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Abstract: Synthesis and structural determination by the Rietveld method of a new compound with pyrochlore-like structure (Bi1.524Cu0.476)(Sb1.524Cu0.476)O7+δ . A new polycristalline compound with pyrochlore-like structure and chemical formula (Bi1,524Cu0,476)(Sb1,524Cu0,476)O7+δ has been synthesized using the classical solid-state reaction method. The Rietveld structure determination shows that the cubic cell parameter is a =10.430(1) Å and the space group Fd m with eight formula units per cell. The reliability factors are R p =7.1; R wp =9.28 and R exp =5.33. The electric resistivity measured by means of the four probe method at room temperature on sintered pellets is about 105 Ω cm. The magnetic susceptibility measurements achieved between 300 and 800 K show the existence of an effective moment μeff =2.27 μB. To cite this article: M. Sellami et al., C.R. Chimie 8 (2005) . [Copyright &y& Elsevier]