Orange prismatic crystals of the supramolecular coordination polymer (SCP) ∞3[Cu(CN)2(Me3Sn)(Pyz)], SCP1, were synthesized using a self‐assembly method under ambient conditions. Nanosized 1 was obtained using the same molar ratio in water by ultrasonic irradiation. SCP1 was characterized using single‐crystal X‐ray diffraction, elemental analysis, thermal analysis and Fourier transform infrared spectroscopy. SCP1 and its nanosized 1 particles were also examined using powder X‐ay diffraction and scanning electron microscopy. The luminescence emission of SCP1 was studied as well as its use as a sensor for the detection of common organic solvents and metal ions. Also, the catalytic activities of nanosized 1 towards various organic dyes were investigated under ambient conditions, UV irradiation and ultrasonic irradiation. Nanosized 1 as a heterogeneous nanoparticle catalyst exhibits high catalytic activity for the degradation of eosin‐Y and acid blue dyes. The mechanism of degradation investigated using various scavenger techniques is proposed and discussed. The catalytic oxidation process is mainly caused by •OH radicals.

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The supramolecular coordination polymers (SCP); ∞3[Cu (CN)2(Me3Sn)(pyz)], pyrazine‐trimethyltin‐bis (cyanide) copperI SCP1, [Cu2(CN)3(Ph3Sn)(pyz)], pyrazine‐triphenyltin‐tris (cyanide) dicopperI SCP3 and [Cu2(CN)4(Ph3Sn)(Pyz2caH)2], bis‐pyrazine‐2‐carboxylic acid‐ triphenyltin‐tetrakis (cyanide) dicopperI SCP4 and the coordination complex (CC), [CuII (Pyz2‐ca)2(H2O)2]; diaquo‐bis‐(pyrazine‐2‐carboxylato) copper(II) complex: CC2, are synthesized by self‐assembly method at ambient conditions. Single crystal X‐ray structures of SCP1 and CC2 indicate the presence of CuI and CuII which adopt tetrahedral and octahedron geometry, respectively. The structures of SCP3 and SCP4 are solved by the density functional theory (DFT) calculations and spectroscopic methods. The Cu centers acquire triagonal plane, linear and tetrahedral geometry, respectively. The CN‐R3Sn‐NC spacer and pyrazine or pyrazine‐2‐carboxylic acid ligands extend the structures to 3D‐network. The tested compounds 1–4 are designed and synthesized to examine their effects on viability and proliferation of five human cancer cell lines. Also, they are tested for antioxidant activity using ABTS assay and rate erythrocyte hemolysis.