Lai Zhenzhen, Li Aimin, Peng Sangshan, Sessler Jonathan L, He Qing
State Key Laboratory of Chemo/Biosensing and Chemometrics, College of Chemistry and Chemical Engineering, Hunan University Changsha 410082 P. R. China
Department of Chemistry, The University of Texas at Austin 105 East 24th Street, Stop A5300 Austin Texas 78712 USA.
Chem Sci. 2021 Aug 12;12(35):11647-11651. doi: 10.1039/d1sc03713g. eCollection 2021 Sep 15.
Crystalline supramolecular architectures mediated by cations, anions, ion pairs or neutral guest species are well established. However, the robust crystallization of a well-designed receptor mediated by labile anionic solvate clusters remains unexplored. Herein, we describe the synthesis and crystalline behaviors of a trimacrocyclic hexasubstituted benzene in the presence of guanidium halide salts and chloroform. Halide hexasolvate clusters, [Cl(CHCl)], [Br(CHCl)], and [I(CHCl)], were found to be critical to the crystallization process, as suggested by the single-crystal structures, X-ray powder diffraction (XRPD), thermogravimetric analysis (TGA), scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS), and NMR spectroscopy. This study demonstrates the hitherto unexpected role that labile ionic solvate clusters can play in stabilizing supramolecular architectures.
由阳离子、阴离子、离子对或中性客体物种介导的晶体超分子结构已得到充分证实。然而，由不稳定的阴离子溶剂化物簇介导的精心设计的受体的稳健结晶仍未被探索。在此，我们描述了一种三大环六取代苯在卤化胍盐和氯仿存在下的合成及晶体行为。单晶结构、X射线粉末衍射（XRPD）、热重分析（TGA）、带能谱的扫描电子显微镜（SEM-EDS）和核磁共振光谱表明，卤化物六溶剂化物簇[Cl(CHCl)]、[Br(CHCl)]和[I(CHCl)]对结晶过程至关重要。这项研究证明了不稳定的离子溶剂化物簇在稳定超分子结构中迄今未被预料到的作用。
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