Synthesis and X-ray characterization of a polymeric 1:3 complex of copper(II) nitrate with pyrazine

The structure of poly--pyrazine-bis(pyrazine)(dinitrato-O)copper(II), Cu(pyz)₃(NO₃)₂, has been investigated by X-ray diffraction. The compound crystallizes in the triclinic space group with a = 6.8040 (10), b = 7.2860 (10), c = 9.289 (2) Å, = 69.65 (2), = 68.51 (2), = 67.51 (2)°, and Z = 1. The structure consists of linear chains of copper ions bridged by bidentate pyrazine groups, with monodentate terminal pyrazine and nitrate groups completing the distorted octahedral geometry about the copper ions.     

Synthesis and structural characterization of the dinuclear tetrakis(guanidino) bis(2-cyanoguanidine)dicopper(II) complex

The synthesis and crystal structure of a new dinuclear complex Cu₂(C₂H₄N₄)₂ (CH₃N₃)₄ are reported. It crystallizes in the monoclinic system of space group P2₁/c, with a = 8,459(1) Å, b = 15,481(3) Å, c = 8,714(2) Å, = 110,60(1)°, and Z = 2. The centrosymmetric molecular structure of Cu₂(C₂H₄N₄)₂(CH₃N₃)₄ comprises a tetrakis(guanidino)-bridged dinuclear copper(II) core with axially located cnge moities.     

Synthesis,characterization and photoluminescence studies of new Cu(II) complex

In the current work, a new coordination complex, [Cu(HL)₂], 1 [H₂L = 2–((E)–(2–hydroxypropylimino)methyl)–4–nitrophenol] was successfully synthesized and characterized by IR, UV-vis and photoluminescence spectroscopic techniques, single crystal and powder X-ray diffraction measurements. In the crystalline structure of complex 1, the aliphatic –OH group of the ligand is not coordinated and points away from the metal coordination zone, and also actively participates in intermolecular bifurcated O?H···O hydrogen bonds which link the molecules to form hydrogen-bonded linear chains. C?H···π and π···π contacts also connect the molecules in the structure which form to 3D structure. This hydrogen bonded polymeric networks lie in the bc-plane and stacks along to the a-axis. Furthermore, complex 1 and its ligand H₂L display an intense navy-blue emission and blue emission in the solid state at room temperature, respectively, when they are excited under UV light.     

Synthesis and structural characterization of a novel polymeric gadolinium(III)–copper(II) complex of iminodiacetic acid

A novel polymeric Gd₂Cu₃ complex of iminodiacetic acid (H₂L¹=NH{CH₂COOH}₂), namely, Gd₂Cu₃(L¹)₆, 1, has been synthesized and structurally characterized. In the title complex, the Gd³⁺ ion is nine-coordinated by six O atoms from three bidentate chelating carboxylate groups and three O atoms from three anti-anti bridging carboxylic groups of six L¹ ligands; the Cu²⁺ ion is six-coordinated by four O and two N atoms from two chelating L¹ ligands. Each pair of Gd(III) atoms is bridged by three L¹ ligands, each of which also chelates with one copper(II) ion, thus forming a Gd₂Cu₃ cluster unit. Such cluster units are cross-linked by flexible L¹ ligands into a three-dimensional coordination framework. The title complex crystallizes in the trigonal space group P-3c1 (No. 165) with a = b = 13.433(4), c = 14.770(6) Å; V = 2308(1) ų; D_calca = 1.859 g cm^–3; Z = 2.     

Synthesis and characterization of carboxylate-bridged copper(II) dinuclear complex

The dinuclear copper(II) complex {[Cu(pmea)Cl][Cu(H₂O)₃Cl]}(Cl)·H₂O (1) (pmea =bis(2-pyridylmethyl)amino-2-ethanoic acid) has been synthesized and characterized. It crystallizes in the monoclinic system P2₁/c, a = 9.0057(11), b = 28.031(3), c = 8.5669(10) Å, β = 104.267(2)°, V = 2095.9(4) ų, Z = 4. Crystal structure of 1 reveals a syn-anti carboxylate-bridged dinuclear complex, in which the coordination environment around each copper atom exhibits a distorted square-pyramid. Magnetic susceptibility measurement for 1 exhibits a weak intermolecular antiferromagnetic exchange interaction with 2J = −1.17(9) cm⁻¹. The cyclic voltammogram of 1 gives one oxidation and two reduction processes.     

Synthesis and structure of a hexaazamacrocyclic copper(II) complex with maleato ligand

A hexaazamacrocyclic copper(II) complex Cu(L)(H₂O) (O₂CCH = CHCO₂)⋅H₂O (1) (L = 3,10-bis(2-hydroxyethyl)-1,3,5,8,10,12-hexaazacyclotetradecane) was prepared and structurally characterized by a combination of analytical, spectroscopic, and crystallographic methods. In complex 1, the coordination geometry about the copper(II) ion is six-coordinate with four equatorial nitrogen atoms from the macrocycle and two oxygen atoms from the axial maleato and aqua ligands. In 1, the one end of the maleato ligand coordinates to the central copper atom, while the other end is not bonded. The macrocycle and the axial ligands are highly involved in multiple types of hydrogen bonding interactions, resulting in the stabilization of the maleato ligand as a “coordinated ligand counter anion.”     

Synthesis and structure of bis(2,6-dimethylpyrazine)(THF)copper(II) nitrate

Attempts to crystallize Cu(2,6-dmpz)(NO₃)₂ (2,6-dmpz = 2,6-dimethylpyrazine) by reaction of 2,6-dmpz with Cu(NO₃)₂·3H₂O in THF resulted in the synthesis of Cu(2,6-dmpz)₂(NO₃)₂·THF. The compound crystallized in the monoclinic space group C2/c and exists as isolated molecules with distorted square pyramidal geometry: a = 11.609(4) Å, b = 10.415(3) Å, c = 18.256(6) Å, = 108.332(4)°. The 2,6-dmpz molecules coordinate to the Cu ions through the distal (remote from the methyl) nitrogens. The molecules are arrayed in stacks parallel to the b-axis.     

Synthesis and crystal structure of a terephthalato-bridged copper(II) complex [Cu2(tpt)(bpy)2(H2O)4] [Cu2(tpt)3 (bpy)2(H2O)2]

A terephthalato-bridged copper(II) complex [Cu₂(tpt)(bpy)₂(H₂O)₄][Cu₂(tpt)₃(bpy)₂ (H₂O)₂] (1) (tpt = terephthalate, bpy =; 2,2'-bipyridine) was synthesized by the reaction of Cu(ClO₄)₂ 6H₂O and terephthalic acid in the presence of 2,2'-bipyridine in H₂O solution. Crystal structure of 1 was determined by X-ray diffraction analysis in the triclinic space group P , with a = 10.7327(10) Å, b = 11.1658(11) Å, c = 17.3768(16) Å, = 108.063(2), = 91.064(2), = 116.721(2), V = 1737.5(3) ų, and Z = 2. Both the anion and the countercation in 1 are copper(II) complexes linked by terephthalate bridges in the bis(monodentate) (syn–anti) mode. The anion and the countercation are also linked by two hydrogen bonds between coordinating water molecules and terephthalate ligand.     

Synthesis and crystallographic characterization of a six coordinate Cu(II) complex based on hexamethylenetetramine ligand

The title compound, Cu(H₂O)₆]Cl₂.2{(CH₂)₆N₄}.4H₂O ( 1 ), has been prepared under mild hydrothermal conditions. Each Cu^II atom, located on a centre of symmetry, is coordinated by six water molecules in distorted octahedral coordination geometry. The hexamethylenetetramine molecule does not coordinate to the Cu atom but links with the Cu complex via three O—H…N hydrogen bonds. The remaining N atom of the hexamethylenetetramine is hydrogen‐bonded to the solvent water molecule. In the crystal structure, intermolecular O—H…O, O—H…N and O—H…Cl hydrogen bonds link the components into a three‐dimensional network. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and structure of a novel copper (II) nitrate complex of 2,4-dioxo-4-phenylbutanoic acid

2,4-Dioxo-4-phenylbutanoic acid, 1, was synthesized as a biproduct of the attempted synthesis of 1,6-bisphenyl-1,3,4,6-hexanetetrone. Crystals of [Cu(H2O)(bipy) (L)][Cu(bipy)(L)(NO3)] (H2O)(NO3) (L = 2,4-dioxolato-4-phenylbutanoic acid and bipy = 2,2′-bipyridine), 2, were grown by slow evaporation of a solution of Cu(NO₃)₂·3 H₂O, 2,2′-bipyridine, and 1 in a mixture of ethanol and water. The compound crystallized in the triclinic space group P-1 and is made up of two distinct molecular units each with approximately square pyramidal geometry: a = 10.663(2) ?, b = 13.275(3) ?, c = 15.071(3) ?, α = 80.26(3)°, β = 74.13(3)°, γ = 89.12(3)°. The copper ions are chelated by molecules of 1 and molecules of bipyridine. The molecular units are arrayed in rows held together by pi-stacking interactions and hydrogen bonding.     

Synthesis, characterization and crystal structure of a mononuclear zinc(II) complex derived from 2-methoxy- 6-[(3-cyclohexylaminopropylimino)methyl]phenol

Colourless block-shaped crystals of Dichloro{2-methoxy-6-[(3-cyclohexylaminopropy-limino)methyl]phenolato}zinc(II) methanol, [Zn(C₁₇H₂₆N₂O₂)Cl₂].CH₃OH, have been obtained and characterized by elemental analysis, IR and X-ray single crystal determination. The complex crystallizes in the monoclinic space group P2₁/n with unit cell dimensions a=12.980(3) ?, b=13.139(3) ?, c=13.277(3) ?, β=107.00(3)°, V=2165.4(8) ?³, Z=4, R ₁=0.0631 and wR2=0.1110. X-ray structure determination revealed that the complex consists of a [Zn(C₁₇H₂₆N₂O)Cl₂] moiety and a lattice MeOH molecule. In the crystal structure, molecules are linked through intermolecular N–HO, C–HCl and O–HCl hydrogen bonds, forming chains. It is the first complex derived from the Schiff base ligand 2-methoxy-6-[(3-cyclohexylaminopropylimino)methyl]phenol.Supplementary materialCCDC-606067 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at http://www.ccdccam.ac.uk/const/retrieving.html or from the Cambridge Crystallographic Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223-336033 or e-mail: deposit@ccdc.cam.ac.uk.     

二维异核铜-钠配位聚合物的合成和晶体结构

合成了铜-钠混合金属配位聚合物 [(CuL)2(CH3OO)Na(H2O)4]2 (简写为1)并进行了元素分析和单晶X射线衍射分析,L为{2-(2′-酚基)- Δ 2-噻唑-4-羧酸}.晶体结构分析表明配合物形成Cu4Na2的六核混合金属大环.相邻的Cu4Na2环之间通过进一步的配位作用连结成包含更大的Cu8Na4大环的二维网状结构.该晶体属于三斜晶系Pī空间群,晶胞参数分别为:a = 1.0777(4) nm, b = 1.5221(6) nm, c = 1.6994(6) nm, α = 84.58(1)°, β = 76.31(1)°, γ = 89.97(1) °, V = 2.696 (2) nm3, Z = 2, Mr= 1447.26, dc = 1.783 g·cm-3, T = 293(2) K, μ = 1.816 mm-1, F(000) = 1472, R1 = 0.0794, wR2 = 0.1819 [I>2σ(I)].     

Self-assembly in transition metal complexes: structural characterization of a copper histamine nitrate [Cu(II)(him)2(NO3)2]

A new monomeric copper (II) complex with histamine (him), [Cu(II)(him)₂(No₃)₂], has been prepared by the reaction of Cu(NO₃)₂ with histaminium dichloride and its structure was determined by x-ray crystallography. The complex crystallizes in the triclinic system, space group with a = 5.7238(4), b = 8.7094(7), c = 9.2481(11) Å, = 69.693(8), = 73.242(7), = 71.050(7)°, V = 400.84(6) ų, and Z = 1. The structure consists of discrete [Cu(II)(him)₂(NO₃)₂] molecules in which the metal atom is centrosymmetrically coordinated by two histamine ligands forming an equatorial plane with Cu–N(imidazole ring) being 2.032(2) and Cu–N(NH₂ group) being 2.023(2) Å. Two O atoms from nitrate anions coordinate on the elongated axial positions with Cu–O being 2.549(2) Å. In the crystal structure, the molecules are organized by hydrogen bonds forming a two-dimensional network.     

Crystal structure and spectroscopy of bis-[bis(2-benzimidazolyl)propane]copper(II) bis(triflate)monohydrate, a copper complex with a geometry intermediate between tetrahedral and square planar

The structure of a mononuclear copper(II) compound with the ligand bis(2-benzimidazolyl)propane (abbreviated as tbz) is reported. The compound [Cu(tbz)₂](CF₃SO₃)₂(H₂O) crystallizes in the triclinic space group P , with a = 12.363(6), b = 13.218(9), c = 15.365(8) Å, = 82.74(5), = 68.04(4), = 65.30(5), and Z = 2. The Cu(II) atom has a geometry intermediate between tetrahedral and square planar, consisting of four nitrogen atoms of two tbz ligands. The Cu—N—Cu angles are about 135°, while the dihedral angle between them amounts to 62° (0° for square planar and 90° for a tetrahedron). Ligand field bands are observed at 10.2 × 10³, 13.8 × 10³, and 20.3 × 10³ cm^–1, while the most characteristic infrared vibrations of the triflate anion are observed at 1273, 1260, 1238, 1221, 1171, and 1157 cm^–1.     

Synthesis and characterization of copper(II) hexaazamacrotetracyclic complex with thiocynate ligand

A mononuclear complex [Cu(L)(NCS)](ClO₄) (1) (L = 1,3,10,12,16,19-hexaazatetracyclo [17,3,1, 1^12.16,0^4.9]tetracosane) has been synthesized and structurally characterized by X-ray crystal structure analysis. The crystals are monoclinic P2₁2₁2₁ with a = 9.596(1), b = 11.285(1), c = 22.446(2) Å, V = 2430.7(3) ų, Z = 4. The copper atom is coordinated by two secondary and two tertiary amines of the macrocycle and one nitrogen atom of the thiocynate ligand in a distorted square-pyramidal geometry. The cyclic voltammogram of 1 exhibits two waves of a one-electron transfer corresponding to Cu^II/Cu^III and Cu^II/Cu^I processes.     

Synthesis and structure of bis(dibenzoylmethane)copper(II)

Bis(dibenzoylmethane)copper Cu(dbm)₂ has been synthesized and its structure determined by x-ray diffraction. It crystallizes in the monoclinic system, space group C2/c, with a = 25.936(3), b = 5.9806(8), c = 16.4908(16) Å, = 114.998(8)°, Z = 4, and V = 2318.3(4) ų. The Cu atom is located at a symmetry center and surrounded by four O atoms from two dbm molecules to form a plane square coordination environment. On the a–c plane the molecules are orderly arranged to result in a layered structure, and parallel to crystallographic b-axis they form a molecular column due to the effect of aromatic stacking.     

Synthesis and structural characterization of dihexamethylenetetraminetetraaquocobalt(II) hexaaquocobalt(II) sulfate hexahydrate

The synthesis and crystal structure of a new three dimensional cobalt(II) complex [Co(C₆H₁₂N₄)₂(H₂O)₄Co(H₂O)₆][SO₄]₂.6H₂O are reported. It crystallizes in the triclinic space group P-1 with a = 13.394(3), b = 16.077(3), c = 9.282(2) Å, = 89.71(2), = 90.42(2), = 114.02(2)°, V = 1825.6(7)ų and Z = 2. The structure is comprised of [Co(C₆H₁₂N₄)₂ (H₂O)₄Co(H₂O)₆][SO₄]₂ units and H₂O molecules. Two molecules of ligand and four molecules of water chelate one type of Co^II in an octahedral fashion through two N and four O atoms: the four O atoms form the equatorial plane and the two N atoms occupy the apical positions. The other type of Co^II cation is chelated by six water molecules.     

Synthesis and structural properties of a 1-D copper(I) coordination polymer

A coordination polymer catena-chloro(4-pyridinecarboxylic acid)copper(I): [Cu(C₆H₅ O₂N)Cl]_n (1) has been prepared directly by reacting Cu^IICl₂ 2H₂O and 4-cyanopyridine in the presence of disodium maleate under hydrothermal conditions at 140°C. Crystal data for 1 are as follows: monoclinic, P2₁/n, a = 16.4623(9) Å, b = 3.7795(2) Å, c = 24.7612(11) Å, = 101.534(1)°, V = 1509.5(1) ų, Z = 4, D _calc. = 1.955 g cm^–3, R1 = 0.0511, wR2 = 0.1060 for all 2666 reflections. In this 1-D stair-polymer, two [Cu–Cl–Cu]_n zigzag chains are held together by weak interchain Cu–Cl bonds. The 4-pyridinecarboxylic acid ligands derived from the 4-CNpy molecules coordinate to the approximately tetrahedral Cu(I) centers through pyridyl-N atoms. The carboxyl ends of 4-pyridinecarboxylic acid participate in interchain hydrogen-bonding interactions to form a 2-D supramolecular network.     

Synthesis and crystal structure of copper(II) complex with 1,9-diamino-5-methyl-5-nitro-3,7-diazanonane

Condensation of bis(ethanediamine)copper(II) perchlorate with formaldehyde and nitroethane in basic methanol was found to generate (1,9-diamino-5-methyl-5-nitro-3,7-diazanonane)copper(II) perchlorate, [Cu(L₁)](ClO₄)₂. The copper(II) complex was characterized by elemental analysis and infrared and electronic spectra studies. The structure of [Cu(L₁)](ClO₄)₂ was determined by X-ray diffraction. The crystal structure revealed that the copper ion is in an elongated octahedral coordination with four nitrogens at the equational position and perchlorate anions at the axial positions and that one of the perchlorate anions bridges two copper ions, leading to a linear polymeric structure in the crystal.     

(Imidazole)(3,3′-trimethylenedinitrilo bis (2-butanone oximate)) copper(II) perchlorate: Synthesis and crystal structure of a five-coordinate copper-protein model complex

The synthesis and crystal structure of the novel pentacoordinated complex [Cu(DOHPN)(IMI-DAZOLE)] (ClO4), (DOHPN=(3,3′-trimethylenedinitrilo bis 2-butanone oxime) are reported. The X-ray crystal structure (space groupP2₁/n, a=11.349(2) Å,b=14.241(3) Å,c= 12.635(3) Å; α=90°, β=100.21 (3)°, γ=90°) shows that the copper(II) ion occupies a distorted square-pyramidal geometry with the imidazole ligand occupying the axial position. The copper(II)-(N)imidazole distance is 2.125(3) Å and the copper(II)-tetraaza plane distance is 0.385/Å. The tetraaza ligand DOHPN adopts a “butterfly-like” geometry with a dihedral angle of 149.69°. The title complex is the first structurally characterized compound of the series [Cu(DOHPN)(axial ligand)]ⁿ⁺ where the axial ligand is a neutral N-heterocycle with known biological relevance. A comparison of the structural parameters with those observed when the axial ligand is H₂O or NCS^? (N-bonded) gives the following series with increasing metal-ligand interaction: H₂O>IMIDAZOLE>NCS^? (N-bonded).