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Cocrystallizationof a versatile organic tecton, 3,3′,5,5′-tetramethyl-4,4′-bipyrazole(tmbpz), with aliphatic dicarboxylic acid suberic acid (H2sub) and sebacic acid (H2seb) generates two supramolecularsolids [(tmbpz)2·(H2sub)] (1) and [(tmbpz)2·(H2seb)] (2). In the present case, both cocrystals could be obtained from eithersolution evaporation or mechanochemical solid-state reaction. Single-crystalstructural analyses reveal that the 1and 2are 4-fold and 5-fold 2D → 2D parallel interpenetrated 63-hcb networks, respectively. The substantial dissimilaritiesin the degree of interpenetration are modulated by the different lengthsof dicarboxylic acids. The thermal stabilities and photoluminescencebehaviors of them were also discussed. [ABSTRACT FROM AUTHOR]