银袋内酯乙的乙酰化物的晶体结构和分子结构

本文报道从变色马兜铃(Aristolochia versicolar)的块根中提取的一种新倍半萜内酯-银袋内酯乙的乙酰化物的晶体结构和分子结构.分子式为C~17H~22O~4,分子量290.4,晶体属单斜晶系,空间群为P2~1,a=0.9594(5),b=0.6626(6),c=1.2924(12)um,β=94.48(6)`,V=0.819(1)nm^3,Z=2,Dx=1,18g.cm^-^3,F(000)=266e,μ=0.77cm^-^1(MoKa).结构用直接法解出,经最小二乘法修正后1280个衍射点偏离因子为R=5.5%,Rw=5.2%.分子由椅型.椅型的1,5二烯十员环([2323]矩形)和共用两个相邻DunitzIII型碳C(4),C(5),一个Dunitz II型碳C(6)的五员内酯环组成.十员环与五员内酯环之间夹角为99.该分子骨架拓扑在迄今已知的倍半萜内酯中只与银袋内酯丙相似.所有非氢原子的键长和键角均在实验误差范围内接近理论值。     

奇蒿内酯晶体结构及绝对构型的测定

奇蒿内酯是从中草药刘寄奴提取的新化合物.用X射线单晶衍射方法确定了其三维结构,此单晶属单斜晶系,空间群:P21,晶胞参数:a=12.184(7),b=7.480(14),c=10.424(9)A,β=-104.44(6);Z=2.用直接法RANTAN)得分子初结构模型,采用块对角矩阵最小二乘法对此初结构进行修正,最后一致性因子R=0.085.并利用氧原子反常散射确定了分子的绝对构型。     

异雷公藤内酯四醇的晶体结构

在Rigakui AFC5R四圆衍射仪上测定了异雷藤内酯四醇的晶体结构.晶体属单斜晶系的空间群P2~1,晶胞参数为:a=1.021(1),b=1,126(1),c=1.8209(9)nm,β=98.84(5)°V~c=2.09(3)nm^3,Z=4.表2     

19-O-β-D-吡喃葡萄糖基脱氧穿心莲内酯的晶体结构

19—O-β-D-吡喃葡萄糖基脱氧穿心莲内酯是从中草药爵床科须药草属穿心莲植物中分离而得的一种甙类化合物,具有抗菌、消炎、解毒等性能本文测定其晶体结构,证明葡萄糖以β-甙键的形式与脱氧穿心莲内酯的C_(19)羟基连接.单晶由南京药学院提供.     

雷公藤内酯甲的制备和晶体结构

从雷公藤(TripterygiumwilfordiiHook.F.)根心部分的乙醇提取液中,采用硅胶柱色谱法和TLC方法得到纯的雷公藤内酯甲(WilforlideA).用IR,¹HNMR和元素分析表征,并测定其单晶结构.化合物分子式为C₃₀H₄₆O₃,M_r=454.70,晶体属正交晶系,P2₁2₁2₁空间群,晶胞参数:a=0.732(4)nm,b=1.283(7)nm,c=2.693(6)nm,V=2.5327nm₃,Z=4,D_c=1.192g·cm^-3,μ(MoKα)=0.695cm^-1,F(000)=1107,R=0.039,R_W=0.044,分子为五环三萜γ-内酯.分子中C22-C23为烯键,C11连有羟基,C33_O3为羰基,整个分子呈起伏状,不在同一平面内.从AM1计算结果可以看出,仲羟基中的O1及γ-内酯中的O3原子净电荷大,致使分子极性较大,易在O1和O3部位发生亲核反应和氧化还原反应,显示分子的反应活性     

异青蒿素B_2的晶体结构测定

异青蒿素B_2,C_(15)H_(20)O_3,是无色透明的晶体,属正交晶系,空间群为D_4~2-P2_1,2_1,2_1。晶胞参数为α=7.145(2)(?),b=28.566(5)(?),C=6.523(1)(?),Z=4。用四圆衍射仪收集衍射强度数据,得到独立可观察点1305个。用直接法确定晶体结构并用块对角矩阵最小二乘法修正结构参数。由差值Fourier综合获得全部氢原子坐标,最后的偏离因子R=0.058。结果表明题目化合物是具有β-环氧的异青蒿素B_2。     

大苞雪莲内酯的分子结构和晶体结构

新疆雪莲(Saussurea involucrata Kar. et Kin)为我国西北地区名贵中草药,可用于治疗风湿性关节炎和妇科疾病,从中分离得到一种新的倍半萜内酯的β葡萄糖苷,命名为大苞雪莲内酯(右图),其结晶为无色透明针状,m.p.219～221℃。     

雷公藤内脂四醇的晶体结构

雷公藤系卫矛科植物( Tripterygium wlfordii Hook. f) , 1972) 年,Kupechan从分得三种环二萜内酯类化合物,显示出较强的抗白血压病活性。为了寻找低毒有效的类似物,本文从雷公藤根皮乙醇提取物的氯仿溶出部分,反复经硅胶柱层析分理,得到一种新的环氧二萜酯;雷共藤内酯四醇(Tripletraolide)。在乙酸乙酯重结晶,得无色长极状晶体,m.p.258~260℃。经高分辩质谱确定其分子为C~0H~26O~8,M~r=394.2。     

一种新型CPT非内酯环类似物的合成与晶体结构

通过简单的溶剂扩散法,在合成E环开环衍生物的配合物的过程中,得到了一个新型喜树碱非内酯环类似物2,并通过元素分析、IR、X-射线单晶衍射对其进行了结构表征。结果表明,化合物2(C19H18N2O4)属于单斜晶系Cc,a=2.2432(5),b=9.7320(19),c=7.4280(15),β=97.95(3)°,Z=2,V=1606.0(6)3,Mr=338.35,F(000)=712,R=0.0456,wR=0.1090。结构分析表明,化合物2的每个分子由1个喜树碱类似物分子和1个水分子组成,2个喜树碱类似物分子通过短程相互作用形成柱状堆积,相邻的柱状堆积通过与水分子之间的氢键作用形成二维网络结构。     

罗丹明B内酯单晶的生长及晶体结构

从含有罗丹明B的溶胶-凝胶中首次水热合成了罗丹明B内酯的单晶,并测定了其晶体结构。每个不对称单位含有两个独立分子。     

Synthesis and properties of oil-soluble butyl crystal violet lactone

A novel compound of butyl crystal violet lactone (BCVL) has been prepared by oxidizing leuco butyl crystal violet lactone (LBCVL), which was obtained by the mixture of N,N-dibutylaniline, p-(dibutylamino) benzaldehyde and methyl-m-(dibutylamino) benzoate. The structure of BCVL was characterized by ¹H-nuclear magnetic resonance (NMR), infrared (IR), and mass spectrometry (MS). The color of BCVL can change reversibly in some acid or alkali solvents. The result of the dissolution experiment showed that solubility of BCVL in organic solvent was improved compared with crystal violet lactone (CVL). Translated from Journal of Fudan University (Natural Science), 2006, 45(3): 375–379 [译自: 复旦学报(自然科学版)]     

龙眼三萜-A的晶体结构

用直接法测定了龙眼三萜-A的晶体结构。晶体属单斜晶系, 空晶群C2, 晶胞参数:a=1.3419(4), b=0.6422(2), c=2.9586(7)nm, β=91.91(2)°, Vc=2.548(1)nm^3;z=4, Dc=1.12g/cm^3, Dm=1.10g/cm^3, F(000)=960。结构在MICRO VAX 计算机上用TEXSAN程序包求解、晶体结构用全矩阵最小二乘法修正, 得到最后的偏离因子R=0.068。     

Synthesis,characterization and cytotoxicity of some triarylbismuth(V) di(N‐p‐toluenesulfonyl) aminoacetates and the crystal structure of (4‐CH3C6H4SO2NHCH2CO2)2Bi(C6H4Cl‐4)3

A series of triarylbismuth(V) di(N‐p‐toluenesulfonyl)aminoacetates with the formula (4‐CH₃C₆H₄SO₂NHCH₂CO₂)₂BiAr₃ (Ar?C₆H₅, 4‐CH₃C₆H₄, 4‐ClC₆H₄, 4‐BrC₆H₄) were synthesized and characterized by elemental analysis, IR, ¹H NMR and mass spectra. The crystal structure of (4‐CH₃C₆H₄SO₂NHCH₂CO₂)₂Bi(C₆H₄Cl‐4)₃ was determined and shows the bismuth to exist in a distorted trigonal bipyramidal geometry. Four human neoplastic cell lines (HL‐60, PC‐3MIE8, BGC‐823 and MDA‐MB‐435) were used to screen these compounds. The results indicate that these compounds at 10 μM show cytotoxicity. Copyright © 2004 John Wiley & Sons, Ltd.     

二茂铁衍生物的合成及单晶结构研究

近年来 ,二茂铁金属有机液晶材料因其特异的液晶性能和较高的应用价值 ,引起了人们广泛的研究兴趣 ,得到了迅速的发展 ,使该类液晶材料的种类不断增加[1～ 4] 。本文报道的二茂铁衍生物是一个含有苯基、酯基和Ｓｃｈｉｆｆｓ的金属有机化合物 ,是一种潜在的金属有机液晶材料 ,其合成路线如下 :1　实验1 1　仪器与试剂仪器 :显微熔点测定仪。核磁共振仪为ＲｒａＫｅｒＡＶＡＮＣＥ - 30 0Ｇ型 ,ＴＭＳ作为内标。红外光谱仪为Ｐｅｒｋｉｎ Ｅｌｍｅｒ1 730型 ,ＫＢｒ压片。单晶测定仪为ＳｉｅｍｅｎｓＰ4型衍射仪。试剂均为国产化学纯。1 2…     

The crystal structure of β-Thallium perrhenate

β-TlReO₄, the room temperature modification of thallium perrhenate, has been investigated by means of single crystal X-ray diffraction. It crystallizes in the monoclinic space group P112₁/a with a = 5.636(1), b = 17.428(3), c = 13.353(3) Å, γ = 89.86(2)° and Z = 12. The structure has been refined to R = 0.063 (wR = 0.053) using 2 020 absorption-corrected reflections. The title compound can be described as an intergrowth of β-CsReO₄ and scheelite type blocks at unit cell level. The structure of β-TlReO₄ consists of isolated ReO₄ tetrahedra linked together by TlO₈ and TlO₉ polyhedra. Based upon group theoretical considerations the structural relationships between β-TlReO₄, β-CsReO₄, α-CsReO₄ and scheelite type are discussed.     

The crystal structure of Bi14I4 condensed bismuth clusters

The crystal structure of Bi₁₄I₄ — the final known member of binary bismuth halides — was determined by the single crystal X-ray diffractometer technique (P2₁/m, Z = 1, a = 13.309(3) Å, b = 11.447 (3) å, c = 4.342(1) å, γ = 92.08(3)°, R/R_w = 0.060/0.060 for 369 reflections, sinθ/λ≤ 0.593, MoKγ). The structure consists of condensed bismuth clusters and is build up from infinite one-dimensional bismuth nets running along the c-axis and limited by iodine atoms in another direction. The common structural features of bismuth subhalides containing condensed clusters are also considered based on the analysis of interatomic distances and bond angles. The influence of the lone pair of electrons of the bismuth atom on the geometry of bismuth coordination polyhedra, and the connection between bismuth atoms coordination and the formal oxidation state of these atoms is discussed.     

Two New Sequiterpenoids from Helicteres angustifolia

A new sesquiterpenoid lactone, 3,6,9-trimethyl-pyrano[2,3,4-de]chromen-2-one (1) and a novel sesquiterpenoid quinone, 6-[2-(5-acetyl-2,7-dimethyl-8-oxo-bicyclo[4.2.0]octa-l,3,5-trien-7-yl)-2-oxo-ethyl]-3,9-dimethylnaphtho[1,8-bc]pyran-7,8-dione (2) together with a known perezone (3) were isolated from the roots of Helicteres angustifolia. The structures were elucidated as mainly on the basis of ID and 2D NMR spectroscopic data.