Single crystals of triclinic NbSe 2 I 2 have been grown by a reliable two-tube CVT method that also produces quasi-one-dimensional (Nb 4 Se 15 I 2 )I 2 , and the P 1 crystal structure has been verified. The exfoliation of NbSe 2 I 2 down to few-layer and mono-layer structures was shown, and Raman spectroscopy was conducted on bulk, few-layer, and monolayer samples. Distinct Raman peaks are observed in the few-layer samples, while mono-layers may suffer from beam damage or environmental degradation. Polarized Raman spectroscopy showed different transitions for different orientations, corresponding with the lattice symmetry of the crystal. NbSe 2 I 2 is a semiconductor, which has been shown by PBE-DFT calculations, as well as resistivity measurements. It does not undergo phase transformations below room temperature, and it stays as a diamagnet. It remains to be seen if strain can be a factor to alter the electronic structure of NbSe 2 I 2 or to change the transition temperature between the triclinic and monoclinic phases. Furthermore, thin film heterostructures are also possibilities to tune the property of NbSe 2 I 2 or to utilize NbSe 2 I 2 as a media to introduce strain due to its triclinic to monoclinic structural transition at around 200 • C. Moreover, the in-plane angle γ = 61.