摘要
通过2,9-二甲基-1,10-菲啰啉和氰基硼氢化钠的反应,成功制备了2,9-二甲基-1,2,3,4,7,8,9,10-八氢-1,10-菲啰啉(1),并用元素分析、核磁共振、高分辨质谱等方法对所合成的化合物进行了表征,并采用挥发法培养了化合物1的单晶,并利用X-射线单晶衍射技术测定和研究了化合物1的晶体结构。在化合物1中,2,9-二甲基-1,2,3,4,7,8,9,10-八氢-1,10-菲啰啉分子采取受限扭曲的椅式构象,分子之间以交错平行模式堆积,并通过弱的C-H…π作用相互连接成为一维超分子链。晶体结构数据:三斜晶系,空间群P-1,a=9.052(9),b=10.241(9),c=14.809(12),α=71.07(5),β=79.79(3),γ=77.22(4),Z=1,V=1258(2)3。
The 2,9-dimethyl-1,2,3,4,7,8,9,10-octahydro-1,10-phenanthroline( 1) was successfully synthesized by the reaction of 2,9-dimethyl-1,10-phenanthroline and sodium cyanoborohydride,and characterized by elemental analysis,nuclear magnetic resonance and high resolution mass spectrum. The single crystals of compound 1 were growth by volatilization method and characterized by X ray single crystal diffraction. In compound 1,the 2,9-dimethyl-1,2,3,4,7,8,9,10-octahydro-1,10-phenanthroline molecule adopted a twisted chair conformation. The adjacent molecules pack with cross-stacking mode,and connect each other with weak C-H…π interaction,forming 1D supramolecule chain. Crystal data were triclinic,space group P-1,a = 9. 052( 9),b = 10. 241( 9) ,c = 14. 809( 12),α = 71. 07( 5),β = 79. 79( 3) ,γ = 77. 22( 4) ,Z = 1,and V = 1258( 2)3.
引文
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