Assembly of Seven Supramolecular Compounds with <i>p</i>-Sulfonatocalix[6]arene

Seven supramolecular compounds comprising p-sulfonatocalix[6]arene and transition metals, {[Cu(Imz)(phen)(H2O)]4[C6AS]}·10H2O (1), {[Cu(Imz)2(phen)]2[Cu(Imz)(phen)(H2O)2]2[C6AS]}·13.3H2O (2), {[M(phen)2(H2O)][M(phen)2]2[C6AS]}·nH2O (3 and 4) (3: M = Co and n = 29.6; 4: M = Zn and n = 29.9), {[Cu(phen)2]4[C6AS]}2·13H2O (5), [H3O]2[Co(phen)3]2[C6AS]·10.7H2O (6), and [Cu(phen)2(H2O)]2{[Cu(phen)2]2[C6AS]}·8H2O (7) (phen = 1,10-phenanthroline, C6AS = p-sulfonatocalix[6]arene, Imz = imidazole), have been synthesized by a hydrothermal method and structurally characterized by IR spectroscopy, thermogravimetric-differential thermal analysis (TG-DTA), and single crystal X-ray diffraction. It is found that not only the acidity of the feeds plays an important role in the syntheses, but also the kind of metals, the molar ratio of the reactants, and the cochelating ligands influence the final extended structures. The extended structures are featured with two-dimensional (2D) coordination layers, one-dimensional chains, or zero-dimensional fragments. Notedly, the 2D metal-C6AS coordination layer was observed for the compounds of p-sulfonatocalix[6]arene for the first time. In these structures, all the C6AS ligands adopt a 1,2,3-alternate conformation.