title: Accurate determination of one-bond heteronuclear coupling constants with "pure shift" broadband proton-decoupled CLIP/CLAP-HSQC experiments.
abstract: We report broadband proton-decoupled CLIP/CLAP-HSQC experiments for the accurate determination of one-bond heteronuclear couplings and, by extension, for the reliable measurement of small residual dipolar coupling constants. The combination of an isotope-selective BIRD((d)) filter module with a non-selective (1)H inversion pulse is employed to refocus proton-proton coupling evolution prior to the acquisition of brief chunks of free induction decay that are subsequently assembled to reconstruct the fully-decoupled signal evolution. As a result, the cross-peaks obtained are split only by the heteronuclear one-bond coupling along the F2 dimension, allowing coupling constants to be extracted by measuring simple frequency differences between singlet maxima. The proton decoupling scheme presented has also been utilized in standard HSQC experiments, resulting in a fully-decoupled pure shift correlation map with significantly improved resolution.
authors.affiliation: Department of Inorganic and Analytical Chemistry, University of Debrecen, Egyetem tér 1, H-4032 Debrecen, Hungary.
authors.forename: István
authors.initials: I
authors.lastname: Timári
authors.affiliation: Clemens-Schöpf-Institut für Organische Chemie und Biochemie, Technische Universität Darmstadt, Alarich-Weiss-Straße 4, D-64287 Darmstadt, Germany.
authors.forename: Lukas
authors.initials: L
authors.lastname: Kaltschnee
authors.affiliation: Clemens-Schöpf-Institut für Organische Chemie und Biochemie, Technische Universität Darmstadt, Alarich-Weiss-Straße 4, D-64287 Darmstadt, Germany.
authors.forename: Andreas
authors.initials: A
authors.lastname: Kolmer
authors.affiliation: School of Chemistry, University of Manchester, Oxford Road, Manchester M13 9PL, United Kingdom.
authors.forename: Ralph W
authors.initials: RW
authors.lastname: Adams
authors.affiliation: School of Chemistry, University of Manchester, Oxford Road, Manchester M13 9PL, United Kingdom; Department of Food Science, University of Copenhagen, Rolighedsvej 30, DK-1958 Frederiksberg C, Denmark.
authors.forename: Mathias
authors.initials: M
authors.lastname: Nilsson
authors.affiliation: Clemens-Schöpf-Institut für Organische Chemie und Biochemie, Technische Universität Darmstadt, Alarich-Weiss-Straße 4, D-64287 Darmstadt, Germany.
authors.forename: Christina M
authors.initials: CM
authors.lastname: Thiele
authors.affiliation: School of Chemistry, University of Manchester, Oxford Road, Manchester M13 9PL, United Kingdom.
authors.forename: Gareth A
authors.initials: GA
authors.lastname: Morris
authors.affiliation: Department of Inorganic and Analytical Chemistry, University of Debrecen, Egyetem tér 1, H-4032 Debrecen, Hungary. Electronic address: kover@science.unideb.hu.
authors.forename: Katalin E
authors.initials: KE
authors.lastname: Kövér
keywords: Broadband proton decoupling; F(2)-coupled HSQC; IPAP; Pure absorption; RDC