A tridentate 3-pyridyl-based ligand containing a hexaazaphenalene skeleton (3-TPHAP − ) with topologically isolated p orbitals was prepared by a onepot reaction. It was successfully reacted with a Co 2+ salt and a 1,4benzenedicarboxylic acid co-ligand to give a porous coordination network. In the structure, the hexaazaphenalene skeleton interacts with water to form an internal hydrogen bonding network, allowing the entire pore space to be revealed by single-crystal X-ray diffraction (SXRD). The network structure consists of dimeric Co clusters featuring labile sites occupied by solvent molecules. Several guest molecules, namely, anthracene, triphenylene, and iodine, were incorporated inside the network. The resultant encapsulated structures were elucidated by SXRD, revealing unusual host−guest interactions with a subtle structural modulation.
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