A large fraction of our research effort is devoted to the development of new magnetic resonance techniques to study molecular structure and dynamics. Typical of the problems that we address is the design of experiments to measure 13C-13C and 13C-15N dipolar couplings, and therefore to perform spectral assignments and to measure internuclear distances and torsion angles, in solids from magic angle spinning (MAS) NMR spectra. This information leads directly to molecular structures of amyloid and membrane peptides and proteins (vide infra). In addition, we are developing high field dynamic nuclear polarization (DNP)/NMR experiments. The motivation behind this research is the possibility to obtain large nuclear spin polarizations, and therefore increased NMR signal intensities. This increased signal intensities should enable many new applications to be addressed. As part of this project, we are also performing CW and pulsed EPR experiments at 140 GHz. For systems not susceptible to g-strain, the higher EPR frequencies offer considerably increased resolution and ease of interpretation of the spectral lineshapes. Finally, we are also involved in the development of approaches for investigating dynamic processes in solids. Generally, these experiments involve analysis of 2H NMR powder patterns, and details concerning the rates and mechanism of the motion are derived from the lineshapes.