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The design for non-Cu-based catalysts with the function of producing C 2 + products requires systematic knowledge of the intrinsic connection between the surface state as well as the catalytic activity and selectivity. In this work, photochemical in situ spectral surface characterization techniques combined with the first principle calculations (DFT) were applied to investigate the relationships between the composition of surface states, coordinated motifs, and catalytic selectivity of a titanium oxynitride catalyst. When the catalyst mediates CO 2 photoreduction, C 2 product selectivity is positively correlated with the surface Ti 2 + /Ti 3 + ratio and the surface oxidation state is regulated and controlled by coordinated motifs of NÀ Ti-O/V [O], which can reduce the potential dimerization energy barriers of *COÀ CO* and promote spontaneous formation of the subsequent *COÀ CH 2 * intermediate. This phenomenon provides a new perspective for the design of heterogeneous catalysts for photoreduction of CO 2 into useful products.

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