The University of Southampton
University of Southampton Institutional Repository

Synthesis and properties of [NR4]3[SbS4] (R = Me, Et, n-Pr, n-Bu) and the crystal structures of [N(n-Bu)4]3[SbS4]⋅6H2O and [N(n-Bu)4]3[Sb(S2O3)3]·2THF

Synthesis and properties of [NR4]3[SbS4] (R = Me, Et, n-Pr, n-Bu) and the crystal structures of [N(n-Bu)4]3[SbS4]⋅6H2O and [N(n-Bu)4]3[Sb(S2O3)3]·2THF
Synthesis and properties of [NR4]3[SbS4] (R = Me, Et, n-Pr, n-Bu) and the crystal structures of [N(n-Bu)4]3[SbS4]⋅6H2O and [N(n-Bu)4]3[Sb(S2O3)3]·2THF

The tetra-alkylammonium tetrathioantimonate(V) salts, [NR4]3[SbS4] (R = Me, Et, n-Pr, n-Bu), have been prepared in basic solution from aqueous [NR4]OH, sulfur and Sb2S3, and characterised by microanalysis, IR, Raman, 1H and 121Sb NMR spectroscopy. The crystal structure of [N(n-Bu)4]3[SbS4]·6H2O shows the presence of the tetrahedral [SbS4]3− anion (disordered over two sites), and also connected through an H-bonding network with the lattice water molecules. The alkylammonium salts are soluble in water and, with the exception of [NMe4]3[SbS4], are also soluble in weakly polar organic solvents, including halocarbons and MeCN. Solubility increases with the R group Me < Et < n-Pr < n-Bu, making the [N(n-Bu)4)3[SbS4] a convenient reagent to explore coordination chemistry or materials applications for which water as the solvent is not suitable. [N(n-Bu)4]3[Sb(S2O3)3]·2THF, the first thiosulfate complex of a p-block element, was produced by slow decomposition of [N(n-Bu)4]3[SbS4] in THF solution in the presence of the [NH(n-Bu)3]Cl (as a source of H+), confirming the instability of the [SbS4]3− anion in acidic media, and the crystal structure of [N(n-Bu)4]3[Sb(S2O3)3]·2THF shows a trigonal antiprismatic coordination geometry with a S3O3 donor set at the antimony(III) centre in the anion.

0022-2860
King, Rhys P.
2f9548b8-fc3b-447c-a5df-de5a3e513a39
Levason, William
e7f6d7c7-643c-49f5-8b57-0ebbe1bb52cd
Reid, Gillian
37d35b11-40ce-48c5-a68e-f6ce04cd4037
King, Rhys P.
2f9548b8-fc3b-447c-a5df-de5a3e513a39
Levason, William
e7f6d7c7-643c-49f5-8b57-0ebbe1bb52cd
Reid, Gillian
37d35b11-40ce-48c5-a68e-f6ce04cd4037

King, Rhys P., Levason, William and Reid, Gillian (2023) Synthesis and properties of [NR4]3[SbS4] (R = Me, Et, n-Pr, n-Bu) and the crystal structures of [N(n-Bu)4]3[SbS4]⋅6H2O and [N(n-Bu)4]3[Sb(S2O3)3]·2THF. Journal of Molecular Structure, 1278, [134925]. (doi:10.1016/j.molstruc.2023.134925).

Record type: Article

Abstract

The tetra-alkylammonium tetrathioantimonate(V) salts, [NR4]3[SbS4] (R = Me, Et, n-Pr, n-Bu), have been prepared in basic solution from aqueous [NR4]OH, sulfur and Sb2S3, and characterised by microanalysis, IR, Raman, 1H and 121Sb NMR spectroscopy. The crystal structure of [N(n-Bu)4]3[SbS4]·6H2O shows the presence of the tetrahedral [SbS4]3− anion (disordered over two sites), and also connected through an H-bonding network with the lattice water molecules. The alkylammonium salts are soluble in water and, with the exception of [NMe4]3[SbS4], are also soluble in weakly polar organic solvents, including halocarbons and MeCN. Solubility increases with the R group Me < Et < n-Pr < n-Bu, making the [N(n-Bu)4)3[SbS4] a convenient reagent to explore coordination chemistry or materials applications for which water as the solvent is not suitable. [N(n-Bu)4]3[Sb(S2O3)3]·2THF, the first thiosulfate complex of a p-block element, was produced by slow decomposition of [N(n-Bu)4]3[SbS4] in THF solution in the presence of the [NH(n-Bu)3]Cl (as a source of H+), confirming the instability of the [SbS4]3− anion in acidic media, and the crystal structure of [N(n-Bu)4]3[Sb(S2O3)3]·2THF shows a trigonal antiprismatic coordination geometry with a S3O3 donor set at the antimony(III) centre in the anion.

Text
1-s2.0-S0022286023000261-main - Version of Record
Available under License Creative Commons Attribution.
Download (1MB)

More information

Accepted/In Press date: 4 January 2023
e-pub ahead of print date: 6 January 2023
Published date: 18 January 2023
Additional Information: Funding Information: We thank the EPSRC for funding through grants EP/P025137/1 and EP/N035437/1.

Identifiers

Local EPrints ID: 475516
URI: http://eprints.soton.ac.uk/id/eprint/475516
ISSN: 0022-2860
PURE UUID: 159dcd83-f97a-4233-a2e3-e7268871cc88
ORCID for William Levason: ORCID iD orcid.org/0000-0003-3540-0971
ORCID for Gillian Reid: ORCID iD orcid.org/0000-0001-5349-3468

Catalogue record

Date deposited: 21 Mar 2023 17:33
Last modified: 28 Aug 2024 01:33

Export record

Altmetrics

Contributors

Author: Rhys P. King
Author: William Levason ORCID iD
Author: Gillian Reid ORCID iD

Download statistics

Downloads from ePrints over the past year. Other digital versions may also be available to download e.g. from the publisher's website.

View more statistics

Atom RSS 1.0 RSS 2.0

Contact ePrints Soton: eprints@soton.ac.uk

ePrints Soton supports OAI 2.0 with a base URL of http://eprints.soton.ac.uk/cgi/oai2

This repository has been built using EPrints software, developed at the University of Southampton, but available to everyone to use.

We use cookies to ensure that we give you the best experience on our website. If you continue without changing your settings, we will assume that you are happy to receive cookies on the University of Southampton website.

×