Synthesis and Crystal Structure of 1-（4-Bromobenzoyl）-3- [5-（E）-styryl-1,3,4-thiadiazol-2-yl]urea

1 INTRODUCTION 1,3,4-Thiadiazole derivatives represent an interes- ting class of compounds possessing broad spectrum biological activities[1~4]. Aroyl ureas are known to exhibit diverse biological effects, such as insecticidal, fungicidal, herbicidal and plant growth regulating activities[5~8]. Therefore, it is worthwhile to investi- gate the compounds incorporating both 1,3,4-thiadia- zole nucleus and aroyl urea group. In the previous paper[9], a series of aroyl ureas containing 1,3,4-t…     

Synthesis and Crystal Structure of Spiro[1-bromo(S)-4-(R)-hydroxy-5-oxa-6-oxo-bicyclo[3.1.0]hexane-2,2''''-(3''''-diethyl-α-(S)-4''''''''-Cl-benzyloxyphosphonyl-4''''-(1R,2S,5R)-menthyloxybutyrolactone)]

1 INTRODUCTION In recent years, phosphorus compounds havebeen playing an important role in the new “high-tech” areas including life science and industrial te-chnology[1, .At the same time, the asymmetric syn- 2]thesis of various natural compounds containing cyc-lopropane components and organophosphorus grouphas attracted much attention due to their special bio-logical functions and antibiological activities[3～5].Despite the great advances in these areas, no novelapproach to the efficien…     

Synthesis, Crystal Structure, Antibacterial Activities and Theoretical Computation of 3-（2-Hydroxybenzly）-4-（4-isopropylbenzylideneamino）-（1H）-1,2,4-triazole-5-thione

1INTRODUCTION Recently,compounds containing pyrazole,imida-zole,triazole(including benzotriazole),pyridine,tetrazole and indole have attracted much interest because they exhibit some fungicidal activity,plant-growth regulating activity and antibacterial acti-vity[1～10].Schiff bases also constitute a good type of biologically active substructure[11～14],and the sulfur-containing Schiff bases are particularly effective.Studies of pyrazole Schiff base-type fungicides andtriazole compounds c…     

Synthesis and Crystal Structure of Dichlorodianiline Palladium （Ⅱ） （C6H5NH2）2PdCl2

1 INTRODUCTION Palladium compounds have attracted much attention as a consequence of their application in homogeneous and heterogeneous catalyses[1]. For instance, palladium compounds are the most active catalysts for the carbonylation, such as palladium-catalyzed carbonylation of nitroarenes, aryl halides, alkyne and so on[2～4]. Some dramatic results in the homogeneous catalysis of the reactions of organic compounds, particularly the successful commercial exploitation of the Wacker on…     

Crystal Structure of 10-(2'''',5''''-Dimethoxybenzylidene) Anthrone

1 INTRODUCTION The 10-benzylidene anthrones which are important intermediate for organic syntheses[1～3] usually possess thermochromism[4] and photo- chromism[5], and have been found recently to have evident anti-cancer activity[6]. We found that the substituents in the phenyl ring will affect the bioactivity of those compounds. For more deeply investigating the structure-activity relationships (SAR) and understanding interactions between the three dimensional structure of the compound …     

Synthesis and Crystal Structure of 1,7,7-Trimethyl- 4-（4-methoxyphenyl）-4,6,7,8-tetrahydroquinoline- 2,5（1H,3H）-diones under Microwave Irradiation

1 INTRODUCTION Various quinolone derivatives are known to dis- play interesting biological properties ranging from microbial activity to cytotoxicity[1]. They have been reported as antiviral (HIV-1)[2] and antitumor agents[3] as well as used as tubulin[4], topoisomerase[5] and thrombocyte inhibitors[6]. As a member of the quino- lone family, substituted N-phenyl-2-quinolones re-present the structural basis of many biologically active compounds, such as protein kinase inhibitors, immunodu…     

Synthesis and Crystal Structure of N-（1-Phenyl-3-methyl-4-benzal-pyrazolone-5）-furoic Hydrazide

1 INTRODUCTION In recent years, investigations on the com- pounds containing hydrazide or hydrazone moieties have been increased considerably because of their potentially biological activities, especially as poten- tial inhibitors for many enzymes[1～5]. The presence of weak molecular interactions such as hydrogen- bonding controls the conformational and structural features which are important to the drug action[6, 7]. We have synthesized the photochromic compounds of pyrazolone thiosemi…     

Synthesis and Structural Characterization of Pd[CH3O（O）C6H3CHNNC（S）NH2]（C5H5N）

1 INTRODUCTION Palladium (Ⅱ) coordination and organometallic compounds usually show square planar environments at the metal center[1], and have experienced an im- portant development in the past years due to their acting as intermediates in different types of catalytic reactions and numerous applications in organic synthesis[2]. Although palladium plays an increase- ingly recognized role as a biometal[3], little is known about the structure and function of palladium compounds in living …     

Synthesis and Crystal Structure of （4S）-5-（2-Methoxy-2-oxoethylamino）-5-oxo-4-（3,4,5-trimethoxybenzamido） Pentanoic Acid

1 INTRODUCTION Aminopeptidase N (APN), a member of mem- brane-bound zinc-dependent exopeptidase, is known to be high expression on the brush border membran- es of the small intestine and renal proximal tubules[1]. The over-expression of APN has been involved in several pathological conditions including cancer[2], leukemia, diabetic nephropathy[3], rheumatoid arth- ritis[4], angiogenesis[5] and central nervous system di- seases, such as Alzheimer’s disease[6]. This has led to the sear…     

Synthesis and Crystal Structure of N-cyclopropyl-9 -（3,4-dicholophenyl）- 1,2,3,4,5,6,7,8,9,10-decahydroacridine -1,8-dione under Microwave Irradiation

1 INTRODUCTION aryl or methyl group to the nitrogen atom of these compounds leads to enhanced activities of fluo- A lot of natural and synthetic compounds con- rescence[7, . Since the pyridine scaffold is included 8] taining acridine skeletons display interesting biolo- in decahydroacridine-1,8-dione, a question is whether gical and physical activities[1]. Acridinedione, for the same modification on the nitrogen atom of de- example, has been identified as antimalarial and cahydroacridine-1…     

螺[1-溴-4-(1R,2S,5R)-l-孟氧基-5-氧杂-6-氧代双环[3.1.0]己烷-2,2'-(3'-α-膦酸二乙酯基-(S)-苯甲氧基-4'-l-(1R,2S,5R)-孟氧基丁内酯)]的晶体结构

报道了标题化合物合成和晶体结构。X-射线结构分析表明,该化合物的分子式为C39H58BrO10P,Mr = 797.74,晶体属于单斜晶系,空间群为P21,晶胞参数a = 12.858(3), b = 25.130(5), c = 14.125(3) ? = 105.15(3), V = 4405(2) ?, Z = 4, Dc = 1.203 g/cm3, ?= 1.019 mm-1, F(000) = 1688,R = 0.0726, wR = 0.1201,共收集到9691个独立衍射点,其中可观测点5638个(I≥2s(I))。每个分子中有6个环,13个手性中心,2个五员环呈信封式构象,并分别与三员环组合成[2.4]螺环和[3.1.0]桥环化合物,4个新生成的手性中心的绝对构型为C(6)(S), C(7)(S), C(3)(R), C(2)(R),新引入的磷酸酯官能团C(9)为S构型。     

Synthesis and Crystal Structure of Spiro[1-bromo(S)-4-(R)-hydroxy- 5-oxa-6-oxo-bicyclo[3.1.0]hexane-2,2''-(3''-diethyl-(-(S)-4''-Cl-benzyloxyphosphonyl-4''-(1R,2S,5R)-menthyloxybutyrolactone)]

The title compound, spiro[1-bromo(S)-4-(R)-hydroxy-5-oxa-6-oxo-bicyclo[3.1.0]-hxane-2,2'-(3'-diethyl-α-(S)-4'-Cl-benzyloxyphosphonyl-4'-(1R,2S,5R)-menthyloxybutyrolactone)] has been synthesized via the tandem asymmetric reaction and it crystallizes in a monoclinic system, space group P21 with a = 11.067(3), b = 12.484(2), c = 12.356(2)(A), β = 101.95°,C29H39BrC1O10P, Mr = 693.93, V= 1670.2(6) (A)3, Z= 2, Dc= 1.380 g/cm3, λ(MoKα) = 0.071073nm, μ = 1.410 mm-1, F(000) = 720, the final R = 0.0570 and wR = 0.0758 for 6190 observed reflections with I ＞ 2σ(I). The structure is characterized by the special combination of biologic phosphonyl group and one cyclopropane as well as two butyrolactones. The intermolecular hydrogen bond between O(3)-H(3A)…O(10) in the crystal lattice has been observed.     

Dinuclear gold(I) dithiophosphonate complexes: synthesis,luminescent properties,and X-ray crystal structures of [AuS(2)PR(OR')](2) (R = Ph,R' = C(5)H(9); R = 4-C(6)H(4)OMe,R' = (1S,5R,2S)-(--)-menthyl; R = Fc,R' = (CH(2))(2)O(CH(2))(2)OMe)

2,4-Diaryl- and 2,4-diferrocenyl-1,3-dithiadiphosphetane disulfide dimers (RP(S)S)(2) (R = Ph (1a), 4-C(6)H(4)OMe (1b), FeC(10)H(9) (Fc) (1c)) react with a variety of alcohols, silanols, and trialkylsilyl alcohols to form new dithiophosphonic acids in a facile manner. Their corresponding salts react with chlorogold(I) complexes in THF to produce dinuclear gold(I) dithiophosphonate complexes of the type [AuS(2)PR(OR')](2) in satisfactory yield. The asymmetrical nature of the ligands allows for the gold complexes to form two isomers (cis and trans) as verified by solution (1)H and (31)P[(1)H] NMR studies. The X-ray crystal structures of [AuS(2)PR(OR')](2) (R = Ph, R' = C(5)H(9) (2); R = 4-C(6)H(4)OMe, R' = (1S,5R,2S)-(-)-menthyl (3); R = Fc, R' = (CH(2))(2)O(CH(2))(2)OMe (4)) have been determined. In all cases only the trans isomer is obtained, consistent with solid state (31)P NMR data obtained for the bulk powder of 3. Crystallographic data for 2 (213 K): orthorhombic, Ibam, a = 12.434(5) A, b = 19.029(9) A, c = 11.760(4) A, V = 2782(2) A(3), Z = 4. Data for 3 (293 K): monoclinic, P2(1), a = 7.288(2) A, b = 12.676(3) A, c = 21.826(4) A, beta = 92.04(3) degrees, V = 2015.0(7) A(3), Z = 2. Data for 4 (213 K): monoclinic, P2(1)/n, a = 11.8564(7) A, b = 22.483(1) A, c = 27.840(2) A, beta = 91.121(1) degrees, V = 7419.8(8) A(3), Z = 8. Moreover, 1a-c react with [Au(2)(dppm)Cl(2)] to form new heterobridged trithiophosphonate complexes of the type [Au(2)(dppm)(S(2)P(S)R)] (R = Fc (12)). The luminescence properties of several structurally characterized complexes have been investigated. Each of the title compounds luminesces at 77 K. The results indicate that the nature of Au...Au interactions in the solid state has a profound influence on the optical properties of these complexes.     

Coordination chemistry of silver(I) with the nitrogen-bridged ligands (C(6)H(5))(2)PN(H)P(C(6)H(5))(2) and (C(6)H(5))(2)PN(CH(3))P(C(6)H(5))(2): the effect of alkylating the nitrogen bridge on ligand bridging versus chelating behavior

The coordination chemistry of silver(I) with the nitrogen-bridged ligands (C(6)H(5))(2)PN(R)P(C(6)H(5))(2) [R = H (dppa); R = CH(3) (dppma)] has been investigated by (31)P NMR and electrospray mass spectrometry (ESMS). Species observed by (31)P NMR include Ag(2)(mu-dppa)(2+), Ag(2)(mu-dppa)(2)(2+), Ag(2)(mu-dppa)(3)(2+), Ag(2)(mu-dppma)(2+), Ag(2)(mu-dppma)(2)(2+), and Ag(eta(2)-dppma)(2)(+). Species observed by ESMS at low cone voltages were Ag(2)(dppa)(2)(2+), Ag(2)(dppa)(3)(2+), Ag(2)(dppma)(2)(2+), and Ag(dppma)(2)(+). (C(6)H(5))(2)PN(CH(3))P(C(6)H(5))(2) showed a strong tendency to chelate, while (C(6)H(5))(2)PN(H)P(C(6)H(5))(2) preferred to bridge. Differences in the bridging versus chelating behavior of the ligands are assigned to the Thorpe-Ingold effect, where the methyl group on nitrogen sterically interacts with the phenyl groups on phosphorus. The crystal structure of the three-coordinate dinuclear silver(I) complex (Ag(2)[(C(6)H(5))(2)PN(H)P(C(6)H(5))(2)](3))(BF(4))(2) has been determined. Bond distances include Ag-Ag = 2.812(1) A, Ag(1)-P(av) = 2.492(3) A, and Ag(2)-P(av) = 2.509(3) A. The compound crystallizes in the monoclinic space group Cc at 294 K, with a = 18.102(4)(o), Z = 4, V = 7261(3) A(3), R = 0.0503, and R(W) = 0.0670.     

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 (E)2-(3'-Bromo-5'-chloro-salicylidene amino)-4-methyl Pyridine

A new Schiff base compound,2-bromo-4-chloro-6-[(4-methylpyridin-2-ylimino)me-thyl]phenol(C13H10BrClN2O),has been synthesized by the condensation of equimolar 3-bromo-5-chlorosalicylaldehyde and 4-methylpyridin-2-ylamine in a methanol solution.The compound Was characterized by elemental analysis,IR spectra,and single-crystal X-ray diffraction.The crystal belongs to the monoclinic system,space group P21 with a=6.048(3),b=14.063(7),c=7.623(4)(A),β=97.703(7)°,Z=2,V=642.5(6)(A)3,Dc=1.683 g/cm3,Mr=325.59,λ(MoKa)=0.71073(A),μ=3.395 mm-1,F(000)=324,R=0.0370 and wR=0.0662.A total of 3879 reflections were collected,of which 1970 with,I＞2σ(I)were observed.As expected.the molecule adopts a trans configuration about the C=N double bond.The benzene and pyridine rings are nearly coplanar(mean deviation from the combined plane is 0.031(3)(A)),with their dihedral angle of 3.3(3)°.The preliminary biological tests show that the compound has excellent antibacterial activities.     

Synthesis, Crystal Structure and Antitumor Activity of （E）-4-tert-Butyl-N-（2,4-dichlorobenzylidene）-5-（1,2,4-triazol-1-yl）-thiazol-2-amine

The title compound (E)-4-tert-butyl-N-(2,4-dichlorobenzylidene)-5-(1,2,4-triazol-1-yl)-thiazol-2-amine was synthesized by the reaction of 4-tert-butyl-5-(1,2,4-triazol-1-yl)-thiazol-2-amine with 2,4-dichlorobenzaldehyde, and its crystal structure was determined by singlecrystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 7.9748(4), b = 10.1803(5), c = 11.4603(6), α = 102.882(1), β = 100.253(1), γ = 104.457(1)°, V = 850.95(7)3, Z = 2, F(000) = 392, C16H15Cl2N5S, Mr = 380.29, Dc = 1.484 g/cm3, S = 1.095, μ = 0.512 mm-1, the final R = 0.0301 and wR = 0.0965 for 3334 observed reflections (I 2σ(I)). The preliminary antitumor activity shows that for the title compound the IC50 of Hela is 0.175 μmol/mL and that of Bel7402 is 0.156 μmol/mL.     

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…     

Hydrothermal Synthesis and Structure of [Mn(C8H5NO4)·H2O]n·2nH2O

A novel 5-aminoisophthalate compound, [Mn(C8H5NO4)(H2O]n(2nH2O 1, has been synthesized by the hydrothermal assembly of 5-aminoisophthalic acid with manganese acetate. Ele- mental analysis, X-ray crystal structure analyses, IR spectra, FT-Raman and ESR were carried out for the structural determination and characterization of the title compound. Compound 1 crystallizes in triclinic, space group Pī with a = 7.7562(2), b = 8.6121(3), c = 8.7107(2)(A), α = 85.411(2), β = 76.030(2), γ = 66.510(2)o, V = 517.76(3)(A)3, MnC8H11NO7, Mr = 288.12, Z = 2, Dc = 1.848 g/cm3, μ = 1.300 mm-1, F(000) = 294, R = 0.0381 and wR = 0.1043 for 1652 observed reflections (I > 2σ(I)).     

Novel metal-organic frameworks with specific topology from new tripodal ligands: 1,3,5-tris(1-imidazolyl)benzene and 1,3-bis(1-imidazolyl)-5-(imidazol-1-ylmethyl)benzene

Reactions of two new tripodal ligands 1,3,5-tris(1-imidazolyl)benzene (4) and 1,3-bis(1-imidazolyl)-5-(imidazol-1-ylmethyl)benzene (5) with metal [Ag(I), Cu(II), Zn(II), Ni(II)] salts lead to the formation of novel two-dimensional (2D) metal-organic frameworks [Ag(2)(4)(2)][p-C(6)H(4)(COO)(2)].H(2)O (6), [Ag(4)]ClO(4) (7), [Cu(4)(2)(H(2)O)(2)](CH(3)COO)(2).2H(2)O (8), [Zn(4)(2)(H(2)O)(2)](NO(3))(2) (9), [Ni(4)(2)(N(3))(2)].2H(2)O (10), and [Ag(5)]ClO(4) (11). All the structures were established by single-crystal X-ray diffraction analysis. Crystal data for 6: monoclinic, C2/c, a = 23.766(3) A, b = 12.0475(10) A, c = 13.5160(13) A, beta = 117.827(3) degrees, Z = 4. For compound 7: orthorhombic, P2(1)2(1)2(1), a = 7.2495(4) A, b = 12.0763(7) A, c = 19.2196(13) A, Z = 4. For compound 8: monoclinic, P2(1)/n, a = 8.2969(5) A, b = 12.2834(5) A, c = 17.4667(12) A, beta = 96.5740(10) degrees, Z = 2. For compound 9: monoclinic, P2(1)/n, a =10.5699(3) A, b = 11.5037(3) A, c = 13.5194(4) A, beta = 110.2779(10) degrees, Z = 2. For compound 10: monoclinic, P2(1)/n, a = 9.8033(3) A, b = 12.1369(5) A, c = 13.5215(5) A, beta = 107.3280(10) degrees, Z = 2. For compound 11: monoclinic C2/c, a = 18.947(2) A, b = 9.7593(10) A, c = 19.761(2) A, beta = 97.967(2) degrees, Z = 8. Both complexes 6 and 7 are noninterpenetrating frameworks based on the (6, 3) nets, and 8, 9 and 10 are based on the (4, 4) nets while complex 11 has a twofold parallel interpenetrated network with 4.8(2) topology. It is interesting that, in complexes 6,7, and 11 with three-coordinated planar silver(I) atoms, each ligand 4 or 5 connects three metal atoms, while in the case of complexes 8, 9, and 10 with six-coordinated octahedral metal atoms, each ligand 4 only links two metal atoms, and another imidazole nitrogen atom of 4 did not participate in the coordination with the metal atoms in these complexes. The results show that the nature of organic ligand and geometric needs of metal atoms have great influence on the structure of metal-organic frameworks.