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We demonstrate, for the first time, that state‐specific x‐ray photoelectron diffraction can be used to determine the structural environment of reacted substrate atoms at a metal/semiconductor interface. Such measurements reveal that extensive reactivity at the Ni/GaAs(001) interface is followed by epitaxial regrowth of a CsCl phase in which Ni atoms occupy one sublattice and disrupted Ga and As atoms occupy the other sublattice.