13C Direct detected experiments: Optimization for paramagnetic signals

Journal of Magnetic Resonance

Volumn 174, Issue 1, 2005, Pages 125-132

  Bertini, Ivano ^a   Jiménez, Beatriz ^a   Piccioli, Mario ^a  

^a UNIVERSITY OF FLORENCE   (Italy)

Author keywords

(CO)CACO; 13C Direct detection; CACO; Hyperfine interaction; Paramagnetic NMR

Indexed keywords

CALCIUM; NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY; OPTIMIZATION; PARAMAGNETISM; PH EFFECTS; POSITIVE IONS; PROTEINS; QUANTUM THEORY;

(CO)CACO; 13C DIRECT DETECTION; CACO; HYPERFINE INTERACTIONS; PARAMAGNETIC NMR;

SIGNAL DETECTION;

CALBINDIN; CARBON;

ANIMAL; ARTICLE; CATTLE; CHEMISTRY; METHODOLOGY; NUCLEAR MAGNETIC RESONANCE;

ANIMALS; CALCIUM-BINDING PROTEIN, VITAMIN D-DEPENDENT; CARBON ISOTOPES; CATTLE; NUCLEAR MAGNETIC RESONANCE, BIOMOLECULAR;

EID: 15844421620     PISSN: 10907807     EISSN: None     Source Type: Journal    
DOI: 10.1016/j.jmr.2005.01.014     Document Type: Article

References (69)

1. I. Bertini, C. Luchinat, and M. Piccioli Paramagnetic probes in metalloproteins. Turning limitations into advantages Methods Enzymol. 339 2001 314 340
2. M. Ubbink, J.A.R. Worrall, G.W. Canters, E.J.J. Groenen, and M. Huber Paramagnetic resonance of biological metal centers Annu. Rev. Biophys. Biomol. Struct. 31 2002 393 422
3. A.F. Frederick, L.E. Kay, and J.H. Prestegard Localization of divalent ion sites in acyl carrier protein using relaxation perturbed 2D NMR FEBS Lett. 238 1988 43 48
4. A.M. Petros, L. Mueller, and K.D. Kopple NMR identification of protein surfaces using paramagnetic probes Biochemistry 29 1990 10041 10048
5. M. Scarselli, A. Bernini, C. Segoni, H. Molinari, G. Esposito, A.M. Lesk, F. Laschi, P. Temussi, and N. Niccolai Tendamistad surface accessibility to the TEMPOL paramagnetic probe J. Biomol. NMR 15 1999 125 133
6. S. Vathyam, R.A. Byrd, and A.F. Miller Mapping the effects of metal ion reduction and substrate analog binding to Fe-superoxide dismutase by NMR spectroscopy Magn. Reson. Chem. 38 2000 536 542
7. L.W. Donaldson, N.R. Skrynnikov, W.-Y. Choy, D.R. Muhandiram, B. Sarkar, J.D. Forman-Kay, and L.E. Kay Structural characterization of proteins with an attached ATCUN motif by paramagnetic relaxation enhancement NMR spectroscopy J. Am. Chem. Soc. 123 2001 9843 9847
8. V. Gaponenko, S.P. Sarma, A.S. Altieri, D.A. Horita, J. Li, and R.A. Byrd Improving the accuracy of NMR structures of large proteins using pseudocontact shifts as long/range restraints J. Biomol. NMR 28 2004 205 212
9. J. Wöhnert, K.J. Franz, M. Nitz, B. Imperiali, and H. Schwalbe Protein alignment by a coexpressed lanthanide-binding tag for the measurement of residual dipolar couplings J. Am. Chem. Soc. 125 2003 13338 13339
10. T. Ikegami, L. Verdier, P. Sakhaii, S. Grimme, P. Pescatore, K. Saxena, K.M. Fiebig, and C. Griesinger Novel techniques for weak alignment of proteins in solution using chemical tags coordinating lanthanide ions J. Biomol. NMR 29 2004 339 349
11. G. Pintacuda, A. Moshref, A. Leonchiks, A. Sharipo, and G. Otting Site-specific labelling with a metal chelator for protein-structure refinement J. Biomol. NMR 29 2004 351 361
12. J.C. Hus, D. Marion, and M. Blackledge De novo determination of protein structure by NMR using orientational and long-range order restraints J. Mol. Biol. 298 2000 927 936
13. 9k J. Biomol. NMR 21 2001 85 98
14. 9k Biochemistry 42 2003 13066 13073
15. F. Kateb, and M. Piccioli New routes to the detection of relaxation allowed coherence transfer in paramagnetic molecules J. Am. Chem. Soc. 125 2003 14978 14979
16. 15N labeled paramagnetic proteins J. Am. Chem. Soc. 126 2004 2963 2970
17. A. Eletsky, O. Moreira, H. Kovacs, and K. Pervushin A novel strategy for the assignment of side-chain resonances in completely deuterated large proteins using (13) C spectroscopy J. Biomol. NMR 26 2003 167 179
18. K. Hu, A. Eletsky, and K. Pervushin Backbone resonance assignment in large protonated proteins using a combination of new 3D TROSY-HN(CA)HA, 4D TROSY-HACANH and 13C detected HACACO experiments J. Biomol. NMR 26 2003 69 77
19. 13C NOESY: An attractive alternative to study large macromolecules J. Am. Chem. Soc. 126 2004 464 465
20. I. Bertini, L. Duma, I.C. Felli, M. Fey, C. Luchinat, R. Pierattelli, and P. Vasos A heteronuclear direct detection NMR experiment for protein backbone assignment Angew. Chem. Int. Ed. 43 2004 2257 2259
21. I. Bertini, Y.-M. Lee, C. Luchinat, M. Piccioli, and L. Poggi Locating the metal ion in calcium-binding proteins by using cerium(III) as a probe Chem. Bio Chem. 2 2001 550 558
22. M. Piccioli, and L. Poggi Tailored HCCH-TOCSY experiment for resonance assignment in the proximity of a paramagnetic center J. Magn. Reson. 155 2002 236 243
23. U. Kolczak, J. Salgado, G. Siegal, M. Saraste, and G.W. Canters Paramagnetic NMR studies of blue and purple copper proteins Biospectroscopy 5 1999 S19 S32
24. T.E. Machonkin, W.M. Westler, and J.L. Markley 13C-13C 2D NMR: A novel strategy for the study of paramagnetic proteins with slow electronic relaxation times J. Am. Chem. Soc. 124 2002 3204 3205
25. 2+-containing acireductone dioxygenase J. Am. Chem. Soc. 124 2002 9054 9055
26. 13C direct detection experiments on the paramagnetic oxidized monomeric copper, zinc superoxide dismutase J. Am. Chem. Soc. 125 2003 16423 16429
27. E. Babini, I. Bertini, F. Capozzi, I.C. Felli, M. Lelli, and C. Luchinat Direct carbon detection in paramagnetic metalloproteins to further exploit pseudocontact shift restraints J. Am. Chem. Soc. 126 2004 10496 10497
28. 13C NMR spectrosocpic studies suggest the active participation of the heme in macrocycle hydroxylation J. Am. Chem. Soc. 125 2003 11842 11852
29. T.-M. Chan, and J.L. Markley Nuclear magnetic resonance studies of two-iron-two-sulfur ferredoxins. 5. Hyperfine-shifted peaks in proton and carbon-13 spectra Biochemistry 22 1983 6008
30. B.-H. Oh, W.M. Westler, P. Darba, and J.L. Markley Protein carbon-13 spin systems by a single two-dimensional nuclear magnetic resonance experiment Science 240 1988 908 911
31. 13C NMR study of labeled vinyl groups in paramagnetic myoglobin derivatives Biochim. Biophys. Acta 912 1987 220 229
32. J. Mispelter, M. Momenteau, and J.M. Lhoste Heteronuclear magnetic resonance: Application to biological and related paramagnetic molecules L.J. Berliner J. Reuben NMR of paramagnetic molecules 1993 Plenum Press New York
33. 13C and proton NMR studies of horse ferricytochrome c FEBS Lett. 194 1986 73 77
34. Z. Serber, C. Richter, D. Moskau, J.-M. Boehlen, T. Gerfin, D. Marek, M. Haeberli, L. Baselgia, F. Laukien, A.S. Stern, J.C. Hoch, and V. Doetsch New carbon-detected protein NMR experiments using cryoprobes J. Am. Chem. Soc. 122 2000 3554 3555
35. 13C residual dipolar coupling in uniformly deuterated proteins J. Am. Chem. Soc. 126 2004 2414 2420
36. 9k Biochemistry 26 1987 6723 6735
37. 9k J. Mol. Biol. 220 1991 173 189
38. M. Allegrozzi, I. Bertini, M.B.L. Janik, Y.-M. Lee, G. Liu, and C. Luchinat Lanthanide induced pseudocontact shifts for solution structure refinements of macromolecules in shells up to 40 A from the metal ion J. Am. Chem. Soc. 122 2000 4154 4161
39. 9k J. Biomol. NMR 23 2002 115 125
40. 3+ substituted form Biochemistry 41 2002 5104 5111
41. 9k observed by X-ray crystallography J. Mol. Biol. 223 1992 601 606
42. W. Bermel, I. Bertini, L. Duma, L. Emsley, I.C. Felli, R. Pierattelli, P. Vasos, Towards complete assignment of heteronuclear protein resonances by protonless NMR, Angew. Chem. Int. Ed. (2005) in press
43. P. Brodin, T. Grundstrom, T. Hofmann, T. Drakenberg, E. Thulin, and S. Forsén Expression of bovine intestinal calcium binding protein from a synthetic gene in Escherichia coli and characterization of the product Biochemistry 25 1986 5371 5377
44. C. Johansson, P. Brodin, T. Grundstrom, E. Thulin, S. Forsén, and T. Drakenberg Biophysical studies of engineered mutant proteins based on calbindin D9K modified in the pseudo EF-hand Eur. J. Biochem. 187 1990 455 460
45. 9k: Direct evidence from two-dimensional 1H NMR spectroscopy Proc. Natl. Acad. Sci. USA 86 1989 2195 2198
46. 9k Biochemistry 37 1998 2586 2595
47. L. Emsley, and G. Bodenhausen Optimization of shaped selective pulses for NMR using a quaternion description of their overall propagators J. Magn. Reson. 97 1992 135 148
48. D. Marion, and K. Wüthrich Application of phase sensitive correlated spectroscopy (COSY) for measurements of proton-proton spin-spin coupling constants in proteins Biochem. Biophys. Res. Commun. 113 1983 967 974
49. A.J. Shaka, P.B. Barker, and R. Freeman Computer-optimized decoupling scheme for wideband applications and low-level operation J. Magn. Reson. 64 1985 547 552
50. A.J. Shaka, J. Keeler, and R. Freeman Evaluation of a new broadband decoupling sequence: WALTZ-16 J. Magn. Reson. 53 1983 313 340
51. I. Bertini, C. Luchinat, R. Macinai, M. Piccioli, A. Scozzafava, and M.S. Viezzoli Paramagnetic metal centers in proteins can be investigated through heterocorrelated NMR spectroscopy J. Magn. Reson. Ser. B 104 1994 95 98
52. I. Bertini, C. Luchinat, and D. Tarchi Are true scalar proton-proton connectivities ever measured in COSY spectra of paramagnetic macromolecules? Chem. Phys. Lett. 203 1993 445 449
53. P.K. Madhu, P.K. Mandal, and N. Muller Cross-correlation effects involving Curie spin relaxation in methyl groups J. Magn. Reson. 155 2002 29 38
54. 1H NMR of horse ferricytochrome c J. Magn. Reson. Ser. A 104 1993 197 202
55. I. Bertini, C. Luchinat, M. Piccioli, and D. Tarchi COSY spectra of paramagnetic macromolecules, observability, scalar effects, cross correlation effects, relaxation allowed coherence transfer Concepts Magn. Reson. 6 1994 307 335
56. I. Gelis, N. Katsaros, C. Luchinat, M. Piccioli, and L. Poggi A simple protocol to study blue copper proteins by NMR Eur. J. Biochem. 270 2003 600 609
57. L. Müller Sensitivity enhanced detection of weak nuclei using heteronuclear multiple quantum coherence J. Am. Chem. Soc. 101 1979 4481 4484
58. G. Bodenhausen, and D.J. Ruben Natural abundance nitrogen-15 NMR by enhanced heteronuclear spectroscopy Chem. Phys. Lett. 69 1980 185 188
59. J.L. Markley, A. Bax, Y. Arata, C.W. Hilbers, R. Kaptein, B.D. Sykes, P.E. Wright, and K. Wüthrich Recommendations for the presentation of NMR structures of proteins and nucleic acids. IUPAC-IUPMB-IUPAB inter-union task group on the standardization of data bases of protein and nucleic acid structures determined by NMR spectroscopy Eur. J. Biochem. 256 1998 1 15
60. J.-M. Boehlen, and G. Bodenhausen Experimental aspects of chirp NMR spectroscopy J. Magn. Reson. Ser. A 102 1993 293 301
61. M. Zweckstetter, and T.A. Holak An adiabatic multiple spin-echo pulse sequence: removal of systematic errors due to pulse imperfections and off-resonance effects J. Magn. Reson. 133 1998 134 147
62. M. Ottiger, F. Delaglio, and A. Bax Measurement of J and dipolar couplings from simplified two-dimensional NMR spectra J. Magn. Reson. 131 1998 373 378
63. M.H. Lerche, A. Meissner, F.M. Poulsen, and O.W. Sørensen Pulse sequences for measurement of one-bond (15)N-(1)H coupling constants in the protein backbone J. Magn. Reson. 140 1999 259 263
64. 13C spin-diffusion J. Biomol. NMR 30 2004 245 251
65. R. Riek, G. Wider, K. Pervushin, and K. Wuthrich Polarization transfer by cross-correlated relaxation in solution nmr with very large molecules Proc. Natl. Acad. Sci. USA 96 1999 4918 4923
66. S. Grzesiek, and A. Bax Improved 3D triple-resonance NMR techniques applied to a 31 kDa protein J. Magn. Reson. 96 1992 432 440
67. K. Pervushin, and A. Eletsky A new strategy for backbone resonance assignment in large proteins using a MQ-HACACO experiment J. Biomol. NMR 25 2003 147 152
68. α splitting in protein NMR spectra by deconvolution with maximum entropy reconstruction J. Am. Chem. Soc. 125 2003 2382 2383
69. 13CO chemical shift anisotropy relaxation mechanisms by multiple quantum NMR J. Am. Chem. Soc. 121 1999 9165 9170