河北师范大学学报—

期刊信息

刊名：河北师范大学学报（自然科学版）Journal of Hebei Normal University (Natural Science)
主办：河北师范大学
ISSN： 1000-5854
CN： 13-1061/N
中国科技核心期刊
中国期刊方阵入选期刊
中国高校优秀科技期刊
华北优秀期刊
河北省优秀科技期刊

协同采编系统

友情链接

含氮杂环钌簇合物的合成与表征

商成喜^1,2

马志宏³

韩亚雪¹

韩占刚¹

郑学忠¹

林进¹

1. 河北师范大学化学与材料科学学院, 河北石家庄 050024;
2. 承德护理职业学院涉外护理系, 河北承德 067000;
3. 河北医科大学基础医学院, 河北石家庄 050017
DOI： 10.13763/j.cnki.jhebnu.nse.2015.03.010

Synthesis and Characterization of Ruthenium Cluster Compounds Containing N-heterocycle

SHANG Chengxi^1,2, MA Zhihong³, HAN Yaxue¹, HAN Zhangang¹, ZHENG Xuezhong¹, LIN Jin¹

PDF
下载
HTML

摘要/Abstract

摘要：

3-(2-吡嗪基)茚、 9-(2-吡嗪基)芴和 9-(2-吡啶基)芴分别与Ru₃(CO)₁₂在二甲苯或庚烷中加热回流,得到了3个新的三核簇合物 1~3.通过元素分析、红外光谱、核磁共振氢谱对簇合物的结构进行了表征,并用X射线单晶衍射法测定了簇合物 1 的结构.结果表明:晶体属于三斜晶系,P_T空间群,其晶胞参数a=0.9329(3)nm,b=1.0885(3)nm,c=1.1970(3)nm,α=87.622(4)°,β=74.807(3)°,γ=78.951(4)°,V=1.1513(6)nm³,Z=2,D_c=2.156g/cm³,μ=1.999mm^-1,F(000)=716,R₁=0.0457,wR₂=0.1153.CCDC:937927.

Abstract：

The 3-(2-pyrazinyl)indene,9-(2-pyrazinyl)fluorene and 9-(2-pyridyl) fluorene reacted with Ru₃(CO)₁₂ in refluxing xylene or heptane to give three trinuclear cluster compounds 1~3.Three new cluster compounds were characterized by IR,elemental analysis and ¹HNMR spectra,respectively.The crystal structure of compound 1 was determined by X-ray single crystal diffraction.Crystal data:triclinic system,space group P_T,a=0.9329(3)nm,b=1.0885(3)nm,c=1.1970(3)nm,α=87.622(4)°,β=74.807(3)°,γ=78.951(4)°,V=1.1513(6)nm³,Z=2,D_c=2.156g/cm³,μ=1.999mm^-1,F(000)=716,R₁=0.0457,wR₂=0.1153.CCDC:937927.

关键词

关键词： 茚 ; 芴 ; 羰基钌 ; X射线单晶衍射 ; 簇合物

Key words： indene ; fluorine ; ruthenium carbonyl ; X-ray single crystal diffraction ; cluster compound

参考文献 22

[1] KING R B.Pentamethylcyclopentadienyl Metal Complexes:An Entry to Metal Carbonyl Derivatives with Metal-metal Multiple Bonding[J].Coord Chem Rev,1976,20:155-169.
[2] JUTZI P,BURFORD N.Structurally Diverse π-cyclopentadienyl Complexes of the Main Group Elements[J].Chem Rev,1999,99:969-990.
[3] SITZMANN H.Maximum Spin Cyclopentadienyl Complexes of 3d Transition Metals[J].Coord Chem Rev,2001,214:287-327.
[4] ARNDT S,OKUDA J.Mono-cyclopentadienyl Complexes of the Rare-earth Metals[J].Chem Rev,2002,102:1953-1976.
[5] 马志宏,郭凯明,李素贞,等.乙基四甲基环戊二烯基铁羰基化合物的合成及晶体结构[J].河北师范大学学报:自然科学版,2013,147(1):51-55.
[6] QIAN Y L,HUANG J L,BALA M D,et al.Synthesis,Structures and Catalytic Reactions of Ring-substituted Titanium(Ⅳ) Complexes[J].Chem Rev,2003,103:2633-2690.
[7] WITTE P,LAL T K,WAYMOUTH R M.Synthesis of Unbridged Bis(2-R-indenyl)zirconocenes Containing Functional Groups and Investigations in Propylene Polymerization[J].Organometallics,1999,18:4147-4155.
[8] RESCONI L,CAVALLO L,FAIT A,et al.Selectivity in Propene Polymerization with Metallocene Catalysts[J].Chem Rev,2000,100:1253-1346.
[9] STRADIOTTO M,MCGLINCHEY M J.η¹-indenyl Derivatives of Transition Metal and Main Group Elements:Synthesis,Characterization and Molecular Dynamics[J].Coord Chem Rev,2001,221:311-378.
[10] CALHORDA M J,FÉLIX V,VEIROS L F.Bonding and Structural Preferences of Indenyl Complexes:MInd₂L_n (n=0~3)[J].Coord Chem Rev,2002,230:49-64.
[11] ZARGARIAN D.Group 10 Metal Indenyl Complexes[J].Coord Chem Rev,2002,233:157-176.
[12] CECCON A,SANTI S,ORIAN L,et al.Electronic Communication in Heterobinuclear Organometallic Complexes Through Unsaturated Hydrocarbon Bridges[J].Coord Chem Rev,2004,248:683-724.
[13] GLADYSZ J A.Frontiers in Metal-catalyzed Polymerization:Designer Metallocenes,Designs on New Monomers,Demystifying,Metathesis Dishabille[J].Chem Rev,2000,100:1167-1168.
[14] CALHORDA M J,ROMÃO C C,VEIROS L F.The Nature of the Indenyl Effect[J].Chem Eur J,2002,8:868-875.
[15] GRIMMER N E,COVILLE N J,SMITH J M,et al.Zirconium Bis-indenyl Compounds:Synthesis and X-ray Crystallography Study of 1- and 2-substituted Bis(R-indenyl)zirconium Dichloride Metallocenes[J].J Organomet Chem,2000,616:112-127.
[16] TRIFONOV A A,FEDOROVA E A.Bridging μ-η⁵:η⁴-coordination of an Indenyl Ligand and Reductive Coupling of Diazabutadienes in the Assembly of Di- and Tetranuclear Mixed-valent Ytterbium Indenyldiazabutadiene Complexes[J].Chem Eur J,2006,12(10):2752-2757.
[17] BRUCE M I,SKELTON B W,WHITE A H,et al.Cyclisation of Allenylidene Ligands to Indenyl Groups on Ruthenium Clusters[J].J Cluster Sci,2002,13(2):235-247.
[18] TAN Y L K,LEONG W K.Reactivity of the Heteronuclear Cluster RuOs₃(μ-H)₂(CO)₁₃ with Indene[J].J Organomet Chem,2007,692(4):768-773.
[19] CHEN D F,LI Y,WANG B Q,et al.Reactions of Pyridyl Side-chain-functionalized Cyclopentadienes with Metal Carbonyl:Intramolecular C-H Activation of Pyridine[J].Organometallics,2006,25(1):307-310.
[20] NAGA N,SAKAI H,USUI C,et al.Synthesis of Polyethylene and Polypropylene Containing Fluorene Units in the Side Chain[J].J Polym Sci,Part A:Polym Chem,2010,48:3542-3552.
[21] LI X F,WANG X Y,TONG X,et al.Aluminum Effects in the Syndiospecific Copolymerization of Styrene with Ethylene by Cationic Fluorenyl Scandium Alkyl Catalysts[J].Organometallics,2013,32:1445-1458.
[22] FLECKENSTEIN C A,PLENIO H.9-fluorenylphosphines for the Pd-catalyzed Sonogashira,Suzuki,and Buchwald-hartwig Coupling Reactions in Organic Solvents and Water[J].Chem Eur J,2007,13:2701-2716.