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从剩余二极合常数来确定溶液中的糖结构:方法和适用于甲基β-D-xylopyranoside的方法

Tran N Pham¹, Sarah L Hinchley, David W H Rankin

¹Contribution from the School of Chemistry, University of Edinburgh, West Mains Road, Edinburgh EH9 3JJ, Scotland, U.K.

Journal of the American Chemical Society

|October 8, 2004

概括

我们开发了一种新的NMR方法,使用稀释液晶中的残留二极合物来确定溶液中的小分子结构. 这种技术准确地解决了甲基β-d-xylopyranoside的结构.

科学领域:

结构生物学结构生物学
核磁共振 (NMR) 光谱学核磁共振 (NMR) 光谱学
计算化学计算化学

背景情况:

在化学和生物学中,确定小分子溶液结构至关重要.
传统的NMR方法在较大的分子中可能受到光谱复杂性的限制.
剩余二极合器 (RDC) 提供有价值的远程定向信息,但需要分子对齐.

研究的目的:

开发和验证一种新的方法来确定使用RDCs的小分子溶液结构.
通过解决甲基β-d-xylopyranoside的结构来证明这种方法的实用性.
在NMR研究中克服与强烈对齐液晶相关的局限性.

主要方法:

在稀释液晶中测量残余二极合常量 (D(HH),D(CH和nD(CH).
利用基于强度的J调节的NMR技术,并开发了新的恒时HMBC NMR实验.
结构的改进包括使用振动平均RDC优化几何和顺序参数.

主要成果:

成功地确定了甲基β-d-xylopyranoside的溶液结构,并且具有很高的准确性.
测量了30个RDC,精度优于+/- 0.02 Hz.
精细的结构与初始计算有很好的一致性,大多数角度的差异为<=0.8度.

结论:

开发的方法使得使用稀释液晶中的RDCs精确确定溶液中的小分子的结构.
这种方法减轻了在强烈对齐的媒体中遇到的光谱复杂性问题.
该技术对于具有超过12个质子的分子的结构研究是有价值的.

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