Veinot Alex J, Hendsbee Arthur 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 Apr 21;73(Pt 5):735-737. doi: 10.1107/S2056989017005825. eCollection 2017 May 1.
The title compound, CHClNOP, was synthesized by reacting phosphoryl chloride with ,'-bis-(2,6-diiso-propyl-phen-yl)ethane-1,2-di-amine in the presence of -methyl-morpholine which acted as an auxilliary base to quench the HCl released as a by-product. The resultant -heterocyclic phosphine five-membered ring adopts a half-chair conformation and features a tetra-coordinate P atom ligated by the chelating di-amine [P-N = 1.6348 (14) and 1.6192 (14) Å], one double-bonded O atom [P1-O1 = 1.4652 (12) Å] and one Cl atom [P1-Cl1 = 2.0592 (7) Å]. The sterically hindered 2,6-diiso-propyl-phenyl (Dipp) groups twist away from the central heterocycle, with torsion angles of -75.66 (19) and 83.39 (19)° for the P-N-C-C links. A number of intra-molecular C-H⋯N, C-H⋯O and C-H⋯Cl close contacts occur. In the crystal, mol-ecules are linked by C-H⋯O hydrogen bonds to generate [010] chains. C-H⋯π inter-actions are also observed.
标题化合物CHClNOP是通过使磷酰氯与1,2-双（2,6-二异丙基苯基）乙烷-1,2-二胺在作为辅助碱以淬灭作为副产物释放的HCl的N-甲基吗啉存在下反应而合成的。所得的含磷杂环五元环呈半椅构象，其特征是一个四配位的P原子，由螯合二胺[P-N = 1.6348 (14) 和1.6192 (14) Å]、一个双键连接的O原子[P1-O1 = 1.4652 (12) Å]和一个Cl原子[P1-Cl1 = 2.0592 (7) Å]配位。空间位阻较大的2,6-二异丙基苯基（Dipp）基团扭转远离中心杂环，P-N-C-C连接的扭转角为-75.66 (19) 和83.39 (19)°。存在许多分子内C-H⋯N、C-H⋯O和C-H⋯Cl紧密接触。在晶体中，分子通过C-H⋯O氢键连接形成[010]链。还观察到C-H⋯π相互作用。
