This study presents the synthesis and characterization of the metal orthophosphate salt Pb(Sb0.5Al0.5)(PO4)2. The compound was meticulously prepared via solid-state reactions under ambient air conditions. The crystal structure was determined using Rietveld refinement based on powder X-ray diffraction data, providing detailed information on their atomic arrangements and spatial configurations. Pb(Sb0.5Al0.5)(PO4)2 adopts a low-yavapaiite structure crystallizing in the monoclinic lattice with space group C2/c and Z = 4; a = 16.605(9) Å; b = 5.128(6) Å; c = 8.073(3) Å; β = 115.17(1)°; V = 631(1) Å3. Complementary Raman and infrared spectroscopy techniques allowed us to study in more detail the structural and bonding properties of the crystalline solid. In addition, the morphology was studied, and the chemical composition was confirmed by scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS). The material's optical bandgap was estimated using ultraviolet–visible (UV–Vis) spectroscopy, and the result was roughly 3.8 eV. The insulating nature of a material cannot be verified by optical observation alone, although the wide bandgap increases the likelihood of such an occurrence. Measuring electrical conductivity is necessary for certain verification of an insulating nature. This study also presents a comprehensive study of the dielectric and electrical conductivity properties of this new material with mixed Sb5+ and Al3+ ions in the octahedral sites of the yavapaiite structure which exhibits very high electrical resistivity over a wide range of frequencies and temperatures. The study uses an approach combining the analysis of permittivity, impedance, complex modulus, and alternating current (AC) conductivity curves, which is very useful for understanding the electrical conduction and relaxation mechanisms in this type of material.