Synthesis and Molecular Structure of (E)-1-(Morpholino)-2-(thiomethyl)-2-phenylvinylphosphonate

1 INTRODUCTION Phosphorus-containing vinyl compounds havebeen widely studied due to their versatile physiolo-gical activities and applications in transition metalchemistry, asymmetric catalysis and photorearrange-ment[1～4]. In our previous papers, we have reportedthe syntheses of 2,2,4,5-tetrasubstituted-1,3-dithio-les[5] and 2,5-bis(morpholino)-3,4-bis-(p-chloro-phe-nyl)thiophenes[6] by the reactions of α-thioaroyl-thiofor-mamide with trimethyl phosphite at room tempera-ture and in refl…     

基于呋喃-3-酮配体的铜(Ⅱ)配合物的合成及其晶体结构

以4-甲酰基-2,2,5,5-四甲基四氢呋喃-3-酮和间甲基苯胺为原料,经缩合反应制得配体(Z)-4-[(间甲苯胺基)亚甲基]-2,2,5,5-四甲基二氢呋喃-3(2H)-酮(L);以Cu(CH_3COO)_2为铜源,L经配位反应合成了一个新型的铜(Ⅱ)配合物[Cu(L)_2]_n(I),其结构经FT-IR,X-射线单晶衍射和元素分析表征。I属单斜晶系,P2(1)/c空间群,晶胞参数a=11.361 3(19)?,b=24.564(4)?,c=12.026(2)?,α=γ=90°,β=110.452(3)°,V=3 144.6(9)?~3,Dc=1.226 g·cm~(-3),Z=4,R_1=0.051 5,wR_2=0.113 2。     

[Co(N-(3-Aminopropyl)-1,3-propanediamine)(2-(Aminomethyl)pyridine) Cl][ZnCl_4]的一对差向异构体的合成及晶体结构

用过氧化物法合成了 [Co(3,3-tri)(amp)Cl][ZnCl4]的两个经式异构体,晶体结构解析表明两者互为差向异构体。其中反式异构体 (仲氢相对于 Cl)晶体属单斜晶系,空间群 C2/c, a=2.7663(7)nm, b=0.9505(1)nm, c=1.8288(4)nm,β =105.57(2)°, V=4.632(1)nm3, Dc=1.706g· cm-3, Z=8, F000=2432.00,μ (MoKα )=23.51cm-1, R=0.033, Rw=0.041;顺式异构体 (仲氢相对于 Cl)晶体属三斜晶系,空间群, a=1.0790(2)nm, b=1.1749(1)nm, c=0.8920(1)nm,α =90.73(1)°,β =109.573(9)°,γ =80.60(1)°, V=1.0500(2)nm3, Dc=1.71g· cm-3, Z=2, F000=548.00,μ (MoKα )=25.73cm-1, R=0.022, Rw=0.030。两异构体中 Co3＋为六配位,其差异仅表现在 3,3-tri仲胺上氢的取向不同。     

Synthesis and Molecular Structure of 1-Acetyl-1-（4-iodophenyl）-3-cyclohexylurea

1INTRODUCTION N-acyl urea is an important class of compounds because of their various bioactivities,and they can be used as pesticides[1]and pharmaceuticals[2].On the other hand,many natural products bearing N-acylurea functionality also exhibit the inter…     

Solid State Synthesis and Structural Characterization of Binuclear Cu(I)-SbPh3 Complex [Cu(SbPh3)2I]2

Dimeric complex [Cu(SbPh3)2I]2 has been synthesized by a solid state reaction at a low heating temperature and its crystal structure has been analyzed by X-ray crystallography. The crystal is monoclinic, space group P21/a (#14), a = 20.436(5), b=14.125(3), c=24.683(3)(A), β=110.67(1)°, Z=4, V=6666(2)(A)3; C72H60Sb4I2Cu2, Mr = 1792, Dc = 1.787 g.cm-3, μ(MoKα) = 31.88 cm-1, F(000)=3440, R=0.038 and Rw=0.043 for 5632 observed reflections (I≥3.0σ(I)) and 361 refined parameters. The result reveals the copper and the bridging iodide atoms form an approximately planar rhomboid array. Effects of the bulkiness of the ligands upon the structures of the analogous complexes are discussed.     

Crystal and Molecular Structure of 5，6，7，8，9，10－Hexahydro－3－（4－methylphenylamino）－2－thioxoquinoxaline

ＣｒｙｓｔａｌａｎｄＭｏｌｅｃｕｌａｒＳｔｒｕｃｔｕｒｅｏｆ５，６，７，８，９，１０－Ｈｅｘａｈｙｄｒｏ－３－（４－ｍｅｔｈｙｌｐｈｅｎｙｌａｍｉｎｏ）－２－ｔｈｉｏｘｏｑｕｉｎｏｘａｌｉｎｅＳｕｎＤａ－Ｑｉｎｇ；ＬａｎｇＪｉａｎ－Ｐｉｎｇ；ＬｕＺｈ...     

Syntheses and Crystal Structures of 4-Amino-3- （3-hyd roxyp ropyl）- 1H-1,2,4-triazole-5（4H）-thione and 6-（4-Biphenylyl）-3-（3-hydroxypropyl）-7H-1,2,4-triazolo[3,4-b][1,3,4]thiadiazine

1INTRODUCTION It has been reported that3,6-disubstituted-7H-1,2,4-triazolo[3,4-b][1,3,4]thiadiazines have a broad spec-trum of bioactivities,such as antimicrobial[1],antibac-terial,antifungal[2],anti-inflammatory[3],diuretic[4],an-thelmintic and analgesic[5].They can also be used as plant-growth regulating agents[6],photographic coup-lers,dyes for improved preservability and absorption characteristics,and inhibitors of malignant cellularZOU K.H.et al.:Syntheses and Crystal Structures o…     

Synthesis and Crystal Structure of (Z)-Ethyl-4-(4-methoxy)benzylidene-2-(3,5-dimethoxypheny-tetrahydrofuran-3,3-dicarboxylate

The title compound (Z)-ethyl-4-(4-methoxy)benzylidene-2-(3,5-dimethoxyphenyl)- tetrahydrofuran-3,3-dicarboxylate has been synthesized, and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1-, with a = 8.140(3), b = 11.966(4), c = 13.771(5) α = 67.366(4), β = 85.165(5), γ = 75.806(4)°, V = 1200.1(7) 3, Z = 2, C26H30O8, Mr = 470.50, Dc = 1.302 g/cm3, F(000) = 500, λ(MoKα) = 0.71073 , μ = 0.096 mm–1, R = 0.0659 and wR = 0.1841 for 3080 observed reflections (I > 2σ(I)). As a key intermediate of HIV-1 integrase inhibitor, the synthesis and structure confirmation of the title compound are important for further studies.     

Synthesis and Crystal Structure of（E）-Ethyl 2-（4-（2,4-dimethoxybenzylideneamino）-5-（3,4,5-trimethoxyphenyl）-4H-1,2,4-triazol-3-ylthio）acetate

The crystal structure of the title compound(E)-ethyl 2-(4-(2,4-dimethoxy benzylide-neamino)-5-(3,4,5-trimethoxyphenyl)-4H-1,2,4-triazol-3-ylthio)acetate(4,C24H28N4O7S,Mr = 516.17) was synthesized and determined by X-ray single-crystal diffraction.The crystal belongs to the monoclinic system,space group P21/n with a = 13.162(2),b = 8.4506(13),c = 22.602(4) ,β = 99.888(3)°,μ = 0.183 mm-1,V = 2476.5(7)3,Z = 4,Dc = 1.385 g/cm3,F(000) =1088,T = 110(2) K,R = 0.0426 and wR = 0.1216 for 3859 observed reflections with I > 2σ(Ⅰ).     

Synthesis and Crystal Structure of （Z）-Methyl-3-methoxy-2-{2-[（4-（E-3-p-tolylacryloyl）phenoxy）methyl]phenyl}acrylate

The title compound,(Z)-methyl-3-methoxy-2-{2-[(4-(E-3-p-tolylacryloyl)phenoxy)-methyl]phenyl}acrylate,was synthesized and determined by X-ray single-crystal diffraction. The crystal belongs to the triclinic system,space group P1 with a = 8.0157(8),b = 12.5748(13),c = 13.3768(14) ,α = 64.770(2),β = 75.720 (2),γ = 89.784(2)°,μ = 0.085 mm-1,Mr = 442.49,V = 1174.1(2) 3,Z = 2,Dc = 1.252 g/cm3,F(000) = 468,T = 294(2) K,R = 0.0603 and wR = 0.1498 for 2644 observed reflections with I 2σ(I). X-ray diffraction analysis reveals that the single crystal contains strong non-classical hydrogen bonds. The preliminary bioassay showed that the title compound exhibits inhibitory activity against the Pseudoperoniospora cubensis and Rhizoctonia solani at the test concentration of 200 mg/L.     

Synthesis and Crystal Structure of (1-Naphthyl){[3- (2,6-dibromo-4-methylphenylimino)methyl]-5-chloro- 2-hydroxy-benzaldehyde}(triphenylphosphine) Nickel(II) Triphenylphosphine

1INTRODUCTION Over the past decades,olefin oligomerization and polymerization based on late transition metal catalysts have been the most exciting developments in the area of organometallic chemistry and polymer science[1～3].In this broad context,neutral nickel(II)complexes have attracted much attention for their less sensitivity to protonic solvents and polar mon-mers.The most typical one is the SHOP-type cata-lyst[4～6],which contains an anionic[P,O]chelate ring and shows high activ…     

Syntheses and Crystal Structures of Methyl 2-（4,5-Dibromo- 1-methylpyrrole-2-carbonylamino）-3-phenyl propanoate and 4,5-Dibromo-1-methyl-2-trichloroacetylpyrrole

1 INTRODUCTION Pyrrole and its derivatives have attracted much attention due to their chemical properties as well as biological activities[1]. They have been widely used as the materials to produce pharmaceutical, essences, biochemicals, etc. It has been found that a great deal of pyrrole derivatives present bioactivities, such as antitumor and antiviral activities[2~5]. Thus, due to the interest in exploring the syntheses of potential bioactive materials which contain pyrrole ring andna…     

(Z)-1[2-(苯基二溴化锡基)乙烯基]-1-环己醇的合成及晶体结构

报道了标题化合物〔C14H18Br2OSn〕的合成及晶体结构。该晶体属于单斜晶系，空间点群为P21/c，晶胞参数a=11.711(2)，b=9．114（2），c=16．864（3）A，β=102.94（1）°，V=1604.55（0）A3，Mr=480．78，Z=4，Dc=1．99g／cm3，u=65．20cm－1，F（000）=919，R=0．050，Rw=0．050．晶体结构由直接法解出。标题化合物分子中的锡原子被配体的2个碳、2个溴和1个氧原子配位，配位原子呈畸变的三角双锥构型，环已基为椅式构象，五员杂环为信封构象。     

Molecular Structure of 1- (Diisopropyl )amino-2-(p-methyl )phenyl-3-methyl-phosphetane 1-oxided

lINTR0DUCTIONThechemistryofstablephospheniumcati0n[Rl-P-R2j hasbeenextensivelyknowntl-3).Wereportedsynthesesandreactions0fthephospheniumcati0nsfeatur-ingwithanS-P-Nlinkage.(4-8)Recentlywefoundthatphospheniumion[i-Pr2N-P-Clj [AlC'j-canregiOselectivelyinsertintophenylcyclopropaneringattwocycliccarbon-carbonb0ndsadjacenttophenylgr0uptogivel-(diisopropyl)amin0-2-(p-methyl)phenyl-3-methyl-phosphetanel-oxide(1).Inordertodisclosetherelativesterelchemistry,itssinglecrystalwasobtainedfromn-he…     

Synthesis, Crystal Structure and Fungicidal Activity of 3- ( 4- Chloro- 3- ethyl- 1 -methyl- 1 H- pyrazol- 5-yl ) - 6- (E) phenylvinyltriazolo [ 3, 4-b ] - 1,3, 4-thiadiazole

1　ＩＮＴＲＯＤＵＣＴＩＯＮＩｎｒｅｃｅｎｔｙｅａｒｓ ,ｔｒｉａｚｏｌｏ[3,4, ｂ] 1 ,3,4 ｔｈｉａｄｉａｚｏｌｅｄｅｒｉｖａｔｉｖｅｓｈａｖｅｂｅｅｎａｔ ｔｒａｃｔｉｎｇｍｕｃｈａｔｔｅｎｔｉｏｎｆｒｏｍｃｈｅｍｉｓｔｓａｎｄｐｈａｒｍａｃｏｌｏｇｉｓｔｓｂｅｃａｕｓｅｔｈｅｙｓｈｏｗｂｒｏａｄｓｐｅｃｔｒａｏｆｂｉｏｌｏｇｉｃａｌａｃｔｉｖｉｔｉｅｓ,ｓｕｃｈａｓｉｎｓｅｃｔｉｃｉｄａｌ[1 ] ,ａｎｔｉｆｕｎｇａｌ[2 ] ,ｈｅｒｂｉｃｉｄａｌ[3] ,ａｎ ｔｉｂａｃｔｅｒｉａｌ[4] ,ｈｙｐｏｔｅｎｓｉｖ…     

Synthesis and Crystal Structure of Ethyl 3-（4-Chlorophenyl）-3,4-dihydro-6-methyl-4-oxo-2- （pyrrolidin-1-yl）furo[2,3-d]pyrimidine-5-carboxylate

The crystal structure of the title compound ethyl 3-（4-chlorophenyl）-3,4-dihydro-6- methyl-4-oxo-2-（pyrrolidin-1-yl）furo[2,3-d]pyrimidine-5-carboxylate （C20H20ClN3O4, Mr= 401.84） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 20.6215（9）, b = 8.5311（4）, c = 21.6886（9） A^°, β = 91.607（1）°, V = 3814.0（3）A^°^3, Z = 8, Dc = 1.400 g/cm^3, F（000） = 1680, μ = 0.233 mm^-1, R = 0.0718 and wR = 0.1545 for 6717 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals two crystallographically independent molecules in the asymmetric unit.     

Crystal Structure of 5-(l-Menthyloxy)-3-Bromo-4-(R)-(+)-Methylbenzylamino-2(5H)-Furanone

１ＩＮＴＲＯＤＵＣＴＩＯＮＳｅｖｅｒａｌｉｍｐｏｒｔａｎｔａｐｐｒｏａｃｈｅｓｔｏｔｈｅｓｙｎｔｈｅｓｉｓａｎｄｐｒｏｐｅｒｔｉｅｓｏｆｃｈｉｒａｌγ ａｌｋｙｌｏｘｙｂｕｔｅｎｏｌｉｄｅｓｈａｖｅａｔｒａｃｔｅｄｍｕｃｈａｔｅｎｔｉｏｎｏｗｉｎｇｔ...     

Synthesis and Crystal Structure of Ethyl 1-（2-bromoethyl）-3-（4-meth-oxyphenyl）-1H-pyrazole-5-carboxylate

The title compound ethyl 1-(2-bromoethyl)-3-(4-methoxyphenyl)-1H-pyrazole-5-carboxylate 1 has been synthesized and structurally characterized by single-crystal X-ray diffraction.The crystal is of monoclinic(C15H17BrN2O3,Mr = 353.22),space group C21 with a = 24.691(7),b = 6.7678(17),c = 17.884(5) ,β = 97.184(5)o,V = 2965.1(13) 3,Z = 8,Dc = 1.583 g.cm-3,F(000) = 1440,μ = 2.784 mm-1,the final R = 0.0260 and wR = 0.0596 for 2684 observed reflections with I > 2σ(I).All the carbon atoms in the molecule are nearly coplanar except C(15),with a large conjugated system among the carbonyl group,pyrazole ring and the benzene ring.Three non-classical intermolecular hydrogen bonds help to stabilize the crystal lattice.The regioselectivity was rationalized based on the coordination of potassium ion with the N-anion and the carbonyl oxygen atom.     

Synthesis and Crystal Structure of （Z）-1- （3-Fluorobenzyl）-5-（（3-fluorobenzylimino）（2-hydroxy-4-methoxyphenyl）methyl）pyridin-2（1H）-one

The title compound （Z）-1-（3-fluorobenzyl）-5-（（3-fluorobenzylimino）（2-hydroxy-4- methoxyphenyl）methyl）pyridin-2（1H）-one （C27H22F2N2O3,Mr = 460.47） was synthesized and crystallized. The crystal belongs to the triclinic system,space group P1 with a = 9.951（6）,b = 10.059（6）,c = 12.927（7）A,α = 109.828（7）,β = 102.304（7）,γ = 104.898（7）°,Z = 2,V = 1110.2（11）A^3,Dc =1.377 Mg/m^3,μ（MoKα） = 0.102 mm^-1,F（000） = 480,the final R = 0.0449 and Rw = 0.1250 for 4595 observed reflections （I 〉 2σ（I））. X-ray analysis reveals that both m-fluorobenzyl groups are diorientationally disordered because of the rotation of C–C single bond which was represented as F（1）,F（2） and F（1＇）,F（2＇）. The diorientational disorder was refined and gave the occupancies of 0.665（4） and 0.335（4） for F（1） and F（1＇）,0.631（3） and 0.369（3） for F（2） and F（2＇）. Hydrogen bonds existing in the cell link different components to stabilize the crystal structure. The active data proved that the title compound has good anti-HBV activity.     

Synthesis, Crystal Structure and Fluorescent Properties of 1-（4-（Dimethylamino）benzylidene）- 4-（naphthalen- 1-yl） Thiosemicarbazide

1 INTRODUCTION Recently, for the fluorescent properties, Schiff base has been more and more important and widely studied in density optical memories, nonlinear op- tics (NLO), organic light-emitting diodes (OLED), polymer LED and electrogenerated chemilumines- cence (ECL)[1~5]. Thiosemicarbazones are a kind of Schiff bases with thiourea and good ligands easily chelating with transition metal ions. Although they have been studied extensively for a long time due to their chemical and b…