Here we show how CVT reactions produce compounds in the Nb-Se-I ternary system and we present an exfoliable two-dimensional compound NbSe 2 I 2 , which has the space group of P 1 at room temperature, with an inplane crystallographic angle γ = 61.3 • . First, an efficient synthesis of NbSe 2 I 2 by CVT is reported. Next, the exfoliation of NbSe 2 I 2 down to few-layer and mono-layer structure is shown, and Raman spectroscopy was utilized to study the difference of bulk, few-layer, and mono-layer NbSe 2 I 2 . Electronic band structure calculated by density functional theory (DFT), together with transport, thermal, optical, and magnetic measurements, unveils the property of an exfoliable transition metal chalcogenide NbSe 2 I 2 .