Applications of advanced solid-state NMR methods for probing intermolecular interactions, notably hydrogen bonding are presented: Homonuclear 1H-1H double-quantum (DQ) experiments reveal proximities (typically under 3.5 Angstroms) among pairs of hydrogen atoms, for example distinguishing between ribbon-like or quartet-like self assembly in guanosine supramolecular structures [1-2] or pushing...
The difficulty to automate data acquisition and analysis of complex protein spectra has been one of the major bottlenecks for the widespread use of NMR spectroscopy in structural biology. A promising approach are spectra of high dimensionality (>3) which yield multiple nuclear correlations within fewer experiments, provide high resolution and unambigouos sequential resonance assignment, thus...
Solid-state NMR is a very flexible and powerful technique for the elucidation of geometry and dynamics information on a variety of samples. However, there is still a need to overcome sensitivity and resolution aspects along with the necessity to carry out multidimensional experiments in a short span of time. In order to overcome these challenges, we have made use of two approaches.
First...
In this presentation I will discuss various implementations of multiple detection experiments for accelerating assignment, structure determination and relaxation measurements in the solid state NMR. Methods will include multiple receiver variants of time-shared TSAR experiments for obtaining long distance restraints, 1H-detected and 13C-detected experiments for spectral...
We have developed experimental methods for initiating nonequilibrium structural conversion processes (e.g., protein folding, peptide self-assembly, ligand/receptor complex formation, etc.) by rapid mixing and for trapping intermediate states by rapid freezing after a defined time interval, on the millisecond time scale. When combined with low-temperature dynamic nuclear polarization,...