配合物Nd(C7H7N2O2)3(H2O)3的合成及其晶体结构

用水热法合成了3,5-二氨基苯甲酸与Nd(Ⅲ)的配合物Nd(C7H7N2O2)3(H2O)3(1),其结构经IR,元素分析和X-射线单晶衍射仪表征。1为单核结构,属六方晶系,R3空间群,晶胞参数:a=1.887 29(18)nm,b=1.887 29(18)nm,c=0.603 53(12)nm,β=90,°γ=120°,V=1.861 7(4)nm3,Z=3,μ=2.154 mm-1,Dc=1.744 g.cm-3,R1=0.014 3,wR2=0.033 2。1中Nd(Ⅲ)与来自3个3,5-二氨基苯甲酸的6个氧原子及3个配位水的氧原子进行配位,形成9配位化合物。     

配位聚合物[Zn(3-aba)2]n·nH2O和[Cd(3-aba)2]n的合成与晶体结构

用水热法合成了2个新的配位聚合物[Zn(3-aba)₂]_n·nH₂O (1)和[Cd(3-aba)₂]_n (2)(3-aba=间氨基苯甲酸阴离子)，对它们进行 了元素分析、热分析、红外光谱和X射线单晶衍射等表征。配位聚合物1晶体属正交晶系，Pca2₁空间群，晶体学数据为：a=0.926 26(8) nm，b=1.600 73(15) nm，c=1.885 22(17) nm，β=90°，V=2.795 2(4) nm³，Z=4，μ=1.783 mm^-1，D_c=1.690 g·cm^-3，R₁=0.027 9，wR₂=0.064 8；配位聚合物2晶体属单斜晶系，P2₁/n空间群，晶体学数据为：a=0.900 68(7) nm，b=0.452 03(4) nm，c=1.568 02(12) nm，β=106.075 0(10)°，V=0.613 43(9) nm³，Z=1，μ=1.799 mm^-1，D_c=2.082 g·cm^-3，R₁=0.019 8，wR₂=0.055 8。在配合物1中，配体分子以双齿配位模式与锌离子配位，而在配合物2中，它以三齿配位模式与镉离子配位。2个配合物均具有二维网状结构。     

Schiff碱钼(Ⅵ)配合物的合成、谱学研究与晶体结构

通过水杨醛与乙醇胺(或邻氨基酚)和乙酰丙酮氧化钼在无水乙醇中反应得到双核配合物1[MoO2·SAE]2(SAE为N-亚水杨醛基-2-氨基乙醇)和单核配合物2[MoO2·SAP·(C2H5OH)](SAP为N－亚水杨醛基-2-氨基苯酚)。并用元素分析,IR,1^HNMR和热分析进行表征,测定了配合物1的单晶结构。1晶体属正交晶系,空间群为Pbca.晶胞参数:a=1.31007(16)nm,b=0.89636(11)nm,c=1.6841(2)nm,Mr=582.22,V=1.9777(4)nm^3,Z=4,Dc=1,955Mg/m^3,R1=0.0293,ωR2=0.0819.$521Thereactionofsalicylalwith2-aminoethenol(or-2-aminophenol)and[MoO2(acac)2])acac=acetylacetonate)inabsoluteethanolgavedinuclearmolybdenumcomplex1[MoO2·SAE]2(SAE=N-salicylidene-2-aninophenol).andmononuclearcomplex2[MoO2·SAP·(C2H5OH)](SAP=N-salicylidene-2-aminophenol).Theyhavebeencharacterizedbyelementalanalysis,IR,1^HNMRandTGA.Thesinglecrystalstructureofcomplex1hasbeendetermined.Itbelongstoorthorhombic,spacegroupPbcawitha=1.31007(16)nm,b=0.89636(11)nm,c=1.6841(2)nm,Mr=582.22,V=1.9777(4)nm^3,Z=4,Dc=1,955Mg/m^3,R1=0.0293,ωR2=0.0819.     

Synthesis and Crystal Structure of [H-amp]4[Mo8O26(DMF)2]·2H2O (amp = 2-Amino-6-methyl-pyridine)

The reaction of MoO2(acac)2 with 2-amino-6-methyl-pyridine (amp) in the mixed solvent of DMF (N,N-dimethylformamide) and water affords the title complex [H-amp]4- [Mo8O26(DMF)2]·2H2O which was characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction analysis with the following crystallographic data: C30H54Mo8N10O30, Mr = 1802.35, monoclinic, P21/n, a = 8.631(1), b = 24.260(3), c = 13.351(2)A,β= 104.688(3)°, V = 2704.2(7) A3, Z = 2, Dc = 2.213 g/cm3, μ =1.890 mm－1 and F(000) = 1760. The final R = 0.0281 and Wr = 0.0620 for 4935 observed reflections with I > 2σ(I). X-ray structure analysis has confirmed the existence of γ-[Mo8O26]4－ anion in the molecule. Eight MoO6 distorted octahedra share edges with short terminal Mo-O bonds from 1.691(3) to 1.749(2)A, medium bonds from 1.868(2) to 1.965(2) A And long bonds from 2.059(2) to 2.450(2) A. In the terminal site there exist two DMF ligands bound to the Mo atom through O atoms with the Mo-ODMF bond length of 2.166(3) A, affording a bond strength of 0.433. A three-dimensional network structure was formed through hydrogen bonds.     

含异烟酸和2,6-二羧酸吡啶的双核铜(Ⅱ)配合物合成和晶体结构

用水热法合成了含2,6-二羧酸吡啶和异烟酸的双核铜(Ⅱ)配合物[Cu2(pydca)2(Hinic)2- (H2O)2]3H2O (H2pydca = 2,6-二羧酸吡啶, Hinic = 异烟酸), 并通过X射线单晶衍射测定其结构。晶体属三斜晶系, Pi空间群, 晶胞参数:a = 0.72375(10), b = 1.22205(17), c = 1.7078(2) nm, a = 90.463(2), b = 91.830(2), g = 93.563(2), V = 1.5067(4) nm3, Dc = 1.749 g/cm3, (C26H26Cu2N4O17) (Mr = 793.59), Z = 2, F(000) = 808, m = 1.501 mm-1, R = 0.0259, wR = 0.0741。配合物中1个铜(Ⅱ)离子配位数为5, 配位多面体为畸变的四方锥构型;另一个铜(Ⅱ)离子配位数为6, 配位多面体为畸变的八面体构型。配合物分子之间通过氢键连接, 形成三维网状结构。     

稀土与N-对甲基苯磺酰甘氨酸和邻菲咯啉配合物的合成与晶体结构

Three new lanthanide complexes with the formulae [Eu2（TsGly）6（phen）2（H2O）2] （1）, [Ln（TsGly）2（phen）2-（H2O）2]C1·2H2O [Ln=Er（2a） and Yb （2b）, TsGly=N-p-tolylsulfonylglycinate, phen= 1,10-phenanthroline] were synthesized. Crystallographic data for 1： monoclinic, P21/n, a= 1.29791（16） nm, b= 1.9034（2） nm, c= 1.7596（2） nm,β=93.410（3）°, V=4.3394（9） nm^3, Z=4, R1 =0.0326, wR2=0.0771; and for 2b： triclinic, P1, a= 1.2674（2） nm, b= 1.4405（2） nm, c= 1.4809（3） nm, a= 113.256（3）°, β= 108.253（3）°, γ=94.739（3）°, V=2.2922（7） nm°3, Z=2, R1=0.0292, wR2=0.0669. X-ray diffractional analysis reveals that compound 1 adopts dinuclear structure with fourfold bridging TsGly ligands between the Eu（Ⅲ） centers, while compound 2b features an unusual mononuclear structure.     

微波载银对纳米二氧化钛相变及光催化性能的增效作用

用微波法制备系列载Ag纳米TiO2,发现微波载Ag对纳米TiO2的相变和光催化活性具有增效作用。采用X-射线粉末衍射(XRD),透射电镜(TEM),X-射线光电子能谱仪(XPS),激光Raman光谱及漫反射光谱(DRS)方法对比研究纳米TiO2与载Ag纳米TiO2的性质。结果表明,所制得载Ag纳米TiO2是以锐钛矿为主相的混晶,平均粒径约为10 nm,负载Ag促进纳米TiO2中锐钛矿相转化金红石相相变,减小纳米晶尺寸,并使纳米TiO2光响应范围向可见光区移动 6 nm。在低浓度范围,微波法能均匀地将Ag负载于纳米TiO2表面,并以Ag0/Ag+的形式存在,抑制光生电子与光生空穴复合,大大地提高了纳米TiO2光催化活性。在近紫外-可见光照射下,载Ag量为0.05 mol %的纳米TiO2对罗丹明B的光催化降解效果最好。     

Syntheses and Crystal Structures of Cobalt(II) and Nickel(II) Coordination Polymers with 3-Aminobenzoic Acid Ligand

1 INTRODUCTION Much research interest has been focused on metal- organic coordination polymers in past years because of the structural and topological novelty of these compounds and their potential applications as func- tional materials, such as catalyst, ion-exchange, gas sorption, optical material and molecule-based ma- gnet[1~6]. In this field, many organic bridging ligands such as bipyridine, polyaromatic carboxylate and re- lated species have been used to produce various types of met…     

两种含氨基吡啶衍生物铜(Ⅱ)配合物的合成和晶体结构

Copper(Ⅱ) complexes Cu(C₆H₆N₂)₂(ClO₄)₂ (1) and Cu₂(OAc)₄(C₅H₅ClN₂)₂ (2) with amino-pyridine deriva-tives ligands have been synthesized and characterized by elemental analysis and IR spectrum. Their crystal struc-tures are determined by X-ray diffraction method. Compound 1， C₁₂H₁₆C₁₂CuN₄O₈， M_r=478.73， triclinic， space group ， a=0.7641(1)nm， b=0.7987(1)nm， c=0.7990(1)nm， α=106.78(1)°，β=95.71(1)°， γ=108.85(1)°， V=0.4317(1)nm³， Z=1， D_c=1.841g·cm^-3， μ=1.627mm^-1， F(000) =243，R₁=0.0264， ωR₂=0.0641 (I>2σ(I)). In 1， the center metal ion Cu(Ⅱ) possesses distorted octahedral geometry. Compound 2， C₁₈H₂₂C₁₂Cu₂N₄O₈， M_r=620.38，monoclinic， space group C2/c， a=1.9888(3)， b=0.9158(1)， c=1.4241(2)nm， β=115.89(1)°， V=2.3336(5)nm³， Z=4， D_c=1.766mg·cm^-3， μ=2.104mm^-1， F(000)=1256， R₁=0.0263， wR₂=0.0676 (I>2σ(I)). Compound 2 is dinuclear structure， in which each Cu(Ⅱ) adopts five-coordinated distorted square pyramid geometry. CCDC： 193109; 193110.     

4,4′-联吡啶锌(Ⅱ)配合物的合成及其晶体结构

苦味酸锌与4,4'-联吡啶反应,得到一种新型配合物[Zn(4,4′-bpy)2(H2O)2](pic)2@2H2O(4,4′-bpy4,4′-联吡啶,pic-苦昧酸根),并用元素分析、红外光谱等进行表征.X-射线单晶衍射结果表明,晶体属单斜晶系,空问群Cc,晶胞参数a=1.4390(2),b=1.1418(1),c=2.2908(3)nm,β=95.08(1)°,V=3.749(1)nm3,Z=4该配合物由4,4′-联吡啶与金属配位形成多孔的二维网,二维网再由未配位的水分子及苦味酸根离子通过氢键作用沿a轴方向堆积得三维网状结构,且未配位的水分子、苦味酸根离子被包合在网络之中,展示出一定的包合现象.