A green, simple, and efficient room-temperature aqueous synthetic route for the fabrication of novel porous coordination polymer nanoparticles (NPs) composed of Cu2+ and imidazolate was developed. Colloidal stability, morphology changes, and structural and chemical integrity of the developed NPs, in several solvents having different polarity, were investigated. Basic physicochemical properties of selected NPs (i.e., NP1, NP2, and NP3), such as size, optical and magnetic activity, porosity, thermal stability, structure, aging, and catalytic activity, were determined. Data indicate that the addition of the surfactant hexadecyltrimethylammonium bromide (CTAB) and the final solvent determine the size, morphology, and structure of the different NPs.