Issue 41, 2019

Accessing γ-Ga2S3 by solventless thermolysis of gallium xanthates: a low-temperature limit for crystalline products

Abstract

Alkyl–xanthato gallium(III) complexes of the form [Ga(S2COR)3], where R = Me (1), Et (2), iPr (3), nPr (4), nBu (5), sBu (6) and iBu (7), have been synthesized and fully characterised. The crystal structures for 1 and 3–7 have been solved and examined to elucidate if these structures are related to their decomposition. Thermogravimetric analysis was used to gain insight into the decomposition temperatures for each complex. Unlike previously explored metal xanthate complexes which break down at low temperatures (<250 °C), to form crystalline metal chalcogenides, powder X-ray diffraction measurements suggest that when R ≥ Et these complexes did not produce crystalline gallium sulfides until heated to 500 °C, where γ-Ga2S3 was the sole product formed. In the case of R = Me, Chugaev elimination did not occur and amorphous GaxSy products were formed. We conclude therefore that the low-temperature synthesis route offered by the thermal decomposition of metal xanthate precursors, which has been reported for many metal sulfide systems prior to this, may not be appropriate in the case of gallium sulfides.

Graphical abstract: Accessing γ-Ga2S3 by solventless thermolysis of gallium xanthates: a low-temperature limit for crystalline products

Supplementary files

Article information

Article type
Paper
Submitted
16 май 2019
Accepted
26 юли 2019
First published
07 авг 2019

Dalton Trans., 2019,48, 15605-15612

Accessing γ-Ga2S3 by solventless thermolysis of gallium xanthates: a low-temperature limit for crystalline products

S. A. Alderhami, D. Collison, D. J. Lewis, P. D. McNaughter, P. O'Brien, B. F. Spencer, I. Vitorica-Yrezabal and G. Whitehead, Dalton Trans., 2019, 48, 15605 DOI: 10.1039/C9DT02061F

To request permission to reproduce material from this article, please go to the Copyright Clearance Center request page.

If you are an author contributing to an RSC publication, you do not need to request permission provided correct acknowledgement is given.

If you are the author of this article, you do not need to request permission to reproduce figures and diagrams provided correct acknowledgement is given. If you want to reproduce the whole article in a third-party publication (excluding your thesis/dissertation for which permission is not required) please go to the Copyright Clearance Center request page.

Read more about how to correctly acknowledge RSC content.

Social activity

Spotlight

Advertisements