Distance measurement between a spin-1/2 and a half-integer quadrupolar nuclei by solid-state NMR using exact analytical expressions

Chen, Lei; Lu, Xingyu; Wang, Qiang; Lafon, Olivier; Trébosc, Julien; Deng, Feng; Amoureux, Jean‐Paul

doi:10.1016/j.jmr.2010.07.009

Cited by 60 publications

(56 citation statements)

References 45 publications

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“…This scrambling results in an apparent saturation of the magnetization of a powder sample. This phenomenon has been used for hetero-nuclear distance measurement [40][41][42][43][44][45][46]. Fig.…”

Section: Robustness To Offset and Selectivitymentioning

confidence: 99%

Broadband excitation in solid-state NMR using interleaved DANTE pulse trains with N pulses per rotor period

Trébosc

Lafon

et al. 2013

Journal of Magnetic Resonance

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N Broadband excitation DANTE MAS Paramagnetic samples a b s t r a c tWe analyze the direct excitation of wide one-dimensional spectra of nuclei with spin I = 1/2 or 1 in rotating solids submitted to pulse trains in the manner of Delays Alternating with Nutations for Tailored Excitation (DANTE), either with one short rotor-synchronized pulse of duration s p in each of K rotor periods For nuclei with I = 1 (e.g., for 14 N), the response to basic D K 1 pulse train is moreover affected by inhomogeneous decay due to 2nd-order quadrupole interactions, since these are not of rank 2 and therefore cannot be eliminated by spinning about the magic angle. For large quadrupole interactions, the signal decay produced by second-order quadrupole interaction can be minimized by (i) reducing the length of D K N pulse trains using N > 1, (ii) fast spinning, (iii) large rf-field, and (iv) using high magnetic fields to reduce the 2nd-order quadrupole interaction.

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Section: Robustness To Offset and Selectivitymentioning

confidence: 99%

Broadband excitation in solid-state NMR using interleaved DANTE pulse trains with N pulses per rotor period

Trébosc

Lafon

et al. 2013

Journal of Magnetic Resonance

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“…Hence, S‐RESPDOR has proven to be an efficient sequence for the distance measurement between spin‐1/2 and quadrupolar nuclei involving the pairs { 31 P– 51 V}, { 13 C– 67 Zn}, { 13 C– 17 O}, and { 13 C– 14 N} 16. 17…”

Section: Introductionmentioning

confidence: 99%

Measurement of Aluminum–Carbon Distances Using S‐RESPDOR NMR Experiments

et al. 2012

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It is demonstrated that reliable aluminum-carbon distances can be measured in samples with (13)C natural abundance by NMR spectroscopy. Overcoupled resonators, with only one radio-frequency synthesizer and one amplifier, are used to irradiate in the same pulse sequence (27)Al and (13)C nuclei, which differ by only 3.6 % in Larmor frequencies. The combination of (27)Al saturation pulse with heteronuclear dipolar recoupling yields dipolar dephasing of the (13)C signal, which only depends on the Al-C distance and the efficiency of the saturation pulse. Therefore, reliable distances can be obtained by rapid fitting of experimental data to an analytical expression. It is demonstrated that with natural isotopic abundance this approach allows recovery of Al-C distances of 216 pm for the covalent bond in lithium tetraalkyl aluminates, commonly used as a co-catalyst in olefin polymerization processes, and which range from 274 to 381 pm for the three carbon atoms in aluminum lactate. The accuracy of the measured internuclear distances is carefully estimated.

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“…Many recent papers provide an in-depth analysis of the REDOR/REAPDOR experiment when quadrupolar nuclei are involved, just to mention Gullion and Vega [15] and Nimerovsky and Goldbourt [16], or in case the adiabatic pulse is replaced by a saturation pulse S-RESPDOR (Symmetry-based Rotational resonance saturation pulse double resonance) by Gan and Lu et all [11, 17]. For a REAPDOR experiment with a train of refocusing π pulses applied on 13 C, Goldbourt et al [18] suggests an empirical formula specific to spin 5/2, while for RESPDOR experiment Amoreux and coworkers [19] propose a general fornula valid for every spin. In addition, for a REDOR experiment between two quadrupolar I>1/2 nuclei, Bertmer et al [20] demonstrates that the central transition approximation, which assumes that only the central transition of the half-integer quadrupolar nuclei contributes to the dephasing, is adequate for analysis of the initial part of the dephasing curve.…”

Section: Introductionmentioning

confidence: 99%

Localization of Cl-35 nuclei in biological solids using rotational-echo double-resonance experiments

Iuga

Rossi

Herzfeld

et al. 2017

Solid State Nuclear Magnetic Resonance

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Chloride ions play important roles in many chemical and biological processes. This paper investigates the possibility of localizing 35Cl nuclei using solid-state NMR. It demonstrates that distances shorter than 3.8 Å, between 13C atoms and 35Cl atoms in 10% uniformly labeled 13C L-tyrosine · HCl and natural abundance Glycine · HCl can be measured using rotational-echo (adiabatic passage) double-resonance (RE(AP)DOR). Furthermore the effect of quadrupolar interaction on the REDOR/REAPDOR experiment is quantified. The dephasing curve is plotted in a three dimensional chart function of the dephasing time and function of the strength of quadrupolar interaction felt by each orientation. During spinning each orientation feels a quadrupolar interaction that varies in time, and therefore at each moment in time we reorder the crystallite orientations as a function of their contribution to the dephasing curve. In this way the effect of quadrupolar interaction on the dipolar dephasing curve can be fitted with a polynomial function. The numerical investigation performed allows us to generate REDOR/REAPDOR curves which are then used to simulate the experimental data.

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Distance measurement between a spin-1/2 and a half-integer quadrupolar nuclei by solid-state NMR using exact analytical expressions

Cited by 60 publications

References 45 publications

Broadband excitation in solid-state NMR using interleaved DANTE pulse trains with N pulses per rotor period

Broadband excitation in solid-state NMR using interleaved DANTE pulse trains with N pulses per rotor period

Measurement of Aluminum–Carbon Distances Using S‐RESPDOR NMR Experiments

Localization of Cl-35 nuclei in biological solids using rotational-echo double-resonance experiments

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