Review on technical aspects of biological NMR

Technical aspects of NMR spectroscopy with biological macromolecules and studies of hydration in solution

Gerhard Wider in ©Progress in NMR Spectroscopy 32, 193-275 (1998)

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1. Introduction

2. Basic principles

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2.1. Theoretical aspects
2.1.1. Magnetization, precession and Bloch equations
2.1.2. Operators, coherence and product operator formalism
2.1.3. Descriptive representations of experimental schemes
2.1.4. Relaxation
2.1.5. Through bond correlations
2.1.6. Through space correlations
2.2. Radio frequency pulses
2.2.1. Rectangular pulses
2.2.2. Amplitude modulated pulses
2.2.3. Amplitude and phase modulated pulses
2.3. Magnetic field gradients
2.4. Data acquisition
2.4.1. Digitizing the signal
2.4.2. Handling the water resonance
2.4.3. Decoupling during the acquisition
2.4.4. Oversampling and digital filtering
2.5. Multidimensional NMR
2.6. Data processing
2.6.1. Transforming the time domain data into a spectrum
2.6.2. Referencing the chemical shift

3. NMR instrumentation

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3.1. Layout of a high resolution NMR spectrometer
3.2. Spectrometer configuration for biomolecular NMR
3.3. Radio frequency components
3.3.1. The transmitting path
3.3.2. The receiving path
3.3.3. The lock system
3.4. The magnet
3.5. The probe
3.5.1. The radio-frequency coil
3.5.2. The magnetic field gradient coil
3.5.3. The variable temperature operation
3.6. Stability of the system

4. Basic segments of pulse sequences

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4.1. Evolution segments
4.2. Transfer segments
4.2.1. Homonuclear through-bond transfer
4.2.2. Homonuclear through-space transfer
4.2.3. Heteronuclear transfer
4.3. Decoupling sequences
4.4. Pulsed magnetic field gradients
4.5. Combinations of basic segments
4.5.1. The HSQC and the HMQC segment
4.5.2. Concatenating basic segments
4.5.3. Sensitivity enhancement
4.6. Artifact reduction

5. Hydration studies

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5.1. Hydration
5.2. NMR and hydration
5.3. Basic experiments
5.3.1. NOEs between water and protein protons
5.3.2. HYDRA
5.3.3. Measurement of exchange rates using diffusion filter experiments
5.3.4. Relaxation dispersion measurements
5.4. Artifacts in hydration studies at high magnetic field
5.4.1. Radiation damping and demagnetizing field effects
5.4.2. Minimizing artifacts in hydration measurements
5.4.3. Consequences of radiation damping and demagnetizing field effects

6. Conclusions and general remarks

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Acknowledgements

Appendix

A.1. The Bloch equations
A.2. The product operator formalism

References

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