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

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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

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Publication details

The article was received on 16 May 2019, accepted on 26 Jul 2019 and first published on 07 Aug 2019


Article type: Paper
DOI: 10.1039/C9DT02061F
Dalton Trans., 2019, Advance Article

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    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, Advance Article , DOI: 10.1039/C9DT02061F

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