The CVT synthesis of NbSe 2 I 2 gained its insight from the CVT synthesis of (TaSe 4 ) 2 I 38 as well as the discovery of (Nb 4 Se 15 I 2 )I 2 . Thin sheets of NbSe 2 I 2 crystals were first discovered from a trial CVT synthesis with the starting ingredients at 460 • C and the crystals grown at a lower temperature at 420 • C. This unusual CVT growth from higher temperature to lower temperature matches with the published synthesis of many Nb-Se-I ternary compounds. However, very few NbSe 2 I 2 crystals smaller than 1 × 1 mm were obtained, mixing with other compounds, likely the binary compound between selenium and iodine. Moreover, we found that this synthesis is not easily reproducible and that (NbSe 4 ) 3 I crystals occasionally grew instead of NbSe 2 I 2 crystals.