Schiff碱水杨醛缩异烟肼和水杨醛缩4-氨基安替吡啉的合成和晶体结构

Syntheses and Crystal Structures of Schiff Base N-Isonicotinamidosalicylaidimine and 4-Salicylaldehydylaminoantipyrine

通过水杨醛和异烟肼,4-氨基安替吡啉的缩合反应分别合成了Schiff 碱水杨醛缩异烟肼1,水杨醛缩4-氨基安替吡啉2,并获得其单晶结构。用元素分析,UV-Vis和IR谱进行表征。晶体结构通过X-射线衍射法测定,晶体结构均用直接法解出, 经全矩阵最小二乘法对原子参数进行修正。化合物1:化学计量式为:C13H11N3O2,Mr = 241.25,晶体属于单斜晶系,空间群P21/n, 晶胞参数:a = 8.153(1),b = 15.574(4) , c = 9.554(2) ? b =105.48(1)? V =1169.1(4) ? , Z = 4, Dc =1.371 g/cm3 , m =0.096 mm-1, F(000) = 504,结构偏离因子R = 0.0832, wR = 0.1158,共收集到2384个独立衍射点,其中其I >2(I)的可观测点为2059个。化合物2:化学计量分子式为:C18H17N3O2,Mr = 307.35,晶体属于单斜晶系,空间群P21/n, 晶胞参数: a = 7.597(1),b = 7.500(1) , c = 27.266(5) , b = 95.31(1), V = 1546.7(4) ? , Z = 4, Dc = 1.320 g/cm3 , m = 0.088 mm-1, F(000) = 648,结构偏离因子R = 0.0413, wR = 0.0952,共收集到3282个独立衍射点,其中其I >2(I)的可观测点为2711个。X-射线分析显示化合物1和2的晶体结构均由分子间氢键和-弱相互作用堆积而成的二维层状结构。

The Schiff base N-isonicotinamidosalicylaidimine 1 and 4-salicylaldehydylaminoantipyrine 2 were synthesized by the reaction of salicylaldehyde with isonicotinyl hydrazide and 4-aminoantipyrine, respectively. Their crystal structures were determined by single-crystal X-ray diffraction method and characterized by elemental analysis, UV-Vis and IR spectra. Compound 1: monoclinic, space group P2(1)/n with cell parameters: a = 8.153(1), b = 15.574(4), c = 9.554(2) Angstrom, beta = 105.48(1)degrees, V= 1169.1(4) Angstrom(3), Z= 4, C13H11N3O2, M-r = 241.25, D-c = 1.371g/cm(3), mu = 0.096 mm(-1), F(000) = 504, the final R = 0.0832 and wR = 0.115. 2384 independent reflections were collected and 2059 (I >2sigma (I)) can be observed. Compound 2: monoclinic, space group P2(1)/n with cell parameters: a = 7.597(1), b = 7.500(1), c = 27.266(5) Angstrom, beta = 95.31(1)degrees, V= 1546.7(4) Angstrom(3), Z= 4, C18H17N3O2, M-r = 307.35, D-c = 1.320 g/cm(3), mu = 0.088 mm(-1), F(000) = 648, the final R = 0.0413 and wR = 0.0952. 3282 independent reflections were collected and 2711 (I >2sigma (1)) can be observed. The structure was solved by direct methods and refined by full-matrix least-squares techniques. The X-ray analysis reveals that the crystal structures of compounds 1 and 2 are two-dimensional layer structures through intramolecular hydrogen bonding and pi -pi stacking.