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Spectral density mapping at multiple magnetic fields suitable for (13)C NMR relaxation studies

P. Kadeřávek, V. Zapletal, R. Fiala, P. Srb, P. Padrta, JP. Přecechtělová, M. Šoltésová, J. Kowalewski, G. Widmalm, J. Chmelík, V. Sklenář, L. Žídek,

. 2016 ; 266 (-) : 23-40. [pub] 20160308

Language English Country United States

Document type Journal Article, Research Support, Non-U.S. Gov't

Persistent link   https://www.medvik.cz/link/bmc18011277

Standard spectral density mapping protocols, well suited for the analysis of (15)N relaxation rates, introduce significant systematic errors when applied to (13)C relaxation data, especially if the dynamics is dominated by motions with short correlation times (small molecules, dynamic residues of macromolecules). A possibility to improve the accuracy by employing cross-correlated relaxation rates and on measurements taken at several magnetic fields has been examined. A suite of protocols for analyzing such data has been developed and their performance tested. Applicability of the proposed protocols is documented in two case studies, spectral density mapping of a uniformly labeled RNA hairpin and of a selectively labeled disaccharide exhibiting highly anisotropic tumbling. Combination of auto- and cross-correlated relaxation data acquired at three magnetic fields was applied in the former case in order to separate effects of fast motions and conformational or chemical exchange. An approach using auto-correlated relaxation rates acquired at five magnetic fields, applicable to anisotropically moving molecules, was used in the latter case. The results were compared with a more advanced analysis of data obtained by interpolation of auto-correlated relaxation rates measured at seven magnetic fields, and with the spectral density mapping of cross-correlated relaxation rates. The results showed that sufficiently accurate values of auto- and cross-correlated spectral density functions at zero and (13)C frequencies can be obtained from data acquired at three magnetic fields for uniformly (13)C-labeled molecules with a moderate anisotropy of the rotational diffusion tensor. Analysis of auto-correlated relaxation rates at five magnetic fields represents an alternative for molecules undergoing highly anisotropic motions.

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$a Kadeřávek, Pavel $u National Centre for Biomolecular Research, Faculty of Science, Masaryk University, Kamenice 5, CZ-625 00 Brno, Czech Republic; Central European Institute of Technology, Masaryk University, Kamenice 5, CZ-625 00 Brno, Czech Republic; Institute of Biophysics of Academy of Sciences of the Czech Republic, Královopolská 135, CZ-612 65 Brno, Czech Republic. Electronic address: kada@chemi.muni.cz.
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$a Spectral density mapping at multiple magnetic fields suitable for (13)C NMR relaxation studies / $c P. Kadeřávek, V. Zapletal, R. Fiala, P. Srb, P. Padrta, JP. Přecechtělová, M. Šoltésová, J. Kowalewski, G. Widmalm, J. Chmelík, V. Sklenář, L. Žídek,
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$a Standard spectral density mapping protocols, well suited for the analysis of (15)N relaxation rates, introduce significant systematic errors when applied to (13)C relaxation data, especially if the dynamics is dominated by motions with short correlation times (small molecules, dynamic residues of macromolecules). A possibility to improve the accuracy by employing cross-correlated relaxation rates and on measurements taken at several magnetic fields has been examined. A suite of protocols for analyzing such data has been developed and their performance tested. Applicability of the proposed protocols is documented in two case studies, spectral density mapping of a uniformly labeled RNA hairpin and of a selectively labeled disaccharide exhibiting highly anisotropic tumbling. Combination of auto- and cross-correlated relaxation data acquired at three magnetic fields was applied in the former case in order to separate effects of fast motions and conformational or chemical exchange. An approach using auto-correlated relaxation rates acquired at five magnetic fields, applicable to anisotropically moving molecules, was used in the latter case. The results were compared with a more advanced analysis of data obtained by interpolation of auto-correlated relaxation rates measured at seven magnetic fields, and with the spectral density mapping of cross-correlated relaxation rates. The results showed that sufficiently accurate values of auto- and cross-correlated spectral density functions at zero and (13)C frequencies can be obtained from data acquired at three magnetic fields for uniformly (13)C-labeled molecules with a moderate anisotropy of the rotational diffusion tensor. Analysis of auto-correlated relaxation rates at five magnetic fields represents an alternative for molecules undergoing highly anisotropic motions.
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$a Zapletal, Vojtěch $u National Centre for Biomolecular Research, Faculty of Science, Masaryk University, Kamenice 5, CZ-625 00 Brno, Czech Republic; Central European Institute of Technology, Masaryk University, Kamenice 5, CZ-625 00 Brno, Czech Republic. Electronic address: vojtis@mail.muni.cz.
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$a Fiala, Radovan $u National Centre for Biomolecular Research, Faculty of Science, Masaryk University, Kamenice 5, CZ-625 00 Brno, Czech Republic; Central European Institute of Technology, Masaryk University, Kamenice 5, CZ-625 00 Brno, Czech Republic. Electronic address: fiala@chemi.muni.cz.
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$a Srb, Pavel $u Central European Institute of Technology, Masaryk University, Kamenice 5, CZ-625 00 Brno, Czech Republic. Electronic address: pavel.srb@gmail.com.
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$a Padrta, Petr $u Central European Institute of Technology, Masaryk University, Kamenice 5, CZ-625 00 Brno, Czech Republic. Electronic address: padrta@chemi.muni.cz.
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$a Přecechtělová, Jana Pavlíková $u Central European Institute of Technology, Masaryk University, Kamenice 5, CZ-625 00 Brno, Czech Republic. Electronic address: j.precechtelova@gmail.com.
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$a Šoltésová, Mária $u Faculty of Mathematics and Physics, Charles University, V Holešovičkách 2, CZ-180 00 Prague, Czech Republic. Electronic address: maria.soltesova@gmail.com.
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$a Kowalewski, Jozef $u Department of Materials and Environmental Chemistry, Arrhenius Laboratory, Stockholm University, S-106 91 Stockholm, Sweden. Electronic address: jozef.kowalewski@mmk.su.se.
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$a Widmalm, Göran $u Department of Organic Chemistry, Arrhenius Laboratory, Stockholm University, S-106 91 Stockholm, Sweden. Electronic address: gw@organ.su.se.
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$a Chmelík, Josef $u Institute of Microbiology, Academy of Sciences of the Czech Republic, Vídeňská 1083, CZ-142 00 Prague 4 - Krč, Czech Republic. Electronic address: chmelik@biomed.cas.cz.
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$a Sklenář, Vladimír $u National Centre for Biomolecular Research, Faculty of Science, Masaryk University, Kamenice 5, CZ-625 00 Brno, Czech Republic; Central European Institute of Technology, Masaryk University, Kamenice 5, CZ-625 00 Brno, Czech Republic. Electronic address: sklenar@chemi.muni.cz.
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$a Žídek, Lukáš $u National Centre for Biomolecular Research, Faculty of Science, Masaryk University, Kamenice 5, CZ-625 00 Brno, Czech Republic; Central European Institute of Technology, Masaryk University, Kamenice 5, CZ-625 00 Brno, Czech Republic. Electronic address: lzidek@chemi.muni.cz.
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