ONE AND TWO DIMENSIONAL NMR SPECTROSCOPY
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1 ONE AND TWO DIMENSIONAL NMR SPECTROSCOPY Atta-ur-Rahman H.E.J. Research Institute of Chemistry, University ofkarachi, Karachi 32, Pakistan ELSEVIER Amsterdam Oxford New York Tokyo 1989
2 IX CONTENTS Chapter-l 1 BASIC PRINCIPLES OF MODERN NMR SPECTROSCOPY Introduction Some Fundamental Considerations in NMR Spectroscopy Instrumentation The Magnet The Probe Probe Tuning Shimming Deuterium Lock Creating a Signal Pulse NMR Data Acquisition and Storage The Dynamic Range Problem Digital Resolution Quadrature Detection PeakFolding Fourier Transformation Signal-to-Noise Ratio "Manipulating" the Spectrum - Window Functions Sensitivity Enhancement Resolution Enhancement Rotating Frame of Reference Pulse Angle Rotation of Vectors Phase Cycling Phase Cycling and Coherence Pathways Pulse Widths Composite Pulses Time Proportional Phase Increment (TPPI) Tailored Suppression and Excitation - Solvent Suppression Techniques Presaturation 42
3 X Tailored Excitation Method Jump and Retum Method The Inversion Recovery Method Solvent Suppression by Paramagnetic Reagents Selective Excitation by DANTE (Delays Alternating with Nutation for Tailored Excitation) Improvements in Instrumentation Design 48 (a) Probehead Design 48 (b) Offset Equivalence of Transmitter and Decoupler Channels 48 (c) Fast Switching of Decoupler Power Nuclear Overhauser Enhancement (NOE) Theoretical Approaches to Pulsed NMR Bloch's Semi-classicalApproach Density Matrix Approach Product OperatorApproach Effect of a Pulse on the Nucleus Coherence Transfer Homonuciear Coherence Transfer Heteronuclear Coherence Transfer Multiple Quantum Filters Other Selective Detection Techniques p-spin Filtering z-filters 71 Chapter-2 2 SPIN-ECHO AND POLARISATION TRANSFER Spin-Echo Formation in Homonuciear and Heteronuclear Systems Spin-Echo Production in Heteronuclear Systems Pulse Applied Simultaneously to NucleiA andx (f Pulse Applied Selectively to Partner Nucleus X Spin-Echo Production in Homonuciear Systems (or Heteronuclear Systems with
4 Non-Selective Application of Pulses) (f x Pulse Applied Simultaneously to NucleiA and X Attached Proton Test (APT), Gated Spin-Echo (GASPE) or Spin-Echo Fourier Transform (SEFT) Measurements Escort Editing ofapt Spectra 93 Cross-polarisation Selective Population Transfer Non-Selective Polarisation Transfer Insensitive Nuclei Enhanced by Polarisation Transfer (INEPT) Refocussed INEPT INEPT Reverse INEPT Semi-Selective Excitation for Polarisation Transfer (SESET) SESET-RELAY Distortionless Enhancement by Polarisation Transfer (DEPT) and Related Experiments DEPT Anomalies in Polarisation Transfer Experiments 116 (a) Intensity Anomalies 116 (b) Multiplet Anomalies 116 (c) Phase A nomalies 116 (d) Incomplete Separation of Subspectra DEPT DEPT DEPT GL MODEPT Universal Polarisation Transfer (UPT) Phase Oscillation to Maximise Editing (POMMIE) Reverse DEPT Subspectral Editing Using a Multiple Quantum Trap (SEMUT) SEMUT GL 123
5 XII 23 Problems Solutions to Problems 133 Chapter-3 3 CARBON-CARBON CONNECTIVITY - ID INADEQUATE 141 SPECTRA 3.1 Introduction One-dimensional INADEQUATE 13 C-NMR Spectra Factors Affecting the Intensity of the 13 C Satellite Signals Some Practical Suggestions SEMUTEditingof INADEQUATE Spectra (SEMINA) INEPT-INADEQUATE DEPT-INADEQUATE INADEQUATE Sensitivity Improvement by Proton Indirect Detection (INSIPID) Saturation INADEQUATE Double-Quantum Transitions for Chapter-4 Finding Unresolved Lines (DOUBTFUL) THE NUCLEAR OVERHAUSER EFFECT Introduction Relaxation Pathways Spin-Lattice Relaxation Other Relaxation Mechanisms How noe Occurs Other Factors Governing Relaxation and noe Internuclear Distance and noe Internuclear Distances in Two-Spin Systems 179
6 XIII Three-Spin Systems Linear Arrangement Three-Spin Effect Non-Linear Arrangement Heteronuclear noe NOE Difference Spectra Some Practical Examples of noe Difference Spectroscopy Problems Solutions to Problems 197 Chapter-5 5 TWO-DIMENSIONAL NMR SPECTROSCOPY BASIC PRINCIPLES Chapter-6 6 HETERONUCLEAR 2D J-RESOLVED SPECTROSCOPY The Gated Decoupler Method The Refocussed Fold-over Corrected (RE-FOCSY) Gated Decoupler Method The Spin-Flip Method The Selective Spin-Flip Method The Semi-Selective Spin-Flip Method Indirect J-Spectroscopy with Selective Spin-Flip Heteronuclear 2D J-resolved Spectra with Polarisation Transfer Heteronuclear 2D J-resolved Spectra with Driven Pulses Problems Solutions to Problems 239
7 XIV Chapter-7 7 HOMONUCLEAR 2D J-RESOLVED SPECTROSCOPY Double Resonance in 2D J-Resolved Spectra Constant Time 2D J-Resolved Spectra Absorption mode 2D J-Resolved Spectra Differentiation of Homonuclear Multiplets by Indirect 2D J-Resolved Spectroscopy Problems Solutions to Problems 264 Chapter 8 8. HOMONUCLEAR 2D SHIFT CORRELATED 269 SPECTROSCOPY 8.1 COSY Spectra Introduction The Nuts and Bolts of COSY Magnetization Transfer Phase Cycling The Birthofa COSY Spectrum Intensity of Cross-Peaks Digital Resolution in COSY Other Practical Considerations in COSY Some Examples of COSY Spectra Improvements in COSY Spectra Elimination of Artifact Axial Peaks Parallel to vi from COSY Spectra Noise in COSYSpectra Quad Detection and Suppressing Quad Images in COSY Spectra Phase-Sensitive COSY Spectra Pure-Phase 2D Spectra by Cosine Transformation with respect to ti Coupling Constants from Phase-Sensitive COSY Spectra 299
8 COSY by Echo or Anti-echo Selection Basic Peakshapes in 2D Spectra Pure 2D Absorption Peakshape Pure 2D Dispersion Peakshape Mixed Absorption-Dispersion Peakshape (Phase-twisted Peakshape) Absolute Value Peakshape Shaping Functions in 2D Spectra Foldingof Signals in COSY Spectra Symmetrization Coherence Transfer Pathways in COSY Modifications in COSY Spectra COSY-45 Spectra Pattern Recognition Signs of Coupling Constants COSY-45 Spectra with Decoupling in vi Dimension COSY Optimized for Long Range Couplings (DELAYED COSY) Super COSY Exclusive Correlation Spectroscopy (E. COSY) Homonuclear Relayed Coherence Transfer (Relayed COSY or R COSY) Homonuclear Chemical Shift Correlation by Heteronuclear Relayed Coherence Transfer (HERPECS) Total Correlation Spectroscopy (TOCSY) SECSY z-filtered SECSY Spectra FOCSY Spectra Super SECSY Difference SECSY vi -Decoupled SECSY Spectra Problems 349
9 XVI 8.4 Solutions to Problems 352 Chapter-9 9 CHEMICAL SHIFT CORRELATION THROUGH 359 CROSS - RELAXATION AND EXCHANGE 9.1 Introduction Nuclear Overhauser Enhancement Spectroscopy (NOESY) Homonuclear Relayed NOESY Heteronuclear Relayed NOESY D Chemical Exchange Spectra Rate Constant by "Accordion" Spectroscopy - Three-Dimensional NMR CAMELSPIN OR ROESY (Rotating Frame Overhauser Enhancement Spectroscopy) Two-Dimensional Heteronuclear NOE Spectroscopy (HOESY) Combined COSY-NOESY Experiment (COCONOSY) DQ NOESY Problems Solutions to Problems 384 Chapter HETERONUCLEAR 2D-SHIFT CORRELATION 391 SPECTROSCOPY 10.1 Principles of Heteronuclear 2D Shift Correlation Spectroscopy Modifications of Heteronuclear 2D-Shift Correlation Experiment With Homonuclear vi Decoupling Long Range Heteronuclear Chemical Shift Correlation using (TANGO) Improved Decoupling Modulation Procedures
10 XVII in 2D Long-Range Heteronuclear Chemical Shift Correlation Spectra Correlation Spectroscopy via Long-Range Coupling (COLOC) H-Detected Heteronuclear Multiple-Quantum Coherence (HMQC) for Correlating Directly Bonded X H- 13 C Nuclei Sensitivity Enhanced Detection of Heteronuclear Multiple Bond Connectivity (HMBC) by 2D Multiple-Quantum NMR D DEPT Heteronuclear Shift Correlation Spectroscopy Sensitivity of Heteronuclear Coherence Transfer Experiments Heteronuclear Relayed Coherence Transfer Spectroscopy (or Heteronuclear Relayed COSY) Low Pass J-Filtered 2D Heteronuclear Shift Correlated Spectra Relayed Coherence Transfer From a Heteronucleus through Proton Spin Systems Heteronuclear Relayed Coherence Transfer via Hartmann-Hahn type Cross-Polarisation Problems Solutions to Problems 429 Chapter CROSS POLARISATION IN THE ROTATING FRAME Introduction 11.2 Homonuclear Hartmann-Hahn Spectroscopy (HÖHAHA)
11 XVIII Chapter D MULTIPLE-QUANTUM SPECTROSCOPY Introduction Multiple-Quantum Spectra oftwo Spin Systems Two Dimensional INADEQUATE 13 C-NMR Spectroscopy Proton MonitoredINADEQUATE (INSIPID) Multiple-Quantum Spectra of Three-Spin Systems Double-Quantum Spectra of Three-Spin Systems Linear Systems 459 (i) Signals due to Direct Connectivity 462 (ü) Magnetically Equivalent Nuclei 462 (iii) Remote Nuclei Triple-Quantum Spectra of Three-Spin Systems Constant Time Double-Quantum Spectroscopy Multiple-Quantum Spectra in Four-Spin Systems Uniform Excitation of Multiple-Quantum Coherence Multiple-Quantum Filtered COSY Spectra Homonuclear Zero-Quantum Spectroscopy Improved HZQC Method SUCZESS Problems Solutions to Problems 487 Chapter TACKLING THE STRUCTURE Choice of Experiment ACase Study 495 (a) 1D 'H-NMR Studies 496 (b) Homonuclear 2D J-Resolved Spectrum 499
12 XIX (c) 2D Homonuclear Shift Correlated Spectrum (COSY-45) 499 (d) DEPTSpectra 499 (e) 2D Heteronuclear Shift Correlated Experiment 503 (f)! H, 13 C-COLOC 505 (g) NOESY and NOE Difference Spectra 507 (h) 2D1NADEQUA TE Spectrum 510 Chapter PRODU CT OPERATOR APPROACH TO 2D-NMR 511 SPECTROSCOPY 14.1 Scalar Coupling Dipolar Coupling Phase Cycling and Product Operators 521 Appendix-1 SOME TERMS, SYMBOLS AND ACRONYMS USED IN NMR SPECTROSCOPY 527 Appendix-2 SUMMARY OF IMPORTANT 2D NMR TECHNIQUES 537 Index 553
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