Reported here is the highly efficient separation of industrially important cis-and trans-1,2-dichloroethene (cis-DCE and trans-DCE) isomers by activated crystalline 2,2',4,4'tetramethoxyl biphen[3]arene (MeBP3) materials,M eBP3a. MeBP3 can be synthesized in excellent yield (99 %), and ac yclic pentamer is also obtained when using 1,2-dichloroethane as the solvent. The structure of MeBP3 in the CH 3 CN@MeBP3 crystal displays at riangle-shape topology, forming 1D channels through window-to-windowp acking. Desolvated crystalline MeBP3 materials,M eBP3a,p referentially adsorb cis-DCE vapors over its trans isomer.MeBP3a is able to separate cis-DCE from a5 0:50 (v/v) cis/trans-isomer mixture,y ielding cis-DCE with ap urity of 96.4 %i nas ingle adsorption cycle.S ingle-crystal structures and powder X-ray diffraction patterns indicate that the uptake of cis-DCE triggers as olid-state structural transformation of MeBP3, suggesting the adaptivity of MeBP3a materials during the sorption process.M oreover,t he separation can be performed over multiple cycles without loss of separation selectivity and capacity.

Reported here is a molecule‐Lego synthetic strategy for macrocycles with functional skeletons, involving one‐pot and high‐yielding condensation between bis(2,4‐dimethoxyphenyl)arene monomers and paraformaldehyde. By changing the blocks, variously functional units (naphthalene, pyrene, anthraquinone, porphyrin, etc.) can be conveniently introduced into the backbone of macrocycles. Interestingly, the macrocyclization can be tuned by the geometrical configuration of monomeric blocks. Linear (180°) monomer yield cyclic trimers and pentamers, while V‐shaped (120°, 90° and 60°) monomers tend to form dimers. More significantly, even heterogeneous macrocycles are obtained in moderate yield by co‐oligomerization of different monomers. This series of macrocycles have the potential to be prosperous in the near future.

The complexation and separation of industrially important cis- and trans-1,2-dichloroethene (cis- and trans-DCE) isomers using perethylated pillar[5]arene (EtP5) are described.