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

Abstract

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 as a function of the dephasing time and 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.