Single crystals of Pb 2 CuB 2 O 6 were grown from a PbO/CuO/B 2 O 3 flux, and crystallize in a monoclinic cell of dimensions a = 5.6311(6), b = 8.7628(9), c = 6.2025(6) Å , and b = 115.7060(10)8 with Z = 2; the space group is P2 1 /c (no. 14). The structure was determined from 662 unique reflections and refined to the final residuals R 1 = 0.0217, wR 2 = 0.0586. The structure is characterized by the two-dimensional layer of interconnected rectangular planar CuO 4 and triangular planar BO 3 groups. The results of quantitative analysis ICP, DTA, vibrational spectroscopy, and magnetic investigations are also presented. #