1,3,2-氧氮磷杂环戊烷衍生物晶体结构研究

Crystal Structures of 1,3,2-Oxazaphospholidine Derivatives

用X射线衍射方法测定了两个1,3,2-氧氮磷杂环戊烷衍生物的晶体结构:2-二乙氨基-3-(4′-甲基苯甲酰基)-2-硫代-1,3,2-氧氮磷杂环戊烷,C_(14)H_(21)N_2O_2PS(1),空间群为P_(bco),α=0.9057(5)nm,b=1.3974(6)nm,c=2.5130(7)nm,Z=8,R=0.051;2-二乙氨基-3-(2′,4′-二氯苯甲酰基)-2-硫代-1,3,2-氧氮磷杂环戊烷,C_(13)H_(17)N_2O_2PSCl_2(2),空间群P2_1/c,α=0.7375(1)nm,b=1.4370(3)nm,c=1.6015(7)nm,β=93.70(2)°,Z=4,R=0.054。结构均由直接法解出。两个化合物中氧氮磷杂五元环均为半椅式构象。其中P—N键长环内分别为0.1712(2)nm和0.1723(0)nn;环外为0.1620(3)nm和0.1620(0)nm,由于成环作用所致环内P—N键长大于环外的。

The crystal and molecular structures of 2-diethylamino-3-(4'-methylbenzoyl)-2-thione-l, 3, 2-oxazaphospholidine (1) and 2-diethylamino- 3- ( 2', 4' -dichlorobenzoyl) - 2-thione-1,3, 2-oxaza-phospholidine(2) were determined by X-ray diffraction method. The diffraction data were collected on a CAD4 single crystal diffractometer. The crystallographic data are as follows; (1) C14H21N2O2PS, orthorhombic, space group Pbca α=0. 9057(5) nm, 6=1.3974(6) nm, c=2. 5130(7) nm, Z = 8, V = 3. 1806 nm3, R=0. 051. (2) C13H17N2O2PSCl2, monoclinic, space group P21/c, α=0. 7375(1) nm, 6=1. 4370(3) nm, c=l. 6015(7) nm, β=93. 70(2)°/, Z=4, V=1. 6895 nm3, R=0. 054. The structures of the two compounds were solved by the direct method. The five-membered oxaza-phospholidine ring has a half chair conformation in both of the molecules.