One—dimesional Infinite Chain Organotin Compounds： Synthesis and structural Characterization of Triphenyltin Thiazole—2—carboxylate and Triphenyltin 3—Pyridinylcarboxylate

Triphenyitin thiazole-2-carboxylate(1) and triphenyltin 3-pyridinylcar boxylate(2) were synthesized by the reaction of sodium thiazole-2-carboxylate or sodium 3-pyridinylcarboxylate with the triphenyltin chloride and their crystal structures were determined by single crystal X-ray diffraction analysis.In the structure of 1, the tin atom is five-coordinated in a distorted trigonal bipyramidal structure.Due to the presence of a close intermolecular Sn…S interaction distance of 0.3666nm,the structre can be described as a weakly-bridged on-dimensional chain compound.In the structure of 2,the tin atom is five-coordinated with bridging 3-pyridinylcarboxylate ligands N atom and resulting structure is one-dimensional chain compound.     

一维链状三苯基锡肉桂酸酯配合物的合成、结构及量子化学研究

三苯基氯化锡与肉桂酸按物质的量比1∶1在苯和乙醇混合溶剂中反应合成了一维链状三苯基锡肉桂酸酯。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=1.281 28(9)nm,b=1.145 90(8)nm,c=1.829 01(4)nm,β=120.784(4)°,V=2.307 0(3)nm3,Z=4,Dc=1.431 g.cm-3,μ(Mo Kα)=11.27 cm-1,F(000)=1 000,R1=0.025 2,wR2=0.058 0。配合物通过肉桂酸羧基桥联,形成五配位的三角双锥构型的链状结构。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。     

Synthesis and Structural Characterization of a New One-dimensional Infinite Chain of Silver(I) Complex with Triphenylphosphine

1 INTRODUCTION The tertiary phosphine silver(I) complexes for- mulated as [AgLnL] (L = tertiary phosphine; n = 1～4; L = coordinating or un-coordinating anions) were first prepared in 1937 by Mann, et al.[1]. Sil- ver(I), whose coordination number ranges…     

一维链状有机锡配位聚合物[(PhCH2)3Sn·(O2CC5H4N)·(H2O)]n的合成及晶体结构

[(PhCH₂)₃Sn·(O₂CC₅H₄N)·(H₂O)]_n was synthesized by the reaction of 4-pyridine car-boxylic acid with the tribenzyltin oxide and was characterized by IR,¹H NMR and MS.Its crystal structure was determined by X-ray single crystal diffraction.The crystal belongs to monoclinic.The space group P2₁/c with unit cell parameters a=1.2241(8)nm,b=0.9660(6)nm,c=2.3708(15)nm,β=102.722(12)°,V=2.734(3)nm³,Z =4,D_c=1.298g·cm^-3.In crystal,the tin atom rendered five-coordinate in a trigo nal bipyramidal structure which is bridged by 4-pyridine carboxy-late into one-dimensional chain polymers.     

一维链状有机锡配合物[Ph3Sn(OCOC5H4NO)]n的合成和晶体结构

有要锡配合物因基具有很强的生物活性以及多变的结构而日益受到人们的关注[1～4].有关该化合物的结构研究表明,中心锡原子的配位形式决定于直接与锡原子相连接的烃基的结构和羧酸基配体的类型[5～7].为了进一步探索有机锡羧配合物的结构类型、羧酸配体中带额外孤电子对的杂原子与锡原子的作用方式,本文合成了一个有机锡羧酸配合物[Ph3Sn(OCOC5H4NO)]n,并用X-射线衍射单晶结构分析方法测定了它的晶体结构.     

Synthesis and Crystal Structure of a One-dimensional Infinite Chain Organotin Complex [(n-Bu)_3Sn(OCOC_5H_4NO)]_n

1 INTRODUCTION Organotin esters of carboxylic acid are widely used as biocides and fungicides and as homogeneous cata- lysts in industry[1~3]. In recent years, the pharmaceu- tical properties of carboxylic acid have been investi- gated for the antitumour activity[4~6]. In general, bio- cidcal activities of organotin complexes are greatly influenced by the molecular structures and coordina- tion numbers of the tin atom[7, 8]. It is revealed that organotin complexes containing carboxylate l…     

一维链配位聚合物[Mn(acacen){N(CN)2}]n的合成、结构和性质的研究(英)

The manganese(Ⅲ) complex [Mn(acacen){N(CN)₂}]_n [H₂acacen=bis(acetylacetone)ethylenediimine] has been synthesized and the structure has been determined. The complex forms a one-dimensional chain structure via the bidentate bridge ligand μ_1,5-[N(CN)₂]^- linking [Mn(acacen)] moiety. The magnetic property of the compound (75～300 K) shows the existence of an antiferromagnetic exchange interaction among paramagnetic centers along the chain. CCDC: 244940.     

三苯基锡硫代苯甲酸酯的合成、性质和晶体结构

用三苯基氯化锡与硫代苯甲酸在三乙胺存在下反应，合成了三苯基锡硫代苯甲 酸酯，并进行了红外光谱及核磁共振氢谱表征。X射线单晶衍射表明，化合物属正 交晶系，空间群P2_12_12_1，晶胞参数：a = 0.8306(3) nm, b = 1.6906(5) nm, c = 3.1459(10)) nm, V = 4.417(2) nm~3, Z = 8, D_c = 1.465 g/cm~3, R_1 = 0.0472, wR_2 = 0.1012。该化合物的晶体是由孤立的分子所组成，四配位的锡 原子呈畸变的四面体构型，配体羧基上的氧原子和锡原子之间存在弱的配位作用。     

一维链状配位聚合物[Ni(p-CPOA)(2,2''''-bipy)(H_2O)]_n的合成与晶体结构

合成了一个新的配位聚合物[Ni(p-CPOA)([(2,2)0(')]-bipy)(H2O)]n(p-CPOA= 4-羧基苯氧乙酸根[(, )(2,2)0(')( )]-bipy= [(2,2)0(')( )]-联吡啶), 并对其进行了元素分析、红外和单晶 X-射线的表征。结果表明:配合物的化学式为C19H16N2O6[(Ni)(, /c, 晶胞参数[(a)( )]= 14.254(3), b = 13.085(3), c = 19.372(4) ? ?= 104.89(3),V = 3491.8(12) 3, Z = 8, Mr = 427.05, Dc = 1.625 g/cm3, μ = 1.153mm-1, F(000) = 1760, 最终R = 0.0345, wR = 0.0565。Ni原子为扭曲的六配位八面体构型, 每个p-CPOA2-配体桥联2个Ni原子形成一维折叠链状结构[(, )22.7(Ni)]…Ni原子之间的距离为[(9.67)(5)], 且通过分子间氢键将一维链连接成双链结构。     

Triphenyltin Esters of N-(2-Carboxybenzylidene)anilines: Synthesis,Spectroscopic Characterization,X-ray Structure Analysis and Fungicidal Activity

Four triphenyltin carboxylates formulated as o- Ph₃SnOCOC₆H₄CH=N–Ar (Ar=C₆H₅; p -CH₃C₆H₄; o -CH₃C₆H₄; o -HOC₆H₄) were prepared and spectroscopically characterized. The crystal structure of o -Ph₃SnOCOC₆ H₄CH=NC₆H₅ indicates that the tin atom, in each of the two molecules comprising the asymmetric unit, exists in a distorted tetrahedral geometry owing to an intramolecular acyl O. . .Sn contact. These new triphenyltin carboxylates display marked toxicity against the fungus Ceratocystis ulmi .     

三苯基锡N-(5-氯亚水杨基)-α-氨基酸酯的合成及结构表征

利用三苯基氯化锡和现场生成的5-氯水杨醛缩-α-氨基酸钾反应合成了6种三苯基锡N-(5-氯亚水杨基)-α-氨基酸酯1～6, 通过元素分析、IR和NMR对其结构进行了表征. 利用X射线单晶衍射测定了三苯基锡N-(5-氯亚水杨基)缬氨酸酯(3)和三苯基锡N-(5-氯亚水杨基)异亮氨酸酯(5)的晶体结构. 结果表明锡原子是五配位的, 通过单齿羧基氧原子和相邻分子的酚氧原子对锡的配位形成了具有反式-O₂SnC₃三角双锥结构的一维链状聚合物.     

一种3-吲哚甲酸吡唑酯的合成、结构及荧光性能

以3-吲哚甲酸与1-苯基-3-甲基-5-吡唑啉酮为原料合成3-甲基-1-苯基吡唑-5-基-1H-吲哚-3-甲酸酯（3）,用IR、1 H NMR、热重分析、X-射线单晶衍射对化合物结构进行了表征,并对其荧光光谱进行了研究.X-射线单晶衍射结果表明：该晶体为斜方晶系,Pbca空间群,a=1.090 90（10）nm,b=1.618 93（14）nm,c=1.819 11（16）nm,α=β=γ=90.00°,V=3.212 7（5）nm3,Z=8,dC=1.312g/cm3,μ=0.088mm-1,F（000）=1 328.     

具有Cl…Cl作用的一维链状有机锡化合物四(2，4-二氯苄基)锡的合成、表征和晶体结构

The tetra(2, 4-dichlorobenzyl)tin was synthesized and characterized by elementary analysis, IR and ¹H NMR. The crystal and molecular structure were determined by X-ray single crystal diffraction. The crystal of the title compound belongs to triclinic, space group P1 with a=1.089 7(3) nm, b=1.050 33(4) nm, c=1.858 5(4) nm, α=96.822(4)°, β=94.477(4)°, γ=94.636(3)°, V=3.001 3(12) nm³, Z=4, D_c=1.679 Mg·m^-3, μ(Mo Kα)=1.582 mm^-1, S=1.005, F(000)=1 496, R₁=0.040 7, wR₂=0.076 3. In compound, the tin atom has a distorted tetrahedral coordination configuration. The molecules are packed in one-dimensional chain polymer through a weak interaction between the chlorine atoms from adjacent molecules, respectively. CCDC: 286106.     

一维链钴配位聚合物{[Co(H2O)4(3,3′-azpy)](3,3′-azpy)3(PF6)2}n的结构和性质的研究

The complex {[Co(H₂O)₄(3,3′-azpy)](3,3′-azpy)₃(PF₆)₂}_n(3,3′-azpy=3,3′-azobispyridine) has been synthesized and characterized. The crystal (C₄₀H₄₀F₁₂CoN₁₆O₄P₂, M_r=1157.75) belongs to the triclinic system, space group P1 with the following crystallographic parameters: a=10.759(2),b=11.012(2), c=23.207(4)?; α=85.330(10), β=83.470(10),γ=69.770(10)°;V=2560.6(8)?³,D_c=1.502g·cm^-3, μ(MoKα)= 0.498mm^-1,F(000)=1178,Z=2, and final R₁=0.0469, wR₂=0.1053 for observed reflections 5549 (I> 2.00σ(I)).The X-ray analysis reveals that cobalt(Ⅱ) cation coordination environment is a distorted octahedral geometry, the Co²⁺ ion is coordinated by four oxygen atoms of water in the equatorial plane, while the two nitrogen atoms of 3,3′-azpy occupy the axial positions. The complex forms a one-dimensional chain structure via 3,3′-azpy bridging ligand. The one-dimensional chain forms three-dimensional network by hydrogen bonds and π-π inter-actions.     

Biocidal Organotin Compounds. Part 2. Synthesis,Characterization and Biocidal Properties of Triorganotin(IV) Hydantoic Acid Derivatives and the Crystal Structures of Triphenyltin and Tricyclohexyltin Hydantoates

The preparation and spectroscopic (¹H NMR, UV and IR) characterization of three R₃Sn(O₂CCH₂N(H)C(O)NH₂) [R=Ph, c-Hex (cyclohexyl) or n-Bu] compounds are reported. A different mode of coordination is indicated for the hydantoate ligand in the R=Ph compound compared with the R=c-Hex and R=n-Bu compounds, as confirmed by a crystallographic analysis. The structure of [Ph₃Sn(O₂CCH₂N(H)C(O)NH₂)] is polymeric owing to the presence of bridging hydantoate ligands such that each ligand coordinates one tin atom, via one of the carboxylate oxygen atoms, and a symmetry-related tin atom via the carbonyl group at the other end of the molecule. The structure features distorted trigonal-bipyramidal tin atom geometries with a trans -R₃SnO₂ motif. The structure of [c-Hex₃Sn(O₂CCH₂N(H)- C(O)NH₂)], by contrast, is monomeric, distorted tetrahedral, as the carboxylate group is monodentate and there are no additional tin–ligand interactions. The structures are each stabilized by a number of intermolecular hydrogen bonds. Fungitoxicity and phytotoxicity studies indicate that the R=n-Bu derivative is the more active compound.     

Synthesis and crystal structure of ethyl 1-benzyl-2-hydroxy-5-methyl-3-oxo-2-phenacyl-2,3-dihydropyrrole-4-carboxylate

Reaction of 5-phenyl-2,3-dihydro-2,3-furandione with ethyl 3-benzylamino-2-butenoate, resulting in ethyl 1-benzyl-2-hydroxy-5-methyl-3-oxo-2-phenacyl-2,3-dihydropyrrole-4-carboxylate and benzylamide ofN-benzoylpyruvic acid, was studied. The structure of the pyrrole derivative was confirmed by X-ray analysis.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1552–1555, August, 1995.     

双核有机锡(Ⅳ)配合物[Ph_3Sn(CH_3OH)O_2CC_6H_4CO_2(CH_3OH)-SnPh_3]·2CH_3OH和[Ph_3SnS_2CN(CH_2CH_2)_2NCS_2SnPh_3]·2CH_3OH的合成、表征和晶体结构

利用三苯基氯化锡和对苯二甲酸二钠、哌嗪荒酸二钠在甲醇中反应 ,合成了双核有机锡 (Ⅳ )配合物 [Ph3 Sn (CH3 OH)O2 CC6H4 CO2 (CH3 OH)SnPh3 ]·2CH3 OH (1)和 [Ph3 SnS2 CN(CH2 CH2 ) 2 NCS2 SnPh3 ]·2CH3 OH (2 ) .通过元素分析、红外光谱和核磁共振氢谱对其结构进行了表征 .用X射线单晶衍射测定了这两个化合物的晶体结构 .化合物 1为单斜晶系 ,空间群P2 1/n ,a =1.5 199(5 )nm ,b =0 .90 0 0 (3)nm ,c =1.82 0 6 (6 )nm ,β =113.970 (5 )° ,Z =2 ,V =2 .2 75 5(13)nm3 ,Dc=1.413g/cm3 ,μ =1.146mm-1,F(0 0 0 ) =980 ,R1=0 .0 35 3,wR2 =0 .0 6 0 6 .化合物 2为单斜晶系 ,空间群P2 1/c,a =1.5 0 6 6 (5 )nm ,b =1.0 875 (4 )nm ,c =1.35 42 (5 )nm ,β =91.6 14(5 )°,Z =2 ,V =2 .2 178(14)nm3 ,Dc=1.498g/cm3 ,μ =1.35 1mm-1,F(0 0 0 ) =10 0 8,R1=0 .0 40 1,wR2 =0 .1148.在 1和 2的晶体中 ,锡原子呈五配位畸变三角双锥构型 .配合物 1由未配位的甲醇分子通过氢键作用形成二维网状结构     

可控粒径及一维链状纳米Fe3O4的制备

采用氧化共沉淀相转化法, 控制适当的pH(9～11.5)和反应温度(20～100 ℃), 制备了不同粒径(20.6～45.0 nm)的纳米Fe₃O₄, 同时对纳米Fe₃O₄一维成链的影响因素进行了分析. 研究发现: 磁场强度和溶液的pH值对纳米Fe₃O₄一维成链有影响, 磁场强度在低于75 mT, pH值在9～11.5时, Fe₃O₄呈现一维链状排列, 且成链趋势随pH值的减小而增强. 纳米Fe₃O₄粒子的链状结构是由外部磁场和其表面电荷的协同效应影响的. 纳米Fe₃O₄均呈现出铁磁性行为, 一维链状纳米Fe₃O₄具有相对较大的矫顽力和剩磁.     

铁-锡多核金属有机化合物的合成及表征

铁-锡多核金属有机化合物;二茂铁羧酸;铁-锡多核金属有机化合物的合成及表征     

Design,Synthesis and Crystal Structure of Two One-dimensional Zigzag Chain-like Compounds

Two one-dimensional chain-like cyanide-bridged compounds, [Fe（Phen）2（CN）2Ni（Cyclam）]（ClO4）2·DMF-2H2O 1 （Cyclam = 1,4,8,11-tetraaza-cyclotetradecane, Phen = 1,10-phenanthroline, and DMF = N,N-dimethylformamide） and [Fe（Phen）2（CN）2Zn（Cyclam）]（PF6）2·CH3CN 2, were prepared by the reaction of [Fe（Phen）2（CN）2]·2H2O with M（Cyclam）^2＋ （M = Ni, Zn）. In complexes 1 and 2, the metal atoms are connected alternatively with CN groups. X-ray structure and IR analyses for 1 and 2 were performed. Structure analysis revealed that both complexes are centrosymmetric and the geometry around each metal atom is an octahedron. The two complexes crystallize in triclinic with space group of P^1-. For 1, a = 10.439（4）, b = 14.976（7）, c = 15.914（8）A,α = 83.168（15）, β = 74.338（15）, γ = 78.023（15）°, V = 2338.3（18）A^3, Z = 2, Mr = 1035.37, Dc = 1.471 g/cm^3, F（000） = 1076,μ = 0.895 mm^-1, the final R = 0.0616 and wR = 0.1414 for 5849 observed reflections （1 〉 2σ（I））. For 2, a = 9.656（6）, b = 15.404（9）, c = 15.822（10）A, α = 78.68（2）, β= 78.917（19）, γ = 77.15（2）°, V = 2223（2）A^3, Z = 2, Mr = 1064.87, Dc = 1.587 g/cm^3, F（000） = 1078,μ = 1.032 mm^-1, the final R = 0.0672 and wR = 0.1595 for 6819 observed reflections （I 〉 2σ（I））.