Isolation and Crystal Structure of Horminone

1　INTRODUCTIONhorminoneRabdsia serra( Maxim) hara,a tradi-tional Chinese medicine for the treatmentofhepatitis,enteritis,acute cholecystitis anddysentery,is a perennial herb distributedmainly in central and southeastern parts ofChina〔1〕.In previous reports,four diter-penoids,Rabdoserrin A,Rabdoserrin B,Excisanin A and Kamebakaurin which be-long to ent- kaurene diterpenoids have beenisolated from this source〔2 ,3〕.Horminonewhich has the structure of abietane quinonewas once isolate…     

唐卡主色矿物颜料光谱分析

唐卡作为一件艺术品,具有较高的历史价值和艺术价值。对唐卡的矿物颜料进行鉴别分析,对唐卡的鉴定、修复、数字化存档、再现等具有非常重要的意义。该研究对唐卡主色矿物颜料进行体系性的光谱分析,选用唐卡绘制过程中5种主色常用的矿物颜料,深入分析矿物颜料的可见光、近红外、短波红外光谱特征产生机理,总结了不同色系矿物颜料可见光、近红外、短波红外谱段光谱特征。通过分析同一矿物颜料粉末、调和骨胶颜料以及颜料上布色卡光谱特征,发现粉状颜料调和骨胶后,反射率整体下降,在1 447和1 928 nm附近出现两个水的强吸收特征。而当骨胶溶物涂绘上布后,随着膏状颜料中水分的减少,上述两个吸收特征均变弱,个别颜料在1 447 nm处的吸收特征甚至消失。因此,矿物颜料粉末和颜料上布色卡光谱极为接近,可以在后期的唐卡颜料分析中直接利用唐卡矿物颜料粉末光谱进行匹配分析。唐卡红色矿物颜料为朱砂,矿物成分主要为HgS,其光谱在可见光波段先降后升,500 nm附近形成一个较深的吸收特征,且吸收峰较宽（430～530 nm）,红光谱段附近反射率急速升高,近红外波段反射率变化较为平直,在1 940和2 250 nm附近有弱吸收特征。唐卡黄色矿物颜料主要有三种：土黄（雄黄、雌黄）,赭石及金箔,主要成分分别为硫化砷、氧化铁及金。其特征光谱在可见光谱段集中在400～500 nm之间,不同颜料的吸收特征位置和吸收深度均不同。赭石在近红外波段的反射率整体较低,且860 nm附近还出现了吸收特征;而雄黄、雌黄和土黄则在近红外和短波红外谱段表现出反射率较高且波形平直,在1 890和2 230 nm附近有弱吸收特征;金箔在可见光波段的吸收特征窄浅,可作为区分的依据。唐卡蓝色矿物颜料为石青,主要矿物成分为蓝铜矿,其光谱在500～1 000,1 500,2 040,2 285和2 350 nm附近均有较强吸收特征,而在1 885和1 980 nm处有弱吸收特征。唐卡绿色矿物颜料为石绿,主要矿物成分为孔雀石,其光谱在550～1 000 nm有较强的宽吸收特征,在2 270和2 350 nm有明显吸收特征。尽管石青和石绿主要矿物成分皆为碳酸铜,但石绿在900～1 900 nm红-近红外谱段反射率增加较缓,1 500 nm无吸收特征,可以作为区分石青和石绿的依据。唐卡白色矿物颜料为砗磲和白土,主要矿物成分分别为碳酸钙和高岭土。在可见光谱段范围,砗磲在370 nm有弱吸收特征,而白土则在370和730 nm处有两个明显的吸收特征,可作为区分。在短波红外和近红外谱段,白土在1 425,1 930和2 230 nm均具有明显吸收特征,砗磲则在1 930和2 320 nm有明显吸收特征,1 440 nm处吸收特征较弱。且同种矿物颜料粉末,矿物粉末颗粒越大,颜料颜色越深,其光谱特征反射率越低。     

铁铂硫原子簇化合物的合成与结构研究 V: [MoFe3S4]类立方烷簇合物的转化反应和[Et4N]3[Mo2Fe6S8(SC6H4CH3-m)3Cl6]的晶体结构

具[MoFe2S4]类立方烷结构单元的双类立方烷化合物[Et4N]4[Mo2Fe7S8(SR)12](1a,R=Ph; 1b, R=tolyl-m)或单类立方烷化合物[MoFe3S4(dteR2)5](2a, R=Me; 2b, R=Et)与酰氯在乙腈中反应, 分别得到不含Fe桥的双类立方烷化合物(Et4N)3[Mo2Fe6S8(SR)3Cl6](3a, R=Ph; 3b, R=toly-m)与[MoFe3S4]骨架支解后的Fe(dteR2)2Cl(4a, R=Me; 4b, R=Et)。说明在相同反应条件下, [MoFe3S4]单元在1中比在2中稳定, 本文首次将1型与3型结构通过一步化学反应连系起来。3型化合物的产生得到X射线衍射测定及^1H NMR谱的证实。本文报道3b的单晶结构及3的^!H NMR数据, 3b属六方晶系, P63/m, a=1.6827(3), c=1.5951(16)nm; V=3.91158nm^3; Dc=1.491g/cm^3;Z=2; F(000)=1780; 偏离因子R=0.048, 化合物2与酰氯反应产生4, 由红外及紫外可见光谱证实。     

新磺酰脲类化合物的合成、结构及构效关系研究(Ⅵ)1—N-〔2-(4-甲基)嘧啶基〕-2-甲酸甲酯-苄基磺酰脲的晶体及分子结构

合成了标题化合物 C6H4 (CO2 CH3 ) CH2 SO2 NHCONHC4 N2 H2 CH3 (C15H16N4 O5S,Mr=36 4 .38) ,用 X-射线晶体衍射法测定了其晶体结构。它属单斜晶系 ,空间群为P2 1/ c,a=10 .2 2 0 (1) ,b=9.938(1) ,c=17.2 4 6 (2 ) ,β=10 6 .2 6 (2 )°,V=16 81.6(3) 3 ,Z=4 ,Dc=1.4 39Mg/ m3 ,μ=0 .2 2 7mm-1,F (0 0 0 ) =76 0。结构由直接法解出 ,全矩阵最小二乘法修正 ,最终偏离因子 R=0 .0 4 98,w R=0 .132 7(I>2 σ(I) ) ,独立可观测点数为 3448。分子中的嘧啶磺酰脲、苯环及酯基分别形成 3个独立的平面共轭体系。     

Crystal structure and ionic conductivity of Mg-doped apatite-type lanthanum silicates LaloSi6-xMgxO27-x （x= 0-0.4）

Lanthanum silicates LaloSi6 xMgxO27_x （x = 0-0.4） were prepared by solid state synthesis to investigate the effect of Mg doping on crystal structure and ionic conductivity. Rietveld analysis of the powder XRD patterns reveals that Mg substitution on Si site results in significant enlargement of channel triangles, favoring oxide-ion conduction. Furthermore, an increase of Mg concentration significantly influences the linear density of interstitial oxygen, which plays an important role in ionic conductivity. The Arrhenius plots of LaloSi6_xMgxO27 x （x = 0-0.4） suggest that Mg-doped samples present higher conductivity and lower activation energy than non-doped La10Si6027, and LaloSis.8Mgo.2026.8 exhibits the highest conductivity with a value of 3.0× 10-2 S .cm 1 at 700 ℃. Such conductive behavior agrees well with the refined results. The corresponding mechanism has been discussed in this paper.     

茂基稀土邻氨基苯甲酰胺基双负离子配合物的合成及其环胺羰化反应和脒基化反应

Cp₃Ln与邻氨基苯甲酰胺在甲苯中反应,之后在HMPA和甲苯中结晶,以中等到高收率得到四核稀土有机配合物[CpLn（ μ-η²：η²-NHC₆H₄CONH）（ μ₃-η¹：η¹：η²-NHC₆H₄CONH）LnCp（HMPA）}₂（Ln=Yb,1a;Er,1b;Y,1c）。化合物 1与4倍物质的量的PhNCO在甲苯中反应形成1,3-喹唑啉二氧基（Quo）双负离子稀土配合物[Cp₂Ln（ μ₃-η²：η²：η¹-Quo）]₃Ln（HMPA）₂（Ln=Yb,2a;Er,2b;Y,2c）,表明化合物1中的Ln-NHAr键和ArCONH-Ln键能与异氰酸酯分子发生连续加成/胺消除反应,形成1,3-喹唑啉二氧基骨架。但化合物1a~1c与ⁱPrN=C=NⁱPr反应,仅得到ArNH基单加成产物{Cp₂Ln[ μ-η¹：η¹：η²-ⁱPrNC（NHⁱPr）NC₆H₄CONH]}₃Ln（HMPA）₃ （Ln=Yb,3a;Er,3b;Y,3c）。而Cp₃Ln与邻氨基苯甲酰胺和ⁱPrN=C=NⁱPr在甲苯中进行“一锅”反应,则形成双核配合物{CpLn[ μ-η¹：η²：η²-NHCOC₆H₄ NC（NHⁱPr）NⁱPr]}₂（Ln=Yb,4a;Er,4b;Y,4c）。值得注意的是,HMPA 能够诱导配合物4发生配体重排反应,转化成化合物3。     

Synthesis and Crystal Structure of 1,2-Bis(1-phenyl-3-methylthio- 4-iminopyrazolo[3,4-d]pyrimidin-5-yl) ethane

1 INTRODUCTION As purine analogs, pyrzolo[3,4-d]pyrimidines have anti-tumor[1], antibacterial[2] and anti-leukemic activities[3,4]. Few of these, however, have been studied for pesticidal activity. It is reported that some substituted pyrzolo[3,4-d]pyrimidines have good fungicidal activity[5~7]. These prompted us to study pyrazolo[3,4-d]pyrimidines analogs further. It is shown that two possible products can be formed in the reaction of ethyl N-pyrazolylformimidate with alkylamines as sh…     

关于同伦满态与覆叠空间

本文在点标道路连通ＣＷ空间的同伦范畴中，利用同伦推出示性了同伦满态，得出了若ｆ：Ｘ－Ｙ是同伦满态，则对π１Ｙ的任一正规子群Ｈ，升腾映射ｆ：Ｘ（ｆ－１＃（Ｈ））→■（Ｈ）也是同伦满态．     

Synthesis and Molecular Structure of 5, 5-Dimethyl-2- (4' -methoxy)phenyl-1, 3, 2- thiazaphospholidine-4-thione 2-sulfide

1 INTRODUCTION In our previous study [1], we found that 1, 3, 2-thiazaphospholidine-4-thione 2-sulfide deriva- tives possessed various bioactivities such as herbicidal, antiviral, fungicidal activity, Which the is strongly held our interest to exploit new method for the synthesis of such phosphorohe- terocycles and investigate their biological activities. Different method for the preparation of 1, 3, 2-thiazaphospholidine-4-thione (one) 2-sulfides have been reported [2~4]. According to …     

Structural Regularities of the Transition Metal Complexes Containing o-Benzenedithiol (H_2bdt)——Synthesis and Structure of Fe_3(bdt)_3(PBu_3~n)_3

Complex Fe_3(bdt)_3(PBu_3~n)_3 was synthesized in the presence of PBu_3~n and the structural regularities in a series of transition metal complexes containing bdtH_2 ligand were summarized. The title complex crystallizes in the triclinic space group P-, Mr=1195.19, cell parameters: a=13.283(3), b=20.115(5), c=13.156(3), (?)=90.33(2), β= 116.47 (1), γ=92.19(2)°, V=3143.5(2.7)~3, Z=2, d_c=1.26g/cm~3. The structure was solved by direct methods from 4122 unique reflections with I>4σ(I) and reached the final convergence factor of R(Rw) = 0.053 (0.060). The complex exhibits strong paramagnetism.