000204313 001__ 204313
000204313 005__ 20181203023724.0
000204313 0247_ $$2doi$$a10.1021/ja308135r
000204313 022__ $$a0002-7863
000204313 02470 $$2ISI$$a000309566400066
000204313 037__ $$aARTICLE
000204313 245__ $$aDynamic Nuclear Polarization NMR Spectroscopy of Microcrystalline Solids
000204313 260__ $$bAMER CHEMICAL SOC$$c2012
000204313 269__ $$a2012
000204313 336__ $$aJournal Articles
000204313 520__ $$aDynamic nuclear polarization (DNP) solid-state NMR has been applied to powdered microcrystalline solids to obtain sensitivity enhancements on the order of 100. Glucose, sulfathiazole, and paracetamol were impregnated with bis-nitroxide biradical (bis-cyclohexyl-TEMPO-bisketal, bCTbK) solutions of organic solvents. The organic solvents were carefully chosen to be nonsolvents for the compounds, so that DNP-enhanced solid-state NMR spectra of the unaltered solids could be acquired. A theoretical model is presented that illustrates that for externally doped organic solids characterized by long spin-lattice relaxation times (T-1(H-1) > 200 s), H-1-H-1 spin diffusion can relay enhanced polarization over micrometer length scales yielding substantial DNP enhancements (epsilon). epsilon on the order of 60 are obtained for microcrystalline glucose and sulfathiazole at 9.4 T and with temperatures of ca. 105 K. The large gain in sensitivity enables the rapid acquisition of C-13-C-13 correlation spectra at natural isotopic abundance. It is anticipated that this will be a general method for enhancing the sensitivity of solid-state NMR experiments of organic solids.
000204313 700__ $$0248569$$aRossini, Aaron J.$$g251584
000204313 700__ $$aZagdoun, Alexandre
000204313 700__ $$aHegner, Franziska
000204313 700__ $$aSchwarzwalder, Martin
000204313 700__ $$aGajan, David
000204313 700__ $$aCoperet, Christophe
000204313 700__ $$aLesage, Anne
000204313 700__ $$0248253$$aEmsley, Lyndon$$g251248
000204313 773__ $$j134$$k40$$q16899-16908$$tJOURNAL OF THE AMERICAN CHEMICAL SOCIETY
000204313 909C0 $$0252518$$pLRM$$xU12975
000204313 909CO $$ooai:infoscience.tind.io:204313$$pSB$$particle
000204313 937__ $$aEPFL-ARTICLE-204313
000204313 970__ $$aISI:000309566400066/LRM
000204313 973__ $$aOTHER$$rREVIEWED$$sPUBLISHED
000204313 980__ $$aARTICLE