Date of Award
Chemistry and Biochemistry
Schurko, Robert (Chemistry and Biochemistry)
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This thesis demonstrates that solid-state NMR (SSNMR) spectroscopy of quadrupolar nuclei provides a powerful means of characterizing a diverse set of materials. Complementary techniques such as pXRD and quantum chemical calculations are also explored. First, information on the structure and function of methylalumoxane (MAO) is obtained via 27Al and 91Zr SSNMR experiments at two different magnetic field strengths. In particular, 27Al NMR and accompanying first principles calculations reveal the nature of the Al sites in the cage-like MAO structures, and lend insight into the interactions that lead to the formation of the MAO/metallocene adducts. Second, a series of hydrochloride (HCl) pharmaceuticals are characterized via 35Cl SSNMR, and arrangements of close-contact hydrogen bonds are correlated to 35Cl EFG tensor parameters. Plane-wave density functional theory calculations of these parameters are in good agreement with experiment. 35Cl SSNMR is also shown to act as an unambiguous "fingerprint" for polymorphs of HCl pharmaceuticals.
Hildebrand, Marcel, "Solid-State NMR of Quadrupolar Nuclei for Structural Elucidation" (2012). Electronic Theses and Dissertations. 305.