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In this contribution, the preparation of the supramolecular nano-/microcrystals [Co ? (NH 3 ) 5 Cl] 3 [Fe ? (CN) 6 ] 2 via a simple and efficient solution ionic self-assembly approach was reported. The results demonstrated that the morphologies of these microcrystals could be changed arbitrary by tuning the solvent. Various shapes such as polyhedron, microrod, rectangular tube, tubular hexagonal prism, and tubular hexagonal prism were obtained in different solvents. The polarity and the acidity of solvent showed a significant effect on the shape of the products. The regrowth process and its possible mechanism of these microcrystals were also recounted in detail.

Ionic Self-Assembly in Solution: Synthesis, Morphology Control, and Mechanism of [CoIII(NH3)5Cl]3[FeII(CN)6]2 Micro-Crystals