Studies in two-dimensional long-range heteronuclear chemical shift correlation NMR spectroscopy



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The work described in this dissertation revolves around the two- dimensional long-range heteronuclear chemical shift correlation NMR experiment. This experiment provides a means of correlating heteronuclei which, for the purposes of this dissertation, will be limited to 1H and 13C, through two- three- and occasionally four-bond coupling pathways. Importantly, the technique allows the investigator to transfer magnetization to, and thus identify quaternary carbons. In addition, the correlation of heteronuclei across quaternary carbons and heteronuclei is possible with this long-range experiment. Long range heteronuclear chemical shift correlation has proven very useful in solving 1H- and 13C-NMR spectral assignment and structure elucidation problems. The only other NMR experiment capable of providing unequivocal chemical shift correlation to and across quaternary carbons is the extremely insensitive 13C-13C double quantum coherence (INADEQUATE) experiment, with which the long- range chemical shift correlated experiment was directly compared in this work. [...]



Nuclear magnetic resonance spectroscopy