An investigation of the interaction of Bi(III) with an aqueous solution of p-toluenesulfonic acid at 70 degrees C is performed. As a result, a new composition [Bi6O6(OH)(3)](C7H7SO3)(3) is precipitated. The product synthesized is characterised by various methods: elemental analysis, FTIR, DTA, TG-MS, and powder X-ray diffraction. The symmetry - orthorhombic F222 space group, and unit cell parameters: a = 9.8056 angstrom, b = 17.1970 angstrom and c = 39.256 angstrom are determined. Based on the experimental results, X-ray diffraction indexation, as well as thermal decomposition products of the compound are suggested. (C) 2014 Elsevier B.V. All rights reserved.