Synthesis and Crystal Structure of 5-Methyl- 2-phenyl-4-[（2-p-bromophenylamino）-furylmethylene]-3（2H）-one

A novel 4-heterocyclic acylpyrazolone-based Schiff base compound 5-methyl- 2-phenyl-4-[（2-p-bromophenylamino）-furylmethylene]-3（2H）-one （C21H16N3O2Br） has been synthesized by the reaction of 1-phenyl-3-methyl-4-（α-furoyl）-pyrazolone-5 （HPMαFP） and p-bromoaniline. Elemental analysis, IR spectra and X-ray single-crystal diffraction were carded out to determine the composition and crystal structure of the compound. Crystal data： triclinic system, space group P1^-, a = 9.0936（3）, b = 9.8067（4）, c = 11.6863（4） A, α = 102.512（10）, β = 90.9630（10）, γ = 114.327（10）°, Mr= 422.28, Z= 2, F（000） = 428.0, V= 920.46（11）A^3, Dc = 1.524 g/cm^3,μ = 2.254mm^-1, R = 0.0476 and wR = 0.1318 for 9389 independent reflections （Rint = 0.0122） and 3281 observed reflections （I 〉 2σ（I））. Structural analysis indicates that the compound exists in an amine-one form.     

Enamine Configuration of 5-Methyl-2-phenyl-4-[（Z）-3-tolylamino-phenylmethylene]pyrazol-3（2H）-one

1 INTRODUCTION In contrast to the old-line academic and practical studies of 1-phenyl-3-methyl-4-benzoyl-5-pyrazo- lone (PMBP) on the metal coordination chemistry[1], the complexes of β-ketoamines derivated from PMBP received little attention due to its complicated com- plexation. However, in recent years, there has a sudden growth of this area as a result of its timely interest in biological activities[2]. Recently, a series of β-ketoamines[3] containing PMBP have been prepared fro…     

2-甲基-5-(2-吡啶基)-1,3,4-噁二唑Cu(II),Cd(II)配合物的合成,晶体结构和表征

以2-甲基-5-（2-吡啶基）-1,3,4-噁二唑（L）为配体合成了[Cu₂L₂（μ-Cl）₂Cl₂]（1）和[CdL₂（NO₃）₂]（2）,测定了X射线单晶结构,用红外光谱、紫外光谱、荧光及热重分析进行了表征。配体L和配合物2属于单斜晶系,配合物1属于三斜晶系。L,1和2的空间群分别为P2₁/c,P1和C2/c。配合物1是通过2个氯原子（Cl1,Cl1ⁱ）桥联形成的双桥双核Cu(II)配合物,具有畸变四方锥构型[CuCl₃N₂]。配合物2具有畸变八面体构型[CdN₄O₂]。     

Synthesis and Crystal Structure of （Z）-Methyl-3-methoxy-2-{2-[（4-（E-3-p-tolylacryloyl）phenoxy）methyl]phenyl}acrylate

The title compound,(Z)-methyl-3-methoxy-2-{2-[(4-(E-3-p-tolylacryloyl)phenoxy)-methyl]phenyl}acrylate,was synthesized and determined by X-ray single-crystal diffraction. The crystal belongs to the triclinic system,space group P1 with a = 8.0157(8),b = 12.5748(13),c = 13.3768(14) ,α = 64.770(2),β = 75.720 (2),γ = 89.784(2)°,μ = 0.085 mm-1,Mr = 442.49,V = 1174.1(2) 3,Z = 2,Dc = 1.252 g/cm3,F(000) = 468,T = 294(2) K,R = 0.0603 and wR = 0.1498 for 2644 observed reflections with I 2σ(I). X-ray diffraction analysis reveals that the single crystal contains strong non-classical hydrogen bonds. The preliminary bioassay showed that the title compound exhibits inhibitory activity against the Pseudoperoniospora cubensis and Rhizoctonia solani at the test concentration of 200 mg/L.     

Synthesis and characterization of Co(II), Ni(II) and Cu(II) complexes of 3-[(2,4-dinitrophenyl)hydrazono]butane-2-one oxime

In this study, Co(II), Ni(II) and Cu(II) complexes of 3-[(2,4-dinitrophenyl)hydrazono]butane-2-one oxime were synthesized and characterized by means of IR, UV-Vis, ¹H NMR spectroscopic techniques, magnetic measurements, and elemental analyses. The ligand (HL) behaves as a monoanionic bidentate ligand coordinating via azomethine nitrogen of the hydrazone and the oxime oxygen with the displacement of a hydrogen atom from the oxime group. The text was submitted by the authors in English.     

Synthesis,Crystal Structures,and Magnetic Properties of Two Copper(II) Radical Heterospin Complexes

Two heterospin complexes [Cu(NIT3Py)(cda)H₂O] · H₂O ( 1 ) and [Cu(NIT2Py)(cda)H₂O] · H₂O · CH₃OH ( 2 ) with Cu^II ions and pyridyl‐substituted nitronyl nitroxide radicals (NITxPy = 2‐(x′‐pyridyl)‐4,4,5,5‐tetramethyl‐imidazoline‐1‐oxyl‐3‐oxide, x = 3, 2; H₂cda = 4‐hydroxy‐pyridine‐2,6‐dicarboxylic acid) were synthesized and characterized structurally and magnetically. The single crystal structures show that the two complexes are both two‐spin complexes, in which the different radicals make the two complexes have different hydrogen bonding interactions to form 2D and 1D supramolecular network for complexes 1 and 2 , respectively. The magnetic measurements indicate that complexes 1 and 2 both exhibit antiferromagnetic interactions between Cu^II and radicals.     

3-甲基-1-苯基-4-{4-([5-甲基-2-(4-取代芳基)-噁唑-4-基]甲氧基)-芳亚甲(苄)基}-2-吡唑啉-5-酮的设计、合成与降血糖活性

设计合成了具有降血糖活性的3-甲基-1-苯基-4-[4-[[5-甲基-2-(4-取代芳基)-噁唑-4-基]甲氧基]-芳亚甲(苄)基]}-2-吡唑啉-5-酮类化合物.用丁二酮单肟和(取代的)苯甲醛环合、氯化得到氯甲基噁唑衍生物,与对羟基苯甲醛或香兰醛缩合,再与3-甲基-1-苯基-2-吡唑啉-5-酮进行Knoevenagel反应及催化氢化得到目标化合物(Ⅰ和Ⅱ),共合成了16个未见文献报道的新化合物,并利用元素分析、IR、MS和1HNMR确证了化合物的结构.初步药理试验结果表明,所合成的化合物有抑制血糖升高的倾向以及能明显加强和延长外源性胰岛素的降血糖作用,其中化合物Ⅰb,Ⅰd和Ⅰf尤为突出,说明这类化合物可能有增强胰岛素敏感性的作用.     

Synthesis,Crystal Structures and Magnetic Properties of Three New Polynuclear Cu(II) Complexes Based on the Methoxybenzoate Isomers

In this paper, self-assembly reactions of copper(II) ions, methoxybenzoate isomers and 2,2′-bipyridine yield two copper-oxygen polynuclear complexes: [Cu₂(bpy)₂(2-C₈H₇O₃)₃]·(2-C₈H₇O₃)·14H₂O 1, [Cu₄(bpy)₄(H₂O)(OH)₄]·4(3-C₈H₇O₃)·17H₂O 2, and a simple mononuclear complex [Cu(bpy)(H₂O)(4-C₈H₇O₃)₂] 3. (bpy = 2,2′-bipyridine, C₈H₇O₃ = methoxybenzoate ion). Single crystal X-ray diffraction analyses reval that compound 1 is a dinuclear copper(II) complex which bridged by three carboxylate groups, and 2 presents a discrete step-like tetra-nuclear copper Cu₄O₄ core. Compound 3 shows a square pyramidal mononuclear geometry. The magnetic susceptibility of complex 1 measured from 2 to 300 K, revealed an antiferromagnetic interaction between the Cu(II) ions. Furthermore, the results about IR spectra and thermal analyses were discussed.     

Synthesis,Crystal Structure and Anti-TMV Activity of(Z)-4-[3-(4-Methyl-1,2,3-thiadiazol-5-yl)-3-(4-trifluoromethylphenyl)acryloyl]morpholine

The target compound(Z)-4-[3-(4-methyl-1,2,3-thiadiazol-5-yl)-3-(4-trifluoromethylphenyl)acryloyl]morpholine was synthesized by the nucleophilic substitution,Horner-Emmons reaction,ester hydrolysis,and condensation.Its structure was characterized by NMR,H RMS and single-crystal X-ray diffraction.The crystal of the target compound belongs to monoclinic system,space group P2₁ with a=11.5058(15),b=6.6626(10),c=23.184(3)?,V=1777.3(4)?³,Z=8,D_c=1.496 Mg/m³,F(000)=792 andμ=0.229 mm^–1.X-ray analysis indicated C–H....O intermolecular H-bonds in this crystal structure.The target compound exhibited 53%curative activity against TMV.     

Synthesis,Crystal Structures and Magnetic Properties of Copper(II) Complexes with Nitronyl Nitroxide Radicals

Two new copper(II) compounds with imino nitroxide radicals [Cu(IM‐MeImz)₂ · (SCN)] 0.5[Cu(SCN)₄] ( 1 ) and [Cu(IM‐MeImz)₂ · (SCN)]ClO₄ · H₂O ( 2 ) (IM‐meImz = 2‐(5‐methylimidazol‐4‐yl)‐4,4,5,5‐tetramethyl‐2‐imidazoline‐1‐oxyl) have been synthesized and characterized structurally and magnetically. X‐ray analysis demonstrates that complex 1 contains Cu^II ions in both square‐pyramidal and square planar coordination. There are complete charge separation into [Cu(IM‐MeImz)₂(SCN)]⁺ cations and 0.5[Cu(SCN)₄]^? anions, in a 2:1 ratio. The complex 1 was connected as a one‐dimensional polymer by intermolecular interactions. In complex 2 , the coordination around the copper atom is distorted square pyramidal and the apical position is occupied by one nitrogen atom of SCN^? anion. The 2‐D network structure was formed and arranged through intermolecular H‐bonds interactions. The complex 1 exhibits intramolecular weak ferromagnetic coupling between Cu^II ion and the radicals.     

3-(2-吡啶基)-1,2,4-三唑配体Co(II)Cu(II)和Cd(II)配合物的合成、结构及荧光性质

利用3-（2-吡啶基）-1,2,4-三唑配体（HL）和不同的金属盐设计合成了5个配合物[Co（HL）₂（H₂O）₂]（NO₃）₂（1）、[Cu₂（L）₂（NO₃）₂（H₂O）₄] （2）、[Cu₂（L）₂（AcO）₂（H₂O）₂]·6H₂O （3）、[Cu₂（L）₂（HL）₂（ClO₄）₂]·2CH₃CN （4）和[Cd₂（L）₂（HL）₂（NO₃）₂]·2H₂O （5）,并通过X射线单晶衍射、红外、元素分析、X射线粉末衍射和热重对配合物结构进行了表征。测试结果表明配合物1具有单核结构,并且可以通过氢键的相互作用形成二维超分子结构。配合物2~5为双核结构。配合物2和5可以通过氢键的相互作用形成二维超分子结构。配合物3通过氢键的相互作用形成三维超分子结构。研究了配合物中HL配体的配位模式。此外,研究了配体HL和配合物1和5的固态荧光性质及荧光寿命。     

2-(5-甲基-1,3,4-噻二唑)-硫乙酸锌(II)配合物的合成、晶体结构和性质

合成了2个锌配合物[Zn（mtyaa）₂（H₂O）4]·4H₂O （1）和[Zn（bpe）（mtyaa）₂（H₂O）₂]_n （2）（Hmtyaa=2-（5-甲基-1,3,4-噻二唑）-硫乙酸;bpe=1,2-双（4-吡啶基）乙烷）,用X射线单晶衍射仪测定了配合物的单晶结构,并对它进行了元素分析、红外光谱、热重和粉末X射线衍射等表征。配合物1和2的晶体分别属于三斜晶系和单斜晶系,空间群分别为P1和C2/c。π-π相互作用以及配位水和游离水分子与羧基氧之间的氢键作用将配合物1的单分子结构连成三维网状结构。配合物2中配位水与羧基氧以及配体中的氮原子之间的氢键作用将相邻链连接成二维平面结构。     

Synthesis,Spectroscopic and Magnetic Studies on Metal Complexes of 5-Methyl-3-(2-Hydroxyphenyl)Pyrazole

A tridentate ONN donor ligand, 5-methyl-3-(2-hydroxyphenyl)pyrazole; H₂L, was synthesized by reaction of 2-(3-ketobutanoyl)phenol with hydrazine hydrate. The ligand was characterized by IR, ¹H NMR and mass spectra. ¹H NMR spectra indicated the presence of the phenolic OH group and the imine NH group of the heterocyclic moiety. Different types of mononuclear metal complexes of the following formulae [(HL)₂M][sdot]xH₂O (M=VO, Co, Ni, Cu, Zn and Cd), [(HL)₂M(H₂O)₂] (M=Mn and UO₂) and [(HL)LFe(H₂O)₂] were obtained. The Fe(III) complex, [(HL)LFe(H₂O)₂] undergoes solvatochromism. Elemental analyses, IR, electronic and ESR spectra as well as thermal, conductivity and magnetic susceptibility measurements were used to elucidate the structures of the newly prepared metal complexes. A square-pyramidal geometry is suggested for the VO(IV) complex, square-planar for the Cu(II), Co(II) and Ni(II) complexes, octahedral for the Fe(III) and Mn(II) complexes and tetrahedral for the Zn(II) and Cd(II) complexes, while the UO₂(VI) complex is eight-coordinate. Transmetallation of the UO₂(VI) ion in its mononuclear complex by Fe(III), Ni(II) or Cu(II) ions occurred and mononuclear Fe(III), Ni(II) and Cu(II) complexes were obtained. IR spectra of the products did not have the characteristic UO₂ absorption band and the electronic spectra showed absorption bands similar to those obtained for the corresponding mononuclear complexes. Also, transmetallation of the Ni(II) ion in its mononuclear complex by Fe(III) has occurred. The antifungal activity of the ligand and the mononuclear complexes were investigated.     

Cu(II), Ni(II), and Co(II) Complexes of Tetradentate Azomethine Ligands: Chemical and Electrochemical Syntheses,Crystal Structures,and Magnetic Properties

Russian Journal of Coordination Chemistry - Complexes CuL1 ? MeOH (Ia), NiL1 ? MeOH (Ib), CоL1 ? MeOH (Ic), CuL2 (IIa), NiL2 (IIb), and CоL2 (IIc) of the tetradentate...     

Synthesis,Characterization, and Crystal Structures of [Cu(ca2en)2]ClO4, and [Cu(ca2en)(PPh3)2]ClO4 Complexes

Synthesis, spectroscopy, and crystal structures of [Cu(ca₂en)₂]ClO₄ ( 1 ) and [Cu(ca₂en)(PPh₃)₂]ClO₄ ( 2 ) (ca₂en=N,N′‐bis(trans‐cinnamaldehyde)ethylenediimine) are reported. Compound 1 crystallizes in the orthorhombic space group Pbca, with a=12.5647(7), b=21.8203(11), c=27.992(2) Å, V=7674.3(7) ų, Z=8. Compound 2 crystallizes in the triclinic space group P , with a=13.0540(11), b=14.2935(13), c=14.9863(13) Å, α=84.130(2), β=69.761(2), γ=87.749(2)°, V=2609.8(4) ų, Z=2. The coordination polyhedron about the Cu^I center in the two complexes is best described as a distorted tetrahedron. The ¹H‐NMR and electronic spectra of these complexes are also reported and discussed. The cyclic voltammetry of the complexes indicate a quasireversible redox behavior for complex 1 (E_1/2=0.51 V). However, complex 2 displays an irreversible oxidation wave at 0.91 V. A weak emission is observed for complex 2 in CHCl₃ at room temperature.     

Synthesis, spectroscopic characterizations and quantum chemical computational studies of (Z)-4-[(E)-(4-fluorophenyl)diazenyl]-6-[(3-hydroxypropylamino)methylene]-2-methoxycyclohexa-2,4-dienone

In this study, the molecular structure and spectroscopic properties of the title compound were characterized by X-ray diffraction, FT-IR and UV-vis spectroscopies. These properties were also investigated using DFT method. The most convenient conformation of title compound was firstly determined. The geometry optimizations in gas phase and solvent media were performed by DFT methods with B3LYP adding 6-31G(d) basis set. The differences between crystal and computational structures are due to crystal packing in which hydrogen bonds play an important role. UV-vis spectra were recorded in different organic solvents. The results show that title compound exists in both keto and enol forms in DMSO, EtOH but it tends to shift towards enol form in benzene. The polar solvents facilitate the proton transfer by decreasing the activation energy needed for Transition State. The formation of both keto and enol forms in DMSO and EtOH is due to decrease in the activation energy. TD-DFT calculations starting from optimized geometry were carried out in both gas and solution phases to calculate excitation energies of the title compound. The non-linear optical properties were computed at the theory level and the title compound showed a good second order non-linear optical property. In addition, thermodynamic properties were obtained in the range of 100-500K.