IN RECENT YEARS, silver (I) COORDINATION POLYMERS HAVE RECEIVED MUCH ATTENTION BECAUSE silver (I) SHOWS A TENDENCY TO FORM COORDINATION POLYMERS WITH UNIQUE METAL-CARBON AND METAL-METAL INTERACTIONS [1]. SEVERAL METHODS CAN BE APPLIED TO SYNTHESIZE silver NANOPARTICLES WITH WELL-DEFINED SHAPES. CONTINUING OUR PREVIOUS WORK ON silver (I) COORDINATION POLYMERS [2,3] AND STUDIES ON THE RELATION BETWEEN THE silver (I) COORDINATION POLYMER DIMENSION AND THE DIMENSION OF THE RESULTING silver NANO-STRUCTURE, IN THIS PAPER WE DESCRIBE THE PREPARATION OF A NEW silver (I) COORDINATION POLYMER FROM silver (I) THIOCYANATE AND 4-BPDB LIGAND, [AG(4-BPDB)(SCN)]N (1), 4- BPDB = 1,4-BIS (4-PYRIDYL)-2,3-DIAZA-1,3-BUTADIEN AND ITS USE AS A PRECURSOR FOR THE PREPARATION OF silver NANOSTRUCTURES. REACTION BETWEEN THE ORGANIC NITROGEN DONOR-BASED LIGAND 4-BPDB AND silver (I) NITRATE PROVIDED A CRYSTALLINE MATERIAL WITH THE GENERAL FORMULA [AG(4-BPDB)(SCN)]N (1). THE IR SPECTRUM OF COMPOUND 1 SHOWS CHARACTERISTIC BAND OF THE THIOCYANATE ANION APPEARS AT 2120 CM-1. SINGLE X-RAY CRYSTAL ANALYSIS REVEALS THAT COMPOUND 1 CRYSTALLIZES IN THE MONOCLINIC SPACE GROUP P121C1 THAT CONSISTS OF TWO-DIMENSIONAL SHEETS OF [AG(4-BPDB)(SCN)]N (FIG. 1.A). THE THERMAL STABILITY OF COMPOUND 1 WAS STUDIED BY THERMAL GRAVIMETRIC (TG) AND DIFFERENTIAL THERMAL ANALYSES (DTA). ALSO, DIFFERENT NANO POWDERS AND NANOSTRUCTURES HAVE BEEN PREPARED VIA DIRECT CALCINATION OF COMPOUND 1 AT 300, 400, 500 AND 600 °C (FIG. 1.B). THE MORPHOLOGY, STRUCTURE AND SIZE OF THE FOUR SAMPLES PREPARED BY THE CALCINATION METHOD AT DIFFERENT TEMPERATURE WERE INVESTIGATED BY SCANNING ELECTRON MICROSCOPY (SEM) AND X-RAY POWDER DIFFRACTION (XRD). THIS STUDY DEMONSTRATES THAT COORDINATION POLYMERS MAY BE SUITABLE PRECURSORS FOR THE PREPARATION OF NANO SCALE MATERIALS.