Date of Award
Chemistry and Biochemistry
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Wideline and ultra-wideline (UW) (i.e., > 250 kHz broad) solid-state NMR (SSNMR) spectra are acquired for a wide variety of nuclei (i.e., 119Sn, 195Pt, 199Hg, 207Pb, 27Al, 71Ga) using multiple acquisition techniques. The WURST-CPMG pulse sequence is shown to acquire such patterns efficiently and without the need for piecewise acquisition. Preliminary investigations into the use of optimal control theory (OCT) are also carried out, and show promise for future studies. Additionally, a series of Pb(II) thiolate species, which exhibit unique Pb bonding environments, are characterized with 207Pb SSNMR. Density Functional Theory (DFT) calculations are performed to determine chemical shielding (CS) tensor orientations within the molecular frame, which are then correlated to the experimental spectra. Finally, several group 13 guanidinates (guan = MeN-C(N iPr2)-NMe) are studied via 27Al and 71Ga SSNMR at 9.4 T and 21.1 T, and experimental data is complemented with ab initio calculations, and the CS and electric field gradient tensor parameters are found to have a great dependence on metal coordination number and the nature of the metal-ligand bond.
MacGregor, Alan W., "Development and application of techniques for the acquisition of ultra-wideline solid-state NMR spectra" (2010). Electronic Theses and Dissertations. 7950.