||New double perovskites LaPbMSbO6, where M2+ = Mn2+, Co2+, and Ni2+, were synthesized as polycrystals by an aqueous synthetic route at temperatures below 1000 Â°C. All samples are monoclinic, space group P21/n, as it is observed from Rietveld analysis of X-ray powder diffraction patterns. The distribution of M2+ and Sb5+ among the two octahedral sites have 3% of disorder for M2+ = Ni2+, whereas for M2+ = Mn2+ and Co2+ less disorder is found. The three samples have an antiferromagnetic transition, due to the antiferromagnetic coupling between M2 + through super-superexchange paths M2+-O2--Sb5+-O2--M2+. Transition temperatures are low: 8, 10 and 17 K for Mn2+, Co2+, and Ni2 + respectively, as a consequence of the relatively long distances between the magnetic ions M2+. Besides, for LaPbMnSbO6 a small transition at 45 K was found, with ferrimagnetic characteristics, possibly as a consequence of a small disorder between Mn2+ and Sb5+. This disorder would give additional and shorter interaction paths: superexchange Mn2+-O2--Mn2+.