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Synthesis and crystal structure of 1,3-di-tert-butyl-2-chloro-4,4-diphenyl-1,3,2?3,4-di-aza-phospha-siletidine.


ABSTRACT: The chemical reaction of di-lithium N,N'-di( t but-yl)-Si,Si-di-phenyl-silanedi-amide and PCl3 yielded an off-white solid. Sublimation of the crude product under reduced pressure at elevated temperature gave colourless prismatic crystals of the title compound, C20H28ClN2PSi, which crystallizes in the non-centrosymmetric monoclinic space group Cc. The asymmetric unit of the crystal structure contains one mol-ecule and it is dominated by the central SiN2P 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 nitro-gen 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 PCl3 [2.034?Å; Galy & Enjalbert (1982). J. Solid State Chem. 44, 1-23].

SUBMITTER: Mo D 

PROVIDER: S-EPMC6399688 | biostudies-literature | 2019 Mar

REPOSITORIES: biostudies-literature

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Synthesis and crystal structure of 1,3-di-<i>tert</i>-butyl-2-chloro-4,4-diphenyl-1,3,2λ<sup>3</sup>,4-di-aza-phospha-siletidine.

Mo Dennis D   Frank Walter W  

Acta crystallographica. Section E, Crystallographic communications 20190228 Pt 3


The chemical reaction of di-lithium <i>N</i>,<i>N</i>'-di( <sup><i>t</i></sup> but-yl)-<i>Si</i>,<i>Si</i>-di-phenyl-silanedi-amide and PCl<sub>3</sub> 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<sub>20</sub>H<sub>28</sub>ClN<sub>2</sub>PSi, which crystallizes in the non-centrosymmetric monoclinic space group <i>Cc.</i> The asymmetric unit of the crystal structure contains  ...[more]

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