Synthesis and Crystal Structure of 1,3-Trans-1,4-cis- 3,4-di(4-bromophenyl)-1',2',3'-trihydro-1-hydroxy- benzo[g]bicyclo[3.3]octane-2-spiro-2'-indene-1'-one

1 INTRODUCTION Low-valent titanium reagents have exceedinglyhigh abilities to promote reductive coupling of car-bonyl compounds and they are attracting increasinginterest in organic synthesis[1]. Many other func-tional groups can also be coupled[2~8]. Recently, wehave reported some intermolecular reductive cou-pling reactions[9~12] and some new intramolecular re-ductive coupling reactions[13~16] induced by low-va-lent titanium reagents. The spiro[4.4]nonane skeleton has been found inmany…     

Synthesis and Crystal Structure of 3-(Pyrrole-2''-carboxamido)propanoic Acid·(1/2)H2O

3-(Pyrrole-2'-carboxamido)propanoic acid I has been synthesized from the reaction of β-alanine methyl ester with 2-trichloroacetylpyrrole followed by saponifying and acidating in 85.4% yield, and the crystal structure of 3-(pyrrole-2'-carboxamido)propanoic acid· (1/2)H2O (C8H11N2O3.5, Mr = 191.19) was obtained and determined by X-ray diffraction method. The crystal is of monoclinic, space group C2/c with a = 19.010(4), b = 8.3515(17), c = 13.788(3) (A), β = 125.88(3)°, V = 1773.6(6) (A)3, Z = 8, Dc = 1.432 g/cm3, λ = 0.71073 (A), μ-MoKα) = 0.114 mm-1 and F(000) = 768. The structure was refined to R = 0.0354 and wR = 0.0942 for 1642 observed reflections with I > 2σ(I). It is revealed that the title compound has one pyrrole ring and one propionic acid subchain linked by an amido bond at C(4), and there are 8 molecules of com- pound I and 4 crystal water molecules in each unit cell. The supramolecular layers are stabilized by the hydrogen bonds of N(2) H…O(2), N(1) H…O(4), O(4) H(1W)…O(2) and O(3) H…O(1).     

Synthesis, Crystal Structure and Antibacterial Activities of 3-[（2-Hydroxy-4-diethylamino-phenyl）methylenehydrazinocarbonyl]-4-hydroxy-6-methyl-2（1H）-pyridinones

1 INTRODUCTION Recently, compounds containing pyrazole, imida- zole, triazole (including benzotriazole), pyridine, tetrazole and indole have attracted much interest because of their fungicidal activity, plant-growth regulating activity and antibacterial activity[1～3]. Schiff bases also constitute a good type of biolo- gically active substructures[4～7]. Studies of pyri- dine Schiff base-type fungicides have been repor- ted[8]. However, some structures of pyridine com- pounds containing h…     

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…     

Crystal Structure of 1, 1-Dichloro-la, 3-diphenyl-1, la, 2, 3-tetrahydro-azirino [2, 1-d ] [1, 5]benzothiazepine (C_(22),H_(17)Cl_2NS )

1INTR0DUCTI0NBenzoheteroazepinecompoundsareimportantpharmaceuticalagents"-".Inre-centyears,ithasbeenfoundthatbenzoheter0azepinetricyclicderivatives,especiallythosefusedwithotherfiveorsix-memberedheterocycle,area1soofpotentialphar-maceuticalinterestst4-6j.Hence,muchattentionhasbeenpaidtothesynthesesofthem,suchasl,3-oxazino[3,2-djt1,5jbenzothia/diazepin-l-onet"'J,1,2,4-tria-zolo[4,3-dj[1,5jbenzothia/diazepine"',1,2,4-oxadiazolo[4,5-dj[l,5jbenzothia/diazepine',',andsoon.Meanwhiletheirstructur…     

Synthesis and Crystal Structure of a Novel Ternary Ni(II) Complex with 2-Hydroxyl-1,10- phenanthroline and 2-Hydroxynicotinic Acid as Ligands

1 INTRODUCTION The chelate ligand phenanthroline (phen) and its derivatives have played an important role in the development of coordination chemistry[1～6]. In the last few years, the synthesis and reaction mechanism of 2-hydroxyl-phenanthroline (HOphen) complexes, in particular, attract much attention due to their unusual “anomalies”. Gillrad[7] proposed the mecha- nism about this kind of reaction as follows: nucleo- philic -OH or H2O attacking α-C of coordinated he- terocyclic lig…     

湿化学法合成LiNi_(1/3)Mn_(1/3)Co_(1/3)O_2及其表征(英文)

利用琥珀酸为鳌合剂的湿化学法成功合成了一系列锂离子电池正极材料LiNi1/3Mn1/3Co1/3O2,在合成过程中改变琥珀酸与金属离子摩尔比(R)并研究了这一参数对合成LiNi1/3Mn1/3Co1/3O2材料物理及电化学性质的影响.采用热重、X射线衍射、Rietveld精修、扫描电镜以及超导量子干涉仪对反应机理、材料的结构、形貌以及磁学性质进行了详细表征.得到最佳合成条件为R=1,此时LiNi1/3Mn1/3Co1/3O2的阳离子混排度最低.此外,通过Rietveld精修得到该材料阳离子混排度的结果与通过磁学方法得到的结果定量相符,如对于在R=1条件下合成的样品,Rietveld精修结果显示其阳离子混排度为1.85%,而超导量子干涉仪的测试结果为1.80%.当充放电区间为3.0-4.3V,电流密度为0.2C(1C=160mA·g-1)时,该样品的首次放电容量为161mAh·g-1,库仑效率为93.1%,经过50次循环后,容量保持率可达91.3%.     

Synthesis and Crystal Structure of 2-(4-Fluoro-2-(4-fluorophenoxy) phenyl)-1-(1H-1,2,4-triazol-l-ylmethyl)-3-methoxy-isopropy Alcohol

The title compound 2-(4-fluoro-2-(4-fluorophenoxy)phenyl)-1-(1H-1,2,4-triazol-z 1-ylmethyl)-3-methoxy-isopropy alcohol has been synthesized by the treatment of 1-[2-(4-fluoro-2-(4-fluorophenoxy)phenyl)-2,3-epoxypropyl]-1H-1,2,4-tdazole with sodium methoxide. It be-longs to orthorhombic, space group P212121, with a=9.7229(19), b=11.516(2), c=16.047(3) A, C18H17F2N3O3, Mr-361.35, V=1796.7(6) A3, Z=4, Dc=1.3359 g/cm3, F(000)=752,μ=0.106 mm-1, the final R=0.0329 and wR=0.0803 for 1821 unique reflections. The dihedral angles made by the triazole ring with two benzene rings are 43.56(3) and 54.78(2)°, respectively. The intermolecular hydrogen bond in the crystal lattice plays an important role in stabilizing the structure.     

TiO2包覆对LiCO1/3Ni1/3Mn1/3O2材料的表面改性

为了提高材料LiCo1/3Ni1/3MnO2的循环件能,采用浸渍-水解法对其进行TiO2包覆.用X射线衍射(XRD)、电化学交流阻抗谱(EIS)、电感耦合等离子体发射光谱(ICP-OES)和恒流允放电测试研究包覆材料的结构和电化学性能.TiO2仅在材料表面形成包覆层,并未改变材料的结构.TiO2包覆能提高材料LiCo1/3Ni1/3Mn1/3O2的倍率性能和循环性能,TiO2包覆后的材料在5.0C(1.0C=160 mA·g-1)下的放电容量达到0.2C下的66.0%,而包覆前的材料在5.0C下的放电容量仅为其0.2C下的31.5%.包覆后的材料在2.0C下循环12周后的容最没有衰减,而未包覆的材料容量保持率仅为94.4%.EIS测试表明包覆材料性能的提高是由于循环过程中材料的界面稳定性得到了提高.循环后材料的XRD和ICP-OES测试表明,包覆层能提高材料LiCo1/3Ni1/3Mn1/3O2的结构稳定性.     

Synthesis and Crystal Structure of 5-[（1H-1,2,4-Triazol-1- yl）methyl]-4-（2,3-dimethoxybenzylideneamino）-2- 2H-1,2,4-triazole-3（4H）-thione Monohydrate

1 INTRODUCTION Heterocyclic compounds bearing the 1,2,4-tri- azole moiety have attracted considerable attention over the past few decades since they exhibit some fungicidal activities against Puccinia recondite and applications in the field of root-growth regu- lation[1~3]. Meanwhile, 4-amino-5-mercapto-1,2, 4-triazole moiety has great versatility in fusing tovarious ring systems and possesses a broad spec- trum of biological activities[4, 5]. In our con- tinuous work directed towards the…     

Synthesis, Crystal Structure and Fungicidal Activity of （Z）-3,3-Dimethyl-1-（1H-1,2,4-triazol-1-yl）butan-2-one O-2-Chlorobenzyl Oxime Nitrate

The title compound has been synthesized by the reaction of 3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65～68% HNO3. Its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 14.5481(8), b = 9.3351(5), c = 13.1911(7) , β = 98.9450(10)°, Z = 4, V = 1769.67(17) 3, Mr = 369.81, Dc = 1.388 g/cm3, S = 1.06, μ = 0.247 mm-1, F(000) = 776, the final R = 0.0352 and wR = 0.0960 for 3069 observed reflections (I > 2σ(I)). X-ray crystal structure presents the intramolecular N–H…O hydrogen bond. The packing is nearly parallel without π-π stacking interactions between two adjacent phenyl rings and stabilized by Van der Waals force. The preliminary bioassay shows that the title compound possesses fungicidal activity against Gibberella zeae at the dosage of 25 mg/L.     

Synthesis and Crystal Structure of 2-（4-Fluoro-2-（4-fluorophenoxy）phenyl）-1-（1H- 1,2,4-triazol-1-ylmethyl）-3-methoxy-isopropy Alcohol

The title compound 2-（4-fluoro-2-（4-fluorophenoxy）phenyl）-1-（1H-1,2,4-triazol- 1-ylmethyl）-3-methoxy-isopropy alcohol has been synthesized by the treatment of 1-[2-（4-fluoro- 2-（4-fluorophenoxy）phenyl）-2,3-epoxypropyl]-1H-1,2,4-triazole with sodium methoxide. It belongs to orthorhombic, space group P212121, with a = 9.7229（19）, b = 11.516（2）, c = 16.047（3）A, C18H17F2 N3O3, Mr = 361.35, V = 1796.7（6）A^3, Z = 4, Dc = 1.3359 g/cm^3, F（000） = 752, p = 0.106 mm^-1, the final R = 0.0329 and wR = 0.0803 for 1821 unique reflections. The dihedral angles made by the triazole ring with two benzene rings are 43.56（3） and 54.78（2）°, respectively. The intermolecular hydrogen bond in the crystal lattice plays an important role in stabilizing the structure.     

Synthesis and Crystal Structure of 3-(Pyrrole-2′-carboxamido)propanoic Acid·(1/2)H_2O

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 to produce pharmaceutical, essences, biochemicals, etc. It has been found that a great number of pyrrole derivatives present antitumor and antiviral activi- ties[2 ~ 5]. During our searches for bioactive com- pounds, a series of pyrrole derivatives were synthe- sized[6, 7]. We report here the synthesis of 3-(pyrrole- 2?-…     

Two New Three-dimensional Supramolecular Complexes with 5-Carboxyl-1-carboxymethyl-2-oxidopyridinium: Syntheses and Crystal Structures

Two new supramolecular complexes [MnL(H2O) 4](1) and [ZnL(H2O) 5]·0.25H2O(2) (H2L = 5-carboxy-1-carboxymethyl-2-oxidopyridinium) have been synthesized and structurally characterized by elemental analysis,IR and X-ray single-crystal structure determination. Complex 1 crystallizes in the monoclinic system,space group P21/n with a = 5.1537(2) ,b = 21.2008(9) ,c = 10.9727(4) ,β = 99.182(2) °,V = 1183.54(8) 3,C8H13MnNO9,Mr = 322.13,Dc = 1.808,Z = 4,F(000) = 660,μ = 1.160,R = 0.0372 and wR = 0.0750 for 2217 observed reflections(I > 2σ(I)) . Complex 2 crystallizes in the triclinic system,space group P1 with a = 7.730(2) ,b = 8.030(2) ,c = 11.400(2) ,α = 104.27(3) ,β = 92.93(3) ,γ = 102.67(3) °,V = 664.9(2) 3,C8H15.5ZnNO10.25,Mr = 355.08,Dc = 1.774,Z = 2,F(000) = 365,μ = 1.899,R = 0.0243 and wR = 0.0695 for 2759 observed reflections(I > 2σ(I)) . Their thermal properties have been studied.     

Crystal Structure of (1R,4R;1S,4S)2-Amino-3-Cyano-1,4-Diphenyl-2-Cyclopentene-1-ol

1INTRODUCTIONIntheearly1970'sthreegroupsofinvestigatorsL,~,'foundthatlow-valenttita-nium,preparedbythereactionofstrongreducingagentswithtitaniumtrichlorideortitaniumtetrachlorideintetrahydrofuran,canabstractoxygenfromketonesoraldehydes,leadingtotheforma-tionofolefins.Theinterestinthereactioninducedbylow--valenttitaniumreagentsisincreasingandalargenumberoffunctionalgroupscanbereduceds4-6).Recent-ly,wefoundthatthetitlecompoundisObtainedbycy-cllzatlonreactionof(3--oxo-1,3-diphenyl)propyl-pro…     

TiO2包覆对LiCo1/3Ni1/3Mn1/3O2材料的表面改性

为了提高材料LiCo1/3Ni1/3Mn1/3O2的循环性能, 采用浸渍-水解法对其进行TiO2包覆. 用X射线衍射(XRD)、电化学交流阻抗谱(EIS)、电感耦合等离子体发射光谱(ICP-OES)和恒流充放电测试研究包覆材料的结构和电化学性能. TiO2仅在材料表面形成包覆层, 并未改变材料的结构. TiO2包覆能提高材料LiCo1/3Ni1/3Mn1/3O2的倍率性能和循环性能, TiO2包覆后的材料在5.0C(1.0C=160 mA·g-1)下的放电容量达到0.2C下的66.0%, 而包覆前的材料在5.0C下的放电容量仅为其0.2C下的31.5%. 包覆后的材料在2.0C下循环12周后的容量没有衰减, 而未包覆的材料容量保持率仅为94.4%. EIS测试表明包覆材料性能的提高是由于循环过程中材料的界面稳定性得到了提高. 循环后材料的XRD和ICP-OES测试表明, 包覆层能提高材料LiCo1/3Ni1/3Mn1/3O2的结构稳定性.     

Synthesis and Crystal Structure of Trans-4-[(5-(2,4-Dichlorophenoxy)-3-methyl-1-phenyl-1H-pyrazol-4-yl)methyleneamino]-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one

The title compound trans-4-[(5-(2,4-dichlorophenoxy)-3-methyl-1-phenyl-1H-pyra-zol-4-yl)methyleneamino]-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 (C28H23Cl2N5O2, Mr = 532.41) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1 with a = 8.9438(4), b = 11.6065(5), c = 14.2215(6) , α = 112.566(1), β = 92.324(2), γ = 102.91(1)o, V = 1315.65(10) 3, Z = 2, Dc = 1.344 g/cm3, μ(MoKα) = 0.282 mm-1, λ = 0.71073 , F(000) = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections (I > 2σ(I)). X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra-and intermolecular C(12)-H(12)···O(1) and C(28)-H(28)···O(1)#1 hydrogen bonds were observed in the title compound.     

Crystal structure of the 1:2:2 adduct of piperazine, o-phthalic acid and water.

The adduct of piperazine, o-phthalic acid and water (1:2:2), C20H26N2O10, crystallizes in the monoclinic space group P21/c with a = 6.129(1), b = 12.810(2), c = 13.137(2)A, beta = 95.87(1) degrees, V = 1026.0(3)A3, Z = 2. The piperazinium adopts a chair comformer, and is tied with the hydrogen orthophthalate via a hydrogen bond of the N-H...O type. Because of bifurcated hydrogen bonding of C(sp3)H-O [3.0801(17) and 3.1408(18)A] and the shortest hydrogen bond of C(sp3)H-O [2.9758(17)A], C(sp3)H-O hydrogen bonds play important roles in stablizing the title adduct.     

Crystal Structure of Trans-2-Amino-3-Cyano-4-(3',4'-Methylenedioxyphenyl)-1-Phenyl-2-Cyclopentene-r-1-ol

1INTRODUCTIONIntheearlyseventiesthreegroupsofinvestigators('--"establishedthatlow--va-lenttitanium,preparedbythereactionofstrongreducingagentsontitaniumtrichlo-rideortitaniumtetrachlorideintetrahydrofuran,canabstractoxygenfromketonesoraldehydes,leadingtotheformationofolefins.Anincreasinginterestinthereac-tioninducedbylow--valenttitaniumreagentsisobservedandalargenumberoffunc-tionalgroupscanbereducedt4--6).However,thereactionoflow-valenttitaniumreagentwith4,4--dicyano--1,3--diaryl--l-butano…     

Crystal Structures of Schiff Base from 4-Aminoantipyrine and Pyridine- 2-carboxaldehyde and Its Perchlorate

The Schiff base pyridine-2-carboxaldehyde-4-aminoantipyrine （CI7H16N4O 1） and its perchlorate （C17H17N4O·ClO4 2） have been prepared and characterized by elemental analysis, IR spectra and single-crystal X-ray crystallography analysis. Both 1 and 2 crystallize in the monoclinic system, space group P21/c. For 1, a = 8.6820（12）, b = 24.934（3）, c = 7.0064（10） A,, β= 97.942（3）°, V = 1502.2（4） A^3, Z = 4, Dc = 1.293 g/cm^3, F（000） = 616,μ = 0.084 mm^-1, the final R = 0.0592 and wR = 0.1244. For 2, a = 5.9302（2）, b = 20.347（7）, c = 14.663（6） A, β= 90.200（9）°, V= 1769.201） A^3, Z = 4, Dc = 1.475 g/cm^3, F（000） = 816, μ = 0.254 mm^-1, the final R = 0.0533 and wR = 0.0819. As expected, both molecular structures of 1 and 2 adopt a trans configuration about the central C=N double bond. 2 is an ionic compound with the protonation at N（1） of pyridine-2-carboxaldehyde-4- aminoantipyrine.