Measurement of Multiple Torsion Angles in Uniformly 13C,15N-Labeled <img src="http://pubs.acs.org/images/gifcha
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- 作者：Vladimir Ladizhansky ; Christopher P. Jaroniec ; Annette Diehl ; Hartmut Oschkinat ; and Robert G. Griffin
- 刊名：Journal of the American Chemical Society
- 出版年：2003
- 出版时间：June 4, 2003
- 年：2003
- 卷：125
- 期：22
- 页码：6827 - 6833
- 全文大小：122K
- 年卷期：v.125,no.22(June 4, 2003)
- ISSN：1520-5126
文摘
We demonstrate the simultaneous measurement of several backbone torsion angles <IMG SRC="/images/gifchars/psi.gif" BORDER=0 > in theuniformly 13C,15N-labeled 
-Spectrin SH3 domain using two different 3D 15N-13C-13C-15N dipolar-chemicalshift magic-angle spinning (MAS) NMR experiments. The first NCCN experiment utilizes double quantum(DQ) spectroscopy combined with the INADEQUATE type 13C-13C chemical shift correlation. The decayof the DQ coherences formed between 13C'i and 13Ci spin pairs is determined by the "correlated" dipolarfield due to 15Ni-13Ci and 13C'i-15Ni+1 dipolar couplings and is particularly sensitive to variations of thetorsion angle in the regime 
> 140
. However, the ability of this experiment to constrain multiple -torsionangles is limited by the resolution of the 13C-13CO correlation spectrum. This problem is partially addressedin the second approach described here, which is an NCOCA NCCN experiment. In this case the resolutionis enhanced by the superior spectral dispersion of the 15N resonances present in the 15Ni+1-13Ci part ofthe NCOCA chemical shift correlation spectrum. For the case of the 62-residue -spectrin SH3 domain,we determined 13 angle constraints with the INADEQUATE NCCN experiment and 22 constraintswere measured in the NCOCA NCCN experiment.
-Spectrin SH3 domain using two different 3D 15N-13C-13C-15N dipolar-chemicalshift magic-angle spinning (MAS) NMR experiments. The first NCCN experiment utilizes double quantum(DQ) spectroscopy combined with the INADEQUATE type 13C-13C chemical shift correlation. The decayof the DQ coherences formed between 13C'i and 13Ci spin pairs is determined by the "correlated" dipolarfield due to 15Ni-13Ci and 13C'i-15Ni+1 dipolar couplings and is particularly sensitive to variations of thetorsion angle in the regime > 140. However, the ability of this experiment to constrain multiple -torsionangles is limited by the resolution of the 13C-13CO correlation spectrum. This problem is partially addressedin the second approach described here, which is an NCOCA NCCN experiment. In this case the resolutionis enhanced by the superior spectral dispersion of the 15N resonances present in the 15Ni+1-13Ci part ofthe NCOCA chemical shift correlation spectrum. For the case of the 62-residue -spectrin SH3 domain,we determined 13 angle constraints with the INADEQUATE NCCN experiment and 22 constraintswere measured in the NCOCA NCCN experiment.