MRC, Frydman, 23Na SSNMR of sodium sites in Na-nucleotide complexes

Magnetic Resonance in Chemistry
Vol: 44, Issue: 3, March 2006
pp. 366 - 374

Title: Solid-state NMR investigation of sodium nucleotide complexes
Authors: Grant, Christopher V.a; McElheny, Danb; Frydman, Veronicac; Frydman, Lucioc
Affiliations: a. Department of Chemistry and Biochemistry, University of California, San Diego, La Jolla, CA 92093, USA
b. Department of Biochemistry and Molecular Biology, The University of Chicago, Chicago, IL 60637, USA
c. Weizmann Institute of Science, Rehovot, 76100, Israel
Keywords: NMR; MQMAS; 23Na spectra; ATP; nucleotide binding motifs; REDOR; quadrupolar relaxation
Abstract (English):

Solid-state NMR has been used to analyze the chemical environments of sodium sites in powdered crystalline samples of sodium nucleotide complexes. Three of the studied complexes have been previously characterized structurally by crystallography (disodium deoxycytidine-5’-monophosphate heptahydrate, disodium deoxyuridine-5’-monophosphate pentahydrate and disodium adensoine-5’-triphosphate trihydrate). For these salts, the nuclear quadrupole coupling parameters measured by 23Na multiple-quantum magic-angle-spinning NMR could be readily correlated with sodium ion coordination environments. Furthermore, two complexes that had not been previously characterized structurally, disodium uridine-3’-monophosphate and a disodium uridine-3’-monophosphate/disodium uridine-2’-monophosphate mix, were identified by solid-state NMR. A spectroscopic assignment of the four sites of an additional salt, disodium adensoine-5’-triphosphate trihydrate, is also presented and discussed within the context of creating a general approach for the spectroscopic assignment of multiple sites in sodium nucleotide complexes. Copyright © 2006 John Wiley & Sons, Ltd.