8.3. 2.4 ROESY, Rotating Frame Overhauser Enhanced Spectroscopy 230 8. 3.2.5 NOESY VS ROESY 231 8.3.2.6 Other Homonuclear Autocorrelation Experiments 23 8.3.3 Gradient Homonuclear 2D NMR Experiments 232 8.3.4 Heteronuclear Shift Correlation 234 8.3.5 Direct heteronuclear Chemical Shift Correlation Methods 234 8.3.5.1 HMQC, Heteronuclear Multiple Quantum Coherence 234 HSQC, Heteronuclear Single Quantum Coherence Chemical Shift 8.3.6.1 Multiplicity-edited Heteronuclear Shift Correlation Experiments 237 8.3.6.2 Accordion-optimized Direct Heteronuclear Shift Correlation Experiments 239 Long-range Heteronuclear Chemical Shift Correlation 240 8.3.7.1 HMBC, Heteronuclear Multiple Bond Correlation 242 8.3.7.2 Variants of the Basic HMBC Experiment 243 8.3.7.3 Accordion-optimized Long-range Heteronuclear Shift Correlation Methods. 244 8.3.7. 4 JJ-HMBC 248 8.3.7.5 Relative Sensitivity of Long-range Heteronuclear Shift Correlation Experiments 251 8.3.7.6 Applications of Accordion-optimized Long-range Heteronuclear Shift Correlation Experiments 252 8.3.8 Hyphenated-2D NMR Experiments 252 8.3.9 One-dimensional Analogues of 2D NMR Experiments 255 8.3.10 Gradient 1D NOESY 255 8.3.11 Selective 1D Long- range Heteronuclear Shift Correlation Experiments 257 8.3.12 Small Sample NMR Studies 257 9 Solid- State NMr 269 Solid-state NMR Lineshapes 272 9.2.1 The Orientational Dependence of the NMR Resonance Frequency 272 9.2.2 Single-crystal NMR 273 9.2.3 Powder Spectra 275 9.2.4 One-dimensional ZH NMR 278 Magic-angle Spinnin 9.3.1 CP MAS NMR 281 9.3.2 H Solid- State Nmr 285 Recoupling Methods 287 9.4.1 Heteronuclear Dipolar-coupled Spins: REDOR 287 Homonuclear Dipolar-coupled Spins 290 94.3 The CSA: CODEX 291 Homonuclear Two-dimensional Experiments 2928.3.2.4 ROESY, Rotating Frame Overhauser Enhanced Spectroscopy 230 8.3.2.5 NOESY vs. ROESY 231 8.3.2.6 Other Homonuclear Autocorrelation Experiments 231 8.3.3 Gradient Homonuclear 2D NMR Experiments 232 8.3.4 Heteronuclear Shift Correlation 234 8.3.5 Direct Heteronuclear Chemical Shift Correlation Methods 234 8.3.5.1 HMQC, Heteronuclear Multiple Quantum Coherence 234 8.3.6 HSQC, Heteronuclear Single Quantum Coherence Chemical Shift Correlation Techniques 236 8.3.6.1 Multiplicity-edited Heteronuclear Shift Correlation Experiments 237 8.3.6.2 Accordion-optimized Direct Heteronuclear Shift Correlation Experiments 239 8.3.7 Long-range Heteronuclear Chemical Shift Correlation 240 8.3.7.1 HMBC, Heteronuclear Multiple Bond Correlation 242 8.3.7.2 Variants of the Basic HMBC Experiment 243 8.3.7.3 Accordion-optimized Long-range Heteronuclear Shift Correlation Methods. 244 8.3.7.4 2 J 3 J-HMBC 248 8.3.7.5 Relative Sensitivity of Long-range Heteronuclear Shift Correlation Experiments 251 8.3.7.6 Applications of Accordion-optimized Long-range Heteronuclear Shift Correlation Experiments 252 8.3.8 Hyphenated-2D NMR Experiments 252 8.3.9 One-dimensional Analogues of 2D NMR Experiments 255 8.3.10 Gradient 1D NOESY 255 8.3.11 Selective 1D Long-range Heteronuclear Shift Correlation Experiments 257 8.3.12 Small Sample NMR Studies 257 8.4 Conclusions 262 9 Solid-State NMR 269 9.1 Introduction 269 9.2 Solid-state NMR Lineshapes 272 9.2.1 The Orientational Dependence of the NMR Resonance Frequency 272 9.2.2 Single-crystal NMR 273 9.2.3 Powder Spectra 275 9.2.4 One-dimensional 2 H NMR 278 9.3 Magic-angle Spinning 280 9.3.1 CP MAS NMR 281 9.3.2 1 H Solid-State NMR 285 9.4 Recoupling Methods 287 9.4.1 Heteronuclear Dipolar-coupled Spins: REDOR 287 9.4.2 Homonuclear Dipolar-coupled Spins 290 9.4.3 The CSA: CODEX 291 9.5 Homonuclear Two-dimensional Experiments 292 Contents IX