50 and More Essential NMR Experiments

Matthias Findeisen studied Physics at the University of Leipzig. During his Diploma course he joined 1979 the group of Prof. Artur Lösche, who established in the fifties radio frequency spectroscopy in the Physical Institute and was one of the pioneers in NMR in East Germany. This gave M.F. a little taste of NMR and, had been nosey, he stayed there for his PhD work on the field of liquid crystalline substances. Afterwards he switched to the East German Academy of Science in Leipzig and operated an NMR routine lab, which focused him to NMR in liquids and chemical analytical problems. Returning back to the Leipzig University in 1992 he kept this focus in the group of Prof. R. Borsdorf, later on conducted by Stefan Berger, than concentrating to methodological NMR subjects. Stefan Berger was intrigued by NMR after having won a bottle of beer during an introductory course in organic NMR led by Prof. H. Suhr at the University Tübingen in 1968. After a PhD thesis with Prof. Anton Rieker, in 1973 he joined Prof. J. D. Roberts at Caltec for postdoctoral work, where he also met Prof. D. M. Grant and Prof. D. Seebach, who were then guest professors in Pasadena. This period was decisive in trying for a Habilitation in NMR spectroscopy, which was achieved at the University Marburg. At the University of Leipzig he tries to combine methodological development of NMR with its application to bioorganic problems.

PREFACE

THE ORGANIC SET OF NMR SPECTRA
The 1H NMR Experiment
APT-13C NMR
COSY
NOESY
HSQC
HMBC

ADVANCED ORGANIC NMR SPECTROSCOPY
2D J-Resolved 1H NMR Spectroscopy
ROESY
TOCSY
HSQC-TOCSY
HOESY
INADEQUATE
ADEQUATE
J-HMBC
Gated Decoupling

SELECTIVE METHODS
Water suppression by Presaturation
Solvent Suppression by 1D-NOESY
Water Suppression by SOGGY Excitation Sculpting
Solvent Suppression using WET
SELTOCSY
SELNOESY
SELINCOR
SELINQUATE
Band Selective HMBC

HETERONUCLEAR NMR
11B NMR Spectroscopy
15N NMR Spectroscopy
17O NMR Spectroscopy
19F NMR Spectroscopy
29Si NMR Spectroscopy
57Fe NMR Spectroscopy
195Pt NMR Spectroscopy

EXPERIMENTS IN PHYSICAL ORGANIC CHEMISTRY
Measurement of the Spin - Lattice Relaxation Time T1
Measurement of the Spin - Spin Relaxation Time T2
Dynamic 1H NMR Spectroscopy
Diffusion Measurement with DOSY
Residual Dipolar Couplings (RDC)

ORGANIC CHEMISTRY APPLICATIONS
ASIS
Chirality Determination
Advanced Mosher Method
Quantitative NMR and Relaxation Reagents
Determination of Association Constants Ka
STD NMR
A Kinetic Experiment

AN EXCURSION TO THE SOLID STATE AND TO STRUCTURAL BIOLOGY
The CP/MAS Experiment
High-Resolution Magic-Angle Spinning
HN-HSQC
HNCA

MAINTENANCE AND CALIBRATION
Calibration of Pulse Duration in the Transmitter Channel
Calibration of the Pulse Duration in the Indirect Channel
Shaped Pulses
Adiabatic pulses
Temperature Calibration in NMR
Calibration of Pulsed Field Gradients

APPENDIX
Answers
Pulse Programs
Elementary Product Operator Formalism Rules
Chemical Shift and Spin-Coupling Data for Strychnine
Picture Credits

INDEX