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Synthesis and crystal structure of 1,3-di-tert-butyl-2-chloro-4,4-diphenyl-1,3,2λ(3),4-di­aza­phospha­siletidine

The chemical reaction of di­lithium N,N′-di((t)but­yl)-Si,Si-di­phenyl­silanedi­amide and PCl(3) yielded an off-white solid. Sublimation of the crude product under reduced pressure at elevated temperature gave colourless prismatic crystals of the title compound, C(20)H(28)ClN(2)PSi, which crystalliz...

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Autores principales: Mo, Dennis, Frank, Walter
Formato: Online Artículo Texto
Lenguaje:English
Publicado: International Union of Crystallography 2019
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6399688/
https://www.ncbi.nlm.nih.gov/pubmed/30867959
http://dx.doi.org/10.1107/S2056989019002627
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author Mo, Dennis
Frank, Walter
author_facet Mo, Dennis
Frank, Walter
author_sort Mo, Dennis
collection PubMed
description The chemical reaction of di­lithium N,N′-di((t)but­yl)-Si,Si-di­phenyl­silanedi­amide and PCl(3) yielded an off-white solid. Sublimation of the crude product under reduced pressure at elevated temperature gave colourless prismatic crystals of the title compound, C(20)H(28)ClN(2)PSi, which crystallizes in the non-centrosymmetric monoclinic space group Cc. The asymmetric unit of the crystal structure contains one mol­ecule and it is dominated by the central SiN(2)P four-membered ring, which is almost planar with a mean deviation of the atoms from the best plane of 0.014 Å. The angles between the plane defined by the silicon atom and the two nitro­gen atoms and the best planes of the Si-phenyl groups are 85.1 (2) and 77.4 (2)°, with the tilt of the phenyl rings in the opposite direction. Both tert-butyl groups suffer from a two-position rotational disorder with site occupancies of 0.752 (6)/0.248 (6) and 0.878 (9)/0.122 (9). The P—Cl bond [2.2078 (17) Å] is remarkably elongated compared to the P—Cl distance in PCl(3) [2.034 Å; Galy & Enjalbert (1982). J. Solid State Chem. 44, 1–23].
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spelling pubmed-63996882019-03-13 Synthesis and crystal structure of 1,3-di-tert-butyl-2-chloro-4,4-diphenyl-1,3,2λ(3),4-di­aza­phospha­siletidine Mo, Dennis Frank, Walter Acta Crystallogr E Crystallogr Commun Research Communications The chemical reaction of di­lithium N,N′-di((t)but­yl)-Si,Si-di­phenyl­silanedi­amide and PCl(3) yielded an off-white solid. Sublimation of the crude product under reduced pressure at elevated temperature gave colourless prismatic crystals of the title compound, C(20)H(28)ClN(2)PSi, which crystallizes in the non-centrosymmetric monoclinic space group Cc. The asymmetric unit of the crystal structure contains one mol­ecule and it is dominated by the central SiN(2)P four-membered ring, which is almost planar with a mean deviation of the atoms from the best plane of 0.014 Å. The angles between the plane defined by the silicon atom and the two nitro­gen atoms and the best planes of the Si-phenyl groups are 85.1 (2) and 77.4 (2)°, with the tilt of the phenyl rings in the opposite direction. Both tert-butyl groups suffer from a two-position rotational disorder with site occupancies of 0.752 (6)/0.248 (6) and 0.878 (9)/0.122 (9). The P—Cl bond [2.2078 (17) Å] is remarkably elongated compared to the P—Cl distance in PCl(3) [2.034 Å; Galy & Enjalbert (1982). J. Solid State Chem. 44, 1–23]. International Union of Crystallography 2019-02-28 /pmc/articles/PMC6399688/ /pubmed/30867959 http://dx.doi.org/10.1107/S2056989019002627 Text en © Mo and Frank 2019 http://creativecommons.org/licenses/by/4.0/ 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/4.0/
spellingShingle Research Communications
Mo, Dennis
Frank, Walter
Synthesis and crystal structure of 1,3-di-tert-butyl-2-chloro-4,4-diphenyl-1,3,2λ(3),4-di­aza­phospha­siletidine
title Synthesis and crystal structure of 1,3-di-tert-butyl-2-chloro-4,4-diphenyl-1,3,2λ(3),4-di­aza­phospha­siletidine
title_full Synthesis and crystal structure of 1,3-di-tert-butyl-2-chloro-4,4-diphenyl-1,3,2λ(3),4-di­aza­phospha­siletidine
title_fullStr Synthesis and crystal structure of 1,3-di-tert-butyl-2-chloro-4,4-diphenyl-1,3,2λ(3),4-di­aza­phospha­siletidine
title_full_unstemmed Synthesis and crystal structure of 1,3-di-tert-butyl-2-chloro-4,4-diphenyl-1,3,2λ(3),4-di­aza­phospha­siletidine
title_short Synthesis and crystal structure of 1,3-di-tert-butyl-2-chloro-4,4-diphenyl-1,3,2λ(3),4-di­aza­phospha­siletidine
title_sort synthesis and crystal structure of 1,3-di-tert-butyl-2-chloro-4,4-diphenyl-1,3,2λ(3),4-di­aza­phospha­siletidine
topic Research Communications
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6399688/
https://www.ncbi.nlm.nih.gov/pubmed/30867959
http://dx.doi.org/10.1107/S2056989019002627
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