Broad-Band DREAM Recoupling Sequence.

We describe a more broad-banded version of the DREAM double-quantum dipolar-recoupling sequence, which is devised by superimposing a phase-alternating RF irradiation scheme, that is, XiX pulses, on top of the original DREAM sequence. We call this sequence XiX(CW) DREAM. The recoupling conditions and the corresponding first-order effective Hamiltonian are analyzed using triple-mode Floquet theory. The performance of the XiX(CW) DREAM sequence is compared to the original DREAM sequence by numerical simulations and experiments on small model substances and the model protein ubiquitin. The results confirm that XiX(CW) DREAM shows a wider recoupling bandwidth compared to that of DREAM, therefore making the choice for the position of the carrier frequency less critical.

[1]  B. Meier,et al.  Amplitude-modulated low-power decoupling sequences for fast magic-angle spinning NMR , 2013 .

[2]  B. Meier,et al.  Properties of the DREAM scheme and its optimization for application to proteins , 2012, Journal of biomolecular NMR.

[3]  B. Meier,et al.  Solid-state NMR sequential assignments of α-synuclein , 2011, Biomolecular NMR Assignments.

[4]  N. Nielsen,et al.  Efficient and Robust Heteronuclear Cross-Polarization for High-Speed-Spinning Biological Solid-State NMR Spectroscopy. , 2012, The journal of physical chemistry letters.

[5]  B. Meier,et al.  Extensive de novo solid-state NMR assignments of the 33 kDa C-terminal domain of the Ure2 prion , 2011, Journal of biomolecular NMR.

[6]  P. Schanda,et al.  Accurate measurement of one-bond H-X heteronuclear dipolar couplings in MAS solid-state NMR. , 2011, Journal of magnetic resonance.

[7]  R. Riek,et al.  Protocols for the Sequential Solid‐State NMR Spectroscopic Assignment of a Uniformly Labeled 25 kDa Protein: HET‐s(1‐227) , 2010, Chembiochem : a European journal of chemical biology.

[8]  V. Ladizhansky.  Homonuclear dipolar recoupling techniques for structure determination in uniformly 13C-labeled proteins. , 2009, Solid state nuclear magnetic resonance.

[9]  R G Griffin,et al.  Dipolar recoupling in solid state NMR by phase alternating pulse sequences. , 2008, Journal of magnetic resonance.

[10]  B. Meier,et al.  Operator-based triple-mode Floquet theory in solid-state NMR. , 2007, The Journal of chemical physics.

[11]  B. Meier,et al.  Amplitude-modulated decoupling in rotating solids: a bimodal Floquet approach. , 2006, Solid state nuclear magnetic resonance.

[12]  Thorsten Lührs,et al.  Correlation of structural elements and infectivity of the HET-s prion , 2005, Nature.

[13]  R. Griffin,et al.  Rotational resonance NMR: separation of dipolar coupling and zero quantum relaxation. , 2003, Journal of magnetic resonance.

[14]  B. Meier,et al.  Adiabatic dipolar recoupling in solid-state NMR: the DREAM scheme. , 2001, Journal of magnetic resonance.

[15]  H. Oschkinat,et al.  Backbone and Side‐Chain 13C and 15N Signal Assignments of the α‐Spectrin SH3 Domain by Magic Angle Spinning Solid‐State NMR at 17.6 Tesla , 2001, Chembiochem : a European journal of chemical biology.

[16]  R. Griffin.  Dipolar recoupling in MAS spectra of biological solids , 1998, Nature Structural Biology.

[17]  M. Hohwy,et al.  Broadband dipolar recoupling in the nuclear magnetic resonance of rotating solids: A compensated C7 pulse sequence , 1998 .

[18]  B. Meier,et al.  A homonuclear spin-pair filter for solid-state NMR based on adiabatic-passage techniques , 1998 .

[19]  K. Takegoshi,et al.  Selective homonuclear polarization transfer in the tilted rotating frame under magic angle spinning in solids. , 1997, Journal of magnetic resonance.

[20]  N. Nielsen,et al.  Double‐quantum homonuclear rotary resonance: Efficient dipolar recovery in magic‐angle spinning nuclear magnetic resonance , 1994 .

[21]  T. Oas,et al.  Rotary resonance recoupling of dipolar interactions in solid‐state nuclear magnetic resonance spectroscopy , 1988 .

[22]  J. H. Van Vleck,et al.  The Dipolar Broadening of Magnetic Resonance Lines in Crystals , 1948 .

[23]  Angelika Sebald,et al.  Dipolar recoupling under magic-angle spinning conditions , 2000 .

[24]  B. Meier,et al.  Computer Simulations in Magnetic Resonance. An Object-Oriented Programming Approach , 1994 .