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) A†, 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 language | English |
|---|---|
| Pages (from-to) | 795-801 |
| Number of pages | 7 |
| Journal | Organometallics |
| Volume | 13 |
| Issue number | 3 |
| Publication status | Published - 1994 |
| Externally published | Yes |
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ASJC Scopus subject areas
- Inorganic Chemistry
- Organic Chemistry
Cite this
Synthesis and structure of all-trans-1,2,3,4-tetra-tert-butyl-1,2,3,4-tetrachlorocyclotetrasilane. / Kyushin, Soichiro; Kawabata, Motoo; Sakurai, Haruaki; Matsumoto, Hideyuki; Miyake, Michihiro; Sato, Mitsuo; Goto, Midori.
In: Organometallics, Vol. 13, No. 3, 1994, p. 795-801.Research output: Contribution to journal › Article
}
TY - JOUR
T1 - Synthesis and structure of all-trans-1,2,3,4-tetra-tert-butyl-1,2,3,4-tetrachlorocyclotetrasilane
AU - Kyushin, Soichiro
AU - Kawabata, Motoo
AU - Sakurai, Haruaki
AU - Matsumoto, Hideyuki
AU - Miyake, Michihiro
AU - Sato, Mitsuo
AU - Goto, Midori
PY - 1994
Y1 - 1994
N2 - 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) A†, 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.
AB - 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) A†, 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.
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UR - http://www.scopus.com/inward/citedby.url?scp=0001323583&partnerID=8YFLogxK
M3 - Article
AN - SCOPUS:0001323583
VL - 13
SP - 795
EP - 801
JO - Organometallics
JF - Organometallics
SN - 0276-7333
IS - 3
ER -