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徐善生, Bin Li a, Baiquan Wang a, b, *, Shansheng Xu a, Xiuzhong Zhou a
Journal of Organometallic Chemistry 690(2005)5309-5317,-0001,():
-1年11月30日
Reductive coupling of phenylfulvene with amalgamated calcium metal followed by hydrolysis yields CpPhCHCHPhCp (1) in high yield. Refluxing ligand 1 and Fe(CO)5 in xylene produces (PhCHCHPh)-coupled bis(cyclopentadienyl) tetracacrbonyl dirron (PhCHCHPh)[(η5-C5H4)Fe(CO2]2 (2) as a mixture of meso (2-meso) and racemis isomers (2-rac). The pure reacmic isomers of the Mo and W analogues (3-rac and 4-rac) have been synthesized by lithiation of ligand 1 and addition of (MeCN)3M(CO)3(M=Mo,W) followed by oxidation with 2 equiv. of ferrocenium tetrafluroborate. All the new complexs have been fully charac-terrized. The meolecular structure of 1-meso, 2-meso, 2-rac, 3-rac, and 4-rac have been determinde by X-ray diffraction analysis.
Metal-metal bond, Cyclopentadienyl, Metal carbonyl
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徐善生, Baiquan Wang, *[a] Bin Mu, [a] Xiaobin Deng, [a] Huiling Cui, [a] Shansheng Xu, [a] Xiuzhong Zhou, [a] Fenglou Zou, [b] Yang Li, [b] Ling Yang, [c] Yufei Li, [c] and Youliang Hu[c]
Chem. Eur. J. 2005, 11, 669-679,-0001,():
-1年11月30日
合成了一系列亚环烷基桥连环戊二烯基茂金属化合物(CH2)nC(C5H4)2MCI2[M=Ti,n=4(4),5(5),6(6); M=Zr,n=4(10)、5(11)、6(12)],用甲基铝氧烷(MAO)作助催化剂研究了其催化乙烯聚合反应。其中亚环烷基桥连环戊二烯基钛化合物的催化活性远高于相应的锆和铪类似物,且在较高温度显示其最高活性。为进行对比,合成了亚硅杂环戊基桥连环戊二烯基茂金属化合物(CH2)4Si(C5H4)2MCI2(M-Ti,Zr)和亚异丙基桥连环戊二烯基茂金属化合物Me2C(C5H4)2MCI(M=Ti,Zr)并用于催化乙烯聚合。在这两种催化剂中,钛化合物的催化活性都远离于相应的锆类似物,尤其是在较低温度下。用X-射线衍射分析测定了化合物4~9的晶体结构。对催化剂结构与催化活性的关系,特别是桥链的影响进行了讨论。
bridging ligands, metallocenes, structure-activity relationships, titanium, zirconium
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【期刊论文】Diels-Alder Reactions of Benzyne with Indenyl Iron Complexes
徐善生, Baiquan Wang, * Bin Mu, Dafa Chen, Shansheng Xu, and Xiuzhong Zhou
Organometallcs 2004, 23, 6225-6230,-0001,():
-1年11月30日
The indenyl iron compound (η5-C9H7)Fe(η5-C5H5) (1) was found to react with benzyne, generated from o-trimethylsilylphenyl triflate by fluoride-induced 1, 2-elimination, to afford the Diels-Alder adduct 1,2-(1,4-dihydro-naphthalen-1,4-diyl)ferrocene (2). When the bis-(indenyl) iron complexes (η5-R-C9H6)2Fe [R=H(3); 2-Me(6); 1-SiMe3(9)] reacted with benzyne, the bisadducts [R=H(5); 2-Me(8); 1-SiMe3(11)] were obtained along with the corresponding monoadducts [R=H(4); 2-Me(7); 1-SiMe3(10)]. The reaction of teramethyl-dislyene-bridged bis(indenyl) iron (Me2SiSiMe2)(η5-C9H6)2Fe(12) with benzyne gave only the monoadduct (13). Complex 2 was also tested for ring-opening metathesis polymerization (ROMP) in the presence of Grubbs' catalyst [(PCy3)2RuCl2=CHPh] but was found to be inactive under normal conditions. The molecular structures of 2, 5, 8, and 13 have been determinde by X-ray diffraction.
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【期刊论文】Reactions of Doubly Bridged Bis (cylopentadienes) with Iron Pentacarbonyl
徐善生, Baiquan Wang, * Bin Zhu, Jianyong Zhang, Shansheng Xu, Xiuzhong Zhou, and Linhong Weng†
Organometallics 2003, 22, 4842-4852,-0001,():
-1年11月30日
When the doubly bridged bis(cyclopentadiene) ligand (Me2C)(Me2Si)(C5H4)2 (1) reacted with Fe(CO)5 in refluxing toluene, the unusual product [(C5H6)(Me2C)(Me2Si)(η5-C5H3)Fe(CO)]2-(μ-CO)2 (2) with a hydrogenated double bond in one of the cyclopentadiene ligands, the diiron complex (Me2C)(Me2Si)[(η5-C5H3)Fe(CO)2]2 (3), and the desilylation product 4 were obtained. When the reaction was performed in refluxing xylene, the novel complex (Me2C)(η5-C5H3)-(η5:η1-C5H3)[(Me2Si)Fe(CO)2][Fe(CO)2] (5) with and Fe-Si bond, which should be accompanied by the cleavage of a C-Si bond in the ligand, was isolated in addition to the complees 2~4. When bis(cyclopentadienyl) ligands bridged with R2C (R2C=Me2C, (CH2)5C)AND Me2E(E=Si, Ge) groups were used instead of 1, the similar novel complexes (R2C)(η5-C5H3)(η5:η1-C5H3)[(Me2E)Fe(CO)2] (R2C=Me2C, E=Ge (7); R2C=(CH2)5C, E=Si(17), Ge (21)) with and Fe-E bond were obtained in addition to the diiron complexes (R2C)(Me2E)-[(η5-C5H3)Fe(CO)]2[Fe(CO)2](R2C=Me2C, E=Ge (8); R2C=(CH2)5C,E=Si (18), Ge (22)) and the desilylation or degermylation products. When a tert-butyl group was introduced into the cyclopentadienyl rings, or two phenyl groups were introduced at the bridging silicon atom instead of two methyl groups in 1, only the diiron complexes (Me2C)(Me2E)[η5-t-BuC5H2]Fe(CO)2]2 (E=Si(10), Ge (13)) and (Me2C)(Ph2Si)[(η5-C5H3)Fe(CO)2]2 (15) were obtained, in addition to the desilylatin or degermylation products. Whem a methylene bridge was used instead of an isopropylene bridge in 1 and 6, the partially hydrogenated complexes (Me2E)(η3-CHC5H6)(η5-C5H3)Fe(CO)3Fe(CO)2(E=Si(24),Ge (28)), the diiron complexes (CH2)(Me2E)[(η5-C5H3)Fe(CO)]2(μ-CO)2(E=Si (25), Ge (29)), and the desilylation or degermylation products were obtained. The molecular structures of 2, 3, 5, 7, 8, 10, 11t, 15, 17, 18, 21, 24, 25, 28, and 29 were determinde by X-ray diffraction.
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【期刊论文】Reactions of Doubly Bridged Biscylopentadienes with Molybdenum (Tungsten) Carbonyl
徐善生, Baiquan Wang, * Blin Zhu, Shansheng Xu, and Xiuzhong Zhou
Organometallics 2003, 22, 4842-4852,-0001,():
-1年11月30日
Dimolybdenum complexes (X) (Y) [(η5-C5H3)Mo(CO)3]2 [Y=Me2Si, X=Me2C, (CH2)5C, CH2; Y=Ph2Si, X=Me2C] and desilylation products (X)[(η5-C5H4)Mo(CO3)2 were obtained from the reactions of carbon and sliicon doubly bridged biscyclopentadiene ligands (X) (Y) (C5H4)2 with Mo(CO)6 in refluxing xylene. When these ligands reacted with W(CO)6, under similar conditions, in addition to ditungsten complexes (X) (Y) [(η5-C5H3)W(CO)3]2 [X=Me2C; Y=Me2Si, Ph2Si] and desilylation products (X) [(η5-C5H4)W(CO)3]2, a class of structurally novel comolexes (X) (η5-C5H3) [(Y)W(CO)3][W(CO)3][for X=Me2C, (CH2)5C; Y=Me2-Si] with a W-Si bond were also isolated. The reactions of carbon and germanium dobuly bridged biscyclopentadiene ligands (X)(Me2Ge)(C5H4)2[X=Me2C, (CH2)5C] with Mo(CO)6 or W(CO)6 gave similar novel complexes (X)(η5-C5H3)(η5, η1-C5H3)[(Me2Ge)M(CO)3][M(CO)3][X=Me2C, (CH2)5C; M=Mo, W] with a M-Ge bond. The reactions also produced degermylation products. However, the corresponding dimolybdenum or ditungstem complexes were not isolated in these cases. The molecular structures of 2, 6, 8, 10, 11, 13, 14, 15, 19, 21, 22, 25t, and 26t have benn determinde by X-ray diffraction. The M-M distances in complexes 2 [3.4328(12)A], 8 [3.453(2)A], and 11 [3.403(2) A] are conspicuously elongated and are in fact the longest ever reported among the biscyclopentadienyl dimolybdenum or ditungsten complexes. The factors affecting the structures of dimolybdenum or ditungsten complexes are discussed.
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