A new coordination polymer containing mixed ligands, namely [Ni(S₂COiBu)₂(DBPMF)·(CHCl₃)]_∞ (DBPMF = 2,7-dibromo-9,9-(4-pyridylmethyl)fluorine), has been synthesized and structurally characterized by elemental analysis and single-crystal X-ray diffractions. X-ray structural analysis reveals that each Ni atom is coordinated by two isobutyl xanthogenate molecules and two nitrogen atoms from two DBPMF ligands to form octahedral coordination geometry. DBPMF acts as a bridge to form a coordination polymer. Fluorescence property of this coordination polymer displays a broad emission band at λ = 413 nm. Thermal analysis shows that the solvent molecule CHCl₃ can be stabilized in the crystal structure until 140 °C.