Synthesis and magnetic properties study of solids solutions (Bi1.524–xMxCu0.476)[Sb1.524Cu0.476]O7+δ with M = Ca et Pb. The solid solutions with pyrochlore-like structure and general chemical formula (Bi1.524–xMxCu0.476)[Sb1.524Cu0.476]O7+δ (M = Ca2+, Pb2+) have been synthesized by solid-state chemical reaction at high temperature. The two solutions crystallize in the cubic system, with Fdm space group. Domains of homogeneity are 0 ≤ x ≤ 0.30 and 0 ≤ x ≤ 0.26 for calcium and lead, respectively. A regular decreasing of the cell parameter has been observed in the calcium solid solution. The state oxidation +5 of antimony has been put in evidence by the Mössbauer spectrometry of 121Sb. Magnetic susceptibility measurements showed that the effective magnetic moment of copper in these compounds decreases when bismuth is substituted for calcium. To cite this article: M. Sellami et al., C. R. Chimie 9 (2006).