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Yet directing O\n                    <jats:sub>2<\/jats:sub>\n                    activation toward an energy\u2010transfer (ET) pathway producing mild singlet oxygen (\n                    <jats:sup>1<\/jats:sup>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    ), rather than a charge\u2010transfer (CT) pathway generating radicals, remains difficult because the catalysts must favor triplet\u2010energy transfer to O\n                    <jats:sub>2<\/jats:sub>\n                    while avoiding electron transfer. We show that ultrasmall amorphous FeO\n                    <jats:sub>x<\/jats:sub>\n                    supported on porous carbon nitride (PCN) redirects O\n                    <jats:sub>2<\/jats:sub>\n                    photoactivation from a mixed CT\/ET process to a predominantly ET pathway. Compared with the crystalline counterpart, trace ultrasmall amorphous FeO\n                    <jats:sub>x<\/jats:sub>\n                    (\u223c3.8\u00a0nm, 0.29 wt% Fe) localizes photoexcitation in a triplet\u2010favored excited state by increasing exciton binding energy (45.69 meV) and accelerating intersystem crossing (\n                    <jats:italic>\u03c4<\/jats:italic>\n                    <jats:sub>1<\/jats:sub>\n                    = 19.88\u00a0ps). It also promotes O\n                    <jats:sub>2<\/jats:sub>\n                    capture and suppresses electron transfer owing to weak interfacial coupling. This dual regulation shifts reactive oxygen species generation from mixed \u2022O\n                    <jats:sub>2<\/jats:sub>\n                    <jats:sup>\u2212<\/jats:sup>\n                    \/\n                    <jats:sup>1<\/jats:sup>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    to predominantly\n                    <jats:sup>1<\/jats:sup>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    , achieving a\n                    <jats:sup>1<\/jats:sup>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    yield of 982.2\u00a0\u00b5mol L\n                    <jats:sup>\u22121<\/jats:sup>\n                    , 2.5 times that of crystalline FeO\n                    <jats:sub>x<\/jats:sub>\n                    . Such a\n                    <jats:sup>1<\/jats:sup>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    \u2010mediated pathway enables selective photooxidation of 5\u2010hydroxymethylfurfural (HMF) to 2,5\u2010furandicarboxylic acid (FDCA) under ambient air, delivering 92.1% FDCA selectivity and a formation rate of 461\u00a0\u00b5mol g\n                    <jats:sup>\u22121<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    despite ultralow Fe loading, identifying ultrasmall amorphous oxides as atom\u2010efficient sites for route\u2010selective O\n                    <jats:sub>2<\/jats:sub>\n                    activation for advanced aerobic photocatalysis.\n                  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