Two successive single crystal phase transitions involving the coordination sphere of antimony in PhSb(dmit), the first organo-antimony(III) dithiolene complex.

摘要: PhSb(dmit) (dmit2-, 4,5-dithiolato-1,3-dithiole-2-thione), the first neutral organo-antimony dithiolene complex, has been synthesized by addition of PhSbCl2 on a suspension Na2(dmit). The complex was characterized spectroscopic (1H and 13C NMR IR) methods elemental analysis. Its crystal structure determined X-ray diffraction at room temperature in monoclinic P21/c space group, with = 12.580(3), b 8.9756(18), c 15.905(3) A, β 109.06(3)°, V 1697.5(6) A3, Z 4. A coordinating THF molecule found coordination geometry around antimony atom is distorted pseudopentagonal bipyramid type, if taking into account Sb···O secondary Sb···S interactions, as well stereochemically active 5s2 lone pair. intermolecular S···S contacts, shorter than sum van der Waals radii corresponding atoms, lead to formation three-dimensional polymeric network solid state. second experiment, per...