Proton-selective 17O-1H distance measurements in fast magic-angle-spinning solid-state NMR spectroscopy for the determination of hydrogen bond lengths.
We present a proton-selective method to determine 17O-1H distances in organic, biological, and biomimetic materials by fast magic-angle-spinning solid-state NMR spectroscopy. This method allows the determination of internuclear distances between specific (17O, 1H) spin pairs selectively. It enables the estimation of medium-range 17O...1H distances across hydrogen bonds in the presence of short-range 17O-1H contacts sharing the same 17O site. The method employs the newly developed symmetry-based radiofrequency pulse sequence SR%@mt;sys@%4%@sx@%1%@be@%2%@sxx@%%@mx@% applied to the protons to achieve heteronuclear dipolar recoupling, while simultaneously decoupling the homonuclear proton dipolar interactions. Fast MAS (50 kHz) and high static magnetic fields (18.8 T) achieve the required proton spectral resolution.
Brinkmann
Andreas
A
Physical Chemistry/Solid State NMR, Institute for Molecules and Materials, Radboud University Nijmegen, Toernooiveld 1, 6525 ED Nijmegen, The Netherlands. a.brinkmann@science.ru.nl
Kentgens
Arno P M
AP
D006860:Hydrogen Bonding; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008958:Models, Molecular; D010103:Oxygen Isotopes / Q000737:chemistry*; D011522:Protons
D010103:Oxygen Isotopes; D011522:Protons