Veinot Alex J, Blair Amber D, Masuda Jason D
Department of Chemistry, Saint Mary's University, 923 Robie St., Halifax, Nova Scotia, B3H 3C3, Canada.
Acta Crystallogr E Crystallogr Commun. 2017 May 31;73(Pt 6):905-907. doi: 10.1107/S2056989017007642. eCollection 2017 Jun 1.
The title compound, CHNP, was synthesized by reacting 2-chloro-1,3-bis-(2,6-diiso-propyl-phen-yl)-1,3,2-di-aza-phospho-lidine with sodium azide and a catalytic amount of lithium chloride in tetra-hydro-furan. The title compound is the first structurally characterized 2-azido-1,3,2-di-aza-phospho-lidine and exhibits a P atom in a trigonal pyramidal geometry. The azide P-N bond length of 1.8547 (16) Å is significantly longer than the P-N separations for the chelating di-amine [P-N = 1.6680 (15) and 1.6684 (14) Å]. The sterically hindered 2,6-diiso-propyl-phenyl groups twist away from the central heterocycle, with dihedral angles between the central heteocyclic ring and benzene rings of 76.17 (10) and 79.74 (9)°. In the crystal, a weak C-H⋯N link to the terminal N atom of the azide group leads to [100] chains.
标题化合物CHNP是通过使2-氯-1,3-双（2,6-二异丙基苯基）-1,3,2-二氮杂磷杂环戊烷与叠氮化钠和催化量的氯化锂在四氢呋喃中反应合成的。该标题化合物是首个经结构表征的2-叠氮基-1,3,2-二氮杂磷杂环戊烷，其磷原子呈三角锥几何构型。叠氮基的磷-氮键长为1.8547 (16) Å，明显长于螯合二胺的磷-氮间距[P-N = 1.6680 (15)和1.6684 (14) Å]。空间位阻较大的2,6-二异丙基苯基基团从中心杂环扭转开，中心杂环与苯环之间的二面角为76.17 (10)和79.74 (9)°。在晶体中，与叠氮基团末端氮原子的弱C-H⋯N连接导致形成[100]链。
