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Atom‐by‐atom substitution is a promising strategy for designing new cluster‐based materials, which has been used to generate new gold‐ and silver‐containing clusters. Here, the first study focused on atom‐by‐atom substitution of Fe and Ni to the core of a well‐defined cobalt sulfide superatom [Co6S8L6]+ ligated with triethylphosphine (L = PEt3) to produce [Co5MS8L6]+ (M = Fe, Ni) is reported. Electrospray...