The PXRD patterns from the HT crystallization screen that could not be assigned to 3-, 4-, or 5-fold structures were mostly crystallized using the structurally-related anti-solvents o-xylene, m-xylene, p-xylene, mesitylene, 1,2-dimethoxybenzene, and 1,3-dimethoxybenzene (SI, Figure ). We used the THF crystallizations with the following anti-solvents to determine the X-ray crystal structures for three of these hits: o-xylene (ADTA_2-27), 1,2-dimethoxybenzene (ADTA_2-34), and 1,3-dimethoxybenzene (ADTA_2-35) (SI, Table ). In the crystal structure of ADTA_2-34 we found ordered 1,2-dimethoxybenzene between ADTA molecules, whereas the aromatic solvents in ADTA_2-27 and ADTA_2-35 were too disordered to model accurately. However, the three structures, ADTA_2-27, ADTA_2-34, and ADTA_2-35 have the same underlying 2-fold interpenetrated structure. The crystallized 2-fold interpenetrated structures that we isolated experimentally did not have exact matches on the crystal structure landscape. In the case of ADTA_2-34, there are two symmetrically inequivalent ADTA molecules in the structure, which was not considered in the CSP search. For the other observed structures with 2-fold interpenetration of hydrogen bond networks, the absence of exact experimental matches can be rationalized by the larger solvent content with respect to the 3-fold and 4-fold structures, and the effect of solvent molecules on the relative arrangement of the two hydrogen bonding networks of ADTA molecules.