Resolved Dipolar Coupling Spectra of Dilute Nuclear Spins in Solids

Hester, R.K.; Ackerman, Jerome L.; Cross, V. R.; Waugh, J. S.

doi:10.1103/physrevlett.34.993

Cited by 131 publications

(49 citation statements)

References 9 publications

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“…One of the most typical applications for homonuclear dipolar decoupling pulse sequences is as an element in separated-local-field (SLF) experiments for measurement of heteronuclear dipolar couplings [70]. For example, this is of interest for determination of the orientation of N-H internuclear axes relative to the external magnetic field in single crystals or uniaxially oriented peptide samples as described by Opella and coworkers [33].…”

Section: Typical Examples Of Simpson Simulationsmentioning

confidence: 99%

SIMPSON: A general simulation program for solid-state NMR spectroscopy

Bak

Rasmussen

Nielsen

2011

Journal of Magnetic Resonance

1,361

308

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A computer program for fast and accurate numerical simulation of solid-state NMR experiments is described. The program is designed to emulate a NMR spectrometer by letting the user specify high-level NMR concepts such as spin systems, nuclear spin interactions, rf irradiation, free precession, phase cycling, coherence-order filtering, and implicit/explicit acquisition. These elements are implemented using the Tcl scripting language to ensure a minimum of programming overhead and direct interpretation without the need for compilation, while maintaining the flexibility of a fullfeatured programming language. Basicly, there are no intrinsic limitations to the number of spins, types of interactions, sample conditions (static or spinning, powders, uniaxially oriented molecules, single crystals, or solutions), and the complexity or number of spectral dimensions for the pulse sequence. The applicability ranges from simple 1D experiments to advanced multiple-pulse and multiple-dimensional experiments, series of simulations, parameter scans, complex data manipulation/visualization, and iterative fitting of simulated to experimental spectra. A major effort has been devoted to optimize the computation speed using state-of-the-art algorithms for the timeconsuming parts of the calculations implemented in the core of the program using the C programming language. Modification and maintenance of the program are facilitated by releasing the program as open source software (General Public License) currently at http://nmr.imsb.au.dk. The general features of the program are demonstrated

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Section: Typical Examples Of Simpson Simulationsmentioning

confidence: 99%

SIMPSON: A general simulation program for solid-state NMR spectroscopy

Bak

Rasmussen

Nielsen

2011

Journal of Magnetic Resonance

1,361

308

View full text Add to dashboard Cite

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“…18 -20 'DipShift,' dipolar shift spectroscopy, is a 2D solid-state NMR method designed to measure heteronuclear bond lengths. 21 This and other separated local field (SLF) spectroscopic methods 22 have been used for N-H bond length measurements for DNA 23 15 N-enriched L-histidine in a water-acetone (1 : 1) solution; more water was added to dissolve the reaction product, 6 µl of 0.1 M CuCl 2 (<0.1 mol%) was added and the solution was placed in a heat insulated container to allow slow cooling and further evaporation.…”

Section: Introductionmentioning

confidence: 99%

N?H bond stretching in histidine complexes: a solid-state NMR study

Song¹,

Rienstra²,

McDermott³

2001

Magn. Reson. Chem.

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N -H bond lengths in imidazolium-carboxylate pairs were studied as models for enzyme active site motifs. The bond lengths were measured using '2D 2f-DipShift,' a solid-state NMR method wherein the N,H dipolar coupling is determined using heteronuclear dipolar spinning sideband patterns. Like the situation for compressed O -H· · ·O systems, some complexes exhibit very short N· · ·O distances and weaker N,H dipolar coupling. The weaker time-average N,H dipolar coupling for systems with short N· · ·O hydrogen bonds can be most likely associated with an altered potential well for the proton, or a 'stretched' covalent bond, although other interpretations involving a double well potential are discussed. The range or variation in average bond lengths seen in this study is much narrower than that previously reported for O -H· · ·O systems (1.01-1.07Å for N -H vs 1.0-1.3Å for O -H bonds).

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“…In this case, the one bond C-H dipolar coupling D 1 CH is nearly the same as the coupling of this carbon to its orthoproton D 2 CH due to the effect of ordering being different along different directions. In such cases, where the carbon is coupled to more than one proton, the evolution of magnetization is expected to proceed in a locked mode [17] and the oscillation frequency is given…”

Section: Inclusion Of Homonuclear Decoupling During Cpmentioning

confidence: 99%

“…Another approach that has been proposed and implemented is the use of a variant of the SLF 2D experiment that uses the transient oscillations observed during cross polarization [16,17] for estimating dipolar couplings [18]. Modifications to the standard crosspolarization pulse scheme such as the use of homonuclear decoupling during cross polarization (CP) and the use of polarization inversion have also been suggested [19,20].…”

Section: Introductionmentioning

confidence: 99%

Ordering in nematic liquid crystals from NMR cross-polarization studies

Ramanathan

Sinha

2003

Pramana - J Phys

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Abstract. The measurement of dipolar couplings between nuclei is a convenient way of obtatining directly liquid crystalline ordering through NMR since the coupling is dependent on the average orientation of the dipolar vector in the magnetic field which also aligns the liquid crystal. However, measurement of the dipolar coupling between a pair of selected nuclei is beset with problems that require special solutions. In this article the use of cross polarization for measuring dipolar couplings in liquid crystals is illustrated. Transient oscillations observed during cross polarization provide the dipolar couplings between essentially isolated nearest neighbour spins which can be extracted for several sites simultaneously by employing two-dimensional NMR techniques. The use of the method for obtaining heteronuclear dipolar couplings and hence the order parameters of liquid crystals is presented. Several modifications to the basic experiment are considered and their utility illustrated. A method for obtaining proton-proton dipolar couplings, by utilizing cross polarization from the dipolar reservoir, is also presented.

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Resolved Dipolar Coupling Spectra of Dilute Nuclear Spins in Solids

Cited by 131 publications

References 9 publications

SIMPSON: A general simulation program for solid-state NMR spectroscopy

SIMPSON: A general simulation program for solid-state NMR spectroscopy

N?H bond stretching in histidine complexes: a solid-state NMR study

Ordering in nematic liquid crystals from NMR cross-polarization studies

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