In the latest decade, two-dimensional (2D) p-d conjugated metal organic frameworks (MOFs) constructed from metal ions with square-planar coordination geometry and benzene-or triphenylenederived ligands with ortho-disubstituted N, O, or S donor atoms have received great research interests because of their exceptional physical properties and promising applications. New MOFs of this class are constantly being reported, but 2D metal bis(diselenolene) MOFs based on organic ligands with ortho-disubstituted Se donor atoms have not been synthesized. Herein, a Lewis-acid-induced dealkylation protocol is introduced to the synthesis of arenepolyselenols and related coordination polymers. A triphenylene-derived diselenaborole compound is synthesized and employed as precursor reagent for the synthesis of 2,3,6,7,10,11-triphenylenehexaselenol (H 6 TPHS) and the first conductive metal organic framework namely Co-TPHS based on triphenylenehexaselenolate (TPHS 6À). Co-TPHS exhibits porous honeycomb 2D structure and electrically conductive and glassy magnetic properties.

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Four conjugated polymers are synthesized through indacenodithiohene (IDT) unit copolymerized with thiophene and thiophene derivatives. Indacenodithiohene‐co‐thieno[3,2‐b]thiophene (IDT‐TT) and indacenodithiohene‐co‐trans‐1,2‐di(2‐thienyl)ethylene (IDT‐TVT) exhibit better charge transport mobilities than indacenodithiohene‐co‐thiophene (IDT‐T) and indacenodithiohene‐co‐3,4‐ethoxylene dioxythiophene (IDT‐EDOT), and also display superior thermoelectric properties after doping. Theoretical calculations suggest that IDT‐EDOT and IDT‐TVT have better coplanarities; the inferior performance for IDT‐EDOT might be due to its low molecular weight. Meanwhile, it is worth mentioning that via the synergistic effect of two dopants (CN6CP, CuTFSI), the electrical conductivities of the polymers are further improved. The XPS data shows that the coordination interaction between copper ion and the cyano groups of CN6CP introduces cupric ions into the polymer films, which leads to the increase of the doping ratio.