Summary: The coordination networking of discrete metal-organic polyhedra (MOPs) involving different ligands as well as metals is a challenging task due to the features of limited solubility and chemical stability of these polyhedra. An unusual approach, ligand-oriented polyhedral networking via click chemistry and further metal coordination is reported here. An alkyne decorated Cu(II)-MOP self-catalyzes the regioselective click reaction (1,3-dipolar cycloaddition) using azide-functionalized ligands under unconventional reaction conditions. Introducing new metal ions, M(II), interlinks the carboxylic groups on the MOP surfaces creating coordination networks. On the other hand, exposure of the respective individual ligand components in the presence of Cu(II) promotes an in-situ click reaction along with metal coordination generating a new 3D-framework. These materials demonstrated a high drug hosting potential exhibiting a controlled progressive release of anticancer (5-flourouracil) and stimulant (caffeine) drugs in physiological saline at 37 °C. These innovative and unconventional MOP networks provide a significant conceptual advance in understanding.
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