Trimacrocyclic hexasubstituted benzene linked by labile octahedral [X(CHCl3)6]− clusters |
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| Authors: | Zhenzhen Lai Aimin Li Sangshan Peng Jonathan L Sessler Qing He |
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| Institution: | 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 |
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| Abstract: | 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 2 in the presence of guanidium halide salts and chloroform. Halide hexasolvate clusters, viz. Cl(CHCl3)6]−, Br(CHCl3)6]−, and I(CHCl3)6]−, 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.We report the synthesis and robust crystallization of a trimacrocyclic hexasubstituted benzene and guanidium mediated by unprecedented labile halide hexasolvate clusters, viz. Cl(CHCl3)6]−, Br(CHCl3)6]−, I(CHCl3)6]−, and Br(CHBr3)6]−. |
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