Investigation of multiaxial molecular dynamics by MAS NMR spectroscopy

Kristensen, J.H.; Hoatson, Gina L.; Vold, Robert L.

doi:10.1016/s0926-2040(98)00074-5

Cited by 48 publications

(45 citation statements)

References 27 publications

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“…This dynamic broadening effect can be viewed as an obstacle to resolution or as a useful probe of molecular motion [6][7][8][9][10][11]. However, it is sometimes possible to select experiments that exhibit linebroadening in one dimension while retaining high-resolution in a second dimension.…”

Section: Introductionmentioning

confidence: 99%

Magic angle spinning (MAS) NMR linewidths in the presence of solid-state dynamics

Thrippleton

Cutajar

Wimperis

2008

Chemical Physics Letters

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In solid-state NMR, the magic angle spinning (MAS) technique fails to suppress anisotropic spin interactions fully if reorientational dynamics are present, resulting in a decay of the rotational-echo train in the time-domain signal. We show that a simple analytical model can be used to quantify this linebroadening effect as a function of the MAS frequency, reorientational rate constant, and magnitude of the inhomogeneous anisotropic broadening. We compare this model with other theoretical approaches and with exact computer simulations, and show how it may be used to estimate rate constants from experimental NMR data.3

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Section: Introductionmentioning

confidence: 99%

Magic angle spinning (MAS) NMR linewidths in the presence of solid-state dynamics

Thrippleton

Cutajar

Wimperis

2008

Chemical Physics Letters

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“…[20][21][22] The high-resolution 2 H MAS spectra of 1-D in Figure 4 show three resonances at isotropic chemical shifts d iso = 2.19, 3.24, and 7.09 ppm. The very narrow resonance at d = 2.19 ppm (marked with * ) is assigned to residual [D 6 ]acetone, which was used in the preparation of 1-D.…”

mentioning

confidence: 99%

“…10 7 s À1 . [21][22][23] Decreasing the temperature leads to line broadening, and the linewidths observed at 246 K for both water resonances are so large that spinning sidebands are barely observable. The rate of the motions in this intermediate regime is typically in the range 10 7 s À1 !…”

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confidence: 99%

A Synthetic Zwitterionic Water Channel: Characterization in the Solid State by X‐ray Crystallography and NMR Spectroscopy

et al. 2005

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Bio-inspired supramolecular frameworks are of both fundamental value as models and of practical importance in areas such as materials science, catalysis, and molecular electronics. [1][2][3] Many of these synthetic materials are constructed from metal ions as connectors and ligands as linkers, and are referred to as coordination polymers.[4] Porous materials are of particular interest, as the nanosized cavities lead to novel phenomena, with applications in separation, storage, and catalysis. In this respect, attempts to generate synthetic water channels that mimic aquaporin water channels [5] have met with some success. [6][7][8][9][10] Here we describe a zwitterionic, helical tube of nanodimensions that to some extent mimics aquaporin, and provide a detailed study of the water incorporated inside the channel over a wide temperature range by solidstate 2 H NMR spectroscopy. Reaction of the carboxy-functionalized imidazolium salt N,N'-diacetic acid imidazolium bromide [11] with zinc in aqueous solution affords zwitterionic coordination polymer 1 in crystalline form. The structure of 1 was characterized by single-crystal X-ray diffraction at 140 K and is shown in Figure 1. To ensure that the encapsulated water does not undergo any structural changes at ambient temperature, the structure was also determined at 293 K (see Supporting Information). The macrostructure is formed from ZnBr(H 2 O) units linked by bridging dicarboxylate anions, which assemble into helical channels and appear to be supported by weak pstacking interactions between the imidazolium moieties and by intrahelical hydrogen bonds. The strongest hydrogen bonds stem from contacts of the carboxy oxygen atom O2 to H3 and H6 in the next layer. Two molecules constitute a full cycle within the helix with distances between the layers of 6.234 . The cavity of the channel is occupied by water molecules, which form a one-dimensional chain with distances between the oxygen atoms of 3.157 .The coordination sphere around the zinc anion in 1 is best described as a distorted tetrahedron with angles between 92.5(2) and 117.1(1)8. Zinc-oxygen bond lengths lie between 1.997(2) and 2.014(3) , and both angles and bond lengths are in good agreement with those of comparable zinc dicarboxylate polymers. [12] The helices are packed in a hexagonal-based array with pronounced interhelical hydrogen bonding (Figure 2 b). Each asymmetric unit has five contacts shorter than 3 to neighboring helices, which arise from medium-strength interactions from O1 and O3 and weaker contacts from the bromide ligands. The hydrogen atoms H61 and H62 of the encapsulated water molecule are engaged in strong hydrogen

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“…These parameters often correlate with structural parameters, such as bond angles and bond lengths, and are important sources of information about molecular structure. In addition to its usefulness for structural analysis, the MAS NMR experiment has been introduced as a valuable method for investigating molecular motion in solids [10][11][12][13][14]. In the presence of molecular motion, the spectra exhibit lineshape modulations that may be analyzed to determine the motional mechanism.…”

Section: Introductionmentioning

confidence: 99%

“…These have been used to calculate motional effects on deuteron MAS NMR spectra [8,9,12,14]. We have elaborated on deuteron experiments because these are used extensively for investigations of molecular motion.…”

Section: Introductionmentioning

confidence: 99%

Design and Implementation of Runge–Kutta Methods for MAS NMR Lineshape Calculations

Kristensen¹,

Hoatson²,

Vold³

2001

Journal of Computational Physics

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Investigation of multiaxial molecular dynamics by MAS NMR spectroscopy

Cited by 48 publications

References 27 publications

Magic angle spinning (MAS) NMR linewidths in the presence of solid-state dynamics

Magic angle spinning (MAS) NMR linewidths in the presence of solid-state dynamics

A Synthetic Zwitterionic Water Channel: Characterization in the Solid State by X‐ray Crystallography and NMR Spectroscopy

Design and Implementation of Runge–Kutta Methods for MAS NMR Lineshape Calculations

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