Development of signal processing techniques and experimental design for the solid-state NMR of carbonaceous and nitrogenous materials

The elucidation of the molecular structure of carbon- and nitrogen-containing materials has a wide variety of applications, some of which are related to drug design, polymer synthesis and the development of an understanding of biological systems. Solid-state NMR is a well-established method of extracting structural information from such materials and may be used to probe the structure of both crystalline and amorphous materials. In particular, the Rotational-Echo Double Resonance (REDOR) experiment has traditionally been utilized to measure atomic distances present in systems containing an isolated, heteronuclear IS (i.e. 13C15N) spin pair of atoms. Presented here are modifications to, and additional uses for, the REDOR experiment. The addition of a double cross-polarization (DCP) filter to traditional REDOR and the extension of REDOR to geometry parameter measurement for spin triads are demonstrated. Methods of data processing and error analysis are utilized in order to shape experimental design and to determine the theoretical limit on the precision to which structural parameters may be measured. The DCP filter, combined with single cross-polarization and single resonance 13C and 15N experiments, is also used to elucidate the structure and mechanism of formation of a complex (HCN)_x heteropolymer relevant to origin of life research.