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Synthesis and complexation of the mixed tellurium-oxygen macrocycles 1-tellura-4,7-dioxacyclononane, 9 aneO(2)Te, and 1,10-ditellura-4,7,13,16-tetraoxacyclooctadecane, 18 aneO(4)Te(2) and their selenium analogues

Record type: Article

1,10-Ditellura-4,7,13,16-tetraoxacyclooctadecane ([18] aneO(4)Te(2)) has been synthesised in good yield (50 - 55%) from Na2Te and ClCH2CH2OCH2CH2OCH2CH2Cl in liquid ammonia, and fully characterised by NMR spectroscopy (H-1, C-13{H-1} and Te-125{H-1}) and mass spectrometry, and by the preparation of the Te(IV) derivatives [18] aneO(4)Te(2)Me(2)I(2) and [18] aneO(4)Te(2)Cl(4). A minor by-product (ca. 4%) of the preparation is 1-tellura-4,7-dioxacyclononane ([9] aneO(2)Te) which has been isolated and similarly characterised. The corresponding reaction of Na2Se with ClCH2CH2OCH2CH2OCH2CH2Cl in liquid ammonia is less satisfactory and gives variable yields of 1,10-diselena-4,7,13,16-tetraoxacyclooctadecane ([18] aneO(4)Se(2)), which is better obtained from the same reagents in ethanol solution under high dilution conditions. [18] aneO(4)Se(2) has also been thoroughly characterised spectroscopically. In these reactions the nine-membered ring 1-selena-4,7-dioxacyclononane is generally produced only in trace amounts. A range of complexes of [18] aneO(4)Te(2) (L) in which the ligand behaves only as a Te-2 donor has been synthesised, including cis-[MX2L] (M = Pd or Pt, X = Cl or Br), [RhCl2L2] Y (Y = Cl or PF6), [CuL2] BF4, [AgL2] BF4 and [Cu2L][BF4](2). The complexes have been characterised by microanalysis, multinuclear NMR spectroscopy (H-1, Te-125{H-1}, Pt-195, Cu-63), ES+ mass spectrometry, UV/visible and IR spectroscopy as appropriate. Two complexes of [9] aneO(2)Te, cis-[MCl2{[9] aneO(2)Te}(2)] (M = Pd or Pt) are also reported, together with the selenoether complex [PtCl2{[18] aneO(4)Se(2)}]. The X-ray structures of [MCl2{[18] aneO(4)Te(2)}] (M = Pt or Pd) and [ PtCl2{[18] aneO(4)Se(2)}] all reveal cis square planar coordination with no interaction between the metal and the ether oxygens.

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Citation

Hesford, M.J., Levason, W., Matthews, M.L. and Reid, G. (2003) Synthesis and complexation of the mixed tellurium-oxygen macrocycles 1-tellura-4,7-dioxacyclononane, 9 aneO(2)Te, and 1,10-ditellura-4,7,13,16-tetraoxacyclooctadecane, 18 aneO(4)Te(2) and their selenium analogues Dalton Transactions, 2003, (14), pp. 2852-2858. (doi:10.1039/b303365c).

More information

Published date: 2003
Keywords: transition-metal complexes, thiacrown ether 1, 10-dithia-18-crown-6, nuclear-magnetic-resonance, x = cl, ditelluroether complexes, coordination polymers, crystal-structures, palladium, platinum, 4, 7, 13, 16-tetraoxa-1, 10-dithiacyclooctadecane

Identifiers

Local EPrints ID: 19980
URI: http://eprints.soton.ac.uk/id/eprint/19980
ISSN: 1477-9226
PURE UUID: 97b9a210-fcbb-4a0e-ad00-5b058a93d56a
ORCID for W. Levason: ORCID iD orcid.org/0000-0003-3540-0971

Catalogue record

Date deposited: 22 Feb 2006
Last modified: 17 Jul 2017 16:29

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Contributors

Author: M.J. Hesford
Author: W. Levason ORCID iD
Author: M.L. Matthews
Author: G. Reid

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