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Hybrid organic-inorganic halide perovskites (HOIPs) have received continued interest for their structure diversity and potential application in optoelectronic, solar cells, nonlinear optics (NLO), and ferroelectrics. Structural symmetry breaking induced by water molecules in single-crystal-to-single-crystal (SCSC) transformations is beneficial to develop ferroelectrics or second-harmonic generation (SHG) materials. Along this line, a water-containing two-dimensional (2D) double perovskite, (C

Nine supramolecular self-assembly entities consisting of cucurbit[5]uril, potassium salts, and hydroxybenzene or its derivatives were constructed by conventional methods. In this supramolecular architectural system, Q[5]s and the metal ions (K+) form infinite chains through coordination and ion−dipole interaction, and the stacking of these supramolecular chains then forms wavelike “walls”. The layers of hydroxybenzene or its derivatives are sandwiched by these wavelike walls, and the counteranions are captured in the molecular channels formed by the supramolecular chains. The gap between the adjacent walls is dependent on the size of the hydroxybenzene or its derivatives.