This study aimed to evaluate the X-linked hypophosphatemic rickets (XLHR)-related compositional and microhardness tooth aspects. One affected and one non-affected teeth by XLHR were sectioned transversely, and each section was separated for Micro-Raman spectroscopy, Knoop microhardness and scanning electron microscopy with energy dispersive x-ray microanalysis (SEM-EDS). The outcomes of these analyses were assessed. Outcomes of Raman analysis of inorganic/organic components (~958/~1250+~1450 cm?1) and carbonate/phosphate (~1070/~958 cm?1) ratios showed areas of altered enamel and dentin (interglobular dentin, calcospherites, and mantle dentin) with an increase of inorganic content in the rickets tooth. Microhardness reduction was observed in the affected tooth, with a more evident drop in regions of mantle dentin, interglobular dentin, and calcospherites. SEM-EDS analysis showed demonstrated the absence of calcium and phosphorus in interglobular spaces. In conclusion, compositional and structural deficiencies were observed in deciduous tooth affected by XLHR. Also, it was observed the absence of hydroxyapatite in the interglobular dentin by using Raman spectroscopy analysis.