两种不同构型的吡唑啉酮衍生物的合成与结构

报道了PMBP-PCH(PCH为2-吡啶甲酰肼)和PMBP-INTH(INTH为异烟酰肼)2种化合物的合成与晶体结构分析,PMBP-PCH属三斜晶系,具有P空间群,a=7.783(2),b=10.993(3),c=12.621(3)?=92.96(2),=103.87(2),g=101.54(2),V=1021.5(5)3,Z=2,Dc=1.307g/cm3,m(MoK?=0.088mm-1,F(000)=421,R=0.0436,wR=0.0937.晶体结构表明,在此分子内形成了一个大的共轭体系,由于分子间氢键力的作用,使它们在晶体中以二聚体的形式存在.PMBP-INTH晶体属单斜晶系,具有P21/c空间群,a=14.083(4),b=13.865(3),c=10.609(2)?=101.66(2)o,V=2028.8(8)3,Z=4,Dc=1.301g/cm3,m(MoK?=0.087mm-1,F(000)=832,R=0.0473,wR=0.0898.此化合物在O(1)原子与邻近分子的N(1)原子之间存在较强的氢键,在结晶的过程中,通过分子间质子迁移,使该化合物形成了1个以N(2)为负电荷中心,N(1)为正电荷中心的两性离子结构,且分子通过此氢键形成了一维链状结构,并沿b轴呈层状堆积.

Syntheses and Crystal Structures of Derivants of Pyrazolone with Two Different Configurations

PMBP-PCH and PMBP-INTH have been synthesized and their crystal structures were determined by X-ray single-crystal diffraction. The crystal structure of PMBP-PCH belongs to triclinic, space group P with a = 7.783(2), b = 10.993(3), c = 12.621(3) ? a = 92.96(2), b=103.87(2), g = 101.54(2), V = 1021.5(5) 3, Z = 2, Dc = 1.307 g/cm3 , m(MoKa) = 0.088 mm-1, F(000)= 421, R = 0.0436 and wR = 0.0937. The dimer was formed through intermolecular hydrogen bonds. The crystal structure of PMBP-INTH is of monoclinic, space group P21/c with a = 14.083(4), b = 13.865(3), c = 10.609(2) , b=101.66(2), V = 2028.8(8) 3 , Z = 4, Dc = 1.301 g/cm3, m(MoKa)= 0.087 mm-1, F(000)=832, R = 0.0473 and wR = 0.0898. The intermolecular proton transfer leads to the formation of zwitterionic structure (PMBP-INTH), in which the N(2) and N(1) atoms are the centers of negative and positive charges, respectively.