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Issue 41, 2020
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Synthesis and characterization of zinc di(O-2,2-dimethylpentan-3-yl dithiocarbonates) bearing pyridine or tetramethylethylenediamine coligands and investigation of their thermal conversion mechanisms towards nanocrystalline zinc sulfide

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Abstract

Metal xanthates are versatile single source precursors for the preparation of various metal sulfides. In this study, we present the synthesis of the two novel zinc xanthate complexes bis(O-2,2-dimethylpentan-3-yl-dithiocarbonato)(N,N,N′,N′-tetramethylethylenediamine)zinc(II) and bis(O-2,2-dimethylpentan-3-yl-dithiocarbonato)(pyridine)zinc(II). A thorough investigation of these compounds revealed distinct differences in their structural and thermal properties. While in the complex containing the chelating tetramethylethylenediamine, the xanthate groups coordinate in a monodentate way, they are bidentally coordinated to the zinc atom in the pyridine containing complex. Both compounds show a two-step thermal decomposition with an onset temperature of 151 °C and 156 °C for the tetramethylethylenediamine and pyridine containing complex, respectively. Moreover, different mechanisms are revealed for the two phases of the decomposition based on high resolution mass spectrometry investigations. By the thermal conversion process nanocrystalline zinc sulfide is produced and the coligand significantly influences its primary crystallite size, which is 4.4 nm using the tetramethylethylenediamine and 11.4 nm using the pyridine containing complex for samples prepared at a temperature of 400 °C.

Graphical abstract: Synthesis and characterization of zinc di(O-2,2-dimethylpentan-3-yl dithiocarbonates) bearing pyridine or tetramethylethylenediamine coligands and investigation of their thermal conversion mechanisms towards nanocrystalline zinc sulfide

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Supplementary files

Article information


Submitted
01 Sep 2020
Accepted
06 Oct 2020
First published
14 Oct 2020

This article is Open Access

Dalton Trans., 2020,49, 14564-14575
Article type
Paper

Synthesis and characterization of zinc di(O-2,2-dimethylpentan-3-yl dithiocarbonates) bearing pyridine or tetramethylethylenediamine coligands and investigation of their thermal conversion mechanisms towards nanocrystalline zinc sulfide

E. Vakalopoulou, C. Buchmaier, A. Pein, R. Saf, R. C. Fischer, A. Torvisco, F. Warchomicka, T. Rath and G. Trimmel, Dalton Trans., 2020, 49, 14564
DOI: 10.1039/D0DT03065A

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