[Cs⁺(Cryptand[2.2.2])]I⁻ (1; Cryptand[2.2.2] = C222) was characterized via single‐crystal X‐ray diffraction and was shown to crystallize in the monoclinic space group I2/c system with a = 8.9605 (2), b = 23.5073 (5), c = 11.7563 (3) Å, and β = 93.792 (2)°. Stationary and magic angle spinning (MAS) experiments under different magnetic fields allowed for the separation of the chemical shift and quadrupole coupling tensor parameters. Remarkably, MAS spectra showing pure second‐order quadrupole powder patterns at 4.23 T were observed for ¹³³Cs nuclei with small quadrupole moments owing to the large electric field gradients (EFGs) caused by short CsO and CsN bond distances in the [Cs⁺(C222)] ions. Stationary NMR powder patterns with a combination of the chemical shifts and second‐order quadrupolar interactions were observed. The EFG and chemical shift tensor components calculated using the atomic coordinate files and Gaussian 09 were reasonably consistent with the experimental values.

中文翻译：

---

[Cs +（Cryptand [2.2.2]）] X（X = I-，SCN-·H2O）的固态133Cs NMR光谱中的化学位移和二级四极效应

[铯⁺（穴醚[2.2.2]）]我^-（1;穴状配体- [2.2.2] = C222）通过单晶X射线衍射进行了表征，并示出的单斜空间群结晶I2 / C系统其中a = 8.9605（2），b = 23.5073（5），c = 11.7563（3）Å，β = 93.792（2）°。在不同磁场下的固定和魔术角旋转（MAS）实验允许分离化学位移和四极耦合张量参数。值得注意的是，由于短Cs引起的大电场梯度（EFGs），在小四极矩的¹³³ Cs核中观察到了在4.23 T处显示纯二阶四极粉末模式的MAS光谱。 O和Cs的 N的[CS键距离⁺（C222）]离子。观察到具有化学位移和二阶四极相互作用的组合的固定NMR粉末模式。使用原子坐标文件和高斯09计算出的EFG和化学位移张量分量与实验值基本一致。