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Lanthanide nitrate complexes of diphenylmethylphosphine oxide: synthesis and spectroscopic studies. Crystal structures of La(Ph2MePO)(3)(NO3)(3) , La(Ph2MePO)(4)(NO3)(3).xMe(2)CO and Yb(Ph2MePO)(4)(NO3)(2) PF6

Lanthanide nitrate complexes of diphenylmethylphosphine oxide: synthesis and spectroscopic studies. Crystal structures of La(Ph2MePO)(3)(NO3)(3) , La(Ph2MePO)(4)(NO3)(3).xMe(2)CO and Yb(Ph2MePO)(4)(NO3)(2) PF6
Lanthanide nitrate complexes of diphenylmethylphosphine oxide: synthesis and spectroscopic studies. Crystal structures of La(Ph2MePO)(3)(NO3)(3) , La(Ph2MePO)(4)(NO3)(3).xMe(2)CO and Yb(Ph2MePO)(4)(NO3)(2) PF6
The reaction of Ln(NO3)3·6H2O (Ln=lanthanide except Pm) with Ph2MePO in a 1:3 or 1:4 ratio in acetone or ethanol produces [Ln(Ph2MePO)3(NO3)3] which have been characterised by analysis, IR, 1H and 31P{1H} NMR spectroscopy and conductance measurements. The [Ln?(Ph2MePO)3(NO3)3] (Ln?=Pr–Tb) exist only as tris complexes in solution and are unaffected by the presence of excess Ph2MePO. In contrast the [Ln?(Ph2MePO)3(NO3)3] (Ln?=Ho–Lu) partially decompose in CH2Cl2 solution into [Ln?(Ph2MePO)4(NO3)2]+, and [Ln?(Ph2MePO)4(NO3)2]PF6 are readily isolated from Ln?(NO3)3, Ph2MePO and NH4PF6 in acetone. For lanthanum only, a neutral 1:4 complex [La(Ph2MePO)4(NO3)3] was isolated. X-ray crystal structures show that [La(Ph2MePO)3(NO3)3] contains nine-coordinate La, whilst [La(Ph2MePO)4(NO3)3]·xMe2CO contains a ten-coordinate metal centre. The structure of [Yb(Ph2MePO)4(NO3)2]PF6 reveals an eight-coordinate cation and all complexes contain bidentate nitrato-groups.
lanthanide, phosphine oxide, x-ray structure
0277-5387
2055-2062
Bosson, M.
a3ec99fe-63a0-4407-b3be-9cad9b93a948
Levason, W.
e7f6d7c7-643c-49f5-8b57-0ebbe1bb52cd
Patel, T.
c5c80c13-ba55-4bd0-9c01-f0e5362f9aef
Popham, M. C.
02a55e82-8c1d-4256-ac28-955979aaf0f1
Webster, M.
f26c6e36-cb2e-486e-b2ed-b0d25a3a71f7
Bosson, M.
a3ec99fe-63a0-4407-b3be-9cad9b93a948
Levason, W.
e7f6d7c7-643c-49f5-8b57-0ebbe1bb52cd
Patel, T.
c5c80c13-ba55-4bd0-9c01-f0e5362f9aef
Popham, M. C.
02a55e82-8c1d-4256-ac28-955979aaf0f1
Webster, M.
f26c6e36-cb2e-486e-b2ed-b0d25a3a71f7

Bosson, M., Levason, W., Patel, T., Popham, M. C. and Webster, M. (2001) Lanthanide nitrate complexes of diphenylmethylphosphine oxide: synthesis and spectroscopic studies. Crystal structures of La(Ph2MePO)(3)(NO3)(3) , La(Ph2MePO)(4)(NO3)(3).xMe(2)CO and Yb(Ph2MePO)(4)(NO3)(2) PF6. Polyhedron, 20 (15-16), 2055-2062. (doi:10.1016/S0277-5387(01)00796-3).

Record type: Article

Abstract

The reaction of Ln(NO3)3·6H2O (Ln=lanthanide except Pm) with Ph2MePO in a 1:3 or 1:4 ratio in acetone or ethanol produces [Ln(Ph2MePO)3(NO3)3] which have been characterised by analysis, IR, 1H and 31P{1H} NMR spectroscopy and conductance measurements. The [Ln?(Ph2MePO)3(NO3)3] (Ln?=Pr–Tb) exist only as tris complexes in solution and are unaffected by the presence of excess Ph2MePO. In contrast the [Ln?(Ph2MePO)3(NO3)3] (Ln?=Ho–Lu) partially decompose in CH2Cl2 solution into [Ln?(Ph2MePO)4(NO3)2]+, and [Ln?(Ph2MePO)4(NO3)2]PF6 are readily isolated from Ln?(NO3)3, Ph2MePO and NH4PF6 in acetone. For lanthanum only, a neutral 1:4 complex [La(Ph2MePO)4(NO3)3] was isolated. X-ray crystal structures show that [La(Ph2MePO)3(NO3)3] contains nine-coordinate La, whilst [La(Ph2MePO)4(NO3)3]·xMe2CO contains a ten-coordinate metal centre. The structure of [Yb(Ph2MePO)4(NO3)2]PF6 reveals an eight-coordinate cation and all complexes contain bidentate nitrato-groups.

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Published date: 30 June 2001
Keywords: lanthanide, phosphine oxide, x-ray structure

Identifiers

Local EPrints ID: 19420
URI: http://eprints.soton.ac.uk/id/eprint/19420
ISSN: 0277-5387
PURE UUID: c021b06a-ce9f-418b-bc8e-489e9c6a2ca6
ORCID for W. Levason: ORCID iD orcid.org/0000-0003-3540-0971

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Date deposited: 13 Feb 2006
Last modified: 03 Dec 2019 02:07

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Contributors

Author: M. Bosson
Author: W. Levason ORCID iD
Author: T. Patel
Author: M. C. Popham
Author: M. Webster

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