2,9-二甲基-1,2,3,4,7,8,9,10-八氢-1,10-菲啰啉的晶体结构研究
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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.
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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[2]J.Martinez-Lillo,T.F.Mastropietro,R.Lappano,A.Madeo,M.E.Alberto,N.Russo,M.Maggiolini,M.G.De.Rhenium(IV)compounds inducing apoptosis in cancer cells[J].Chem.Commun.,2011,47:5283-5285.
[3]J.Toneatto,G.A.Argueello.New advances in the study on the interaction of[Cr(phen)2(dppz)]3+complex with biological models,association to transporting proteins[J].J.Inorg.Biochem.,2011,105:645-651.
[4]R.Y.Kuang,X.C.Zhou,L.J.Liu,J.Y.Lin.A new 1D coordination polymer constructed by CaCl2with 5-a association to transporting proteinsminoisophtalic acid(H2AIP)and 1,10-phenanthroline ligands using the water bath method[J].Russ.J.Coord.Chem.,2010,36:918-922.
[5]O.O.E.Onawumi,O.O.P.Faboya,O.A.Odunola,T.K.Prasad,M.V.Rajasekharan.Mixed ligand tris-chelate of copper(II)with N,N-donor ligands:Synthesis,structure and spectra of[Cu(en)(phen)2]X2·2phen·8H2O(X=Cl-,NO-3)[J].Polyhedron,2011,30:725-729.
[6]A.Wojciechowska,M.Daszkiewicz,Z.Staszak,M.Boczar,J.Jezierska,M.Cieslak-Golonka.Monodentate coordinated chromate(VI)ion in[Cu(phen)2OCrO3](phen)0.5·4H2O completing the square pyramidal geometry of the copper(II)in the solid state[J].Struct.Chem.,2010,21:337-345.
[7]F.-Y.Yi,Q.-P.Lin,T.-H.Zhou,J.-G.Mao.A Series of New Manganese(II)Sulfonate-Arsonates with 2D Layer,1D Chain,and 0D Clusters Structures[J].Inorg.Chem.,2010,49:3489-3500.
[8]F.-Y.Yi,Q.-P.Lin,T.-H.Zhou,J.-G.Mao.A Series of Novel Lanthanide(III)Trisulfonates Based on Dinuclear Clusters[J].Cryst.Growth Des.,2010,10:1788-1797.
[9]A.-x.Chen,G.Liu,H.Li,J.-d.Wang,F.Yue.Synthesis.Crystal structure and luminescence property of a chiral magnesium(II)mixed-ligand complex[Mg(H2O)2(phen)(HBDC)2](phen)[J].J.Chem.Crystallogr.,2011,41:143-146.
[10]C.Bianchini,V.Dal Santo,A.Meli,S.Moneti,R.Psaro,L.Sordelli,F.Vizza.Selective hydrogenation of 1,10-phenanthrolines by silica-supported palladium nanoparticles[J].Inorg.Chim.Acta.,2008,361:3677-3680.
[11]C.Metallinos,F.B.Barrett,J.L.Chaytor,M.E.A.Heska.A Benzimidazole-Based N-Heterocyclic Carbene Derived from 1,10-Phenanthroline[J].Org.Lett.2004(6):3641-3644.
[12]G.M.Sheldrick.SHEXTL(Xprep,SADABS,XS,XL).Crystallographic Software Package,version 5.1,Bruker-AXS,Madison,WI,1998.