二{氧合-二[2-呋喃甲酸二苄基锡(Ⅳ)]}的合成、性质及晶体结构

以二苄基氧化锡和2-呋喃基羧酸反应,合成了新的化合物二{氧合-二[2-呋喃甲酸二苄基锡(Ⅳ)]}.生物活性测试结果表明,该配合物具有较强的体外抗癌活性.X射线单晶衍射测定表明,配合物是以Sn2O2四元环为中心的、中心对称的二聚体结构,内环锡为六配位的畸变八面体结构,外环锡为五配位的加帽畸变三角双锥结构.     

二烃基锡二茂铁羧酸酯的合成及研究

通过二烃基氧化锡与取代二茂铁羧酸缩合，合成14个末见文献报道的二烃基锡 二茂铁羧酸酯化合物．通过对化合物的核磁共振谱、红外光谱、元素分析的研究， 确定化合物的组成和结构及形成结构的原因．化合物12的X衍射单晶测定表明，化 合物是以Sn2O2四元环为中心的中心对称二聚体结构、内环锡为5配位的畸变三角双 锥结构、外环锡为6配位的畸变八面体结构。化合物的抗癌活性实验结果表明，部 分化合物有较高的抗KB肿瘤细胞和抗Bel-7402肿瘤细胞活性．     

二{氧合—二[2—呋喃甲酸二苄基锡（IV）]}的合成、性质及晶体结构

以二苄基氧化锡和2-呋喃基羧酸反应，合成了新的化合物二[氧合-二[2—呋喃甲酸二苄基锡(IV)]}．生物活性测试结果表明，该配合物具有较强的体外抗癌活性．X射线单晶衍射测定表明，配合物是以Sn2O2四元环为中心的、中心对称的二聚体结构，内环锡为六配位的畸变八面体结构，外环锡为五配位的加帽畸变三角双锥结构．     

有机锡化合物二{氧合-二[杂环羧酸二丁基锡(Ⅳ)]}的合成、表征和二{氧合-二[2-噻吩甲酸二丁基锡(Ⅳ)]}的晶体结构

利用二丁基氧化锡与杂环羧酸反应,合成8个有机锡化合物二{氧合-二[杂环羧酸二丁基锡(Ⅳ)]}.通过元素分析、红外光谱、核磁共振氢谱和锡谱对其结构进行了表征.用X射线单晶衍射测定了二{氧合-二[2-噻吩甲酸二丁基锡(Ⅳ)]}的晶体结构,结果表明,该化合物是以Sn2O2四面体为中心的,中心对称的二聚体结构,内、外环锡原子均为六配位的畸变八面体构型.该化合物晶体属单斜晶系,空间群P2(1)/n,a=1.3721(10)nm,b=1.7297(13)nm,c=1.3721(10)nm,β=93.709(8)°,Z=2,V=3.249(4)nm3,Dc=1.505g/cm3,μ=1.695mm-1,F(000)=1480,R=0.0480,ωR=0.0978.     

水合三环己基锡4-吡啶甲酸酯配合物的合成、结构及抗癌活性

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。     

一苄基锡三（2－吡啶甲酸酯）的合成和晶体结构

利用三苄基氯化锡和2－吡啶甲酸在三乙胺存在下以1：摩尔比反应，合成了非 预期的去苄基化产物一苄基锡三（2－吡啶甲酸酯）。通过元素分析、红外光谱、 核磁共振氢谱和X射线单晶衍射对其结构进行了表征。测试结果表明：该化合物为 单斜晶系，空间群P21，a=1.3141(2)nm,b=1.13127(17)nm,c=1.7122(3)nm,β-110. 581(2°），Z=4,V=2.3829(6)nm^3,Dc=1.606g/cm^3,μ=1.118mm^-1,F(000)=1152, R1=0.0397,wR2=0.0881。该化合物为单体结构，锡原子呈七配位畸变五角双锥构型 。     

有机锡化合物二{氧合-二[杂环羧酸二丁基锡（IV）]}的合成、表征和二{氧合-二[2-噻吩甲酸二丁基锡（IV）]}的晶体结构

利用二丁基氧化锡与杂环羧酸反应 ,合成 8个有机锡化合物二 {氧合 -二 [杂环羧酸二丁基锡 (IV) ] }.通过元素分析、红外光谱、核磁共振氢谱和锡谱对其结构进行了表征 .用X射线单晶衍射测定了二 {氧合 -二 [2 噻吩甲酸二丁基锡(IV) ] }的晶体结构 ,结果表明 ,该化合物是以Sn2 O2 四面体为中心的 ,中心对称的二聚体结构 ,内、外环锡原子均为六配位的畸变八面体构型 .该化合物晶体属单斜晶系 ,空间群P2 ( 1) /n ,a =1.3 72 1( 10 )nm ,b =1.72 97( 13 )nm ,c =1.3 72 1( 10 )nm ,β =93 .70 9( 8)° ,Z =2 ,V =3 .2 49( 4 )nm3 ,Dc=1.5 0 5g/cm3 ,μ =1.695mm-1,F( 0 0 0 ) =14 80 ,R =0 .0 480 ,wR =0 0 978.     

1,3-二氯-1,1,3,3-不对称四烃基二锡氧烷的合成及结构表征

通过氧化二烃基锡与二氯二烃基锡的反应,合成了不对称四烃基二锡氧烷[ClR₂SnOSnR'₂Cl]₂ (R=Bu,Pr; R'=Me,Ph,Cy,Oct).通过对化合物1和5的X-衍射晶体结构分折,表明该类化合物在晶体状态 时是含有中心对称Sn₂O₂四元环的梯状二聚体,内环锡与外环锡均为五配位的畸变三角双锥构型.     

两个有机锡杂环羧酸酯配合物的合成、结构及抗癌活性

合成了2个有机锡杂环羧酸酯配合物：二（邻溴苄基）锡二（2-吡啶甲酸）酯（1）和三（2-甲基-2-苯基丙基）锡3-吲哚丁酸酯（2）。通过元素分析、红外光谱、核磁共振谱（¹H、¹³C和¹¹⁹Sn）、X射线衍射、热重分析进行了表征,用X射线单晶衍射方法测定了配合物的晶体结构,进行了配合物的结构量子化学从头计算和体外抗癌活性研究。结果显示：配合物均为单锡核分子,锡原子分别为六配位的畸变八面体构型和四配位的畸变四面体构型;配合物对人肝癌细胞（HUH7）、人肺癌细胞（A549）、人表皮癌细胞（A431）、人结肠癌细胞（HCT-116）和乳腺癌细胞（MDA-MB-231）的抑制活性均比临床使用的顺铂强。     

二苄基锡N,N-二甲基氨荒酸酯的合成及晶体结构

利用二苄基二氯化锡和N, N-二甲基氨荒酸钠反应, 合成了二苄基锡N, N-二甲基氨荒酸酯(C20H26N2S4Sn, Mr = 541.36)。通过元素分析、红外光谱、核磁共振氢谱和质谱对其结构进行了表征。用X-射线单晶衍射测定了该化合物的晶体结构。化合物为单斜晶系, 空间群P21/n, a = 1.3926(5), b = 0.9832(4), c = 1.7080(7) nm, b = 103.541(6), V = 2.274(2) nm3, Z = 4, Dc = 1.581 g/cm3, m(MoKa) = 1.500 mm-1, F(000) = 1096, R = 0.0482, wR = 0.1162. 在化合物的晶体中, 锡原子为六配位的畸变八面体构型。     

二正丁基锡水杨醛缩对氨基苯甲酸酯配合物的合成、表征及结构研究

The title complex {[ⁿBu₂Sn(2-OHC₆H₄CH=NC₆H₄COO)]₂O}₂·2H₂O was synthesized by the reaction of N-(4-carboxyphenyl)-salicylideneimine with dibutyltin(IV) oxide in 1∶1 molar ratio. The compound has been characterized by elemental analysis, IR, ¹H NMR spectra and X-ray single crystal diffraction. It crystallizes in triclinic system with space group P1. The crystal data are: a=1.242 9(2) nm, b=1.261 3(2) nm, c=1.594 9(3) nm, α=102.06(2)°, β=92.884(3)°, γ=95.939(3)°, Z=2, D_c=1.342 g·cm^-3, F(000)=1 000, V=2.425 2(7) nm³, R₁=0.041 5, wR₂=0.104 4. The compound is in centro-symmetric dimer structure mode with a four-member central endo-cyclic Sn₂O₂ unit in which the bridging oxygen atoms are tri-coordinated. All the tin atoms are five-coordinated with geometry of distorted trigonal bipyramid. CCDC:286105.     

Crystallographic report: Aquadicylcohexyltin(IV) bis(2‐picolinate) ethanol solvate

The tin atom in the title compound is in a distorted pentagonal bipyramidal geometry defined by two sets of nitrogen and oxygen donors derived from the carboxylate ligands, two carbon atoms from the cyclohexyl substituents and an oxygen atom from the coordinated water molecule; C? Sn? C 170.85(15)°. Extensive hydrogen bonding occurs in the lattice. Copyright © 2004 John Wiley & Sons, Ltd.     

二{氧合-二[3-二茂铁基丙烯酸二正丁基锡(Ⅳ)]} 配合物的晶体结构及溶液中的 配位互变平衡机理

测定了配合物{[(n-Bu)2Sn(FcCH=CHCO2)]2O}2(Fc=Ferrocenyl)晶体结构,它属三斜晶系,空间群P1,晶胞参数a=1.3943(3)nm,b=1.4635(3)m,c=1.2792(3)nm,α=94.32(3)°,β=116.27(3)°,γ=109.08(3)°,Z=2,V=2.1362(8)nm^3,Dc=1.542g/cm^3,F(000)=1004。最终偏差因子R=0.0401,Rw=0.1076。该分子中存在着内环锡和外环锡配位单元,锡原子均形成具有假六配位的单加帽畸变三角双锥配位构型。Sn2O2中心内环与丙烯酸酯基茂环等共轭体系之间相互未能共平面。配合物中四个羧基配体划分为两类：两个为桥式双齿配位(μ-COO),跨接于一个内环锡和一个外环锡;另两个仅以单齿配位方式各连接一个外环锡。根据核磁共振谱信息表明分子在溶液中存在着配位互变异构体之间的快交换。我们提出振动模式的假说,认为可能是羧酸酯基氧在其平面内快速摇摆建立了动态平衡之故。     

二[氧合-二(3-二茂铁基丙烯酸二正丁基锡(Ⅳ))]配合物的合成及谱学表征

由FcCH=CHCO2H和(n Bu)2SnO反应合成了{[(FcCH=CHCO2)Sn(n Bu)2]2O}2(A)新配合物[其中Fc=(η5 C5H5)Fe(η5 C5H4)].经红外光谱和核磁共振(1H、13C、119Sn)谱学研究, 确定其组成和结构.提出 [(RCOOSnR′2)2O]2类化合物中一一指认与内环锡、外环锡键连的两类烷基R′中各个碳峰的原则.     

μ3-O-{[μ-(n-Bu)2Sn(μ-FcCO2)(n-Bu)2Sn]FcCO2}二聚物的晶体结构和分子结构

标题配合物Ｍｒ＝９３３．８４,属单斜晶系,空间群Ｐ２_１／ｎ,晶胞参数ａ＝１５．２４４（４）Ａ,ｂ＝２０．８９５（７）Ａ,ｃ＝１２． ３７５（４）Ａ,β＝９７．３９（３）°,Ｚ＝４,Ｖ＝３９０９（２）Ａ~３,Ｄｃ＝１．５８７９·ｃｍ~（－３）,Ｆ（０００）＝１８７２,最终偏差因子Ｒ＝０．０６８４。该配合物分子呈中心对称,是具有Ｓｎ_２Ｏ_２中心内环的二聚体,Ｓｎ_２Ｏ_２中的每个桥氧原子又各连接一个外环锡而形成了四核分子。分子中四个羧酸酯基有桥联双齿（μ－ＣＯＯ）和单齿两种不同的配位模式;在内环锡和外环锡的配位单元中,锡均形成具有五配位的畸变三角双锥配位构型,同时另有一氧原子与中心锡原子之间有弱相互作用。它与类似物［ＦｃＣＯ_２Ｓｎ（ｎ－ＢＵ）_２］Ｏ｝_２·４Ｃ_６Ｈ_６的晶体结构完全不同,却又存在着内在的联系。     

One-step preparation,structural assignment,and X-ray study of 2,2-di-n-butyl- and 2,2-diphenyl-6-aza-1,3-dioxa-2-stannabenzocyclononen-4-ones derived from amino acids

Twenty-four 2,2-di-n-butyl- and 2,2-diphenyl-6-aza-1,3-dioxa-2-stannabenzocyclononen-4-ones, each having a transannular N-->Sn bond, have been prepared by one-step reactions of alpha-amino acids (1 a-l), salicylaldehyde (2), and either di-n-butyltin(IV) oxide (3) or diphenyltin(IV) oxide (4). The new methodology constitutes an easy, highly efficient one-step synthesis of diorganotin(IV) derivatives, such as 5 a-l and 6 a-l, from iminic tridentate ligands without isolation of the Schiff bases. The structures of all the compounds have been established by a combination of (1)H, (13)C, (15)N, and (119)Sn NMR spectroscopy, IR spectroscopy, mass spectrometry, and elemental analysis. In all cases, the (119)Sn chemical shifts, as well as the (1)J((119)Sn,(13)C) coupling constants, are indicative of pentacoordinated tin atoms in solution. The structures of compounds 5 a, d, f, 6 a, b, b-racemic, c, d, f, g, and l have been established by single-crystal X-ray diffraction analyses. The tin atoms in 5 d, f, 6 a, b, b-racemic, c, d, g, and l each have a distorted trigonal-bipyramidal (TBP) geometry, with the oxygen atoms from the phenol and carboxylate moieties occupying the axial positions, and the imine nitrogen and phenyl or n-butyl substituents occupying the equatorial positions. Compounds 5 a and 6 f show distorted octahedral (DOC) geometries due to intermolecular coordination of the carbonyl oxygen to the tin atom, in a trans disposition to the N-->Sn bond, leading to trimeric 5 a and a polymeric structure for compound 6 f. Additionally, measurement of the one-bond coupling constants (1)J((119)Sn,(13)C) in diphenyltin(IV) complexes (6 a-l) and their correlation with the CSn-C bond angles has allowed the derivation of an equation that can be applied to assess the geometry around the tin atom for other diphenyltin(IV) compounds in solution.     

二聚体有机锡配合物{[n-Bu2Sn(O2CCH2CS2NC4H8)]2O}2的合成，表征及晶体结构(英)

The title compound, {[n-Bu₂Sn(O₂CCH₂CS₂NC₄H₈)]₂O}₂, has been synthesized by the reaction of (tetrahydro-pyrrodithiolocarbamoylthio)acetic acid with the di-n-bubyltin oxide in 1∶1 molar ratio. The complex has been characterized by elemental analysis, IR and NMR. The crystal structure of it has been determined by X-ray single crystal diffraction. And the results showed that the crystal belongs to triclinic system with space group P1 and some crystal parameters: a=1.220 2(9) nm, b=1.315 8(10) nm, c=1.380 4(10) nm, α=111.215(9)°， β=99.357(9)°， γ=96.075(10)°, V=2.006(2) nm³, Z=1, F(000)=908, μ=1.489 mm^-1, D_c=1.474 g·cm^-3, R₁=0.037 5, wR₂=0.0839. The complex has a centrosymmetric dimer structure mode with a four-membered central endo-cyclic Sn₂O₂ unit in which two bridged oxygen atoms both connect with an exo-cyclic tin atom which has a distorted octahedron. Each of the endo-cyclic tin atoms exhibits a distorted trigonal bipyramid coordination geometry with an additional weak coordination carboxylate oxygen. Four carboxylate ligands are divided into two types. And two of them are bidentate and connecting to each of exo-cyclic tin atoms by using both oxygen atoms, whereas the others bridge to each pair of exo-and endo-cyclic tin atoms utilizing one oxygen atom only. CCDC: 220513.     

Syntheses, crystal structures, and quadratic nonlinear optical properties in four “push-pull” diorganotin derivatives

Four “push-pull” diorganotin compounds obtained by reaction of methoxysalicylaldehyde or 4-diethylaminosalicylaldehyde, 2-amino-5-nitrophenol and dibutyltin or diphenyltin oxide are reported. The molecular structures for the diphenyl derivatives, in the solid state, show a tin in a distorted trigonal bipyramid geometry with the oxygen atoms in axial positions and the organic moieties and iminic nitrogen in equatorial ones. For the dibutyl derivative, a dimeric structure was favored due to intermolecular interactions between the tin and oxygen atoms, in this case, the tin atom shows a distorted octahedral geometry. A computational study of the diethyl derivatives constructed from the available dibutyl structure, at DFT level, revealed that the main differences between the solid and gas phases are the geometry around the tin atom and the π-conjugated organic backbone which is nearly planar in the solid state and distorted in the gas phase. The electric field induced second-harmonic (EFISH) of the nonlinear optical (NLO) response for the dibutyl derivatives revealed that the change from boron to tin increases 1.5 times the hyperpolarizabilities (β).     

The chloro­(diethyl­amino)­di­methyl­tin dimer

The title compound, di‐μ‐diethyl­amido‐N:N‐bis­[chloro­di­methyl­tin(IV)], consists of discrete [Sn₂Cl₂(CH₃)₄(C₄H₁₀N)₂] dimer mol­ecules, with Sn atoms linked by bridging diethyl­amido groups. The coordination geometry about the metal atom is distorted trigonal bipyramidal, with the two methyl C atoms and one N atom in the equatorial plane, and the Cl and second N atom in axial positions.