Rational regulation of electronic structures and functionalities of framework materials still remains challenging. Herein, reaction of 4,4',4''-nitrilo-tribenzhydrazide with tris(μ -4-carboxaldehyde-pyrazolato-N,N')-tricopper (Cu Py ) generates the crystalline copper organic framework USTB-11(Cu). Post-modification with divalent nickel ions affords the heterometallic framework USTB-11(Cu,Ni). Powder X-ray diffraction and theoretical simulations reveal their two-dimensional hexagonal structure geometry. A series of advanced spectroscopic techniques disclose the mixed Cu /Cu state nature of Cu Py in USTB-11(Cu,Ni) with a uniform bistable Cu (Cu Cu ) : Cu (Cu Cu ) (ca. 1 : 3) oxidation state, resulting in a significantly improved formation efficiency of the charge-separation state. This endows the Ni sites with enhanced activity and USTB-11(Cu,Ni) with outstanding photocatalytic CO to CO performance with a conversion rate of 22 130 μmol g h and selectivity of 98 %.
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