Carbon-13 solid-state NMR studies on synthetic model compounds of [4Fe-4S] clusters in the 2+ state

Journal of Physical Chemistry A

Volumn 104, Issue 44, 2000, Pages 9990-10000

  Crozet, Marielle ^a,c   Chaussade, Marc ^a,d   Bardet, Michel ^a   Emsley, Lyndon ^b   Lamotte, Bernard ^a   Mouesca, Jean Marie ^a  

^a CEA GRENOBLE   (France)

^b UNIVERSITÉ DE LYON   (France)

^c Service d'Etude et de Modélisation des Procédés   (France)

^d Rhodia Europe   (France)

Author keywords

[No Author keywords available]

Indexed keywords

ANTIFERROMAGNETIC MATERIALS; CARBON; CRYSTAL STRUCTURE; FLUORINE COMPOUNDS; MAGNETIC RELAXATION; MAGNETIC SUSCEPTIBILITY; PARAMAGNETISM; PROTEINS; RADIOISOTOPES; SULFUR COMPOUNDS; THERMAL EFFECTS;

ANTIFERROMAGNETIC EXCHANGE COUPLINGS;

PHYSICAL CHEMISTRY;

EID: 0034323364     PISSN: 10895639     EISSN: None     Source Type: Journal    
DOI: 10.1021/jp002005o     Document Type: Article

References (70)

1. Chacko, V. P.; Ganapathy, S.; Bryant, R. G. J. Am. Chem. Soc. 1983, 105 (5), 5491-5492.
2. Ganapathy, S.; Chacko, V. P.; Bryant, R. G.; Etter, M. C. J. Am. Chem. Soc. 1986, 108, 3159-3165.
3. Ganapathy, S.; Bryant, R. G. J. Magn. Reson. 1986, 70, 149-152.
4. Campbell, G. C.; Haw, J. F. Inorg. Chem. 1988, 27, 3706-3709.
5. Campbell, G. C.; Reibenspies, J. H.; Haw, J. F. Inorg. Chem. 1991, 30, 171-176.
6. Cheetham, A. K.; Dobson, C. M.; Grey, C. P.; Jakeman, R. J. B. Nature 1987, 328, 706-707.
7. Grey, C. P.; Dobson, C. M.; Cheetham, A. K.; Jakeman, R. J. B. J. Am. Chem. Soc. 1989, 111, 505-511.
8. Grey, C. P.; Smith, M. E.; Cheetham, A. K.; Dobson, C. M.; Dupree, R. J. Am. Chem. Soc. 1990, 112, 4670-4675.
9. Clayton, A. N.; Dobson, C. M.; Grey, C. P. J. Chem. Soc., Chem. Commun. 1990, 72-74.
10. Brough, A. R.; Grey, C. P.; Dobson, C. M. J. Am. Chem. Soc. 1993, 115(5), 7318-7327.
11. Stoll, M. E.; Majors, T. J. Phys. Rev. 1981, B24, 2859-2862.
12. Nayeem, A.; Yesinowski, J. P. J. Chem. Phys. 1988, 89, 46004608.
13. Liu, K.; Ryan, D.; Nakanishi, K.; McDermott, A. J. Am. Chem. Soc. 1995, 117, 6897-6906.
14. Spaniol, T. P.; Kubo, A.; Terao, T. J. Chem. Phys. 1997, 106, 5393-5405.
15. Hentsch, F.; Heimle, M.; Kongeter, D.; Mehring, M. Phys. Rev. 1988, B37, 7205-7208.
16. Michel, P.; Moradpour, A.; Penven, P.; Firlej, L.; Bemier, P.; Levy, B.; Ravy, S.; Zahab, A. J. Am. Chem. Soc. 1990, 112, 8285-8292.
17. Mustarelli, P.; Massarotti, V.; Bini, M.; Capsoni, D. Phys. Rev. 1997, B55, 12018-12024.
18. Schwerk, U.; Michel, D.; Pmski, M. J. Magn. Reson. 1996, A119, 157-164.
19. Kubo, A.; Spaniol, T. P.; Terao, T. J. Magn. Reson. 1998, 133, 330-340.
20. Garroway, A. N.; VanderHart, D. L.; Earl, W. L. Philos. Trans. R. Soc. London 1981, A299, 609-628.
21. VanderHart, D. L.; Earl, W. L.; Garroway, A. N. J. Magn. Reson. 1981, 44, 361-401.
22. Alla, M.; Lippmaa, E. Chem. Phys. Lett. 1982, 87, 30-33.
23. Johnson, M. K. In Encyclopedia of Inorganic Chemistry; King, R. B., Ed.; Wiley: New York, 1994; Vol. 4, pp 1896-1915.
24. Beinert, H.; Holm, R. H.; Münck, E. Science 1997, 277, 653659.
25. Lamotte, B.; Mouesca, J.-M. C. R. Acad. Sei. Paris 1997,324, 1 IT132.
26. Bertini, I.; Ciurli, S.; Luchinat, C. Struct. Bonding 1995, 83, 1 -54.
27. Bertini, I.; Luchinat, C. NMR of Paramagnetic Substances', Elsevier: Amsterdam, 1996; Vol. 150.
28. Wang, P. L.; Donaire, A.; Zhou, Z. H.; Adams, M. W. W.; LaMar, G. N. Biochemistry 1996, 35, 11319-11328.
29. Calzolai, L.; Gorst, C. M.; Bren, K. L.; Zhou, Z. H.; Adams, M. W. W.; LaMar, G. N. J. Am. Chem. Soc. 1997, 119, 9341-9350.
30. Huber, J. G.; Moulis, J.-M.; Gaillard, J. Biochemistry 1996, 35, 12705-12711.
31. Kyritsis, P.; Huber, J. G.; Quinkal, I.; Gaillard, J.; Moulis; J.-M. Biochemistry 1997, 36, 7839-7846.
32. Laskowski, E. J.; Frankel, R. B.; Gillum, W. O.; Papaefihymiou, G. C.; Renaud, J.; Ibers, J. A.; Holm, R. H. J. Am. Chem. Soc. 1978, 100, 5322-5337.
33. Papaefthymiou, G. C.; Laskowski, E. J.; Frota-Pessóa, S.; Frankel, R. B.; Holm, R. H. Inorg. Chem. 1982, 21, 1723-1728.
34. Mascharak, P. K.; Hagen, K. S.; Spence, J. T.; Holm, R. H. Inorg. Chim. Acta 1983, 80, 157-170.
35. Mouesca, J.-M.; Rius, G.; Lamotte, B. J. Am. Chem. Soc. 1993, 115 (5), 4714-4731.
36. Christou, G.; Gamer, C. D. J. Chem. Soc., Dalton Trans. 1979, 1093.
37. Bielecki, A.; Burum, D. P. J. Magn. Reson. 1995, A116, 215-220.
38. Gann, S. L.; Baltisberger, J. H.; Pines, A. Chem. Phys. Lett. 1993, 270, 405-410.
39. Hu, J. Z.; Alderman, D. W.; Ye, C.; Pugmire, R. J.; Grant, D. M. J. Magn. Reson. 1993, A105, 82.
40. Hodgkinson, P.; Emsley, L. J. Chem. Phys. 1997, 107, 4808.
41. Clayton, A. N.; Dobson, C. M.; Grey, C. P. J. Chem. Soc., Chem. Commwn. 1990, 72-74.
42. Averill, B. A.; Herskovitz, T.; Holm, R. H.; Ibers, J. A. J. Am. Chem. Soc. 1973, 95, 3523-3534.
43. Bominaar, E. L.; Hu, Z.; Münck, E.; Girerd, J.-J.; Borshch, S. A. J. Am. Chem. Soc. 1995, 117, 6976-6989.
44. Herzfeld, J.; Berger, A. E. J. Chem. Phys. 1980, 73, 6021.
45. Hodgkinson, P.; Emsley, L. Prog. NMR Spectrosc. 2000, 36, 201.
46. In II and III, we have tried to determine with X-rays toward the low temperatures whether these rotations of the t-Bu groups and the movements of the methyl carbons of the counterions become blocked. In effect, at 90 K, the two compounds present a new phase and a different structure of lower symmetry than that observed at 300 K. This structure is fairly complicated (probably triclinic but with α, β, and γ angles very close to 90°), and it probably contains a large number of inequivalent molecules. We have been unable to solve it without ambiguity. The change from this low-symmetry phase to the phase described at room temperature occurs at ∼120-130 K for II and ∼150-160 K for III. Therefore, these X-ray observations confirm that the movements-in the solid state and especially the rotations of the t-Bu groups of the thiolate ligands are operative in the whole range of temperatures where we perform these solid-state NMR experiments.
47. Bencini, A.; Gatteschi, D. EPR of Exchange Coupled Systems; Springer-Verlag: Berlin, 1990.
48. Band, L.; Bertini, I.; Luchinat, C. Structure and Bonding; Sprinaer-Verlag: Berlin, 1990; Vol. 72, pp 113-136.
49. Noodleman, L.; Pens, C. Y.; Case, D. A.; Mouesca, J.-M. Coord. Chem. Rev. 1995, 144, 199-244.
50. Middleton, P.; Dickson, D. P. E.; Johnson, C. E.; Rush, J. D. Eur. J. Biochem. 1978, 88, 135.
51. Middleton, P.; Dickson, D. P. E.; Johnson, C. E.; Rush, J. D. Eur. J. Biochem. 1980, 104, 289-296.
52. Papaeflhymiou, V.; Girerd, J.-J.; Moura, I.; Moura, J. J. G.; Münck, E. J. Am. Chem. Soc. 1987, 109, 4703.
53. 1+/3+ systems.
54. Bertini, I.; Turano, P.; Vila, A. J. Chem. Rev. 1993, 93, 2833-2932.
55. Blondin, G.; Girerd, J.-J. JBIC 1996, J, 170-172.
56. Kröckel, M.; Grodzicki, M.; Papaefthymiou, V.; Trautwein, A. X.; Kostikas, A. JBIC 1996, 1, 173-176.
57. Noodleman, L.; Case, D. A.; Mouesca, J.-M.; Lamotte, B. JBIC 1996, 1, 177-182.
58. Bertini, I.; Luchinat, C. JBIC 1996, 1, 183-185.
59. Belinsky, M. I. JBIC 1996, 1, 186-188.
60. Borshch, S. A.; Bominaar, E. L.; Blondin, G.; Girerd, J.-J. J. Am. Chem. Soc. 1993, 115, 5155-5168.
61. Bominaar, E. L.; Borshch, S. A.; Girerd, J.-J. J. Am. Chem. Soc. 1994, 116, 5362-5372.
62. 13C lines will be published in a separate note.
63. 13C chemical shift measured for the β-caibon of reduced cysteine is between 27 and 28 ppm, depending on the nearestneighbor amino acid (Wishart et al. J. Biomol. NMR, 1995, 5, 67-81), whereas we measured it to be 32 ppm in the solid state. In the case of the t-Bu thiolate sodium salt, we measured 49 and 36 ppm for the quaternary and methyl carbon nuclei, respectively.
64. Le Pape, L.; Lamotte, B.; Mouesca, J.-M.; Rius, G. J. Am. Chem. Soc. 1997, 119, 9771-9781.
65. Mouesca, J.-M.; Noodleman, L.; Case, D. A.; Lamotte, B. Inorg. Chem. 1995, 34, 4347-4359.
66. 2 carbon p orbital pointing toward the thiolate sulfur bears some spin density leading to a non-negligible anisotropy contribution, we took this term explicitly into account, evaluating its relative weight from density functional calculations, in a manner described elsewhere. This is in contrast to the proton case, whose s Orbitals do not allow for some local source of dipolar anisotropy. Results to be published.
67. Bertini, I.; Capozzi, F.; Luchinat, C.; Piccioli, M.; Vila, A. J. J. Am. Chem. Soc. 1994, 116, 651-660.
68. Noodleman, L. Inorg. Chem. 1988, 27, 3677-3679.
69. Jordanov, J.; Roth, E. K. H.; Fries, P. H.; Noodleman, L. Inorg. Chem. 1990, 29, 4288-4292.
70. Banci, L.; Bertini, I.; Briganti, F. Luchinat, C.; Scozzafava, A.; Vincens Oliver, M. Inorg. Chem. 1991, 30, 4517-4524.