二维网状铜(Ⅱ)配合物的合成及晶体结构表征

A Cu(Ⅱ) complex [Cu(L)_1.5(OSO₃)]·3H₂O (1) [L=1,4-bis(imidazol-1-yl)benzene] was synthesized by reaction of ligand L with CuSO₄·5H₂O using solvothermal method and its structure was determined by X-ray crystal structure analysis. The structure indicates that the complex crystallizes in triclinic, space group P1 with a=0.948 8(2), b=1.078 5(2), c=1.108 4(2) nm, α=74.820(2), β=81.331(2), γ=72.638(2)°, V=1.041 5(3) nm³, Z=2, D_calc=1.687 g·cm^-3, F(000)=544, μ=1.205 cm^-1, the final R=0.062 3 and wR=0.132 8. The Cu(Ⅱ) atom has distorted square-pyramidal environment with a N₃O₂ donor set. Each L ligand links two Cu(Ⅱ) atoms using its imidazole groups to form an infinite one-dimensional (1D) ladder-like chain, which further linked by SO₄^2- to form a two-dimensional (2D) network structure. The 2D sheets are further connected by C-H…O hydrogen bonds to give a three-dimensional (3D) structure. CCDC: 650388.     

含5-氯水杨醛Schiff碱配体的镍和铜配合物的合成及晶体结构

合成了2个含三齿Schiff碱配体和单齿N-杂环分子的多核过渡金属配合物:1个含5-氯水杨醛缩对硝基苯甲酰腙(H2L1)和吗啡啉(Mf)的镍髤配合物[Ni(L1)(Mf)](1),1个含5-氯水杨醛缩水杨酰腙(H2L2)和吡啶(Py)的铜髤配合物[Cu2(L2)2(Py)2](2),并通过元素分析、红外光谱、紫外光谱以及单晶衍射等手段进行表征。在配合物1中,中心Ni髤与酰腙配体(L12-)的酚氧、亚胺氮、去质子酰胺氧原子以及中性吗啡啉氮原子配位形成平面四方形的N2O2配位构型,相邻配合物通过分子间氢键作用构筑成一维超分子链状结构。配合物2中含有2个晶体学上独立的双核铜髤配合物,相邻配合物分子的酚氧原子分别桥联2个[Cu(L2)(Py)]基本单元,形成2个含有Cu2(μ-O)2核心的配合物。每个Cu髤原子具有五配位的NONO(O)四角锥配位构型。     

STRUCTURE OF A Cu (Ⅱ) COMPLEX WITH MIXED LIGANDS, DIETHYLENETRIAMINE ETH YLENEDIAMINE COPPER (Ⅱ) DIPERCHLORATE

<正> CuC6H21N5O8Cl2, Mr = 425. 5, monoclinic, P21/n, a = 8. 418 (2), b = 14.450(4), c= 12. 940(3)A, β=98. 13(2)% V = 1572. 9A3,Z = 4, Dx= 1. 797g. cm-3,μ(MoKa) = 18. 3cm-1. The crystal structure consists of discrete complex cations and perchlorate anions. The coordination geometry around Cu(Ⅱ) atom is a distorted square pyramid. The complex cations are disordered in the crystal,the ethylenediamine ligand chelates to the Cu(Ⅱ ) atom in δ arid λ conformation in different cells. The average Cu-N distance is 2. 03 A in the equatorial plane while the Cu -N distance is 2. 25 A in the axial direction.     

Synthesis and Crystal Structure of 1-D Chain Copper(Ⅱ) Complex:[Cu(L)Cl2]n(L = 2,5-Di-2-pyridyl-1,3,4-oxodiazole)

The title complex, [Cu(L)Cl2]n (L = 2,5-di-2-pyridyl-1,3,4-oxodiazole) 1, has mixture solvent of CH3CN and CH2Cl2 (L is generated from the metal-assisted hydrolysis reaction of bptz) and structurally characterized. It crystallizes in space group C2/c of monoclinic system with cell parameters: a = 9.812(2), b = 12.679(3), c = 1 1.111(2) A, β = 103.92(3)°, V = 1341.6(5)A3, Z = 4, Dc = 1.776 g/cm3, Mr= 358.66, F(000) = 716, μ = 2.024 mm-1 and S = 1.004. The final R = 0.0346 and wR = 0.0938 for 1011 observed reflections with I ＞ 2σ(I). The Cu( Ⅱ ) ion is six-coordinated by four N atoms of two L ligands and two Cl- ions in a distorted octahedral geometry. The ligand L acts as a bis-bidentate ligand to bridge the Cu( Ⅱ ) ions, resulting in an infinite chain structure.     

异烟酰肼缩水杨醛Schiff碱及其铜(Ⅱ)配合物的合成及表征

制备了异烟酰肼缩水杨醛Schiff碱(H2L)及其铜(II)配合物,经元素分析、IR光谱、UV-Vis光谱、电导率和热分析表征,确定了配合物的组成为[Cu(NO3)HL].2H2O,其中H2L=C13H11O2N3.     

Copper(II) mediated anion dependent formation of Schiff base complexes

A tetranuclear mixed ligand copper(II) complex of a pyrazole containing Schiff base and a hydroxyhexahydropyrimidylpyrazole and copper(II) and nickel(II) complexes of the Schiff base having N-donor atoms have been investigated. A 2 equiv amount of 5-methyl-3-formylpyrazole (MPA) and 2 equiv of 1,3-diamino-2-propanol (1,3-DAP) on reaction with 1 equiv of copper(II) nitrate produce an unusual tetranuclear mixed ligand complex [Cu4(L1)2(L2)2(NO3)2] (1), where H2L1 = 1,3-bis(5-methyl-3-formylpyrazolylmethinimino)propane-2-ol and HL2 = 5-methyl-3-(5-hydroxyhexahydro-2-pyrimidyl)pyrazole. In contrast, a similar reaction with nickel(II) nitrate leads to the formation of a hygroscopic intractable material. On the other hand, the reaction involving 2 equiv of MPA and 1 equiv each of 1,3-DAP and various copper(II) salts gives rise to two types of products, viz. [Cu(T3-porphyrinogen)(H2O)]X2 (X = ClO4, NO3, BF4 (2)) (T3-porphyrinogen = 1,6,11,16-tetraza-5,10,15,20-tetrahydroxy-2,7,12,17-tetramethylporphyrinogen) and [Cu(H2L1)X]X x H2O (X = Cl (3), Br (4)). The same reaction carried out with nickel(II) salts also produces two types of compounds [Ni(H2L1)(H2O)2]X2 [X = ClO4 (5), NO3 (6), BF4 (7)] and [Ni(H2L1)X2] x H2O [X = Cl (8), Br (9)]. Among the above species 1, 3, and 5 are crystallographically characterized. In 1, all four copper atoms are in distorted square pyramidal geometry with N4O chromophore around two terminal copper atoms and N5 chromophore around two inner copper atoms. In 3, the copper atom is also in distorted square pyramidal geometry with N4Cl chromophore. The nickel atom in 5 is in a distorted octahedral geometry with N4O2 chromophore, where the metal atom is slightly pulled toward one of the axial coordinated water molecules. Variable-temperature (300 to 2 K) magnetic susceptibility measurements have been carried out for complex 1. The separations between the metal centers, viz., Cu(1)...Cu(2), Cu(2)...Cu(2)A, and Cu(2)A...Cu(1)A are 3.858, 3.89, and 3.858 A, respectively. The overall magnetic behavior is consistent with strong antiferromagnetic interactions between the spin centers. The exchange coupling constants between Cu(1)...Cu(2) and Cu(2)...Cu(2A) centers have turned out to be -305.3 and -400.7 cm(-1), respectively, resulting in a S = 1/2 ground state. The complexes are further characterized by UV-vis, IR, electron paramagnetic resonance, and electrochemical studies.     

一种双肟四核铜(Ⅱ)配合物的合成、结构及热稳定性研究

由螯合双肟配体3,3′-二甲氧基-2,2′-[(1,3-亚丙基)二氧双(氮次甲基)]二酚(H₂L)与四水合苦味酸铜作用,合成了一种新的四核铜(Ⅱ)配合物 [Cu₄L₂(pic)₄(H₂O)₂]·2CH₃COCH₃·2H₂O(pic^-=苦味酸根)。用X-射线单晶衍射仪测定了该配合物的晶体结构：配合物属单斜晶系,P2₁/c空间群,由4个Cu^Ⅱ离子,2个四齿的L2-单元,4个配位的苦味酸根(pic^-),2个配位的水分子,2个结晶的丙酮分子和2个结晶的水分子组成。Cu^Ⅱ离子的配位数为6,都具有稍微扭曲的八面体结构。且配合物分子通过分子间O-H…O氢键作用形成了1个二维超分子结构。     

A Tetranuclear Complex Assembled from N,N''-Bis(4-(3''-formyl-5''-methylsalicyclidene)-iminoethyl)-4-methyl-2,6-bimethyliminophenol

The reaction of 2,6-diformyl-4-methylphenol, ethylenediamine and Cu(Ⅱ) in the proportion of 3:2:2 yields a new tetranuclear copper(Ⅱ) complex, [Cu2L]2(ClO4)2·2H2O (H3L = N,N'-bis(4-(3'-formyl-5'-methylsalicyclidene)iminoethyl)-4-methyl-2,6-bimethyliminophenol). The complex has been characterized by ES-MS, IR and X-ray diffraction analysis, and its crystal crystallizes in the triclinic system, space group P1 with a = 10.8673(11), b = 12.0829(12), c = 14.4834(15) A, α = 111.946(2), β = 105.828(2), γ = 99.583(2)°, V = 1618.5(3) A3, Dc = 1.605 g/cm3, Z = 2, Mr = 1564.26, F(000) = 800.0,μ(MoKa) = 1.460/mm, S = 1.063, R = 0.0612 and wR = 0.1163 for 6245 observed reflections (I > 2σ(Ⅰ)). The complex is a dimer of dinuclear copper(Ⅱ) acylic enantiomorph subunit [Cu2L]CIO4·H2O, held together by π…π, weak coordination and hydrogen bonding interactions. In addition, the π…π interactions related to phenyl moieties as well as CH=N…π interactions were also found to stabilize the supramolecular architectures in the solid state.     

Syntheses and Crystal Structures of Mono- and Binuclear Copper( Ⅱ ) Mixed-ligand Complexes Involving Schiff Base

The mononuclear copper(Ⅱ) complex [Cu(L)(2-AP)] 1 and binuclear copper(Ⅱ)complex [Cu(L)(py)]2 2 (L = C1oH1 1O5NS, taurine o-vanillin, py = prydine, 2-AP = 2-aminopyridine)with mixed ligand have been synthesized and characterized by X-ray diffraction method. Crystal data for 1: orthorhombic, space group Pbca with a = 11.921(4), b = 15.816(6), c = 17.076(6) (A), V=3219.7(19) (A)3, C15H17CuN3O5S, Z = 8, Mr = 414.92, Dc = 1.712 g/cm3,μ(MoKα) = 1.520 mm-1,F(000) = 1704, the final R = 0.0300 and wR = 0.0705 for 2840 observed reflections with I ＞ 2σ(I);and crystal data for 2: monoclinic, space group P21/c with a = 7.929(3), b = 17.038(5), c = 11.734(4)(A), β = 98.162(6)°, V = 1569.1 (9) (A)3, C15H16CuN2O5S, Z = 4, Mr = 399.90, Dc = 1.693 g/cm3, F(000)= 820,μ(MoKα) = 1.554 mm-1, the final R = 0.0351 and wR = 0.0848 for 2767 observed reflections (I ＞ 2o(I)). The molecular structure of complex 1 consists of one tetra-coordinated Cu(Ⅱ) atom generating a slightly distorted square plane, and a one-dimensional chain structure is formed by intermolecular hydrogen bonds. Complex 2 consists of a diphenolic hydroxyl O-bridged binuclear copper(Ⅱ) structure. The crystal structures of complexes 1 and 2 reveal that the coordinate copper centers are bound to both nitrogen and oxygen atom donors. The usual N,O-trans arrangement of ligands is observed in both cases.     

Synthesis and Crystal Structure of the Copper(Ⅱ) Complex with Tris- (1,10-phenanthroline-5,6-dione)

The title complex [ CuL3 ] (C1O4)2 · 2H2O· 2CH3CN (L = 1, 10-phenanthroline-5, 6-dione) has been synthesized and characterized by elemental analysis, conductivity, infrared and UV-Vis spectra. X-ray diffraction analysis at room temperature indicates that the complex (C40H28Cl2 CuNsO16, Mr = 1011.14) crystallizes in orthorhombic system, space group P21 21 21 with a = 13. 983(1), b = 14. 310 (1), c =20.890(2) (A。), V = 4179.7(6) (A。)3, Z = 4, Dc= 1.607g/cm3, F(000) = 2026,μ(MoKa) = 0.736 mm-1. The final R and w,R factors are 0.0446 and 0. 1212 respectively with 8545 independent reflections. The title complex is composed of a discrete [CuL3 ]2+ cation, uncoordinated ClO4- anions, H2O and CH3CN molecules. The central Cu(Ⅱ) atom is six-coordinated by six nitrogen donors of three ligands. The coordination geometry of Cu(Ⅱ) could be considered as an approximately ideal octahedral configuration with little static Jahn-Teller distortion (the longest and shortest Cu- N bonds are 2. 102 vs 2. 139 (A。) with the mean length of 2. 122 (A。) ), which is very rare for a six-coordinated Cu(Ⅱ) complex.     

Synthesis, Structure and Spectral Characterization of a Discrete Binuclear Copper (II) Complex

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Synthesis and Crystal Structure of Tri(4-(3-hydroxy2-ethyl-4-pyridinone-1-yl)-aniline Condensation Salicylaldehydato) Monohydratotricopper(II)Dimethylformamide Monohydrate Solvate

1 INTRODUCTION Synthesis of transition-metal complexes with Schiff-base has been a subject of considerable im- portance[1, 2]. These complexes are not only good coordination agents for Schiff-base, but also good bactericide and antitumour agent[3, 4]. A number of hydroxypyridinones are nontoxic compounds that have been applied in bioinorganic chemistry over many years[5], and their iron(III) complexes have been assessed for the amelioration of anaemia[6]. They have also been examined …     

Thermodynamic Stability Research of Metal Complexes with a Tripodal Amide Ligand and Crystal Structure of its Cobalt（Ⅲ） Complex

A new Co（Ⅲ） complex with a tripodal amide ligand [CoL（N3）3] （L = N-acetyl- N＇,N＇-bis-[（2-pyridyl）methyl]-ethylenediamine） has been synthesized and characterized structurally by X-ray diffraction. It crystallizes in orthorhombic, space group Pnma with a = 9.2515（19）, b = 12.729（3）, c = 17.273（4） A, V = 2034.0（7） A3, C16H20CoN13O, Mr = 469.38, Dc = 1.533 g/cm3, μ（MoKα） = 0.884 mm^-1, F（000） = 968, Z = 4, the final R = 0.0392 and wR = 0.0818 for 2430 observed reflections. In the complex, the amide ligand L acts as a tridentate fashion and coordinates to the Co（Ⅲ） ion through three nitrogen atoms, while the other three positions of the Co（Ⅲ） center are occupied by three terminal azide anions. The complex is connected as a 1D chain structure by intermolecular hydrogen bonds between the uncoordinated amide groups. In order to investigate the coordination ability, thermodynamic stability of the ligand L with the first-series transition metal ions （Co（Ⅱ）, Ni（Ⅱ）, Cu（Ⅱ） and Zn（Ⅱ）） has been studied by potentiometric titration, and the results show that the order of their stability constants conforms to the Irving-Williams sequence.     

Synthesis and Crystal Structure of Copper(Ⅱ) Compound with Didentate Schiff-base Ligand

The title complex [Cu(L)2] (HL=4-salicylideneamino-3,5-dimethanol-1,2,4-triazole) was synthesized by the reaction of Cu(CH3COO)2·2H2O with 4-salicylideneamino-3,5-dimethanol- 1,2,4-triazole in the methanol. The single-crystal X-ray study reveals that the compound crystallizes in monoclinic, space group P21/n with a = 11.746(5), b = 8.145(3), c = 12.786(5)A,β = 106.64(1)°, V = 1172(1)A3, Z = 2, Dc = 1.581 g/cm3, μ= 0.989 mm-1, F(000) = 574, C22H22Cu- N8O6, Mr = 558.02, T = 293(2) K, R = 0.0394 and Rw = 0.0835 for 2376 observed reflections with I > 2σ(I). The complex comprises a four-coordinated copper(Ⅱ) center, with an N2O2 planar coordi- nation environment. The molecules are connected by hydrogen bonds to form one-dimensional chains which are further linked to form a two-dimensional plane.     

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 and Crystal Structure of catena-Poly[[[2,4-dibromo-6-[(3-dimethylaminopropylimino)-methyl]phenolato]copper(Ⅱ)]-μ-azido]

A novel end-to-end azido-bridged polynuclear Schiff-base copper(H) complex,[Cu(C12H15Br2N2O)(N3)]n, was prepared and characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction.The crystal belongs to the orthorhombic system, space group Pbcn with a = 24.588(5), b = 10.377(2), c = 13.022(3)(A),V= 3322.6(12)(A)3, Z = 8, Dc = 1.874 g/cm3, Mr= 468.65, λ(MoKα) = 0.71073 (A),μ= 6.130 mm-1, F(000) = 1832, R = 0.0637 and wR = 0.1176.The Cu atom in the complex is five-coordinated in a square pyramidal geometry by three donoratoms of the Schiff-base ligand, and two N atoms from two bridging azide ligands.The [2,4-dibromo-6-[(3-dimethylaminopropylimino)methyl]phenolato]copper(Ⅱ) units are linked by the bridging azide ligands, giving zigzag polymeric chains with backbones of the [-Cu-N-N-N-Cu]n type running along the b axis.     

New mononuclear, cyclic tetranuclear, and 1-D helical-chain Cu(II) complexes formed by metal-assisted hydrolysis of 3,6-di-2-pyridyl-1,2,4,5-tetrazine (DPTZ): crystal structures and magnetic properties

The reactions of 3,6-di-2-pyridyl-1,2,4,5-tetrazine (DPTZ) with different Cu(II) salts generate two new ligands, 2,5-bis(2-pyridyl)-1,3,4-oxodiazole (L(1)) and N,N'-bis(alpha-hydroxyl-2-pyridyl)ketazine (H(2)L(2)), from the metal-assisted hydrolysis of DPTZ, and form three new complexes: a mononuclear complex [Cu(L(1))(2)(H(2)O)(2)] .2ClO(4) (1), a linear coordination polymer [Cu(L(1))(NO(3))(2)](8) (2), and a cyclic tetranuclear complex [Cu(4)(L(2))(2)(Im)(2)(NO(3))(4)(H(2)O)(2)] (3) (Im = imidazole). Crystal data for 1: space group P2(1)/n with a = 10.339(3) A, b = 10.974(2) A, c = 13.618(4) A, beta = 103.24(1) degrees, and Z = 2. Crystal data for 2: space group C2/c with a = 13.9299(14) A, b = 9.2275(9) A, c = 12.1865(13) A, beta = 111.248(2) degrees, and Z = 4. Crystal data for 3: space group P2(1)/n with a = 9.3422(14) A, b = 15.987(2) A, c = 13.963(2) A, beta = 108.587(3) degrees, and Z = 2. L(1) acts as a bidentate chelating ligand in 1 and as a bis-bidentate chelating ligand in 2 with the shortest intramolecular Cu...Cu distance of 6.093 A. L(2) is a hexadentate ligand to bridge four Cu(II) ions, forming an interesting neutral cyclic tetranuclear complex 3 with Cu...Cu distances varying from 4.484 to 9.370 A. The mechanism of the metal assisted hydrolysis of DPTZ is discussed in detail. Magnetic susceptibility measurements indicate that 2 shows weak ferromagnetic interaction (J = 2.85 cm(-1)) along the 1-D helical chain, and that 3 displays weak antiferromagnetic interaction (J = -1.19 cm(-1) for the N-N bridge) and ferromagnetic interaction (j = 0.11 cm(-1) for the O-C=N bridge) between the adjacent Cu(II) ions.     

Synthesis and Crystal Structure of [Copper(1,10-phenanthroline)_2(pyridine)]perchlorates

1 INTRODUCTIONThe molecular structures of five-coordinated copper (II) complexes show an extensive variability ranging from trigonal bipyramidal to square pyramidal stereochemistry, with most complexes displaying a structure which is intermediate between these two extremes[1,2]. Most crystal structures of 1,10-phenanthroline with copper (II) complexes are known, [Cu (phen)2X]Y, where X = Cl, Br, I, CN, NCS, H2O or thiourea and Y = perchlorate, nitrate, tetrafluoroborate, chloride o…     

Role of anions on the crystal structures of copper(II) and zinc(II) complexes of a tunable butterfly cyclophane macrocycle

Three crystal structures of a ditopic cyclophane ligand (L) in which two 1,5,8,12-tetraamine molecules have been attached through methylene spacers to the ortho positions of a benzene ring are reported. The first one (1) corresponds to the tetraprotonated free macrocycle (H4L4+) having two tetrachlorozincate(II) counteranions (C24H54O2N8Cl8Zn2, a = 9.1890(2) A, b = 14.0120(3) A, c = 15.3180(3) A, alpha = 89.2320(7) degrees , beta = 82.0740(6) degrees , gamma = 83.017(1) degrees , Z = 2.00, triclinic, P); the second one (2) is of a binuclear Cu2+ complex having coordinated chloride anions and perchlorate counteranions (C24H58O14N8Cl4Cu2 a = 9.9380(2) A, b = 30.2470(6) A, c = 53.143(1) A, orthorhombic, F2dd, Z = 18), and the third one (3) corresponds to an analogous Zn2+ complex that has been crystallized using triflate as counteranion (C26H(51.2)O(6.6)N8Cl2F6S2Zn2 a = 8.472(5) A, b = 9.310(5), c = 13.745(5) A, alpha = 84.262(5) degrees , beta = 77.490(5) degrees , gamma = 73.557(5) degrees , triclinic, P, Z = 2). The analysis of the crystallographic data clearly shows that the conformation of the macrocycle and, in consequence, the overall architecture of the crystals are controlled by the anions present in the moiety, pi-pi-stacking associations, and hydrogen bonding interactions. The protonation and stability constants for the formation of the Cu2+ and Zn2+ complexes in aqueous solution have been determined potentiometrically in 0.15 mol dm(-3) NaClO4 at 298.1 K. Intramolecular hydrogen bonding defines the protonation behavior of the compound. Positive cooperativity is observed in the formation of the Cu2+ complexes.     

双烷氧桥联的双核铜(Ⅱ)Schiff碱配合物的合成及配合行为

通过Salen型双肟配体H₂L¹(H₂L¹=5,5′-二(N,N′-二乙胺)-2,2′-[乙二氧双(氮次甲基)]二酚)与乙酸铜反应,合成了一种双核铜(Ⅱ)配合物[Cu₂(L²)₂](H₂L²=4-(N,N′-二乙胺)水杨醛O-(2-羟乙基)肟),并对其进行了X-射线衍射单晶结构分析。