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Mechanistic studies are performed on the alkane hydroxylation with m‐CPBA (m‐chloroperbenzoic acid) catalyzed by nickel(II) complexes, NiII(L). In the oxidation of cycloalkanes, NiII(TPA) acts as an efficient catalyst with a high yield and a high alcohol selectivity. In the oxidation of adamantane, the tertiary carbon is predominantly oxidized. The reaction rate shows first‐order dependence on [substrate]...