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Single crystals of AgSCN supramolecular coordination polymer, SCP1 and the nanosized particles of AgSCN, 2, are synthesized by self-assembly and ultrasonic radiation methods, respectively. The structure comprises of the simple AgSCN molecule fabricated by a tetrahedral Ag atom and one thiocyanate group. The SCN ligand connects four Ag atoms via µ3-S and one nitrogen atom. Two silver atoms and two sulfur atoms form rhombic mini-cycle (Ag2S2) motif exhibiting argentophilic interaction. The structure of SCP1 extends three-dimensionally via coordinate bonds creating different fused polygons. The chemical structure and morphology of nanosized 2 are characterized by powder X-ray diffraction and transmission electron microscopy (TEM) and spectroscopic methods. The heterogeneous catalytic and photo-catalytic activity of nanosized 2 exhibit very efficient catalytic activity towards degradation of Acid Blue-92 and Eosin-Y dyes within very short times under UV-light or ultrasonic radiation. The good limit of detection and the high quenching efficiency of SCP1 towards selective quantitative determination of nitrobenzene (NB) and Fe3+ ions support its behavior as an efficient luminescent sensor.