Synthesis and Structural Characterization of a Nickel(II) Complex with Unsymmetrical NNO-Donor Schiff Base Ligand

Abstract  

The nickel(II) complex, Ni[C₅H₄N–CH=N–N=C(O)–C₆H₅]₂ (1) containing a N,N,O-donor hydrazone ligand, which is the 1:1 condensation product of benzhydrazide and pyridine-2-carboxaldehyde has been synthesized and characterized by single crystal X-ray diffraction technique, spectral study and room-temperature magnetic moments. Structural investigation shows that 1 crystallizes to a monoclinic system, having space group P2(1)/c, a = 11.221(4), b = 8.893(3), c = 23.026(8) ?, β = 90.605(14)°, and Z = 4. The central nickel atom is in an N₄O₂ coordination sphere developed with the NNO donor sets of the two independently hydrazone ligands. The Ni–N (pyridine), Ni–N (imine) and Ni–O (enolate) bond distances are 2.144(2) and 2.128(2); 1.980(2) and 1.985(2); 2.0782(17) and 2.1106(17) ?, respectively. The effective magnetic moment (μ _eff) value of 1 is found to be 3.10 B.M. at 300 K.     

Synthesis and Structural Characterization of Hydrazine Bridged Imidazole and its Fumarate Salt

Abstract  

Hydrazine bridged imidazole (1) and its fumarate salt (2) have been synthesized and structurally characterized. Hydrazine bridged imidazole (1) crystallizes in the monoclinic, space group P2(1)/n, with a = 12.809(7) ?, b = 5.102(3) ?, c = 14.401(8) ?, β = 96.859(10)°, V = 934.3(9) ?³, Z = 2. In 1, the two imidazolyl rings are located anti-parallely above and below the benzene planes, respectively. This arrangement leads the imidazolyl rings to be in the trans conformation. In addition at each C=N bond, the larger groups linked to C and N atoms are located in the same side of the double bond, thus in the solid state the conformation of the bis-imidazole (1) is E, E.     

Synthesis and Structural Characterization of a Nickel(II) Complex with Unsymmetrical NNO-Donor Schiff Base like Hydrazone Ligand

Abstract  

The nickel(II) complex Ni[C₅H₄N–C(CH₃)=N–N=C(O)–C₆H₅]₂ (1), containing the potentially tridentate Schiff base like hydrazone ligand (LH) which is the 1:1 condensation product of benzhydrazide and 2-acetylpyridine, was prepared and characterized by IR and UV–Vis spectra, thermal analysis and single crystal X-ray diffraction measurements. Structural investigation shows that the molecule prefers a monoclinic lattice, having space group Cc, a = 10.248(6), b = 19.692(11), c = 12.281(7) ?, β = 91.523(10)o, Z = 4. The central Ni atom is in N₄O₂ coordination sphere developed with the NNO donor sets of the two independently Schiff base like hydrazone ligands with the two Ni–N(pyridine) bonds being significantly longer than the two Ni–N(imino) bonds, 2.096(6), 2.105(6) versus 1.972(6), 2.008(6) ?. The two Ni(II) amide-O bond distances of the chelating ligands are 2.090(6) and 2.092(6) ? respectively.     

Structural Aspects and Spectroscopic Characterization of a Mn(II) Complex with Unsymmetrical NNO-Donor Hydrazone Ligand

Abstract  

The manganese(II) complex, Mn[C₅H₄N–C(CH₃)=N–N=C(O)–C₆H₅]₂ (1) containing N,N,O-donor hydrazone ligand is characterized by X-ray diffraction study. The ligand is the 1:1 condensation product of benzhydrazide and 2-acetylpyridine. The spectral, cyclic voltammetric and room-temperature magnetic moment data are used to establish structure and electronic structure of the compound. Structural investigation shows that 1 crystallizes to a monoclinic system, space group C2/c, a = 22.8367(13), b = 10.1523(6), c = 12.0736(7) Å, α = γ = 90°, β = 116.5930(10)°, and Z = 4. The central manganese atom is in an N₄O₂ coordination sphere constituted by the NNO donor sets of the two independently hydrazone ligands. The Mn–N1, Mn–N2 and Mn–O1 bond distances are 2.3255(15), 2.1854(13) and 2.1361(13) Å, respectively. The effective magnetic moment (μ_eff) value of 1 is found to be 5.92 B.M. at 300 K. Cyclic voltammetry shows Mn(III)/Mn(II) couple at 0.9 V and imine reductions at −0.68 and at −1.3 V.     

Synthesis and Structural Characterization of a Di-nuclear Uranyl Complex with Quinoline-6-carboxylate

Crystallography Reports - A di-nuclear uranyl complex with the formula of [(UO2)2(L)4(H2O)2]?4H2O (1) (HL = quinoline-6-carboxylic acid) was synthesized hydrothermally and characterized by...     

Hydrothermal Synthesis,Characterization, and Property of a Thulium Dinuclear Complex Based on Sulfonate-Phenol Ligand and 1,10-Phenanthroline

Crystallography Reports - A new lanthanide metal complex [Tm2(H2L)3(phen)2] (1) (Na2H2L = 4,5-dihydroxy-1,3-benzenedisulfonic acid disodium salt, phen = 1,10-phenanthroline) was synthesized by...     

Synthesis,Characterization and Crystal Structure of a Polymeric Zinc(II) Complex Containing the Antimalarial Quinine as Ligand

Abstract A novel polymeric zinc(II) complex of quinine, [chlorosulphato (2-ethenyl)-4-azabicyclo[2.2.2]oct-5-ylium-(6-methoxyquinolin-4-yl) methanol zinc(II)] has been synthesized and characterized. Single-crystal X-ray diffraction analysis of the complex (C₂₀H₂₅ClN₂O₆SZn) revealed that quinine forms a zigzag coordination polymeric complex with Zn(II) of extended chains –ZnCl–O–SO₂–O–Zn–O–SO₂–O–ZnCl–. The crystals are monoclinic, space group C2 with a = 20.5035(5), b = 9.7943(2), c = 11.7814(4) ?, β = 96.578(2)°, Z = 4, V = 2350.3(1) ?³. The complex exhibits a tetrahedral geometry. Each Zn(II) centre is thus coordinated to an O atom from each of two sulphate bridges, a Cl atom and quinoline atom N(4) of the quinine moiety. The second quinuclidine nitrogen in the quinine is protonated. In the crystal, there is linkage of two polymeric chains related by a twofold rotation axis, resulting in a bilayer. The linking is achieved by hydrogen bonding from the quinine cation which provides two donors (–OH, N⁺–H), to oxygen atoms of sulphate groups which act as acceptors. Graphical Abstract The new polymeric zinc(II) complex of quinine, [chlorosulphato (2-ethenyl)-4-azabicyclo[2.2.2]oct-5-ylium-(6-methoxy quinolin-4-yl) methanol Zinc(II)] has been synthesized and structurally characterized The compound was characterized by IR spectroscopy, elemental analysis and X-ray diffraction. X-ray analysis showed that quinine forms a zigzag coordination polymeric complex with Zn(II) of extended chains –ZnCl–O–SO2–O–Zn–O–SO2–O–ZnCl–.      

Solid-State Synthesis and Structural Characterization of Hydrated Zinc (II) Tartrate Complex

Abstract  

A new dinuclear hydrated zinc (II) tartrate complex has been successfully synthesized via a solid-state reaction at low temperature under the presence of polyethylene glycol 400 as a structure-directed agent and structurally characterized by single-crystal X-ray diffraction, and further identified by element analyses, FT-IR spectra and TG/DTA measurements. It formulates as [Zn₄(C₄H₄O₆)₄(H₂O)₈]·(H₂O)₁₂ and crystallizes in monoclinic system, and the space group is P2 (1)/c with cell parameters a = 13.681(3), b = 17.059(3), c = 18.483(4) ?, β = 96.62(3)°, and Z = 4. The structure of the title complex consists of two crystallographic independent dimeric units of [Zn₂(C₄H₄O₆)₂(H₂O)₄], 12 lattice water molecules. In each dimeric unit, two tartrate dianions bridges the two Zn (II) ions by using one hydroxy oxygen and one carboxy oxygen atoms as donor atoms, respectively. Each Zinc atom is six-coordinated by four oxygen atoms from two tartrate dianions and two oxygen atoms from the water molecules.     

吡啶鎓盐配体构筑的多钼酸基配合物的合成、结构及光催化性能

本文在水热条件下合成了一例同多钼酸阴离子[δ-Mo₈O₂₆]^4-基配合物[Co(bipbc)(δ-Mo₈O₂₆)_0.5(H₂O)₃] (bipbc=4,4-双[(4-羧基吡啶)甲基]联苯),其为一维链状结构,包含环型双核钴配合物[Co₂(bipbc)₂]⁴⁺和[δ-Mo₈O₂₆]^4-簇。该配合物结晶于单斜晶系,P2₁/n空间群,a=1.147 9(8) nm,b=1.440 9(11) nm,c=2.082 9(16) nm,β=93.469(2)°,V=3.438 8(4) nm³,Z=4,M_r=1 129.18,F(000)=2 204,μ=1.979 mm^-1,D_c=2.181 mg·m^-3,S=1.019,R₁=0.056 2,wR₂=0.137 7。光催化性质研究表明,在可见光、近红外光和全光谱的光照条件下,标题配合物对龙胆紫(GV)和亚甲基蓝(MB)的降解,表现出一定的光催化活性。     

Synthesis,Structural Characterization and Fluorescent Property of Cd(II) Coordination Polymer Based on N-nicotinoylglycine Ligand

Crystallography Reports - A new six-coordinated Cd(II) polymer {[CdL2(H2O)2]?(H2O)}n (1) (HL = N-nicotinoylglycine) was synthesized with N-nicotinoylglycine, Cd(NO3)2?4H2O, NaOH and...     

Synthesis and Characterization of New Phosphorescent Heteroleptic Iridium (III) Complex by Using Tetrazole as an Ancillary Ligand for Organic Light-Emitting Diodes

The yellow emitting tetrazole based heteroleptic iridium(III) complex, bis(diphenylquinoline)iridium(pyridyltetrazole) [(DPQ)₂Ir(PyTz)], was synthesized and conformed by ¹H-,¹³C NMR spectral techniques. The purity was also confirmed by HPLC. The thermal, electrochemical, photophysical and electroluminescent properties were intrinsically investigated. The Ir(III) complex is thermally more stable having thermal decomposition temperature (T_d, 5% weight loss) more than 350°C and it shows very high glass transition temperature T_g-233°C. We have followed the easy and cost effective solution process for (DPQ)₂Ir(PyTz) device fabrication and achieved better performance yellow phosphorescent organic light-emitting diodes (PhOLEDs), maximum external quantum efficiency (EQE) of 5.68%, luminance efficiency 12.63 cd/A, and CIE coordinate of (0.56, 0.43).     

Synthesis and Crystal Structure of a Dinuclear Palladium (II) Complex with a Bulky Acridine-based Ligand

Abstract  

The reaction of PdCl₂ with a bulky acridine-based ligand afforded a novel Pd^II complex [Pd₂(L)Cl₄(CH₃CN)](CH₃CN)_0.5 (1) (L = 9-[3-(2-pyridyl)pyrazol-1-yl]-acridine) exhibiting intra- and intermolecular C–H···Pd H-bonding interactions, which was characterized by elemental analysis, IR, and single-crystal X-ray diffraction analysis (triclinic system, space group P-1, with a = 8.774(6), b = 12.742(9), c = 14.149(10) ?, α = 67.573(11), β = 72.601(11), γ = 83.674(12)°, V = 1395.4(17) ?³, and Z = 2). Complex 1 has an asymmetrical dinuclear structure, which are further assembled into a one-dimensional (1D), and then two-dimensional (2D) network via intra- and/or inter-molecular C–H···Pd and C–H···Cl H-bonding interactions from different crystallographic directions. This work offers a new example in which the N donor of the acridine ring coordinates to a metal ion in a supramolecular coordination system.     

Synthesis and Characterization of Co(II) Coordination Polymer with a Flexible Bidentate Ligand

Crystallography Reports - A coordination polymer, {[Co(bib)3](BF4)2}n, was prepared for the first time at room temperature via the reaction between cobalt(II) chloride and flexible linker ligand,...     

奥沙拉秦钙配合物的合成、结构及表征

本文通过CaCl2·2H2O与药物奥沙拉秦及辅助配体邻菲罗啉在水热条件下得到了一个新的奥沙拉秦配合物[ Ca(L) (Phen)·4(H2O)]n(H2L=奥沙拉秦=3,3-azo-bis-6-hydroxybenzoic acid)(1).通过元素分析、红外对配合物进行了表征,并利用X单晶射线衍射仪测定了其结构.结构解析表明,配合物1属三斜晶系,空间群P-1,晶胞参数a=0.8001 (3) nm,b=1.1245(4) nm,c=1.5129(6) nm,α=89.450(6)°,β=86.297(6)°,γ=77.633(6)°,V=1.3268(9) nm3,Z=2,F(000) =636,最终偏差因子(对Ⅰ＞2σ(Ⅰ)的衍射点),R1=0.0521,wR2 =0.1538,S=1.045.在该结构中,中心Ca(Ⅱ)离子周围形成了一个稍微扭曲的五角双锥体,分别与一个来自奥沙拉秦配体的羧基氧原子(单齿)、两个邻菲罗啉中的两个N原子和四个水分子配位.     

8-氨基喹啉席夫碱锌配合物的合成,晶体结构及发光性质

合成了一个新的锌配合物[Zn(8-ahsb)(N3)](1)(8-ahsb=8-氨基喹啉水杨醛席夫碱阴离子),并对其进行了元素分析、红外光谱和X-射线单晶衍射表征.配合物1属于单斜晶系,空间群为C2/c,a=0.6762(3)nm,b=2. 2842(9)nm,c=1.8162(8)nm,β=91.309(7)°,V=2.805(2)nm3,Z=8.中心离子Zn(II)为三角双锥配位构型,分别与四个N原子、一个氧原子配位,其中1个8-氨基喹啉席夫碱配体提供了2个N原子、一个氧原子,剩余两个N原子分别来自于两个N3-阴离子,且每个N-3桥联邻近的两个Zn2+形成一维无限链状结构.荧光光谱的分析表明该化合物具有强的绿色发光性能,且可作为荧光探针检测低浓度的铜离子.     

Synthesis and Crystal Structure of a New Dinuclear Holmium(III) Complex with a Bulky Anthracene-Based Carboxylate Ligand

Abstract  

The reaction of Ho(NO₃)₃ with the bulky anthracene-9-carboxylic acid (HL) and 1,10-phenanthroline (phen) in the presence of 2,6-dimethylpyridine afforded a dinuclear Ho^III complex [Ho₂(L)₆(phen)₂] (1) (L = anthracene-9-carboxylate), which was characterized by elemental analysis and single-crystal X-ray diffraction analysis (triclinic system, space group Pī, with a = 12.4994(3), b = 13.3556(3), c = 14.9751(3) ?, α = 110.7630(1), β = 103.0680(1), γ = 106.8530(1)°, V = 2080.59(9) ?³, and Z = 1). Complex 1 has a centrosymmetric binuclear cage structure in which two Ho^III atoms are both nine-coordinated and bridged by four bulky anthracnene-9-carboxylate (L) ligands with a non-bonding Ho∙∙∙Ho separation of 3.9076 (2) ?. The anthracene-9-carboxylate groups coordinate each Ho^III atom in three different ways. The adjacent discrete dinuclear subunits are arranged into a one-dimensional (1D) chain along the [111] direction by intermolecular π···π stacking interactions, with the centroid–centroid separation of 3.724(2) ?.     

双配体锌配合物的合成、结构及其荧光与化感调控性能研究

以对氨基苯甲酸、邻菲罗啉和与Zn(Ⅱ)通过溶剂扩散法得到配合物[Zn(C7H6O2N)(C12H8N2)Cl]浅黄色颗粒状晶体,通过元素分析、红外光谱、TG分析等方法对其进行了表征,并对目标配合物的荧光性质进行了探讨.X-射线单晶衍射分析表明,该配合物晶体属于单斜晶系,空间群为C2/c,晶体结构中丰富的氢键将分子连接成三维无限网络结构.生长调节实验表明:该配合物对水稻种子的萌发生长具有明显的调控作用,表现出低浓度下促进高浓度抑制的整体态势.