title: Proton-detected 3D (15)N/(1)H/(1)H isotropic/anisotropic/isotropic chemical shift correlation solid-state NMR at 70kHz MAS.
abstract: Chemical shift anisotropy (CSA) tensors offer a wealth of information for structural and dynamics studies of a variety of chemical and biological systems. In particular, CSA of amide protons can provide piercing insights into hydrogen-bonding interactions that vary with the backbone conformation of a protein and dynamics. However, the narrow span of amide proton resonances makes it very difficult to measure (1)H CSAs of proteins even by using the recently proposed 2D (1)H/(1)H anisotropic/isotropic chemical shift (CSA/CS) correlation technique. Such difficulties due to overlapping proton resonances can in general be overcome by utilizing the broad span of isotropic chemical shifts of low-gamma nuclei like (15)N. In this context, we demonstrate a proton-detected 3D (15)N/(1)H/(1)H CS/CSA/CS correlation experiment at fast MAS frequency (70kHz) to measure (1)H CSA values of unresolved amide protons of N-acetyl-(15)N-l-valyl-(15)N-l-leucine (NAVL).
authors.affiliation: RIKEN CLST-JEOL Collaboration Center, Yokohama, Kanagawa 230-0045, Japan.
authors.forename: Manoj Kumar
authors.initials: MK
authors.lastname: Pandey
authors.affiliation: RIKEN CLST-JEOL Collaboration Center, Yokohama, Kanagawa 230-0045, Japan.
authors.forename: Jayasubba Reddy
authors.initials: JR
authors.lastname: Yarava
authors.affiliation: Biophysics and Department of Chemistry, University of Michigan, Ann Arbor, MI 48109-1055, USA.
authors.forename: Rongchun
authors.initials: R
authors.lastname: Zhang
authors.affiliation: Biophysics and Department of Chemistry, University of Michigan, Ann Arbor, MI 48109-1055, USA.
authors.forename: Ayyalusamy
authors.initials: A
authors.lastname: Ramamoorthy
authors.affiliation: RIKEN CLST-JEOL Collaboration Center, Yokohama, Kanagawa 230-0045, Japan; JEOL RESONANCE Inc., Musashino, Akishima, Tokyo 196-8558, Japan. Electronic address: yunishiy@jeol.co.jp.
authors.forename: Yusuke
authors.initials: Y
authors.lastname: Nishiyama
keywords: (1)H CSA; (1)H detection; 3D NMR; Amide proton; Solid-state NMR; Ultrafast MAS; peptide