The nanosized supramolecular coordination polymers (SCPs)³_∞[Cu(μ²CN)₂]₂.(Me₃Sn)₂.(phen)₂],SCP1,and [Cu₂(CN)₄(Ph₃Sn)₂(phen)],SCP2, were prepared utilizing self‐assembly method under ultrasonic irradiation. Single crystal X‐ray diffraction (XRD) of SCP1supports the presence of two anionic [Cu(μ²CN)₂]⁻fragments connected by two (Me₃Sn)⁺cations, while the two phenanthroline (phen) molecules coordinate to the Cu atoms. The two Cu atoms are crystallographically different, while they are chemically identical forming tetrahedral geometry. The structure of SCP2was achieved by calculations using DFT (the density functional theory) and spectroscopic studies. The geometries around the Cu atoms adopt triagonal plane and tetrahedral structure. Spectroscopic data, energy‐dispersive X‐ray spectroscopy (EDX), transmission electron microscopy (TEM), and analytical analysis confirm the chemical formula of SCP2. The nanosized tested compounds1and2are designed to investigate their action on viability and proliferation of five human cancer cell lines. In addition, 2, 2'‐azino‐bis (3‐ethyl benzthiazoline‐6‐sulfonic acid) (ABTS) assay and rate erythrocyte hemolysis were used to test the antioxidant activity of the nanosized SCP1and SCP2. Also, the SCP1and2exhibit good antimicrobial activity keeping them as promising drug candidates for the treatment of bacterial and fungal infections.