Inverse Detection and Heteronuclear Editing in 1H–15N Correlation and 1H–1H Double-Quantum NMR Spectroscopy in the Solid State under Fast MAS

Investigation of an N���H hydrogen bond in a solid benzoxazine dimer by1H-15N NMR correlation techniques under fast magic-angle spinning

“…In the case of 1 H, a significant advantage is obtained for the inverse variant on account of detecting the nuclei with the higher magnetogyric ratio and, hence, the higher sensitivity. In combination with fast MAS, inverse detection has not been widely applied in solid-state NMR, and has only recently attracted renewed attention, 23,61 whereas it is routinely used in solution-state NMR. 62 Regarding the 15 N-labelled benzoxazine sample investigated here, it is important to note that spectral resolution of resonances in the 1 H dimension is vital in order to distinguish the different proton species present in the sample and to identify the N-H coupling of interest.…”

“…One approach by which this can be achieved is the combination of MAS with 1 H-1 H doublequantum (DQ) spectroscopy. 3,4,21,22 Using the 1 H DQ MAS method, it has been shown that valuable insight into the hydrogen-bonded structures adopted by different alkylsubstituted benzoxazine dimers, 13 as well as the change in the quadrupole hydrogen-bonding arrangement formed by dimers of 2-ureido-4-pyrimidone units upon a ketoenol tautomerism, 23 could be obtained. In addition, it has recently been demonstrated that an analysis of 1 H DQ MAS sideband patterns allows the quantitative determination of proton-proton distances for the complex hydrogen-bonded arrangement adopted by the biologically important molecule bilirubin.…”

Nanostructuring of Hybrid Silicas through a Self‐Recognition Process

“…[16,17] Double quantum 1 H-1 H back-to-back (BABA) experiments [18] were performed to further demonstrate the DDAA scheme for 1. This approach has been previously applied to the fine description of H-bonding in adenine-thymine hybrid materials [12b] and was well suited to the current system.…”

Proton micro-magic-angle-spinning NMR spectroscopy of nanoliter samples

“…Both approaches have so far been used to obtain 1 H spectra [4], 13 C cross-polarization (CP) MAS spectra [2] and [3], 13 C double-quantum spectra [3], and 29 Si one-dimensional (1D) spectra [4]. In addition, 27 Al 1D MAS spectra were recorded on a single crystal of mesolite [3]. Inukai and Takeda showed that the high rf field strengths available in microcoils lead to higher efficiencies in the excitation of multiple-quantum (MQ) coherences in half-integer quadrupolar nuclei [5].…”

“…Other factors such as the size of the external magnetic field, rf inhomogeneity and phase narrow and efficient polarization transfer is possible [26]. Inverse detection of 15 N signals at fast MAS to achieve 1 H resolution has been used by Spiess and coworkers to study multiple hydrogen-bonded systems [27], [28] and [29]. Furthermore, the group of Pruski designed both 1 H detected two-dimensional (2D) 1 H-13 C through-space and throughbond experiments at fast MAS and applied them to organic-inorganic hybrid materials [30] and [31].…”