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1.
三环己基氢氧化锡与4-吡啶甲酸按物质的量比1:1在乙醇溶剂中反应,合成了水合三环己基锡4-吡啶甲酸酯配合物。采用元素分析、红外光谱、核磁共振、差热分析和X-射线单晶衍射等对配合物进行了结构表征,并对配合物进行量子化学计算和体外抗癌活性研究。结果表明:配合物中心锡原子为五配位畸变三角双锥构型;配合物对人肝癌细胞(HUH7)、人肺腺癌细胞(A549)、人表皮癌细胞(A431)和人结肠癌细胞(HCT-116)的抑制活性高于顺铂。  相似文献   

2.
利用三有机锡氢氧化物和手性配体(4R)-3-[[(2S)-5-氧-2-吡咯烷基]羰基]-4-噻唑烷甲酸(HL)反应合成了3个三有机锡(4R)-3-[[(2S)-5-氧-2-吡咯烷基]羰基]-4-噻唑烷甲酸酯R3SnL[1,R=c-C6H11(a),C6H5(b),C6H5C(CH3)2CH2(c)],通过元素分析、IR、1H NMR和X-射线单晶衍射表征了其结构。化合物1a属正交晶系,P212121空间群;化合物1b属单斜晶系,P21空间群。二者均为由羧基氧和内酰胺羰基氧桥联配位形成的右螺旋链状有机锡配位聚合物,锡原子具有五配位[SnC3O2]畸变三角双锥构型。化合物1a和1b对体外2种人癌细胞Colo205和Bcap37增殖均有强的抑制作用,其活性为1b1a。  相似文献   

3.
以2,2′-联苯二甲酸(H2DPA)分别与双(三(2-甲基-2-苯基丙基)锡)氧化物、三环己基氢氧化锡和二丁基氧化锡反应,合成了3个有机锡2,2′-联苯二甲酸酯:[((Ph C(Me)2CH2)3Sn)2(DPA)](1)、[(Cy)3Sn(DPA)]n (2)和[(n-Bu)2Sn(DPA)]n (3)。通过IR、NMR、元素分析、热重及X射线单晶衍射对配合物进行表征分析。配合物1、2、3均属单斜晶系,配合物1为双核结构,配合物2、3为一维链状结构,锡原子的配位数依次增大,分别为4、5、6。体外抗癌活性实验表明,配合物1、2、3对人肺癌细胞(NCI-H460)、人乳腺腺癌细胞(MCF-7)、人肝癌细胞(Hep G2)的增殖具有较强的抑制作用。  相似文献   

4.
2-(苯亚胺基次甲基)吲哚铕胺基配合物[η1∶η1-2-(C6H5NH=CH)C8H5N]2Eu[N(Si Me3)2](1)与二芳基取代甲脒(2,6-R2C6H3N=CHNH(C6H3R2-2,6)(R=iPr(2),Me(3))经过配体交换反应,分别得到了含吲哚基脒基铕配合物[η1∶η1-2-(C6H5NH=CH)C8H5N]Eu[(η3-2,6-iPr2C6H3)N=CHN(C6H3iPr2-2,6)][N(Si Me3)2](4)和含脒基的稀土铕配合物[(η3-2,6-Me2C6H3)N=CHN(C6H3Me2-2,6)]2Eu[N(Si Me3)2](5)。结果表明,脒基的位阻显著影响了吲哚基稀土金属胺基配合物与二芳基取代甲脒的配体交换反应。配合物4和5通过IR、元素分析和X射线单晶衍射分析进行了表征。  相似文献   

5.
利用 2 -甲氧羰基乙基三氯化锡与硫代水杨醛缩邻氨基苯酚 (H2 L)进行反应合成了标题配合物 [2 -(2 -羟基苯基 )亚氨甲基苯硫酚根 (2 -) -N,O,S](2 -甲氧羰基乙基 -C,O)氯化锡 CH3OCOCH2 CH2 Sn Cl L(L=2 -SC6 H4 CH NC6 H4 O-2 ) ,该配合物与二甲基亚砜 (DMSO)、六甲基磷酰胺 (HMPA)等单齿配体反应生成混配配合物 CH3OCOCH2 CH2 Sn Cl LL′(L′=DMSO,HMPA) ,与醇 (ROH)反应生成相应的 2 -烷氧羰基乙基锡配合物 ROCOCH2 CH2 Sn Cl L.通过元素分析、红外光谱、核磁共振谱等对配合物的结构进行了表征 .用 X射线单晶衍射测定了标题配合物的晶体结构 ,晶体属三斜晶系 ,P1空间群 ,Z=2 ,晶胞参数 a=0 .870 4(2 )nm,b=0 .93 93 (3 ) nm,c=1 .45 1 1 (3 ) nm,α=98.0 5 (3 )°,β=1 0 3 .0 3 (3 )°,γ=96.99(3 )°.该配合物具有分子内羰基氧原子和配体 L的硫、氮、氧原子对锡原子配位的畸变八面体结构 .  相似文献   

6.
三环己基氢氧化锡与2-氨基-6-氯苯甲酸按物质的量比1∶1在苯溶剂中反应合成了三环己基锡2-氨基-6-氯苯甲酸酯。经X-射线衍射方法测定了其晶体结构,配合物属单斜晶系,空间群为P21/c,晶体学参数a=0.952 00(4)nm,b=0.918 55(3)nm,c=2.909 12(12)nm,β=93.187(2)°,V=2.539 97(17)nm3,Z=4,Dc=1.409 g.cm-3,μ(Mo Kα)=11.31 cm-1,F(000)=1 112,R1=0.038 2,wR2=0.098 6。中心锡与环己基碳原子和氧原子构成畸型四面体。对其结构进行量子化学从头计算,探讨了配合物的稳定性、分子轨道能量以及一些前沿分子轨道的组成特征。通过循环伏安法研究了其电化学性质。  相似文献   

7.
合成了 3 个有机锡 9-芴酮-4-甲酸酯:三苯基锡 9-芴酮-4-甲酸酯[(C6H5)3Sn(C14H7O3)] (1)、三环己基锡 9-芴酮-4-甲酸酯[(C6H11)3Sn(C14H7O3)] (2)和三(2-甲基-2-苯基丙基)锡 9-芴酮-4-甲酸酯[(C6H5C(CH3)2CH2)3Sn(C14H7O3)] (3)。通过元素分析、红外光谱、核磁共振谱(1H、13C和 119Sn)、热重分析进行了表征;用单晶X射线衍射方法测定了化合物的晶体结构,并对其进行了量子化学计算和体外抗癌活性研究。结果显示:化合物1为一维链状结构,中心锡原子为五配位的畸变三角双锥构型;化合物23均为单核分子,锡原子均为四配位的畸变四面体构型。化合物对人宫颈癌细(HeLa)、人肝癌细胞(HUH-7)、人非小细胞肺癌细胞(A549)、人肺腺癌细胞(H1975)和人乳腺癌细胞(MCF-7)都有较好的抑制活性。  相似文献   

8.
合成了3个有机锡9-芴酮-4-甲酸酯:三苯基锡9-芴酮-4-甲酸酯[(C6H5)3Sn(C14H7O3)](1)、三环己基锡9-芴酮-4-甲酸酯[(C6H11)3Sn(C14H7O3)](2)和三(2-甲基-2-苯基丙基)锡9-芴酮-4-甲酸酯[(C6H5C(CH3)2CH2)3Sn(C14H7O3)](3)。通过元素分析、红外光谱、核磁共振谱(1H、13C和119Sn)、热重分析进行了表征;用单晶X射线衍射方法测定了化合物的晶体结构,并对其进行了量子化学计算和体外抗...  相似文献   

9.
(Na[Fe(CO)2C5H5]2)n的形成和反应特性的研究   总被引:1,自引:1,他引:0  
King[1]认为,双环戊二烯基二羰基铁[Fe(CO)2C5H5]2与钠汞齐(Na/Hg)作用可直接得到环戊二烯基二羰基铁钠Na[Fe(CO)2C5H5].但我们在研究合成异核金属配合物过程中,按文献[1]所述方法制得的环戊二烯基二羰基铁钠,分别与主族金属元素锡的配合物L3SnCl (L=C6H11,C6H5)和过渡金属稀土元素的配合物(C5Me5)2 LnCl(Ln=Dy,Gd,Sm,Nd,Pr) 在相同反应条件下作用,却得到了金属间具有完全不同成键形式的两类异核金属配合物.为此,我们对[Fe(CO)2C5H5]2与钠汞齐(Na/Hg)反应产物的结构形式和其在异核金属配合物合成中的反应特性进行了初步研究.  相似文献   

10.
在乙醇钠催化下, 将3-(1,2亚丙二硫基)亚甲基-2,4-二羰基戊烷与2-羰基苯氧乙酸进行缩合反应, 获得了柔性二元酸配体1[4-(1,2-亚丙二硫基)亚甲基-3,5-二羰基-1,6-庚二烯-1,7-二(2-羰基苯)氧乙酸(LH2)]. 再将配体1与二正丁基氧化锡进行脱水反应, 获得新型二正丁基锡羧酸酯配合物2. 采用元素分析、1H NMR、 IR及晶体结构测定等手段对配体1和配合物2进行了结构表征, 配合物2是以菱形环Sn2O2为中心对称的二聚体结构, 中心菱形环通过氧原子与2个环外锡原子相连. 每个羧基分别与环内锡和环外锡原子配位, 形成2个对称的六元环, 3个环呈梯形排列, 将整个分子分割成2个对称的二十二元大环. 初步研究了其杀菌活性和抗癌活性.  相似文献   

11.
Some tri- and diorganotin(IV) compounds of the general formula, RnSnL4-n (where n=2, R=Me, n-Bu and Ph; n=3, R=Me, n-Bu, n-Pr and Ph; HL=5-amino-3H-1,3,4-thiadiazole-2-thione) have been synthesized by the reaction of RnSnCl4-n (where n=2 or 3, R=Me, n-Bu, n-Pr and Ph) and the sodium salt of the ligand. Oct2SnL2 was obtained by the reaction of Oct2SnO with HL in a 1:2 molar ratio under azeotropic removal of water. The bonding and coordination behavior in these derivatives are discussed on the basis of IR, Far-IR, multinuclear (1H, 13C and 119Sn) NMR and 119Sn M?ssbauer spectroscopic studies. These investigations suggest that in all the compounds the ligand acts as monoanionic bidentate coordinating through ring N(3) and exocyclic S. Thermal studies of five compounds, viz., Ph3SnL, Me2SnL2, n-Bu2SnL2, Oct2SnL2 and Ph2SnL2 have been carried out in the temperature range 25-1000 degrees C using TG, DTG and DTA techniques under an atmosphere of dry nitrogen.  相似文献   

12.
Kaolinite is a dominant clay mineral in the soils in tropical and subtropical regions, and its dissolution has an influence on a variety of soil properties. In this work, kaolinite dissolution induced by three kinds of low-molecular-weight organic acid, i.e., citric, oxalic, and malic acids, was evaluated under far-from-equilibrium conditions. The rates of kaolinite dissolution depended on the kind and concentration of organic acids, with the sequence R(oxalate)>R(citrate)>R(malate). Chemical calculation showed the change in concentration of organic ligand relative to change in concentration of organic acid in suspensions of kaolinite and organic acid. The effect of organic acid on kaolinite dissolution was modeled by species of organic anionic ligand. For oxalic acid, L(2-)(oxalic) and HL(-)(oxalic) jointly enhanced the dissolution of kaolinite, but for malic and citric acids, HL(-)(malic) and H2L-(citric) made a higher contribution to the total dissolution rate of kaolinite than L(2-)(malic) and L(3-)(citric), respectively. For oxalic acid, the proposed model was R(Si)=1.89x10(-12)x[(25x)/(1+25x)]+1.93x10(-12)x[(1990x1)/(1+1990x1)] (R2=0.9763), where x and x1 denote the concentrations of HL(oxalic) and L(oxalic), respectively, and x1=10(-3.81)xx/[H+]. For malic acid, the model was R(Si)=4.79x10(-12)x[(328x)/(1+328x)]+1.67x10(-13)x[(1149x1)/(1+1149x1)] (R2=0.9452), where x and x1 denote the concentrations of HL(malic) and L(malic), respectively, and x1=10(-5.11)xx/[H+], and for citric acid, the model was R(Si)=4.73x10(-12)x[(845x)/(1+845x)]+4.68x10(-12)x[(2855x1)/(1+2855x1)] (R2=0.9682), where x and x1 denote the concentrations of H2L(citric) and L(citric), respectively, and [Formula: see text] .  相似文献   

13.
One novel copper(II)-organic compound,namely Cu[Cu2(PP)2](CBPC)2]·2(H2O)(1,H2CBPC = 1-[(2'-carboxybiphenyl-4-yl)methyl]-2-propylimidazole-4-carboxylic acid,HPP = 3-(2-pyridyl)pyrazole),was designed and synthesized under hydrothermal conditions.X-ray diffraction analysis reveals that two Cu(II)ions in the quasi-planar dimmer of [Cu2(PP)2] are linked by the carboxylate oxygen atoms on the phenyl ring and the imidazole ring,respectively,yielding one snake-shaped structure.Magnetic measurements reveal that compound 1 shows the strongly antiferromagnetic property.Crystal data of 1:C58H52Cu3N10O10,Mr = 1239.72,monoclinic,P21/c,a = 14.900(7),b = 15.029(7),c = 12.308(6),β = 102.519(9)o,V = 2691(2)3,Z = 2,Dc = 1.530 g/cm3,F(000)= 1274,μ = 1.246 mm-1,R = 0.0416,wR = 0.0780(I > 2σ(I))and S = 0.999.  相似文献   

14.
A new polyoxomolybdate compound [Ag3(HL)4](PMol204o)] 1 (HE = 3-(2-pyridyl)pyrazole) has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction,elemental analyses,TG and IR spectroscopy. The compound crystallizes in trielinie,space group P(1) with a = 10.375(3),b = 12.076(3),c= 13.196(4) (A°),α= 84.170(4),β =71.961(3),γ = 86.326(4)°,V = 1563.1(7) (A°)3,C32H28Ag3Mo12N12O40P,Mr= 2726.52,Dc = 2.897g/cm3,μ(MoKα) = 3.366 mm-1,F(000) = 1284,Z = 1,the final R = 0.0587 and wR = 0.1312 for 4139 observed reflections (Ⅰ > 2σ(I)). X-ray diffraction analyses reveal that the PMo12O403- clusters in compound 1 are linked by four Ag3(HL)43+ units via the terminal oxygen atoms to form a two-dimensional architecture. The symmetrical unit of Ag3(HL)43+ exhibits two distinct Ag(Ⅰ)environments:a two-coordinate {AgN2} site and a five-coordinate {AgN3O2} site which links to two molybdate clusters.  相似文献   

15.
A new polyoxomolybdate compound [Ag 3 (HL) 4 ](PMo 12 O 40)] 1 (HL=3-(2-pyridyl)pyrazole) has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction,elemental analyses,TG and IR spectroscopy.The compound crystallizes in triclinic,space group P1 with a=10.375(3),b=12.076(3),c=13.196(4),α=84.170(4),β=71.961(3),γ=86.326(4)°,V=1563.1(7)3,C 32 H 28 Ag 3 Mo 12 N 12 O 40 P,M r=2726.52,D c=2.897 g/cm 3,μ(MoKα)=3.366 mm 1,F(000)=1284,Z=1,the final R=0.0587 and wR=0.1312 for 4139 observed reflections (I > 2σ(Ⅰ)).X-ray diffraction analyses reveal that the PMo 12 O 40 3clusters in compound 1 are linked by four Ag 3 (HL) 4 3+ units via the terminal oxygen atoms to form a two-dimensional architecture.The symmetrical unit of Ag 3 (HL) 4 3+ exhibits two distinct Ag(Ⅰ) environments:a two-coordinate {AgN 2 } site and a five-coordinate {AgN 3 O 2 } site which links to two molybdate clusters.  相似文献   

16.
魏春英  杨频等 《中国化学》2002,20(5):453-461
Fourteen new di-n-butyltin(IV)complexes of hydroxamic acids of the formula Bu2SnL2(HL-hydroxamic acids)were synthesized by the reaction of Bu2SnO and hydroxamic acids in dry toluene and ethanol media.The compounds were characterized by elemental analyses,molecular weight,IR and 1H NMR spectoscopy.The results indicate that n-Bu2SnL2 have distorted trans-octahedral structure.The antitumor activity in vitro against human A-549 tumor cells and P388 leukemia was presented,and their structure-activity relationship was discussed.  相似文献   

17.
An unprecedented, intramolecular metal-to-metal silyl ligand migration reaction has been discovered in a series of phosphido-bridged iron-platinum complexes and which may be triggered by an external nucleophile. Thus, reaction of solutions of [(OC)3-(R1/3Si)Fe(mu-PR2R3)Pt(1,5-COD) (1a R1 = OMe, R2 = 3 = Ph; 1b R1 = OMe, R2 = R3 = Cy; 1c R1 = Ph, R2 = R3 = Ph; 1d R1 = Ph, R2 = R3 = Cy; 1e R1 = Ph, R1 = H, R3 = Ph) in CH2Cl2 with CO rapidly afforded the corresponding complexes [(OC)4Fe(mu-PR2R3)Pt(SiR1/3)-(CO)] (2a-e) in which the silyl ligand has migrated from Fe to Pt, while two CO ligands have been ligated, one on each metal. When 1a or 1c was slowly treated with two equivalents of tBuNC at low temperature, quantitative displacement of the COD ligand was accompagnied by silyl migration from Fe to Pt and coordination of an isonitrile ligand to Fe and to Pt to give [(OC)3-(tBuNC)Fe(mu-PPh2)Pt[Si(OMe)3](CNtBu)] (3a) and [(OC)3(tBuNC)-Fe(mu-PPh2)Pt[SiPh3](CNtBu)] (3c). Reaction of 2a with one equivalent of tBuNC selectively led to substitution of the Pt-bound CO to give [(OC)4-Fe(mu-PCy2)Pt[Si(OMe)3](CNtBu)] (4b), which reacted with a second equivalent of tBuNC to give [(OC)4Fe(mu-PCy2)-Pt[Si(OMe)3](CNtBu)2] (5b) in which the metal-metal bond has been cleaved. Opening of the Fe-Pt bond was also observed upon reaction of 3a with tBuNC to give [(OC)3(tBuNC)-Fe(mu-PPh2)Pt[Si(OMe)3](CNtBu)2] (6). The silyl ligand migrates from Fe, in which it is trans to mu-PR2R3 in all the metal-metal-bonded complexes, to a position cis to the phosphido bridge on Pt. However, in 5a,b and 6 with no metal-metal bond, the Pt-bound silyl ligand is trans to the phosphido bridge. The intramolecular nature of the silyl migration, which may be formally viewed as a redox reaction, was established by a cross-over experiment consisting of the reaction of 1a and 1d with CO; this yielded exclusively 2a and 2d. The course of the silyl-migration reaction was found to depend a) on the steric properties of the -SiR1/3 ligand, and for a given mu-PR2R3 bridge (R2 = R3 = Ph), the migration rate decreases in the sequence Si(OMe)3> SiMe2Ph> SiMePh2>SiPh3; b) on the phosphido bridge and for a given silyl ligand (R1 = OMe), the migration rate decreases in the order mu-PPh2 > mu-PHCy; c) on the external nucleophile since reaction of 1c with two equivalents of P(OMe)3, P(OPh)3 or Ph2PCH2C(O)Ph led solely to displacement of the COD ligand with formation of 11a-c, respectively, whereas reaction with two equivalents of tBuNC gave the product of silyl migration 3c. Reaction of [(OC)3-[(MeO)3Si]Fe(mu-PPh2)Pt(PPh3)2] (7a) with tBuNC (even in slight excess) occurred stereoselectively with replacement of the PPh3 ligand trans to mu-PPh2, whereas reaction with CO led first to [(OC)3((MeO)3Si)Fe(mu-PPh2)Pt(CO)-(PPh3)] (8a), which then isomerized to the migration product [(OC)4Fe(mu-PPh2)Pt[Si(OMe)3](PPh3)] (9a). Most complexes were characterized by elemental analysis, IR and 1H, 31P, 13C, and 29Si NMR spectroscopy, and in five cases by X-ray diffraction.  相似文献   

18.
Dias HV  Jin W 《Inorganic chemistry》1996,35(22):6546-6551
The N-methyl-2-(methylamino)troponimine [(Me)(2)ATI]H reacts with bis[bis(trimethylsilyl)amido]tin(II) to yield [(Me)(2)ATI](2)Sn in excellent yield. The treatment of [(Me)(2)ATI](2)Sn with GaI and InCl led to the bis(ligand)gallium(III) and -indium(III) compounds [(Me)(2)ATI](2)GaI and [(Me)(2)ATI](2)InCl. These metal complexes were characterized by elemental analysis, (1)H and (13)C NMR spectroscopy, and X-ray crystallography. All three metal adducts show fluxional behavior in solution at room temperature. [(Me)(2)ATI](2)Sn exhibits a pseudo trigonal bipyramidal structure in the solid state. The gallium and indium atoms in [(Me)(2)ATI](2)GaI and [(Me)(2)ATI](2)InCl adopt trigonal bipyramidal geometry around the metal center with the halide occupying an equatorial site. A convenient, high-yield route to [(Me)(2)ATI]H is also reported. Crystal data with Mo Kalpha (lambda = 0.710 73 ?) at 183 K: [(Me)(2)ATI](2)Sn, C(18)H(22)N(4)Sn, a = 8.4347(11) ?, b = 10.5564(13) ?, c = 11.5527(11) ?, alpha = 66.931(8) degrees, beta = 73.579(9) degrees, gamma = 67.437(7) degrees, V = 863.3(2) ?(3), triclinic, space group P&onemacr;, Z = 2, R = 0.0224; [(Me)(2)ATI](2)GaI, C(18)H(22)GaIN(4), a = 12.947(2) ?, b = 9.5834(9) ?, c = 16.0132(12) ?, beta = 107.418(8) degrees, V = 1895.8(3) ?(3), monoclinic, space group P2(1)/c, Z = 4, R = 0.0214; [(Me)(2)ATI](2)InCl, C(18)H(22)ClInN(4), a = 24.337(3) ?, b = 8.004(2) ?, c = 19.339(3) ?, beta = 101.537(13) degrees, V = 3691.1(11) ?(3), monoclinic, space group C2/c, Z = 8, R = 0.0224.  相似文献   

19.
[{Micro-(phthalazine-N2:N3)}Fe2(micro-CO)(CO)6](1) reacts with organolithium reagents, RLi (R = CH3, C6H5, p-CH3C6H4, p-CH3OC6H4, p-CF3C6H4, p-C6H5C6H4), followed by treatment with Me3SiCl to give the novel diiron carbonyl complexes with a saturated N-N six-membered diazane ring ligand, [{C6H4CH(R)NNCH2}Fe2(C=O)(CO)6](2, R = CH3; 3, R = C6H5; 4, R =p-CH3C6H4; 5, R =p-CH3OC6H4; 6, R =p-CF3C6H4; 7, R =p-C6H5C6H4). Compounds 4 and 5 were treated with [(NH4)2Ce(NO3)6] to afford the aryl-substituted phthalazine-coordinated diiron carbonyl compounds [(micro-{1-(p-CH3C6H4)-phthalazine-N2:N3})Fe2(micro-CO)(CO)6](8) and [(micro-{1-(p-CH3OC6H4)-phthalazine-N2:N3})Fe2(micro-CO)(CO)6](9), respectively. The structures of complexes 4 and 9 have been established by X-ray diffraction studies.  相似文献   

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