4′-苯基-2,2′∶6′,2″-三联吡啶镍配合物的合成与晶体结构

运用水热法合成了1个新的配合物[Ni(Phtpy)2](CH3COO)2(化合物1),(Phtpy=4′-苯基-2,2′∶6′,2″-三联吡啶),并通过X-射线单晶衍射方法确定了该化合物的晶体结构.结构分析表明化合物1属于三斜晶系,P-1空间群,晶胞参数a=0.905 60(8)nm,b=1.103 07(9)nm,c=2.020 14(15)nm,α=94.383 0(10)°,β=100.983 0(10)°,γ=106.312 0(10)°,V=1.883 1(3)nm3,Z=2,R1=0.087 2,wR2=0.183 1.配合物中存在3种氢键和多种π-π相互作用,使其成为一个3D配合物.     

基于类salen配体的二苯基锡配合物的合成、抗肿瘤活性及其与DNA相互作用

利用类salen配体二苯乙二酮苯甲酰腙或二苯乙二酮水杨酰腙与二苯基二氯化锡反应,合成了2个二苯基锡配合物[(C_6H_5(O)C=N—N=C(Ph)—(Ph)C=N—N=C(O)—C_6H_5)_2SnPh_2(CH_3OH)]·3CH_3OH (1)和 [(o-OH—C_6H_4(O)C=N—N=C(Ph)—(Ph)C=N—N=C(O)—(o-OH—C_6H_4))_2SnPh_2(CH_3OH)]·CH_3OH (2),通过IR、~1H NMR、~(13)C NMR、~(119)Sn NMR、元素分析、HRMS 以及X射线单晶衍射等表征了配合物结构。测试了配合物1、2的热稳定性及其对癌细胞的体外抑制活性,发现配合物2对癌细胞NCIH460、HepG2、MCF7表现出略优的抑制活性。利用紫外可见吸收光谱、荧光猝灭光谱研究了配合物2与ct-DNA之间的相互作用,结果表明配合物以嵌入模式与DNA结合。     

基于邻香草醛缩2-氨基-4-硝基苯酚的Schiff碱有机锡配合物的合成、晶体结构及生物活性

邻香草醛缩2-氨基4-硝基苯酚(H₂L)分别与二丁基氧化锡、二苄基二氯化锡反应, 合成了二丁基锡Schiff碱配合物(1)和单苄基Schiff碱配合物(2)。配合物经元素分析、¹H NMR、¹³C NMR、IR、UV-Vis表征, 并用X-射线单晶衍射测定了分子结构。研究了配体H₂L及配合物1、2对癌细胞Hela、MCF7、HepG2、Colo205、NCI-H460的抑制活性, 结果表明配合物1对这5种癌细胞的抑制效果优于现有抗癌药物卡铂, 可作为抗癌药物的候选化合物。在Tris缓冲溶液中, 以EB做为荧光探针, 用荧光光谱法研究了配体H₂L及配合物2与鲱鱼精DNA的相互作用, 结果表明配合物与DNA作用主要是由于Schiff碱配体协同效应所致。     

两个有机锡对碘苯甲酸酯的合成、结构、热稳定性和除草活性

在乙醇-苯溶剂中,对碘苯甲酸分别与三苯基氢氧化锡、二丁基氧化锡反应,合成了2个有机锡对碘苯甲酸酯,Ph3Sn(p-IC6H4O2)(1)和{[n-Bu2Sn(p-I-C6H4O2)]2O}2(2)。经IR、1H NMR、元素分析和X射线单晶衍射对配合物进行了表征。配合物1属三斜晶系,空间群为P1,中心锡原子与苯基碳原子、羧基氧原子构成畸型四面体,并且分子间通过氢键和C-I…π共同作用形成二聚体结构;配合物2属单斜晶系,空间群为C2/c,配合物是以Sn2O2构成的平面四元环为中心的二聚体结构,并且分子间通过I…I共同作用形成了一维链状结构。热重分析表明,配合物1和2在230℃以下具有良好的热稳定性。配合物1、2对杂草刺苋(Amaranthus spinosus)、马齿苋(Portulaca oleracea)的抑制活性大于对农作物绿豆的影响,且配合物1的抑制活性高于配合物2的抑制活性,为刺苋、马齿苋除草剂研究提供了一种方法。     

TWO Zn(II)/Cu(II) COMPLEXES BASED ON FLEXIBLE MIXED LIGANDS: SYNTHESES,STRUCTURAL CHARACTERIZATION,AND LUMINESCENCE SENSING OF NITROBENZENE

Journal of Structural Chemistry - Two Zn(II) and Cu(II) complexes formulated as Zn(DMS)(bix)0.5 (1) and Cu(DMS)(bix)0.5 (2) (DMS = 2,2-dimethylsuccinate;...     

Electrochemical Determination of Tyrosine Using Graphene and Gold Nanoparticle Composite Modified Glassy Carbon Electrode

Russian Journal of Electrochemistry - A electrochemical sensor based on graphene and gold nanoparticles modified glassy carbon electrode (GCE) was developed for the determination of tyrosine (Tyr)....     

Synthesis, Crystal Structure and Luminescent Property of the One-dimensional Chain Chlorodibenzyltin 2-Quininate

A one-dimensional chain chlorodibenzyltin 2-quininate has been synthesized and characterized by IR, NMR spectra and elemental analysis. The crystal structure has been determined by X-ray diffraction. The crystal belongs to the monoclinic system, space group I4(—) with a = 19.1171(10), b = 19.1171(10), c = 12.5158(6) , Z = 8, V = 4574.1(4) 3, Dc = 1.477 g·cm-3, μ(MoKα) = 1.252 mm-1, F(000) = 2032, R = 0.0259 and wR = 0.0723. In the complex, the tin atom is six-coordinated to adopt a distorted octahedral configuration with bridging carboxyl of quinoline-2-carboxylic acid. The result of fluorescence spectrum analysis shows that the title complex at room temperature exhibits an intense photoluminescence with maximum emission at 364.2 nm (λex = 303.0 nm).     

Removal of uranium from aqueous solution by using activated palm kernel shell carbon: adsorption equilibrium and kinetics

Activated palm kernel shell carbon (APKSC) was used to remove U(VI) from aqueous solutions in a batch system. The adsorption kinetics, isotherms, and effects of various parameters, such as temperature, contact time, solution pH, adsorbent dosage, and initial U(VI) concentration on the U(VI) adsorption process were studied. Equilibrium was reached after 120 min in the range of studied U(VI) concentrations and temperatures. U(VI) uptake was insignificantly affected by temperature, but was highly pH dependent, and the optimum pH for removal was 5.5. U(VI) removal efficiency increased with the increasing adsorbent dosage. U(VI) sorption capacity increased with increasing initial U(VI) concentration; any further increases in initial U(VI) concentration above a certain point caused insignificant changes in U(VI) sorption capacity. Isotherm data could be described by the Langmuir isotherm model with a maximum U(VI) adsorption capacity of 51.81 mg/g. Kinetic data were fitted to pseudo-first-order and pseudo-second-order equations, which suggested that the U(VI) adsorption onto APKSC was better reproduced by the pseudo-second-order model rather than pseudo-first-order model. Our results indicated that APKSC might be used as a cheap adsorbent in the treatment of uranium-containing wastewater.     

Synthesis and Characterization of Two Binuclear Macrocyclic Zinc(Ⅱ) Complexes by Anion Exchange

Two macrocyclic zinc(II) complexes {[ZnL(VO3)2]·0.33H2O}n(1) and [ZnL(H2O)2][Ni(CN)4](2)(L = 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane) have been obtained from the reactions of [ZnL](ClO4)2 with NH4VO3 and K2[Ni(CN)4], respectively, and structurally characterized by elemental analysis, IR, XRPD, TG and X-ray diffraction. Single-crystal X-ray diffraction analyses indicated that the Zn(II) atom lies on an inversion center and is octahedrally coordinated by four nitrogen atoms of the tetradentate macrocyclic ligand in the equatorial plane and two oxygen atoms of [VO4] tetrahedra in the axial positions in 1, and two oxygen atoms of two water molecules in 2. Complex 1 shows a three-dimensional structure, which is constructed by the links of [VO3]nn- chains with [ZnL]2+, forming one-dimensional channels occupied by guest water molecules. The monomers of [ZnL(H2O)2]2+ and [Ni(CN)4]2- are connected through the intermolecular hydrogen bonds to form a two-dimensional sheet in complex 2.     

Hydrogen bond induced chiral symmetry breaking in the crystallization of nickel(II) complexes

A pair of enantiomers formulated as {Δ-cis-[Ni(en)₂OAc][ClO₄]} _n (Δ-1) and {Λ-cis-[Ni(en)₂OAc][ClO₄]} _n (Λ-1) (en = diaminoethane, OAc^? = acetate anion) were obtained when nickel acetate was reacted with diaminoethane and sodium perchlorate in the absence of any chiral source, whereas the reactions of nickel acetate with 1,3-propanediamine and sodium perchlorate only gave a centrosymmetric complex [Ni(1,3-pn)₂OAc][ClO₄] (2) (1,3-pn = 1,3-propanediamine). Single-crystal X-ray diffraction analyses of all three complexes indicated that the central Ni(II) atoms all have a distorted octahedral coordination geometry, being coordinated by four nitrogen atoms of the diamine ligands, plus two oxygen atoms of OAc^?. In complexes Δ-1 and Λ-1, the monomers of {Δ-cis-[Ni(en)₂OAc]}⁺ and {Λ-cis-[Ni(en)₂OAc]}⁺ are connected through intermolecular hydrogen bonds to generate one-dimensional right- and left-handed homochiral helical chains, respectively, while the monomers of [Ni(1,3-pn)₂OAc]⁺ are linked by similar intermolecular hydrogen bonds to form one-dimensional zigzag chains instead of helical chains. The chiral natures of complexes Δ-1 and Λ-1 have been confirmed by circular dichroism spectroscopy.