Diacenaphtho [1, 2-c: 1′, 2′-e]-1, 2-dithiin 2 was synthesized in 23% yield by the reaction of acenaphthylene with elemental sulfur at 120° C. This reaction also afforded either diacenaphtho [1, 2-b: 1′, 2′-d] thiophene 1 or diacenaphtho [1, 2-b: 1′, 2′-e]-dihydro [e]- 1, 4-dithiin 3 depending on the reaction time. Compound 2 was desulfurized and converted to 1 under UV–vis irradiation in a benzene solution. Reaction of 2 with Pt (COD) 2 yielded ...