Scandium halide complexes of phosphine- and arsine-oxides: synthesis, structures and Sc-45 NMR studies
Scandium halide complexes of phosphine- and arsine-oxides: synthesis, structures and Sc-45 NMR studies
The reactions of ScCl(3)(.)6H(2)O, ScBr(3)(.)6H(2)O and Scl(3)(.)8H(2)O with Ph3PO, Ph3AsO, Ph2MePO, Me3PO and Me3AsO have been examined in EtOH or Me2CO solution. The new complexes [ScCl(Me3PO)(5)]Cl-2, [Sc(Me3PO)(6)]X-3 (X = Br or 1), [ScX,(Ph3PO)4]X (X = Cl, Br or 1), [ScX2(Ph3AsO)(4)]X, [Sc(Me3AsO)(6)]X-3 (X = Cl, Br or 1), [ScCl3(Ph2MePO)(3)] and [ScBr2(PhMePO)(4)]Br were isolated as solids and were characterised by analysis, IR and multinuclear (H-1, P-31{H}: and Sc-45) NMR spectroscopy and conductance measurements. The crystal structures of [ScBr2(Ph3PO)(4)]Br(.)1/2Et(2)O, [ScCl2(Ph3AsO)(4)]Cl and [Sc(Me3AsO)(6)]Br-3 are also reported. The solution speciation (in CH2Cl2 or MeNO2) in the various systems was examined by multinuclear NMR spectroscopy. The Sc-45 NMR chemical shifts and line widths show systematic trends with donor set and symmetry. which are described. No reaction between these ligands and ScF3.1/2H(2)O was observed.
scandium, phosphine oxide, arsine oxide, x-ray structures, sc-45 nmr
crown-ether complexation, spectroscopic characterization, yttrium
1579-1588
Hill, N. J.
9aa23b1b-287e-4c75-8d49-a7f313dcd00b
Levason, W.
e7f6d7c7-643c-49f5-8b57-0ebbe1bb52cd
Popham, M. C.
02a55e82-8c1d-4256-ac28-955979aaf0f1
Reid, G.
37d35b11-40ce-48c5-a68e-f6ce04cd4037
Webster, M.
f26c6e36-cb2e-486e-b2ed-b0d25a3a71f7
1 July 2002
Hill, N. J.
9aa23b1b-287e-4c75-8d49-a7f313dcd00b
Levason, W.
e7f6d7c7-643c-49f5-8b57-0ebbe1bb52cd
Popham, M. C.
02a55e82-8c1d-4256-ac28-955979aaf0f1
Reid, G.
37d35b11-40ce-48c5-a68e-f6ce04cd4037
Webster, M.
f26c6e36-cb2e-486e-b2ed-b0d25a3a71f7
Hill, N. J., Levason, W., Popham, M. C., Reid, G. and Webster, M.
(2002)
Scandium halide complexes of phosphine- and arsine-oxides: synthesis, structures and Sc-45 NMR studies.
Polyhedron, 21 (16), .
(doi:10.1016/S0277-5387(02)01016-1).
Abstract
The reactions of ScCl(3)(.)6H(2)O, ScBr(3)(.)6H(2)O and Scl(3)(.)8H(2)O with Ph3PO, Ph3AsO, Ph2MePO, Me3PO and Me3AsO have been examined in EtOH or Me2CO solution. The new complexes [ScCl(Me3PO)(5)]Cl-2, [Sc(Me3PO)(6)]X-3 (X = Br or 1), [ScX,(Ph3PO)4]X (X = Cl, Br or 1), [ScX2(Ph3AsO)(4)]X, [Sc(Me3AsO)(6)]X-3 (X = Cl, Br or 1), [ScCl3(Ph2MePO)(3)] and [ScBr2(PhMePO)(4)]Br were isolated as solids and were characterised by analysis, IR and multinuclear (H-1, P-31{H}: and Sc-45) NMR spectroscopy and conductance measurements. The crystal structures of [ScBr2(Ph3PO)(4)]Br(.)1/2Et(2)O, [ScCl2(Ph3AsO)(4)]Cl and [Sc(Me3AsO)(6)]Br-3 are also reported. The solution speciation (in CH2Cl2 or MeNO2) in the various systems was examined by multinuclear NMR spectroscopy. The Sc-45 NMR chemical shifts and line widths show systematic trends with donor set and symmetry. which are described. No reaction between these ligands and ScF3.1/2H(2)O was observed.
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Published date: 1 July 2002
Keywords:
scandium, phosphine oxide, arsine oxide, x-ray structures, sc-45 nmr
crown-ether complexation, spectroscopic characterization, yttrium
Identifiers
Local EPrints ID: 19774
URI: http://eprints.soton.ac.uk/id/eprint/19774
ISSN: 0277-5387
PURE UUID: 3f577aaf-daa7-4c86-b62c-8891507ad400
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Date deposited: 16 Feb 2006
Last modified: 16 Mar 2024 02:43
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Author:
N. J. Hill
Author:
M. C. Popham
Author:
M. Webster
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