Double lithiation of 9, 10-dihydroanthracene (DHA) or 6, 13-dihydropentacene (DHP) with n BuLi, followed by the addition of B2 (NMe2) 2Cl2, affords 9, 10-DHA-9, 10-diyl-(1a) or 6, 13- DHP-6, 13-diyl-bridged B2 (NMe2) 2 (1p) in good yields. Upon treatment with Pt (PEt3) 3 in C6H6 at 60° C, both compounds cleanly insert a Pt (PEt3) 2 moiety into their B–B bonds to furnish the corresponding diboryl Pt (II) complexes 2a and 2p. Compound 2a reacts with ...