基于2-苯基-4-硒唑甲酸镍配合物的合成、晶体结构及生物活性

由2-苯基-4-硒唑甲酸(HL,C10H7O2NSe)、硫酸镍和乙二胺(en)合成了相应的配合物[Ni(en)3](L)2.3H2O。用元素分析、红外光谱、热重分析等表征手段确定了配合物的组成;用单晶X-射线衍射测定了配合物的晶体结构。配合物C26H42N8NiO7Se2属于三斜晶系,空间群P1,晶胞参数:a=1.15673(3)nm,b=1.21755(3)nm,c=1.26326(3)nm,α=86.096(2)°,β=89.461(1)°,γ=69.321(1)°,晶胞体积:V=1.66046(7)nm3,晶胞内结构基元数Z=2,式量Mr=795.29。用溴化乙锭荧光探针法研究了配合物与DNA的相互作用。考察了配体和配合物对大肠埃氏杆菌(E.coli JM109)、大肠杆菌(E.coli DH5α)、表皮葡萄球菌(S.epidermidis)、金黄色葡萄球菌(S.aureus)、鲍曼不动杆菌(baumanii)、草绿色链球菌(S.viridans)六种细菌的抗菌活性及对正常细胞293T和肿瘤细胞RAW 264.7的体外增殖抑制作用。     

2-苯基-4-硒唑甲酸铜(Ⅱ)配合物的合成、晶体结构和生物活性

采用溶液法合成了一种新型铜(Ⅱ)配合物[Cu2(NO3)2L(phen)2(H2O)]NO3(HL=2-苯基-4-硒唑甲酸,phen=1,10-邻菲啰啉)。用元素分析、红外光谱等表征手段确定了配合物的组成;用单晶X-射线衍射测定了配合物的晶体结构。配合物C34H24Cu2N8O12Se属于三斜晶系,空间群P1。用溴化乙锭荧光探针法研究了配合物与DNA的相互作用。分别考察了配体和配合物对五种细菌:大肠埃氏杆菌(E.coli),表皮葡萄球菌(S.epidermidis),草绿色链球菌(S.viridans),金黄色葡萄球菌(S.aureus),鲍曼不动杆菌(A.baumanii)的抗菌活性。同时也考察了配体和配合物对人类胰腺癌PANC-28细胞和人类肝癌HuH7细胞的体外增殖抑制作用。实验结果表明配合物具有良好的生物活性。     

1-对氯苯基-3-苯基-4-苯甲酰基-吡唑啉酮-5缩胺类席夫碱铜配合物的合成与抑菌活性

合成了7种新型酰基吡唑啉酮席夫碱过渡金属铜配合物.7种席夫碱分别为:1-对氯苯基-3-苯基-4-苯甲酰基-吡唑啉酮-5缩苯胺(HS1)、对氯苯胺(HS2)、对溴苯胺(HS3)、糠胺(HS4)、对甲氧苯胺(HS5)、对乙氧苯胺(HS6)和萘胺(HS7)席夫碱.由元素分析、络合滴定法、质谱和摩尔电导值确定配合物的组成通式为[Cu(S)2](S=S1,S2,S3,S4,S5,S6,S7),通过红外光谱、热重谱、核磁共振氢谱和液相色谱-质谱联用技术对配体及配合物的结构进行了表征,同时对7个席夫碱配体及其7个铜配合物的抑菌活性进行了初步研究.表征结果表明:在不同的测试条件下,7个配体的异构体存在方式不同.配位时酮式结构可能转化为烯醇式结构,按去质子方式以烯醇氧负离子和亚胺基氮原子双齿形式与铜中心离子成键.抑菌实验结果显示:所有化合物对受试的4个菌种均有不同程度的抑菌活性,其中配合物普遍强于配体.抑菌能力呈现浓度效应,在浓度为3.0mg·mL-1时最大直径可达16.0mm.     

新型含2,5-二-（3,5-二甲基吡唑-4-巯基）-1,3,4-噻二唑-M(M=Co2+,Cd2+,Mn2+)配合物的合成、晶体结构及其抑菌活性研究

将配体L[2,5-二-(3,5-二甲基吡唑-4-巯基)-1,3,4-噻二唑]与Co(NO3)2 6H2O,Cd(NO3)2 4H2O和MnCl2 4H2O进行配位反应,得到三个配合物[Co(L)2(H2O)4](NO3)2 4(CH3CH2OH)(1),[Cd(L)2(H2O)4](NO3)2 4(CH3CH2OH)(2),[Mn(L)2(Cl)2(CH3OH)2]2(CH3OH)(3),并用元素分析,FT-IR和X射线单晶衍射进行了表征.分析结果表明,配体L呈"U"形,配合物1～3呈"S"形.配合物中Co(II),Cd(II),Mn(II)的配位环境均为扭曲八面体,每个金属离子同时和两个配体进行配位.配体和配合物体外抑菌活性研究结果表明,配体及其配合物都有一定的抑菌活性.     

2-氨甲基-1H-苯并咪唑钴(Ⅱ)和镍(Ⅱ)配合物的合成、晶体结构和抑菌活性(英文)

利用双齿配体2-氨甲基-1H-苯并咪唑(AMBI)和硫氰酸钾以及硝酸钴或硝酸镍在甲醇-水中反应制备了2个新的异质同晶配合物trans-[M(AMBI)2(NCS)2](1:M=Co2+,2:M=Ni2+)。X-射线衍射单晶结构表明:2个配合物属于单斜晶系,C2/c空间群,M(Ⅱ)与来自AMBI的4个氮原子和异硫氰酸根的2个氮原子配位,形成八面体结构。配合物中的N-H…S氢键和π-π相互作用将配合物连接成三维网络结构。用红外光谱、紫外-可见光谱对配合物1和配合物2进行了表征,并对配合物的热稳定性做了研究。选取金黄色葡萄球菌和大肠杆菌作为抑菌菌种,研究了配体AMBI和2个配合物的抑菌能力。     

4-(4′-吡啶)-1,3-二硫代环戊烯-2-酮双核铜(Ⅱ)配合物的合成与晶体结构

用溶液法合成了4-(4′-吡啶)-1,3-二硫代环戊烯-2-酮(C8H5NOS2)与铜(Ⅱ)的配合物,并得到了单晶.通过红外光谱、元素分析和X射线单晶衍射分析对配合物的组成和结构进行了表征.X射线单晶衍射分析表明:配合物属三斜晶系,空间群P-1,是由2个CuSO4、4个配体C8H5NOS2分子、2个配位H2O和6个游离的H2O组成的双核配合物.配合物分子通过S…S短程作用形成了1个二维层状结构,并通过分子间的氢键作用进一步形成了更稳定的三维结构.     

O, O′-二(对叔丁基苯基)二硫代磷酸根双核铅配合物的合成、晶体结构、热稳定性和抑菌活性研究

合成了双核铅配合物[Pb2(S2P(OR1)2)2(μ-S2P(OR1)2)2](R1=对叔丁基苯基),用元素分析、红外光谱、紫外-可见光谱、热重分析和X-射线衍射法进行了结构表征。晶体结构研究表明:配合物为双核结构,形成了具有椅式构型的八元环[Pb2S4P2],且芳环对Pb原子有弱的π配位作用,Pb原子处于Pb(S5ArE)的畸变缺位五角双锥(ψ-PB)环境中。测定了原料(R1O)2PS2NH2Et2和配合物对大肠杆菌(E.Coli)、枯草杆菌(B.Subtilis)和金色葡萄球菌(S.Aureus)的抑菌活性,结果表明:原料和配合物对3种细菌均有抑制作用,配合物对大肠杆菌和枯草杆菌的抑菌活性优于原料。     

2-苯基-4-硒唑甲酸的铜(Ⅱ)配合物的合成、晶体结构和生物活性

采用水热法合成了一种新型铜(Ⅱ)配合物[Cu₂(NO₃)₂L(phen)₂(H₂O)] NO₃(HL=2-苯基-4-硒唑甲酸, phen=1,10-邻菲啰啉)。用元素分析、红外光谱等表征手段确定了配合物的组成;用单晶X-射线衍射测定了配合物的晶体结构。配合物C₃₄H₂₄Cu₂N₈O₁₂Se属于三斜晶系, 空间群P1。用溴化乙锭荧光探针法研究了配合物与DNA的相互作用。分别考察了配体和配合物对五种细菌:大肠埃氏杆菌(E.coli), 表皮葡萄球菌(S.epidermidis), 草绿色链球菌(S.viridans), 金黄色葡萄球菌(S. aureus), 鲍曼不动杆菌(A.baumanii)的抗菌活性。同时也考察了配体和配合物对人类胰腺癌PANC-28细胞和人类肝癌HuH7细胞的体外增殖抑制作用。实验结果表明配合物具有良好的生物活性。     

含O,O’-二(对甲苯基)二硫代磷酸的双核铅配合物的晶体结构、谱学性质和抑菌活性

合成了双核铅配合物{Pb2[S2P(OC6H4Me-p)2]2[μ-S2P(OC6H4Me-p)2]2},并用元素分析、红外光谱、紫外-可见光谱、热重分析和X射线衍射对其进行了结构表征.结果表明,该晶体属于三斜晶系,P1空间群,晶胞参数a=1.06393(6)nm,b=1.15005(6)nm,c=1.45006(5)nm,α=94.109(3)°,β=98.833(4)°,γ=109.242(5)°,V=1.64099(14)nm3,Dc=1.671 Mg.m-3,Z=1,F(000)=808,μ(Mo Kα)=5.523mm!1,S=1.024,R1=0.0596,wR2=0.1464[I〉2σ(I)].该配合物形成了具有椅式构型的八元环[Pb2S4P2],每个Pb原子与1个螯合双齿配体(p-MeC6H4O)2PS-2的2个S原子和2个桥三齿配体μ-(p-MeC6H4O)2PS-2的3个S原子配位,Pb1—S的键长在0.2750～0.3257 nm范围内.芳环对Pb原子有弱的π配位作用[Pb1…Cig为0.3365(2)nm].Pb原子处于Pb(S5ArE)(E代表孤对电子)的畸变缺位五角双锥(Ψ-PB)环境中,1个S原子和1个芳环位于Ψ-PB的轴向位置[键角S1—Pb1—Cig为173.79(5)°],4个S原子和Pb原子的一对立体化学活性的孤对电子占据Ψ-PB的赤道位置.配合物热稳定性高,在287.1℃开始分解.与原料(p-MeC6H4O)2PS2NH2Et2比较,配合物对葡萄球菌(Staphylococcus)、大肠杆菌(E.Coli)和枯草杆菌(B.Subtilis)具有更好的抑菌活性.     

氨基酸席夫碱镍、钴配合物的合成、晶体结构与抑菌活性

合成了1-苯基-3-甲基-4-对氯苯甲酰基-5-吡唑啉酮缩L-苯丙氨酸甲酯Schiff碱Ni(Ⅱ)、Co(Ⅱ)配合物[NiL_2](CH_3OH)(1)和[CoL_2](CH_3OH)(2)。用元素分析、红外光谱和X-射线单晶结构进行了表征,配合物1和2的晶体结构都同时含有两个独立子单元及一个游离的甲醇分子,各子单元都形成六配位的八面体结构。采用琼脂扩散法测定了配体和配合物对大肠杆菌、金黄色葡萄球菌抗菌活性,结果表明配合物2对大肠杆菌的抑制作用最强。     

Syntheses,Crystal Structures and Antibacterial Activities of Complexes [（C_9H_（18）NS_2）_3M（Ⅲ）]（M = Sb and Bi）

Two novel complexes,[(C9H18NS2)3Sb(III)](1) and [(C9H18NS2)3Bi(III)](2),were synthesized and characterized by elemental analysis,IR,TG and X-ray single-crystal diffraction.Both 1 and 2 crystallize in the monoclinic system,P21/c space group.The data for 1:a = 1.6964(3),b = 1.02149(17),c = 2.5650(3) nm,β = 121.824(8)°,Z = 4,V = 3.7766(10) nm3,Dc = 1.293 g·cm-3,F(000) = 1536,μ = 1.082 mm-1,the final R = 0.0500,wR = 0.1562 and S =1.072.The data for 2:a = 1.6802(9),b = 1.0256(6),c = 2.5083(10) nm,β = 121.77(3)°,Z = 4,V = 3.675(3) nm3,Dc = 1.486 g·cm-3,F(000) = 1664,μ = 5.159 mm-1,the final R = 0.0481,wR = 0.1055 and S =1.076.The coordinated geometry of the central M(III) with six sulfur atoms from three ligands is a distorted pentagonal pyramid configuration.The dimer structural system is formed by the weak interactions of M…S and C-H…S between two molecules.The complexes were valued for their antibacterial activities by agar-streak method.It was found that 1 is active against the four test bacterial organisms.     

Synthesis,antimicrobial, antiquorum-sensing and cytotoxic activities of new series of benzothiazole derivatives

New series of benzothiazole derivatives were designed and synthesized. The newly synthesized compounds were screened for their antibacterial activity against Escherichia coli, Staphylococcus aureus and Bacillus cereus. Compounds 6j and 6o showed the highest activity against E. coli and S. aureus. The antifungal activity of these compounds was also tested against Candida albicans and Aspergillus fumigatus293. Compounds 4c, 4g and 6j exhibited the highest activity against C. albicans. In addition, compounds4 a and 6j displayed promising activity against A. fumigatus 293. The same compounds were examined for their antiquorum-sensing activity against Chromobacterium violaceum ATCC 12472, whereas compounds4 a, 6j and 6p showed moderate activity. The in vitro cytotoxicity testing of the synthesized compounds was performed against cervical cancer(Hela) and kidney fibroblast cancer(COS-7) cell lines. Results indicated that all tested compounds have IC50 values 50 mmol/L against both cell lines. Molecular properties, toxicities, drug-likeness, and drug score profiles of compounds 4a–c, 5a, 6g,h, 6j, 6l, 6o and7 c,d were also assessed.     

Three new megastigmane glucopyranosides from the Cardamine komarovii

Three new megastigmane glucopyranosides, komaroveside A [(3S,4R,5Z,7E)-3,4-dihydroxy-5,7-megastigmadien-9-one-3-O-β-D-glucopyranoside] (1), komaroveside B [(3S,4S,5S,6R,7E)-5,6-epoxy-3,4-dihydroxy-7-megastigmen-9-one-3-O-β-D-glucopyranoside] (2) and komaroveside C [(3S,4S,5S,6R,7E,9S)-5,6-epoxy-3,4,9-trihydroxy-7-megastigmen-3-O-β-D-glucopyranoside] (3) were isolated, together with eight known compounds, from Cardamine komarovii. The identification of these compounds and the elucidation of their structures were based on 1D- and 2D-NMR spectral data analysis. The isolated compounds were tested for their cytotoxicity against four human tumor cell lines (A549, SK-OV-3, SK-MEL-2, HCT15) in vitro using the sulforhodamine B bioassay.     

镨配合物的热化学及其对酵母菌作用的热动力学研究

用六水合氯化镨、硫代脯氨酸(C4H7NO2S)和水杨酸(C7H6O3)合成了三元固体配合物[Pr(C7H5O3)2(C4H6NO2S)]-2H2O.根据盖斯定律设计一个热化学循环,用溶解-反应量热法研究得到合成反应的标准摩尔焓变为(133.70±1.02)kJ/mol,配合物298.15K时的标准摩尔生成焓为-(2909.3±3.2)kJ/mol.用TAMair微量热仪测定其在28.00℃时对粟酒裂殖酵母作用的产热曲线,进而算出在配合物作用下,酵母菌生长代谢的最大发热功率Pmax、速率常数κ、传代时间tG、抑制率I和半抑制浓度cI,50等热动力学参数.结果表明:稀土水杨酸硫代脯氨酸配合物在低浓度下对酵母菌有刺激作用,高浓度下为抑制作用,即稀土配合物对微生物的生长具有双向生物效应,也称为Hormesis效应.     

四氯合钴(Ⅱ)-4-氯苄基吡啶季铵盐的制备及其晶体结构和抗菌性能

合成了1种含四氯合钴配阴离子的4-氯苄基吡啶季铵盐[4-ClBzPy]2[CoCl4];利用元素分析仪、X射线单晶衍射仪以及紫外光谱仪和红外光谱仪等分析了其组成、晶体结构及光谱学性质;利用电导仪测定了[4-ClBzPy]2[CoCl4]的电导,并检测了其对金黄色葡萄球菌和大肠杆菌的抗菌活性.结果表明,合成的[4-ClBzPy]2[CoCl4]季铵盐为单斜晶系,P2(1)/c空间群,晶胞参数为a=0.769 5(13)nm,b=1.895 1(3)nm,c=0.946 3(15)nm,β=93.183(2)°,V=1.378 0(4)nm3,Z=2,Dc=1.470g/cm3,GOOF=1.007,R1=0.041 8,wR2=0.100 2.与此同时,季铵盐[4-ClBzPy]2[CoCl4]对金黄色葡萄球菌和大肠杆菌均具有较好的抗菌活性.     

Synthesis and in vitro antimicrobial screening of new pyrano[4,3-b]pyrane derivatives of 1H-pyrazole

A new series of pyrano[4,3-b]pyrane 4a-l bearing 1H-pyrazole has been synthesized by one pot base catalyzed cyclocondensation reaction of 1H-pyrazole-4-carbaldehyde la-1,malononitrile 2 and 4-hydroxy-6-methylpyrone 3.All the synthesized compounds were screened against six bacterial pathogens,namely B.subtilis,C.tetani,S.pneumoniae,S.typhi,V.cholerae, E.coli and antifungal activity against,two fungal pathogens,A.fumigatus and C.albicans using broth microdilution MIC method. Some of the compounds are found to be equipotent or more potent than that of commercial drugs,against most of employed strains.     

Synthesis and biological activity of novel amino acid-(N'-benzoyl) hydrazide and amino acid-(N'-nicotinoyl) hydrazide derivatives

The coupling reaction of benzoic acid and nicotinic acid hydrazides with N- protected L-amino acids including valine, leucine, phenylalanine, glutamic acid and tyrosine is reported. The target compounds, N-Boc-amino acid-(N;-benzoyl)- and N- Boc-amino acid-(N;-nicotinoyl) hydrazides 5a-5e and 6a-6e were prepared in very high yields and purity using N-[(dimethylamino)-1H-1,2,3-triazolo[4,5-b]pyridin-1-yl- methylene]-N-methyl-methanaminium hexafluorophosphate N-oxide (HATU) as coupling reagent. The antimicrobial activity of the Cu and Cd complexes of the designed compounds was tested. The products were deprotected affording the corresponding amino acid-(N;-benzoyl) hydrazide hydrochloride salts (7a-7e) and amino acid-(N;- nicotinoyl) hydrazide hydrochloride salts (8a-8e). These compounds and their Cu and Cd complexes were also tested for their antimicrobial activity. Several compounds showed comparable activity to that of ampicillin against S. aureus and E. coli.     

有机-无机复合杂多化合物的合成、结构及表征

利用常规水溶液法制备了三种基于饱和Keggin结构阴离子的有机-无机复合杂多化合物[Pr(pydc)(H2O)6]2H[PMo12O40]·4H2O(1)、[Nd(pydc)(H2O)6]2H[PMo12O40]·4H2O(2)和[Tb(pydc)(H2O)6]2H[PMo12O40]·4H2O(3)(pydc=2,6...     

由癸二酸柔性配体构筑的包裹水分子的多孔过渡金属配合物的合成及与DNA作用

以柔链配体癸二酸（C10H18O4）为第一配体、邻菲啰啉（phen）为第二配体合成了三个过渡金属配合物[Mn2（C10H16O4）2（phen）4（H2O）].4H2O（1）、[Cu（C10H16O4）（phen）（H2O）].3H2O（2）、[Cd（C10H16-O4）（phen）].3H2O（3）.用元素分析、红外光谱、热重分析等手段表征了配合物;用单晶X射线衍射测定了配合物的结构;其中配合物1和2为癸二酸根桥连的双核结构,配合物3为含有双核节点的配位聚合物.在配合物1中发现了水分子的二聚体,在配合物2中则发现了一维水链,并在配合物3中发现了四元环的六聚水,这些片断通过氢键作用稳定地存在于晶格空隙中,这三种配合物均含有多孔的无限隧道.用溴化乙锭荧光探针法测试了三个配合物对EB-DNA复合体系的荧光猝灭效应,实验结果显示三个配合物均能使EB-DNA复合体系的荧光发生不同程度的猝灭,由此推测配合物均与DNA发生了不同程度的插入作用,其中配合物1的插入作用最强.