Skip to main content
SpringerLink
Log in

EPR Characterization of a Rigid Bis-TEMPO–Bis-Ketal for Dynamic Nuclear Polarization

  • Published:
Applied Magnetic Resonance Aims and scope Submit manuscript

Abstract

We have characterized the rigid binitroxide radical bis-TEMPO–bis-Ketal (bTbK) by continuous-wave (CW) and pulsed electron paramagnetic resonance (EPR) spectroscopy performed at X-band (9 GHz) and G-band (180 GHz) frequencies. bTbK has been successfully used for dynamic nuclear polarization (DNP)-enhanced solid-state nuclear magnetic resonance (SS-DNP) experiments based on the cross-effect, which involves two electrons and one nuclear spin, and gave very high signal enhancements. For a quantitative description of the polarization enhancements and their excitation frequency profile, a detailed information about the values and relative orientation of the magnetic hyperfine-, dipolar-, g-tensors and the exchange interaction of the two unpaired electron spins within the molecule is mandatory. We have determined these tensors and their relative orientation by CW-EPR spectra and pulsed electron double resonance experiments in frozen solution. The potential of using the cross-effect also for DNP in liquid solutions has been experimentally investigated by room-temperature high-field DNP experiments performed at 9.2 T.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8

Similar content being viewed by others

References

  1. K.M. Salikhov (ed.), Appl. Magn. Reson. 34, 213–544 (2008)

    Google Scholar 

  2. A.V. Kessenikh, V.I. Lushchikov, A.A. Manenkov, Y.V. Taran, Sov. Phys. Solid State 5, 321–329 (1963) [Fiz. Tverd. Tela 5, 443–451 (1963)]

    Google Scholar 

  3. A. Abragam, W.G. Proctor, Compt. Rend. 246, 2253–2256 (1958)

    Google Scholar 

  4. T. Maly, G. Debelouchina, V. Bajaj, K.-N. Hu, Ch.-G. Joo, M.L. Mak–Jurkauskas, J.R. Sirigiri, P. van der Wel, J. Herzfeld, R. Temkin, R.G. Griffin, J. Chem. Phys. 128(052211), 1–19 (2008)

    Google Scholar 

  5. C. Song, K. Hu, C. Joo, T. Swager, R.G. Griffin, J. Am. Chem. Soc. 128, 11385–11390 (2006)

    Article  Google Scholar 

  6. K.-N. Hu, C. Song, H.-H. Yu, T.M. Swager, R.G. Griffin, J. Chem. Phys 128(052302), 1–17 (2008)

    Google Scholar 

  7. V.N. Parmon, A.I. Kokorin, G.M. Zhidomirov, J. Struct. Chem. 18, 104–147 (1977) [Zh. Strukt. Khim. 18, 132–177 (1977)]

    Google Scholar 

  8. V.N. Parmon, A.I. Kokorin, G.M. Zhidomirov, J. Magn. Reson. 28, 339–349 (1977)

    Google Scholar 

  9. Y. Matsuki, T. Maly, O. Ouari, H. Karoui, F. Le Moigne, E. Rizzato, S. Lyubenova, J. Herzfeld, T. Prisner, P. Tordo, R.G. Griffin, Angew. Chem. Int. Ed. 121, 5096–5100 (2009)

    Google Scholar 

  10. M.M. Hertel, V.P. Denysenkov, M. Bennati, T.F. Prisner, Magn. Reson. Chem 43, S248–S255 (2005)

    Article  Google Scholar 

  11. B. Epel, I. Gromov, S. Stoll, A. Schweiger, D. Goldfarb, Conc. Magn. Reson. 26B, 36–45 (2005)

    Article  Google Scholar 

  12. J. Low, Phys. Rev. 105, 793–800 (1957)

    Article  ADS  Google Scholar 

  13. O. Burghaus, M. Plato, M. Rohrer, K. Möbius, F. MacMillan, W. Lubitz, J. Phys. Chem. 97, 7639–7647 (1993)

    Article  Google Scholar 

  14. V.P. Denysenkov, M.J. Prandolini, A. Krahn, M. Gafurov, B. Endeward, T.F. Prisner, Appl. Magn. Reson. 34, 289–299 (2008)

    Article  Google Scholar 

  15. S. Stoll, A. Schweiger, J. Magn. Reson. 178, 42–55 (2006)

    Article  ADS  Google Scholar 

  16. D. Margraf, B.E. Bode, A. Marko, O. Schiemann, T.F. Prisner, Mol. Phys. 105, 2153–2160 (2007)

    Article  ADS  Google Scholar 

  17. M.A. Ondar, A.A. Dubinskii, O.Ya. Grinberg, I.A. Grigor’ev, L.B. Volodarskii, Ya.S. Lebedev, J. Struct. Chem. 22, 525–531 (1981) [Zh. Strukt. Khim. 22, 59–66 (1981)]

    Google Scholar 

  18. V.I. Gulin, S.A. Dikanov, Yu.D. Tsvetkov, Chem. Phys. Lett. 170, 211–216 (1990)

    Article  ADS  Google Scholar 

  19. A.W. Overhauser, Phys. Rev. 92, 411–415 (1953)

    Article  MATH  ADS  Google Scholar 

  20. J. Potenza, Adv. Mol. Relax. Proc. 4, 229–354 (1972)

    Article  Google Scholar 

  21. M.J. Prandolini, V.P. Denysenkov, M. Gafurov, B. Endeward, T.F. Prisner, J. Am. Chem. Soc. 131, 6090–6092 (2009)

    Article  Google Scholar 

  22. M.J. Prandolini, V. Denysenkov, M. Gafurov, S. Lyubenova, B. Endeward, M. Bennati, T. Prisner, Appl. Magn. Reson. 34, 399–407 (2008)

    Article  Google Scholar 

Download references

Acknowledgments

We want to thank Burkhard Endeward for experimental support, Deniz Sezer, Mark Prandolini for many fruitful discussions and Dominik Margraf for comments on this paper. This project is funded by the European Commission in the design study project BIO-DNP.

Author information

Authors and Affiliations

  1. Institute of Physical and Theoretical Chemistry, Center of Biomolecular Magnetic Resonance, Goethe University, Max-von-Laue Str.7, 60438, Frankfurt am Main, Germany

    Marat Gafurov, Sevdalina Lyubenova, Vasyl Denysenkov & Thomas Prisner

  2. Provence Chemistry Laboratory, UMR 6264, Provence University, CNRS, 13397, Marseilles Cedex 20, France

    Olivier Ouari, Hakim Karoui, François Le Moigne & Paul Tordo

Authors
  1. Marat Gafurov
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Sevdalina Lyubenova
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Vasyl Denysenkov
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Olivier Ouari
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Hakim Karoui
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. François Le Moigne
    View author publications

    You can also search for this author in PubMed Google Scholar

  7. Paul Tordo
    View author publications

    You can also search for this author in PubMed Google Scholar

  8. Thomas Prisner
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Thomas Prisner.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Gafurov, M., Lyubenova, S., Denysenkov, V. et al. EPR Characterization of a Rigid Bis-TEMPO–Bis-Ketal for Dynamic Nuclear Polarization. Appl Magn Reson 37, 505–514 (2010). https://doi.org/10.1007/s00723-009-0069-4

Download citation

  • Received:

  • Revised:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00723-009-0069-4

Keywords

Search

Navigation