“Structural discrimination from in-situ measurement of 1DCH and 2DHH RDCs” by Núria Marcó, R. R. Gil and Teodor Parella. Magnetic Resonance in Chemistry 2017, DOI:
A fast RDC-assisted strategy involving the simultaneous determination of scalar and total coupling constants from a single 1JCH/2JHH-resolved NMR spectrum is reported. It is shown that the concerted use of the directly measured 1DCH (for all CHn multiplicities) and 2DHH residual dipolar couplings allows an on-the-fly assignment of diastereotopic CH2 protons, as well as of an efficient discrimination between all eight possible diastereoisomeric structures of strychnine, which contains six stereocenters.
Pulse Programs Code for Bruker:
Data set Example:
“Perfect 1JCH-resolved HSQC: Efficient measurement of one-bond proton-carbon coupling constants along the indirect dimension” by Núria Marcó, A.A. Souza, Pau Nolis, R. R. Gil and Teodor Parella. Journal of Magnetic resonance 2017, 276, 37-42. DOI: 10.1016/j.jmr.2017.01.002
A versatile 1JCH-resolved HSQC pulse scheme for the speedy, accurate and automated determination of one-bond proton-carbon coupling constants is reported. The implementation of a perfectBIRD element allows a straightforward measurement from the clean doublets obtained along the highly resolved F1 dimension, even for each individual 1JCHa and 1JCHb in diastereotopic HaCHb methylene groups. Real-time homodecoupling during acquisition and other alternatives to minimize accidental signal overlapping in overcrowded spectra are also discussed.
Pulse Programs Code for Bruker:
Data set Example:
“ 1JCH NMR Profile: Identification of key structural features and functionalities by visual observation and direct measurement of one-bond proton-carbon coupling constants” by Núria Marcó, A.A. Souza, Pau Nolis, Carlos Cobas, R. R. Gil and Teodor Parella. Journal of Organic Chemistry 2017, 276 : 37.42. DOI: 10.1021/acs.joc.6b02873
A user-friendly NMR interface for the visual and accurate determination of experimental one-bond proton-carbon coupling constants (1JCH) in small molecules is presented. This intuitive 1JCH profile correlates directly delta(1H) and 1JCH facilitates the rapid identification and assignment of 1H signals belonging to key structural elements and functional groups. Illustrative examples are provided for some target molecules including terminal alkynes, strained rings, electronegative substituents or lone-pair bearing heteronuclei.
Accurate measurement of JHH in overlapped signals by a TOCSY-edited SERF Experiment
André Fredi, Pau Nolis* and Teodor Parella*
Magnetic Resonance in Chemistry:
Selective Refocusing (GSERF or the recent PSYCHEDELIC) experiments were originally designed to determine all proton-proton coupling constants (JHH) for a selected proton resonance. They work for isolated signals on which selective excitation can be successfully applied but, as happens in other selective experiments, fail for overlapped signals. To circumvent this limitation, a doubly-selective TOCSY-GSERF scheme is presented for the measurement of JHH in protons resonating in crowded regions. This new experiment takes advantage of the editing features of an initial TOCSY transfer to uncover hidden resonances that become accessible to perform the subsequent frequency-selective refocusing.
Development and application of modern pure shift NMR techniques and improved HSQC/HSQMBC experiments
In the following links one can find Data Set Examples of each Publication presented in the Thesis Work, as well as the corresponding Pulse Program Code for Bruker. All 2D spectra have been previously phased and 2ii, 2ir, and 2ri files removed, otherwise data sets would be too big. Continue reading PhD Thesis by Laura Castañar: Pulse Programs and Data Set Examples
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. Continue reading PhD Thesis: Modern NMR Methodologies for the Measurement of Homo- and Heteronuclear Coupling Constants in Small Molecules
“Simultaneous measurement of J(HH) and two different nJ(CH) coupling constants from a single multiply-edited 2D cross-peak”, by Josep Saurí and Teodor Parella; Magn. Reson. Chem. 2013, 51, 397-402. DOI: 10.1002/mrc.3960
Three different J-editing methods (IPAP, E.COSY and J-resolved) are implemented in a single NMR experiment to provide spin-state-edited 2D cross-peaks from which simultaneous measurement of different homonuclear and heteronuclear coupling constants can be performed. Continue reading J-selHSQMBC: Simultaneous measurement of J(HH) and two different nJ(CH) using IPAP, J-resolved and E.COSY principles