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Chalcogenoether complexes of tantalum(V) sulfide trichloride – synthesis, properties and structures

Chalcogenoether complexes of tantalum(V) sulfide trichloride – synthesis, properties and structures
Chalcogenoether complexes of tantalum(V) sulfide trichloride – synthesis, properties and structures
The complexes [TaSCl3(L-L)] (L-L = MeSCH2CH2SMe, iPrSCH2CH2SiPr, PhSCH2CH2SPh, nBuSCH2CH2CH2SnBu, MeSCH2CH2CH2SMe, MeSeCH2CH2SeMe, nBuSeCH2CH2CH2SenBu) have been synthesised and isolated in good yield as powdered solids by the reaction of TaCl5 with the appropriate chalcogenoether in a 1:1 molar ratio in anhydrous CH2Cl2 solution at room temperature, followed by the addition of a CH2Cl2 solution containing one mol. equiv. of S(SiMe3)2. The isolated complexes were characterised by IR, 1H and 77Se{1H} NMR spectroscopy, as appropriate, and elemental analysis. Single crystal X-ray structure analyses for [TaSCl3(MeSCH2CH2SMe)], [TaSCl3(MeSeCH2CH2SeMe)], [TaSCl3(iPrSCH2CH2SiPr)] and [TaSCl3(nBuSCH2CH2CH2SnBu)] have been obtained. The data are compared with the previously described Nb(V) analogues. In contrast to the corresponding [NbSCl3(EnBu2)] (E = S, Se), attempts to isolate [TaSCl3(EnBu2)] were unsuccessful. Low pressure chemical vapour deposition (LPCVD) experiments using [TaSCl3(nBuSCH2CH2CH2SnBu)] did not lead to any deposition, whilst similar experiments using [TaSCl3(nBuSeCH2CH2CH2SenBu)] produced films containing only elemental Se, with no evidence for any deposition of tantalum sulfide or selenide films.
tantalum sulfide trichloride, thioether, selenoether, crystal structure
0277-5387
129-134
Bannister, Robert D.
4dd3eb2a-5ba7-46de-9277-8dd7e8e39b74
Levason, William
e7f6d7c7-643c-49f5-8b57-0ebbe1bb52cd
Reid, Gillian
37d35b11-40ce-48c5-a68e-f6ce04cd4037
Robinson, Fred
8fc7b408-097f-4550-b189-5b6e3a49bf93
Bannister, Robert D.
4dd3eb2a-5ba7-46de-9277-8dd7e8e39b74
Levason, William
e7f6d7c7-643c-49f5-8b57-0ebbe1bb52cd
Reid, Gillian
37d35b11-40ce-48c5-a68e-f6ce04cd4037
Robinson, Fred
8fc7b408-097f-4550-b189-5b6e3a49bf93

Bannister, Robert D., Levason, William, Reid, Gillian and Robinson, Fred (2019) Chalcogenoether complexes of tantalum(V) sulfide trichloride – synthesis, properties and structures. Polyhedron, 169, 129-134. (doi:10.1016/j.poly.2019.04.055).

Record type: Article

Abstract

The complexes [TaSCl3(L-L)] (L-L = MeSCH2CH2SMe, iPrSCH2CH2SiPr, PhSCH2CH2SPh, nBuSCH2CH2CH2SnBu, MeSCH2CH2CH2SMe, MeSeCH2CH2SeMe, nBuSeCH2CH2CH2SenBu) have been synthesised and isolated in good yield as powdered solids by the reaction of TaCl5 with the appropriate chalcogenoether in a 1:1 molar ratio in anhydrous CH2Cl2 solution at room temperature, followed by the addition of a CH2Cl2 solution containing one mol. equiv. of S(SiMe3)2. The isolated complexes were characterised by IR, 1H and 77Se{1H} NMR spectroscopy, as appropriate, and elemental analysis. Single crystal X-ray structure analyses for [TaSCl3(MeSCH2CH2SMe)], [TaSCl3(MeSeCH2CH2SeMe)], [TaSCl3(iPrSCH2CH2SiPr)] and [TaSCl3(nBuSCH2CH2CH2SnBu)] have been obtained. The data are compared with the previously described Nb(V) analogues. In contrast to the corresponding [NbSCl3(EnBu2)] (E = S, Se), attempts to isolate [TaSCl3(EnBu2)] were unsuccessful. Low pressure chemical vapour deposition (LPCVD) experiments using [TaSCl3(nBuSCH2CH2CH2SnBu)] did not lead to any deposition, whilst similar experiments using [TaSCl3(nBuSeCH2CH2CH2SenBu)] produced films containing only elemental Se, with no evidence for any deposition of tantalum sulfide or selenide films.

Text
TaSCl3S ms final 28_03_2019 revised 26_4_19 no highlight - Accepted Manuscript
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Accepted/In Press date: 27 April 2019
e-pub ahead of print date: 9 May 2019
Published date: 1 September 2019
Keywords: tantalum sulfide trichloride, thioether, selenoether, crystal structure

Identifiers

Local EPrints ID: 431401
URI: http://eprints.soton.ac.uk/id/eprint/431401
ISSN: 0277-5387
PURE UUID: 71175c14-0c88-454c-904c-7f1e9720e30e
ORCID for William Levason: ORCID iD orcid.org/0000-0003-3540-0971
ORCID for Gillian Reid: ORCID iD orcid.org/0000-0001-5349-3468

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Date deposited: 31 May 2019 16:30
Last modified: 18 Feb 2021 16:34

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Contributors

Author: Robert D. Bannister
Author: William Levason ORCID iD
Author: Gillian Reid ORCID iD
Author: Fred Robinson

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