Synthesis and crystal and molecular structure of μ-oxo-bis[trifluoroacetato(p-tolyl)iodine

Abstract

Crystal and molecular structure of μ-oxo-bis[trifluoroacetato(p-tolyl)iodine] (I) synthesized by a new procedure was determined by X-ray diffraction analysis. Crystals I are orthorhombic, unstable, space group Pbcn, a=17.684(3), b=8.453(3), c=30.560(4) A, Z=8. The structure of I was solved by direct and Fourier methods and refined by the full-matrix least-squares procedure in an anisotropic-isotropic approximation to R=0.098 (CAD-4 automatic diffractometer, λCuKα, 1200 observed reflections with I≥2σ). In molecule I, two iodine atoms have T-configuration of valence bonds with the average bond angles O−I−O 169(1) and O−I−C 86(2)°, average bond lengths I−Oμ 2.009(9), I−Oacet 2.269(9), and I−Caryl 2.11(1) A, and the bond angle I−O−I 118.1(5)°. In molecule I, two p-Tol substituents are directed to approximately the same side of the medium plane of the central O−I−O−I−O fragment. Crystal structure I has I...O type intra-and intermolecular nonvalent interactions (secondary bonds).