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Cu oxide clusters deposited on the ZrO2 nodes of NU-1000 by AIM catalyze partial oxidation of methane. The state of the Cu was determined by XAS analysis to contain ∼15% Cu+ and ∼85% Cu2+ under ambient conditions. The average structure of the Cu is square planar coordinated by four O atoms (Cu−O ≈ 1.94 Å) with an additional one or two out-of-plane Jahn−Tellerdistorted O atoms, one of them has Cu−O ≈ 2.33 Å). A Cu− Cu distance of ∼2.93 Å was observed and the coordination number of Cu was determined at 1.3 ± 0.3. A combined EXAFS and DFT study indicates that the cluster that predominates in Cu-NU-1000 is likely to be a trimeric Cu-hydroxide-like structure that bridges two nodes across the c-pore of the MOF.