新型磷杂三环化合物的结构研究

Structural Research for New Phosphadiazine Compounds

用X射线衍射方法测定了6,12-二氧代-1-对氯苯亚胺基-11-乙基-1,4,3-硫氮磷杂环己烷并[3,4-b]-1,3,2-苯并二氮磷杂环己烷(1)和6,12-二氧代-1-N-苄亚胺基-11-乙氧甲酰甲基-1,4,3-硫氮磷杂环己烷并[3,4-b]-1,3,2-苯并二氮磷杂环己烷(2)的晶体结构.1的晶体属P2_(1/n)空间群,α=11.276(1),b=10.109(1),c=15.750(2)A;β=94.37(1)°;Z-4,D_m=1.50,D_c=1.51g/cm^3.对于2569个可观测反射点.最终的R=0.033.2的晶体属Pcab空间群,a=10.596(1),b=19.117(2),c=20.744(2)A;Z=8;D_m=1.39,D_c=1.40g/cm^3.对于1809个可观测反射点,最终的R=0.031.对这两种新型的磷杂三环化合物的构象进行了分析,并指出了影响磷杂环构象的原因.

The crystal structures of 6, 12-dioxo-1-(p-chlorophenyl) imino-11-ethyl-1, 4, 3-thiaazaphospha-cyclohexano [3, 4-b]-1, 3, 2-benzodiazaphosphorin (1) and 6, 12-dioxo-1-N-benzyliene-amino-11-ethoxycarbonylmethyl-1, 4, 3-thiaazaphospha-cyclohexano [3, 4-b]-1, 3, 2-benzodiazaphosphorin (2) have been determined by X-ray diffraction method. The crystals of 1 are monoclinic, space group P2_(1/n), with a=11.276 (1), b=10.109(1), c=15.750(2) A, β==94.37(1)°; Z=4, D_c=1.51g/cm^3. The final R=0.033 for 2569 observed independent reflections. The crystals of 2 are orthorhombic, space group Pcab, with a=10.596(1), b=19.117(2), c=20.744(2) A; Z=8, D_c=1.40g/cm^3. The final R=0.031 for 1809 observed independent reflections. The conformations of these two new phosphadiazine compounds and the factors which influence the conformations were discussed.