Synthesis,Crystal Structure,and Selected Properties of [Au(S2CNH2)2]SCN: A Precursor for Gold Macro-Needles Consisting of Gold Nanoparticles Glued by Graphitic Carbon Nitride |
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| Authors: | Dr. Christoph Ludwig Teske Dr. Anna-Lena Hansen Prof. Dr. Richard Weihrich Prof. Dr. Lorenz Kienle Marius Kamp Kasper Pieter van der Zwan Prof. Dr. Jürgen Senker Dr. Carsten Dosche Prof. Dr. Gunther Wittstock Prof. Dr. Wolfgang Bensch |
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| Affiliation: | 1. Institute of Inorganic Chemistry, Christian-Albrechts-Universität zu Kiel, Max-Eyth-Str. 2, 24118 Kiel, Germany;2. Institute for Materials Research Management, University of Augsburg, Sigma Technopark, 86135 Augsburg, Germany;3. Institute for Materials Science, Christian-Albrechts-Universität zu Kiel, Kaiserstr. 2, 24143 Kiel, Germany;4. Inorganic Chemistry III, University of Bayreuth, Universitätsstr. 30, 95447 Bayreuth, Germany;5. Physical Chemistry, University of Oldenburg, 26111 Oldenburg, Germany |
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| Abstract: | A new preparation route is developed for the synthesis of needle-like crystals of [Au(S2CNH2)2]SCN, which avoids disproportionation of the AuI salt used as a starting material. In the crystal structure, the two crystallographically independent AuIII centers are in a square-planar environment of two S2CNH2 ligands. The Hirshfeld surface analysis reveals the presence of noncovalent intermolecular S⋅⋅⋅S interactions, which are essential for the spatial arrangement of the molecules. Density functional theory (DFT) calculations including dispersion and damping corrections result in a unit cell volume very close to the value determined experimentally. Thermal decomposition in an inert atmosphere generates black needles with lengths of up to 500 μm. X-ray powder diffraction and pair distribution function analyses demonstrate that the needles are composed of nanosized crystals with a volume-weighted average domain size of 20(1) nm. According to results of X-ray photoemission experiments, the black needles are covered by a nitrogen-rich carbon nitride with composition near (CN)2N. 13C solid-state NMR investigations indicate that two different carbon species are present, with signals corresponding well to heptazine units as in melon and triazine units as in poly(triazin imide) type compounds. Scanning transmission electron microscopy tomography evidences that the needles are composed of slightly elongated nanoparticles. |
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| Keywords: | gold dithiocarbamate gold nanoparticles pair distribution function transmission electron tomography X-ray diffraction |
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