Synthesis and Structure of all-trans-1,2,3,4-Tetra-tert-butyl-1,2,3,4-tetrachlorocyclotetrasilane

Soichiro Kyushin, Motoo Kawabata, Haruaki Sakurai, Hideyuki Matsumoto, Michihiro Miyake, Mitsuo Sato, Midori Goto

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Abstract

The synthesis of all-trans-[(t-Bu)ClSi]4 (1) via chlorodephenylation of [(t-Bu)PhSi]4 with HCl/AlCl3 is described. Three isomers of [(t-Bu)PhSi]4 (cis-cis-trans-2, cis-trans-cis-2, and all-trans-2) were separated, and each of them was subjected to chlorodephenylation. The X-ray structures are reported for cis-cis-trans-2 and cis-trans-cis-2. Crystal data for cis-cis-trans-2: monoclinic, P21/c, a = 20.924(10) Å, b = 10.813(5) Å, c = 19.443(11) Å, β = 117.57(3)°, V = 3900(3) Å3, Z = 4, R = 0.047, Rw = 0.047 for 2572 reflections. Crystal data for cis-trans-cis-2: monoclinic, P21/n, a = 15.407(4) Å, b = 23.798(6) Å, c = 10.852(2) Å, β = 94.93(2)°, V = 3964(2) Å3, Z = 4, R = 0.043, Rw = 0.046 for 2905 reflections. The chlorodephenylation of cis-cis-trans-2, cis-trans-cis-2, and all-trans-2 gave 1 exclusively. The structure of 1 was established by X-ray crystallography. Crystal data for 1: orthorhombic, Pca21, a = 14.848(2) Å, b = 13.719(1) Å, c = 13.074(4) Å, V = 2663(1) Å3, Z = 4, R = 0.052, Rw = 0.077 for 1992 reflections. 1 has a folded structure, the dihedral angle being 26.6°, which accommodates the chlorine atoms in pseudoaxial positions and the tert-butyl groups in less hindered pseudoequatorial positions. The principal average bond distances are Si-Si 2.375 Å, Si-C 1.905 Å, and Si-Cl 2.086 Å. The Si-Cl bond distances are somewhat longer than usual.

Original languageEnglish
Pages (from-to)795-801
Number of pages7
JournalOrganometallics
Volume13
Issue number3
DOIs
Publication statusPublished - Mar 1 1994

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Organic Chemistry
  • Inorganic Chemistry

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    Kyushin, S., Kawabata, M., Sakurai, H., Matsumoto, H., Miyake, M., Sato, M., & Goto, M. (1994). Synthesis and Structure of all-trans-1,2,3,4-Tetra-tert-butyl-1,2,3,4-tetrachlorocyclotetrasilane. Organometallics, 13(3), 795-801. https://doi.org/10.1021/om00015a012