摘要

The tetraiodotetrasilane (tBu(3)Si)SiI2SiI2(SitBu(3)) can be prepared from precursor (tBu(3)Si)SiH2SiH2(SitBu(3)). When (tBu(3)Si)SiH2SiH2(SitBu(3)) was treated with an excess of iodine at 120 degrees C, (tBu(3)Si)SiI2SiI2(SitBu(3)) was formed. X-ray quality crystals of (tBu(3)Si)SiI2SiI2(SitBu(3)) were grown from benzene at ambient temperature. The tetraiodotetrasilane (tBu(3)Si)SiI2SiI2(SitBu(3)) crystallizes in the monoclinic space group C2/c, a = 10.0110(10) angstrom, b = 13.9130(10) angstrom, c = 25.422(2) angstrom, beta = 99.072(4)degrees, V = 3496.6(5) angstrom(3), Z = 4, d(calcd) = 1.829 g cm(3); R-1 = 0.0844, wR(2) = 0.1854 for 3,017 reflections with I > 2 sigma(I). X-ray-crystallographic data show that the bromo and iodo derivatives (tBu(3)Si)SiX2SiX2(SitBu(3)) (X = Br, I) are isomorphous. The solid-state structure of (tBu(3)Si)SiI2SiI2(SitBu(3)) as well as those of (tBu(3)Si)SiX2SiX2(SitBu(3)) (X = Cl, Br) reveals a staggered conformation which adopts a trans-orientation of the supersilyl substituent. Unequal dihedral angles as found in (tBu(3)Si)SiX2SiX2(SitBu(3)) (X = Cl, Br, I) indicate that these compounds are sterically overcrowded.

  • 出版日期2011-2