ADVANCED NMR FOR INORGANIC AND ORGANIC CHEMISTRY: A PRATICAL APPROACH

NMR techniques are ubiquitous in their applications to the various fields of chemistry : synthetic organic and inorganic, applied and analitycal, biological and pharmaceutical.
Even if they are still evolving, and software automation ensure the availability of their results even to the unskilled personnel, some of the basical mono and bidimensional techniques should be not only used but understood at some depth by any chemistry PhD student to be able to fully achieve his/her own research project.

- The comprehension of the pulsed nmr experiment in the perspective of the Rotating Frame of Reference, of its critical aspects (sensitivity, resolution, digitalization of signals) and of its limitations.
- The understanding, in this view, of the behaviour of simple spin systems (AB between two H, and AX between one H and one 13C) and of the basic principles of Polarization Transfer techniques (INEPT/DEPT spectra) and Overhauser effect (NOE/NOESY spectra).
- The skill in obtaining this spectra on an instrument available to the students, working on the more relevant acquisition parameters.
- The basic understandingof two-dimension nmr spectroscopy and of critical parameters in the practical acquisition process for these spectra (COSY, DQF COSY, HMQC, HMBC etc).
- Hints on diffusion spectroscopy (DOSY).
- Skill in interpretation, comparisonand integrationsof various spectral data to obtain a structural characterization on organic and inorganic molecules.
In general, the target is making the sudents capable and self-confident on the practical techniques and spectral data interpretation in the data harvesting needed for their research project.

The normal knowledge of spectroscopy principles given by standard univerity courses (Physical Chemistry, Analitical Chemistry).

Principles of NMR phenomenon in the rotating frame of reference scheme. Standard 1D NMR experiment in pulsed/FT mode, relaxation, multinuclear NMR (sensitivity, resolution). Digitalization and digital treatment of data.
Pulse sequences (T1/T2 measurement).
Polarization transfer from sensitive (1H) to insensitive (13C, 15N) nuclei : basic INEPT/DEPT pulse sequences; 13C spectrum editing in 1H/13C INEPT/DEPT spectra.
Basic Overhauser effect : homonuclear correlation through space and consequences for molecular structural determinations, NOE spectra (NOESY/ROESY in 2D NMR).
Basic 2D spectroscopy : homonuclear correlation through coupling constants spectra (various COSY techniques); heteronucler correlation (HMQC/HSQC, HMBC etc).
Practical experiences of acquisition of spectra on some instruments (Bruker 300/400).

T.W.D. Claridge : High-Resolution NMR Techniques in Organic Chemistry, 2nd Ed.
Tetrahedron Organic Chemistry Series, vol. 27; Elsevier, 2009; ISBN-13 : 978-0-08-054818-0

D.H. Williams, I. Fleming : Spectroscopic Methods in Organic Chemistry, 6th Ed.
Tata Mcgraw Hill Education; 6 Ed. ISBN-13: 978-0071332767

R.M. Silverstein, et alia : Identificazione spettrometrica di composti organici.
CEA; 3 edizione. ISBN-13: 978-8808183507

Written and practical essay : acquisition and interpretation of 1D and 2D spectra needed to characterize a molecule of interest.

Classes and practical exercises (various kinds of spectra acquisition and interpretation on NMR instruments).

English

PowerPoint presentation (.pdf version) used in lessons will be made available to the students.

written