Last 21st May 2014 I defended my PhD Thesis entitled: Modern NMR Methodologies for the Measurement of Homo- and Heteronuclear Coupling Constants in Small Molecules
The dissertation is focused on the development of modern NMR methodologies for the measurement of homo- and heteronuclear coupling constants in small molecules, and is presented as a compendium of eight (8) publications that have been published in several peer-reviewed journals as original research papers. The starting point was the previous experience and knowledge of our research group in that topic. Taking as a reference the selHSQMBC experiment, several features have been implemented in order to design a complete set of different methodologies that allow us to overcome some of the most typical drawbacks regarding such measurements, namely, a) the magnitude of small nJ(CH) (<2-3 Hz), b) the determination of the sign-sensitive information, and c) measurement in both protonated and non-protonated carbons. In most of the cases the IPAP methodology has been used to achieve an accurate measurement. A spin-state selective technique like the E.COSY pattern, as well as the concept of J-resolved spectroscopy, have been implemented in conjunction with the IPAP methodology to obtain simultaneous measurement of several coupling constants from a single 2D cross-peak. Moreover, advances in the measurement of one-bond proton-carbon coupling constant and geminal proton-proton coupling constants in diastereotopic methylene groups are also presented. Each experiment has been discussed from a methodological point of view. An assessment on its application has been also performed.
Useful Links: Pulse Programs and Data Set Examples, here
