NMR Facility

Department of Chemistry University of Oxford

Modern NMR Spectroscopy for the Research Chemist

Prof Tim Claridge

2-3 pm, Monday Weeks 1-8 (10th October to 28th November)

Wolfson Seminar Room, CRL

Overview

This eight-lecture Graduate level course is designed to introduce the modern NMR techniques most commonly used in chemistry research laboratories and builds on the introductory material found in most undergraduate chemistry courses. It does not introduce the basics of NMR spectroscopy and assumes a basic working knowledge of 1D organic NMR.

It is presented at a level appropriate for Part II, D.Phil and post-doctoral scientists who use NMR spectroscopy as a research tool. It will use non-mathematical descriptions of experiments aimed at highlighting the advantages and limitations of the methods in a practical context, covering basic 1D methods and more sophisticated 2D techniques.

All are welcome and there is no need to register for the course. There are no formal handouts for the course, but a pdf copy of slides will be posted here before each lecture and may be used for note taking (Oxford only). The course is also accompanied by the User Guide to Modern NMR Experiments.

Outline:

Lecture 1: Introducing Modern NMR- historical context, basic elements of NMR, sensitivity, relaxation, repetition, quantification [download pdf]

Lecture 2: 1D NMR methods- optimising 1D data, decoupling, pure shift NMR, sensitivity enhancement (INEPT), spectrum editing (DEPT and DEPTQ) [download pdf]

Lecture 3: 2D NMR methods I- homonuclear correlation spectroscopy (COSY and variants), total correlation spectroscopy (TOCSY), carbon-carbon correlations (INADEQUATE/ADEQUATE) [download pdf]

Lecture 4: 2D NMR methods II- heteronuclear correlation spectroscopy- one-bond correlations (HSQC and HMQC), editing HSQC, long-range correlations (HMBC and H2BC), measuring and using nJCH couplings (HSQMBC), hybrid methods (HSQC-TOCSY) [download pdf]

Lecture 5: the nuclear Overhauser effect- equilibrium vs transient NOEs, 1D and 2D nOe spectroscopy (NOESY), rotating-frame nOes (ROESY), heteronuclear nOes (HOESY) [download pdf]

Lecture 6: Methods for studying molecular interactions-  diffusion NMR spectroscopy (DOSY),  protein-small molecule (ligand) interactions (STD, WaterLOGSY etc), [download pdf]

Lecture 7: Dynamic effects in NMR- Chemical exchange processes, NMR timescales- fast, intermediate and slow exchange, exchange decoupling, rate constants from lineshape analysis and magnetisation transfer experiments, 2D exchange (EXSY), kinetics and thermodynamics of exchange, protein-ligand binding and exchange. [download pdf]

Lecture 8: How NMR works: The spectrometer, signal selection (phase cycling and pulsed field gradients), selective excitation, solvent suppression, inside the spectrometer. [download pdf]

Bibliography:

High-Resolution NMR techniques in Organic Chemistry (3rd Edn), TDW Claridge, Elsevier, 2016.

Spectrometric Identification of Organic Compounds (7th Edn), RM Silverstein, FX Webster and DJ Kiemle, Wiley, 2005.