A Covalent Organic Nanoribbon: Preparation, Single‐Crystal Structure with Chinese Luban Lock Configuration, and Photocatalytic Behavior

The multiple mortise‐and‐tenon joint parts are the core factors to provide the structural stability and diversity of Chinese Luban locks; however, constructing such structures is very challenging. Herein, single crystals of a covalent organic nanoribbon (named CityU‐27) are prepared through the assembly of hexahydroxytriphenylene (HHTP), 4,4′‐vinylenedipyridine (BYE), and phenylboronic acid (BA) together through dative boron←nitrogen (B←N) bonds. The single‐crystal X‐ray diffraction analysis indicates that CityU‐27 has a covalent organic nanoribbon structure, where each nanoribbon forms multiple and tight π–π interactions with four neighboring others to generate a Luban lock‐like configuration. CityU‐27 has been demonstrated to be an efficient photocatalyst in a one‐pot tandem reaction of hydrogen evolution reaction (HER) and semi‐hydrogenation reaction of alkynes in series to produce olefins without any additional photosensitizers and co‐catalysts (metal‐free). The single‐crystal structure of a covalent organic nanoribbon (named CityU‐27) with a width of ca. 6 nm has been shown to exhibit a multiple “mortise‐and‐tenon” like joint 3D network similar to the Chinese traditional Luban lock configuration. CityU‐27 has been demonstrated to be an efficient photocatalyst in the metal‐free one‐pot tandem hydrogen evolution reaction and semi‐hydrogenation reaction of diphenylacetylene derivatives.