Measurement of Magnitude and Sign of Heteronuclear Coupling Constants in Transition Metal Complexes

Journal of Magnetic Resonance

Volumn 137, Issue 2, 1999, Pages 413-429

  Otting, Gottfried ^a   Soler, Linnea P ^b   Messerle, Barbara A ^b  

^a KAROLINSKA INSTITUTE   (Sweden)

^b UNIVERSITY OF SYDNEY   (Australia)

Author keywords

DQ ZQ experiments; E.COSY type experiments; Long range correlation experiments; Sign of scalar coupling constants

Indexed keywords

EID: 0001659344     PISSN: 10907807     EISSN: None     Source Type: Journal    
DOI: 10.1006/jmre.1998.1693     Document Type: Article

References (33)

1. D. S. Moore and S. D. Robinson, Hydrido complexes of the transition metals, Chem. Soc. Rev. 12, 415-452 (1983).
2. H. D. Kaesz and R. B. Saillant, Hydride complexes of the transition metals, Chem. Rev. 72, 231-281 (1972).
3. M. V. Baker and L. D. Field, Relative signs of P-P coupling constants in the NMR spectra of octahedral metal phosphine complexes. Inorg. Chem. 26, 2010-2011 (1987).
4. N. Bampos, L. D. Field, and B. A. Messerle, Measurement of heteronuclear coupling constants in organometallic complexes using high-resolution 2D NMR, Organometallics 12, 2529-2535 (1993).
5. 13C NMR of transition metal phosphine complexes, NMR Basic Princ. Prog. 16, 1-156 (1979).
6. C. J. Jameson, Spin-spin coupling, in "Multinuclear NMR" (J. Mason, Ed.), pp. 89-131, Plenum, New York (1987).
7. F. N. Tebbe, P. Meakin, J. P. Jesson, and E. L. Muetterties, Stereochemically nonrigid six-coordinate hydrides, J. Am. Chem. Soc. 92, 1068-1070 (1970).
8. 1H-detected multinuclear NMR experiments for the measurement of small heteronuclear coupling constants in transition metal complexes, J. Am. Chem. Soc. 119, 5425-5434 (1997).
9. M. H. Levitt, The signs of frequencies and phases in NMR, J. Magn. Reson. 126, 164-182 (1997).
10. 13C NMR experiments for the measurement of small heteronuclear coupling constants and isotopic shifts, J. Am. Chem. Soc. 118, 5096-5102 (1996).
11. N. Ahmad, J. J. Levison, S. D. Robinson, and M. F. Uttley, Triphenylphosphine complexes of transition metals. Complexes of ruthenium, osmium, rhodium, and iridium containing hydride carbonyl or nitrosyl ligands. Inorg. Synth. 15, 45-64 (1974).
12. + (R′ = Me, Et, iPr), J. Organomet. Chem. 366, 245-255 (1989).
13. 15N NMR study of gramicidin S in water and organic solvents, J. Am. Chem. Soc. 106, 1939-1941 (1984).
14. 15N spin-spin coupling constant: The flip angle effect, J. Magn. Reson. 50, 323-327 (1982).
15. 15N spin-spin coupling constants of 3-methyl- and 3,6-dimethyl-pyridazines, J. Chem. Soc., Perkin Trans. 2, 1533-1536 (1985).
16. 15N with side chain Hβ resonances in larger proteins, J. Magn. Reson. 95, 636-641 (1991).
17. 13C J couplings in a 20-kDa protein-peptide complex, J. Am. Chem. Soc. 114, 6923-6925 (1992).
18. A. Bax, G. W. Vuister, S. Grzesiek, F. Delaglio, A. C. Wang, R. Tschudin, and G. Zhu, Measurement of homo- and heteronuclear J couplings from quantitative J correlation, Methods Enzymol. 239, 79-105 (1994).
19. 15N-labeled proteins: Application to the photoactive yellow protein. J. Biomol. NMR 10, 301-306 (1997).
20. D. Marion, M. Ikura, R. Tschudin, and A. Bax, Rapid recording of 2D NMR spectra without phase cycling. Application to the study of hydrogen exchange in proteins, J. Magn. Reson. 85, 393-399 (1989).
21. 13C) coupling constants in linear spin systems, J. Magn. Reson. 124, 503-505 (1997).
22. A. Rexroth, P. Schmidt, S. Szalma, T. Geppert, H. Schwalbe, and C. Griesinger, New principle for the determination of coupling constants that largely suppress differential relaxation effects, J. Am. Chem. Soc. 117, 10389-10390 (1995).
23. C. Griesinger, O. W. Sørensen, and R. R. Ernst, Correlation of connected transitions by two-dimensional NMR spectroscopy, J. Chem. Phys. 64, 6837-6852 (1986).
24. 15N-labeled proteins, J. Am. Chem. Soc. 120, 7989-7990 (1998).
25. J. Jarvet and P. Allard, Phase-sensitive two-dimensional heteronuclear zero- and double-quantum-coherence spectroscopy, J. Magn. Reson. B 112, 240-244 (1996).
26. 15N spectra of proteins: Heteronuclear triple-resonance three-dimensional NMR spectroscopy. Application to calmodulin, Biochemistry 29, 4659-4667 (1990).
27. N. Tjandra and A. Bax, Direct measurement of distances and angles in biomolecules by NMR in a dilute liquid crystalline medium, Science 278, 1111-1114 (1997).
28. O. W. Sørensen, G. W. Eich, M. H. Levitt, G. Bodenhausen, and R. R. Ernst, Product operator formalism for the description of NMR pulse experiments, Prog. NMR Spectrosc. 16, 163-192 (1983).
29. M. S. Silver, R. I. Joseph, and D. I. Hoult, Highly selective π/2 and π pulse generation, J. Magn. Reson. 59, 347-351 (1984).
30. 13C]carbonyl decoupling, J. Am. Chem. Soc. 114, 2108-2112 (1992).
31. G. Bodenhausen and D. J. Ruben, Natural abundance nitrogen-15 NMR by enhanced heteronuclear spectroscopy, Chem. Phys. Lett. 69, 185-189 (1980).
32. G. Otting and K. Wüthrich, Efficient purging scheme for proton-detected heteronuclear two-dimensional NMR, J. Magn. Reson. 76, 569-574 (1988).
33. F. Löhr and H. Rüterjans, Detection of nitrogen-nitrogen J-couplings in proteins, J. Magn. Reson. 132, 130-137 (1998).