caa a22 4500 445325399 CHVBK 20180317142718.0 cr unu---uuuuu 170323e20111201xx s 000 0 eng 10.1007/s10858-011-9578-1 doi (NATIONALLICENCE)springer-10.1007/s10858-011-9578-1 Three-dimensional deuterium-carbon correlation experiments for high-resolution solid-state MAS NMR spectroscopy of large proteins [Elektronische Daten] [Daniela Lalli, Paul Schanda, Anup Chowdhury, Joren Retel, Matthias Hiller, Victoria Higman, Lieselotte Handel, Vipin Agarwal, Bernd Reif, Barth van Rossum, Ümit Akbey, Hartmut Oschkinat] Well-resolved 2H-13C correlation spectra, reminiscent of 1H-13C correlations, are obtained for perdeuterated ubiquitin and for perdeuterated outer-membrane protein G (OmpG) from E. coli by exploiting the favorable lifetime of 2H double-quantum (DQ) states. Sufficient signal-to-noise was achieved due to the short deuterium T 1, allowing for high repetition rates and enabling 3D experiments with a 2H-13C transfer step in a reasonable time. Well-resolved 3D 2HDQ-13C-13C correlations of ubiquitin and OmpG were recorded within 3.5days each. An essentially complete assignment of 2HDQα shifts and of a substantial fraction of 2HDQβ shifts were obtained for ubiquitin. In the case of OmpG, 2HDQα and 2HDQβ chemical shifts of a considerable number of threonine, serine and leucine residues were assigned. This approach provides the basis for a general heteronuclear 3D MAS NMR assignment concept utilizing pulse sequences with 2HDQ-13C transfer steps and evolution of deuterium double-quantum chemical shifts. Springer Science+Business Media B.V., 2011 Solid-state NMR nationallicence Micro-crystalline nationallicence Membrane proteins nationallicence Ubiquitin nationallicence OmpG nationallicence Deuterium-carbon correlations nationallicence Lalli Daniela Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut Schanda Paul Physical Chemistry, ETH Zürich, Wolfgang-Pauli-Strasse 10, 8093, Zurich, Switzerland aut Chowdhury Anup Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut Retel Joren Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut Hiller Matthias Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut Higman Victoria Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut Handel Lieselotte Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut Agarwal Vipin Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut Reif Bernd Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut van Rossum Barth Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut Akbey Ümit Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut Oschkinat Hartmut Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut Journal of Biomolecular NMR Springer Netherlands 51/4(2011-12-01), 477-485 0925-2738 51:4<477 2011 51 10858 https://doi.org/10.1007/s10858-011-9578-1 text/html Onlinezugriff via DOI 1 research-article jats NATIONALLICENCE 856 40 https://doi.org/10.1007/s10858-011-9578-1 text/html Onlinezugriff via DOI NATIONALLICENCE 700 1- Lalli Daniela Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut NATIONALLICENCE 700 1- Schanda Paul Physical Chemistry, ETH Zürich, Wolfgang-Pauli-Strasse 10, 8093, Zurich, Switzerland aut NATIONALLICENCE 700 1- Chowdhury Anup Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut NATIONALLICENCE 700 1- Retel Joren Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut NATIONALLICENCE 700 1- Hiller Matthias Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut NATIONALLICENCE 700 1- Higman Victoria Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut NATIONALLICENCE 700 1- Handel Lieselotte Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut NATIONALLICENCE 700 1- Agarwal Vipin Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut NATIONALLICENCE 700 1- Reif Bernd Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut NATIONALLICENCE 700 1- van Rossum Barth Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut NATIONALLICENCE 700 1- Akbey Ümit Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut NATIONALLICENCE 700 1- Oschkinat Hartmut Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Strasse 10, 13125, Berlin, Germany aut NATIONALLICENCE 773 0- Journal of Biomolecular NMR Springer Netherlands 51/4(2011-12-01), 477-485 0925-2738 51:4<477 2011 51 10858 Metadata rights reserved Springer special CC-BY-NC licence nationallicence BK010053 XK010053 XK010000 NATIONALLICENCE NATIONALLICENCE NL-springer