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有机杂化锑硒化合物的溶剂热合成与晶体结构 被引量：3

Solvothermal synthesis and crystal structure of organic-hybrid selenidoantimonate
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摘要 Selenidoantimonate[Fe（en）3（Hen）]SbSe4（en=ethylenediamine） was solvothermally synthesized by a reaction on FeCl2·4H2O,Sb and Se in en at 140℃.It crystallizes in triclinic crystal system space group Pī,with a=8.8755（15）,b=9.6315（18）,c=14.251（3）,α=104.756（3）°,β=92.65（3）°,γ=109.587（4）°,V=1098.2（3）3,Z=2,Mr=734.86 g.mol-1,Dc.=2.222 g.cm-3,μ=8.526 mm-1,F（000）=700,R1=0.0236,wRw=0.0522.The crystal structure consists of tetrahedral 3- anion,octahedral [Fe（en）3]2+complex cation and protonated + cation.A three-dimensional supramolecular network is formed by the intermolecular N-H...Se and N-H...N hydrogen bonds between anions and cations.The crystal band gap is at 2.52 eV.On heating,the compound losses organic components in two steps under N2 atmospere. Selenidoantimonate [ Fe （en） 3 （Hen） ] SbSe4 （ en = ethylenediamine） was solvothermally synthesized by a reaction on FeCl2·4H2O, Sb and Se in en at 140℃. It crystallizes in triclinic crystal system space group Pi, with a =8. 8755 （15） A, b=9.6315 （18） A, c=14.251 （3） A, α=104.756 （3）°, β=92.65 （3）°, γ=109.587 （4）°, V=1098.2 （3） A^3, Z=2, Mr = 734. 86 g. mol^-1, Dc. =2.222g. cm^-3, μ=8.526mm^-1, F （000） =700, R, =0.0236, wRw=0.0522. The crystal structure consists of tetrahedral [ SbS4 ]^3- anion, octahedral [ Fe （en）3 ]^2＋ complex cation and protonated [ Hen]^＋ cation. A three -dimensional supramolecular network is formed by the intermolecular N -H…Se and N -H…N hydrogen bonds between anions and cations. The crystal band gap is at 2. 52 eV. On heating, the compound losses organic components in two steps under N2 atmospere.
作者 赵前信 邓杰 贾定先 张勇 戴洁
机构地区 苏州大学化学化工学院
出处 《化学研究与应用》 CAS CSCD 北大核心 2006年第7期823-826,共4页 Chemical Research and Application
基金 江苏省高校自然科学研究项目(05KJB150110)资助 苏州大学化学基础课实验教学中心开放课题资助
关键词 金属硒化物 溶剂热合成 晶体结构 光学性质 Selennidantimonate solvothermal synthesis crystal structure optical property
分类号 O641 [理学—物理化学]
  • 相关文献

参考文献13

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共引文献1

同被引文献44

  • 1Sheldrick W S,Wachhold M.Chalcogenidometalates of the heavier group 14 and 15 elements[J].Coord Chem Rev,1998,176:211-322.
  • 2Stephan H O,Kanatzidis M G.[Co(en)3] CoSb4S8:A novel non-centrosymmetric lamellar heterometallic sulfide with large-framework holes[J].J Am Chem Soc,1996,118:1222612227.
  • 3Stephan H,Kanatzidis M G.Low-Dimensional Sulfoantimonates with Metal Complexes as Counterions.Hydrothermal Synthesis and Properties of[M(en)3] Sb2S4(M=Co,Ni)and[M(en)3] Sb4S7(M=Fe,Ni)[J].Inorg Chem,1997,36:6050-6057.
  • 4Chen Z,Wang R J,Huang X Y,et al.Molecular building blocks for solid-state chalcogenides:solvothermal synthesis of[Mn(en)3] Te4 and[Fe(en)3] 2(Sb2Se5)[J].Acta Crystallogr,2000,C56:1100-1103.
  • 5Bensch W,Nther C,Schur M,Solvothermal synthesis of[Mn(en)3] 2[Mn4(en)9(SbSe4)4] ·H2O:the first example of a selenoantimonate(V)acting as a ligand in a transition-metal complex[J].Chem Commun,1997,1773-1774.
  • 6Vaqueiro P,Chippindale A M,Powell A V.[Co(en)3] [Sb12S19] :A new antimony sulfide with a zeolite structure containing one-dimensional channels[J].Inorg Chem,2004,43:7963-7965.
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  • 8Jia D X,Zhu Q Y,Dai J,et al.The first example of solvothermally synthesized thioantimonates(V)with ethylenediamine coordinated lanthanide(III):[Sm(en)4] SbS4·0.5en and[Sm(en)3(H2O)(μ-SbS4)] ∞[J].Inorg Chem,2005,44:819-821.
  • 9Jia D X,Zhao Q X,Zhang Y,et al.Solvothermal Syntheses of[Ln(en)3(H2O)x(μ3-x-SbS4)] (Ln=La,x=0;Ln=Nd,Sm,x=1)and[Ln(en)4] SbS4·0.5en(Ln=Eu,Dy,Yb):a systematic study on the formation and crystal structures of new lanthanide thioantimonates(V)[J].Inorg Chem,2005,44:8861-8867.
  • 10Jia D X,Zhao Q X,Zhang Y,et al.Solvothermal syntheses,crystal structures and properties of new selenidoantimonates[Ln(en)4(SbSe4)] (Ln=La,Nd)and[Sm(en)4] SbSe4·0.5en:the first example of an SbSe43-anion acting as a ligand to a lanthanide complex[J].Eur J Inorg Chem,2006,2760-2765.

引证文献3

化学研究与应用
2006年 第7期

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