Synthesis and Crystal Structure of a Copper（Ⅱ） Complex with Benzilic Acid and 1,10-Phenanthroline

A new complex [Cu（phen）3][（C6H4）2C（OH）COO]2·6H2O was prepared by selfassembly of benzilic acid, 1,10-phenanthroline （phen）, and copper perchlorate. It crystallizes in triclinic, space group P1-, with a = 1.14661（17）, b = 1.6455（2）, c = 1.6457（2） nm, α= 74.779（2）, β = 74.904（3）, γ = 84.424（3）°, V = 2.8914（7） nm^3, Dc = 1.340 g/cm^3, Z = 2, F（000） = 1218, GOOF = 1.018, the final R = 0.0643 and wR= 0.1633. The crystal structure shows that the copper ion is coordinated with six nitrogen atoms from six 1,10-phenanthroline molecules, forming a distorted octahedral coordination geometry.     

Synthesis and Crystal Structure of a New Lanthanum（Ⅲ） 4-Cyanobenzoate Complex

A new dinuclear La（Ⅲ） complex [La2（4-cba）4[H（4-cba）2]2（phen）2（H2O）4] （4-Hcba = 4-cyanobenzoic acid and phen = 1,10-phenanthroline） 1 has been synthesized by solvothermal reaction in an ethanol/water mixed solution at 100 ℃ and structurally characterized by singlecrystal X-ray diffraction. Crystallographic data： C88H58La2N12O20, Mr = 1881.28, triclinic P1, a = 7.518（3）, b = 17.033（6）, c = 17.551（6）A, α = 115.333（4）, β = 92.9910（10）, γ = 99.366（5）°, V = 1985.3（12）A^3, Z = 1, Dc = 1.574 g/cm^3, F（000） = 944 μ = 1.145 mm^–1, the final R = 0.0281 and wR = 0.0686 for 6708 reflections with Ⅰ 〉 2σ（I）. In 1, two nine-coordinated La（Ⅲ） ions are connected by two 4-cba ligands in a syn-syn bidentate coordination mode, and the other six 4-cba ligands terminate the La（Ⅲ） ions, resulting in an isolated dinuclear structure. Two different types of intramolecular hydrogen bonds, asymmetrical O-H…O and symmetrical O…H…O, exist in the crystal. The title complex molecules are connected through hydrogen bonds and weak π-π stacking interactions to generate a 2-D layered network. The thermogravimetric analysis of 1 has also been discussed.     

Synthesis and Crystal Structure of a Novel Tetravanadate Modified by Chiral Racemoid Zirconium Complex

1 INTRODUCTION Polyoxometalate anions are a broad class of dis- crete metal-oxide compounds MxOyn–, which are of both fundamental and practical interest in a range of areas, including catalysis, biochemistry, medicine and solid state devices[1~6]. Recently, the structural chemistry of vanadium oxides in combination with secondary metal-ligand cations has attracted much attention[7~17]. These hybrid materials manifest the structural influences both of coordination preferen- ces of the sec…     

Synthesis and Crystal Structure of a Dinuclear Complex： Bis[aqua（phen）（4- aba）copper（Ⅱ）nitrate（4-abaH）dihydrate]

The title complex has been obtained by the reaction of copper nitrate tri-hydrate with 4-abaH (4-abaH=4-aminobenzonic acid) and phenanthroline in ethanol solution,and its structure was determined by X-ray crystallography with the following data: monoclinic,space group C2/c,Mr=1266.13,Cu2C52H54N10O20,a=25.884(5),b=10.205(2),c=20.849(4) ,β=106.34(3)°,Z=4,V=5284.7(18) 3,F(000)=2616,Dc=1.591 g/cm3,μ=0.896 mm-1,the final R=0.0441 and wR=0.1148 for 4200 observed reflections (I > 2σ(I)). In the molecule of the title complex,the asymmetric unit contains one half molecule. The Cu(Ⅱ) atom is five-coordinated by a terminal water molecule,a bidentate phenanthroline and two monodentate 4-aminobenzoate ligands forming a square pyramidal coordination environment. The two bridging 4-aminobenzoate ligands result in a dinuclear copper(Ⅱ) cluster with a short Cu–Cu distance (3.048 ) and a π-π stacking between the adjacent phenanthroline rings (2.96 ).     

Synthesis and Crystal Structure of a New Diamine Complex CuC14（H2tn）

In an attempt to synthesize a new pyrimidine complex of copper(H) in a solution reaction of CuBr2 with 2,2‘-bis(hexahydropydmidine) and hydro-chloric acid, we unexpectedly obtained a bright yellow chip-like crystal of CuCl4(H2tn) [H2tn=(H3NCH2CH2CH2NH3)^2 ]. Its structure was determined by single-crystal X-ray diffraction analysis. The crystal belongs to orthorhombic system, space group Pnma, with cell parameters: a=0.7216(2)nm, b=1.8308(6)nm, c=0.7553(3)nm, V=0.9953(6)nm^3, Z=4, F(000)=564, Mr=281.49, Dc=1.879 g/cm^3. u(Mo Ka)=3.204 mm^-1, R1=0.0248, wR2=0.0575. The analysis of the crystal structure indicates that the complex has a three-dimensional network structure, which is formed by hydrogen bonds and electrostatic interaction.     

Synthesis and Crystal Structure of a New Three-dimensional Supramolecule of Copper（Ⅱ） Schiff Base Complex

A new three-dimensional supramolecule composed of copper-Schiff base complex, [Cu（naphdien）]Cl·H2O, where naphdien is Schiff base of 2-hydroxy-1-naphthaldehyde and diethylenetriamine, has been synthesized and determined by single-crystal X-ray diffraction. It belongs to the monoclinic system, space group P21/c, with a = 7.3490（15）, b = 7.0847（16）, c = 30.845（3）A, β= 95.33（3）°, V = 1599.0（5）A3, Z = 4, C15 H20ClCuN3O2, Mr = 373.33, De = 1.551 g/cm3, μ = 1.543 mm^-1, F（000） = 772, R = 0.0536 and wR = 0.0927 for 2788 unique reflections with 1659 observed ones （I 〉2σ（I））. In the crystal structure, mononuclear units [Cu（naphdien）]Cl·H2O are linked into a two-dimensional framework via strong hydrogen bonds, and extended into a three-dimensional supramolecular structure through π-π stacking interactions.     

Synthesis and Structure of a La（Ⅲ） Complex of 1,10-Phenanthroline-2,9-dicarboxylate： a Three-dimensional Network via Hydrogen Bonding Interactions

A new La（Ⅲ） complex, {[La（L）（NO3）（H2O）3]·H2O}n （L = 1,10-phenanthroline- 2,9-dicarboxylate）, has been synthesized and structurally determined by X-ray diffraction analysis. The complex crystallizes in the monoclinic system, space group P21/c with a = 7.7358（17）, b = 8.1664（18）, c = 28.271（6） A, β= 95.184（4）°, V= 1778.6（7） A3, Z = 4, C14H14LaN3O11, Mr = 539.19, Dc = 2.014 g/cm^3, μ= 2.471 mm^-1, F（000） = 1056, the final R = 0.0350 and wR = 0.0659. In this complex, each metal center adopts a ten-coordination geometry formed by two N atoms from a ligand L and eight O atoms from three H2O molecules, a nitrate ion and carboxylates of two ligands. Each ligand adopts a N2,O3-pentdentate coordination mode using two N and two O atoms chelating a La（Ⅲ）, and using another O atom of carboxylate to bridge another La（Ⅲ） center resulting in a 1D helical chain molecule. Intermolecular strong O-H…O and weak C-H…O hydrogen bonds extend the 1D chain structure into a 3D supramolecular architecture.     

Synthesis and Crystal Structure of N-（1′-H-Pyrrol- 2′-ylcarbonyl）-5-amino- 1,10-phenanthroline

The title compound, N-（1′-H-pyrrol-2′-ylcarbonyl）-5-amino-1,10-phenanthroline, was synthesized by the reaction of a-pyrrolyl carbonyl chloride and 5-amino-1,10-phenanthroline in pyridine. Determined by X-ray structure analysis, it crystallizes in triclinic system, space group P1 with the following crystallographic data： C20H21N5O3, Mr = 379.42, a = 7.8559（4）, b = 9.1681（6）, c = 14.6818（9） A, α= 73.254（10）,β= 88.938（15）, γ= 68.080（10）°, V= 934.66（10） A3, Z = 2, F（000） = 400, Dc = 1.348 g/cm^3 and p = 0.094 mm-1. The final R = 0.0680 and wR = 0.1419 for 2142 observed reflections with I 〉 2σ（/）, and R = 0.1084 and wR = 0.1643 for all reflections. Two aromatic ring planes （pyrrole and phenanthroline rings） are connected by the amide plane. Two different types of intermolecular hydrogen bonds, O-H…N and N-H…O, exist in the crystal. The title complex molecules are connected through hydrogen bonds and weak π-π stacking interactions to generate a 3-D supramolecule.     

Synthesis and Crystal Structure of a New Mononuclear Nickel（Ⅱ） Mixed Complex Derived from 2-Aminoethyl-bi（3-bi-aminopropyl）amine with 1,10-Phenanthroline

1 INTRODUCTION The research on organic polyamines is currently of great interest because of their potential applica- tions as useful organic ligands, in which the amine nitrogen atoms have strong coordination ability to the transition metal ions and recognition function[1~4]. Their transition metal complexes play an excellent role in catalysis and mimic studies on dismutase and chlorophyll[5~7]. Therefore much attention has been focused on their syntheses and applications[8~11]. Our group…     

Synthesis, Characterization, Crystal Structure and Stability of a Ternary Cu（Ⅱ） complex with 1, 10-Phenanthroline and L-Valinate

It is important to research the mixed-ligand copper complexes containing bioligands, such as amino acids, nucleic acids and proteins, in exploring the functional mechanism of microelement copper in organism because the reaction of any micronutrient with two or more bioligands in the concentrated bioligands background gives mixed-ligand ternary complexes, which are more stable and related with storage of substance and transportationof metal ions in the life process.     

Synthesis and Crystal Structure of Binuclear Complex of Copper（Ⅱ）Chl

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Synthesis and Supramolecular Structure of Chloro（1,10-phenanthroline ）copper（I） Hexahydrate

1INTRODUCTION Atom transfer radical addition is an efficient me-thod for carbon-carbon bond formation in organic synthesis[1,2].In some of these reactions,a transi-tion-metal catalyst acts as a carrier of the halogen atom in a reversible redox process.The transition-metal-catalyzed has been successfully used to con-trol radical polymerization[3].In the process,the transition-metal species initially abstracts halogen atom X from organic halide to form oxidized species and carbon-centered r…     

Synthesis and Crystal Structure of a New Cu（Ⅱ） Dithiocarbamate Complex CuI（prdtc）（phen）

A new mononuclear Cu（Ⅱ） dithiocarbamate complex CuI（prdtc）（phen） 1 （prdtc = N-pyrrolidinyldithiocarbamate, phen = 1,10-phenanthroline） was synthesized and characterized by elemental analysis, IR spectrum, and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 8.7110（9）, b = 14.7143（14）, c = 14.8507（15） A, β = 109.721（6）°, V = 1791.9（3） A3, Z = 4, Dc = 1.916 g/cm3, CI7H16CulN3S2, Mr = 516.89, λ（MoKa） = 0.71073A,μ = 3.178 mm^-1, F（000） = 1012, the final R = 0.0369 and wR = 0.0987. A total of 4082 unique reflections were collected, of which 2916 with I 〉 2σ（I） were observed. The Cu（Ⅱ） atom is five-coordinated in a distorted square-pyramidal geometry by one I atom in the apical position, two S atoms from a prdtc ligand and two N atoms from a phen ligand in the basal plane. There exist face-to-face aromatic π-π stacking interactions between adjacent phen ligands stabilizing the structure and making the complex assemble into a 1D structure along the a axis. It can be concluded that the difference of the dtc flexibility and reaction conditions result in the structural difference between complex 1 and CuI（dmdtc）（phen） （dmdtc = N, N-dimethyldithiocarbamate）.     

Synthesis and Crystal Structure of a New Complex [CuL(Phen)]·NO3

A new mononuclear copper(Ⅱ) complex [CuL(Phen)]·NO3 (L = 2-{2-[(3,5-dibro- mosalicylidene)amino]ethyl}-1H-1,3-benzimidazole, Phen = 1,10-phenanthroline) has been synthe-sized and its crystal structure was determined by X-ray diffraction method. It crystallizes in mono- clinic, space group C2/c with a = 24.966(7), b = 15.673(4), c = 16.600(5) (A), β = 123.981(4)o, C28H20Br2CuN6O4, Mr = 727.86, V = 5386(2) (A)3, Z = 8, Dc = 1.795 g/cm3, μ(MoKα = 3.826 mm-1, F(000) = 2888, the final R = 0.0508 and wR = 0.1024 for 5440 independent reflections with Rint = 0.1134. The title compound is composed of [CuL(Phen)]+ cation and NO3- anion. The coordination geometry around copper atom is a highly distorted trigonal bipyramid consisting of one benzi-midazole nitrogen atom, one phenolato oxygen atom and one phenanthroline nitrogen atom on the equatorial plane together with one imine nitrogen atom and one phenanthroline nitrogen atom occupying the axial positions. The hydrogen bonding and π-π stacking interactions link the copper complex molecules into a 3-D supramolecular structure.     

Synthesis,Crystal Structure and Magnetic Properties of a New Zn（Ⅱ）-Nitronyl Nitroxide Complex

A new complex [Zn（NIT-1′-MeBzlm）Cl2（H2O）] （NIT-1′-MeBzlm = 2-{2′-[（1′- methyl）benzimidazolyl]}-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide） has been prepared and structurally characterized by X-ray diffraction method. Crystal data： monoclinic, space group P21/n, Z = 4, C15H21Cl2N4O3Zn, Mr = 441.63, a = 7.2225（10）, b = 30.849（4）, c = 8.8758（13）A, β = 103.904（2）°, V = 1919.6（5）A^3, Dc = 1.528 g/cm^3, μ（MoKα） = 1.579 mm^-1, F（000） = 908, R = 0.0436 and wR = 0.1029 for 2456 observed reflections with I〉 2σ（I）. X-ray analysis reveals that the Zn（Ⅱ） ion is four-coordinated with a distorted tetrahedron. There also exist H-bonds, π-π piling interactions and weak intermolecular contacts between the NO groups which form a mutual stagger 3-D network configuration. Magnetic investigation reveals that there exists intermolecular antiferro- and ferromagnetic interactions in the title complex.