Synthesis,crystal structure and bioactivity of a novel linear trinuclear nickel(II) complex

A novel linear trinuclear nickel(II) complex, [Ni₃(H₂O)₂(DMA)₂(acbshz)₂]·2DMF (DMA = dimethylamine; acbshz = N-acryloyl-5-bromosalicylhydrazide), has been prepared by self-assembly approach. The three nickel atoms arrange in a strictly linear structure, adjacent molecules are linked by intermolecular H bonds to form a 2D infinite wave-like structure. Antibacterial screening data indicate the formation of the trinuclear complex reduced the antimicrobial activity of the ligand.     

配合物Ni（bacbh）2（Py）2的合成、晶体结构及热稳定性

以苯亚甲基苯乙酮-4-氯苯甲酰腙为配体,水热合成了一个镍的单核配合物Ni(bacbh)2(Py)2(bacbh:苯亚甲基苯乙酮-4-氯苯甲酰腙;Py:吡啶),并利用元素分析、红外光谱、X射线单晶衍射及热失重分析对配合物进行了表征。该配合物为单斜晶系,空间群为P2(1)/n,晶胞学数据:a=1.344 3(6)nm,b=2.471 7(12)nm,c=1.465 1(7)nm,β=98.47°,V=4.815(4)nm3,Z=4,μ=0.561 mm-1,Dc=1.292 mg/m3,F(000)=1 944,最终偏离因子[I>2sigma(I)]R1=0.038 6,wR2=0.096 1(all data),GOF=1.007(CCDC:840865)。     

Synthesis,crystal structure and photophysical properties of a novel Pt(II) complex with multi-functionalized cyclometalating ligand

A novel Pt(II) complex [(L)PtCl] (HL = 4-{p-[N-(4-(9-carbazole))butyl-N-phenyl] aniline}-6-phenyl-2,2′-bipyridine) has been synthesized and verified by ¹H NMR, elemental analysis and X-ray crystallography. The crystal (C₄₄H₃₅N₄ClPt, M_r = 850.30) belongs to monoclinic system, space group P2(1)/c, with a = 21.864(6), b = 9.306(3), c = 17.240(5) Å, β = 96.483(6)°, Z = 4, V = 3485.3(16) ų, D_C = 1.620 g/cm³, μ(Mo-Kα) = 4.141 mm^? 1, F(000) = 1688, R₁ = 0.0591, wR₂ = 0.0976. The coordinate geometry of the Pt atom is a distorted square planar configuration. The complex molecules are stacked by a weak π–π interaction in a head-to-tail fashion along the b axis to form 1D chain and the alternating 1D chains are packed to form the 2D lamellar system. The complex shows an intense metal-to-ligand charge transfer (¹MLCT) (dπ(Pt) → π*(L)) transitions (ε ～ 2 × 10⁴ dm³ mol^? 1 cm^? 1) at 448 nm in the UV–Vis absorption spectrum and a strong phosphorescence at 592 nm in CH₂Cl₂ solution at room temperature. An intramolecular energy transfer process from the carbazole unit to the arylamine-modified [(C^N^N)PtCl] emissive center exists in the complex.     

Synthesis, characterization and crystal structure of a novel thiocyanate–ruthenium(II) complex

The cis-[Ru(dppb)(Me-bipy)(NCS)₂], dppb = 1,4-bis (diphenylphosphino)butane, Me-bipy = 4,4′-dimethyl-2,2′-bipyridine, and NCS = thiocyanate, was synthesized and characterized by spectroscopic and electrochemical techniques and its structure was determined by crystal X-ray analysis. The crystal structure reveals that the coordination geometry around the Ru(II) center is distorted octahedron where two molecules of thiocyanate are bonded to the ruthenium through nitrogen atom in cis orientation. The half-wave formal potential value E_1/2 = 0.8 V (versus Ag/AgCl) observed is considerable higher than that for the cis-[RuCl₂(dppb)(Me-bipy)] complex, E_1/2 = 0.6 V (versus Ag/AgCl), well illustrating the strong π-acceptor effect the NCS ligand toward the backbonding interaction with the Ru(II) metal center. The MLCT absorption bands of the thiocyanate complex present a higher molar absorptivity (about 12%) compared with the cis-[RuCl₂(dppb)(Me-bipy)] complex, in the same experimental conditions. These properties make the complex potentially promising for the photosensitization process.     

Synthesis,crystal structure and magnetic characterization of a dinuclear Mn(II) complex with double end-on azide ligands

A new dinuclear manganese(II) complex [MnL(N₃)₂]₂ · 2CH₃OH 1 has been synthesized and characterized crystallographically and magnetically. L is a tridentate Schiff base ligand which is derived from the reaction of pyridine-2-carbaldehyde and 2-aminoethylbenzimidazole. In the complex 1, each Mn(II) ion is coordinated by one L, one terminal azide ligand and symmetrical double end-on bridging azide ligands. The intermolecular hydrogen bonds extend the structure into a two-dimensional layer. Magnetic determination of 1 indicates that ferromagnetic exchange interaction between the two manganese(II) ions exist in this complex through the double end-on azide bridges.     

Synthesis,crystal structure and DNA-binding studies of a Ru(II) complex containing two main ligands

A new Ru(II)-polypyridyl complex, [Ru(L)(dppz)₂](PF₆)₄ (L = 5,5′-di(1-(trimethylammonio)methyl)-2,2′-dipyridyl cation; dppz = dipyrido[3,2-a:2′,3′-c]phenazine]), has been synthesized and structurally characterized. The binding of this complex with calf thymus DNA (CT-DNA) has been investigated by spectroscopic and viscosity measurement. Results indicate that the complex binds to CT-DNA via an intercalative mode. Moreover, the complex reveals a highly efficient DNA cleavage activity upon irradiation at 365 nm, during which supercoiled pBR322 DNA was converted to nicked DNA.     

Synthesis and crystal structure of three dimensional complex from copper(II) and 1,2,4,5-benzenetetracarboxylate

A copper(II) complex {[Cu(H₂btc) (H₂O)₃]₂(H₄btc)(C₅H₁₁N)₂ · 3H₂O}_n (1) has been synthesized and characterized structurally (H₄btc=1,2,4,5-benzenetetracarboxylic acid). Open channels were formed and can accommodate piperidine molecules. TGA data show that guest water and piperidine molecules are lost at 130 °C.     

Synthesis, crystal structure and luminescent properties of a thiocyanato bridged two-dimensional heteronuclear polymeric complex of cadmium(II) and copper(II)

A novel heteronuclear polymeric complex Cd(SCN)₃Cu(en)₂NO₃ (1) (en = ethylenediamine) has been synthesized and structurally characterized. The Cd(II) atom is surrounded by three S atoms and three N atoms from four 1,3-μ-SCN⁻ and two 1,1,3-μ-SCN⁻ to attain a distorted octahedral coordination geometry. Six Cd(II) centers are linked by twelve thiocyanato bridges to form hexagonal metallocyclic unit [Cd₆(SCN)₁₂] and extend a 2D network. Moreover, a 1,1,3-μ-SCN⁻ links two cadmium and one copper metal atoms. The luminescent properties of 1 in the solid state were investigated.     

2-甲基咪唑-4,5-二羧酸镍配合物的合成及其晶体结构

以配体2-甲基咪唑-4,5-二羧酸与氯化镍反应,合成出了一个新的配合物[Ni(HMIDC-)]2(H2O)2]n;采用单晶X射线衍射方法测定了配合物的晶体结构。结果表明,所合成的配合物属正交晶系,pbca空间群,晶胞参数a=0.683 74 nm,b=1.388 13 nm,c=1.655 19 nm,V=1 570.97 nm3,Z=4,Dc=1.831 g/cm3,F(000)=1 000.0,GOF=1.304。镍原子与两个不同配体H2MIDC中的咪唑上的氮原子、羧基氧原子以及水分子配位,且形成了六配位八面体构型。配合物由分子间氢键构筑成了三维超分子氢键网络结构。     

Synthesis and X-ray crystal structure of a heteroleptic tris-cyclometalated iridium(III) complex

A convenient synthesis of the tris-cyclometalated complex [Ir(ppy)₂(nppy)] (2, ppy = 2-phenylpyridyl, nppy = 2-(4-nitrophenyl)pyridyl) from [{Ir(μ-Cl)(ppy)₂}₂] (1), the ligand 2-(4-nitrophenyl)pyridine, and silver trifluoroacetate as halide abstractor in refluxing methoxyethanol is described. The crystal and molecular structure of 2 was determined by a single-crystal X-ray diffraction study.     

Twisted dinuclear Pd(II) complex with an exo-hexadentate ligand bearing bipyridine and carbamoly groups: Synthesis and structure

Dinuclear Pd(II) compound, [Pd₂(PMCB²⁻)Cl₂] · CH₂Cl₂ (1), has been prepared by the reaction of K₂[PdCl₄] with exo-hexadentate ligand having amide groups (3,3′-bis[N-(2-pyridylmethyl)carbamoly]-2,2′-bipyridine, H₂PMCB) in H₂O/CH₂Cl₂. X-ray crystal structure of 1 indicates that one PMCB²⁻ ligand binds two Pd(II) ions each having a distorted square planar structure. The bipyridine group of the PMCB²⁻ ligand is involved in offset face-to-face π–π interactions, which gives rise to a 1D chain. The 1D chains are linked together via the C–H⋯O hydrogen bondings between a carbon atom of pyridine group and the oxygen of carbamoly group to generate a 2D network. Between the 2D networks there exist the herringbone π–π stackings, which results in a 3D supramolecular structure.     

Synthesis,characterization and crystal structure of one Cu(II) complex with flexible tetrapyridine and fatty acid ligand

One new title compound [Cu₂(TPOM)(adi)₂]_n · 4nH₂O (1) (TPOM = tetrakis(4-pyridyloxymethylene)methane, adi = adipic acid) has been synthesized under hydrothermal condition. The title compound was characterized by IR spectra, thermal analysis, single crystal and powder X-ray diffraction.     

Synthesis,crystal structure and relevant antiproliferative activity against Toxoplasma gondii of a new binuclear Co(II) complex

The crystal structure of [(HPClNOL)Co(-μ-Cl₂)Co(HPClNOL)](ClO₄)₂ 1 (HPClNOL: 1-(bis-pyridin-2-ylmethyl-amino)-3-chloropropan-2-ol) revealed a distorted octahedral geometry around both Co(II) centers. The coordination plane comprised one tertiary amine, one alcohol in the protonated form and two chloride which link the two Co(II) centers, resulting in the binuclear arrangement. Two pyridine nitrogen atoms are coordinated and occupy the axial sites. Investigations in solid state and in solution (dimethylformamide) carried out by electronic spectroscopy suggest that the arrangement in the solid state changes in solution. Furthermore, ESI(+)-MS and conductivimetry studies indicated the formation of mononuclear species in solution in agreement with the lability of the chloride ligands. Complex 1 reduced the growth of Toxoplasma gondii infecting LLC-MK2 host cells. After treatment this complex reduced T. gondii growth by 55%, the ligand HPClNOL had no effect on parasite growth and sulfadiazine (SDZ), traditional terapeutic compound for this parasite, was effective only after 48 h of treatment. These results suggest the relevance of the cobalt ion on the anti-toxoplasma activity.     

Synthesis and X-ray crystal structure of a bis-cyclometalated phosphorescent red-emitting iridium(III) complex

The synthesis of the bis-cyclometalated complex [{Ir(μ-Cl)(ccpz)₂}₂] (1, cppz = 1-chloro-4-(4-chlorophenyl)-phthalazine) from hydrated iridium(III) chloride and the ligand ccpz in refluxing ethoxyethanol is described. Compound 1 was characterized by spectroscopic means and the crystal structure was determined by X-ray crystallography. The absorption and emission spectra exhibit the new compound as a red-emitting phosphorescent complex.     

New μ-oxo-bridged tetranuclear Cu(II) complex with Schiff-base ligand: Synthesis,crystal structure and magnetic properties

A new μ-oxo-bridged Cu(II) complex with cubane-like tetranuclear copper(II) complex, [Cu₄(L¹)₄] · 4H₂O (1) (H₂L¹ = 2-(3-methoxy-salicylidene-amino)-benzyl-alcohol), has been prepared, and structurally characterized by X-ray crystallography. Complex 1 crystallized in the monoclinic space group P₂₁/n and has a tetranuclear core of Cu₄O₄. The temperature dependence of magnetic susceptibility measurements shown that complex 1 exhibits a strong antiferromagnetic interaction with J = −103.4 cm⁻¹.     

Synthesis and crystal structure of scandium(III) and cadmium(II) thiocyanato complexes with dimethylsulfoxide

Two novel complex compounds, molecular fac-[Sc(NCS)₃(DMSO)₃] and polymeric chain [Cd(NCS)_4/2(DMSO)₂]_∞ (DMSO = dimethylsulfoxide), were synthesized and structurally characterized. In both complexes, the metal atoms have octahedral coordination with the NCS⁻ ion serving two different functions: as a terminal ion with the coordination via N in Sc complex and as a bridge ligand with the coordination via N and S in the case of Cd compound, respectively. The DMSO ligands are coordinated by oxygen atoms.     

Synthesis and characterization of nickel(II) and copper(II) complexes with a tetramethyltetraaza macrocycle containing 2-pyridylmethyl pendant arms

The complexes [Ni(L²)](ClO₄)₂·H₂O (1) and [Cu(L²)]Cl₂·4H₂O (2) have been synthesized and characterized by X-ray crystallography, electronic absorption and cyclic voltammetry. The crystal structure of 1 reveals a distorted octahedral geometry with four nitrogen atoms of the macrocycle and two nitrogen atoms of the pendant pyridylmethyl groups. The structure of 2 shows that the complex is centrosymmetric and the metal center has a tetragonally distorted octahedral environment. The electronic spectra and electrochemical behaviors of the complexes are significantly affected by the presence of the pendant arms.