Synthesis and Features of Crystal Structure of Scandium Hexa(isothiocyanato)chromate(III) Complex with Nicotinic Acid

A double complex compound with a polymeric cation of composition [Sc₂(C₆H₅NO₂)₃(C₆H₄NO₂)₃][Cr(NCS)₆] has been synthesized by the reaction between Sc(NO₃)₃, K₃[Cr(NCS)₆], and nicotinic acid (C₅H₅NCOO) in an aqueous solution and studied by chemical analysis, IR spectroscopy, and X-ray diffraction. Crystals are hexagonal, space group P6₃22, Z = 2; a = 12.995(2) Å, c = 17.864(3) Å, V = 2612.3(7) Å3, ρ_calc = 1.559 g/cm³.     

Hexa(isothiocyanato)chromate(III) Hydro-Bis(Pyridine N-Oxide) Complex: Synthesis and Crystal Structure

A new complex of hexa(isothicyanato)chromate(III) hydro-bis(pyridine N-oxide) [(Py)₂H]₃[Cr(NCS)₆] was synthesized and studied by X-ray diffraction analysis. The coordination polyhedra of Cr atoms are the perfect octahedra that form the layered structure. Molecules of pyridine N-oxide form bimolecular cationic associates that compensate the charge on the complex anions. The crystals are triclinic: a = 11.559(2) Å; b = 12.644(3) Å; c = 16,110(4) Å; = 90.02(2)°; = 95.15(2)°; = 98.23(2)°; V = 2320.6(9) ų; _calcd = 1.394 g/cm³. Z = 2, space group P1¯.     

Mixed-Ligand Europium(III) Complexes with 4-Methylbenzoic Acid

Russian Journal of General Chemistry - Europium(III) complexes with p-methylbenzoic acid and nitrogen- or phosphorus-containing neutral ligand with the compositions [Eu(p-MBA)3·D]2·xH2O...     

茂铁基稀土铈配合物的合成与结构

本文利用单羧基二茂铁Fc-COOH和1，1′-二羧基二茂铁HOOC-Fc-COOH作为配体分别合成了双核铈配合物Ce₂(FcCOO)₆ (1)和二维层状配位聚合物Ce₂(OOC-Fc-COO)₃(2)，测定了两种配合物的晶体结构。配合物1中的金属铈离子为九配位结构，分别与周围的羧基二茂铁上的氧原子和作为辅助配体的水分子配位，茂铁间的π-π相互作用将配合物1的二聚体单元连结在一起形成二维的网状结构。配合物2中的金属铈离子亦为九配位结构，分别与周围的羧基二茂铁上的氧原子，作为辅助配体的水分子和甲醇配位形成类似于配合物1的二聚体单元，1，1′-二羧基二茂铁HOOC-Fc-COOH作为桥基配体将二聚体单元连结在一起，形成二维网状的配位聚合物。     

Luminescence Spectral Properties of Europium(III) and Terbium(III) Complexes with Cinnamic Acid

Europium and terbium mixed-ligand complexes with cinnamic acid of composition Ln(Cin)₃· nD · xH₂O, where Ln = Eu³⁺or Tb³⁺, Cin is a cinnamate ion (C₆H₅CH=CHCOO^–), D = 1,10-phenantroline, 2,2"-dipyridyl, benzotriazole (n= 2, x= 0), triphenylphosphine oxide (n= 1, x= 2), or H₂O (n= 0 or 1, x= 0), were synthesized. The compounds were characterized by elemental analysis, IR and luminescence spectroscopy. The Stark structure of the ⁵ D ₀–⁷ F _j(j= 0, 1, 2) electronic transitions in the low-temperature luminescence spectra of europium complexes was analyzed. IR study has revealed a bidentate coordination of the cinnamate ion in the compounds.     

Synthesis, Characterization and Crystal Structures of Lanthanide Phenoxyacetate Complexes with 1,10-Phenanthroline

IntroductionTherehasbeenconsiderableinterestinthecoordinationchemistryoflanthanidecomplexeswithcarboxylateligandsduetotheirpotentialapplicationinmolecularassembliesandluminescentprobesinsystemsofbiologicalrelevance .1 4 Ofthenumerouslanthanidecomplexesthathavebeenwidelystudied,5 9mostofthemarefoundtoexhibitavarietyofdimericorinfinitechainstructure.RecentlywehavereportedpolymericLu(POA) 3(phen)compoundinwhichlutetiumionsforminfinitechainalongtheb axisdirectionthroughthecoordinationofbridgingc…     

两个双核铁（Ⅲ）和三足配体的配合物的合成和晶体结构

运用三足四齿配体三（2－甲基吡啶）胺（TPA）或三（2－甲基苯丙咪唑）胺（TBA）,得到两个双核铁(III)配合物，[Fe₂L₂(μ₂-O)(μ₂-p-NH₂-C₆H₄COO)]³⁺ (L = TPA, 1 和 L = TBA, 2)。两个配合物均为单斜晶系，空间群为P2(1)/c.晶胞参数 1: a = 1.4529(4), b = 1.6622(5), c = 2.0625(6) nm, β= 100.327(5)º, V = 4.900(3) nm³, z = 4, F(000) = 2344, 分子量M_r = 1142.91, Dc = 1.549 g/cm³, R₁ = 0.0544, R₂ = 0.0962. 2: a = 1.3378(4), b = 2.1174(7), c = 2.4351(7) nm, β= 97.315(6)º, V = 6.842(4) nm³, z = 4, F (000) = 3116, 分子量M_r = 1505.08, Dc = 1.444 g/cm³, R₁ = 0.0793, R₂ = 0.1623. 在两个双核铁(III)配合物中，中心的三价铁和配体TPA或TBA上的四个氮原子和两个氧原子通过不同的桥形成一个畸变的八面体构型。     

Thermal and Spectral Studies of Y(III) and Lanthanide(III) Complexes with Mesaconic Acid

Y(III) and lanthanide(III) mesaconates were prepared as crystalline solids with general formula Ln₂(C₅H₄O₄)₃⋅nH₂O, where n=7 for La−Pr, n=4 for Y,Nd−Ho, n=8 for Er−Lu. IR spectra of the prepared mesaconates suggest that carboxylate groups are bidentate bridging anf chelating. During heating the hydrated complexes are dehydrated in one (Y, Nd−Lu) or two steps (La−Pr) and then decompose directly to oxides (Y, Ce, Pr, Sm, Gd−Lu) or with intermediate formation Ln₂O₂CO₃ (La, Nd, Eu). This revised version was published online in August 2006 with corrections to the Cover Date.     

Syntheses and Crystal Structures of Lanthanide Chloride Complexes with Diglyme

Reactions of [LnCl₃(DME)₂] (Ln = Nd, Sm, Ho, Lu; DME = dimethoxyethane) and diglyme (diglyme = diethylen glycol dimethyl ether) in THF resulted in polymeric [LnCl₃(diglyme)]_n (Ln = Nd ( 1 ), Sm ( 2 )) or mononuclear complexes [LnCl₃(diglyme)(THF)] (Ln = Ho ( 3 ), Lu ( 4 )). Neodymium and samarium atoms in 1 and 2 are eight‐coordinated by three oxygen atoms from diglyme, one terminal and four bridging chloride ions. Holmium and lutetium atoms in 3 and 4 are seven‐coordinated by three oxygen atoms from diglyme, three chloride ions and one oxygen atom from THF. [ErCl₃(diglyme)(H₂O)] ( 5 ) resulted from the reaction of ErCl₃·6H₂O, (CH₃)₃SiCl and diglyme in THF. The molecular structures of 3 , 4 and 5 are similar, with either a molecule of THF coordinated to the lanthanide atom in 3 and 4 or with a molecule of water coordinated in 5 .     

Spectroscopic and Crystal Structure of Europium(III) Picrate Complexes with Novel BINOL Derivatives

Two novel ligands N‐Benzyl‐2‐{2′‐[(benzyl‐phenyl‐carbamoyl)‐methoxy]‐[1,1′]binaphthalenyl‐2‐yloxy}‐N‐phenyl‐acetamide (L1) and N‐Methyl‐2‐{2′‐[(methyl‐phenyl‐carbamoyl)‐methoxy]‐[1,1′]binaphthalenyl‐2‐yloxy}‐N‐phenyl‐acetamide (L2), and their europium(III) complexes with picrate, [Eu(pic)₃(L1)] and [Eu(pic)₃(L2)], were synthesized and characterized by elemental analysis, IR, UV‐Vis and fluorescence spectroscopy. The crystal structure of [Eu(pic)₃(L1)]·2CHCl₃ was determined by single crystal X‐ray diffraction. The europium atom is coordinated by nine oxygen atoms of four from the L1 and five from two bidentate and one unidentate picrates. The fluorescent intensity of [Eu(pic)₃(L2)] is about 2.6 times that of [Eu(pic)₃(L1)] in solid states. But in CHCl₃ solution, the fluorescent intensity of [Eu(pic)₃(L1)] is stronger slightly than [Eu(pic)₃(L2)].     

三种新的铕(III)三元配合物的合成及发光性质研究

合成了吡嗪 [2 ,3 f]并邻菲罗啉及其一系列衍生物 ,作为第二配体 ,并以二苯甲酰甲烷为第一配体 ,合成了 3种新的铕 (III)三元配合物 .通过元素分析、红外光谱、核磁共振光谱确定了它们的组成 ,研究了三种配合物的热稳定性、成膜性能和光致发光性能 (发光强度、荧光量子效率和寿命 ) ,并初步从理论上探讨含有不同基团的第二配体的结构对铕 (III)配合物发光的影响 ,结果表明 :这三种铕 (III)三元配合物均为优良的红色发光材料 ,而且在真空条件下均形成均衡的薄膜 ,这为以这三种铕 (III)配合物作为发光层材料制作有机电致发光器件提供了认识基础     

两个外消旋双U形稀土单核配合物的合成、晶体结构及其表征

对氨基苯磺酸(p-AbsH),邻菲咯啉(phen)与稀土硝酸盐在pH=6～7的水溶液中反应,合成了2个新颖的双U形单核配合物[Ln(O-p-Abs)₂(phen)₂(H₂O)₃](NO₃)·2H₂O,其中Ln=La(1)和Ce(2)。X-射线单晶结构测定表明,2种晶体属异质同晶,正交晶系,Pccn空间群。在2个配合物中,Ln(Ⅲ)离子与5个O原子和4个N原子配位,形成1个畸变的三冠三棱柱体LnN₄O₅配位多面体,其中2个氧原子来自于2个对氨基苯磺酸根的磺酸基,另3个O原子则由配位水分子提供,4个N原子来自2个Phen。p-Abs与phen通过π-π作用构成具有手性的螺旋双U形结构,每个晶胞中含有2对构型相反的[Ln(O-p-Abs)₂(phen)₂(H₂O)₃]⁺,整个晶体呈外消旋,2种异构体分子间通过phen间的π-π作用构成超分子螺旋链,并通过氢键作用形成三维超分子结构。     

萘咪唑类稀土配合物的晶体结构和荧光性质

通过2-（2''-羟基-3''-甲氧基）萘咪唑（HL）和Ln（NO）₃·6H₂O反应,合成了4种单核稀土配合物[Ln（HL）₂（NO₃）₃]·CH₂Cl₂（Ln=Sm（1）,Eu（2）,Tb（3））和[Ln（HL）₂（NO₃）₂（CH₃OH）]NO₃·CH₃OH（Ln=Yb（4））。X射线单晶衍射分析表明配合物1~4均通过配体萘环间的π-π作用呈现蝴蝶状结构。荧光性质表明仅有配合物4显示Yb³⁺稀土离子的特征发光,固态和在乙腈溶液中的荧光寿命分别为8.27 μs和4.40 μs。     

萘咪唑类稀土配合物的晶体结构和荧光性质

通过2-（2’-羟基-3’-甲氧基）萘咪唑（HL）和Ln（NO）3·6H₂O反应,合成了4种单核稀土配合物[Ln（HL）₂（NO₃）₃]·CH₂Cl₂（Ln=Sm（1）,Eu（2）,Tb（3））和[Ln（HL）₂（NO₃）₂（CH₃OH）]NO₃·CH₃OH（Ln=Yb（4））。X射线单晶衍射分析表明配合物1~4均通过配体萘环间的π-π作用呈现蝴蝶状结构。荧光性质表明仅有配合物4显示Yb³⁺稀土离子的特征发光,固态和在乙腈溶液中的荧光寿命分别为8.27 μs和4.40 μs。     

Synthesis,Crystal Structures,and Antibacterial Activity of Manganese(III) Complexes with Schiff Bases

Russian Journal of Coordination Chemistry - Two new manganese(III) complexes, [MnL1(EtOH)(Acac)] (I) and [MnL2(DMF)(Esal)] · H2O (II), where L1 and L2 are the dianionic form of...     

5，6-二羧基苯并咪唑双核铕配合物的合成、结构及荧光性能

A europium complex [Eu₂(bmd)₂(Hbmd)₂(H₂O)₈]·8H₂O (H₂bmd=Benzimidazole-5,6-dicarboxylic acid) has been synthesized and structurally determined by X-ray diffraction single crystal structure analysis. The crystal belongs to triclinic, space grounp P1, with a=0.754 49(15) nm, b=1.253 8(3) nm, c=1.405 8(3) nm, α=71.03(3)°, β=82.83(3)°, γ=79.12(3)°, V=1.232 1(5) nm³, Z=1. The complex is a binuclear compound and each Eu(Ⅲ) ion is nine-coordinated. The versatile hydrogen bonds link binuclear units into a three-dimensional (3D) supermolecular network. Furthermore, the fluorescent properties of the complex have been investigated at room temperature. CCDC: 742510.     

3,4'-联苯二甲酸与含氮配体构筑的镧系配合物的合成、晶体结构及荧光传感

通过水热方法合成了2个镧系配合物,[Gd(3,4′-dpdc)_2(HDPP)]_n(1)和{[Dy(3,4′-Hdpdc)_3(H_2O)]·0.5BTB}_n(2)(3,4′-H_2dpdc=3,4′-联苯二甲酸,DPP=1,3-二(4-吡啶基)-丙烷,BTB=1,4-二(1,2,4-三氮唑)-1-丁烷),通过X射线单晶衍射对其结构进行表征。配合物1属单斜晶系,P2_1/c空间群。该配合物为二维层状结构,中心Gd(Ⅲ)离子的配位环境为[GdO_7N]。3,4′-dpdc配体以μ_1∶η~1η~1/μ_2∶η~1η~1和μ_1∶η~1η~1/μ_1∶η~1η~0两种方式桥联Gd(Ⅲ)离子,而HDPP配体是以端基的形式配位于Gd(Ⅲ)离子。配合物2属三斜晶系,P1空间群。配合物2具有一维链状结构,Dy(Ⅲ)离子的配位环境为[Dy O7]。3,4′-Hdpdc配体以μ_2∶η~1η~1配位模式链接相邻的Dy(Ⅲ)离子。未参加配位的BTB通过氢键与一维链连接,进而形成三维超分子结构。固态光致发光测量表明,化合物1和2在350~650 nm范围内显示出宽峰,归因于配体的π*→π跃迁。进一步研究了水溶液中不同沙星类药物对配合物1的发光的影响,实验结果表明该配合物可以识别培氟沙星。     

Synthesis and Crystal Structures of Antimony(III) Complexes With a Bis(amino)silane Ligand

Bis(amino)silane bearing bulky substituents on nitrogen, LH₂ [L = Me₂Si(NDipp)₂, Dipp = 2, 6‐diisopropylphenyl] was reacted with nBuLi (ratio 1:1 and 1:2) in toluene. The Me₂Si(LiNDipp)₂ was treated with SbCl₃ in a 1:1 ratio to yield the four‐membered SiN₂Sb ring compound of composition [η²(N,N)‐Me₂Si(NDipp)₂SbCl] ( 1 ). The mono lithiated bis(amino)silane was used to synthesize the monodentate heterotetraatomic complex [(η¹‐Me₂SiNDipp)NHDippSbCl₂] ( 2 ) by the reaction with SbCl₃. The complexes were characterized by ¹H and ¹³C NMR, elemental analysis, IR, and single‐crystal X‐ray structural analysis.     

Thermal and Spectral Features of Yttrium and Heavy Lanthanide Complexes with 2,4-dimethoxybenzoic Acid

The complexes of yttrium and heavy lanthanides with 2,4-dimethoxybenzoic acid of the formula: Ln(C₉H₉O₄)₃×nH₂O, where Ln=Tb(III), Dy(III), Ho(III), Er(III), Tm(III), Yb(III), Lu(III) and Y(III), n=2 for Tb(III), Dy(III), Ho(III), Er(III), Tm(III) and Y(III), and n=0 for Yb(III) and Lu(III), have been synthesized and characterized by elemental analysis, IR spectroscopy, themogravimetric studies, as well as X–ray and magnetic susceptibility measurements. The complexes have a colour typical of Ln ³⁺ salts (Tb, Dy, Tm, Yb, Lu, Y – white, Ho – cream, Er – pink). The carboxylate group in these complexes is a bidentate, chelating ligand. The compounds form crystals of various symmetry. 2,4-Dimethoxybenzoates of Yb(III) and Lu(III) are isostructural. 2,4-Dimethoxybenzoates of yttrium and heavy lanthanides decompose in various ways on heating in air to 1173 K. The hydrated complexes first lose water to form anhydrous salts and then decompose to the oxides of respective metals. The ytterbium and lutetium 2,4-dimethoxybenzoates decompose in one step to form Yb₂O₃ and Lu₂O₃. The solubilities of the 2,4-dimethoxybenzoates of yttrium and heavy lanthanides in water and ethanol at 293 K are of the order of: ^10–3 and 10^–3 –10^–2 mol dm^–3, respectively. The magnetic moments for the complexes were determined over the range of 77–298 K. They obey the Curie–Weiss law. The results show that there is no influence of the ligand field on the 4f electrons of lanthanide ions. This revised version was published online in August 2006 with corrections to the Cover Date.