Single crystals of Pb2Bi2AlB3O 11 were grown from a PbO/Bi2O3/Al 2O3/H3BO3/PbF2 flux. The single-crystal X-ray structural analysis showed that Pb2Bi 2AlB3O11 crystallizes in the monoclinic space group C2/c (No. 15) with a = 17.263(2) A˚, b = 8.7322(11) A˚, c = 6.8081(9) A˚, α = 90°, β = 90.566(2)°, γ = 90°, Z = 4 and R1 = 0.0393, wR2 = 0.1013. Its structure may be described as three-dimensional frameworks formed of (1 0 0) [Pb6Bi6Al3O6]∞ layers stacked along a-axis. The layers are interconnected via BO3 groups. The IR spectrum further confirmed the presence of BO3 groups in the structure. The thermal analysis suggests that Pb2Bi 2AlB3O11 is a congruently melting compound.