甲基三氧化铼(Ⅶ)席夫碱配合物的合成与晶体结构

A novel methyltrioxorhenium(Ⅶ) (MTO) complex was synthesized by the reaction of MTO with Schiff-base ligand obtained by the condensation of 2-pyridinecarboxaldehyde with 4-bromoaniline in methanol. The complex was characterized by NMR, IR, MS, elemental analysis and X-ray diffraction single crystal structure analysis. The results showed that the crystal belongs to monoclinic, space group P2₁/n with a=0.965 70(19) nm, b=1.410 6(3) nm, c=1.080 4(2) nm, β=109.20(3)°, V=1.390 0(5) nm3, M_r=510.36, Z=4, D_c=2.439 g·cm^-3, F(000)=952 and final R₁=0.034 4, wR₂=0.076 1. The crystal structure indicates that the Re(Ⅶ) atom is coordinated with both nitrogen atoms from the Schiff-base. CCDC: 740159.     

三(2-苯并咪唑亚甲基)胺铜(Ⅱ)配合物的合成、晶体结构和量子化学研究

合成了高氯酸［三(2-苯并咪唑亚甲基)胺］咪唑合铜(Ⅱ)配合物［Cu(C₂₇H₂₅N₉)］(ClO₄)₂·2CH₃OH·H₂O。用X-射线衍射的方法测定了其晶体结构,并对其混合配体进行了量化计算。配合物晶体结构属三斜晶系,空间群为P1,晶胞参数：a=11.377(4), b=12.380(2), c     

铅(Ⅱ)与三(2-(6-甲基吡啶基)甲基)胺配合物的合成及晶体结构的研究

本文合成了标题配合物［Pb(TLA)·NO₃］·NO₃(TLA=三(2-(6-甲基吡啶基)甲基)胺，对其红外光谱及晶体结构进行了研究。结果表明，晶体属单斜晶系，P2₁/n空间群，晶胞参数如下：a=10.234(2)?，b=15.347(3)?，c=15.395(3)?，β=99.93(2)°，V=2382(2)?³，Z=4     

一水合高氯酸三(2-苯并咪唑亚甲基)胺合钴(Ⅱ)配合物的合成及晶体结构

合成了一水合高氯酸三(2-苯并咪唑亚甲基)胺合钴(Ⅱ)配合物,用单晶X- 射线衍射方法测定了它们的晶体结构.测定结果表明,该配合物属正交晶系,Pbcn(No.60) 空间群.晶胞参数a=19.393(9),b=18.232(8),c=17.052(8),α=β=γ=90.000(1)°,V=602 9.33,Z=8,最终偏离因子R1=0.156.配合物中的金属Co(Ⅱ)原子与配体NTB分子中的四个氮原子和高氯酸根中的一个氧原子形成扭曲三角双锥构型.     

6,6‘—二（二苯基氧化膦甲基）—1,1’—氮氧化—2,2‘—联吡啶与…

合成了硝酸铒与四功能团含磷萃取剂６，６’－二（二苯基氧化膦甲基）－１，１’氮氧化－２，２’－联吡啶的配合物。用四圆衍射仪测定了配合物的晶体结构。金属离子周转的配位水分子已全部被取代。     

N-亚水杨醛基-1-氨基金刚烷Schiff碱锌(Ⅱ)配合物的合成和晶体结构

N-亚水杨醛基-1-氨基金刚烷Schiff碱锌(Ⅱ)配合物的合成和晶体结构     

稀土氧化膦取代杯芳烃配合物的合成与结构

合成了一种新的氧化膦取代杯芳烃衍生物的稀土离子(La³⁺,Eu³⁺)硝酸盐配合物.通过元素分析和红外光谱对配合物进行了表征.在无水甲醇中培养出了配合物的单晶,用X射线单晶衍射法测定了其晶体结构.硝酸镧配合物晶体[L·La(OH₂)(NO₃)₂]NO₃{L为四(亚甲基二苯基氧化膦)杯[4]芳烃}属四方晶系,空间群P4₃2₁2,晶胞参数a=b=1.8977(4)nm,c=3.1087(11)nm;Z=4;V=11.196(5)nm³;D_c=1.097g/cm³,F(000)=3712,μ=0.491mm^-1,R₁=0.1181,wR₂=0.1930.硝酸铕配合物晶体[L·Eu(OH₂)(NO₃)₂]NO₃·CH₃OH属单斜晶系,空间群C2/c,晶胞参数a=2.88172(11)nm,b=5.4015(2)nm,c=2.01189(7)nm;β=133.4067(9)°,Z=8;V=22.7511(14)nm³,D_c=1.106g/cm³,F(000)=7464,R₁=0.0671,wR₂=0.1794.2个配合物的晶体结构相类似,配合物中配体的4个磷氧键上的氧原子、2个双齿配位的硝酸根中的4个氧原子还有1个水分子中的氧原子分别参与了配位.中心离子配位数为9,配位多面体为单帽四方反棱柱体.另外在铕配合物的杯芳烃中还包合了1个甲醇分子.     

2′-(2-噻吩亚甲基)-2-羟基苯甲酰腙钴(Ⅲ)配合物的合成、表征及晶体结构

In ethanol, a mononuclear cobalt(Ⅱ) complex incorporating 2′-(2-Thienylidene)-2-Hydroxybenzoylhydra-zide has been synthesized and characterized by IR, UV-Vis, elemental analysis and X-ray crystal structure analysis. The crystal belongs to triclinic system, space group P1 with cell constant, a=1.230 69(10) nm, b=1.329 18(11) nm, c=1.330 56(11) nm, α=113.702(2)°, β=91.590(2)°, γ=100.846(2)°, V=1.944 4(3) nm³, Z=2, μ=0.662 mm^-1, D_c=1.482 g·cm^-3, F(000)=896, R_int=0.048 7. The crystal structure shows an anionic didentate ligand O and N donors in this work. The cobalt(Ⅲ) atom is hexacoordinated with oxygen atom from keto group and nitrogen atom from amide to form a cobalt atom for the core octahedral structure. CCDC: 748882.     

四(三苯基氧化膦)二氯稀土(Ⅲ)-三氯化铜(Ⅱ)配合物的合成和谱学性质

合成了通式为[LnCl_2(Ph_aPO)_4][CuCl_3](Ln=La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Y)的12种新配合物,X射线衍射结构分析证实[GdCl_2(Ph_2PO)_4][CuCl_3]中Gd(Ⅲ)为六配位畸变八面体形,Cu(Ⅱ)为三配位平面三角形.测定了所有配合物的红外光谱、~(31)P NMR和Cu(Ⅱ)的顺磁共振谱,并对[LnCl_2(Ph_3PO)_4][CuCl_3]的生成进行了讨论.     

N-氧化吡啶-2-甲醛衍生物的配合物研究(Ⅰ)——与二胺生成的双Schiff碱铜配合物的合成和晶体结构

报道了N-氧化吡啶-2-甲醛(Pio)与乙二胺(en)及1,3-丙二胺(tn)生成的双Schiff碱Cu(Ⅱ)配合物([Cu(Pioen)H_2O](ClO_4)_2和[Cu(Piotn)(H_2O)_2](ClO_4)2)的合成和晶体结构。晶体[Cu(Pioen)H_2O_3(ClO_4)_2属正交晶系,空间群P2_12_12_2,α=7.9534(19),b=7.6768(48),c=26.1037(189),Z=4,R=0.077 1,R_w=0.0771。晶体[Cu(Piotn)-(H_2O)_2](ClO_4)_2属正交晶系,空间群P~(nam),α=7.1360(24)。b=13.7887(42),0=22.2556(81),Z=4,R=0.0491,R_w=0.0491。结构由Patterson函数及Fourier合成法解出,经全矩阵最小二乘法修正至收敛。     

N-[(1-芳基-3-苯基-吡唑-4-基)次甲基]-2-羟基苯甲酰肼类衍生物的合成、表征及抑菌活性

依据生物活性叠加原理,以邻羟苯基和苯基吡唑为分子核心,构建了6种未见报道的N-[(1-芳基-3-苯基-吡唑-4-基)次甲基]-2-羟基苯甲酰肼衍生物.以芳胺为原料,经重氮化、还原、与苯乙酮缩合及Vilsmeier-Haack反应制得1-芳基-3-苯基-4-甲酰基吡唑,再与水杨酰肼反应制得目标化合物,其结构经IR,1HNMR和元素分析等验证.探讨了制备中间体(3a～3f)的反应机理,结果表明,1位芳环上取代基对关环反应有显著影响,供电基有利于关环反应的进行,吸电基则恰恰相反.抗菌活性测试表明,质量分数为0.01%的化合物对大肠杆菌和白色念珠菌的抑菌率高达100%,有极强的抑菌活性,对金黄色葡萄球菌的抑菌率达70%以上,有一定的抑菌活性,是一类极具潜力的抗真菌和抗革兰氏阴性菌的化合物.构效分析结果表明,1位芳基中引入Cl和Br等卤原子,能显著增强化合物的抑菌活性,而引入NO2和CH3基团,则会降低其抑菌活性.     

Synthesis and Antibacterial Activities of N-[(1-Aryl-3-phenyl-pyrazol-4-yl)methylene]-2-(halo-o-hydroxyphenyl)hydrazide Derivatives

A series of novel N-[(1-aryl-3-phenyl-pyrazol-4-yl)methylene]-2-(halo-o-hydroxyphenyl)hydrazide derivatives was synthesized and the antibacterial activity of each of them was evaluated. The supposed reaction mechanism of acquiring compounds 3a—3d is that catalytic activity is enhanced by the electron-donating groups of the first phenyl ring while decreased by electron-withdrawing groups of that ring. The result of preliminary bioassay shows that the lowest minimal inhibitory concentration(MIC) of the title compounds against Escherichia coli is 2 μg/mL. MIC values against Monilia albican and Staphlococcus aureus are as low as 4 μg/mL. They will be a series of potential antibacterial compounds against fungi and gram-negative bacteria.     

新的吡啶基硫醚苯甲酸的原位合成及其铜配合物

在氧化铜和溴化铜存在的条件下, 4-[1,2-(2-吡啶基)亚甲硫基]-苯甲酸(L′)经原位消去反应, 形成了一个新的有机配体4-[1,2,2-(2-吡啶基)-(2-吡啶亚甲基)亚甲硫基]-苯甲酸(L), 并与铜形成配位聚合物[Cu₂(L)Br₂]_n(1){L=4-[1,2,2-(2-吡啶基)-(2-吡啶亚甲基)亚甲硫基]-苯甲酸}, 通过红外光谱、元素分析和X射线单晶衍射等手段对其结构进行了表征.     

双核Cu(Ⅱ)-2，4-二羟基苯甲醛缩邻氨基苯甲酸Schiff碱配合物的合成、表征和晶体结构

The novel dinuclear copper(Ⅱ) complex with with N-(2，4-dihydroxybenzalidene)-o-aminobenzoic acid ligand， [Cu(C₁₄H₉NO₄)]₂·2H₂O， has been synthesized and characterized by elemental analysis， IR， UV-Vis and thermal analysis. Its crystal structure was determined by single crystal X-ray diffraction techniques. The crystal belongs to monoclinic with space group P2₁/c. The cell parameters are: a=0.82510(11)nm， b=0.68870(9)nm， c=2.3007(3)nm， β=100.847(2)°， V=1.2840(3)nm³， Z=2，D_c=1.742Mg·m^-3， μ(Mo Kα)=1.723mm^-1， F(000)=684. The structure was refined to final R₁=0.0267， wR₂=0.0735. The complex molecule structure has dinuclear centrosymmetric dimeric structure in which a planar Cu₂O₂ core features. The ligand N-(2，4-dihydroxybenzalidene)-o-aminobenzoic acid dianion is μ₂-tridentate， chelating one copper(Ⅱ) ion via one nitro-gen， one hydroxy oxygen atom and one carboxylate oxygen atom， and the hydroxy oxygen atom simultaneously co-ordinates to the other copper(Ⅱ) ion of the dimer. In the structure the copper(Ⅱ) ion rendered four-coordination in a distorted square-planar geometry structure. CCDC: 212695.     

配合物二乙基锡N-[(2-氧苯基)亚甲基]甘氨酸酯的合成、结构表征和生物活性

合成了5个新的二乙基锡N-[(2-氧苯基)亚甲基]甘氨酸酯(CH3CH2)2Sn(2-O-3-X-5-YC6H2CH=NCH2COO)(X,Y=H,H,1;H,Cl,2;H,Br,3;Cl,Cl,4;Br,Br,5),利用元素分析、IR、1H和129Sn NMR表征了其结构.通过X-射线单晶衍射测定了1和4的晶体结构.化合物1的晶体属单斜晶系,P21空间群;化合物4的晶体属三斜晶系,P1空间群.2个化合物均为由羧基桥联形成的[Sn3O6C3]十二元大环三聚体结构,锡原子的配位构型为六配位[SnC2NO3]畸变八面体.生物活性测试结果表明,化合物5对3种人癌细胞HeLa、CoLo205和MCF-7及大肠杆菌均有抑制活性.     

N-[3-(4-乙氧基苄基)-4-氯苯基]-1-脱氧野尻霉素的合成及其降血糖作用

以具有降血糖活性的达格列净、卡格列净和脱氧野尻霉素为参照,设计合成了新化合物N-[3-(4-乙氧基苄基)-4-氯苯基]-1-脱氧野尻霉素(A)。以2-氯-5-硝基苯甲酸为原料,先将羧酸转化为酰氯、再经Friedel-Crafts酰基化、羰基还原及硝基还原,合成了中间体2-氯-5-氨基-4'-乙氧基二苯基甲烷;另一方面,以单丙酮葡萄糖为原料,经选择性氧化和水解反应得到5-氧化-D-葡萄糖。该化合物和2-氯-5-氨基-4'-乙氧基二苯基甲烷发生双还原胺化反应得到化合物A的粗品。将粗品A与乙酸酐反应,经柱色谱分离得到高纯度的四乙酰基-N-[3-(4-乙氧基苄基)-4-氯苯基]-1-脱氧野尻霉素(B),再将其水解制得纯的化合物A。将化合物A口服给药SD大鼠后,发现该化合物可以降低SD大鼠血糖,增加尿量和葡萄糖从尿液中的排出。     

Synthesis and Lipase-Catalyzed Acetylation of N-[(2-Alkoxycarbonyl)Benzoyl]-4-Hydroxyisoxazolidines

Several N-[(2-alkoxycarbonyl)benzoyl]-4-hydroxyisoxazolidines were prepared as the racemic mixtures, and resolved by the lipase-mediated acylation.     

Magnetic properties of stable N-[(dichlorophenyl)thio]-2,4,6-triphenylphenylaminyl and N-[(dichlorophenyl)thio]-2,4,6-tris(chlorophenyl)phenylaminyl radical crystals

The magnetic properties of N-[(dichlorophenyl)thio]-2,4,6-triarylphenylaminyl radical crystals are reported. The three stable thioaminyls show ferromagnetic behaviors described using the one-dimensional Heisenberg model with the large ferromagnetic interaction of 2J/k_B = 28.0, 11.4, and 3.6 K. The other two radicals show the antiferromagnetic alternating chain behaviors with 2J/k_B = −16.8 K, = 0.55 and 2J/k_B = −128.8 K, = 0.90. The low-temperature susceptibility and heat capacity measurements of the crystal showing 2J/k_B = 28.0 K reveal a magnetic phase transition at 0.4 K. The ordered phase shows spin-flop transition which reveals an antiferromagnetic long range order.