ChemInform Abstract: SYNTHESIS OF TETRAKIS(ALKYLTHIO)TETRATHIAFULVALENES FROM TETRAKIS(BENZOYLTHIO)TETRATHIAFULVALENES

Studies of stannylated-1,2-dithiolato compounds: Synthesis and crystal structure of co-crystalline 4,5-bis[(triphenylstannyl)methylthiolato]-1,2-dithiole-3-thione (Ph3SnCH2)2(dmt) and 5-[(triphenylstannyl)methylthiolato]-4-[(triphenylstannyl)thiolato]-1,2-dithiole-3-thione (Ph3SnCH2)(Ph3Sn)(dmt) [72:28]

“…Thus S(6) indicates relocation of the sulphur atom S(4) when the methylene group [C (6)] is absent. In other words, the structural model now represents a solid solution between 4,5-bis[(triphenylstannyl)-methylthiolato]-1, 2-dithiole-3-thione, the major component (8), and 4-[(triphenylstannyl)thiolato]-5-[(triphenylstannyl)methylthiolato]-1,2-dithiole-3-thione, the minor component (9). The ratio of major to minor components was refined to values of 0.712(15):0.288(15) at 298 K and 0.718(9):0.282(9) at 120 K and are, within error, the same for both sample crystals, i.e., 0.72: 0.28.…”

“…1. A large number of studies of dmit compounds have been reported, a smaller number for dmio compounds [7] and fewer still for the compounds of the unsymmetrical isomer of dmit 2À , 4,5-dithiolato-1,2-dithiole-3-thione, dmt 2À (7), the latter being available on rearrangement of suitable dmit species (e.g., [8,9]). …”

“…As we now report, the compound, obtained after work-up and recrystallisation, was a co-crystalline mixture of 4,5-bis[(triphenylstannyl)methylthiolato]-1,2-dithiole-3-thione (Ph 3 SnCH 2 ) 2 (dmt) (8) and 4-(triphenylstannylmethyl)-thiolato-5-(triphenylstannyl)thiolato-1,2-dithiole-3-thione, (Ph 3 SnCH 2 )(Ph 3 Sn)(dmt) (9). This was particularly intriguing since the same batch of Ph 3 SnCH 2 I had been used in the preparations of 3 and 4 and no formation of a Ph 3 Sn-S compound had been indicated in those syntheses.…”