Chlorine-35/37 NMR Detection of Chlorine Atoms Directly Bound to Paramagnetic Metal Ions in Solids

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Bauder, Lukas Benjamin Tashi

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thesis

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eng

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Paramagnetic shift , Hyperfine coupling tensor , Quadrupole coupling tensor , Co(II) compounds , V(III) compounds , 35/37Cl NMR

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Since the very first NMR experiments in the 1940s, NMR has established itself as one of the most powerful tools in the analysis of chemical substances. However, an overwhelming majority of NMR applications deals with diamagnetic compounds. In contrast, NMR is less successful in studies of paramagnetic compounds. This is largely because the unpaired electrons in paramagnetic compounds often cause the NMR signals to be significantly shifted and broadened, making them difficult to be observed. It is particularly difficult to probe atoms directly bound to paramagnetic metal centres. This thesis demonstrates for the first time that high-quality 35/37Cl NMR spectra can be obtained and interpreted for chlorine atoms directly bound to paramagnetic cobalt(II) (S = 3/2) and vanadium(III) (S = 1) metal ions in solid powder samples. In particular, on the basis of spectra obtained at three magnetic fields (11.7 T, 14.1 T and 16.5 T), 35/37Cl hyperfine and quadrupolar parameters were obtained for CoCl2, CoCl2 ·2 H2O, CoCl2 ·6 H2O, Co(terpy)Cl2 (where terpy = 2,2’:6’,2”- terpyridine), VCl3 and VCl3(thf)3 (where thf=tetrahydrofuran). These experimental results were found to be in reasonable agreement with quantum chemical calculations performed with the AMS/BAND program.

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