title: Distance measurements in nucleic acids using windowless dipolar recoupling solid state NMR.
abstract: A windowless, homonuclear dipolar recoupling pulse sequence (DRAWS) is described and a theoretical basis for describing its recoupling performance is developed using numerical techniques. It is demonstrated that DRAWS recouples weak dipolar interactions over a broad range of experimental and molecular conditions. We discuss two spectroscopic control experiments, which help to take into account effects due to insufficient proton decoupling, relaxation, and static dipolar couplings to nearby 13C spins at natural abundance. Finally DRAWS is used in combination with selective 13C labeling to measure 13C-13C distances in five doubly labeled DNA dodecamers, [d(CGCGAAT*T*CGCG)]2, which contain the binding site for the restriction enzyme EcoRI. The longest distance reported is 4.8 A. In most cases the distances agree well with those derived from X-ray crystallographic data, although small changes in hydration level can result in relatively large changes in internuclear distances.
authors.affiliation: Department of Chemistry, University of Washington, Seattle 98195, USA.
authors.forename: M A
authors.initials: MA
authors.lastname: Mehta
authors.forename: D M
authors.initials: DM
authors.lastname: Gregory
authors.forename: S
authors.initials: S
authors.lastname: Kiihne
authors.forename: D J
authors.initials: DJ
authors.lastname: Mitchell
authors.forename: M E
authors.initials: ME
authors.lastname: Hatcher
authors.forename: J C
authors.initials: JC
authors.lastname: Shiels
authors.forename: G P
authors.initials: GP
authors.lastname: Drobny
mesh_terms: D002247:Carbon Isotopes; D003198:Computer Simulation; D018360:Crystallography, X-Ray; D004247:DNA / Q000737:chemistry*; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008432:Mathematical Computing; D009690:Nucleic Acid Conformation; D009696:Nucleic Acids / Q000737:chemistry*
chemical_list: D002247:Carbon Isotopes; D009696:Nucleic Acids; D004247:DNA