The sequential reaction of selected polycyclic aromatic hydrocarbons with butyllithium/TMEDA/ hexane and sulfur allows preparation of ring-fused dithiins, dithioles, and thiophenes. In this manner, phenanthrene has been converted to phenanthro[4,5-~de][1,2]dithiin and phenanthro[l,IOc~-1,2dithiole. Yellow crystals of the dithiin form inoC2/c (#15) space group .with < = 4, a = 13.537(3) A, b = 8...