400 MHz Festkörper-NMR-Spektrometer
Zusammenfassung der Projektergebnisse
Due to the rapid development of computational resources and measuring techniques, solid state NMR has developed into a benchmark analytical tool for materials, precursors and molecular model systems. Due to the prevalence of NMR data in the solution phase it is also an increasingly important method to relate solution structure to the solid state. In detail the focus of our attention rests on the following applications of solid state NMR: (1) The emerging trend to reiterate the behavior of potent homogenous transition metal catalysts by typically more abundant and environmentally benign maingroup equivalents requires a thorough understanding of reversible binding of potential substrates to lowvalent molecular entities with vacant coordination sites. In cases where the often rapid dynamic processes in solution cannot be resolved unambiguously by lowering the temperature, solid state NMR has turned into the method of choice to gather spectroscopic data on at least one stationary state of the molecule. In addition, the chemical shift anisotropy as apparent from rotational side bands of a signal allows for a good estimate of the p-character of the bonding of an atom in question. (2) Hybrid nanoparticles containing silicon, silica, carbon and other materials are characterized inter alia by solid state NMR in order to determine the surface coverage with functionalizing agents. For example, organically functionalized hybrid particles are studied by 13C or 1H MAS NMR, in cases in which characteristic signals such as those of phenyl or vinyl groups are available. In addition, solid state NMR can provide important information about the network structure of the particles, e.g. crosslinking.
Projektbezogene Publikationen (Auswahl)
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“Important Reaction Parameters in the Synthesis of Phenylphosphonic Acid Functionalized Titania Particles by Reactive Milling”; New J. Chem. 2014, 38, 1264-1270
A. Betke, G. Kickelbick
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“Interaction and UV-stability of various organic capping agents on the surface of anatase nanoparticles”; Materials 2014, 7, 2890-2912
M. Raza, A. Bachinger, N. Zahn, G. Kickelbick
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“Long alkyl chain organophosphorus coupling agents for in situ surface functionalization by reactive milling”; Inorganics 2014, 2, 410-423
A. Betke, G. Kickelbick
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“Synthesis and aggregation behavior of hybrid amphiphilic titania Janus nanoparticles via surfacefunctionalization in Pickering emulsions”; Colloids Surf. A 2014, 461, 142-150
N. Zahn, G. Kickelbick;
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(Olig)aromatic species with one or two conjugated Si=Si bonds: near-IR emmission of antracenyl-bridged tetrasiladiene, Dalton Trans. 2017, 46, 8839
N. Obeid, L. Klemmer, D. Maus, M. Zimmer, J. Jeck, I. Bejan, A. J. P. White, V. Huch, G. Jung, D. Scheschkewitz
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Carbide-derived carbon beads with tunable nanopores from continuously produced polysilsesquioxanes for supercapacitor electrodes, Sust. Energy & Fuels 2017, 1, 1588
B. Krüner, C. Odenwald, A. Tolosa, A. Schreiber, M. Aslan, G. Kickelbick, V. Presser
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Disilenyl silylene reactivity of a cyclotrisilene, Angew. Chem. Int. Ed.
H. Zhao, K. Leszczynska, L. Klemmer, V. Huch, M. Zimmer, D. Scheschkewitz
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Synthesis and Structure of [2]Tetrelocenophanes, Eur. J. Inorg. Chem. 2017, 35-38
A. Schäfer, K. Rohe, A. Grandjean, V. Huch
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Mono- and Dicoordinate Germanium(0) as Four Electron Donor, Chem. Eur. J.
D. Mandal, D. Dhara, A. Maiti, L. Klemmer, H. S. Rzepa, D. Scheschkewitz, A. Jana
