<p>The superconducting phase (orthorhombic) of niobium sulfide (<i>o</i>-NbS), remains largely unexplored in terms of its structural and morphological characteristics. In this study, we report the first comprehensive investigation of pristine and selenium-doped <i>o-</i>NbS using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), and Raman spectroscopy. The retention of the Pnma phase upon doping is revealed with subtle lattice expansion. SEM imaging reveals rod-like crystallites in both pristine and doped <i>o</i>-NbS. The EDS confirms successful incorporation of selenium with 10.8% doping concentration. XPS analysis reveals the presence of Nb²⁺ and S bonding. Raman spectroscopy reveals a red shift in the peaks suggesting softening of lattice vibrations upon doping. Our study establishes a foundational understanding of the structural and morphological nature of <i>o-</i>NbS and demonstrates influence of anion doping on its microstructure, laying the groundwork for future investigations into its superconducting behaviour and physical properties.</p>