Accurate measurement of small heteronuclear coupling constants from pure-phase α/β HSQMBC cross-peaks

Journal of Magnetic Resonance

Volumn 213, Issue 1, 2011, Pages 145-150

  Gil, Sergi ^a   Espinosa, Juan Félix ^b   Parella, Teodor ^a  

^a UNIVERSITAT AUTÒNOMA DE BARCELONA   (Spain)

^b ELI LILLY AND COMPANY   (Spain)

Author keywords

HSQMBC; IPAP; Long range proton carbon coupling constants; NMR; Spin state selective

Indexed keywords

ACCURATE MEASUREMENT; COUPLING CONSTANTS; EXPERIMENTAL CONDITIONS; FITTING PROCEDURE; HETERONUCLEAR COUPLING; HSQMBC; IN-PHASE; IPAP; LONG-RANGE PROTON-CARBON COUPLING CONSTANTS; MULTIPLET PATTERNS; PHASE DISTORTIONS; POST PROCESSING; RELATIVE DISPLACEMENT; SIGNAL INTENSITIES; SMALL MOLECULES; SPIN-STATE;

PROTONS;

PROTON; STRYCHNINE;

ARTICLE; ARTIFACT; CHEMISTRY; METHODOLOGY; NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY; REPRODUCIBILITY; SIGNAL PROCESSING;

ARTIFACTS; MAGNETIC RESONANCE SPECTROSCOPY; PROTONS; REPRODUCIBILITY OF RESULTS; SIGNAL PROCESSING, COMPUTER-ASSISTED; STRYCHNINE;

EID: 80055089976     PISSN: 10907807     EISSN: 10960856     Source Type: Journal    
DOI: 10.1016/j.jmr.2011.09.036     Document Type: Article

References (19)

1. R. Riccio, G. Bifulco, P. Cimino, C. Bassarello, and L. Gomez-Paloma Stereochemical analysis of natural products. Approaches relying on the combination of NMR spectroscopy and computational methods Pure Appl. Chem. 2-3 2003 295 308
2. G. Bifulco, P. Dambruoso, L. Gomez-Paloma, and R. Riccio Determination of relative configuration in organic compounds by NMR spectroscopy and computational methods Chem. Rev. 107 2007 3744 3779 (Pubitemid 47534317)
3. nJ(C,H) heteronuclear coupling constants in small molecules Magn. Reson. Chem. 39 2001 499 530
4. T. Parella 2D Methods for the measurement of long-range proton-carbon coupling constants G.A. Morris, J.W. Emsley, Multidimensional NMR Methods for the Solution State 2010 John Wiley & Sons Ltd. Chichester, UK 305 314
5. W. Koźmiński Simplified multiplet pattern HSQC-TOCSY experiment for accurate determination of long-range heteronuclear coupling constants J. Magn. Reson. 137 1999 408 412 (Pubitemid 129608270)
6. P. Nolis, and T. Parella Spin-edited 2D HSQC-TOCSY experiments for the measurement of homonuclear and heteronuclear coupling constants: application to carbohydrates and peptides J. Magn. Reson. 176 2005 15 26 (Pubitemid 41162471)
7. P. Nolis, J.F. Espinosa, and T. Parella Optimum spin-state selection for all multiplicities in the acquisition dimension of the HSQC experiment J. Magn. Reson. 180 2006 39 50
8. nJCH + DCH)-couplings at natural abundance J. Magn. Reson. 186 2007 131 141 (Pubitemid 46635253)
9. 1H coupling constants from HMBC spectra J. Magn. Reson. 166 2004 53 68
10. R.T. Williamson, B.L. Márquez, W.H. Gerwick, and K.E. Kövér One- and two-dimensional gradient-selected HSQMBC NMR experiments for the efficient analysis of long-range heteronuclear coupling constants Magn. Reson. Chem. 38 2000 265 273
11. K.E. Kövér, G. Batta, and K. Feher Accurate measurement of long-range heteronuclear coupling constants from undistorted multiplets of an enhanced CPMG-HSQMBC experiment J. Magn. Reson. 181 2006 89 97 (Pubitemid 43866541)
12. S. Boros, and K.E. Kövér Low-power composite CPMG HSQMBC experiment for accurate measurement of long-range heteronuclear coupling constants Magn. Reson. Chem. 49 2011 106 110
13. A. Meissner, and O.W. Sorensen Measurement of J(H,H) and long-range J(X,H) coupling constants in small molecules. Broadband XLOC and J-HMBC Magn. Reson. Chem. 39 2001 49 52
14. V. Krishnamurthy Excitation-sculptured indirect-detection experiment (EXSIDE) for long-range CH coupling-constant measurement J. Magn. Reson. A. 121 1996 33 41 (Pubitemid 126751770)
15. S. Gil, J.F. Espinosa, and T. Parella IPAP-HSQMBC: measurement of long-range heteronuclear coupling constants from spin-state selective multiplet J. Magn. Reson. 207 2010 312 321
16. A. Bax, K.A. Farley, and G.S. Walker Increased HMBC sensitivity for correlating poorly resolved proton multiplets to carbon-13 using selective or semi-selective pulses J. Magn. Reson. A 119 1996 134 138 (Pubitemid 126753482)
17. W. Koźmiński, and D. Nanz Sensitivity improvement and new acquisition scheme of heteronuclear active-coupling-pattern-tilting spectroscopy J. Magn. Reson. 142 2000 294 321
18. J.F. Espinosa, P. Vidal, T. Parella, and S. Gil Measurement of long-range proton-carbon coupling constants from pure in-phase 1D multiplets Magn. Reson. Chem. 49 2011 502 507
19. T. Jippo, O. Kamo, and K. Nagayama Determination of long-range proton-carbon 13 coupling constants with selective two-dimensional INEPT J. Magn. Reson. 66 1986 344 348