双核配合物[Cu2(L-Asp)(phen)3(NO3)](NO3)·4H2O的合成及晶体结构

The new complex [Cu₂(L-Asp)(phen)₃(NO₃)](NO₃)·4H₂O (L-Asp=L-aspartic acid and phen=1,10-phenanthroline) has been synthesized and its crystal structure has been determined. The complex crystallizes in the monoclinic with space group P2₁/c, The cell parameters are: a=1.261 3(2) nm, b=1.500 8(4) nm, c=2.230 7(4) nm, β=99.55(1)°, and V=4.164 1(16) nm³，D_c=1.587 g·cm^-3. The complex contains two six-coordinated copper ions, and these two copper ions are connected together by L-aspartate to give rise to a binuclear structure. Hydrogen bonds and π-π stacking interactions are observed in the complex. CCDC: 249250.     

混合配体的铜(Ⅱ)配合［Cu(C2H4O2N)(C12H8N2)(H2O)］.ClO4.2.5H2O的合成、性质及晶体结构

本文对甘氨酸、1,10-邻菲咯啉铜(Ⅱ)固体配合物进行了合成和表征,并利用X射线分析研究了其晶体结构。     

配合物[Cu(H2O)(C12H8N2)2].2ClO4的合成、性质及晶体结构

合成了配合物[Cu(H2O)(C12H8N2)2]*2ClO4(C12H8N2为1,10-邻菲咯啉),用元素分析、摩尔电导、红外光谱及电子光谱进行了表征,并测定了配合物的晶体结构.该晶体属单斜晶系,空间群为CC;晶胞参数a=1.9177(2)nm,b=0.81994(0)nm,c=1.62458(14)nm,β=100.104(6)°;V=2.5419(4)nm3,Z=4,F(000)=1300,DC=1.693g/cm3,R=0.0430,wR=0.1195.中心铜(Ⅱ)离子与两个1,10-邻菲咯啉的四个N原子和一个水分子的氧原子配位,形成了一个变形的三角双锥结构.     

四元混配配合物[Ce(CH2=C(CH3)-COO)2(NO3)(phen)]2的合成、表征及晶体结构

A new complex with mixed-quadriligand [Ce(CH₂=C(CH₃)-COO)₂(NO₃)(phen)]₂ has been synthesized in aqueous solution of slight acidity and characterized by elementary analysis, IR and TGA. The crystal structure determination shows that the complex belongs to triclinic, space group P1, a=9.614?, b=10.047?, c=11.821?, Z=2, α=100.88(3)°, β=106.29(3)°, γ=97.93(2)°, V=1054(5)?³, D_c=1.741g·cm^-3, F(000)=546.00, μ(MoKα)=22.06cm^-1. And the crystal is consisted of a binuclear molecule. The coordina-tion of Ce³⁺ is nine.     

配合物[Mn(phendione)(PDC)(H2O)2]·2H2O的合成与晶体结构

The title compound [Mn(phendione)(PDC)(H₂O)₂]·2H₂O (H₂PDC=pyridine-2，6-dicarboxylic acid) has been prepared in aqueous solution and characterized by single X-ray diffraction structure determination， elemental analysis， IR spectroscopy， and thermal analyses. The compound crystallizes in Monoclinic system， space group C2/c， a=1.017 51(11) nm， b=1.483 25(11) nm， c=1.461 21(13) nm， β=109.86(10)°， V=2.074 1(3) nm³， Z=4， F(000)=1 028， μ=0.701 mm^-1， D_c=1.609 g·cm^-3， R₁=0.028 9， wR₂=0.078 8 [I>2σ(I)]. Crystal structure reveals that complex consists of one-dimensional chain framework bridged by hydrogen bonds that formed by uncoordinated water and oxygen atom of carboxyl group in PDC^2-. Furthermore， the complexes form a three-dimensional super-molecular structure through hydrogen bonds. CCDC: 648570.     

配合物[Sm(o-MOBA)3(phen)·H2O]2·4H2O的合成与晶体结构

The title complex [Sm(o-MOBA)₃(phen)·H₂O]₂·4H₂O has been synthesized by the reaction of SmCl₃·6H₂O with o-methoxybenzoic acid and 1,10-phenanthroline in 1∶3∶1 molar ratio. The crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to triclinic system, space group P1 with a=1.203(10) nm, b=1.293(10) nm, c=1.306(11) nm, α=64.50(10)°, β=81.93(10)°, γ=74.81(10)°. The molecular structure shows that the Sm³⁺ ion coordinates to nine atoms. The carboxylate groups are bonded to the samarium ion in three modes: monodentate, bidentate chelating, tridentate chelating-bridging. CCDC: 603740.     

配合物[La(pic)3(phen)2]·CH3CN的合成及晶体结构

The Lanthanum picrate complex with 1,10-phenanthroline was synthesized, whose chemical formula can be written in [La(pic)₃(phen)₂]·CH₃CN. The crystal Xray diffraction analysis shows that crystal belongs to monoclinic with space group P2₁/a and unit cell parameters:a=17.072(4),b=16.083(4),c=17.789(4),β=106.34(2)°,V=4687(4)³, Z=4,Dc=1.735g·cm³, μ=10.106cm¹,F(000)=2448,R=0.0589,Rw=0.0589. The coordination number of La³⁺ is nine. Acetonitrile, a solvent molecule is not coordinated. Between three Pic ligands, that possesses 2 bidentate forms six member ring with La. The other is unidentate ligand. As usually, phen is bidentate ligand.     

配合物[Mn2(α-Furacrylic radical)4(phen)2(H2O)]·H2O的合成、晶体结构及热稳定性

One novel manganese(Ⅱ) complex [Mn2(α-Furacrylic radical)4(phen)2(H2O)]·H2O with α-furacrylic acid radical and 1,10-phenanthroline has been synthesized and characterized. Crystal data for this complex:monoclinic,space group C2/c,a=1.082 34(16)nm,b=2.445 8(4) nm,c=1.857 4(3) nm,β=104.353(2)°,V=4.763 5(12) nm3,Dc=1.471 g·cm-3,Z=4,F(000)=2 168. Final GooF=1.004,R1=0.039 7,wR2=0.108 7. The crystal structure shows that two neighboring manganese(Ⅱ) ions are linked together by two bridging α-furacrylic acid radicals and one bridging water molecule,forming a cage structure. The Mn(1)…Mn(1A) bond distance is 0.357 6 nm. Each manganese(Ⅱ) ion is coordinated with two nitrogen atoms of one 1,10-phenanthroline molecule and four oxygen atoms from three α-furacrylic acid radicals and one water molecule,forming distorted octahedral coordination geometry. Thermal stability of the complex was also discussed.     

配合物[Cu2(C4H2O6)(Phen)2(H2O)]·8H2O的合成、晶体结构和抗菌活性

在pH≈10的乙醇-水溶液中以硫酸铜、酒石酸和邻菲咯啉反应合成了分子式为[Cu₂(C₄H₂O₆)(Phen)₂(H₂O)]·8H₂O的配合物单晶。用X-射线单晶衍射测定了晶体结构，并研究了配合物对大肠杆菌、金黄色葡萄球菌、枯草杆菌的抗菌活性。晶体属单斜晶系，空间群P2₁。标题化合物为双核铜配合物，2个铜原子配位数不同。Cu(1)是五配位的，具有扭曲的四方锥结构，5个配位原子分别是酒石酸的去质子的羟基氧和羧基氧、邻菲咯啉的2个氮原子及1个水分子的氧原子。Cu(2)为四配位的，配位原子分别是酒石酸的去质子的羟基氧和羧基氧和邻菲咯啉的2个氮原子。分子中Cu(1)…Cu(2)间的距离为0.354 8 nm。存在分子内邻菲咯啉-邻菲咯啉的面—面π-π相互作用，面间距为0.381 3 nm。配合物对大肠杆菌、金黄色葡萄球菌、枯草杆菌具有较强的抗菌活性。     

[Ag(4，4′-bpy)]+及[Zn(phen)2(H2O)2]2+两种配合物的合成、结构与荧光性质

用水热法和溶液法分别合成了2个新的配合物{[Ag(4,4′-bpy)]·3-HSBA.H2O}n(1)和[Zn(phen)2(H2O)2]·(A-2,5-DSA)·3H2O(2)(3-HSBA=3-羧基苯磺酸根,A-2,5-DSA=苯氨-2,5-二磺酸根,4,4′-bpy=4,4′-联吡啶,phen=1,10-邻菲咯啉),用X-射线单晶衍射结构分析方法测定了其晶体结构。配合物1是一维链状结构。在1个不对称单元中包含1个[Ag(4,4′-bpy)]+阳离子,1个3-羧基苯磺酸根阴离子和1个晶格水分子。Ag髣离子与2个4,4′-联吡啶的2个氮原子配位。配合物2是单核结构。在1个不对称单元中包含1个[Zn(phen)2(H2O)2]2+阳离子,1个苯氨-2,5-二磺酸根阴离子和3个晶格水分子。Zn髤离子与2个1,10-邻菲咯啉的4个氮原子和2个水氧原子配位。配合物1和2中,配位阳离子、抗衡阴离子以及晶格水分子之间存在丰富的氢键,进而构筑成超分子网络结构。配合物的荧光均来自于配体的π-π*电子跃迁。     

4-羧基苯氧乙酸锰配位聚合物[Mn(p-CPOA)(H2O)3]n的合成与晶体结构

The coordination polymer of [Mn(p-CPOA)(H₂O)₃]_n (p-CPOA=4-carboxylphenoxyacetate) was synthesized and characterized by elemental analysis, IR， X-ray single crystal diffraction. The title complex crystallizes in mono-clinic with space group P2₁/c, a=0.699 8(1) nm, b=1.6235(3) nm, c=1.014 3(2) nm, β=99.55(3)°. V=1.136 5(4) nm³, Z=4, D_c=1.772 g·cm^-3, μ=1.193mm^-1, F(000)=620, R=0.026 8, wR=0.074 5. The manganese atom is seven-coordinate involving four oxygen atoms of different p-CPOA^2- ligands and three coordinated water, forming a distorted pentagonal bipyramindal environment. Two manganese atoms are bridged by p-CPOA^2- ligand, forming a one-dimensional zigzag chain structure along p axis. The adjacent distance of Mn…Mn atoms is 1.021 0 nm. The three-dimensional hydrogen bonding network was formed by the intermolecular hydrogen bonds. CCDC: 219358.     

配合物[Mn(NPA)2(Phen)(H2O)2]的合成、晶体结构及热稳定性

合成了一个Mn(Ⅱ)的配合物[Mn(NPA)₂(Phen)(H₂O)₂](NPA=N-苯基代邻氨基苯甲酸，Phen=邻菲咯啉)，经红外光谱、紫外光谱、元素分析、差热，X射线单晶衍射等表征，其晶体结构为单斜晶系，C2/c空间群。标题配合物中的Mn原子与2个N-苯基代邻氨基苯甲酸的2个氧原子、1个Phen的2个N原子，2个水分子的氧原子形成六配位八面体结构。     

新配合物[Cd(H2O)2(phen)2](PA)2的制备及晶体结构

The new compound was prepared by the reaction of Cd(ClO₄)₂·6H₂O,1,10-phenanthroline (phen)and picric acid (HPA)(ratio 1∶3∶2) in methanol-aqueous solution refluxing for 4 hours. The crystals used for X-ray analysis was obtained by slow evaporation of the solution at room temperature. The crystal compound is in triclinic with space group with a=1.1363(4)nm,b=1.2593(2)nm,c=1.3972(4)nm,α=93.97(2)?,β=100.84(3)?,γ=106.29(2)?,Z=2,V=1.8690(9)nm³,D_c=1.715g·cm^-3, μ(MoKα)=0.677mm^-1,F(000)=972,R=0.0907,wR=0.2240. In the complex, the Cd(Ⅱ) cation is octahedrally coordinated to two 1,10-phenanthroline ligands and two water molecules in cis disposition. As outer sphere, picrate anions are combined with inner by hydrogen bond and static electricity interaction.     

[Mn(phen)3](ClO4)2(H2O)·0.5(azpy)的合成和晶体结构

锰在生物体系的新陈代谢过程中有重要作用。锰有机配合物的研究成为生物无机化学研究领域的一个热点[1]。本文报道用高氯酸锰、1,10 邻菲咯啉和4,4 偶氮联吡啶[2 4]合成的锰配合物[Mn(phen)3](ClO4)2(H2O)·0 5(azpy)的晶体结构。1　实验部分1 1　Mn(Ⅱ)配合物的合成将0 0724g(0 2mmol)Mn(ClO4)2·6H2O溶于8mL水,缓慢加入含有0 1190g(0 6mmol)1,10 邻菲咯啉(phen)和0 0277g(0 15mmol)4,4′ 偶氮联吡啶(azpy)的15mL甲醇溶液,搅拌0 5h,室温下静置,一周后得[Mn(phen)3](ClO4)2(H2O)·0 5(azpy)晶体。元素分析(计算值)/%:C54 19(54 …     

一维链状锰配位聚合物[Mn(C10H9O3)2(4，4′-bipy)(H2O)2]n的合成、晶体结构及荧光性质分析

锰元素不仅在生物化学的酶催化过程中扮演重要的角色[1-3],而且在合成分子磁体、开展多核间磁交换作用的研究方面也受到人们的关注[4-6],锰配合物的的研究已引起人们的极大兴趣.     

一维链状配位聚合物[M(H2bpb)(H2O)4](SO4)2·6H2O[M=Zn(Ⅱ)，Cu(Ⅱ)]的合成及晶体结构表征

设计并合成了一个含吡啶基团的柔性配体：N，N′-Bis(3-pyridylmethyl)-1，4-benzenedimethylamine(bpb)。通过bpb与硫酸锌及硫酸铜反应得到了两个新型具有一维链状结构的配位聚合物：[M(H₂bpb)(H₂O)₄](SO₄)₂·6H₂O[M=Zn(Ⅱ) 1，Cu(Ⅱ) 2]。X-射线晶体结构测定表明，这两个     

L-丙氨酸桥联配位聚合物[Cu2(L-ala)2(phen)2]n·2nClO4·2nH2O的合成及其结构

The complex, [Cu₂(L-ala)₂(phen)₂]_n·2nClO₄·2nH₂O(L-ala=L-alaninate, phen=1,10-phenanthroline) has been synthesized and investigated by elemental analysis, IR spectroscopy, and X-ray diffraction methods. The complex crystallizes in the monoclinic space group P2₁ with a=1.161 1(4) nm, b=0.717 2(2) nm, c=2.074 1(7) nm, β=101.028(6)°, V=1.695 4(9) nm³, D_c=1.760 g·cm^-3, Z=4, μ=1.493 mm^-1, F(000)=916, R=0.052 2, wR=0.127 9 for 7 131 unique reflections. The cations of [Cu₂(L-ala)₂(phen)₂]_n²ⁿ⁺ have an one-dimensional polymeric structure, due to the bridging of two Cu(phen)²⁺ units by a carboxylate group of L-alaninate, and each Cu(Ⅱ) ion is in a slightly distorted square-pyramidal coordination geometry, with the phen (N,N′) and the L-ala(N,O) acting as bidentate ligands in the equatorial plane and another carboxylate oxygen atom from a symmetry-related neighboring L-alaninate ion in the apical position. CCDC: 277541.     

配合物[Cu(m-TFBA)(phen)(H2O)2]·(m-TFBA)的水热合成、晶体结构及量子化学研究

以醋酸铜、间三氟甲基苯甲酸(m-TFBA)和邻菲咯啉(phen)为原料在甲醇水介质中通过水热反应,合成了一个新的单核 铜?髤配合物[Cu(m-TFBA)(phen)(H₂O)₂]·(m-TFBA),用元素分析、红外光谱和热重分析对配合物进行了表征。X-射线单晶衍射表明,配合物属三斜晶系,空间群P1,晶胞参数：a=1.001 61(10) nm,b=1.150 69(12) nm,c=1.286 49(12) nm,α=82.217(2)°,β=84.767(2)°,γ=66.371(2)°,V=1.344 8(2) nm³,Z=2,D_c=1.625 g·cm^-3,R₁[I>2σ(I)]=0.042 1,wR₂[I>2σ(I)]=0.095 8。铜(Ⅱ)分别与来自邻菲咯啉的2个氮原子、间三氟甲基苯甲酸的1个氧原子和2个水分子中的2个氧原子配位,形成变形的四方锥结构。配合物通过强的O-H…O氢键作用形成了二聚体结构,该二聚体又通过分子间弱的C-H…O氢键作用形成了一维链状结构。配合物中配位的间三氟甲基苯甲酸上的三氟甲基基团具有无序结构。对配合物中[Cu(m-TFBA)(phen)(H₂O)₂]⁺进行了量子化学从头计算,探讨了配合物的稳定性、分子轨道能量以及一些前沿分子轨道的组成特征。     

配合物[Mn(bipy)3](ClO4)2的晶体结构和热分析研究

The complex [Mn(bipy)₃]·(ClO₄)₂ was synthesied and characterized by X-ray diffraction. X-ray diffraction result for the single crystal showed that the crystal belongs to triclinic, space group P1, a=0.8123(2),b=1.1024(2), c=1.8646(4)nm,α=102.30(3)°,β=91.00(3)°,γ=99.69(3)°,V=1.6056(6)nm³,Z=2,D_c=1.494g·cm^-3. The thermal decomposition of [Mn(bipy)₃](ClO₄)₂ occurred in a three steps pattern. The reaction mechanism of the first step decomposition was deduced as n(1-α)[-ln(1-α)](n-1)/n with the activation energy of 130kJ·mol^-1.     

三维羧基氧桥联双核铜配合物[Cu2(nta)(Phen)3]NO3·6H2O的合成、表征与晶体结构

由H₃nta(H₃nta=nitriloriacetic acid)、Phen(Phen=1,10-phenanthroline)与Cu²⁺离子反应,合成标题配合物[Cu₂(nta)(Phen)₃]NO₃·6H₂O。该配合物的晶体属单斜晶系,空间群为P2₁/c。在配合物中,2个中心铜原子分别与配位原子构成变形八面体和变形三角双锥结构。晶体中结构单元通过分子间氢键和π-π堆积,形成了三维网络结构。TG分析结果表明标题配合物在194 ℃以下是稳定的。