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Ivanova, Svetlana; Köster, Eva; Holstein, Julian J.; Keller, Niklas; Clever, Guido H.; Bein, Thomas and Beuerle, Florian (2021): Isoreticular Crystallization of Highly Porous Cubic Covalent Organic Cage Compounds**. In: Angewandte Chemie-International Edition, Vol. 60, No. 32: pp. 17455-17463

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Modular frameworks featuring well-defined pore structures in microscale domains establish tailor-made porous materials. For open molecular solids however, maintaining long-range order after desolvation is inherently challenging, since packing is usually governed by only a few supramolecular interactions. Here we report on two series of nanocubes obtained by co-condensation of two different hexahydroxy tribenzotriquinacenes (TBTQs) and benzene-1,4-diboronic acids (BDBAs) with varying linear alkyl chains in 2,5-position. n-Butyl groups at the apical position of the TBTQ vertices yielded soluble model compounds, which were analyzed by mass spectrometry and NMR spectroscopy. In contrast, methyl-substituted cages spontaneously crystallized as isostructural and highly porous solids with BET surface areas and pore volumes of up to 3426 m(2) g(-1) and 1.84 cm(3) g(-1). Single crystal X-ray diffraction and sorption measurements revealed an intricate cubic arrangement of alternating micro- and mesopores in the range of 0.97-2.2 nm that are fine-tuned by the alkyl substituents at the BDBA linker.

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