO)(4)(NO3)(2)]NO3. The species [Y(R3PO)(4)(NO3)(2)]NO3 (R3PO=Ph2MePO or Me3PO) were formed from [Y(R3PO)(3)(NO3)(3)] and an excess of R3PO in CH2Cl2 solution and identified spectroscopically, but have not been isolated as solids. Corresponding reactions of hydrated scandium(III) nitrate produced [Sc(Ph3PO)(2)(NO3)(3)], [Sc(Ph2MePO)(3)(NO3)(3)], [Sc(Ph2MePO)(4)(NO3)(2)]NO3, [Sc(Me3PO)(2)(EtOH)(NO3)(3)], and [Sc(Me3PO)(6)][NO3](3). All complexes were characterised by elemental analysis, IR and H-1 NMR spectroscopy and conductance measurements. Variable temperature Y-89, Sc-45 and P-31-{H-1} NMR spectroscopies have been used to identify species present in solution, and probe the interconversions. P-31-{H-1} NMR studies show that exchange with added R3PO in solution is slow on the NMR timescale. Crystal structures were determined for [Y(Ph3PO)(2)(EtOH)(NO3)(3)] and [Y(R3PO)(3)(NO3)(3)] (R3PO=Ph3PO, Ph2MePO or Me3PO): all contain 9-co-ordinate Y with symmetrically co-ordinated bidentate nitrate groups. Structures of the 8-co-ordinate [Sc(Ph3PO)(2)(NO3)(3)] and [Sc(Ph2MePO)(4)(NO3)(2)]NO3 are also described.

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Citation

Deakin, L., Levason, W., Popham, M. C., Reid, G. and Webster, M. (2000) Syntheses, structures and multinuclear NMR (Sc-45, Y-89, P-31) studies of Ph3PO, Ph2MePO and Me3PO complexes of scandium and yttrium nitrates Journal of the Chemical Society Dalton Transactions, (14), pp. 2439-2447. (doi:10.1039/b001669l).

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Published date: 2000

Identifiers

Local EPrints ID: 18892
URI: http://eprints.soton.ac.uk/id/eprint/18892
ISSN: 1472-7773
PURE UUID: d335eb46-3f9a-48cb-82c6-6a53197eb80a

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Date deposited: 20 Dec 2005
Last modified: 17 Jul 2017 16:34

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Contributors

Author: L. Deakin
Author: W. Levason
Author: M. C. Popham
Author: G. Reid
Author: M. Webster

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