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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 1.82 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. File list (8) download file view on ChemRxiv 2021_02_Ivanova_manuscript_ChemRxiv.pdf (3.17 MiB) download file view on ChemRxiv 2021_02_Ivanova_SI_ChemRxiv.pdf (9.00 MiB) download file view on ChemRxiv ek20_sq-finalcif.cif (3.79 MiB) download file view on ChemRxiv ek27_sq-finalcif.cif (2.93 MiB) download file view on ChemRxiv si30_sq-finalcif.cif (1.64 MiB) download file view on ChemRxiv 2Me_channel.mp4 (2.20 MiB) download file view on ChemRxiv 2Et_channel.mp4 (2.33 MiB) download file view on ChemRxiv 2nBu_channel.mp4 (2.64 MiB)

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