TY - JOUR
T1 - The di(thiourea)gold(I) complex [Au{S=C(NH2)2}2][SO3Me] as a precursor for the convenient preparation of gold nanoparticles
AU - Kossmann, Alexander
AU - Ehnert, Rayko
AU - Preuß, Andrea
AU - Rüffer, Natalia
AU - Korb, Marcus
AU - Schulze, Steffen
AU - Tegenkamp, Christoph
AU - Köster, Frank
AU - Lang, Heinrich
PY - 2020/3
Y1 - 2020/3
N2 - The synthesis of [Au{S=C(NH2)2}2][SO3Me] (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)3 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-1) 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.
AB - The synthesis of [Au{S=C(NH2)2}2][SO3Me] (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)3 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-1) 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.
KW - bis(thiourea) gold complex
KW - electrolysis
KW - nanoparticles
KW - solid-state structure
KW - thermal behavior
UR - http://www.scopus.com/inward/record.url?scp=85081717609&partnerID=8YFLogxK
U2 - 10.1515/znb-2019-0213
DO - 10.1515/znb-2019-0213
M3 - Article
AN - SCOPUS:85081717609
SN - 0932-0776
VL - 75
SP - 239
EP - 249
JO - Zeitschrift fur Naturforschung - Section B Journal of Chemical Sciences
JF - Zeitschrift fur Naturforschung - Section B Journal of Chemical Sciences
IS - 3
ER -