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Determination of peptide φ angles in solids by relayed anisotropy correlation NMR
Authors:Yoshitaka Ishii   Koichi Hirao   Takehiko Terao   Tsutomu Terauchi   Makoto Oba   Kozaburo Nishiyama  Masatsune Kainosho
Affiliation:

a Department of Chemistry, Graduate School of Science, Kyoto University, Kyoto 606-8502, Japan

b Department of Material Science and Technology, Tokai University, 317 Nishino, Numazu, Shizuoka 410-03, Japan

c Department of Bioscience, School of Science and Engineering, Teikyo University, Toyosatodai 1-1, Utsunomiya 320, Japan

d Toray Research Center, Shiga, 3-7 Sonoyama 3-chome, Otsu, Shiga 520, Japan

Abstract:A solid state NMR method is presented for determination of a backbone dihedral angle φ in peptides, being based on the previously reported method, relayed anisotropy correlation (RACO) NMR [Y. Ishii et al., Chem. Phys. Lett. 256 (1996) 133]. In the present method, the and the dipolar tensors in the system are two-dimensionally (2D) correlated via polarization transfer from to under magic angle spinning (MAS). This method was applied to N-acetyl,-valine, and the H–C–N–H dihedral angle was determined to be 154.0±1.4° or 206.0±1.4°, the former agreeing with the X-ray value of 154±5°.
Keywords:2D MAS NMR   2D powder pattern   Dihedral angle
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