Solid-State NMR techniques ( 04CR3587 , 04COP96 ), and 04COP554 ) can be applied to:

Large proteins and protein complexes that may not crystallize ( 99JACS7500 , 99NAT141 , and 00JB313 )

Membrane-bound systems

Noncrystalline solid systems such as fibrillar protein and peptides ( 01METH390 )

Micro- and Nanocrystalline proteins ( 05JB217-31 and ( 05JACS8618 )

The structure determination of isotopically labeled proteins by solid-state NMR requires sequence-specific 13C and 15N resonance assignment ( B03ZER243). In principle, analogous correlation schemes of those widely applied in solution can also be employed in designing multidimensional magic-angle (MAS) experiments ( 96JB239 , 00JB209 , 00JACS1443 ). Some reported experiments on proteins are:

2D Homonuclear:

DREAM ( 98CPL421-287 and 01JMR81-150 )

TOBSY ( 01JMR459-148 )

2D Heteronuclear

2D TEDOR is one of the most simplest techniques for obtaining 13C-15N dipolar chemical shift correlation spectra of biological systems ( 02JACS10728 ). Incorporation of adiabatic recoupling pulses ( 05JB49-31 ).

PISEMA ( 99JMR131-140 , 02JB239 , 03JB283-26 ). The experiment correlates the 15N chemical shift and the NH dipolar splitting of all residues. The assignment and determination of the orientation of each peptide plane is achieved by fitting the experimentally determined chemical shift/dipolar (CS/D) pai to calculated parameters ( 05JB101-31 , 00JMR150-144 , 00JMR162-144 )

APHH CP ( 96JMRA140-118 ). Apllication on 1H-15N ( 04JB303-30 ).

2D N(CO)CA experiment ( 99JB1-15 )

2D 1H-15N and 3D 1H-15N-13C dipolar correlation experiments (03JB217-25)

PDSD Experiment: Proton Driven Spin Diffusion

RAD: RF Assisted Diffusion

RADCP

IseRAD: Isotope-edited RAD experiment ( 04JACS7196 )

DARR: Dipolar Assisted Rotational Resonance ( 01CPL631-344 )

SPECIFIC-CP for inter-residual assignments

2D C-C Correlations

C-C correlation using DARR scheme ( 05JACS8618 )

ROCSA (Recoupling of chemical shift anisotropy ( 03JCP8378 and 03JACS11828 )

3D Heteronuclear

3D NCACB experiment ( 99JB1-15 )

3D NCA(CO)CX and NCOCACX

Applications:

• Methods for resonance assignments in uniformly 13C,15N labeled proteins 01JB203-20
• Measurement of dipolar couplings in uniformly 13C,15N-labeled membrane peptides ( 01JACS12929 )
• CA CSA in helical peptides ( 02JB51-24 ) which is sensitive to secondary structure.
• Sequential resonance assignments and conformational analysis of a dimeric protein (2*10.4 kDa) ( 03JB323-27 )
• Detection of dynamic water molecules in a microcrystalline sample ( 05JB295-31 )
• Pulsed Field Gradients in ssNMR experiments for coherence selection ( 99JMR29-141 ) and for solvent suppression purposes ( 05JB295-31 )