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Ehnert, Rayko
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article
The di(thiourea)gold(I) complex [Au{S=C(NH2)2}2][SO3Me] as a precursor for the convenient preparation of gold nanoparticles
Abstract
<p>The synthesis of [Au{S=C(NH<sub>2</sub>)<sub>2</sub>}<sub>2</sub>][SO<sub>3</sub>Me] (1) (a) by the anodic oxidation of gold metal in an anolyte of thiourea and methansulfonic acid and (b) by the reaction of Au(OH)<sub>3</sub> with an aqueous solution of methanesulfonic acid in the presence of thiourea is reported. The structure of 1 in the solid state has been determined by single-crystal X-ray diffraction showing a linear S-Au-S unit with the thiourea ligands in a leaflet structure folded by 113.2(3)°. The cation of complex 1 is a dimer, based on short S · · · C interactions between two adjacent mononuclear cations. The thermal decomposition behavior of 1 was studied by TG and TG-MS confirming that it decomposes under inert gas or oxygen atmosphere in four steps in the temperature range of 200-650°C. Initial decomposition starts with the release and fragmentation of one of the thiourea ligands, followed by the anion degradation. Powder X-ray diffraction studies specified the formation of gold metal. Based on this observation, complex 1 was used as precursor for the formation of gold nanoparticles (Au NPs) in 1-hexadecylamine (c = 4.0 mol L<sup>-1</sup>) at T = 330°C without any addition of reducing agents. TEM, electron diffraction, and UV/Vis spectroscopy studies were carried out. Au NPs of size 15 ± 4 nm were formed, showing the characteristic surface plasmon resonance at 528 nm.</p>