(C6H8N3)^＋I3^-和[(Cu3I4)(C8H17N2)]配体原位合成与结构表征

Synthesis and Structure Characterization of(C_6H_8N_3)^+I_3^- and [(Cu_3I_4)(C_8H_(17)N_2)] Based on in situ Ligand Reaction

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.