Abstract
Reaction of FeCl 2 · 4H 2O with o-benzenedithiolate and AsPh 4 + gives the paramagnetic (μ eff 3.55 BM, 295 K) compound (AsPh 4) 2[Fe(S 2C 6H 4) 2], whose structure consists of discrete tetrahedral AsPh 4 + cations and mononuclear planar [Fe(S 2C 6H 4) 2− anions forming a distorted antifluorite lattice. From the reaction mixture of FeCl 2 · 4H 2O, o-benzenedithiolate and an excess of PMe 3, the 16e diamagnetic [Fe(S 2C 6H 4)(PMe 3) 3] could be isolated, which, in contrast to original expectations, contains pentacoordinate iron in a distorted square-pyramidal ligand sphere. [Fe(S 2C 6H 4)(PMe 3) 3] looses PMe 3 on reaction with CO and yields [Fe(S 2C 6H 6)(PMe 3) 2(CO) 2]; applying equivalent amounts of CO the binuclear complex [Fe(S 2C 6H 4)(PMe 3) 2CO] 2 is formed.
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