Synthesis and structure of a complex of copper(II) bromide with bis(benzotriazol-1-yl)methane

The preparation technique of a complex of copper(II) bromide with bis(benzotriazol-1-yl)methane (L), (Cu₂L₂Br₄)_n, is developed. The compound is studied by single crystal and powder X-ray diffraction and static magnetic susceptibility techniques. According to single crystal XRD data, the complex has a layered structure determined by bidentate bridging coordination of L with N(3) and N(3′) atoms to copper(II). The elementary unit of {Cu₂(μ-Br)₂Br₂} polymer has a binuclear structure. The coordination polyhedron is a trigonal pyramid, and the coordination core is CuN₂Br₃. The temperature dependence of effective magnetic moment is studied within an interval of 2–300 K. The nature of the μ_eff(T) dependence indicates that antiferromagnetic exchange interactions dominate in exchange clusters of the complex with an even number of paramagnetic centers. Original Russian Text Copyright ? 2007 by E. V. Lider, A. S. Potapov, E. V. Peresypkina, A. I. Smolentsev, V. N. Ikorskii, A. I. Khlebnikov, and L. G. Lavrenova __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 48, No.3, pp.543–547, May–June, 2007.     

Theoretical investigation on molecular structure of a new mononuclear copper(II) thiocyanato complex with tridentate Schiff base ligand

An asymmetrical Schiff base ligand, 4-bromo-2-(2-pyridylmethyliminomethyl)phenol (HL), and its copper(II) complex, [Cu(L)SCN] (1), have been synthesized. Complex 1 is experimentally characterized by elemental analysis, FT-IR and UV–vis spectroscopic techniques, and cyclic voltammetry. The structure of the complex has been established by single-crystal X-ray diffraction studies, which reveal a square planar geometry of the central copper(II) ion in 1. The neighboring molecules of the complex connect each other by π–π stacking interactions with centroid-to-centroid ring distance 3.653 Å. The ligand can display two possible tautomeric forms; therefore, 1 can have an alternate molecular structure. DFT calculations have been employed to investigate the structure and relative stabilities of the suggested tautomeric forms of the ligand and its corresponding copper(II) complex.     

双大环配体与铜双核配合物的合成、晶体结构和磁偶合性质

由新型双功能配体2,6-双(1,5,9-三氮杂环十二烷)-2,6-二甲基苯甲酸(L)与溴化铜在甲醇中反应得到新型铜双核配合物[Cu~2LBr~2]Br.3H~2O单晶。晶体结构分析表明:2个Cu(II)中心离子由配体L中的羧酸基团桥联;2个等价的Cu(II)中心离子均由双功能配体L的1,5,9-三氮杂环十二烷([12aneN~3)的3个氮原子和羧酸的1个氧原子及1个Br^-离子配位,并都处在三角双锥的配位环境中;分子内Cu...Cu双核间的距离为0.5884(6)nm。变温磁化率数据表明:在同一分子中的2个铜核之间存在反铁磁偶合作用(J=-22.49cm^-^1)。     

A new stepped tetranuclear copper(II) complex: synthesis,crystal structure and photoluminescence properties

Binuclear and tetranuclear copper(II) complexes are of interest because of their structural, magnetic and photoluminescence properties. Of the several important configurations of tetranuclear copper(II) complexes, there are limited reports on the crystal structures and solid‐state photoluminescence properties of `stepped' tetranuclear copper(II) complexes. A new Cu^II complex, namely bis{μ₃‐3‐[(4‐methoxy‐2‐oxidobenzylidene)amino]propanolato}bis{μ₂‐3‐[(4‐methoxy‐2‐oxidobenzylidene)amino]propanolato}tetracopper(II), [Cu₄(C₁₁H₁₃NO₃)₄], has been synthesized and characterized using elemental analysis, FT–IR, solid‐state UV–Vis spectroscopy and single‐crystal X‐ray diffraction. The crystal structure determination shows that the complex is a stepped tetranuclear structure consisting of two dinuclear [Cu₂(L )₂] units {L is 3‐[(4‐methoxy‐2‐oxidobenzylidene)amino]propanolate}. The two terminal Cu^II atoms are four‐coordinated in square‐planar environments, while the two central Cu^II atoms are five‐coordinated in square‐pyramidal environments. The solid‐state photoluminescence properties of both the complex and 3‐[(2‐hydroxy‐4‐methoxybenzylidene)amino]propanol (H₂L ) have been investigated at room temperature in the visible region. When the complex and H₂L are excited under UV light at 349 nm, the complex displays a strong blue emission at 469 nm and H₂L displays a green emission at 515 nm.     

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…     

Synthesis and structure of tetranuclear copper(Ⅱ) complex containing μ4-oxo bridge

A new dinucleating Schiff base ligand HL(L=C13H17N2O3) has been synthesised and characterized.The single crystal structure of its complex [L2Cu4O(AcO4)]·2H2O has beendetermined by X-ray diffraction methods.The result indicates that every Cu atom has its square pyramidal coordination polyhedron and there is a tetrahedral Cu4O core in the complex molecule.Its active sites where catalytic oxidation of dioxygen occurs have been inferred.     

N-乙酰皮考林酰肼合铜的合成和晶体结构

N-乙酰皮考林酰肼(HL)与一水乙酸铜在甲醇溶剂中形成配合物Cu(Ⅱ)L2·0 5H2O(C16H17CuN6O4 5,Mr=428 90),晶体属单斜晶系,空间群为C2/c,a=2 8355(2)nm,b=0.90009(4)nm,c=1.49351(9)nm,β=107.974(2)°,V=3 6258(3)nm3,Z=8,F(000)=1760,μ(MoKα)=1 24mm-1,R=0 0338,wR=0 0955.Cu(Ⅱ)原子的配位介于六配位的严重扭曲的八面体和四配位的不规则多面体之间,其中Cu与O(羰基)距离为0 2653(2)和0 2591(7)nm.量子化学从头算方法计算结果表明,铜与羰基氧之间存在弱配键,晶体通过分子间氢键作用形成一维的无限链状结构     

Crystal structure and photoluminescence properties of a new monomeric copper(II) complex: bis(3‐{[(3‐hydroxypropyl)imino]methyl}‐4‐nitrophenolato‐κ3O,N,O′)copper(II)

Copper(II)–Schiff base complexes have attracted extensive interest due to their structural, electronic, magnetic and luminescence properties. The title novel monomeric Cu^II complex, [Cu(C₁₀H₁₁N₂O₄)₂], has been synthesized by the reaction of 3‐{[(3‐hydroxypropyl)imino]methyl}‐4‐nitrophenol (H₂L ) and copper(II) acetate monohydrate in methanol, and was characterized by elemental analysis, UV and IR spectroscopies, single‐crystal X‐ray diffraction analysis and a photoluminescence study. The Cu^II atom is located on a centre of inversion and is coordinated by two imine N atoms, two phenoxy O atoms in a mutual trans disposition and two hydroxy O atoms in axial positions, forming an elongated octahedral geometry. In the crystal, intermolecular O—H…O hydrogen bonds link the molecules to form a one‐dimensional chain structure and π–π contacts also connect the molecules to form a three‐dimensional structure. The solid‐state photoluminescence properties of the complex and free H₂L have been investigated at room temperature in the visible region. When the complex and H₂L are excited under UV light at 349 nm, the complex displays a strong green emission at 520 nm and H₂L displays a blue emission at 480 nm.     

Crystal Structure of a Copper(II) Complex with 2,3-Dioxo-5,6:13,14-dibenzo-9-methyl-7,12- bis(ethoxycarbonyl)-1,4,8,11- tetraazacyclotetradeca-7,11-diene

1 INTRODUCTIONThe coordination chemistry of macrocyclic compounds has received considerable attention for several decades, primarily due to its importance in biological processes[1]. A variety of 12 ~ 15 membered polyamine and polyoxotetraaza macrocycles have been found to be especially effective in stabilizing oxidation states of the complexed metal ion that are inaccessible for complexes with noncyclic ligands[2~5]. Very recently, we demonstrated that a series of macrocyclic oxamido Sch…     

Synthesis,crystal structure and biological properties of a cis‐dichloridobis(diimine)copper(II) complex

The mechanisms of interaction of inorganic complexes with DNA are important in the design and development of new metal‐based drug molecules. The limitations of cis‐platin have encouraged the design and development of new metal‐based target‐specific anticancer drugs having reduced side effects. The complex cis‐dichloridobis(1,2,5‐thiadiazolo[3,4‐f][1,10]phenanthroline‐κ²N¹,N¹⁰)copper(II), [CuCl₂(C₁₂H₆N₄S)₂], has been synthesized and characterized. The complex crystallizes in the monoclinic space group C2/c. The covalent binding of the complex with DNA was studied by absorption spectroscopy. The anticancer activity of the complex on the Human Lung Carcinoma (A549) cell line was investigated by MTT assay. The complex exhibits higher toxicity than cis‐platin and induces an apoptotic mode of cell death.     

Preparation and X-Ray crystal structure of a Novel Nickel(II) complex with dithiocarbimate

The reaction of potassiumN-(methanesulfonyl)-dithiocarbimate, K₂[S₂C=NSO₂CH₃], with nickel(II) chloride hexahydrate, NiCl₂·6H₂O, formed the complex anion bis(N-(methanesulfonyl)-dithiocarbimate)nickelate(II), [Ni(S₂C=NSO₂CH₃)₂]^2}-, which was isolated as its tetra-n-butylammonium salt. The UV-Vis data obtained were consistent with the formation of a nickelsulfur diamagnetic planar complex. The¹H NMR and the¹³C NMR spectra showed the expected signals for then-Bu₄N⁺ cation and the dithiocarbimate moiety. The single-crystal structure analysis showed that tetra-n-butylammonium bis(N-(methanesulfonyl)-dithiocarbimate)nickelate(II), (Bu₄N)₂[Ni(S₂C=NSO₂CH₃)₂], crystallizes in the monoclinic space groupP2_l/c witha=9.3197(5),b=15.0795(8),c=17.5286(9) å,=91.262(3),V=2462.8(3) å³, andZ=2. The nickel atom is coordinated to four sulfur atoms.     

Differential polarography of copper(II) complex

A differential polarographic study has been carried out on the interaction product formed in the interaction of copper(II) with bis(2-hydroxymethyl-5-hydroxy-4-pyrone-6)ketone. The data obtained using the differential pulse method show that copper(II) exhibits a coordination number of one and a reproducible formation constant that is fairly consistent over a moderate concentration range.     

Synthesis and structure of 5-p-ethoxyphenyl-3-methoxycarbonyl-1-p-tolyl-4-p-tolyloxamoylpyrazole

4-p-Ethoxybenzoyl-5-methoxycarbonyl-1-p-tolylpyrrole-2,3-dione reacts withp-tolylhydrazine to form 5-p-ethoxyphenyl-3-methoxycarbonyl-1-p-tolyl-4-p-tolylxamoylpyrazole. The molecular and crystal structure of the title compound was studied by X-ray diffraction analysis. Deceased Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 3, pp. 610–613, March, 1999.     

Synthesis of a novel copper(II) complex and its crystal structure

One novel chiral copper(II) complex was successfully synthesized from the reaction of chiral 1,3-thiazolidine-2-thione ligand with CuCl₂ in dichloromethane in the presence of Et₃N and DMAP at room temperature. Its unique crystal structure was unambiguously disclosed by X-ray analysis. The crystal is tetragonal, space group I4(1), space group a=15.0875(11), b=15.0875(11), c=19.362(3) Å, =90, β=90, γ=90°, V=4407.4(8) ų, Z=8, ρ_calc=1.639 mg cm⁻³.     

Crystal Structure of Copper(II) Complex with 3-Hydroxyl-1,5-diazacycloheptane-N,N-diacetate

Crystal structure of copper (II) complex with a new aminocarboxylate ligand, 3-hydroxyl-1, 5-diazacycloheptane-N,N-diacetate, C9H14CuN2O5.H2O, Mr=311.78 is reported. It crystallizes in orthorhombic Pna21 with a=13.340(4), b=8.127(1), c=10.583(4) , V=1147.2(7)3 , Z=4, Dc=1.805g/cm3, μ=19.287cm-1 (MoKα), F(000)=644. The final R and Rw are 0.049 and 0.065 for 888 observed reflections with I≥3σ(I). The result of X-ray structure determination shows that the Cu(Ⅱ) forms a planar complex with two oxygen atoms and two nitrogen atoms of the ligand.     

Synthesis,crystal structures,and biological properties of a new naphthalimide Schiff base and its copper(II) complex

A new naphthalimide Schiff base N-allylamine-4-(ethylenediamine-3-methoxysalicylidene)-1,8-naphthalimide (HL) and its copper(II) complex {N-allylamine-4-(ethylenediamine-3-methoxysalicylidene)-1,8-naphthalimide copper(II)} (CuL₂) have been synthesized and characterized. The crystal structure of CuL₂ has been determined by X-ray single crystal diffraction. The central Cu(II) ion is four-coordinate with an N₂O₂ donor set which is afforded by two L ligands, forming a slightly distorted square planar geometry. The interactions of HL and CuL₂ with calf thymus DNA were investigated using electronic absorption titration, fluorescence titration, and viscosity measurements. The results indicate that free HL and CuL₂ bind to DNA in an intercalation mode, and their binding affinity for DNA takes the order CuL₂ > HL. Moreover, the antioxidant assay in vitro also shows that HL and CuL₂ possess significant antioxidant activities and CuL₂ is more effective than free HL.     

Synthesis,crystal structure and magnetic properties of the binuclear copper (II) complex of a new bis (1, 4, 7, 10‐tetraazacyclododecane) ligand

A new binucleating macrocyclic ligand 2,6‐bis (1,4,7,10‐tetraazacyclododecan‐10‐ylmethyl) methoxy‐benzene (L) and its binuclear copper (II) complex, [Cu₂LBr₂] (CIO₄ )₂ · 3H₂O (1), was prepared and the structure was determined by X‐ray crystallography. Complex 1 crystallizes in monoclinic crystal system, P2₁/n space group with a = 0.8206(3), b =2.0892(8), c = 2.3053(7) mn, β = 95.83(2)°, V = 3.932 nm³, Mr=1017.57, Z = 4, D_c =1.692 g/cm³, and R= 0.0489, R_w 0.0552 for 6571 observed reflections with I ≥ 2σ (1). Both of the copper(II) centers are coordinated by four amine nitrogen donors of cyclen subunits and a bromide anion, and each copper(II) ion is in a square‐pyramidal coordination environment. Variable temperature magnetic susceptibility studies indicate that there exists weak intramolecular antiferro‐magnetic coupling ( ?2J = 2.06 cm^?1) between the two copper (II) centers.     

Synthesis and Crystal Structure of the Copper(II) Complex with N,N'-Cyclohexanebis(3- formyl- 5-tert-butyl-salicylaldimine)

INTRODUCTION Schiff-base complexes are some of the most important stereochemical models in transition metal coordination chemistry, with their ease of preparation and structural variation.[1~4] Metal derivatives of Schiff-base have been studied extensively, and copper(II) and nickel (II) complexes play major roles in both synthetic and structural research. The geometry of the coordination sphere is usually planar in the case of Ni, but of Cu, a tetrahedral distortion is often observed.[…