Solid-state QCPMG NMR of low-γ quadrupolar metal nuclei in natural abundance
Solid-state QCPMG NMR of low-γ quadrupolar metal nuclei in natural abundance
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DOI：
10.1021/ja0003526
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发表时间：
2000-07-26
影响因子：
15
通讯作者：
Nielsen, NC
中科院分区：
文献类型：
--
作者：
Larsen, FH;Skibsted, J;Nielsen, NC
利用一个数量级的灵敏度增强的四极回波（QE）的固态NMR光谱的采样在四极Carr-Purcell-Meiboom-Gill（QCPMG）脉冲序列中获得的优势，我们证明了低γ四极金属核的配位环境，可以研究这些核在自然丰度的粉末常规。通过对K2 MoO 4、KVO 3、Mg（VO 3）（2）、Zn（CH 3COO）（2）的K-39、Mg-25、Zn-67和Sr-87 QCPMG固态NMR实验证明了该方法的普遍适用性。2H（2）O，Zn（Ala）（2）. H2O、Sr（NO3）（2）和SrMoO 4。对于所有样品的四极耦合参数和各向同性化学位移提取的数值模拟和迭代拟合的自旋回波边带光谱中观察到的实验QCPMG NMR谱。根据化合物的晶体结构讨论了这些参数。
Taking advantage of an order of magnitude in sensitivity enhancement obtained by sampling of quadrupolar-echo (QE) solid-state NMR spectra during a quadrupolar Carr-Purcell-Meiboom-Gill (QCPMG) pulse sequence, we demonstrate that the coordination environment of low-gamma quadrupolar metal nuclei can be studied routinely for powders with these nuclei in natural abundance. The general applicability of the method is demonstrated by K-39, Mg-25, Zn-67, and Sr-87 QCPMG solid-state NMR experiments for K2MoO4, KVO3, Mg(VO3)(2), Zn(CH3COO)(2). 2H(2)O, Zn(Ala)(2). H2O, Sr(NO3)(2), and SrMoO4. For all samples the quadrupolar coupling parameters and the isotropic chemical shifts are extracted by numerical simulation and iterative fitting of the spin-echo sideband spectra observed in the experimental QCPMG NMR spectra. These parameters are discussed in light of the crystal structures for the compounds.