顺式—｛内（外）消旋—1，2—双[烷基（芳基）亚砜]乙烷｝合钯（Ⅱ）配合物

本文报道了高、低熔点的RS（O）CH2CH2S（O）R（R＝n-C3H7,n-C8H17,C6H5)与钯（Ⅱ）的配合物（PdCl2·L）的合成也性质，并对R=n-C3H7的一对配合物进行了单晶分析，发现高熔点配体为内消旋体，低熔点配体为外消旋体。     

Synthesis and Crystal Structure of cis-[1,2-Bis(phenyl-thiomethyl)benzene]dichloroplatinum(Ⅱ)·0.5acetonitrile

1 INTRODUCTION The coordination chemistry of bithioethers with noble metal ions has received considerable attention for a very long time due to their appli- cations in extracting noble metals. A number of Pt(Ⅱ) complexes with such ligands have been reported[1～7], among which some crystal structures have been determined[4～7]. However, most of these structures are Pt(Ⅱ) complexes of a few bithioether ligands with flexible alkyl spacers, RS(CH2)nSR. To our knowledge, the crystal str…     

二氯[1,2-二(2-甲酰甘氨酸苯硫基)乙烷]合钯(Ⅱ)的合成和结构

本文首次报道标题化合物的合成和分子结构。该配合物属单斜晶系。空间群为Ｃ２／ｃ。ａ＝１．６３４（２）ｎｍ，ｂ＝０．８０７（１）ｎｍ，ｃ＝２．２２３（２）ｎｍ；β＝１２０．３８（５）。Ｒ＝０．０２５７，ｗＲ２＝０．０６７１。结构测定表明，Ｐｄ（Ⅱ）与硫和氯形成四方平面形配合物。硫原子采取不等性ｓｐ３杂化。在该配合物中未形成Ｐｄ（Ⅱ）－酰胺氮配键     

配位聚合物[HgI2(bpea)]n[bpea=1,2-双(4-吡啶基)乙烷]的合成结构表征和光学折射效应

制备4,4-连吡啶基二卤加和物[MX2(4,4′-bipy)]n仍然有较大困难.这类化合物数量不多且已报道的多为难处理的微晶材料.本文在室温下通过简单的操作合成了新的碘化汞连吡啶乙烷加和物[HgI2(bpea)]nox-射线单晶衍射分析表明其中的汞原子通过与两个碘原子以及吡啶乙烷的两个氮原子配位形成扭曲的四面体构型.每个HgI2单元由bpea桥连形成锯齿状链.其非线性光学性质用8-纳秒激光在532nm波长进行了研究.该化合物相对于入射光表现为一定的光学吸收和强的自聚焦效应,其三阶非线性吸收系数α2=1.1×10-11m@W-1,折射系数n2=5.29×10-188m2@w-1.     

二氯[1,2-二(2-甲酰甘氨酸苯硫基)乙烷]合钯(Ⅱ)的合成和结构

本文首次报道标题化合物的合成和分子结构.该配合物属单斜晶系.     

1,2-二(2-芳基-1,3,4-三唑-5-硫代)乙烷和1,3-二(2-芳基-1,3,4-三唑-5-硫代)丙烷的合成研究

以２－芳基－５－巯基－１，３，４－三唑为原料，在稀碱存在下与二卤代烷反应合成了１０个新的标题化合物。经元素分析确定了化合物的组成，红外光谱、核磁共振氢谱和质谱确证了其结构。初步考查了它们的生物活性。     

顺式-{内(外)消旋-1,2-双[烷基(芳基)亚砜]乙烷}合钯(Ⅱ)配合物的立体化学及晶体结构

本文报道了高、低熔点的RS(O)CH_2CH_2S(O)R(R=n-C_3H_7,n-C_8H_(17),C_6H_5)与钯(Ⅱ)的配合物(PdCl_2·L)的合成与性质.并对R=n-C_3H_7的一对配合物进行了单晶分析,发现高熔点配体为内消旋体,低熔点配体为外消旋体.     

双-(2,2'-联吡啶)和二硫烯钌(Ⅱ)混配配合物合成、光谱表征和电化学性质

近二十年来,多吡啶钌?的配合物引起了人们极大的兴趣。这类配合物的光物理、光化学和电化学性质适合作为研究电子转移和能量迁移的超分子体系的建筑块,而且在光化学分子器件（PMDs）方面具有应用前景犤１～５犦。三－（２,２'－联吡啶）钌?配合物,在可见光区具有强的金属到配体电荷转移吸收带,这种电荷转移跃迁涉及分子内的快速氧化－还原过程。当三－（２,２'－联吡啶）钌?配合物中的一个２,２'－联吡啶分子被其它配体取代后,电荷转移激发态的氧化－还原性质明显受到影响犤６,７犦。通过改变钌?中心周围的配体,可微调钌?中心的…     

1,2-二（二苯基膦）乙烷氯化钯(II)的合成及催化活性

以卤化钯（X=Cl、 Br、 I）为原料,乙腈为溶剂,与1,2-二（二苯基膦）乙烷反应,合成了1,2-二（二苯基膦）乙烷卤化钯[Pd(dppe)X₂, dppe=1,2-二（二苯基膦）乙烷],产率均高于96％,其结构经¹H NMR, XRD和元素分析确证。以Suzuki反应和Stille C—C偶联反应为模板反应,研究了Pd(dppe)Cl₂的催化活性。结果表明：Pd(dppe)Cl₂对2-氯噻吩和对甲氧基苯硼酸的Suzuki偶联反应、4,7-二氯苯并噻二唑核或其他含苯并噻二唑核的卤代芳烃与其他芳香核的锡试剂的Stille C—C偶联反应的催化转化率分别为80%~85%和52%~60%,催化活性优于四（三苯基膦）钯(70%~85%和43%~50%)。     

Synthesis and Crystal Structure of 1,2-Bis（2-benzimidazolyl）benzene

The title compound C6H4(C7H5N2)2 was prepared by the condensation of o-phenylenediamine with o-phthalic acid and characterized by elemental analysis, IR, UV and ^1H NMR spectra, and its structure was determined by single-crystal X-ray diffraction,showing the compound molecule belongs to (72 point group. A ID chain structure was formed by the intermolecular hydrogen bonds (N(2)H…N(I)).     

1,2-二(2-胺基苯氧基)乙烷银配合物的合成与晶体结构

本文采用配体1, 2-二(邻氨基苯氧基)乙烷(L)分别与AgPF6, AgCF3SO3, AgNO3和AgSbF6 进行配位反应,依次得到了四个配合物1 [Ag2(L)2(PF6)]、2 [Ag2(L)2(CF3SO3)2]、3 [Ag(L)NO3]n 和4 [Ag(L)2SbF6]n,并通过FTIR、元素分析、以及X射线单晶衍射等对配合物的结构与组成进行了表征。单晶衍射结果表明,配合物1和2为双核银(I)配合物,3和4为银(I)的配位聚合物。配合物1具有穴状结构,2经Ag?Ag键桥连两个配体形成扭曲的非平面结构。聚合物3的结构为一维(1D)“之”字链,4具有三维(3D)多孔的结构框架。在四个配合物结构中,相应的抗衡阴离子均未参与Ag(I)进行配位作用。     

Synthesis and Crystal Structure of 2,6-Bis（benzimidazo（1,2-c）- quinazolin-6-yl）pyridine Tetrahydrate

The title compound, 2,6-bis（benzimidazo（1,2-c）quinazolin-6-yl）pyridine tetrahydrate, was synthesized by simple condensation of 2-（2-sminophenyl） benzimidazole with pyfidine- 2,6-dicarboxylic acid and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 22.226（8）, b = 16.730（7）, c = 16.820（5）A, β = 115.796（13）°, V = 5631（4）A^3, C33H27NTO4, Mr = 585.62, Z = 8, Dc = 1.381 g/cm^3, λ（MoKα） = 0.71073 A, F（000） = 2448 and μ = 0.09 mm^-1. The structure was refined to the final R = 0.0730 and wR = 0.1573 for 6346 independent reflections （Rint = 0.0801） and 3384 observed reflections （I 〉 2σ（I））. In the crystal, the molecules are linked through intermolecular O-H…O and O-H…N hydrogen bonds. Intermolecular π-π interactions （with distances of about 3.45 A） are pronounced in the crystal structure.     

Synthesis and Crystal Structure of 3,4—Bis（azidoacetamino）furazan

1INTRODUCTIONDuringthepastthreedecades,1,2,5-oxadiazole(furazan)hasbeenstudiedintheN.D.ZelinskyInstituteofOrganicChemistry[1,2],anditwasfoundthatthearomaticityoffurazanringusuallyincreasesthethermalstabilityofitsderivativesandtheplanarityoftheringprovidesthemwithhighdensity.TheweaknessoftheNObondsinfurazanwassuggestedbyananalysisofitsmass-spectrum[3].Itagreeswiththeresultsoftheresonanceformsoffurazan,whichiscalculatedbySaegebrath[4].Thereby,whenthechloroacetaminogroupwasintroducedintot…     

1,2-二乙酰氧甲基碳硼烷的合成

以6,9-二乙腈十硼烷和1,4-二乙酰氧基-2-丁炔为原料,合成了高纯度的1,2-二乙酰氧甲基碳硼烷,产率81.2%,纯度96.2%,其结构经UV-Vis,<'1>H NMR,<'11>B N-MR,IR和元素分析表征.     

Synthesis and Crystal Structure of 2,3-Bis(dinitrofluoromethyl)-1,4-dioxane

For the first time the dinitromethyl group was modified to dinitrofluoromethyl group in the series of aliphatic polynitro compounds in the case of the reaction of 1,1,4,4-tetranitro-2,3-butanediol diacetate with ammonium fluoroxysulfate in the presence of sodium bicarbonate and ethylene glycol. Previously unknown 2,3-bis(dinitrofluoromethyl)-1,4-dioxane was synthesized. Its structure was determined by X-ray diffraction analysis.     

The Synthesis of 1,2-Bis(phenylsulfonyl)cycloalkenes

Reaction of the 2-(phenylthio)cycloalkanones 11–13 with thiophenol and chlorotrimethylsilane afforded the 1,2-bis(phenylthio)cycloalkenes 8–10 together with the corresponding 2,3-isomers 15–17 respectively. Treatment of compounds 7–10 with hydrogen peroxide in acetic acid gave the 1,2-bis(phenylsulfonyl)cycloalkenes 1–4.     

Synthesis and Crystal Structure of a Cadmium Coordination Polymer with Dicyanamide and 1,2-Bis（1,2,4-triazol- 1-yl）ethane

The new cadmium(II) coordination polymer [Cd(bte)2(dca)2]n 1 (bte = 1,2-bis(1,2,4- triazol-1-yl)ethane, dca = dicyanamide) was synthesized and characterized by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 8.7148(15), b = 8.6142(17), c = 15.204(3) A, β = 92.100(10)o, V = 1140.6(4) A3, Z = 2, Mr = 572.87, Dc = 1.668 g/cm3, F(000) = 572, μ = 1.004 mm-1, the final R = 0.0654 and wR = 0.1429 for 1737 observed reflections (I > 2σ(I)). The cadmium atom is coordinated equatorially by four nitrogen atoms from four bte ligands and axially by two nitrogen atoms from two dca anions to adopt a distorted octahedral geometry. Each bte molecule bridges two cadmium(II) atoms. Two strands of bte molecules are wrapped around each other, and held together by cadmium(II) atoms. 1 Forms a double chain structure containing eighteen-membered Cd2(bte)2 rings.     

Synthesis and Crystal Structure of 1,4-Bis(2-hydroxymethylphenyl)-1,4-dioxabutane

1 INTRODUCTION Macrocyclic ligands and their metal complexes have received much attention due to their applications in ion transport, ion separation and as models in biomimic researches[1~7]. The synthetic methods of macrocyclic ligands and their metal complexes are mainly divided into three kinds[8]. The first one is synthesizing free ligand, then forming the metal complexes; the second is template synthesis; and the third is synthesizing the end-off or side-off precursor ligand, then c…