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Crystal structures of 2-bromo-1,1,1,3,3,3-hexa­methyl-2-(tri­methyl­sil­yl)tris­ilane and 2-bromo-1,1,1,3,3,3-hexa­isopropyl-2-(triiso­propyl­sil­yl)tri­silane

The synthesis and crystal structures of two tris­(tri­alkyl­sil­yl)silyl bromide compounds, C(9)H(27)BrSi(4) (I, HypSiBr) and C(27)H(63)BrSi(4) (II, TipSiBr), are described. Compound I was prepared in 85% yield by free-radical bromination of 1,1,1,3,3,3-hexa­methyl-2-(tri­methyl­sil­yl)tris­ilane us...

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Autores principales: Gulotty, Eva M., Staples, Richard J., Biros, Shannon M., Gaspar, Peter P., Rath, Nigam P., Winchester, William R.
Formato: Online Artículo Texto
Lenguaje:English
Publicado: International Union of Crystallography 2018
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6072994/
https://www.ncbi.nlm.nih.gov/pubmed/30116580
http://dx.doi.org/10.1107/S2056989018009696
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author Gulotty, Eva M.
Staples, Richard J.
Biros, Shannon M.
Gaspar, Peter P.
Rath, Nigam P.
Winchester, William R.
author_facet Gulotty, Eva M.
Staples, Richard J.
Biros, Shannon M.
Gaspar, Peter P.
Rath, Nigam P.
Winchester, William R.
author_sort Gulotty, Eva M.
collection PubMed
description The synthesis and crystal structures of two tris­(tri­alkyl­sil­yl)silyl bromide compounds, C(9)H(27)BrSi(4) (I, HypSiBr) and C(27)H(63)BrSi(4) (II, TipSiBr), are described. Compound I was prepared in 85% yield by free-radical bromination of 1,1,1,3,3,3-hexa­methyl-2-(tri­methyl­sil­yl)tris­ilane using bromo­butane and 2,2′-azobis(2-methyl­propio­nitrile) as a radical initiator at 333 K. The mol­ecule possesses threefold rotational symmetry, with the central Si atom and the Br atom being located on the threefold rotation axis. The Si—Br bond distance is 2.2990 (12) Å and the Si—Si bond lengths are 2.3477 (8) Å. The Br—Si—Si bond angles are 104.83 (3)° and the Si—Si—Si bond angles are 113.69 (2)°, reflecting the steric hindrance inherent in the three tri­methyl­silyl groups attached to the central Si atom. Compound II was prepared in 55% yield by free-radical bromination of 1,1,1,3,3,3-hexa­isopropyl-2-(triiso­propyl­sil­yl)tris­ilane using N-bromo­succinimide and 2,2′-azobis(2-methyl­propio­nitrile) as a radical initiator at 353 K. Here the Si—Br bond length is 2.3185 (7) Å and the Si—Si bond lengths range from 2.443 (1) to 2.4628 (9) Å. The Br—Si—Si bond angles range from 98.44 (3) to 103.77 (3)°, indicating steric hindrance between the three triiso­propyl­silyl groups.
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spelling pubmed-60729942018-08-16 Crystal structures of 2-bromo-1,1,1,3,3,3-hexa­methyl-2-(tri­methyl­sil­yl)tris­ilane and 2-bromo-1,1,1,3,3,3-hexa­isopropyl-2-(triiso­propyl­sil­yl)tri­silane Gulotty, Eva M. Staples, Richard J. Biros, Shannon M. Gaspar, Peter P. Rath, Nigam P. Winchester, William R. Acta Crystallogr E Crystallogr Commun Research Communications The synthesis and crystal structures of two tris­(tri­alkyl­sil­yl)silyl bromide compounds, C(9)H(27)BrSi(4) (I, HypSiBr) and C(27)H(63)BrSi(4) (II, TipSiBr), are described. Compound I was prepared in 85% yield by free-radical bromination of 1,1,1,3,3,3-hexa­methyl-2-(tri­methyl­sil­yl)tris­ilane using bromo­butane and 2,2′-azobis(2-methyl­propio­nitrile) as a radical initiator at 333 K. The mol­ecule possesses threefold rotational symmetry, with the central Si atom and the Br atom being located on the threefold rotation axis. The Si—Br bond distance is 2.2990 (12) Å and the Si—Si bond lengths are 2.3477 (8) Å. The Br—Si—Si bond angles are 104.83 (3)° and the Si—Si—Si bond angles are 113.69 (2)°, reflecting the steric hindrance inherent in the three tri­methyl­silyl groups attached to the central Si atom. Compound II was prepared in 55% yield by free-radical bromination of 1,1,1,3,3,3-hexa­isopropyl-2-(triiso­propyl­sil­yl)tris­ilane using N-bromo­succinimide and 2,2′-azobis(2-methyl­propio­nitrile) as a radical initiator at 353 K. Here the Si—Br bond length is 2.3185 (7) Å and the Si—Si bond lengths range from 2.443 (1) to 2.4628 (9) Å. The Br—Si—Si bond angles range from 98.44 (3) to 103.77 (3)°, indicating steric hindrance between the three triiso­propyl­silyl groups. International Union of Crystallography 2018-07-24 /pmc/articles/PMC6072994/ /pubmed/30116580 http://dx.doi.org/10.1107/S2056989018009696 Text en © Gulotty et al. 2018 http://creativecommons.org/licenses/by/2.0/uk/ This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.http://creativecommons.org/licenses/by/2.0/uk/
spellingShingle Research Communications
Gulotty, Eva M.
Staples, Richard J.
Biros, Shannon M.
Gaspar, Peter P.
Rath, Nigam P.
Winchester, William R.
Crystal structures of 2-bromo-1,1,1,3,3,3-hexa­methyl-2-(tri­methyl­sil­yl)tris­ilane and 2-bromo-1,1,1,3,3,3-hexa­isopropyl-2-(triiso­propyl­sil­yl)tri­silane
title Crystal structures of 2-bromo-1,1,1,3,3,3-hexa­methyl-2-(tri­methyl­sil­yl)tris­ilane and 2-bromo-1,1,1,3,3,3-hexa­isopropyl-2-(triiso­propyl­sil­yl)tri­silane
title_full Crystal structures of 2-bromo-1,1,1,3,3,3-hexa­methyl-2-(tri­methyl­sil­yl)tris­ilane and 2-bromo-1,1,1,3,3,3-hexa­isopropyl-2-(triiso­propyl­sil­yl)tri­silane
title_fullStr Crystal structures of 2-bromo-1,1,1,3,3,3-hexa­methyl-2-(tri­methyl­sil­yl)tris­ilane and 2-bromo-1,1,1,3,3,3-hexa­isopropyl-2-(triiso­propyl­sil­yl)tri­silane
title_full_unstemmed Crystal structures of 2-bromo-1,1,1,3,3,3-hexa­methyl-2-(tri­methyl­sil­yl)tris­ilane and 2-bromo-1,1,1,3,3,3-hexa­isopropyl-2-(triiso­propyl­sil­yl)tri­silane
title_short Crystal structures of 2-bromo-1,1,1,3,3,3-hexa­methyl-2-(tri­methyl­sil­yl)tris­ilane and 2-bromo-1,1,1,3,3,3-hexa­isopropyl-2-(triiso­propyl­sil­yl)tri­silane
title_sort crystal structures of 2-bromo-1,1,1,3,3,3-hexa­methyl-2-(tri­methyl­sil­yl)tris­ilane and 2-bromo-1,1,1,3,3,3-hexa­isopropyl-2-(triiso­propyl­sil­yl)tri­silane
topic Research Communications
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6072994/
https://www.ncbi.nlm.nih.gov/pubmed/30116580
http://dx.doi.org/10.1107/S2056989018009696
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