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Chem Sci. 2017 Mar 1;8(3):2235-2240. doi: 10.1039/c6sc04578b. Epub 2016 Dec 15.

[Ag115S34(SCH2C6H4t Bu)47(dpph)6]: synthesis, crystal structure and NMR investigations of a soluble silver chalcogenide nanocluster.

Author information

1
Institute of Inorganic Chemistry , Karlsruhe Institute of Technology (KIT) , Engesserstraße 15 , 76131 Karlsruhe , Germany . Email: sebastian.bestgen@kit.edu ; Email: dieter.fenske@kit.edu.
2
Institute of Nanotechnology and Karlsruhe Nano Micro Facility (KNMF) , Karlsruhe Institute of Technology (KIT) , Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen , 76021 Karlsruhe , Germany.
3
Lehn-Institute for Functional Materials , School of Chemistry and Chemical Engineering , Sun Yat-Sen University , Guangzhou , People's Republic of China.
4
Helmholtz-Institute Ulm for Electrochemical Energy Storage (HIU) , Karlsruhe Institute of Technology (KIT) , 89081 Ulm , Germany.
5
Institute for Water Chemistry and Water Technology , Institute for Mechanical Process Engineering and Mechanics , Karlsruhe Institute of Technology , Adenauerring 20b , 76131 Karlsruhe , Germany.
6
Zhejiang Provincial Key Laboratory for Chemical and Biochemical Processing Technology of Farm Products , School of Biological and Chemical Engineering , Zhejiang University of Science and Technology , No. 318 Liuhe Road , Hangzhou , 310023 , People's Republic of China.
7
Institute of Physical Chemistry , Karlsruhe Institute of Technology , Kaiserstraße 12 , 76131 Karlsruhe , Germany.

Abstract

With the aim to synthesize soluble cluster molecules, the silver salt of (4-(tert-butyl)phenyl)methanethiol [AgSCH2C6H4t Bu] was applied as a suitable precursor for the formation of a nanoscale silver sulfide cluster. In the presence of 1,6-(diphenylphosphino)hexane (dpph), the 115 nuclear silver cluster [Ag115S34(SCH2C6H4t Bu)47(dpph)6] was obtained. The molecular structure of this compound was elucidated by single crystal X-ray analysis and fully characterized by spectroscopic techniques. In contrast to most of the previously published cluster compounds with more than a hundred heavy atoms, this nanoscale inorganic molecule is soluble in organic solvents, which allowed a comprehensive investigation in solution by UV-Vis spectroscopy and one- and two-dimensional NMR spectroscopy including 31P/109Ag-HSQC and DOSY experiments. These are the first heteronuclear NMR investigations on coinage metal chalcogenides. They give some first insight into the behavior of nanoscale silver sulfide clusters in solution. Additionally, molecular weight determinations were performed by 2D analytical ultracentrifugation and HR-TEM investigations confirm the presence of size-homogeneous nanoparticles present in solution.

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