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国家自然科学基金(20472063)

作品数:15 被引量:17H指数:3
相关作者:沈琪姚英明张勇张振琴黄华更多>>
相关机构:苏州大学南京医科大学泰州师范高等专科学校更多>>
发文基金:国家自然科学基金江苏省有机合成重点实验室资助项目更多>>
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15 条 记 录,以下是 1-10
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二(环戊二烯基)(双烯酮亚胺基)镱配合物的合成和晶体结构被引量:1
2006年
Reaction of the β-diketiminate ytterbium dichloride LYbCl2(THF)2(L=2,6-Pri2C6H3)NC(Me)CHC(Me)N(C6H3-2,60Pri2)(1)with 2equiv off C5H5Na in THF gave rise to the title complex LYb(C5H5)2(2),and the crystal structure of the complex 2 was determined by single-crystal X-ray diffraction.The crystal belongs to orthorhombic,space group P21212 with a=4.3219(6),b=1.6602(2),c=0.9604(1)nm,V=6.891(2)nm3,Z=8,Dc=1.390 Mg·m-3,R=0.0331,wR=0.0535.In the molecular structure of the title complex,the central metal atom Yb is coordinated by two cyclopentadienyl rings and two nitrogen atomes of β-diketiminate group to form an eight-coordinate distorted tetrahedral geometry.
黄华张勇姚英明戚瑞朋沈琪
关键词:晶体结构
Synthesis and Characterization of A Polynuclear Yttrium Trifluoroethoxide and Its Activity for Oligomerization of Phenyl Isocyanate被引量:5
2006年
A polynuclear yttrium trifluoroethoxide was synthesized and its activity for the oligomerization of phenyl isocyanate was tested. Reaction of anhydrous YC13 with CF3CH2ONa in a 1 : 3 molar ratio in THF at room temperature, after workup, gave complex 1 as colorless crystals. The composition of complex 1 is [Y(OCH2CF3)3]6ONa2(THF)12, which was identified by elemental analysis and ^1H NMR. Further X-ray structure determination reveals that complex 1 is a polynuclear ion pair compound, [Y6(μ6-O)(OCH2CF3)18]^2- [Na(THF)6]2+ (1). The crystal data of complex 1 are trigonal, P-3 space group, a = 1.78440(14) nm, b = 1.78440(14) nm, c = 1.27395(12) nm, γ= 120°, V=3.5129(5) nm^3, Z = 1, Dc = 1.607 mg·m^-3, μ = 2.591 mm^- 1(Mo Ka), F(000) = 1710, R = 0.067, wR = 0. 182. Preliminary results demonstrated that complex 1 is a highly effective catalyst for the oligomerization of phenyl isocyanate.
彭红梅姚英明邓明宇张勇沈琪
Synthesis and Characterization of Bis(guanidinate) Zirconium Complexes
2005年
Addition of one equivalent of LiN(i-Pr)2 or LiN(CH2)5 to carbodiimides, RN=C=NR [R=cyclohexyl (Cy), isopropyl (i-Pr)], generated the corresponding lithium of tetrasubstituted guanidinates {Li[RNC(N R^′2)NR](THF)}2 [R=i-Pr, N R^′2=N(i-Pr)2 (1), N(CH2)5 (2); R=Cy, N R^′2=N(i-Pr)2 (3), N(CH2)5 (4)]. Treatment of ZrCl4 with freshly prepared solutions of their lithium guanidinates provided a series of bis(guanidinate) complexes of Zr with the general formula Zr[RNC(N R^′2)NR]2Cl2 [R=i-Pr, N R^′2=N(i-Pr)2 (5), N(CH2)5 (6); R=Cy, N R^′2=N(i-Pr)2 (7), N(CH2)5 (8)]. Complexes 1, 2, 5-8 were characterized by elemental analysis, IR and ^1H NMR spectra. The molecular structures of complexes 1, 7 and 8 were further determined by X-ray diffraction studies.
庞兴安姚英明王俊峰盛鸿婷张勇沈琪
关键词:GUANIDINATEZIRCONIUM
二价双烯酮亚胺基稀土金属配合物催化ε-己内酯开环聚合被引量:1
2005年
Divalent β-diketiminate lanthanide complexes LYbR(THF)(L={(2,6-Me2C6H3)NC(Me)}2CH;R=C9H7(1),CH3C5H4(2),OC6H2-But2-2,6-Me-4(32))were synthesized by reducing the mixed-ligand trivalen(t) β-diketiminate ytterbium chlorides synthesized in situ with Na-K alloy.These divalent lanthanide complexes exhibit good catalytic activity for the ring opening polymerization of ε-caprolactone.
张振琴沈琪张勇姚英明
关键词:Ε-己内酯开环聚合
胺基桥联双芳氧基稀土金属氯化物的合成和表征(英文)
2007年
无水三氯化稀土LnCl_3与1倍量的胺基桥联双芳氧基钠LNa_2[L=Me_2NCH_2CH_2N{CH_2-(2-O-C_6H_2- Bu^t-3-Me-5)}_2]在四氢呋喃中室温下反应生成胺基桥联双芳氧基稀土金属氯化物LLnCl(THF)(Ln=Yb(1),Ln=Er(2)).这些配合物都经过了元素分析和红外光谱表征,并测定了配合物1的晶体结构.配合物1·C_7H_8 (C_(39)H_(58)ClN_2O_3Yb,Mr=811.36)属于单斜晶系,P2_1/c空间群,a=9.361 5(8),b=14.287(1),c=29.493(3)(?),β=98.516(2)°,V=3901.1(6)(?)~3,Z=4,Dc=1.381g·cm^(-3),λ(Mo Kα)=0710 70(?),μ=2.502 mm^(-1),F(000)= 1668,R=0.026 7,wR=0.0616.中心金属与来自胺基桥联双芳氧基配体上的2个氧原子和2个氮原子以及1个氯原子和1个来自四氢呋喃的氧原子配位,形成1个六配位的扭曲的八面体几何构型.
戚瑞鹏王余明马猛涛姚英明张勇沈琪
关键词:稀土金属晶体结构
Unexpected carbon-oxygen bond cleavage of THF promoted by guanidinate titanium complex/lithium diisopropylamide: Synthesis and crystal structure被引量:1
2005年
An unexpected carbon-oxygen bond cleavage of THF (THF = tetrahydrofuran) promoted by guanidinate titanium complex was described. Guanidinate lithium [Pr2iNC(NCy)2]Li (Cy = cyclohexyl) formed in situ reacted with TiCl4(THF)2 in a 2:1 molar ratio to produce the gua- nidinate titanium chloride [Pr2iNC(NCy)2]2TiCl2 (1) in good yield. The reaction of [Pr2iNC(NCy)2]2TiCl2 with lithium diisopropylamide in THF afforded an unexpected [Pr2iNC(NCy)2]2Ti(OBun)2 (2), which was formed by the cleavage of carbon-oxygen bond of THF. Complexes 1 and 2 were fully characterized by elemental analysis, NMR and IR spectroscopies, and X-ray crystal structure determination for complex 2.
ZHANG YongWANG MeiYAO YingmingSHEN Qi
关键词:四氢呋喃钛络合物
Well-defined bis(phenolate) lanthanide methoxides as efficient initiators for the polymerization of cyclic carbonate and lactide被引量:3
2007年
Lanthanide methoxides supported by carbon-bridged bis(phenolate) ligands 2,2′-methylene-bis(6-tert- butyl-4-methylphenoxo) (MBMP2-) [(MBMP)Ln( μ-OMe)(THF)2]2 (Ln = Nd (1), Yb (2)) were synthesized in high yields by the protolysis reaction using (C5H5)3Ln(THF) as starting materials, and complex 1 was structurally characterized. The coordination geometry around the center metal can be best described as a distorted octahedron. Complexes 1 and 2 were shown to be efficient initiators for the ring-opening polymerization of 2,2-dimethyltrimethylene carbonate (DTC) and L-lactide. The mechanism of DTC polymerization was explored by the end group analysis of the oligomer.
XU XiaoPingYAO YingMingZHANG YongSHEN Qi
Synthesis and structural characterization of lanthanide coordination polymers constructed from a 13-membered macrocycle
2007年
The lanthanide coordination polymers bearing a 13-membered macrocycle, [(13-EDTA-pnOH)H2] were synthesized. The products [Ln(13-EDTA-pnOH)(H2O)2·NO3]n (Ln = Eu(1), Tb(2), Dy(3)) have been obtained by MS, IR and element analyses. The solid-state structure of 1 was established by single-crystal X-ray analysis. The coordination geometry around the central metal atom in complex 1 is a nine-coor-dinated, tricapped-trigonal prism having six donor atoms (two amine nitrogen atoms, two amide oxygen atoms and two carboxymethyl oxygen atoms) from one ligand, one oxygen atom from a neighboring ligand, and two more oxygen atoms from two water molecules. The europium atoms are linked by―Eu―O―C―O―Eu―bridges to form an infinite chain.
YAO YingMingSHEN QiWONG Wing Tak
关键词:配位聚合物
A Novel Divalent Ytterbium Complex Supported by a Bridged Diamide Ligand: Synthesis and Structure of [{Me2Si(NPh )2Yb(THF)2}(μ3-CI)(μ4-CI){Li(TH F) }2]2·2THF
2007年
The reaction of anhydrous YbCl3 with 1 equiv, of Li2Me2Si(NPh)2 in THF, after workup, yielded a ytterbium(Ⅲ) chloride [{Me2Si(NPh)2Yb}(μ2-CI)(TMEDA)]2·3PhMe (1) (TMEDA=tetramethylethanediamine). The same reaction followed by treatment with Na-K alloy afforded a new ytterbium(H) complex supported by a bridged diamide with four coordinated LiC1 molecules, [{Me2Si(NPh)2Yb(THF)2}(μ3-CI)(μ4-CI){Li(THF)}2]2·2THF (2) in high yield. Both complexes were structurally characterized by X-ray analysis to be dimers. Complex 1 was a chlorine-bridged dimer with ytterbium in a distorted octahedral geometry. In complex 2 two [Me2Si(NPh)2Yb(THF)2]- (μ3-CI)[Li(THF)]2 moieties were connected with each other by two μ4-CI bridges to form a "chair-form" framework.
陆澄容赵蓓周利英沈琪姚英明张勇
关键词:SYNTHESIS
Synthesis, Characterization, and Reactivity of Amine Bis(phenolato) Cyclopentadienyl Lanthanide Complexes被引量:1
2007年
(C5H5)3Ln(THF)reacted with amine bis(phenol) LH2 [ L = Me2NCH2CH2N {CH2-(2-O-C6H2-But^1-3-Me- 5)}2 ] in a 1:1 molar ratio in THF to generate the amine bis(phenolato) cyclopentadienyl lanthanide complexes LLn(C5H5) (THF)·(THF),(Ln = La (1), n =0; Ln = Sm(2), n = 1) in high yields. Complexes 1 and 2 were fully characterized by elemental analysis, NMR (for 1) and IR spectra, and X-ray structural determination. The crystal data of complex 1 are monoclinic, P21/c space goup, a= 1.1595(1) nm, b = 1.8588(2) nm, c = 1.6647(1) nm, β = 98.490(2)°, V =3.5486(5) nm^3, Z =4, Dc = 1.338 mg· m^3,μ = 1240 mm^-1, F(000)= 1488, R =0.0249, wR = 0.0568. The crystal data of complex 2 are monoclinic, P21/c sp ace goup, a = 0.9692 (1) nm, b = 1.4583 (2) nm, c = 2.8192 (3) nm, = 96.805 (2)°, V = 3.9584 (7) nm^3, Z=4, Dc =1.340 mg · ma, μ = 1.524 mm^-1, F(000)= 1668, R =0.0346, wR =0.0756. The attempts failed to synthesize the amine bis(phenolate) lanthanide alkoxides by the reactions of complexes 1 and 2 with alcohols. The preliminary results revealed that complex 1 can initiate ε-caprolactone polymerization.
周兰芝王余明姚英明张勇沈琪
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