二芳氧基稀土氯化物(ArO)2YCl(THF)2·MePh的合成、表征及晶体结构(ArO=2,6-二叔丁基-4-甲基酚基)

无水YCl3 与二倍量的ArONa(ArO =2 ,6 二叔丁基 4 甲基酚基 )在四氢呋喃 (THF)中反应 ,经甲苯溶液重结晶 ,高产率地合成了二芳氧基稀土氯化物 (ArO) 2 YCl(THF) 2 ·MePh。产物经元素分析和核磁共振表征 ,并测定了其晶体结构。配合物属正方晶系 ,I4( 1) /acd空间群 ,晶胞参数为a =1.8913( 1)nm ,b =1.8913( 1)nm ,c =5 .2 2 39( 1)nm ,V =18.6 86 ( 1)nm3 ,Z =16 ,Dc=1.137mg·m- 3 ,μ =1.342mm- 1 (MoKα) ,F( 0 0 0 ) =6 848,R =0 .0 46 9,Rw=0 .112 2。中心金属钇原子与二个芳氧基中的氧原子、一个氯原子和两个THF分子中的氧原子配位 ,形成一个五配位的扭曲的三角双锥几何构型。Y O(Ar)和Y Cl的键长分别为 0 .2 10 1( 3)和 0 .2 5 17( 6 )nm。     

Ethylene Polymerization Catalyzed by Monocyclopentadienyl Titanium Complex Containing 8-Quinolinolato Ligand and ADF Study on the Formation Mechanism of Active Species

A monocyclopentadienyl titanium complex containing 8-quinolinolato (QCpTiCl_2) was synthesized. Its activities in ethylene polymerization at various Al/Ti molar ratios, different temperatures and activation time were investigated. The activity with a Al/Ti molar ratio of 500 exhibited a maximum of 2.8×10~5 g/(mol.h) at 30℃. The activation time of QCpTiCl_2 with MAO before polymerization also plays a role on the activity. The structural properties of the produced polyethylene (molecular weight, molecular weight distribution and melting point) were discussed. Kinetic behaviors of ethylene polymerization with the QCpTiCl_2/MAO system at different Al/Ti molar ratios were studied. For the QCpTiMeCl/MAO system and the CpTiMe_2Cl/MAO system, binding energies of the examined intermediates were calculated by quantum-mechanical method based on ADF program, respectively. It is confirmed that the chlorinebridged adduct formed by the reaction of QCpTiMeCl with MAO is thermodynamically steady. In the case of the QCp     

Crystallographic report: Bis(µ2‐chloro)‐{bis(diethylether)‐lithium}‐bis(η5‐pentamethyl‐cyclopentadienyl)samarium(III)

The structure is mononuclear with samarium bound by two η⁵‐cyclopentadienyl ligands and two chloride ligands, the latter of which bridge to a doubly ether‐solvated lithium centre. Copyright © 2004 John Wiley & Sons, Ltd.     

Synthesis and Crystal Structure of [（ArO）2Sm（OPPh3）（μ—OH）]2（ArO=2,6—tBu—4—Me—C6H2O）

1 INTRODUCTION In recent years, the syntheses, structures and reactivities of aryloxo lanthanide complexes have attracted a great deal of attention due to their various applications as homogeneous catalysts for organic reactions and precursors for organolan- thanide syntheses[1]. However, the reactivity of divalent lanthanide aryloxides has seldom been studied[2]. We have previously reported that (ArO)2- Sm(THF)4 (ArO = OC6H2-2,6-di-tert-butyl-4-Me) can efficiently initiate the poly…     

Synthesis and Crystal Structure of Complex [Cdq3] [Cd（qH）3]（ClO4）CH3OH（q = 8-Quinolinolate, qH = 8-Quilinolinol）

1 INTRODUCTION 8-Quinolinolate is a very useful ligand and used to synthesize many complexes with special physical properties. For example, the complex tris(8-quinoli- nolate)aluminum(III) displays distinguished physical property in the area of electroluminescence ma- terials[1]. Based on tris(8-quinolinolate)aluminum(III), high-luminance low-voltage driven devices have been made, which opens the route to design low-cost large area displays and illuminators. The crystals thatcontain com…     

铜的喹哪啶配合物[Cu(Me-quin)2H2O]的合成、表征及晶体结构

本文合成了铜的喹哪啶配合物[Cu(Me-quin)     

Crystallographic report: Crystal structure of tris(2,6‐di‐tert‐butyl‐4‐methylphenolato‐O) (tetrahydrofuran‐O) erbium toluene solvate

A low‐coordinate aryloxo erbium complex, [(ArO)₃Er(THF)](MePh), has been synthesized by the reaction of anhydrous ErCl₃ with three equivalents of NaOAr in tetrahydrofuran. The central erbium atom is coordinated by three oxygen atoms of the aryloxo ligands and one oxygen atom of the tetrahydrofuran molecule, resulting in a distorted tetrahedron. Copyright © 2004 John Wiley & Sons, Ltd.     

双核Cd(Ⅱ)-8-喹啉氧基乙酸根离子配合物的合成与晶体结构

A novel cadmium(Ⅱ) complex with 8-quinolinyloxyacetate has been prepared and characterized by X-ray diffraction. The complex is a centrosymmetric [Cd₂L₂Cl₄(MeOH)₂] dinuclear structure and the Cd(Ⅱ) centre is in a distorted octahedron geometry. The crystal is in triclinic system, space group P1, with a=0.752 2(4) nm, b=1.043 1(5) nm, c=1.097 3(6) nm, α=66.11(2)°, β=72.48(2)°, γ=70.28(2)° and Z=1. The most striking feature of this complex is the formation of a 3D network bridged through the intermolecular N-H…O, O-H…O, C-H…O and C-H…Cl hydrogen bonds and stabilized via intermolecular π-π stacking interactions. CCDC: 224677.     

Crystal Structure of the Samarium Chlorosilicate Sm_3 (SiO_4)_2Cl

1INTR0DUCTIONSofarthreetyPesofstructuresoftherareearthchlorosilicateshavebeenreport-ed:La,(SiO')Cl,t"belongstoorthorhombicsystem,Ln3(SiO'),Cl(Ln=La,Pr)[z'sitomonoclinicsystem,Yb,(SiO'),Cl["toorth0rhombicsystem.WerecentlypreparedthesinglecrystalofSm,(SiO'),ClbyhightemperaturesolidstatereactionandvaportransP0rtmethod.Thoughthesamariumislightrareearthelement,thestructureisisostructuralwithYb,(SiO'),Cl.2EXPERmENTALThetitlecompoundSm,(SiO'),Clwasobtainedasanunexpectedcompoundina…     

二(甲基环戊二烯基)钐催化异氰酸苯酯齐聚的研究

研究了二（甲基环戊二烯基）铸催化异氰酸苯酯齐聚反应的性能,对引发反应过程和稀土配位环境的影响作了深入探讨。引发反应速率对表观催化活性影响很大。齐聚反应产物由甲醇不可溶与甲醇可溶两部分组成,其中甲醇不溶部分以二聚物为主,甲醇可溶部分以三聚物为主。ＳｍＩ２和ＳｍＩ２（ｈｍｐａ）４（ｈｍｐａ＝六甲基磷酰三胺）则对ＰｈＮＣＯ齐聚反应没有催化活性。     

Synthesis and Crystal Structure of Lanthanide Schiff Base Complex [2-OC6H4CHN（2,6-i-Pr2C6H3）]2ErCl（THF）

1 INTRODUCTION The Schiff base ligands have been used to provide a stereochemically rigid ligand framework in homogenous precatalysts of some metals, such as salen Cr catalysts in asymmetric ring-opening re- action of epoxide[1] and salen Al in ring-opening polymerization of lactide and related cyclic esters[2]. Recently, it was reported that the bidentate Schiff base complexes of early and late transition metals can be served as promising alternatives to metal- locene catalysts for th…     

Preparation of samarimm(ii) sulfide by the reaction of samarium(II) bis[bis(trimethylsilyl)amide] with hydrogen sulfide

X-ray amorphous samarium(II) sulfide was prepared by the reaction of H₂S with samarium(II) bis[bis(trimethylsilyl)amide] (1) in THF at 10^–2 Torr. Compound1 was prepared by two methods: 1) the reaction of SmI₂ with lithium bis(trimethylsilyl)amide and 2) the reaction of samarium naphthalide with bis(trimethylsilyl)amine. SmS was transformed to the polycrystalline state with the lattice parametera = 5.92 Å by annealing at 400–500 °C.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 241–243, February, 1995.     

二（2，6－二叔丁基－4－甲基苯氧基）钐配合物催化甲基丙烯酸甲酯聚合

二（２，６－二叔丁基－４－甲基苯氧基）钐配合物催化甲基丙烯酸甲酯聚合扈晶余，齐贵中（中国科学院长春应用化学研究所稀土化学与物理开放实验室长春１３００２２）沈琪（苏州大学化学系苏州）关键词钐配合物，甲基丙烯酸甲酯，聚合二价稀土有机化合物具有很强的还原性...     

(C8H8)Sm(C8H8)Na(THF)3的晶体结构

(C_8H_8)Sm(C_8H_8)Na(THF)_3的晶体属单斜晶系,P2_1空间群.晶胞参数为α=12.140(3),b=13.794(3),c=8.944(3)(?),β=111.68(3)°,V=1391.8(7)(?)~3,Z=2,μ=21.93cm~(-1),D_c=1.43g/cm~3,F(000)=610,Mr=598.0。结构经Patterson函数和Fourier技术解出并经最小二乘修正,最终的偏离因子R为0.046.配合物具有双层夹心结构.其中Sm~(3+)和Na~+通过η~8-环辛四烯基连接。     

双-(取代)硼酸)-2-(取代)-8-羟基喹啉酯的结构研究

有机硼化合物是元素有机化合物的一个重要类别,早在1940年 Kruger 就提出在蛋白质中引入一定浓度的硼来作为医学上的一种疗法。六十年代以来化学家们合成了许多含硼的     

Crystal Structure of 4, 5-trans-2-Amino-1, 3, 3-tricyano-4, 5-di (4-chlorophenyl)cyclopentene. Ethanol. Monohydrate

1mTRODUCT10NSincethetimeKaganhasdem0nstratedasimplepreparationofsamariumdiio-didefromsamariummetaland1,2-diiodoethanet1),SmI2hasbeenwidelyusedinsyntheticreactionst23.Thereactivityofsamariumdiiodidetowardsvariousnitrogen-containingcomP0undshasalreadybeenexamined.Thereare,toourknowledge,noliteratureexamplesforthereductionofcyanogrouptoproduceaminowiththisreagent.Inthispaper,wediscussedthecrystalstructureofthetitlecomP0undsyn-thesizedbythereactionofsamariumdii0didereagentwithp-chloroben-zyli…     

Crystal Structure of Di[bis(diphenylphosphino)propane]Copper(Ⅰ) Perchlorate Complex

1INTRODUCT1oNIthasbeenwellknownthatthereactionofcopper(E)saltswithditertiaryphosphinesorarsinesisoftenaconvenientroutetocopper(I)analogues.8-dimethylarsinoquinolinee,3-methylthiopropyldimethylarsineand(o-diphenylarsi-nophenyl)diphenylphosphinesulphideallonlyyieldcopper(I)complexesofthiskindofligandsfromreactioninvolvingcopper(I)salts.Insimilarmanner,copper(I)nitratecomplexesofstoichiometryCu(dppm)(NO,),Cu2(dppe)3(NO,)2,Cu-(dppe),(NO,),andCu(dppe)(NO,)havebeenprepared.ltappearsthatthe…     

{[Sm_2(Gly)_6(H_2O)_4](ClO_4)_6(H_2O)_5}_n的合成和晶体结构

本文合成了标题配合物,对其红外光谱进行了研究.测定了配合物的晶体结构,结果表明,晶体属三斜晶系,P1空间群,单胞参数:α=11.549(2)(?),b=14.122(3)(?),c=15.654(?),α=97.01(2)°,β=102.70(2)°,γ=105.43(2)°,V=2355.94(0.87)(?)~3,Z=2.晶体结构是采用Patterson法和差值Fourier合成解出.经全矩阵最小二乘法修正,最后偏差因子R=0.0337,R_w=0.0364.晶体中甘氨酸与Sm原子的结合方式有三种:第一种甘氨酸的羧基离子以螯合桥式与Sm原子配位;第二种甘氨酸以羧基桥式与同一单元的两个Sm原子配位;第三种甘氨酸以酸基桥式连结两个相邻单元中的相邻Sm原子而形成一维无限长链结构.此外,每个Sm原子还与两个水分子成键,其配位数为9.