Proton-detected 3D ¹⁵N/¹H/¹H isotropic/anisotropic/isotropic chemical shift correlation solid-state NMR at 70 kHz MAS

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• 作者：Manoj Kumar Pandey^a ; Jayasubba Reddy Yarava^a ; ¹ ; Rongchun Zhang^b ; Ayyalusamy Ramamoorthy^b ; Yusuke Nishiyama^a ; ^c ; ^{yunishiy@jeol.co.jp" class="auth_mail" title="E-mail the corresponding author}
• 关键词：Solid-state NMR ; Ultrafast MAS ; 1H CSA ; Amide proton ; 3D NMR ; peptide ; 1H detection
• 刊名：Solid State Nuclear Magnetic Resonance
• 出版年：2016
• 出版时间：June-July 2016
• 年：2016
• 卷：76-77
• 期：Complete
• 页码：1-6
• 全文大小：1063 K

文摘

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 ¹H CSAs of proteins even by using the recently proposed 2D ¹H/¹H 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 ¹⁵N. In this context, we demonstrate a proton-detected 3D ¹⁵N/¹H/¹H CS/CSA/CS correlation experiment at fast MAS frequency (70 kHz) to measure ¹H CSA values of unresolved amide protons of N-acetyl-¹⁵N-l-valyl-¹⁵N-l-leucine (NAVL).