MULTIDIMENSIONAL SOLID-STATE NMR AND POLYMERS
CONTENTS PART I: THE THEORY OF SOLID-STATE NMR AND ITS EXPERIMENTS, THE BASICS OF SOLID-STATE NMR, THE VECTOR MODEL OF PULSED NMR, NUCLEI IN A STATIC, UNIFORM MAGNETIC ?ELD, THE EFFECT OF RF PULSES, THE QUANTUM MECHANICAL PICTURE: HAMILTONIANS AND THE SCHRÖDINGER EQUATION, QUANTUM MECHANICS AND NMR, NUCLEI IN A STATIC, UNIFORM ?ELD, EXPONENTIAL OPERATORS, ROTATION OPERATORS AND ROTATIONS, THE DENSITY MATRIX REPRESENTATION AND COHERENCES, COHERENCES AND POPULATIONS, THE DENSITY OPERATOR AT THERMAL EQUILIBRIUM, TIME EVOLUTION OF THE DENSITY MATRIX, NUCLEAR SPIN INTERACTIONS, THE CHEMICAL SHIFT AND CHEMICAL SHIFT ANISOTROPY, DIPOLE–DIPOLE COUPLING, BASIS SETS FOR MULTISPIN SYSTEMS, QUADRUPOLAR COUPLING, CALCULATING NMR POWDER PATTERNS, GENERAL FEATURES OF NMR EXPERIMENTS, MULTIDIMENSIONAL NMR, PHASE CYCLING, QUADRATURE DETECTION, THE NMR SPECTROMETER, REFERENCES, ESSENTIAL TECHNIQUES FOR SPIN- 1–2 NUCLEI, INTRODUCTION, MAGIC-ANGLE SPINNING (MAS), SPINNING SIDEBANDS, ROTOR OR ROTATIONAL ECHOES, REMOVING SPINNING SIDEBANDS, MAGIC-ANGLE SPINNING FOR HOMONUCLEAR DIPOLAR COUPLINGS, HIGH-POWER DECOUPLING, MULTIPLE PULSE DECOUPLING SEQUENCES, AVERAGE HAMILTONIAN THEORY AND THE TOGGLING FRAME, CROSS-POLARIZATION, THEORY, EXPERIMENTAL DETAILS, CROSS-POLARIZATION AND MAGIC-ANGLE SPINNING, SOLID OR QUADRUPOLE ECHO PULSE SEQUENCE, DIPOLAR COUPLING: ITS MEASUREMENT AND USES, THE DIPOLAR HAMILTONIAN IN TERMS OF SPHERICAL TENSOR OPERATORS, TECHNIQUES FOR MEASURING HOMONUCLEAR DIPOLAR COUPLINGS, RECOUPLING PULSE SEQUENCES, ANALYSIS OF THE DRAMA PULSE SEQUENCE, DOUBLE-QUANTUM ?LTERED EXPERIMENTS, ROTATIONAL RESONANCE, EXCITATION OF DOUBLE-QUANTUM COHERENCE UNDER MAGIC-ANGLE SPINNING, TECHNIQUES FOR MEASURING HETERONUCLEAR DIPOLAR COUPLINGS, ANALYSIS OF THE C7 PULSE SEQUENCE FOR EXCITING DOUBLE-QUANTUM COHERENCE IN DIPOLAR-COUPLED SPIN PAIRS, SPIN-ECHO DOUBLE RESONANCE, THEORY OF ROTATIONAL RESONANCE, ROTATIONAL-ECHO DOUBLE RESONANCE, ANALYSIS OF THE REDOR EXPERIMENT, TECHNIQUES FOR DIPOLAR-COUPLED QUADRUPOLAR (SPIN- 1–2) PAIRS, TRANSFER OF POPULATION IN DOUBLE RESONANCE, ROTATIONAL ECHO, ADIABATIC PASSAGE, DOUBLE RESONANCE, TECHNIQUES FOR MEASURING DIPOLAR COUPLINGS BETWEEN QUADRUPOLAR NUCLEI, CORRELATION EXPERIMENTS, SYSTEMS, HOMONUCLEAR CORRELATION EXPERIMENTS FOR QUADRUPOLAR SPIN SYSTEMS, HETERONUCLEAR CORRELATION EXPERIMENTS FOR SPIN- 1–2, SPIN-COUNTING EXPERIMENTS, THE FORMATION OF MULTIPLE-QUANTUM COHERENCES, IMPLEMENTATION OF SPIN-COUNTING EXPERIMENTS, QUADRUPOLE COUPLING: ITS MEASUREMENT AND USES, THE QUADRUPOLE HAMILTONIAN, HIGH-RESOLUTION NMR EXPERIMENTS FOR HALF-INTEGER QUADRUPOLAR NUCLEI, MAGIC-ANGLE SPINNING, DOUBLE ROTATION, DYNAMIC-ANGLE SPINNING, MULTIPLE-QUANTUM MAGIC-ANGLE SPINNING, RECORDING TWO-DIMENSIONAL DATASETS FOR DAS AND MQMAS, OTHER TECHNIQUES FOR HALF-INTEGER QUADRUPOLAR NUCLEI, QUADRUPOLE NUTATION, SHIELDING AND CHEMICAL SHIFT, THE RELATIONSHIP BETWEEN THE SHIELDING TENSOR AND ELECTRONIC STRUCTURE, MEASURING CHEMICAL SHIFT ANISOTROPIES, MAGIC-ANGLE SPINNING WITH RECOUPLING PULSE SEQUENCES, VARIABLE ANGLE SPINNING EXPERIMENTS, MAGIC-ANGLE TURNING, TWO-DIMENSIONAL SEPARATION OF SPINNING SIDEBAND PATTERNS, PART II: APLICATIONS OF SOLID-STATE NMR, NMR TECHNIQUES FOR STUDYING MOLECULAR MOTION IN SOLIDS, POWDER LINESHAPE ANALYSIS, SIMULATING POWDER PATTERN LINESHAPES, RESOLVING POWDER PATTERNS, USING HOMONUCLEAR DIPOLAR COUPLING LINESHAPES: THE WISE EXPERIMENT, RELAXATION TIME STUDIES, EXCHANGE EXPERIMENTS, ACHIEVING PURE ABSORPTION LINESHAPES IN EXCHANGE SPECTRA, INTERPRETING TWO-DIMENSIONAL EXCHANGE SPECTRA, 2H NMR, MEASURING 2H NMR SPECTRA, 2H LINESHAPE SIMULATIONS, 2H EXCHANGE EXPERIMENTS, RESOLVING 2H POWDER PATTERNS, MOLECULAR STRUCTURE DETERMINATION: APPLICATIONS IN BIOLOGY, USEFUL NUCLEI IN BIOLOGICAL SOLID-STATE NMR, AN OVERVIEW OF NUCLEAR SPIN INTERACTIONS ENCOUNTERED IN BIOLOGICAL SAMPLES, CHEMICAL SHIFTS, IS A PROTEIN IN A DISORDERED OR IN THE NATIVE WELL-STRUCTURED FORM? CHEMICAL SHIFT ANISOTROPY, INTERSPIN DISTANCE MEASUREMENTS, HETERONUCLEAR DISTANCE MEASUREMENTS: THE REDOR EXPERIMENT, HOMONUCLEAR DISTANCE MEASUREMENTS: ROTATIONAL RESONANCE, HOMONUCLEAR DISTANCE MEASUREMENTS: DRAWS, RFDR, (FP)-RFDR, TORSION ANGLE MEASUREMENTS, CHEMICAL SHIFT–CHEMICAL SHIFT TENSOR CORRELATION EXPERIMENTS, DIPOLAR–CHEMICAL SHIFT TENSOR CORRELATION EXPERIMENTS, EXPERIMENTS CORRELATING TWO DIPOLE–DIPOLE COUPLING TENSORS, 13C MULTIPLE-QUANTUM NMR SPECTROSCOPY, NMR STUDIES OF OXIDE GLASS STRUCTURE, THE ‘STRUCTURE’ OF A GLASS, THE EXTENT OF DISORDER, LIQUIDS VS GLASSES, NMR TECHNIQUES FOR STUDYING GLASS STRUCTURE, STATIC SAMPLES, SIMPLE MAS SPECTRA, TECHNIQUES FOR OBSERVING 1H AND 19F IN GLASSES, CROSS-POLARIZATION TECHNIQUES, OTHER DOUBLE RESONANCE EXPERIMENTS, TWO-DIMENSIONAL CORRELATION EXPERIMENTS, TECHNIQUES THAT ELIMINATE SECOND-ORDER QUADRUPOLAR BROADENING (DOR, DAS, MQMAS), SPIN-LATTICE RELAXATION AND STRUCTURE, APPLICATIONS TO SPECI?C GLASS SYSTEMS, BORON-CONTAINING OXIDE GLASSES, SILICATE, ALUMINOSILICATE AND GERMANATE GLASSES, HYDROGEN-CONTAINING SPECIES IN OXIDE GLASSES, PHOSPHATE GLASSES, THERMAL HISTORY EFFECTS, LONG-RANGE STRUCTURAL ANISOTROPY, POROUS MATERIALS, ZEOLITES, ALUMINOPHOSPHATE MOLECULAR SIEVES, MESOPOROUS MOLECULAR SIEVES, SPECTROSCOPIC CONSIDERATIONS, MONITORING THE COMPOSITION OF THE ALUMINOSILICATE FRAMEWORK OF ZEOLITES, ORDERING OF ATOMS IN TETRAHEDRAL FRAMEWORKS, RESOLVING CRYSTALLOGRAPHICALLY INEQUIVALENT TETRAHEDRAL SITES, SPECTRAL RESOLUTION, LINESHAPE AND RELAXATION, DEALUMINATION AND REALUMINATION OF ZEOLITES, NMR STUDIES OF BRØNSTED ACID SITES, CHEMICAL STATUS OF GUEST ORGANICS IN THE INTRACRYSTALLINE SPACE, IN SITU STUDIES OF CATALYTIC REACTIONS, DIRECT OBSERVATION OF SHAPE SELECTIVITY, MULTINUCLEAR STUDIES OF SORBED SPECIES, 129XE NMR, NEW NMR TECHNIQUES FOR THE STUDY OF MOLECULAR SIEVES, CONCLUSIONS, SOLID POLYMERS, STRUCTURE OF POLYMERS, POLYMER DYNAMICS, NMR METHODS FOR STUDYING POLYMER DYNAMICS, PHASE SEPARATION OF POLYMERS, ORIENTED POLYMERS, FLUOROPOLYMERS, LIQUID-CRYSTALLINE MATERIALS, THE LIQUID-CRYSTALLINE STATE, ORIENTATIONAL ORDER, PHASE SYMMETRY, MOLECULAR ORIENTATIONAL ORDER, THE GENERAL, TIME-INDEPENDENT NMR HAMILTONIAN FOR LIQUID- CRYSTALLINE SAMPLES, MOLECULAR ORDER PARAMETERS, DIFFERENT REPRESENTATIONS OF THE ORDER PARAMETERS, MOLECULAR ORDER PARAMETERS AND THE SYMMETRY OF RIGID MOLECULES, DIRECTOR ALIGNMENT, DIPOLAR COUPLINGS BETWEEN NUCLEI IN RIGID MOLECULES IN LIQUID-CRYSTALLINE PHASES, GEOMETRY OF RIGID MOLECULES FROM DIPOLAR COUPLINGS, DEUTERIUM QUADRUPOLAR SPLITTINGS FOR RIGID MOLECULES IN LIQUID-CRYSTALLINE PHASES, SIGNS OF QUADRUPOLAR SPLITTINGS, CHEMICAL SHIFT ANISOTROPY FOR RIGID MOLECULES IN LIQUID-CRYSTALLINE PHASES, ELECTRON-MEDIATED SPIN–SPIN COUPLING IN LIQUID-CRYSTALLINE SAMPLES, THE DETERMINATION OF THE STRUCTURE, ORIENTATIONAL ORDER AND CONFORMATIONS OF ?EXIBLE MOLECULES IN LIQUID-CRYSTALLINE SAMPLES, MOLECULAR ORIENTATIONAL ORDER FOR ?EXIBLE MOLECULES, CONFORMATIONALLY DEPENDENT ORDER PARAMETERS, DETERMINATION OF THE CONFORMATIONALLY DEPENDENT ORIENTATIONAL ORDER PARAMETERS AND THE CONFORMATIONAL DISTRIBUTIONS OF MOLECULES IN LIQUID-CRYSTALLINE PHASES FROM NMR PARAMETERS, THEORETICAL MODELS FOR PLC(BMD, GMD, (JL)), NMR EXPERIMENTS FOR LIQUID-CRYSTALLINE SAMPLES, SIMPLI?CATION OF PROTON SPECTRA BY PARTIAL DEUTERIATION PLUS DEUTERIUM DECOUPLING, MULTIPLE-QUANTUM SPECTRA, SYMMETRY SELECTION BY MULTIPLE-QUANTUM ?LTERING, ROTATION OF LIQUID-CRYSTALLINE SAMPLES, LIQUID-CRYSTALLINE MIXED SOLVENTS CONSISTING OF TWO COMPONENTS OF OPPOSITE SIGN OF THE ANISOTROPY IN THEIR MAGNETIC SUSCEPTIBILITY, THE SEPARATED LOCAL ?ELD EXPERIMENT, SPECTRA OF CHIRAL AND PROCHIRAL MOLECULES IN CHIRAL LIQUID- CRYSTALLINE PHASES,