Synthesis, structure and magnetic properties of the one-dimensional bimetallic oxide [Cu(terpy)Mo2O7]

The hydrothermal reaction of Cu(CH₃CO₂)₂·H₂O, Na₂MoO₄ and terpyridine at 140 °C for 48 h yields [Cu(terpy)Mo₂O₇] (1), a bimetallic one-dimensional oxide. The structure consists of ruffled chains of edge- and corner-sharing {MoO₅} square pyramids, decorated with {CuN₃O₂} ‘4+1’ axially distorted square pyramids. The Cu(II) polyhedra are disposed so as to produce an alternating pattern of Cu-Cu distances across the {Mo₂O₂} rhombi of the chain of 6.25 and 6.82 Å. This structural feature is reflected in the magnetic properties which are characteristic of a dimer rather than a linear chain, consistent with an alternating antiferromagnetic Heisenberg chain.     

有机-无机杂化材料[Na2(H2O)4]2[γ-Mo8O26·(Gly-Gly)2]·4H2O的合成及晶体结构

多金属氧酸盐因其独特的结构而具有较高的抗肿瘤及抗病毒活性,蛋白质和肽是氨基酸的聚合体,氨基酸侧链官能团能与多金属氧酸盐形成新型配合物.了解氨基酸和肽与多金属氧酸盐的相互作用对于深入研究多金属氧酸盐抗肿瘤及抗病毒机理很有意义.我们曾报道了赖氨酸、丙氨酸及甘氨酸二肽与钼磷酸所形成化合物的晶体结构.     

单核铜配合物[Cu~(II)(HIPP)(pydc)(H_2O)]的合成和晶体结构

用溶剂热合成方法合成了一个单核铜配合物CuII(HIPP)(pydc)(H2O),采用元素分析法和X射线单晶衍射法对该配合物的组成和结构进行了表征.配合物CuII(HIPP)(pydc)(H2O)属于正交晶系,空间群是Pbca.a=0.663 93(18)nm,b=2.062 2(6)nm,c=2.619 1(7)nm,α=90°,β=90°,γ=90°,V=3.585 9(17)nm3,Z=8,ρc=1.693g·cm-3,F(000)=1 864,GOF=0.882,R1=0.037 4,wR2=0.111 8[I2σ(I)].中心铜原子与配体脱质子2,6-吡啶二甲酸的2个羧基氧原子和1个氮原子、HIPP的1个氮原子和1个氧原子及1个水分子中的氧原子形成六配位的变形八面体.结构分析表明晶体中分子间含有氢键.     

Organic‐Inorganic Hybrids: Preparation and Structural Characterization of (Bu4N)2[Mo6O17(NAr)2] and (Bu4N)2[Mo6O18(NAr)] (Ar = o‐CH3C6H4)

In the presence of N, N′‐dicyclohexylcarbodiimide (DCC), (Bu₄N)₂[Mo₆O₁₈(NAr)] ( 1 ) and (Bu₄N)₂[Mo₆O₁₇(NAr)₂] ( 2 ), Ar = o‐CH₃C₆H₄, have been synthesized via the reaction of [α‐Mo₈O₂₆]^4— with o‐toluidine. If the hydrochloride salt of o‐toluidine was added into the reactive mixture, only the monofunctionalized imido derivative of [Mo₆O₁₉]^2— was obtained; the bifunctionalized derivative of [Mo₆O₁₉]^2— was exclusively synthesized in the presence of non‐protonated o‐toluidine. The molecular and crystal structures of the hybrid compounds 1 and 2 were determined by X‐ray single crystal diffraction, and their UV, IR and NMR spectra were compared. Additionally, a possible reaction mechanism was proposed.     

Synthesis,structure, and catalytic activity of Keggin-type polyoxometalate coordinated Cu(I): {[Cu(py)2]4[SiW12O40]}, via hydrothermal decarboxylation

A Keggin-type polyoxometalate [SiW₁₂O₄₀]^4? supported transition metal complex, {[Cu(py)₂]₄[SiW₁₂O₄₀]} (py?=?pyridine), has been synthesized by hydrothermal decarboxylation and characterized by elemental analyses, IR spectra, thermal stability analyses, and single-crystal X-ray diffraction. The compound is a 1-D chain containing an inorganic–organic backbone with alternating [SiW₁₂O₄₀]^4? clusters and [Cu(py)₂]⁺ along the c-axis, and with both three- and four-coordinate copper. The luminescence properties indicated that the emission peak is emission of pyridine, assigned to the Cu(I) to pyridine charge transfer. This air-stable Cu(I) complex can efficiently catalyze the O-arylation of both phenols and aryl halides.     

Two New Polyoxovanadate‐supported Transition Metal Complexes: [Zn(en)2][Zn(en)2(H2O)2][{Zn(en)(enMe)}As6V15O42(H2O)]·4H2O and [Zn2(enMe)2(en)3][{Zn(enMe)2}As6V15O42(H2O)]·4H2O

Two novel As‐V‐O cluster supported transition metal complexes, [Zn(en)₂][Zn(en)₂(H₂O)₂][{Zn(en)(enMe)}As₆V₁₅O₄₂(H₂O)]·4H₂O ( 1 ) and [Zn₂(enMe)₂(en)₃][{Zn(enMe)₂}As₆V₁₅O₄₂(H₂O)]·4H₂O ( 2 ), have been hydrothermally synthesized. The single X‐ray diffraction studies reveal that both compounds consist of discrete noncentral polyoxoanions [{Zn(en)(enMe)}As₆V₁₅O₄₂(H₂O)]^4? or [{Zn(enMe)₂}As₆V₁₅O₄₂(H₂O)]^4? cocrystallized with respective zinc coordination complexes. Interestingly, compounds 1 and 2 exhibit the first two polyoxovanadates containing As₈V₁₅O₄₂‐(H₂O)]^6? cluster decorated by only one transition metal complex. Crystal data: 1 , monoclinic, P2₁/n, a = 14.9037(4) Å, b = 18.1243(5) Å, c = 27.6103(7) Å, β = 105.376(6)°, Z = 4; 2 monoclinic, P2₁/n, a = 14.9786(7) Å, b = 33.0534(16) Å, c = 14.9811(5) Å, Z = 4.     

Synthesis and Structural Characterization of a Novel Sphere Compound of Mo_8V_2O_(28)·7H_2O

Polyoxometalates( POMs) are attractivebuilding blocks for functional materials withpotential application in electrocatalysis and thepreparations of molecular electronic,orelectrooptical devices[1,2 ] . With the recentdiscovery of giant nanoporous and spherePOMs[3— 6] ,it remains a great challenge tosynthesize rationally new nanoscale materialspossessing novel structures and desirableproperties.The present paper covers a novelstructure characterization of Mo8V2 O2 8· 7H2 O( abbreviated Mo…     

2,3-吡啶二羧酸铜(Ⅰ)配合物的合成与结构

铜配合物具有多变的配位结构,可活化小分子,可用于氧转移、氧化加成、新陈代谢、均相催化等许多领域。还可以用作金属酶的化学模拟和配合物结构及反应性能研究方面[1-3]。本文以2,3 二羧酸 吡啶为辅助配体及[(PPh3)2Cu(BH4)]作为起始原料,室温下,通过取代反应合成了单核铜(Ⅰ)配合物[(PPh3)2Cu(C7H4NO4)],经元素分析、电导、光电子能谱、红外光谱及单晶XRD方法对配合物进行了表征。1　实验部分1 1　仪器和试剂意大利ERBA 1106元素分析仪,JA96 970等离子光谱仪,Nicolet170SX分析仪(CsI压片),AV 300Bruker分析仪(CDCl3溶剂,8…     

[Mo12S12O12(OH)12(H2O)6]: A Cyclic Molecular Cluster Based on the [Mo2S2O2]2+ Building Block

The pH-dependent self-condensation of the [Mo ₂ S ₂ O ₂ ] ²⁺ complex fragment gives the wheellike Mo₁₂ cluster depicted on the right (ball-and-stick model; large balls: S, medium balls: O, small balls: Mo). Applying this synthetic strategy to other starting materials could provide access to other polyoxothiometalates with well-defined cavities.     

有机/无机杂化钙钛矿(C14H13N2O2)2PbCl4的制备与表征

合成了一种新颖的有机/无机杂化钙钛矿(C14H13N2O2)2PbCl4材料,采用元素分析、红外光谱(FT-IR)、紫外可见吸收光谱(UV-Vis)、透射电镜(TEM)、电子衍射(ED)、紫外可见光声光谱(UV-Vis PAS)和表面光电压谱(SPS)等手段对其分子结构和聚集态、光学性质和光、电特性进行了表征。结果表明,这种材料具有较好的有序性,在紫外光波段同时具有较好的光电响应和光声特性。     

Keggin型配合物（C12H9N2）3[PMo12O40]的水热合成及晶体结构

采用水热反应合成了有机-无机杂化的Keggin型配合物（C12H9N2）3[PMo12O40],并通过X-射线单晶衍射对其结构进行了分析。该配合物为正交晶系P212121空间群,晶胞参数为a=1.20800（1）nm,b=2.10108（4）nm,c=2.24234（5）nm。配合物包含了孤立的Keggin型[PMo1...     

Hydrothermal Synthesis of Brucite Type Copper Hydroxide Squarate [Cu3(OH)2(C4O4)]·4H2O

Herein we report synthesis of a new brucite type copper hydroxide squarate, Cu₃(OH)₂(C₄O₄)₂·4H₂O [P2₁/c, a = 5.6437(4) Å, b = 12.8357(9) Å, c = 9.1507(6) Å, β = 95.892(1)° and Z = 2] by hydrothermal method, and its characterization by single crystal diffraction analysis as well as by IR spectroscopy. The rather wide spread of Cu–O bond lengths, can be primarily rationalised by the Jahn‐Teller effect, and secondarily by the connectivities of the CuO₆ octahedra.     

Synthesis,spectroscopic characterization,X-ray structure and magnetic properties of [Cu(hmquin-7-COOH)2(MeOH)] complex

The reaction of copper(II) chloride dihydrate and 8-hydroxy-2-methylquinoline-7-carboxylic acid (Hhmquin-7-COOH) leads to [Cu(hmquin-7-COOH)₂(MeOH)]. The compound has been studied by IR, UV–Vis, EPR spectroscopy and X-ray crystallography. X-ray studies confirm bidentate coordination mode of the hmquin-7-COOH anions via the pyridine nitrogen atom and deprotonated hydroxyl group. The COOH groups of the hmquin-7-COOH ligands are potentially available for further conjugation. The title complex has been additionally studied by magnetic measurement. The TDDFT/PCM calculations have been employed to discuss the electronic spectrum of [Cu(hmquin-7-COOH)₂(MeOH)] in more detail.     

Crystal structure of (C2H7N4O)2[UO2(C2O4)2(H2O)]

The single crystals of (C₂H₇N₄O)₂[UO₂(C₂O₄)₂(H₂O)] were studied by X-ray diffraction. The crystals are monoclinic, space group Pn, Z = 2, unit cell parameters: a = 9.4123(2) Å, b = 8.4591(2) Å, c = 11.8740(3) Å, β = 105.500(10)°, V = 911.02(4) ų. The main structural units of the crystals of I are islet complex groups [UO₂(C₂O₄)₂(H₂O)]^2? corresponding to the crystal chemical group AB ₂ ⁰¹ M¹ (A = UO UO ₂ ²⁺ , B⁰¹ = C₂O ₄ ^2? , M = H₂O) of uranyl complexes. Uranium-containing mononuclear complexes are connected into a three-dimensional framework through the electrostatic interactions and hydrogen bonding system involving carbamyolguanidinium ions.     

新颖的[CuI(dpq)2]+配合物阳离子修饰的砷钒酸盐[Cu(dpq)2]4[As8V14O42(H2O)]·2H2O的水热合成与结构表征

采用水热方法制备了一个新颖的[CuI(dpq)2]+配合物阳离子修饰的砷钒酸盐[Cu(dpq)2]4[As8V14O42(H2O)]·2H2O, X射线单晶衍射结果表明, 该化合物的结构是由4个[CuI(dpq)2]+阳离子和1个[As8V14O42(H2O)]4-簇阴离子以及2个结晶水组成的, 簇阴离子内部包含一个孤立的水分子.     

The First Hexa-coordinated Tetranuclear Nickel Complex {[Ni(en)2]4[H4L]}(ClO4)4·7H2O with Tetrakis-bidentate Oxamato Bridge

The first tetranuclear nickel complex with the oxamato ligand, {[Ni(en)₂]₄[H₄L]}(ClO₄)₄·7H₂O ( 1 ) (L = N, N′, N″, N‴-methanetetrayltetrakismethylenetetrakis (oxamato)), has been prepared and determined by single-crystal X-ray analysis. 1 crystallizes in the tetragonal space group I4₁/a, with a = 15.2744(9), c = 31.3748(2) Å and Z = 4. Each nickel (II) ion is in a distorted octahedral donor atom environment, which comprises four nitrogen atoms of two en molecules and two oxygen atoms of oxamato bridge. The shape of the entity looks like a propeller. The temperature-dependent magnetic susceptibilities were analyzed by the Curie-Weiss law; the following values were found C = 4.36 cm³ K mol^-1, θ = -24.7 K, respectively.     

Synthesis,crystal structure and magnetic properties of a new complex containing Cu(I) and radicals, [Cu(imme2py)2](ClO4)

A new complex, [Cu(imme2py)₂](ClO₄) (imme2py?=?2-(2′-(6′-methylpyridyl))-4,4,5,5-tetramethyl-1H-imidazolyl-1-oxyl) has been synthesized and structurally characterized by X-ray diffraction methods. It crystallizes in the orthorhombic crystal system, space group P ₂₁₂₁₂₁ . The structure consists of [Cu(imme2py)₂]⁺ cations and chloride anions. The coordination geometry about Cu(I) is tetrahedral with the four coordination sites being occupied by four nitrogen atoms. Magnetic measurements show intramolecular antiferromagnetic interactions between the imino nitroxides.     

Hybrid Tungstocuprate [Cu(2,2'-bpy)3]2H4[CuW12O40]·6H2O Based on Keggin Polyoxoanion [CuW12O40]6-with CuⅡas Heteroatom

A novel hybrid tungstocuprate(Ⅱ) [Cu(2,2'-bpy)3]2H4[CuW12O40]·6H2O(2,2'-bpy=2,2'-bipyridine) was synthesized via hydrothermal method and characterized using elemental analyses, IR, UV, XPS, TG-DSC, EPR, and X-ray single crystal diffraction. The structural analysis shows that the complex consists of an unusual Keggin-type polyoxoanion [CuW12O40]6- and a pair of chiral complex cations [Cu(2,2'-bpy)3] together with four protons and six crystallization water molecules, and the Keggin polyoxoanion is connected with [Cu(2,2'-bpy)3] via multiple C-H…O hydrogen bonds resulting in a dimer.