Straightforward measurement of individual 1J(CH) and 2J(HH) in diastereotopic CH2 groups

Journal of Magnetic Resonance

Volumn 242, Issue , 2014, Pages 33-40

  Saurí, Josep ^a   Castañar, Laura ^a   Nolis, Pau ^a   Virgili, Albert ^a   Parella, Teodor ^a  

^a UNIVERSITAT AUTÒNOMA DE BARCELONA   (Spain)

Author keywords

E.COSY; Inverse INEPT; Methylene spin systems; One bond proton carbon coupling constants; Residual dipolar couplings; Two bond proton proton coupling constants

Indexed keywords

E.COSY; INVERSE INEPT; PROTON-CARBON COUPLING CONSTANTS; PROTON-PROTON COUPLING CONSTANTS; RESIDUAL DIPOLAR COUPLINGS; SPIN SYSTEMS;

POLARIZATION; SPIN DYNAMICS;

PROTONS;

EID: 84897713343     PISSN: 10907807     EISSN: 10960856     Source Type: Journal    
DOI: 10.1016/j.jmr.2014.02.003     Document Type: Article

References (41)

1. C.M. Thiele Residual dipolar couplings (RDCs) in organic structure determination Eur. J. Org. Chem. 2008 5673 5685
2. G. Kummerlowe, and B. Luy Residual dipolar couplings for the configurational and conformational analysis of organic molecules Annu. Rep. NMR Spectrosc. 68 2009 193 230
3. G. Kummerlowe, and B. Luy Residual dipolar couplings as a tool in determining the structure of organic molecules Trend Anal. Chem. 28 2009 483 493
4. A. Enthart, J.C. Freudenberger, J. Furrer, H. Kessler, and B. Luy The CLIP/CLAP HSQC: pure absorptive spectra for the measurement of one-bond couplings J. Magn. Reson. 192 2008 314 322
5. C.M. Thiele Simultaneous assignment of all diastereotopic protons in strychnine using RDCs: PELG as alignment medium for organic molecules J. Org. Chem. 69 2004 7403 7413
6. 3JHH strong coupling in natural abundance J. Magn. Reson. 215 2012 10 22
7. B.W. Yu, H. van Ingen, and D.I. Freedberg Constant time INEPT CT-HSQC (CTi-CT-HSQC) - a new NMR method to measure accurate one-bond J and RDCs with strong 1H-1H couplings in natural abundance J. Magn. Reson. 228 2013 159 165
8. 2JHH + DHH) couplings J. Magn. Reson. 186 2007 193 200
9. K. Fehér, S. Berger, and K.E. Kövér Accurate determination of small one-bond heteronuclear residual dipolar couplings by F1 coupled HSQC modified with a G-BIRD(r) module J. Magn. Reson. 163 2003 340 346
10. C.M. Thiele, and W. Bermel Speeding up the measurement of one-bond scalar (1J) and residual dipolar couplings (1D) by using non-uniform sampling (NUS) J. Magn. Reson. 216 2012 134 143
11. K.E. Kövér, and K. Fehér Measurement of one-bond heteronuclear dipolar coupling contributions for amine and diastereotopic protons J. Magn. Reson. 168 2004 307 313
12. L. Ziani, J. Courtieu, and D. Merlet Visualisation of enantiomers via insertion of a BIRD module in X-H correlation experiments in chiral liquid crystal solvent J. Magn. Reson. 183 2006 60 67
13. 13C edited J/D-resolved NMR techniques Chem. Phys. Lett. 2010 334 341
14. J. Furrer, M. John, H. Kessler, and B. Luy J-spectroscopy in the presence of residual dipolar couplings: determination of one-bond coupling constants and scalable resolution J. Biomol. NMR 37 2007 231 243
15. M. Ottiger, F. Delaglio, J.L. Marquardt, N. Tjandra, and A. Bax Measurement of Dipolar Couplings for methylene and methyl sites in weakly oriented macromolecules and their use in structure determination J. Magn. Reson. 124 1998 365 369
16. 1JCH-modulated spectra with the BIRD inversion pulse J. Magn. Reson. 157 2002 200 209
17. 1DHH dipolar couplings in methylene groups J. Biomol. NMR 17 2000 99 109
18. P. Permi A spin-state-selective experiment for measuring heteronuclear one-bond and homonuclear two-bond couplings from an HSQC-type spectrum J. Biomol. NMR 22 2002 27 35
19. E. Miclet, D.C. Williams Jr., G.M. Clore, D.L. Bryce, J. Boisbouvier, and A. Bax Relaxation-optimized NMR spectroscopy of methylene groups in proteins and nucleic acids J. Am. Chem. Soc. 126 2004 10560 10570
20. 13C natural abundance Magn. Reson. Chem. 46 2008 918 924
21. nS spin systems J. Am. Chem. Soc. 126 2004 9821 9826
22. P. Permi Two simple NMR experiments for measuring dipolar couplings in asparagine and glutamine side chains J. Magn. Reson. 153 2001 267 272
23. 1H dipolar couplings provide a unique probe of RNA backbone structure J. Am. Chem. Soc. 125 2003 15740 15741
24. 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
25. P. Nolis, and T. Parella Solution-state NMR experiments based on heteronuclear cross-polarization Curr. Anal. Chem. 3 2007 47 68
26. 3JCH J. Magn. Reson. B 109 1995 275 283
27. K. Kobzar, H. Kessler, and B. Luy Stretched gelatin gels as chiral alignment media for the discrimination of enantiomers by NMR spectroscopy Angew. Chem. Int. Ed. 44 2005 3145 3147
28. J. Saurí, L. Castañar, P. Nolis, A. Virgili, and T. Parella P.E. HSQMBC: simultaneous measurement of proton-proton and proton-carbon coupling constants J. Magn. Reson. 224 2012 101 106
29. J.R. Garbow, D.P. Weitekamp, and A. Pines Bilinear rotation decoupling of homonuclear scalar interactions Chem. Phys. Lett. 93 1982 504 509
30. D. Uhrín, T. Liptaj, and K.E. Kövér Modified BIRD pulses and design of heteronuclear pulse sequences J. Magn. Reson. A 101 1993 41 46
31. C. Griesinger, O.W. Sørensen, and R.R. Ernst Two-dimensional correlation of connected NMR transitions J. Am. Chem. Soc. 107 1985 6394 6396
32. L. Mueller P.E-COSY, a simple alternative to E.COSY J. Magn. Reson. 72 1986 191 196
33. C. Griesinger, O.W. Sørensen, and R.R. Ernst Practical aspects of the E.COSY technique. Measurement of scalar spin-spin coupling constants in peptides J. Magn. Reson. 75 1987 474 492
34. 2/ NH 3 + groups with two-dimensional heteronuclear correlation spectroscopy J. Magn. Reson. 194 2008 313 316
35. W.P. Aue, L. Muller, and R.R. Ernst Phase separation in two-dimensional spectroscopy J. Magn. Reson. 28 1977 29 39
36. B. Luy, K. Kobzar, and H. Kessler An easy and scalable method for the partial alignment of organic molecules for measuring residual dipolar couplings Angew. Chem. Int. Ed. 43 2004 1092 1094
37. 13C NMR spectra of complex organic molecules by DFT methods: application to natural substances Chem. Eur. J. 12 2006 5514 5525
38. M. Misiak, and W. Koźmiński Determination of heteronuclear coupling constants from 3D HSQC-TOCSY experiment with optimized random sampling of evolution time space Magn. Reson. Chem. 47 2009 205 209
39. J.C. Cobas, V. Constantino-Castillo, M. Martín-Pastor, and F. del Río Portilla A two-stage approach to automatic determination of 1H NMR coupling constants Magn. Reson. Chem. 43 2005 843 848
40. C. Gayathri, N.V. Tsarevsky, and R.R. Gil RDCs analysis of small molecules made easy: fast and tuneable alignment by reversible compression/relaxation of reusable PMMA gels Chem. Eur. J. 16 2010 3622 3626
41. 1H dipolar couplings in weakly aligned proteins J. Biomol. NMR 20 2001 77 82