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1.
由1,4-二碘代苯出发,经过两步Sonogashira偶联反应合成了标题配合物2-甲基4.(4-(吡啶-3-乙炔基)苯基)-3-丁炔-2-醇.通过1H NMR、13C NMR核磁共振、Ⅹ-射线单晶衍射等手段对化合物的结构进行了表征.结果表明,该化合物晶体属于单斜晶系,空间群为P21/c.晶体学参数:a=3.3321 (4) nm,b=1.00539(11) nm,c=0.89158(10) nm,α =90.00°,β=92.442(2)°,y=90.00°,V=2984.2(6) nm3,Z =4. 相似文献
2.
以3-硝基-4-氯苯甲醛和5,5-二甲基-1,3-环己二酮为原料,二甲基甲酰胺为溶剂,不需催化剂合成一种新的氧杂蒽二酮开环衍生物2,2'-(3-硝基-4-氯苯基)次甲基双(3-羟基-5,5-二甲基-2-环己烯-1-酮)晶体,确定最佳反应条件是:芳醛和脂肪环酮的摩尔投料比为1∶2,反应温度为80℃,反应时间为lh;并对其进行熔点、元素分析、红外光谱、氢核磁共振及X-射线单晶衍射测定.该晶体为单斜晶系,空间群=P21/n,a=1.95777(13)nm,b=1.22720(9) nm,c=1.99687(14) nm,β=107.719(2).,V=4.5700(6) nm3,Z=8,dc=1.302 g/m3,μ =0.205mm-1,F(000)=1888. 相似文献
3.
Isabelle Creuven Bernadette Norberg Anne Olivier Christine Evrard Guy Evrard Piet Wigerinck Piet Herdewijn François Durant 《Journal of chemical crystallography》1996,26(11):777-789
Crystal structures of 5-(5-methylthien-2-yl)-2-deoxyuridine (I), 5-(5-thien-2-yl)-2-deoxyuridine (II) and 5-(5-bromothien-2-yl)-2-deoxyuridine (III) have been obtained from data collected on a four-circle Enraf-Nonius diffractometer (CAD-4 system). Space group, unit/cell parameters and finalR indices are:I, monoclinic,P21,a=9.105(2),b=20.819(2),c=7.932(2) Å, =98.79(2)°,R=5.7%;II, monoclinic,P21,a=8.720(4),b=20.793(4),c=7.884(4) Å, =95.06(2)°,R=5.8%;III, monoclinic,P21,a=9.260(2),b=41.655(7),c=7.926(2) Å, =97.996(13)°,R=9.4%. Structural properties of the title compounds are compared with those of 5-(5-chlorothien-2-yl)-2-deoxyuridine (IV) previously reported in order to explain their affinity for HSV-1 thymidine kinase and their eventual interaction with viral DNA polymerase. The main structural features observed are the coplanarity of the uracil and thienyl cycles stabilized by a S–O intramolecular interaction and the formation of dimeric intermolecular H bonds between two uracil moieties. 相似文献
4.
Rajnikant Dinesh Mousmi M.B. Deshmukh S.S. Patil Anshu Sawhney 《Journal of chemical crystallography》2004,34(10):693-696
The three-dimensional molecular and crystal structure of 2-(2'-propanonylthio)3-(o-methyl phenyl)quinazol-4(3H)-one has been determined by X-ray crystallographic methods. This compound crystallizes in the orthorhombic space group Pbca with unit cell parameters: a=9.649(5), b=30.102(10), c=11.403(9)Å. It has been solved by direct methods and refined to a residual index of 0.054. The magnitude of torsion along C16— C11— N3— C4 bond is 93.5(4)°. The dihedral angle between the plane comprising all the ring atoms of quinazoline moiety and the atoms of the methyl substituted phenyl ring is 94.12(1)°. The crystal structure is stabilized by one intramolecular C— HsO interaction and three intermolecular C— HsN contacts. 相似文献
5.
在酸性介质中,3,4-二乙酰基-2,5-己二酮与硝基苯胺作用,满意地得到了2,5-二甲基-3,4-二乙酰基-1-(硝基苯基)吡咯,用IR、1HNMR、高分辨质谱等对其进行了表征,并用X射线衍射测定了2,5-二甲基-3,4-二乙酰基-1-(3-硝基苯基)吡咯的晶体结构.该晶体属单斜晶系,P21/c空间群.晶体学数据如下:a=0.9375(1)nm,b=1.2814(2)nm,c=1.2985(1)nm,β=100.96(1)°,V=1.5315(3)nm3,Z=4,M=300.31,Dc=1.302×103kg/m3. 相似文献
6.
4-(2,5-二甲基-3,4-二乙酰基)-1-吡咯基苯甲酸的合成及其晶体结构 总被引:1,自引:0,他引:1
在强酸性介质中,3,4-二乙酰基-2,5-己二酮与对氨基苯甲酸作用,满意地得到了4-(2,5-二甲基-3,4-二乙酰基)-1-吡咯基苯甲酸,用IR、1H NMR、高分辩质谱等对其进行了表征,用X射线衍射测定了晶体结构.该晶体属三斜晶系,P1空间群,a=0.80950(10)nm,b=0.81910(10)nm,c=1.1900(2)nm,α=101.600(10)°,β=98.820(10)°,γ=104.960(10)°,Z=2,Dc=1.364×103kg/m3.拟合了苯环平面和吡咯环平面的平面方程,并求出两平面之间的二面角为68.11°. 相似文献
7.
Jesús Valdés-Martínez Simón Hernández-Ortega Anne K. Hermetet Lily J. Ackerman Carmina A. Presto John K. Swearingen Diantha R. Kelman Karen I. Goldberg Werner Kaminsky Douglas X. West 《Journal of chemical crystallography》2002,32(11):431-438
Reactions of 2-aminopicolines with 2- and 4-tolyl isothiocyanates yielded N-2-(4-picolyl)-N-4-tolylthiourea, 1, N-2-(3-picolyl)-N-4-tolylthiourea, 2, and N-2-(4-picolyl)-N-2-tolylthiourea, 3. Compound 1 is monoclinic, of space group P21/c with a = 7.456(1) Å, b = 13.135(3) Å, c = 13.959(3) Å, = 104.99(3)°, and V = 1320.5(5) Å3 with Z = 4, for d
calc = 1.294 g/cm3. Compound 2 is triclinic, of space group
with a = 6.877(3) Å, b = 7.590(5) Å, c = 13.213(9) Å, = 78.38(2)°, = 77.96(4)°, = 86.36(4)°, and V = 660.5(7) Å3 with Z = 2, for d
calc = 1.294 g/cm3. Compound 3 is monoclinic, of space group P21/c with a = 12.604(2) Å, b = 15.592(3) Å, c = 6.875(2) Å, = 91.05(2)°, and V = 1350.9(2) Å3 with Z = 4, for d
calc = 1.265 g/cm3. The three thioureas are found in both solid state and solution in a conformation resulting from intramolecular
hydrogen bonding. Compounds 1 and 3 present an intermolecular hydrogen bond involving the thione sulfur and the NH hydrogen, which is not present in 2 owing to the steric hindrance of the methyl group in the phenyl ring. The geometry of the molecule is affected by the position of the methyl groups on the pyridine and aryl rings. 相似文献
8.
9.
嘧啶类衍生物在医药、化工和功能材料等领域有着重要应用。在药物研发,特别是抗癌药物研发领域中,5-溴-2-(4-甲基哌啶-1-基)嘧啶是一种含嘧啶环的重要中间体。本文通过一步芳香亲核取代反应合成了5-溴-2-(4-甲基哌啶-1-基)嘧啶,经溶液结晶法获得其单晶体,并进行了晶体学分析(晶系:正交晶系,空间群:P212121,晶胞:a=10.181 42(6) nm, b=17.620 0(8) nm, c=10.179 02(5) nm,Z=4,ρc=1.478 g·cm-3,R=0.056 6,wR=0.168 8)。标题化合物的最优结构和前线轨道能量在B3LYP/6-311G(d, p)模式下使用密度泛函理论(DFT)计算得到,经DFT优化的结果与实验确定的数据相近。此外,为进一步揭示标题化合物的物理化学性质,通过DFT进一步研究了分子的静电式和前线分子轨道。 相似文献
10.
J. M. M. Smits Paul T. Beurskens J. R. M. Smits R. Plate H. Ottenheijm 《Journal of chemical crystallography》1988,18(1):15-24
The structure of the title compound, C23H24N4O3, was determined by X-rays.M
r
=404.47, orthorhombic, space groupPna21; unit cell dimensionsa=9.0386(4),b=28.0249(14),c=7.8936(9) Å,V
c
=1999.49(3) Å3,Z=4,D
x
=1.344 Mg m–1. CuK radiation (graphite crystal monochromator, =1.54178 Å),(CuK)=0.699 mm–1,F(000)=856,T=295 K. Final conventionalR-factor=0.030,R
w
=0.037 for 3215 unique reflections and 366 variables. The structure was solved by automated rotation functions in vector space, usingDirdif. The absolute configuration of the structure is reported. 相似文献
11.
以1,4,7-三氮杂环癸烷和氯甲基苯并咪唑为起始原料,一步反应合成了一种新的N-功能化的四齿配体,并用X射线衍射法测定了其铜(Ⅱ)配合物([CuClL]·[ClO4])的晶体结构.结果表明,该配合物由阳离子单元[CuClL]+和阴离子单元ClO4-组成,中心铜原子与一个氯离子、大环配体的三个氮原子和苯并咪唑基的一个氮原子配位,形成扭曲的四方锥结构.为了揭示配合物的配位性质与电子结构之间的关系,基于密度泛函理论,利用DFT-B3LYP/6-31G(d)研究了配合物的前沿分子轨道分布(HOMO,LUMO),Mulliken原子电荷和能带.计算结果表明,2-甲基苯并咪唑基侧基的N(4)原子比N(5)原子具有更强的电荷转移能力,因为N(4)的HOMO和LUMO组分比N(5)的大,证明了Cu和N(4)之间形成了配位键.此外,配合物的前线分子轨道能分别为-0.18722 a.u.(HOMO)和-0.10239 a.u.(LUMO).配合物的能级差ΔE(ELUMO-EHOMO)值为0.08483 a.u.,较小,说明其在光照条件下容易激发,不稳定. 相似文献
12.
An homologous series of mesomorphic compounds, the I-(4-alkoxy or alkyl-benzoyloxyphényl)-2-(4′-pentylphenyl)-ethanes, has been synthesized. The compounds with R = alkyl have low-melting points and wide mesomorphic ranges, for example from 33.5°C to 106.5C. The compounds with R = alkoxy exhibit a smectic polymorphism; for example a compound of this series is successively smectic B, F and C. The influence of the central linkage when the ethane group is replaced by an ester, single bond, ethylene, azomethine, azo, methylenecetone or cetone groups, is discussed. 相似文献
13.
The structure of diaquobis--(dimethylsulfoxo)bis(dimethylsulfoxo)dilithium tetraphenyl- borate, [Li2(Me2SO)4(H2O)2][BPh4]2, has been determined at 293 K. The compound crystallizes in the triclinic P-1 space group (a = 11.429(2) Å, b = 14.068(3) Å, c = 19.215(4) Å, = 69.31(3), = 88.98(3), = 89.03(3)). The lithium is coordinated to the oxygens of an aquo ligand, a terminal dimethylsulfoxo ligand, and two bridging dimethylsulfoxo ligands. The coordination geometry of each lithium is significantly distorted from a tetrahedron by the twisting of the plane containing the lithium ion and the two bridging dimethylsulfoxo oxygens relative to the plane containing the lithium ion and the terminal dimethylsulfoxo and aquo oxygen atoms. Hydrogen bonding between the aquo hydrogens and the phenyls of the tetraphenylborate anion is observed but does not result in a polymeric structure as has been observed in other lithium tetraphenylborate salts because of the 1:1 ratio of aquo ligands and tetraphenylborate anions. 相似文献
14.
Khalil J. Asali Tino Ladogana Simon G. Bott Gerard R. Dobson 《Journal of chemical crystallography》2003,33(9):701-704
The title compound crystallizes in the centrosymmetric triclinic unit cell, a = 6.6662(8) Å, b = 8.8584(6) Å, c = 13.574(2) Å, = 71.468(7)°, = 82.182(9)°, = 75.270(7)°, Z = 1. Refinement converged at R = 0.0396 for 1383 observed reflections. The molecule consists of two W(CO)5 fragments bridged centrosymmetrically by the 2,2,9,9-tetramethyl-3,7-dithiadecane ligand. 相似文献
15.
16.
John R. Peterson Terrence P. Everson Robin D. Rogers 《Journal of chemical crystallography》1990,20(1):37-45
CompoundA is (1,2,4)-1,2-diacetoxy-4-(4-methoxyphenyl)-6-methoxy-l,2,3,4-tetrahydronaphthalene, C22H24O6,M
r=384.43, monoclinic, P21/n, witha=11.074(3),b=10.353(4),c=17.616(4)Å,=94.96(2)°,V=2012.1Å3,D
calc=1.27 g cm–3 and=0.55 cm–1 forZ=4. Least-squares refinement of 1371 observed [F
05 (F
0)] reflections led to the final agreement index ofR=0.052. A twofold disorder was observed for the 1-acetoxy group whereas the 2-acetoxy group was ordered. CompoundB, (1,2,4)-1,2-diacetoxy-4-(2-methoxyphenyl)-8-methoxy-l,2,3,4-tetrahydronaphthalene, C22H24O6,M
r=384.43, crystallizes in the monoclinic space group, P21/c, witha=16.209(2),b=10.076(1),c=13.357(4)Å,=111.41(2)°,V=2030.9Å3,D
calc=1.26 g cm–3 and=0.54 cm–1 forZ=4. A final agreement index ofR=0.045 was realized by least-squares refinement of 1486 observed [F
o5 (F
o)] reflections. Intermolecular interactions in the cell lattices of compoundsA andB are noted. The title compoundsA andB were prepared by manganese(III) acetate oxidative dimerization of two molecules of 4-methoxystyrene and 2-methoxystyrene, respectively. 相似文献
17.
K. Yu. Suponitskii D. V. Gusev L. N. Kuleshova M. Yu. Antipin 《Crystallography Reports》2002,47(4):610-615
Two polymorphic modifications of 1-acetyl-3-(4-nitrophenyl)-5-(2′-furyl)pyrazoline (I) are investigated by X-ray diffraction with the purpose of analyzing the factors responsible for the formation of crystal structures of the optical nonlinear organic compounds. Both modifications crystallize simultaneously upon slow evaporation of a solution of compound I in an isopropanol-acetonitrile (3: 1) mixture. It is found that the molecular geometry of the polymorphic modifications is characterized by the rotation of the furan substituent with respect to the plane of the pyrazoline ring. The molecular hyperpolarizabilities (β) of both conformers are calculated. 相似文献
18.
采用水热法,合成了一个Zn(Ⅱ)配位聚合物[Zn3(4-PP)4(OH)2(SO4)2(H2O)2]n(1,4-PP=4-(1H-pyrazol-3-yl) pyridine),并用元素分析、红外光谱和X-射线单晶衍射对其进行了表征,测定了其热重性质和荧光性质.该配位聚合物1属于单斜晶系,P21/c群,其晶胞参数为:a=12.303(3) nm,b =6.0083(12) nm,c=25.308(5) nm,β=101.40(3)°,F(000)=1056,Dc=1.882 g/cm3,V=1833.8(6) nm3,Mr=1038.94,Z=2,μ(MoKα)=2.140 mm-1,R1=0.0672,wR2 =0.1300.在该配位聚合物1中,金属锌(Ⅱ)与SO24-以及OH-形成纯无机的二维层状结构,而4-PP配体仅作为端基配体;二维结构进一步通过氢键的作用形成三维超分子结构. 相似文献
19.
Benyong Lou Xia Guo Qi Lin Jingjing Lin Yiting Chen 《Journal of chemical crystallography》2009,39(11):831-834
Abstract
Ozagrel, (E)-3-[4-(1H-imidiazol-1-ylmethyl)phenyl]-2-propenic acid, crystallizes with fumaric acid in absolute ethanol to give the dihydrous fumarate salt, [(C13H13N2O2)2]2+ [C4H2O4]2−·2H2O, which crystallizes in the monoclinic space group P2(1)/n with a = 4.7981(19), b = 11.101(6), c = 26.930(11) Å, β = 90.567(16)°, V = 1434.3(11) Å3, Z = 4, C15H16N2O5, M r = 304.30, D c = 1.409 g/cm3. In the crystal structure, fumaric acid transfers two protons to imidazole ring N atoms of ozagrel. And the resulting carboxylate anions are simultaneously hydrogen-boned to carboxylic group and imidazole ring of ozagrel to give rise to a 2D layer structure. Hydrogen-bonding interactions between water and fumarate dianion result in a 3D structure. 相似文献20.
The higher-melting (mp 236°C)-isomer of dithioparachloral, i.e.,-2,4,6-tris(trichloromethyl)-1-oxa-3,5-dithian, is orthorhombic,Pnma,a=9.983(2),b=15.318(2),c=10.416(2) Å,V=1592.81 Å3,Z=4. The structure was solved by direct methods, from data collected at room temperature on an Enraf-Nonius CAD4 diffractometer, and refined by least-squares to a finalR value of 0.040 using 1017 reflections. The molecule is in the chair conformation with all threecis-CCl3 groups located pseudoequatorially. Endocyclic parameters are: torsion angles (deg) C-O-C-S 75.1(3), O-C-S-C –63.2(3), C-S-C-S 62.4(3); angles (deg) C-O-C 111.9(2), O-C-S 112.6(3), C-S-C 94.8(2), S-C-S 113.2(1); bond lengths (Å) O-C 1.426(5), C-S 1.824(4), S-C 1.818(3) (quoted in cyclic order). 相似文献