NMR Primer: An HSQC-Based Approach (with Vector Animations)

Dedication
Preface
Vector diagrams and animations
How to obtain the animations
Chapter 1: The simplest one-dimensional NMR experiment
1.1 Nuclei are magnets or spins
1.2 Spins align with a field?
1.3 Conservation of angular momentum: spins precess about a field
1.4 Quantisation of spin orientation: cone of precession
1.5 Thermal energy: net magnetisation
1.6 Magnetisation in the xy-plane: chemical shift and the rotating frame
1.7 B₁ pulses precess
Summary
Chapter 2: Two additional simple NMR experiments: measuring T₁ and T₂
2.1 Relaxation: T₁ and T₂
2.2 Measuring T₁
2.3 Measuring T₂
2.4 Refocusing chemical shift
2.5 T₁ vs T₂
Summary
Chapter 3: J-coupling and the INEPT sequence element
3.1 J-coupling
3.2 ¹J_NH
3.3 J-coupling refocuses itself
3.4 Use of ¹J_NH to transfer magnetisation from ¹H to ¹⁵N: spin operators
3.5 Undesired effects of ¹H chemical shift evolution
3.6 Simultaneous 180º pulses solve the problem
3.7 Creating in-phase ¹⁵N magnetisation
3.8 Advantages of using ¹J_NH to create ¹⁵N excitation: INEPT
Summary
Chapter 4: The HSQC experiment (coupled, decoupled and gradient versions)
4.1 The coupled ¹H,¹⁵N-HSQC
4.2 Detecting the ¹⁵N chemical shift via t₁ incrementation
4.3 The decoupled ¹H,¹⁵N-HSQC
4.4 Pulsed field gradients (PFGs)
4.5 PFG versions of the HSQC
4.6 PFG nomenclature
Summary
Chapter 5: 3D HSQC-based double resonance experiments
5.1 Double resonance experiments
5.2 NOESY-HSQC
5.3 TOCSY-HSQC
Summary
Chapter 6: 3D HSQC-based triple resonance experiments
6.1 Triple resonance
6.2 HNCO
6.3 HNCA
6.4 HN(CO)CA
Summary
Chapter 7: 2D HSQC-based ¹⁵N relaxation experiments
7.1 ¹⁵N T₁
7.2 ¹⁵N T₂
7.3 ¹H,¹⁵N-NOE
Summary
Appendix A: Fourier transform, sign discrimination, artefact suppression
A.1 FID
A.2 Oscillatory components and decay rates → frequency and line width
A.3 Quadrature detection in the direct dimension
A.4 Artefacts associated with quadrature detection: QI and QG
A.5 Phase cycling: removing artefacts
A.6 Placing H₂O at the centre
A.7 Aliasing
A.8 Sign discrimination in the indirect dimension: States and TPPI
A.9 States–TPPI
Summary
Appendix B: Extracting dynamic information from relaxation data
B.1 Global and internal correlation times
B.2 Dominant ¹⁵N relaxation mechanisms
B.3 Dipolar coupling (DD)
B.4 Chemical shift anisotropy (CSA)
B.5 Spectral density function
B.6 Relaxation parameters are determined by J(ω)
B.7 R₂ ≥ R₁
B.8 Internal motions change J(ω)
B.9 Changes in J(ω) change T₁, T₂ and NOE
B.10 More complex motions and relaxation
Summary
Appendix C: Additional HSQC options: sensitivity enhancement, TROSY, deuteration
C.1 Sensitivity enhanced HSQC (SE-HSQC)
C.2 Gradient selection with sensitivity enhancement (GSE-HSQC)
C.3 Practical considerations of SE-HSQC and GSE-HSQC
C.4 TROSY: Transverse Relaxation-Optimised SpectroscopY
C.5 Deuteration and TROSY
Summary
Appendix D: HMQC
Appendix E: Miscellaneous concepts
E.1 Chemical exchange
E.2 Radiation damping
E.3 Initial t₁ value
E.4 Relaxation-optimised INEPT delays
E.5 Bloch–Siegert effect and Bloch–Siegert compensating pulses (BSCP)
Appendix F: Selected bibliography (some of my favourite books)
Appendix G: Partial pulse sequence and concept bibliography
G.1 Bloch–Siegert compensating pulses
G.2 Constant time
G.3 CPMG
G.4 CYCLOPS
G.5 Deuteration
G.6 Echo-antiecho
G.7 EXORCYCLE
G.8 GSE-HSQC
G.9 HMQC
G.10 HN(CO)CA
G.11 HNCA
G.12 HNCO
G.13 HSQC
G.14 Hypercomplex
G.15 INEPT
G.16 NOESY
G.17 Relaxation
G.18 Sensitivity enhancement
G.19 States–TPPI
G.20 TOCSY
G.21 TOCSY-HSQC and NOESY-HSQC
G.22 TPPI
G.23 TROSY
Appendix H: Symbols and definitions
Appendix I: Creating the cover image
Appendix J: Index

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