200 and more NMR experiments : a practical course / Stefan Berger, Siegmar Braun.

Format:

Book

Author/Creator:

Berger, Stefan, 1946-

Contributor:

Braun, Siegmar.

Hazel M. Hussong Fund.

Language:

English

Subjects (All):

Nuclear magnetic resonance spectroscopy.

Physical Description:

xv, 838 pages : illustrations ; 24 cm

Edition:

Third revised and expanded edition.

Other Title:

Two hundred and more NMR experiments

NMR experiments

Place of Publication:

Leipzig : Wiley-VCH, [2004]

Summary:

This third edition of the book, following its two highly successful predecessors, has been revised and expanded to 206 experiments. They are organized in 15 chapters, covering test procedures and routine spectra, variable temperature measurements, the use of auxiliary reagents, 1D multipulse experiments, spectra of heteronuclides, and the application of selective pulses. The second and third dimensions are introduced using pulsed field gradients, and experiments on solid state materials are described. A key part describes 3D experiments on the protein ubiquitin with 76 amino acids.

Contents:

Chapter 1 The NMR Spectrometer 1

1.1 Components of an NMR Spectrometer 1

1.1.1 The Magnet 1

1.1.2 The Spectrometer Cabinet 2

1.1.3 The Computer 3

1.1.4 Maintenance 3

1.2 Tuning a Probe-Head 3

1.3 The Lock Channel 4

1.4 The Art of Shimming 6

1.4.1 The Shim Gradients 6

1.4.2 The Shimming Procedure 8

1.4.3 Gradient Shimming 11

Chapter 2 Determination of Pulse-Duration 14

Exp. 2.1 Determination of the 90[degree] [superscript 1]H Transmitter Pulse-Duration 15

Exp. 2.2 Determination of the 90[degree] [superscript 13]C Transmitter Pulse-Duration 18

Exp. 2.3 Determination of the 90[degree] [superscript 1]H Decoupler Pulse-Duration 21

Exp. 2.4 The 90[degree] [superscript 1]H Pulse with Inverse Spectrometer Configuration 24

Exp. 2.5 The 90[degree] [superscript 13]C Decoupler Pulse with Inverse Configuration 27

Exp. 2.6 Composite Pulses 30

Exp. 2.7 Radiation Damping 33

Exp. 2.8 Pulse and Receiver Phases 36

Exp. 2.9 Determination of Radiofrequency Power 39

Chapter 3 Routine NMR Spectroscopy and Standard Tests 43

Exp. 3.1 The Standard [superscript 1]H NMR Experiment 44

Exp. 3.2 The Standard [superscript 13]C NMR Experiment 49

Exp. 3.3 The Application of Window Functions 54

Exp. 3.4 Computer-Aided Spectral Analysis 58

Exp. 3.5 Line Shape Test for [superscript 1]H NMR Spectroscopy 61

Exp. 3.6 Resolution Test for [superscript 1]H NMR Spectroscopy 64

Exp. 3.7 Sensitivity Test for [superscript 1]H NMR Spectroscopy 67

Exp. 3.8 Line Shape Test for [superscript 13]C NMR Spectroscopy 70

Exp. 3.9 ASTM Sensitivity Test for [superscript 13]C NMR Spectroscopy 73

Exp. 3.10 Sensitivity Test for [superscript 13]C NMR Spectroscopy 76

Exp. 3.11 Quadrature Image Test 79

Exp. 3.12 Dynamic Range Test for Signal Amplitudes 82

Exp. 3.13 13[degree] Phase Stability Test 85

Exp. 3.14 Radiofrequency Field Homogeneity 88

Chapter 4 Decoupling Techniques 91

Exp. 4.1 Decoupler Calibration for Homonuclear Decoupling 92

Exp. 4.2 Decoupler Calibration for Heteronuclear Decoupling 95

Exp. 4.3 Low-Power Calibration for Heteronuclear Decoupling 98

Exp. 4.4 Homonuclear Decoupling 101

Exp. 4.5 Homonuclear Decoupling at Two Frequencies 104

Exp. 4.6 The Homonuclear SPT Experiment 107

Exp. 4.7 The Heteronuclear SPT Experiment 110

Exp. 4.8 The Basic Homonuclear NOE Difference Experiment 113

Exp. 4.9 1D Nuclear Overhauser Difference Spectroscopy 116

Exp. 4.10 1D NOE Spectroscopy with Multiple Selective Irradiation 119

Exp. 4.11 [superscript 1]H Off-Resonance Decoupled [superscript 13]C NMR Spectra 122

Exp. 4.12 The Gated [superscript 1]H-Decoupling Technique 125

Exp. 4.13 The Inverse Gated [superscript 1]H-Decoupling Technique 128

Exp. 4.14 [superscript 1]H Single-Frequency Decoupling of [superscript 13]C NMR Spectra 131

Exp. 4.15 [superscript 1]H Low-Power Decoupling of [superscript 13]C NMR Spectra 134

Exp. 4.16 Measurement of the Heteronuclear Overhauser Effect 137

Chapter 5 Dynamic NMR Spectroscopy 140

Exp. 5.1 Low-Temperature Calibration Using Methanol 141

Exp. 5.2 High-Temperature Calibration Using 1,2-Ethanediol 145

Exp. 5.3 Dynamic [superscript 1]H NMR Spectroscopy on Dimethylformamide 149

Exp. 5.4 The Saturation Transfer Experiment 152

Exp. 5.5 Measurement of the Rotating-Frame Relaxation Time T[subscript 1 rho] 155

Chapter 6 1D Multipulse Sequences 159

Exp. 6.1 Measurement of the Spin-Lattice Relaxation Time T[subscript 1] 160

Exp. 6.2 Measurement of the Spin-Spin Relaxation Time T[subscript 2] 164

Exp. 6.3 [superscript 13]C NMR Spectra with SEFT 167

Exp. 6.4 [superscript 13]C NMR Spectra with APT 170

Exp. 6.5 The Basic INEPT Technique 173

Exp. 6.6 INEPT+ 176

Exp. 6.7 Refocused INEPT 179

Exp. 6.8 Reverse INEPT 182

Exp. 6.9 DEPT-135 185

Exp. 6.10 Editing [superscript 13]C NMR Spectra Using DEPT 188

Exp. 6.11 DEPTQ 191

Exp. 6.12 Multiplicity Determination Using PENDANT 194

Exp. 6.13 1D-INADEQUATE 197

Exp. 6.14 The BIRD Filter 201

Exp. 6.15 TANGO 204

Exp. 6.16 The Heteronuclear Double-Quantum Filter 207

Exp. 6.17 Purging with a Spin-Lock Pulse 210

Exp. 6.18 Water Suppression by Presaturation 213

Exp. 6.19 Water Suppression by the Jump-and-Return Method 216

Chapter 7 NMR Spectroscopy with Selective Pulses 219

Exp. 7.1 Determination of a Shaped 90[degree] [superscript 1]H Transmitter Pulse 220

Exp. 7.2 Determination of a Shaped 90[degree] [superscript 1]H Decoupler Pulse 223

Exp. 7.3 Determination of a Shaped 90[degree] [superscript 13]C Decoupler Pulse 226

Exp. 7.4 Selective Excitation Using DANTE 229

Exp. 7.5 SELCOSY 232

Exp. 7.6 SELINCOR: Selective Inverse H,C Correlation via [superscript 1]J(C,H) 235

Exp. 7.7 SELINQUATE 238

Exp. 7.8 Selective TOCSY 242

Exp. 7.9 INAPT 246

Exp. 7.10 Determination of Long-Range C,H Coupling Constants 249

Exp. 7.11 SELRESOLV 252

Exp. 7.12 SERF 255

Chapter 8 Auxiliary Reagents, Quantitative Determinations, and Reaction Mechanisms 258

Exp. 8.1 Signal Separation Using a Lanthanide Shift Reagent 259

Exp. 8.2 Signal Separation of Enantiomers Using a Chiral Shift Reagent 262

Exp. 8.3 Signal Separation of Enantiomers Using a Chiral Solvating Agent 265

Exp. 8.4 Determination of Enantiomeric Purity with Pirkle's Reagent 268

Exp. 8.5 Determination of Enantiomeric Purity by [superscript 31]P NMR 271

Exp. 8.6 Determination of Absolute Configuration by the Advanced Mosher Method 274

Exp. 8.7 Aromatic Solvent-Induced Shift (ASIS) 277

Exp. 8.8 NMR Spectroscopy of OH Protons and H/D Exchange 280

Exp. 8.9 Water Suppression Using an Exchange Reagent 283

Exp. 8.10 Isotope Effects on Chemical Shielding 286

Exp. 8.11 pK[subscript a] Determination by [superscript 13]C NMR 290

Exp. 8.12 Determination of Association Constants K[subscript a] 293

Exp. 8.13 Saturation Transfer Difference NMR 298

Exp. 8.14 The Relaxation Reagent Cr(acac)[subscript 3] 302

Exp. 8.15 Determination of Paramagnetic Susceptibility by NMR 305

Exp. 8.16 [superscript 1]H and [superscript 13]C NMR of Paramagnetic Compounds 308

Exp. 8.17 The CIDNP Effect 312

Exp. 8.18 Quantitative [superscript 1]H NMR Spectroscopy: Determination of the Alcohol Content of Polish Vodka 315

Exp. 8.19 Quantitative [superscript 13]C NMR Spectroscopy with Inverse Gated [superscript 1]H-Decoupling 318

Exp. 8.20 NMR Using Liquid-Crystal Solvents 321

Chapter 9 Heteronuclear NMR Spectroscopy 324

Exp. 9.1 [superscript 1]H-Decoupled [superscript 15]N NMR Spectra Using DEPT 330

Exp. 9.2 [superscript 1]H-Coupled [superscript 15]N NMR Spectra Using DEPT 333

Exp. 9.3 [superscript 19]F NMR Spectroscopy 336

Exp. 9.4 [superscript 29]Si NMR Spectroscopy Using DEPT 339

Exp. 9.5 [superscript 29]Si NMR Spectroscopy Using Spin-Lock Polarization 342

Exp. 9.6 [superscript 119]Sn NMR Spectroscopy 346

Exp. 9.7 [superscript 2]H NMR Spectroscopy 349

Exp. 9.8 [superscript 11]B NMR Spectroscopy 352

Exp. 9.9 [superscript 17]O NMR Spectroscopy Using RIDE 355

Exp. 9.10 [superscript 47/49]Ti NMR Spectroscopy Using ARING 358

Chapter 10 The Second Dimension 362

Exp. 10.1 2D J-Resolved [superscript 1]H NMR Spectroscopy 367

Exp. 10.2 2D J-Resolved [superscript 13]C NMR Spectroscopy 370

Exp. 10.3 The Basic H,H-COSY Experiment 373

Exp. 10.4 Long-Range COSY 377

Exp. 10.5 Phase-Sensitive COSY 380

Exp. 10.6 Phase-Sensitive COSY-45 383

Exp. 10.7 E.COSY 386

Exp. 10.8 Double-Quantum-Filtered COSY with Presaturation 389

Exp. 10.9 Fully Coupled C,H Correlation (FUCOUP) 393

Exp. 10.10 C,H-Correlation by Polarization Transfer (HETCOR) 396

Exp. 10.11 Long-Range C,H-Correlation by Polarization Transfer 399

Exp. 10.12 C,H Correlation via Long-Range Couplings (COLOC) 402

Exp. 10.13 The Basic HMQC Experiment 405

Exp. 10.14 Phase-Sensitive HMQC with BIRD Filter and GARP Decoupling 409

Exp. 10.15 Poor Man's Gradient HMQC 412

Exp.

10.16 Phase-Sensitive HMBC with BIRD Filter 415

Exp. 10.17 The Basic HSQC Experiment 418

Exp. 10.18 The HOHAHA or TOCSY Experiment 422

Exp. 10.19 HETLOC 426

Exp. 10.20 The NOESY Experiment 430

Exp. 10.21 The CAMELSPIN or ROESY Experiment 434

Exp. 10.22 The HOESY Experiment 438

Exp. 10.23 2D-INADEQUATE 441

Exp. 10.24 The EXSY Experiment 445

Exp. 10.25 X,Y-Correlation 448

Chapter 11 1D NMR Spectroscopy with Pulsed Field Gradients 453

Exp. 11.1 Calibration of Pulsed Field Gradients 455

Exp. 11.2 Gradient Pre-emphasis 458

Exp. 11.3 Gradient Amplifier Test 461

Exp. 11.4 Determination of Pulsed Field Gradient Ring-Down Delays 464

Exp. 11.5 The Pulsed Field Gradient Spin-Echo Experiment 467

Exp. 11.6 Excitation Pattern of Selective Pulses 470

Exp. 11.7 The Gradient Heteronuclear Double-Quantum Filter 474

Exp. 11.8 The Gradient zz-Filter 477

Exp. 11.9 The Gradient-Selected Dual Step Low-Pass Filter 480

Exp. 11.10 gs-SELCOSY 484

Exp. 11.11 gs-SELTOCSY 488

Exp. 11.12 DPFGSE-NOE 492

Exp. 11.13 gs-SELINCOR 496

Exp. 11.14 [alpha]/[beta]-SELINCOR-TOCSY 499

Exp. 11.15 GRECCO 503

Exp. 11.16 WATERGATE 506

Exp. 11.17 Water Suppression by Excitation Sculpting 509

Exp. 11.18 Solvent Suppression Using WET 512

Exp. 11.19 DOSY 515

Exp. 11.20 INEPT-DOSY 518

Exp. 11.21 DOSY-HMQC 521

Chapter 12 2D NMR Spectroscopy With Field Gradients 525

Exp. 12.1 gs-COSY 526

Exp. 12.2 Constant-Time COSY 530

Exp. 12.3 Phase-Sensitive gs-DQF-COSY 534

Exp. 12.4 gs-HMQC 538

Exp. 12.5 gs-HMBC 542

Exp. 12.6 ACCORD-HMBC 546

Exp. 12.7 HMSC 550

Exp. 12.8 Phase-Sensitive gs-HSQC with Sensitivity Enhancement 554

Exp. 12.9 Edited HSQC with Sensitivity Enhancement 558

Exp. 12.10 HSQC with Adiabatic Pulses for High-Field Instruments 563

Exp. 12.11 gs-TOCSY 567

Exp. 12.12 gs-HMQC-TOCSY 571

Exp. 12.13 gs-HETLOC 575

Exp. 12.14 gs-J-Resolved HMBC 581

Exp. 12.15 2Q-HMBC 585

Exp. 12.16 [superscript 1]H-Detected 2D INEPT-INADEQUATE 589

Exp. 12.17 1,1-ADEQUATE 593

Exp. 12.18 1,n-ADEQUATE 597

Exp. 12.19 gs-NOESY 601

Exp. 12.20 gs-HSQC-NOESY 604

Exp. 12.21 gs-HOESY 608

Exp. 12.22 [superscript 1]H, [superscript 15]N Correlation with gs-HMQC 612

Chapter 13 The Third Dimension 616

Exp. 13.1 3D HMQC-COSY 618

Exp. 13.2 3D gs-HSQC-TOCSY 622

Exp. 13.3 3D H,C,P-Correlation 626

Exp. 13.4 3D HMBC 630

Chapter 14 Solid-State NMR Spectroscopy 634

Exp. 14.1 Shimming Solid-State Probe-Heads 635

Exp. 14.2 Adjusting the Magic Angle 639

Exp. 14.3 Hartmann-Hahn Matching 642

Exp. 14.4 The Basic CP/MAS Experiment 645

Exp. 14.5 TOSS 649

Exp. 14.6 SELTICS 653

Exp. 14.7 Connectivity Determination in the Solid State 656

Exp. 14.8 REDOR 659

Exp. 14.9 High-Resolution Magic-Angle Spinning 663

Chapter 15 Protein NMR 666

Exp. 15.1 Pulse Determination for Protein NMR 670

Exp. 15.2 HN-HSQC 673

Exp. 15.3 HC-HSQC 678

Exp. 15.4 MUSIC 682

Exp. 15.5 HN-Correlation using TROSY 688

Exp. 15.6 HN-TOCSY-HSQC 692

Exp. 15.7 HNCA 698

Exp. 15.8 HN(CO)CA 705

Exp. 15.9 HNCO 711

Exp. 15.10 HN(CA)CO 718

Exp. 15.11 HCACO 725

Exp. 15.12 HCCH-TOCSY 732

Exp. 15.13 CBCANH 739

Exp. 15.14 CBCA(CO)NH 746

Exp. 15.15 HBHA(CBCACO)NH 753

Exp. 15.16 HN(CA)NNH 760

Exp. 15.17 HN-NOESY-HSQC 766

Exp. 15.18 HC-NOESY-HSQC 773

Exp. 15.19 3D HCN-NOESY 779

Exp. 15.20 HNCA-J 785

Appendix 1 Pulse Programs 791

Appendix 2 Instrument Dialects 794

Appendix 3 Classification of Experiments 797

Appendix 4 Elementary Product Operator Formalism Rules 799

Appendix 5 Chemical Shift and Spin-Coupling Data for Ethyl Crotonate and Strychnine 802.

Notes:

Includes bibliographical references and index.

Local Notes:

Acquired for the Penn Libraries with assistance from the Hazel M. Hussong Fund.

ISBN:

3527310673

OCLC:

55685718