Single crystals of Pb2CuB2O6 were grown from a PbO/CuO/B2O3 flux, and crystallize in a monoclinic cell of dimensions a = 5.6311(6), b = 8.7628(9), c = 6.2025(6) angstrom, and = 115.7060(10)degrees 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 CuO4 and triangular planar BO3 groups. The results of quantitative analysis ICP, DTA, vibrational spectroscopy, and magnetic investigations are also presented. (C) 2006 Elsevier Ltd. All rights reserved.