LSb(μ-I)2(μ-S)SbL. A neutral triply bridged complex obtained from Sb powder and diiodine activated by tetraphenyldithioimidodiphosphine (HL)

The synthesis of the complex LSb(μ-I)2(μ-S)SbL (I) was accomplished by reacting Sb powder with I2 activated by tetraphenyldithioimidodiphosphine (SPPh2NHPPh2S) (HL). X-ray diffraction (tetragonal, M = 1426.30, space group I41/a (No. 88), Z = 8, a = 18.020(2), c = 33.037(4) Å, V = 10,728(2) Å3, ρc = 1.766 g/cm3, μ(MoKα) = 25.07 cm-1, R1 = 0.0593, wR2 = 0.2065) shows that I is a dinuclear Sb(III) complex, in which the 2 metal ions are bridged by 1 sulfide and 2 iodide anions. An anionic bidentate L ligand completes the coordination sphere of each metal with its 2 S atoms, leading to a slightly distorted pyramidal coordination geometry, since each metal ion shows the presence of a sterically active lone-pair in trans position to the bridging sulfide. 31P CP-MAS NMR and IR spectroscopies are in accordance with the structural features of the complex.