Editors,: P. Diehl E. Fluck H. Gunther R. Kosfeld J. Seelig

Transcription

1 NMR Basic Principles and Progress 34 Editors,: P. Diehl E. Fluck H. Gunther R. Kosfeld J. Seelig Guest-Editors: E. Fluck, H. Gunther Advisory Board: G. Bodenhausen S. Forsen R. K. Harris C. L. Khetrapal T. E. Lippmaa G. J. Martin H. Pfeifer A. Pines B. L. Shapiro

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3 Spin-l NMR By N. Chandrakumar Guest-Editors: E. Fluck and H. Gunther With 68 Figures and 2 Tables, Springer

4 Dr. Narayanan Chandrakumar Central Leather Research Institute Adayaru, Madras, Tamil Nadu I India ISBN-13: e-isbn-13: DOT: / This work is subject to copyright. All rights are reserved, whether the whole or part of the material is concerned, specifically the rights of translation, reprinting, reuse of illustrations, recitation, broadcasting, reproduction on microfilm or in any other way, and storage in data banks. Duplication of this publication or parts thereofis permitted only under the provisions of the German Copyright Law of September 9, 1965, in its current version, and permission for use must always be obtained from Springer Verlag. Violations are liable for prosecution under the German Copyright Law. Springer-Verlag Berlin Heidelberg 1996 Library of Congress Catalog Card Number Softcover reprint of the hardcover 1 st edition 1996 The use of general descriptive names, registered names, trademarks, etc. in this publication does not imply, even in the absence of a specific statement, that such names are exempt from the relevant protective laws and regulations and therefore free for general use. Product liability: The publishers cannot guarantee the accuracy of any information about dosage and application contained in this book. In every individual case the user must check such information by consulting the relevant literature. Typesetting: Thomson Press (India) Ltd, New Delhi Offsetprinting: Saladruck, Berlin; Bookbinding: LOderitz & Bauer, Berlin SPIN: I 0 - Printed on acid-free paper

5 Guest-Editors Prof. Dr. Dr. h.c. Ekkehard Fluck Gmelin-Institut, VarrentrappstraBe 40-42, Frankfurt, FRG Prof. Dr. Harald GUnther Universitat Siegen, Organische Chemie II, HolderlinstraBe 3, Siegen, FRG Editorial Board: Prof. Dr. Peter Diehl Prof. Dr. Ekkehard Fluck Prof. Dr. H. Gunther Prof. Dr. Robert Kosfeld Prof. Dr. J. Seelig Institut flir Physik der Universitlit Basel, KlingelbergstraBe 82, CH-4056 Basel Gmelin-Institut, VarrentrappstraBe40/42, Frankfurt am Main, FRG Universitat Siegen, Organische Chemie n, Postfach , Siegen, FRG In den Atzenbenden 30, Aachen, FRG Biozenbum der Universitat Basel, Abt. Biophysikalische Chemie, K1ingelbergstra6e 70, CH-4056 Basel Advisory Board: Prof. Dr. Geoffrey Bodenhausen Prof. Dr. Sturse Forsen Prof. Dr. Robin K. Harris Prof. Dr. C. L. Khetrapal Prof. Dr. T. E. Lippmaa Prof. Dr. G. J. Marlin Prof. Dr. Harry Pfeifer Prof. Dr. Alex Pines Prof. Dr. Bernard L. Shapiro Section de cbimie, Universite de Lausanne, Rue de labarre 2, CH-I005 Lausanne Departmeut ofphysical Chemistry, Chemical Centre, University oflund,p.o.b. 740, S Lund University of Durham, Departmeut of Chemistry, Science Laboratories, South Road, GB-Durham DHI 3LE Sophisticated Insbuments Facility, Indian Institute of Science, Bangalore , India Institute of Chemical Physics and Biophysics, Academy of Sciences of the Estonian SSR, Lenini paiestee 10, Tallinn I, Estonia Universite de Nantes, U.E.R. de Chimie, ResonanceMagnetiqueNucleaireetReactiviteChimique, UA-CNRS No 472, 2, rue de lahoussiniere, F-440n Nantes Cedex F achbereich Physik, UniversitatLeipzig, Linnestra6e 5, Leipzig,FRG University of California, Berkeley, Department of Chemistry, Berkeley, CA 94720, USA 966 Elsinore Court, Palo Alto, CA 94303, USA

6 Table of Contents 1 The Basic Physics of Spin-l Systems General Introduction Spin States and Matrix Representations of Operators for Spin Spin-1 Operator Algebra L6wdin Projectors for Spin Interactions Relevant in Spin-1 NMR Pulse Rotations Density Matrix Description of the State of Spin-1 Ensembles Evolution of the Spin-1 System Under Quadrupolar Coupling Phase Changes of Spin-1 Wavefunctions Under Rotation Evolution of the Spin-1-Spin-1/2 System Under Scalar Coupling Spin Tickling in a Spin-1/2-Spin-1 Scalar Coupled System Evolution of the Spin-1-Spin-1 System Under Scalar Coupling Coherence Transfer Function for Spin-1 Systems Quadrupolar Relaxation Spin-1 Behavior of Two Equivalent Spins-1/ NMR of Systems Involving Spin-l Nuclei in the Isotropic Phase Chemical Shift Information General Spectral Features Consequent on Coupling to Spin Laboratory Frame Polarization Transfer Involving Spin-1 Nuclei INEPT Polarization Transfer from Spin-1 (S) to Spin-1/2 (I) DEPT Polarization Transfer from Spin-1 (S) to Spin-1/2 (I) Polarization Transfer from Spin-1/2 (I) to Spin-1 (S) Pulse Width Calibration for Polarization Transfer Experiments Polarization Transfer Between Spin-1 Nuclei Two-Dimensional Experiments Involving Spin-1 Nuclei Correlation Spectroscopy (COSY) Heteronuclear Multiple Quantum Spectroscopy Homonuclear Multiple Quantum Spectroscopy Relayed Correlation Spectroscopy Instrumentation for High Resolution Spin-1 NMR 58

7 viii Table of Contents 3 NMR of Spin-l Systems in the Solid State Introduction Quadrupolar Echo leener-broekaert Sequence Deuterium NMR Spectroscopy of Single Crystal Systems Two-Dimensional Deuterium COSY Spectra in the Solid State Deuterium NMR Under Magic Angle Spinning Double Quantum Spectroscopy QUADSHIFT Experiment Overtone Spectroscopy Spin-l/2-Spin-1 Dipolar Coupling Spin Alignment Deuterium Exchange Spectroscopy in Single Crystals Deuterium Exchange Spectroscopy Spin-1 Double Quantum Imaging Instrumentation for Solid State NMR References