三维聚合物双(三丁基锡)戊二酸酯的合成及晶体结构研究

用三丁基氯化锡与戊二羧酸二钠以2:1摩尔比反应,合成了双（三丁基锡）戊二羧酸酯,并用元素分析、红外光谱、核磁共振氢谱及X-射线单晶衍射进行了表征和结构测定。X-射线单晶衍射法测定表明,化合物属单斜晶系,空间群为Cc,晶胞参数:a=13.984（3）,b=16.164（3）,c=16.894（3）A,β=107.457（3）°,V=3642.9（11）A3,Z=4,C29H60O4Sn2,Dc=1.251g/cm3,μ=1.394 mm-1,R=0.0500,wR=0.0874,F（000）=1416。晶体结构中存在2种化学环境不同的三角双锥构型的锡原子,由于配体中2个羧基在不同方向的交联作用,使化合物呈现三维立体骨架结构,并且在骨架结构中存在沿a、b、c轴3个方向伸展的规则的大环直孔道。     

Coriatone and corianlactone, two novel sesquiterpenes from Coriaria nepalensis

Both coriatone (1). a novel highly oxygenated picrotoxane-type sesquiterpene, and corianlactone (2). with an unprecedented sesquiterpene basic skeleton, named coriane, were isolated from Coriaria nepalensis Wall. The structures of 1 and 2 were determined by analysis of their two-dimensional NMR data, and the structure of 2 was confirmed by X-ray analysis. Compounds 1 and 2 showed no remarkable inhibitory activity toward K(562) cells. They are cytotoxic with IC(50) > 50 microg/mL (cis-platinim: IC(50) = 0.49 microg/mL).     

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。     

Alkaloids from Fritillaria Hupehensis

Phytochemical investigation of the bulbs of Fritillaria hupehensis resulted in the isolation and structural elucidation of a new highly conjugated alkaloid of veratramine type identified as 3β,23β-dihydroxy-7,12（14）-dien-5α- veratramin-6-one （1）, together with two known alkaloids, ebeinine （2） and zhebeinine （3）, which were isolated for the first time from F. hupehensis. The structures of alkaloids 1-3 were established by extensive 1D and 2D NMR spectral analyses.     

具有S…S、S…Cl作用的一维链状有机锡化合物氯代二苄基锡哌啶荒酸酯的合成、表征及晶体结构

The chlorodibenzyltin dithiopiperidylcarbamate was synthesized by the reaction of dibenzyltin dichloride with dithiopiperidylcarbamate and was characterized by elemental analysis， IR and ¹H NMR. The crystal structure was determined by X-ray single crystal diffraction. The crystallographic data are as follows： monoclinic， space group P2₁， a=0.63464(13)nm， b=1.9110(4)nm， c=0.87367(17)nm， β=97.67(3)°， Z=2， V=1.0501(4)nm³，D_c=1.571g·cm^-3， μ=1.546mm^-1， F(000)=500， R=0.0209， wR=0.0381 [I≥ 2σ(I)]. The str- uctures consist of discrete molecules containing five-coordinate tin atoms in a seriously distorted trigonal bipyramidal configuration. The molecules are packed in the unit cell in one-dimensional chain complex through a weak inter-action between the chlorine atom， the sulfur atom and one of the other sulfurs of an adjacent molecule. CCDC： 180034.     

Synthesis, Spectroscopic Properties and Crystal Structural Characterization of a Triphenyltin(Ⅳ) Complex with 5-Bromonicotinic Acid

A novel organotin complex [Ph3Sn(C2H5OH)(OCOC5H3NBr)SnPh3(OCOC5H3NBr)]has been synthesized by the reaction of 5-bromonicotinic acid with triphenyltin hydroxide in ethanol and characterized by elemental analysis, IR and 1H NMR. The crystal structure was determined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 15.564(2), b = 24.975(4), c = 12.2973(19) (A), β = 92.224(2)°, Z = 4, V = 4776.5(13) (A)3, Dc = 1.596g/cm3, μ(MoKα) = 2.765 mm-1, F(000) = 2264, R = 0.0385 and wR = 0.0667. In the molecular structure of the title complex, the tin atoms are five-coordinated in a trigonal bipyramidal geometry.     

Lancifodilactone G: a unique nortriterpenoid isolated from Schisandra lancifolia and its anti-HIV activity

[structure: see text]. Lancifodilactone G (1), a novel, highly oxygenated nortriterpenoid featuring a partial enol structure and a spirocyclic moiety, was isolated from the medicinal plant Schisandra lancifolia. Its structure and stereochemistry were determined from extensive one- and two-dimensional NMR and mass spectral data, coupled with single-crystal X-ray analysis. Compound 1 exerted minimal cytotoxicity against C8166 cells (CC50 > 200 microg/mL) and showed anti-HIV activity with EC50 = 95.47 +/- 14.19 microg/mL and a selectivity index in the range of 1.82-2.46.     

铋配合物[Bi(S2CNC5H10)2(NO3)]·[1，10-Phen]·0.5H2O的合成及晶体结构

The bismuth complex with dithiopiperdylcarbamate [Bi(S₂CNC₅H₁₀)₂(NO₃)]·[1，10-Phen]·0.5H₂O was synthesized. The crystal and molecular structure were determined by X-ray single crystal diffraction. The crystal belongs to monoiclinic with space group C2/c, a=3.140(2) nm, b=1.176 4(9) nm, c=2.021 6(15) nm, β=103.081(12)°, V=5.713(7) nm³, Z=8, F(000)=3064, D_c=1.815 g·cm^-3, μ=6.502mm^-1. The final R₁=0.0332, wR₂=0.040 3. In the complex, the bismuth atom is eight-coordinated in a capped distorted pentagonal bipyramidal geometry. CCDC: 222655.     

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.