Content

Part 1

Energy levels and NMR spectroscopy

• The Hamiltonian and spectrum for one spin
• Hamiltonians, energy levels and spectra for two or more coupled spins

The vector model

• Bulk magnetization
• Larmor precession
• Detection
• Pulses (on resonance pulse, pulse phase, off resonance effects and soft pulses)
• Detection in the rotating frame
• The pulse acquire experiment
• Pulse calibration
• The spin echo

Fourier transformation and data processing

• How the FT works
• Representing the FID
• Lineshapes and phase
• Manipulating the FID and the spectrum
• Zero filling
• Truncation

Product operators

• Operators for one spin
• Analysis of pulse sequences for one spin
• Operators for two spins
• In-phase and anti-phase terms
• Hamiltonians for two spins
• Heteronuclear spin systems
• Spin echoes and J-modulation
• Coherence transfer
• The INEPT experiment
• The COSY experiment
• Coherence order and multiple-quantum coherences

Two dimensional NMR

• The general scheme for a 2D experiment
• Modulation and lineshapes
• COSY
• DQF-COSY
• Double-Quantum spectroscopy
• Heteronuclear correlation spectra
• HSQC
• HMQC
• Long-range correlation HMBC
• TOCSY

Relaxation and the NOE

• The origin of relaxation
• Relaxation mechanims
• Describing random motion - the correlation function
• Populations
• Longitudinal relaxation behavior of isolated spins
• Longitudinal dipolar relaxation of two spins
• The NOE
• transient NOE
• steady state NOE
• Two-dimensional NOESY
• Transverse relaxation
• Homogeneous and inhomogeneous line broadening
• Relaxation due to chemical shift anisotropy

Equivalent spins and spin system analysis

• Notation for spin systems
• Equivalent spins: chemical and magnetic equivalence
• Strong coupling in a two spin system
• The AB spectrum, evolution to an AX and A2 spectrum
• Spin systems with more than two spins, conceptual approach
• The ABX system
• Virtual coupling
• The AA’XX’ system

How the spectrometer works

• The components of the spectrometer

Part 2

In the lectures the focus is on advanced applications of NMR spectroscopy such as solving the structure of proteins by 2D/3D NMR methods. Also the application of NMR in drug design and in the study of exchange phenomena and receptor/ligand binding will be discussed.  This part will also cover NMR of some metal nuclei and of paramagnetic complexes. Eventually the students have to independently read and understand an NMR related paper provided by the didactical team.
The following topics will be discussed in more detail:

• Introduction to solving structure of proteins by NMR  (J-modulated spectroscopy, HETCOR, HSQC, HMQC, COSY, NOESY, TOCSY). Introduction to 3D NMR methods used in protein NMR. 
• 2D methods to study exchange phenomena and receptor/ligand binding studied by NMR. 
• Use of NMR techniques in drug design
• Review of heteronuclei giving NMR signals (nuclei with spin ½ and quadrupole nuclei)
• General trends in the chemical shift of heteronuclei (geometry/coordination number/oxidation state/electronegativity/ ...)
• NMR spectra of paramagnetic transition metal complexes
• Diffusion ordered NMR spectroscopy (DOSY) 
• Introduction to solid-state NMR (MAS and CP)

Course material

• Handouts distributed via TOLEDO.
• Screencasts/video material distributed via TOLEDO.
• Paper for reading assignment distributed via TOLEDO.
• Handbook: James Keeler, Understanding NMR spectroscopy. Second Edition; Wiley & Sons:  2010 ISBN 978-0-470-74608-0

Language of instruction: more information

Deze onderwijsleeractiviteit wordt gevolgd door zowel de master of chemistry als de master in de chemie

Content

During the exercises, concepts introduced in the theory sessions are brought into practice and are illustrated using pre-acquired datasets (pulse calibration, relaxation time measurements, spectral processing, effect of weighting functions, phase corrections, ...).

In the exercises, the student learns to work with real NMR datasets at the computer using NMR processing software.

The student has to be able to extract basic information from a dataset concerning:

• type of experiment
• pulse program used
• acquisition parameters
• processing parameters 

This will allow the student to critically evaluate

• the quality of data
• the reliability of the experiment (e.g.were optimal parameters used)
• the need for running extra experiments

After this initial evaluation of the dataset, the student is able to

• select the most appropriate processing parameters for the dataset
• use the data alone or in combination with other info to perform structure assignment tasks or spectral assignment tasks
• process the data and produce high quality figures for inclusion in a thesis, in papers or reports

Course material

• Handouts distributed via TOLEDO
• NMR datasets (1D and 2D)
• Software: Bruker Topspin 4.x or newer (info on TOLEDO)

Format: more information

The exercise sessions are organized in a PC class.