Single crystals of two triptycene-based catechol derivatives 1 and 2 were obtained,and their X-ray crystal structural studies showed that the two tecton molecules had different conformations in the solid state,and they could self-assemble into interesting 3D networks with solvent molecules included inside, in which multiple O-H…O hydrogen bonds played important roles. Single crystals of two triptycene-based catechol derivatives 1 and 2 were obtained, and their X-ray crystal structural studies showed that the two tecton molecules had different conformations in the solid state, and they could be self-assembled into interesting 3D networks with solvent molecules included inside, in which multiple OH ... O hydrogen bonds played important roles.