5-p-甲基苯基偶氮基-25,26,27,28-四羟基杯[4]芳烃的合成与晶体结构

Synthesis and crystal structure of 5-mono[(4-methylphenyl)azo]-25,26,27,28-tetrahydroxycalix[4]arene

合成了标题化合物5-p-甲基苯基偶氮基-25,26,27,28-四羟基杯[4]芳烃,它的结构被氢谱、碳谱、电喷雾质谱、元素分析和X-射线单晶衍射所表征.晶体结构分析表明该化合物属于三斜晶系,P-1空间群,晶胞参数为a=10.9773(9),b=18.4860(15),c=18.8587(16),α=60.820(2),β=77.198(2),γ=89.198(2)o,晶胞体积为V=3238.3(5)3,Z=4,Dc=1.187 mg/m3,μ=0.081 mm-1,F(000)=1224,R=0.0927,wR=0.1577,在固态时该化合物以扭曲锥式构象存在.

The title compound 5-mono [（4-methylphenyl） azo]-25, 26, 27, 28-tetrahydroxycalix [4]arene 1 （C35H30N2O6, Mr = 542.6） has been synthesized and its crystal structure was determined by X-ray diffraction analysis. It crystallizes in a triclinic space group P-1, with a=10. 9773（9）, b=18. 4860（15）, c=18. 8587（16） A, α=60. 820（2）, β=77. 198（2）, γ=89. 198（2）°, V=3238.3（5）A^3 , Z=4, Dc=1. 187 mg/m^3 , μ=0. 081 mm^-1, F（000） =1224, the final R=0.0927 and wR=0. 1577 for 13 941 observed reflections with I〉2σ（I）. Crystal structure indicated that the calix[4]arene moiety of 1 exists in a distorted-cone conformation with intramolecular hydrogen bonds.