The synthesis and structural study of three new AII(SbV0.5FeIII0.5)(PO4)2 (Adouble bond; length as m-dashBa, Sr, Pb) phosphates belonging to the Asingle bond-Sbsingle bond-Fesingle bond-Psingle bond-O system were reported here for the first time. Structures of [Ba], [Sr] and [Pb] compounds, obtained by solid state reaction in air atmosphere, were determined at room temperature from X-ray powder diffraction using the Rietveld method. BaII(SbV0.5FeIII0.5)(PO4)2 [Ba] features the yavapaiite-type structure, with space group C2/m, Z = 2 and a = 8.1568(4) Å; b = 5.1996(3) Å c = 7.8290(4) Å; β = 94.53(1)°. AII(SbV0.5FeIII0.5)(PO4)2 (Adouble bond; length as m-dashSr, Pb) compounds have a distorted yavapaiite structure with space group C2/c, Z = 4 and a = 16.5215(2) Å; b = 5.1891(1) Å c = 8.0489(1) Å; β = 115.70(1)° for [Sr]; a = 16.6925(2) Å; b = 5.1832(1) Å c = 8.1215(1) Å; β = 115.03(1)° for [Pb]. Raman and Infrared spectroscopic study was used to obtain further structural information about the nature of bonding in selected compositions.rtain.