The detection of weak heteronuclear coupling between spin 1 and spin nuclei in MAS NMR; 14N/13C/1H triple resonance experiments

Grey, Clare P.; Veeman, W. S.

doi:10.1016/0009-2614(92)85486-t

Cited by 101 publications

(156 citation statements)

References 14 publications

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“…In contrast, the rotational echo adiabatic passage double-resonance (REAPDOR) (112) and transfer of population in double-resonance (TRAPDOR) (113) experiments are designed specifically to study dipolar interactions involving quadrupolar nuclei. These sequences (shown in Fig.…”

Section: Reapdor and Trapdormentioning

confidence: 99%

Structural information from quadrupolar nuclei in solid state NMR

Ashbrook

Duer

2006

Concepts Magnetic Resonance

146

262

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Solid-state NMR has become the method of choice for determining details of molecular-level structure in heterogeneous systems. Though spin-1/2 nuclei still form the core of most such studies, quadrupolar nuclei are increasingly being used. This review assesses what is currently possible, from achieving high-resolution spectra for quadrupolar nuclei (a prerequisite for most structure determination work), to forming correlation spectra which give qualitative details of spatial proximity of nuclei and the determination of internuclear distances, between quadrupolar spins and quadrupolar and spin-1/2 nuclei. Examples are given of each method discussed, and the advantages and disadvantages of the various experiments for different possible applications are assessed.

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Section: Reapdor and Trapdormentioning

confidence: 99%

Structural information from quadrupolar nuclei in solid state NMR

Ashbrook

Duer

2006

Concepts Magnetic Resonance

146

262

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“…Compounds with several 14 N sites may lead to overlapping overtone patterns, which can, in principle, be separated by combining overtone spectroscopy with dynamic-angle spinning or with double sample rotation. [30][31][32][33][34] It is possible to achieve indirect detection of I = 1 ( 14 N) in samples spinning at the magic angle by recoupling the heteronuclear dipolar interactions DA C H T U N G T R E N N U N G (I, S) with suitable spy nuclei with S = 1/2, such as 13 C. [35][36][37] By applying RF pulses either at w 0 (I) or w 0 (S) in appropriate synchronism with sample rotation, one can interfere with the averaging of heteronuclear dipolar interactions DA C H T U N G T R E N N U N G (I, S). This approach leads to a dephasing of the signals of the S nuclei, thus providing information on the strength of the dipolar interaction.…”

Section: Introductionmentioning

confidence: 99%

“…The spectra are similar to those obtained at 9.4 T, [17] thus providing evidence that the method works at different fields. It is possible to contemplate the indirect detection of other quadrupolar nuclei with S = 3/2, 5/2 and so forth, such as, for example, 35 Cl or 17 O, provided that one can exploit a residual dipolar splitting and/or scalar couplings with suitable spy nuclei S = 1/2 such as 13 C.…”

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confidence: 99%

Indirect Detection of Nitrogen‐14 in Solid‐State NMR Spectroscopy

et al. 2007

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NMR spectra of (14)N (spin I=1) are obtained by indirect detection in powders spinning at the magic angle. The method relies on the transfer of coherence from a neighboring "spy" nucleus with S=1/2, such as (13)C or (1)H, to single- or double-quantum transitions of (14)N nuclei. The transfer of coherence can occur through a combination of scalar and residual dipolar splittings (RDS); the latter are also known as second-order quadrupole-dipole cross terms. The two-dimensional NMR spectra reveal powder patterns determined by second- and third-order quadrupolar couplings. These spectra depend on the quadrupolar coupling constant C(Q) (typically a few megahertz), on the asymmetry parameter eta(Q) of the (14)N nucleus, and on the orientation of the internuclear vector r(IS) between the I ((14)N) and S (spy) nuclei with respect to the quadrupolar tensor. These parameters, which can be subject to motional averaging, can reveal valuable information about the structure and dynamics of nitrogen-containing solids. Application of this technique to various amino acids, either enriched in (13)C or with natural carbon isotope abundance, with spectra recorded at various magnetic fields, illustrates the scope of the method.

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“…In fluorine-bearing aluminosilicate glasses, 19 F{ 27 Al}TRAPDOR ('TRAnsfer of Populations by DOuble Resonance') experiments are also useful to constrain the relative separation of fluorine and aluminum ions [18]. The technique produces two spectra, one that is essentially a 19 F spin-echo MAS spectrum (called the 'control spectrum') and the other (called the 'double resonance spectrum') in which signals from fluoride ions near aluminum can be greatly reduced by heteronuclear dipolar dephasing through irradiation of the 27 Al frequency during the echo time.…”

Section: Introductionmentioning

confidence: 99%