STUDIES IN TWO-DIMENSIONAL LONG-RANGE HETERONUCLEAR CHEMICAL SHIFT CORRELATION NMR SPECTROSCOPY

The work described in this dissertation revolves around the two-dimensional long-range heteronuclear chemical shift correlation NMR experiment. Long range heteronuclear chemical shift correlation has proven very useful in solving ;Chapter 4 describes the strategy employed in making the total, unequivocal assignments of the ;Chapter 5 describes the assignment strategy of the ;Chapter 6 describes two related studies of the long-range heteronuclear experiment performed on the model compound 1-benzthieno (3,2-c) pyridine (6-1). The first objective was to compare a number of variations of the long-range heteronuclear experiment which have recently been demonstrated. The pulse sequences compared include: LROCSCM; underbar co rrelation underbar s pectroscopy via underbar l ong-range underbar c ouplings (COLOC); long-range heteronuclear chemical shift correlation (CSCMLR); and underbar fu lly underbar coup led heteronuclear chemical shift correlation (FUCOUP). The second objective was to examine the role of optimization of long-range polarization transfer in the long-range heteronuclear chemical shift correlation experiments. Experiments were run at several different optimizations and observed responses were tabularized. Observed and predicted response intensities were in good agreement. (Abstract shortened with permisson of author.).;Chapter 1 provides an overview of the stage of development of the various two-dimensional long range heteronuclear chemical shift correlations experiment. Chapter 2 reviews the basic concepts, terminology and conventions of the experiments. General experimental details are presented in Chapter 3.