Living polymerization of 1,3-butadiene by a Ziegler-Natta type catalyst composed of iron(III) 2-ethylhexanoate, triisobutylaluminum and diethyl phosphite

Living characteristics of facilely prepared Ziegler-Natta type catalyst system consisting of iron(III) 2-ethylhexanoate, triisobutylaluminum and diethyl phosphite have been found in the polymerization of 1,3-butadiene in hexane at 40 degrees C. The characteristics have been well demonstrated by: a first-order kinetics with respect to monomer conversion, a narrow molecular weight distribution (M-w/M-n = 1.48-1.52) of polybutadiene in the entire range of polymerization conversion and a good linearity between M-n and the yield of polymer. Feasible post-polymerization of 1,3-butadiene and block co-polymerization of 1,3-butadiene and isoprene further support the living natures of the catalyst bestowed with.

Near-infrared luminescent mesoporous MCM-41 materials covalently bonded with ternary thulium complexes

Two beta-diketones 4,4,4-trifluoro-1-2-thenoyl-1,3-butanedione (Htta) and 4,4,4-trifluoro-1-(2-naphthyl)-1,3-butanedione (Htfnb), which contain trifluoroalkyl chain, were selected as the main sensitizer for synthesizing Tm(L)(3)phen (L = tta, tfnb) complexes. The two near-infrared (NIR) luminescent thulium complexes have been covalently bonded to the ordered mesoporous material MCM-41 via a functionalized 1,10-phenanthroline (phen) group 5-(N,N-bis-3-(triethoxysilyl)propyl)ureyl-1,10-phenanthroline (phen-Si) [The resultant mesoporous materials are denoted as Tm(L)(3)phen-MCM-41 (L = tta, tfnb)]. The Tm(L)(3)phen-MCM-41 (L = tta, tfnb) mesoporous materials were characterized by small-angle Xray diffraction (XRD) and N-2 adsorption/desorption, and they show characteristic mesoporous structure of MCM-41.

catena-Poly[diammonium [diaquabis(pyridine-2,4-dicarboxylato-kappa N-2,O-2)cuprate(II)] [[diaquacopper(II)]-mu-pyridine-2,4-dicarboxylato-kappa N-3,O-2:O-2 '-[tetraaquacadmium(II)]-mu-pyridine-2,4-dicarboxylato-kappa O-3(2):N,O-2 '] hexahydrate]

The title mixed-metal complex, {(NH4)(2)[Cu(C7H3NO4)(2)(H2O)(2)][CdCu(C7H3NO4)(2)(H2O)(6)]center dot 6H(2)O}(n), contains one octahedrally coordinated Cd-II center and two octahedrally coordinated Cu-II centers, each lying on an inversion center. The two Cu-II atoms are each coordinated by two O atoms and two N atoms from two 2,4-pydc (2,4-H(2)pydc = pyridine-2,4-dicarboxylic acid) ligands in the equatorial plane and two water molecules at the axial sites, thus producing two crystallographically independent [Cu(2,4-pydc)(2)(H2O)(2)](2-) metalloligands. One metalloligand exists as a discrete anion and the other connects the Cd(H2O)(4) units, forming a neutral chain.

A monometallic tri-spin single-molecule magnet based on rare earth radicals

A mononuclear tri-spin single-molecule magnet based on the rare earth radical [Tb(hfac)(3)(NITPhOEt)(2)] (NITPhOEt = 4'-ethoxy-phenyl-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide) has been synthesized, structurally characterized and the alternating current signals show a slow relaxation of magnetization and frequency-dependent signals.

Novel, highly efficient blue-emitting heteroleptic iridium(III) complexes based on fluorinated 1,3,4-oxadiazole: tuning to blue by dithiolate ancillary ligands

Novel blue-emitting phosphorescent iridium(III) complexes with fluorinated 1,3,4-oxadiazole derivatives as cyclometalated ligands and dithiolates as ancillary ligands have been synthesized and fully characterized; highly efficient OLEDs have been achieved using these complexes in the light-blue to blueemitting region.

聚对苯二甲酸1,3-丙二醇酯溶液浇铸薄膜形态结构

聚对苯二甲酸 1 ,3-丙二醇酯 ( PTT)是典型的半结晶聚合物 ,从熔体结晶形成球晶 ,在某一结晶温度范围内 ,在球晶中可观察到环带结构[1～ 4 ] .一般认为 ,环带球晶的形成归因于片晶沿球晶径向的周期性扭曲[1,2 ] .本文研究了 PTT溶液浇铸薄膜在溶剂挥发过程中等温结晶的形态结构 .1　实验部分　　 PTT样品为美国壳牌化学公司产品 ,熔点为 2 2 8℃ .将 PTT粒料于 1 1 0℃溶解在苯酚和1 ,1 ,2 ,2 -四氯乙烷 (质量比为 60∶ 40 )的混合溶剂中 ,配成质量分数为 0 .2 %～ 2 %的溶液 ,滴少许溶液在加热的云母片上 ,在预先设定的结晶温度 ( 90～ 2 0 0℃ )下等温结晶 ,然后将 PTT薄膜快速冷却至室温 .用 Leica DMLP偏光显微镜 ( PL M)和 SPA- HV30 0原子力显微镜 ( AFM)进行形态表征 .2　结果与讨论　　图 1为 PTT溶液浇铸薄膜在不同温度下等温结晶后的 PLM图 ,可以清楚地看到 Maltese十字消光现象 .PTT溶液浇铸薄膜在 90～ 1 30℃的结晶温度范围内 ,形成环带球晶 ;当结晶温度为 1 40℃...

2-[2-(Phenylsulfonyl)ethyl]isoindoline-1,3-dione

In the title compound, C16H13NO4S, the phthalimide ring system makes a dihedral angle of 56.7 (1)degrees with the phenyl ring.

catena-Poly[[[di-mu-acetato-kappa O-4 : O '-bis[(acetato-kappa O-2,O ')manganese(II)]]-di-mu-4,4 '-bipyridine-kappa N-4 : N '] monohydrate]

The title compound, {[Mn-2(CH3CO2)(4)(C10H8N2)(2)](H2O)-H-.}(n), is a one-dimensional coordination polymer with a ladder-like structure. Two Mn-II atoms, each coordinated by a chelating acetate ligand, are bridged by two bidentate acetate ligands to form a centrosymmetric [Mn-2(CH3CO2)(4)] unit. Two 4,4'-bipyridine ligands link the [Mn-2(CH3CO2)(4)] units through Mn-N bonds to generate a molecular ladder. The water O atom lies on a crystallographic twofold rotation axis.

BaLiF_3∶Eu,Gd中Gd~(3+)→Eu~(2+)的能量传递

研究了 Ba Li F3中 Gd3+和 Eu2 +的光谱性质及 Gd3+对 Eu2 +的能量传递过程 ,讨论了传递机理 .Gd3+的含量 (物质的量分数 )为 0 .3 %时 ,传递效率最高 ,传递几率 PSA=1 .3 5× 1 0 5s- 1 .当 Gd3+的含量高于 0 .3 %时 ,由于 Gd3+ 和 Eu2 + 竞争吸收 Gd3+ 占优势 ,增加 Gd3+ 含量 ,竞争吸收比相应增加 ,Eu2 + 自身吸收光子数目减少 ,发射强度降低

Synthesis and structure of molybdenum-citrato cluster mu(2)-S bridge

A new molybdenum-citrato cluster containing [Mo2O2(mu-S)(2)(C6H5O7)(C6H4O7)](5-) anion was synthesized and characterized by elemental analysis, IR, UV-Vis spectra, XPS and X-ray diffraction. The parameters of the crystal structure of the compound are monoclinic, space group P2(1)/c, a = 2. 376 6(5) nm, b = 1. 327 4(3) nm, c = 2. 247 1(5) nm, beta = 118. 21 degrees, V = 6. 247(2) nm(3), Z = 8, D-c = 2. 128 g/cm(3), F(000) = 3 984, mu = 1 694 cm(-1), R = 0. 083 1 and R-2,R-w = 0. 154 9. The anion is binuclear molybdenum-citrato complex with mu(2)-S bridge. Each molybdenum atom pocesesses a distorted octahedral struture, which is coordinated with a terminal oxygen, two sulfur atoms, three oxygen atoms of hydroxyl, alpha-carboxylate, beta-carboxylate from citrate.

Spectroscopy of several beta-diketone compounds and their tautomers

Six beta-diketone compounds, 1,3-bis(4-nitrophenyl)-1,3-propanedione (1), 1-(4-nitrophenyl)-3-(3-nitrophenyl)-1,3-propanedione(2), 1,3-bis(3-nitrophenyl)-1,3-propanedione(3) 1,3-bis(4-amimophenyl)-1,3-propanedione(4), 1-(4-amimophenyl)-3-( 3-amimophenyl)-1,3-propanedione(5) and 1,3-bis (3-amimophenyl)-1,3-propanedione(6) were synthesized, Their structures were characterized by IR, UV-Vis, fluorescence and NMR spectroscopy, The percentage of keto tautomer, enol-keto equilibrium constant and enol tautomer ratio of them were also determined, The percentage of keto tautomer is increased in the order from compound 1 to 3 and decreased in the order from compound 4 to 6, which show the effect of substituent on the tautomer. The results of enol tautomer ratio of compounds 2 and 5 indicated that b-form of enol is slightly more favorable than its a-form.

1,3—双烯聚合物的环化

采用AlEt2Cl－C6H5CH2Cl体系成功地对聚异戊二烯、聚了二烯、聚氯丁二烯3种1，3—双烯聚合物进行了环化，并对环化过程进行了比较。

Ce_(1-x)Sm_xO_(2-x/2)的溶胶-凝胶法的合成及氧空位的研究

本文利用溶胶-凝胶法合成了Ce_(1-x)Sm_xO_(2-x/2)(x=0-0.4)系列固体电解质,并且系统地研究了其晶体结构随Sm含量的变化关系。XRD表明:该体系从160℃开始即形成了立方萤石结构,且在所研究的组成范围内全部形成了单相固溶体。此温度远低于传统的高温固相合成法所需的温度,同时也较水热合成法的温度低。高温X-ray衍射研究表明直到800℃Ce_(1-x)Sm_xO_(2-x/2)未出现结构相转变,其晶格常数和晶胞体积随温度升高而增大。EPR测试证实了由于Sm~(3+)部分置换Ce~(4+)固溶体中所存在的单电荷缺陷(Sm_(Ce’),V_o~(oo))结构。在固溶体的Raman谱中观察到:纯CeO_2在465cm~(-1)仅有一个Raman振动模式,随着掺杂量的增大,此振动模式向低频方向移动,而且Raman线变宽且在570cm~(-1)附近出现一新的峰,这些变化都是由Sm~(3+)取代Ce~(4+)所产生的氧空位引起的。

Ce_(1-x)Ca_xO_(2-x)的溶胶-凝胶法的合成及其性质

用溶胶 -凝胶法合成了 Ce1-x Cax O2 -x(x=0～ 0 .3 5 )系列固体电解质 ,系统地研究了其晶体结构随Ca O含量的变化关系 .XRD测试表明 ,该体系于 1 60℃即形成萤石结构纯相 .高温 XRD表明 ,从室温至80 0℃ ,Ce1-x Cax O2 -x(x=0～ 0 .3 5 )未出现结构相变 .此法合成温度远低于传统的高温固相合成法和水热合成法的温度 .合成物的颗粒小 ,粒度均匀 .在 1 3 0 0℃即可烧结成高致密度样品 .XPS测试表明 ,掺杂 Ca O后吸附氧浓度明显增大 ,氧空位增多 ,电导率和氧离子迁移数增大 ,改善了 Ce O2 基固体电解质的性能 .

(Ce_(0.8)RE_(0.2))_(1-x)M_xO_(2-δ)固体电解质的溶胶-凝胶合成及其电性质

利用溶胶 凝胶法合成了 (Ce0 .8RE0 .2 ) 1-xMxO2 -δ(RE :稀土 ,M :碱土 )系列固体电解质 ,XRD表明 80 0℃即形成萤石结构 ,较高温固相反应合成温度低约 70 0℃ .测定了样品的电导率和阻抗谱 .XPS测试表明 ,掺杂碱土氧化物后吸附氧浓度明显增大 ,氧空位增多 ,电导率和氧离子迁移数增大 ,改善了CeO2 基固体电解质的性能 .讨论了碱土及稀土离子对电性质的影响 .(Ce0 .8Sm0 .2 ) 1-0 .0 5 Ca0 .0 5 O2 -δ80 0℃时电导率0 1 2 6S·cm-1,氧离子迁移数 0 .99.