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作 者:宁德宽[1] 毕明辉[1] 李光华[1] 刘国宗[1] 施展[1] 冯守华[1]
机构地区:[1]无机合成与制备化学国家重点实验室,吉林大学化学学院,长春130012
出 处:《高等学校化学学报》2009年第5期845-848,共4页Chemical Journal of Chinese Universities
基 金:国家自然科学基金(批准号:20631010,20671040和20601010)资助
摘 要:在溶剂热条件下,以原位反应为基础合成了两个碘化物(C6H8N3)+I3-(1,C6H8N3=2,3-dihydroimi-dazo[1,2-a]pyrimidin-1-ium,2,3-二氢咪唑[1,2-α]-嘧啶鎓阳离子)和[(Cu3I4)(C8H17N2)](2,C8H17N2=N-ethyl-4-aza-1-azonia-bicyclo[2.2.2]octane,N-乙基三乙烯二铵阳离子).用元素分析、粉末X射线衍射及单晶X射线衍射等对化合物进行了表征.结果表明,化合物1属于三斜晶系,P1空间群,a=0.74281(15)nm,b=0.84241(17)nm,c=0.9993(2)nm,α=82.02(3)°,β=83.30(3)°,γ=82.92(3)°,V=0.6114(2)nm3.化合物2属于单斜晶系,P21/c空间群,a=0.68924(14)nm,b=1.0786(2)nm,c=2.2779(5)nm,β=94.84(3)°,V=1.6874(6)nm3.在两个化合物合成中存在两种不同类型的配体原位合成反应,即化合物1的2-氨基嘧啶和乙醇的成环反应与化合物2的三乙烯二胺和乙醇的烷基化反应.Two I-containing compounds, ( C6H8N3 ) ^+ I3^- (1, C6H7 N3 = 2,3-dihydroimidazo [ 1,2-a] pyrimidine-1-ium) and [ ( Cu3I4 ) ( C8H17N2 ) ] (2, C8H17N2 = N-ethyl-1,4-diazabicyclo[2.2.2] octane), were synthesized under solvothermal conditions based on in situ ligand reaction and characterized via elemental analysis, XRD and single crystal X-ray diffraction analysis. Complex 1 crystallizes in the triclinic system, space group P1^- with a =0.74281(15) nm, b =0.84241(17) nm, c =0.9993(2) nm, α =82.02(3)°, β = 83.30 (3) °, γ = 82.92 ( 3 ) °, V = 0. 6114 (2) nm^3. Complex 2 crystallizes in the monoclinic system, space group P21/c with a =0.68924(14) nm, b = 1. 0786(2) nm, c =2. 2779(5) nm, β =94.84(3)°, V = 1. 6874(6) nm^3. Two kinds of in situ ligand reaction were found in the synthesis of these complexes. (C6H8N3 ) ^+ ligand was synthesized from 2-aminopyrimidine and ethanol in complex 1, whereas (C8 H17 N2 )^ + ligand was synthesized from 1,4-diazabicyclo [ 2.2.2 ] octane and ethanol in complex 2.
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