1) New PbHNSO3 crystals were grown using a double diffusion gel technique with agar gel as the growth medium. Dark brown crystals measuring 0.25x0.30x0.40mm were harvested after 20 days. 2) The crystals were characterized through powder and single crystal XRD, FTIR, photoluminescence spectroscopy, and TG-DSC analysis. XRD confirmed the crystalline nature and FTIR identified the functional groups present. 3) Photoluminescence spectroscopy showed two strong emission peaks at 417nm and 477nm upon excitation at 290nm. TG-DSC analysis revealed a structural change occurring around 537°C and decomposition between 862-