REDOR-Based Heteronuclear Dipolar Correlation Experiments in Multi-Spin Systems: Rotor-Encoding, Directing, and Multiple Distance and Angle Determination

Saalwächter, Kay; Schnell, Ingo

doi:10.1006/snmr.2002.0079

Cited by 78 publications

(127 citation statements)

References 69 publications

(104 reference statements)

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“…The synthesis of N-butylaminocarbonyl-6-tridecyl-isocytosine [22] started from 15 N 3 -guanidine, C(*NH)(*NH 2 ) 2 , such that in the resulting molecules the three nitrogen atoms belonging to the isocytosine unit are 15 N. The pyrimidinone and pyrimidinol forms of the dimers were obtained by recrystallising the material from CHCl 3 and dimethylformamide (DMF), respectively. [22] The 1 H and 15 N solid-state NMR spectra obtained on both compounds under fast MAS conditions provided sufficient spectral resolution to distinguish all different 1 H and 15 N sites.…”

Section: Methodsmentioning

confidence: 99%

“…13 15 N sites in the spectra. The experimental schemes are based on the rotational-echo double-resonance (REDOR) scheme [23][24][25] in order to selectively recouple the heteronuclear 1 H-…”

Section: Nuclear Magnetic Resonance Spectroscopymentioning

confidence: 99%

“…[7][8][9] Magic-angle spinning (MAS), performed at high frequencies (above 25 kHz) and-or in combination with-radio-frequency (RF) pulse schemes, forms the basis of high-resolution solid-state NMR spectroscopy, including 13 C, 15 N and even 1 H, despite their tendency to exhibit notoriously broad lines with little resolution. [5] The chemical-shift resolution of resonance lines allows sites of interest to be distinguished and identified, and the selectivity provided by such spectra can readily be combined with structural information.…”

Section: Introductionmentioning

confidence: 99%

“…Such measurements can be performed in a particularly simple, robust and sensitive manner by using rotor-encoded recoupling schemes. [5,[13][14][15] In two-dimensional experiments, the signal is amplitude-modulated in the indirect (t 1 ) dimension and can readily be converted into a characteristic pattern of spinning sidebands by Fourier transformation. These patterns are resolved in the direct (t 2 or F 2 ) dimension according to the chemical shift of the detected nuclei and sensitively reflect the strength of the underlying dipole-dipole couplings.…”

Section: Introductionmentioning

confidence: 99%

“…The pulse sequences are schematically depicted in Figure 1 where two types of experiment are distinguished, namely rotor-encoded REDOR (REREDOR) [15,26] and heteronuclear dipolar-order rotor encoding (HDOR). [14,27] This distinction refers to the different coherence pathways selected in the two experiments.…”

mentioning

confidence: 99%

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Determining the Geometry of Hydrogen Bonds in Solids with Picometer Accuracy by Quantum‐Chemical Calculations and NMR Spectroscopy

et al. 2005

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The structure of multiply hydrogen‐bonded systems is determined with picometer accuracy by a combined solid‐state NMR and quantum‐chemical approach. On the experimental side, advanced 1H15N dipolar recoupling NMR techniques are capable of providing proton–nitrogen distances of up to about 250 pm with an accuracy level of ±1 pm for short distances (i.e., around 100 pm) and ±5 pm for longer ones (i.e., 180 to 250 pm). The experiments were performed under fast magic‐angle spinning, which ensures sufficient dipolar decoupling and spectral resolution of the 1H resonance lines. On the quantum‐chemical side, the structures of the hydrogen‐bonded systems were computationally optimised, yielding complete sets of nitrogen–proton and proton–proton distances, which are essential for correctly interpreting the experimental NMR data. In this way, nitrogen–proton distances were determined with picometer accuracy, so that vibrational averaging effects on dipole–dipole couplings need to be considered. The obtained structures were finally confirmed by the complete agreement of computed and experimental 1H and 15N chemical shifts. This demonstrates that solid‐state NMR and quantum‐chemical methods ideally complement each other and, in a combined manner, represent a powerful approach for reliable, high‐precision structure determination whenever scattering techniques are inapplicable.

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Section: Methodsmentioning

confidence: 99%

Section: Nuclear Magnetic Resonance Spectroscopymentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

mentioning

confidence: 99%

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Determining the Geometry of Hydrogen Bonds in Solids with Picometer Accuracy by Quantum‐Chemical Calculations and NMR Spectroscopy

et al. 2005

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Nuclear Magnetic Resonance (NMR) Spectroscopy of Inorganic/Organometallic Molecules

Iggo

Liu

Khimyak

2005

Encyclopedia of Inorganic Chemistry

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NMR spectroscopy is an indispensable spectroscopic tool for the characterization of inorganic compounds. This contribution provides a guide to the application of recent advances in high‐resolution, solid‐state, and high‐pressure NMR spectroscopic methods to organometallic/inorganic molecules and solids. The topics covered include methods for the determination of structure, intermolecular interactions, solid‐state organization, reaction kinetics, and diffusion.

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Solid‐StateNMRInvestigations on Complex Disordered Materials

Villanueva-Garibay

Abele

Müller

2011

Encyclopedia of Analytical Chemistry

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We describe the use of solid‐state NMR spectroscopy for studies of order and disorder in solids. A short overview of different aspects of order and disorder in solid materials is given, addressing the differences between static and dynamic disorders. A brief introduction to the basics of broad‐line, high‐resolution, and dynamic solid‐state NMR spectroscopy follows. Subsequently, we present representative applications of solid‐state NMR spectroscopy on various types of disordered materials. The experiments primarily involve dipolar recoupling techniques for structural characterization, as well as dynamic broad‐line and high‐resolution methods for examination of motional features. Selected examples demonstrate the potential of advanced solid‐state NMR methods for characterization of both static and dynamic disorders in the solid state.

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REDOR-Based Heteronuclear Dipolar Correlation Experiments in Multi-Spin Systems: Rotor-Encoding, Directing, and Multiple Distance and Angle Determination

Cited by 78 publications

References 69 publications

Determining the Geometry of Hydrogen Bonds in Solids with Picometer Accuracy by Quantum‐Chemical Calculations and NMR Spectroscopy

Determining the Geometry of Hydrogen Bonds in Solids with Picometer Accuracy by Quantum‐Chemical Calculations and NMR Spectroscopy

Nuclear Magnetic Resonance (NMR) Spectroscopy of Inorganic/Organometallic Molecules

Solid‐StateNMRInvestigations on Complex Disordered Materials

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