单猪屎豆碱（Monocrotaline）的晶体结构

从猪屎豆种子中提取分离,得到单猪屎豆碱(Monocrotaline)。经X射线衍射分析测定了晶体结构。该化合物属正交品系,空间群为P2_12_12_1,晶体学参数:a=10.072(7),b=11.431(1),c=13.560(2)A,V=1561.3(7)A,Z=4,D=1.384g·cm~(-1) ,μ(MoKa)=0.699mm~(-1),F(000)=696,M=325.36,分子式为C_(16)H_(23)NO_6。在1≤3a(1)收集1627个衍射点,最终偏差因子R和R_0分别为0.058和0.05232。     

吡咯并内酰胺生物碱:2-溴-6,7-二氢-1H,5H-吡咯并[2,3-C]氮杂-4,8-二酮的X-ray晶体结构研究

从中国南海海绵Phacellia fusca Schmidt的乙醇浸提物中,分离得到一吡咯并内酰胺2-bro-moaldisin.通过X-射线单晶衍射法测定了该化合物的晶体结构.结果表明晶体属正交晶系,Pbca空间群,a=12.984(7),b=7.429(4),c=18.580(10)A,V=179.2(16)A3,Z=8,Mr=243.07,Dx=1.802mg/cm3,F(000)=960,μ(Mo-Ka)=4.553 mm-1,λ=0.71073 A.在2.19＜θ＜27.27°范围内共收集了1978个独立衍射点,其中可观测衍射点1361个(|F| 2＞4σ|F|2).晶体结构用直接法解出,经全矩阵最小二乘法修正,最终偏离因子R=0.0535,Rw=0.0803.     

蓝桉果实中的脂溶性成分

从蓝桉(Eucalyptus globulusLabill.)果实乙醇提取物的石油醚部位分离鉴定出6个化合物,通过理化和波谱分析结构鉴定为:5-羟基-4′,7-二甲氧基-6-甲基黄酮(1)、blumenol A(2)、蓝桉醇(3)、绿花白千层醇(4)、β-谷甾醇(5)、二十二烷酸(6),其中化合物1~4和化合物6系首次从该植物中分离得到,化合物1和2首次从桉属植物中分离得到.     

链霉菌HS-HY-045抗肿瘤代谢产物的研究

从链霉菌Streptomyces sp.HS-HY-045的发酵代谢产物中分离得到5个对小鼠淋巴瘤细胞系P388D有抑制作用的化合物,通过波谱分析它们分别鉴定为(-)-(2R,4S)-4-hydroxy-2-methoxy-2-(9E-pentenyl)-tetrahydropy-ran(1),Streptenol C(2),36074-11(3),Fujianmycin A(4)和Streptenol A(5),其中化合物3为新化合物。进一步使用人肺腺癌细胞系A549对5个化合物的抗肿瘤活性进行测试表明化合物4表现出较好的抑制作用,其IC50值为5.2μM。     

草珊瑚的化学成分研究

目的:研究草珊瑚Sarcandra glabra的化学成分。方法:采用各种现代色谱技术对草珊瑚进行分离纯化,根据化合物的理化性质和光谱数据进行结构鉴定。结果:从草珊瑚全草中分离得到12个化合物,分别鉴定为:(-)-依斯坦布林A((-)-istanbulin A,1),依斯坦布林B(istanbulin B,2),菊苣苷(cichoriin,3),异秦皮啶(isofraxidin,4),滨蒿内酯(scoparone,5),槲皮素(quercetin,6),大黄素甲醚(physcion,7),大黄素(emodin,8),β-谷甾醇(β-sitosterol,9),东莨菪内酯(scopoletin,10),蜂花酸(melissicacid,11),正二十五烷醇(pentacosanol,12)。结论:化合物3、7、8、11、12均首次从该植物中分离得到,其中化合物3、11、12首次从该属植物中分离得到,化合物7首次从该科植物中分离得到。     

灰毛豆叶片的化学成分研究

从灰毛豆叶片中分离得到10个化合物,通过波谱数据和理化性质分别鉴定为:stigmast-1,5-dien-3β-ol(1),clemaphenol A(2),松脂醇(3),桉素(4),3-吲哚甲醛(5),色氨酸(6),(S)-4-苄基-2-噁唑烷酮(7),4-羟基苯基丙酸(8),buteaspermanol(9),bovatachalcone(10)。其中化合物1、2、4、5、7、8、9首次从该植物中分离得到。     

长序虎皮楠内生真菌Penicilliumsp.DCS82的化学成分

采用色谱技术从长序虎皮楠内生真菌Penicillium sp. DCS82菌株的PDA平板发酵物中分离纯化得到5个化合物。通过波谱数据分析及与文献对照进行结构解析,分别鉴定为:verrucosidinol acetate(1),verrucosidinol(2),viridicatin(3),fructigenine A(4),3-(dimethylaminomethyl)-1-(1,1-dimethyl-2-propenyl)indole(5)。所有化合物都是首次从该菌中分离里得到。     

杨桃根水提取物化学成分及生物活性的研究

为探究杨桃根中具备降血糖功能的活性成分,采用色谱分离方法从其水提取物中分离得到9个化合物,应用波谱技术对它们的化学结构进行了鉴定,分别命名为prismaconnatoside(1),tarennanosides A(2),(+)-catechin(3),fernandoside(4),7a-[(β-glucopyranosyl) oxy]-lyoniresinol(5),(+)-lyoniresinol 3α-O-β-D-glucopyranoside(6),(-)-lyon-iresinol 3α-O-β-D-glucopyranoside(7),(-)-5’-methoxy-isolariciresinol 3α-O-β-D-glucopyranoside(8)和正辛烷(9)。其中化合物1,2,4,5均为首次从杨桃中分离得到,化合物3为首次从杨桃根中分离得到。对部分单体化合物进行了体外α-葡萄糖苷酶和DPP-IV酶抑制活性测试,化合物1具有较强的α-葡萄糖苷酶抑制活性。     

钟花报春花的化学成分研究(Ⅱ)

从钟花报春花Primula sikkmensis Hook.中分离得到5个化合物,通过波谱分析其结构分别鉴定为5-羟基黄酮(1),2-苯基色原酮(2),5,8-二羟基黄酮(3),2’-羟基黄酮(4),3’-羟基-黄酮-4’-O-β-D-吡喃葡萄糖苷(5)。其中化合物1～4首次从该属植物中分离得到,化合物5首次从该植物中分离得到,并首次对3的NMR数据进行了归属。     

开口箭根茎中甾体化合物的研究

从开口箭根茎部位共分离得到9个甾体化合物,经波谱数据分析结合文献对照分别鉴定为3-epi-neoruscogenin-3-β-D-glucopyranoside(1),3-epi-ruscogenin-3-β-D-glucopyranoside(2),ranmogenin A(3),convallagenin B(4),3-epi-neoruscogenin(5),tupichigenin E(6),(20S,22R)-spirost-25(27)-ene-1β,2β,3β,4β,5β,7α-hexaol-6-one(7),β-谷甾醇(8)和胡萝卜苷(9)。其中化合物1、2和4为首次从该植物中分离得到。     

刺山柑果实中硫单质的分离与晶体结构

从刺山柑果实中首次分离纯化得到S8单质。经X-射线单晶衍射分析,确认该化合物为S8晶体,M=256.48。晶体属斜方晶系,空间群Fddd。晶胞参数a=10.456(7),b=12.908(9),c=24.483(17),V=3305(4)3,Z=16,F(000)=2048,R1=0.0915,wR2=0.1820。     

Three-dimensional structure of Schistosoma japonicum glutathione S-transferase fused with a six-amino acid conserved neutralizing epitope of gp41 from HIV.

The 3-dimensional crystal structure of glutathione S-transferase (GST) of Schistosoma japonicum (Sj) fused with a conserved neutralizing epitope on gp41 (glycoprotein, 41 kDa) of human immunodeficiency virus type 1 (HIV-1) (Muster T et al., 1993, J Virol 67:6642-6647) was determined at 2.5 A resolution. The structure of the 3-3 isozyme rat GST of the mu gene class (Ji X, Zhang P, Armstrong RN, Gilliland GL, 1992, Biochemistry 31:10169-10184) was used as a molecular replacement model. The structure consists of a 4-stranded beta-sheet and 3 alpha-helices in domain 1 and 5 alpha-helices in domain 2. The space group of the Sj GST crystal is P4(3)2(1)2, with unit cell dimensions of a = b = 94.7 A, and c = 58.1 A. The crystal has 1 GST monomer per asymmetric unit, and 2 monomers that form an active dimer are related by crystallographic 2-fold symmetry. In the binding site, the ordered structure of reduced glutathione is observed. The gp41 peptide (Glu-Leu-Asp-Lys-Trp-Ala) fused to the C-terminus of Sj GST forms a loop stabilized by symmetry-related GSTs. The Sj GST structure is compared with previously determined GST structures of mammalian gene classes mu, alpha, and pi. Conserved amino acid residues among the 4 GSTs that are important for hydrophobic and hydrophilic interactions for dimer association and glutathione binding are discussed.     

苍白秤钩风(Diploclisia Glaucescens)中的木脂素——左旋丁香脂素的晶体结构研究

通过X 射线单晶衍射法测定了标题化合物的晶体结构。结果表明 :晶体属正交晶系 ,P2 12 12 1空间群 ,a =8 6 0 10 (3) ,b =13 0 830 (9) ,c =18 1130 (11) ,V =2 0 38 2 0 (2 0 ) 3 ,Z =4 ,Mr =4 18 4 9,Dx =1 36 9g/cm3 ,λ(MoKα) =0 710 73 ,μ(MoKα) =1 12cm-1,F(0 0 0 ) =888。在 0 <2θ <5 0°范围内共收集了 1988个独立衍射点 ,其中可观测衍射点 196 3个 [Ⅰ≥ 8σ(Ⅰ ) ]。晶体结构用直接法解出 ,经全矩阵最小二乘法修正 ,最终偏离因子Rf=0 0 6 2 ,Rw=0 0 5 5。     

Channel-forming, self-assembling, bishelical amphiphilic peptides: design, synthesis and crystal structure of Py(Aibn)2, n=2,3,4.

The design, synthesis, characterization and self-assembling properties of a new class of amphiphilic peptides, constructed from a bifunctional polar core attached to totally hydrophobic arms, are presented. The first series of this class, represented by the general structure Py(Aibn)2 (Py=2,6-pyridine dicarbonyl unit; Aib=alpha, alpha'-dimethyl glycine; n=1-4), is prepared in a single step by the condensation of commercially available 2,6-pyridine dicarbonyl dichloride with the methyl ester of homo oligoAib peptide (Aibn-OMe) in the presence of triethyl amine. 1H NMR VT and ROESY studies indicated the presence of a common structural feature of 2-fold symmetry and an NH...N hydrogen bond for all the members. Whereas the Aib3 segment in Py(Aib3)2 showed only the onset of a 3(10)-helical structure, the presence of a well-formed 3(10)-helix in both Aib4 arms of Py(Aib4)2 was evident in the 1H NMR of the bispeptide. X-ray crystallographic studies have shown that in the solid state, whereas Py(Aib2)2 molecules organize into a sheet-like structure and Py(Aib3)2 molecules form a double-stranded string assembly, the tetra Aib bispeptide, Py(Aib4)2, is organized to form a tetrameric assembly which in turn extends into a continuous channel-like structure. The channel is totally hydrophobic in the interior and can selectively encapsulate lipophilic ester (CH3COOR, R=C2H5, C5H11) molecules, as shown by the crystal structures of the encapsulating channel. The crystal structure parameters are: 1b, Py(Aib2)2, C25H37N5O8, sp. gr. P2(1)2(1)2(1), a=9.170(1) A, b=16.215(2) A, c=20.091(3) A, R=4.80; 1c, Py(Aib3)2, C33H51N7O10H2O, sp. gr. P1, a=11.040(1) A, b=12.367(1) A, c=16.959(1) A, alpha =102.41 degrees, beta =97.29 degrees, gamma =110.83 degrees, R1=6.94; 1 da, Py(Aib4)2.et ac, C41H65N9O12.1.5H2O.C4H8O2, sp. gr. P1, a=16.064(4) A, b=16.156 A, c=21.655(5) A, alpha =90.14(1)degrees, beta=101.38(2) degrees, gamma=97.07(1)degrees, Z=4, R1=9.03; 1db, Py(Aib4)2.amylac, C41H65N9O12.H2O.C7H14O2, P2(1)/c, a=16.890(1) A, b=17.523(1)A, c=20.411(1) A, beta=98.18 degrees, Z=4, R=11.1 (with disorder).     

Crystal structure of beta-D-galactopyranosylamine

The crystal structure of beta-D-galactopyranosylamine (C6H13O5N) is orthorhombic, with space group P2(1)2(1)2(1), and cell dimensions a = 7.703(2), b = 7.788(2), c = 12.645(3) A, V = 757.612 A3, Z = 4; Dc and Dm are 1.573 and 1.587 cm-3, respectively. Using MoK alpha radiation (lambda = 0.7107 A), 2841 reflections were measured on a CAD-4 diffractometer. The structure was solved by using MULTAN-78, and refined anisotropically for the non-hydrogen positional and thermal parameters. Final agreement indices are R(F) = 0.074, wR(F) = 0.086, and S = 2.1523. The conformation is 4C1(D). The orientation of the primary alcohol group is gauche/trans. An unexpected feature of the hydrogen bonding is that the amino group accepts a strong O-H---N bond, but has no donor functionality in the crystal structure.     

Synthesis and molecular structure of prolame, N-(3-hydroxy-1,3,5(10)-estratrien-17 beta-yl)-3-hydroxypropylamine; an amino-estrogen with prolonged anticoagulant and brief estrogenic effects

The synthesis and molecular structure of prolame, N-(3-hydroxy-1,3,5(10)-estratrien-17 beta-yl)-3-hydroxypropylamine, is described. It was characterized by ir, nmr, mass spectrometry and chemical analysis. The crystal structure of this compound was determined by single-crystal x-ray diffraction. Prolame belongs to space group P212121. Cell dimensions are: a = 8.356(2), b = 13.343(4) and c = 16.119(4) A. Z = 4; R = 4.1%.     

Crystal Structure Determination of New Antimitotic Agent Bis(p-fluorobenzyl)trisulfide

The purpose of this research was to investigate the physical characteristics and crystalline structure of bis(p-fluorobenzyl)trisulfide, a new anti-tumor agent. Methods used included X-ray single crystal diffraction, X-ray powder diffraction (XRPD), Fourier-transform infrared (FT-IR) spectroscopy, differential scanning calorimetric (DSC) and thermogravimetric (TG) analyses. The findings obtained with X-ray single crystal diffraction showed that a monoclinic unit cell was a = 12.266(1) A, b = 4.7757(4) A, c = 25.510(1) A, beta = 104.25(1) degrees ; cell volume = 1,448.4(2) A(3), Z = 4, and space group C2/c. The XRPD studies of the four crystalline samples, obtained by recrystallization from four different solvents, indicated that they had the same diffraction patterns. The diffraction pattern stimulated from the crystal structure data is in excellent agreement with the experimental results. In addition, the identical FT-IR spectra of the four crystalline samples revealed absorption bands corresponding to S-S and C-S stretching as well as the characteristic aromatic substitution. Five percent weight loss at 163.3 degrees C was observed when TG was used to study the decomposition process in the temperature range of 20-200 degrees C. DSC also allowed for the determination of onset temperatures at 60.4(1)-60.7(3) degrees C and peak temperatures at 62.1(3)-62.4(3) degrees C for the four crystalline samples studied. The results verified that the single crystal structure shared the same crystal form with the four crystalline samples investigated.     

Crystal structure of beta-D-psicopyranose

Here, we report the crystal structure of d-psicose, C(6)H(12)O(6), one of the rare sugars. The compound crystallizes as the beta-anomer with rarely observed in pyranose carbohydrate structures trans-gauche orientation of the hydroxymethyl group relative to the pyranosyl ring. The crystal system is orthorhombic, space group P2(1)2(1)2(1), Z=4, with cell dimensions a=7.727(2), b=8.672(2), c=11.123(3)A, V=745.3(3)A(3). The pyranosyl ring adopts chair (2)C(5) conformation. The crystal structure at 100(2)K is stabilized by three-dimensional network of O-Hcdots, three dots, centeredO and C-Hcdots, three dots, centeredO intermolecular hydrogen bonds.     

Molecular and crystal structure of galactinol dihydrate [1-O-(alpha-D-galactopyranosyl)-myo-inositol dihydrate

The crystal structure of galactinol dihydrate has been determined by X-ray diffraction. The crystal belongs to the orthorhombic system, space group P2(1)2(1)2, a = 15.898(6), b = 19.357(5), c = 5.104(4) A, and Z = 4. The structure was refined to R = 0.044 for 1818 observed structure amplitudes. The primary hydroxyl group exhibits twofold orientational disorder. The linkage conformation is close to those of alpha-(1 --> 4) linkages in methyl alpha-maltotrioside tetrahydrate and erlose trihydrate. Although there is no interring hydrogen bond in galactinol, an indirect interring hydrogen bond including a water molecule is present. The observed conformation is additionally stabilized by the indirect interring hydrogen bond. The global minimum in the relaxed-residue energy map based on the MM3(92) force-field is close to the observed conformation in the crystal structure. All hydroxyl, ring and water oxygen atoms are involved in a complex three-dimensional hydrogen-bonding network.