Truncated dipolar recoupling in solid-state nuclear magnetic resonance

Marín-Montesinos, Ildefonso; Mollica, Giulia; Carravetta, Marina; Gansmüller, Axel; Pileio, Giuseppe; Bechmann, Matthias; Sebald, Angelika; Levitt, Malcolm H.

doi:10.1016/j.cplett.2006.10.101

Cited by 35 publications

(55 citation statements)

References 32 publications

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“…1 and a fast angle switching probe, longer-range C-C distances can be accurately determined in uniformly 13 C labeled samples, notably the greater than 4 Å C 2 (V)-C(L) 20 distance in the dipeptide Ac-VL. The new experimental protocol presented here involves the recording of separate dipolar-modulated and reference spin-echo datasets that correspond to changing the irradiation frequencies of the double Gaussian pulse: this enables the independent 25 determination of the spin-echo dephasing time, T 2 ', such that the dipolar coupling is the only free variable for the fit of the dipolar-modulated data.…”

Section: Discussionmentioning

confidence: 99%

“…U- 13 water and acetone, with crystals formed by slow evaporation of the solvent. 29 The pulse sequence employed is depicted in Fig.…”

Section: Methodsmentioning

confidence: 99%

“…15 SPINAL-64 1 H decoupling 30 at 100 kHz was used during the spin-echo period, , the z-filter and acquisition. A 1 ms contact time was used for cross polarization from 1 H to 13 C with a 70 to 100 % ramp on the 1 H channel. [31][32] The recycle delay was 3 s. For each spin-echo duration, , 16 transients 20 were co-added.…”

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confidence: 99%

“…Note that the so-determined T 2 ' for the off-angle spin-echo evolution includes the effect of dipolar modulation due to like spins, 80 i.e., intermolecular 13 CO-13 CO (U-13 C, 15 N Lhistidine.H 2 O.HCl) and 13 C 2 (V)- 13 C 2 (V) (AcVL) dipolar couplings for the experimental data in Fig. 2.…”

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confidence: 99%

“…Table 1 lists the fitted D (together with the corresponding internuclear distance, r) and T 2 ' values as well as the offset from the magic angle, , and the time shift, t s . 90 The packing together in the solid state of the uniformly 13 C labelled molecules means that intermolecular as well as intramolecular dipolar couplings can contribute to the observed dipolar modulation. This is expressed via the root- Table 1 Table 1), the green squares, blue diamonds, red circles and black ellipsoids correspond to the  (and  and ts) values for the experimental data in (a,b).…”

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confidence: 99%

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Longer-range distances by spinning-angle-encoding solid-state NMR spectroscopy

Becker‐Baldus

Kemp

Past

et al. 2011

Phys. Chem. Chem. Phys.

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A new spinning-angle-encoding spin-echo solid-state NMR approach is used to accurately determine the dipolar coupling corresponding to a C-C distance over 4 Å in a fully labelled dipeptide. The dipolar coupling dependent spin-echo modulation was recorded off magic angle, switching back to the magic angle for the 10 acquisition of the free-induction decay, so as to obtain optimum sensitivity. The retention of both ideal resolution and long-range distance sensitivity was achieved by redesigning a 600 MHz HX MAS NMR probe to provide fast angle switching during the NMR experiment: For 1.8 mm rotors, angle changes of up to~5 degrees in~10 ms were achieved at 12 kHz MAS. A new experimental design that combines a reference and a dipolar-modulated experiment and a master-curve approach to data interpretation is presented.

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Section: Discussionmentioning

confidence: 99%

“…U- 13 water and acetone, with crystals formed by slow evaporation of the solvent. 29 The pulse sequence employed is depicted in Fig.…”

Section: Methodsmentioning

confidence: 99%

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confidence: 99%

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confidence: 99%

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confidence: 99%