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The local atomic environment of the Sb dopant in 2 and 5×1016 ions/cm2 implanted Si samples has been studied by near grazing incidence fluorescence extended x‐ray absorption fine structure at different stages of the Sb deactivation process. The annealings were performed at high temperature (900–1000 °C) during various periods: 30 s–4 h. The Sb out‐diffusion and the high percentage of Sb precipitates are put into evidence especially for Sb‐only implanted samples. The comparison of the Sb and B codiffusion data with the corresponding ones obtained by the diffusion of Sb alone revealed several anomalous effects due to dopant interaction. Moreover, a simulation program including dopant precipitation and donor–acceptor pairing allows us to foresee most of the anomalous phenomena occurring in high‐concentration codiffusion experiments. © 1996 American Institute of Physics.