Chiral Ligands Derived from Carbohydrates. 21.Crystal Structure of Methyl-4,6-O-benzylidene-3-deoxy-3-(salicylideneamino)-α-D-altropyranoside

A new chiral Schiff base derived from carbohydrate, methyl-4,6-O-benzylidene-3- deoxy-3-(salicylideneamino)-α-D-altropyranoside, has been synthesized by reacting methyl 3-ami- no-4,6-O-benzylidene-3-deoxy-α-D-altropyranoside with salicylaldehyde in methanol and charac- terized by IR, 1H NMR, 13C NMR, MS, elemental analysis, and X-ray crystal structure analysis.The crystal belongs to orthorhombic, space group P212121 with a = 8.0856(16), b = 10.786(2), c = 22.690(5) -, V = 1978.8(7) -3, Z = 4, Mr = 385.40, Dc = 1.294 g/cm3, μ = 0.095 mm-1, F(000) = 816, the final R = 0.0379 and wR = 0.0811 for 2597 independent reflections.In the title compound, the pyrano-ring adopts a twisted 1C4 chair conformation.     

Chiral Phosphine Ligands Derived from Sugars 4.Crystal Structure of Methyl 4,6-O-Benzylidene-3-Deoxy-3-(Diphenylphosphino)-α-D-Altropyranoside (3-MBPA)

IINTRODUCTIONChiralphosphinesareveryusefulligandsinenantioselectivecatalysiswithtransitionmetalcomplexes"'.Becausesugarisrichnotonlyinstereochemistrybutalsoinnatureandpossessesmanyhydroxylgroupsassyntheticstartingpoints,theyhavereceivedmuchattentionsincethe1970st2i.However,thetypesofchiralphosphinesinwhichthephosphorusatomsareattacheddirectlytothesecondarycarbonsofsugararefew.Thedifficultiesinthesyntheticprocessesarepartofthereason.Bythenucleophilicreplacementreaction,itisdifficulttolink…     

Chiral Phosphine Ligands Derived fro m Sugars .14 . Crystal Structure of Diphenyl( m ethyl4’,6’-O-benzylidene-3’-deoxy-α- D-altropyranoside-3-)phosphine Oxide

１　ＩＮＴＲＯＤＵＣＴＩＯＮＣｈｉｒａｌｐｈｏｓｐｈｉｎｅｓａｒｅｕｓｅｆｕｌｌｉｇａｎｄｓｉｎｅｎａｎｔｉｏｓｅｌｅｃｔｉｖｅｃａｔａｌｙｓｉｓｗｉｔｈｔｒａｎｓｉｔｉｏｎｍｅｔａｌｃｏｍｐｌｅｘｅｓ〔１〕，ｓｏｍｅｏｆｔｈｅｍｄｅｒｉｖｅｄｆｒｏｍｓｕｇａｒｓａｒｅａｌｓｏｏｆｐｏｔｅｎｔｉａｌａｐｐｌｉｃａｔｉｏｎｓｉｎｂｉｐｈａｓｉｃｃａｔａｌｙｓｉｓ〔２〕ａｎｄｍｅｄｉｃｉｎｅ〔３〕．Ｂｙｔｈｅｎｕｃｌｅｏｐｈｉｌｉｃｒｅｐｌａｃｅｍｅｎｔｒｅａｃｔｉｏｎ，ｉｔｉｓｄｉｆｆｉｃｕｌ…     

Chiral Phosphine Ligands Derived from Sugars. 14. Crystal Structure of Diphenyl(methyl 4',6'-O-benzylidene-3'-deoxy-α-D-altropyranoside-3-)phosphine Oxide

The crystal structure of the title compound, C26H27O6P, has been determined by single-crystal X-ray diffraction analysis. The crystal is orthorhombic with space group P212121, a=6.154(4), b=17.199(8), c=22.180(3)(A), V=2347.6(A)3, Dc=1.32 g/cm3, F(000)=984, μ=1.5cm-1, Z=4, and final R=0.075 and Rw=0.080 for 1417 reflections (I≥3σ(I)). The X-ray diffraction analysis revealed that the structure of the title compound s similar to that of its parent phosphine and the pyranose and 4, 6-O-benzylidene rings remain distorted chair conformations.     

Synthesis and Crystal Structure of Gd3（BSiO6）（SiO4）

1INTRODUCTIONRareearthborosilicateshaverarelybeenreportedinthepastdecade.LnBMO5(M=Ge,Si)(l,z,31exhibitsthestillwellitestructureonlyforlargerlanthanide,initsstructure,twoBO'tetrahedraandoneSiO'tetrahedronareconnectedbycorner-sharedeachothertoformsix-memberringthatconstructinfinitehelicalchainsparal-lelto3lscrewaxis-Serhanetal(43synthesizedNd,BM2O,,(M=Si Ge)whosestructurecontainstri-coordinatedboronatoms.Recently,wehavesynthesizedSm3BSi2O1,andEu,BSi,O,,t"6),herewerffportthesynthes…     

Solvothermal Synthesis and Crystal Structure of Zn（en）3 B5O7（OH）3

Introduction Boratecompounds,inwhichboronisboundonly tooxygen,areofconsiderablemineralogicalandindus trialimportance.Thesecompoundscontaininganionic componentscomposedofBO3andBO4groups,which maybelinkedtogetherbysharingoxygenatoms,can formisolatedringsand…     

Synthesis,Crystal Structure and Blue Photoluminescence of a Metal-organic Framework Constructed from Triangular [Zn3（μ3-OH）] Clusters with Bis（tetrazole）amine Ligands

A new metal-organic framework, {Zn[Zn3（BTA）3（μ3-OH）（H2O）3]2}n 1, has been synthesized under hydrothermal reaction of ZnCl2 and bis（5-tetrazolyl）amine （H2BTA）, and characterized by elemental analysis, FT-IR, Raman spectrum, X-ray single-crystal diffraction, TGA and photoluminescence measurements. Compound 1 crystallizes in the trigonal system, space group P-3cl, a = 13.667（3）, c = 12.981（3） A, V = 2099.6（8） A3 and Z = 2. The BTA2- ligand in 1 assumes theμ3 tetradentate mode with both 1,2- and 1,4-tetrazole bridges, generating an unusual 2-D layer, in which the [Zn3（μ3-OH）] triangular motifs act as three-connecting nodes and the mononuclear Zn atoms as six-connecting nodes that are inter-linked by organic ligands. Adjacent 2-D metal-organic layers are linked by strong hydrogen bonds to form a novel 3-D supramolecular framework. Complex 1 exhibits blue fluorescence emission in the solid state at ambient temperature.     

Synthesis,Crystal Structure and Cytotoxic Activity of a Zinc（Ⅱ） Complex of the Schiff Base Derived from S-benzyldithiocarbazate

A novel zinc(Ⅱ) complex of empirical formula,ZnL2(L=anionic forms of S-benzyl-β-N-(2,4-dichlorobenzylidene) hydrazine carbodithioate),has been synthesized and characterized by elemental analysis,IR spectra and single-crystal X-ray diffraction.The crystal belongs to the triclinic system,space group P with a = 9.3168(9),b = 13.0353(13),c = 14.7702(15) ,α = 71.2860(10),= 87.5140(10),γ = 79.4480(10)o,V = 1670.0(3) 3,Z = 2,Mr = 773.93,Dc = 1.539 g/cm3,μ = 1.334 mm-1,F(000) = 784,the final R = 0.0403 and wR = 0.0800 for 4060 observed reflections with I>2(I).In the crystal structure,the zinc(Ⅱ) complex has a distorted tetrahedral geometry in which the zinc ion is coordinated by the nitrogen and sulfur atoms from two Schiff base ligands,respectively.The preliminary bioassay indicates that the Schiff base and its zinc complex exhibit inhibitory activity against the human gastric cancer cell lines(MKN45) and hepatoma cell lines(HepG2).     

Synthesis and Crystal Structure of 4-（4,6-Dimethoxylpyrimidin-2-yl）- 3-thiourea Carboxylic Acid Ethyl Ester

4-（4,6-Dimethoxyl-pyrimidin-2-yl）-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at room temperature. The crystal structure was determined by X-ray diffraction analysis. Crystallographic data： C10H14N4O4S, M, = 286.31, monoclinic, space group C2/c with a = 2.5309（3）, b = 0.67682（6）, c = 1.74237（19） nm, β = 114.744（3）°, V= 2.7106（5） nm3, Dc = 1.403 g/cm3, p = 0.225 mm-1, F（000） = 1200, Z= 8, R= 0.0514 and wR= 0.1529.     

Synthesis and Crystal Structure of 3-{[（1E） 1-（2- Hydroxyphenyl） methylidene]amino}-4-cyanopyrazole

The title Schiff base compound （C11H8N4O）, a derivative of pyrazole, has been synthesized by the reaction of salicylaldehyde and 3-amino-4-cyanopyrazole in absolute ethanol and characterized by elemental analyses, IR, ^1H NMR and X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/n, with a = 7.5594（7）, b = 18.3342（19）, c = 22.461（2） A^°, β = 98.419（2）°, V = 3079.5（5） A^°3, Mr = 212.21, Z = 12, F（000） = 1320, Dc = 1.373 g/cm^3, T = 298（2） K, 2 = 0.71073 A^°, the final R = 0.0571 and wR = 0.0493. A total of 5412 unique reflections were collected, of which 1612 with I 〉 2σ（I） were observed. The molecular structure adopts a trans configuration about the C=N double bond. The preliminary biological tests show that the compound has high antibacterial activities.     

Synthesis and Crystal Structure of 4-Bromo-5-ethoxy-3-methyl-5- （naphthalen- 1-yl）- 1-tosyl- 1H-pyrrol-2（5H）- one

The title compound 4-bromo-5-ethoxy-3-methyl-5-(naphthalen-1-yl)-1-tosyl-1H- pyrrol-2(5H)-one 1 (C24H22BrNO4S, Mr = 500.40) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/n with a = 8.8562(15), b = 18.118(3), c = 14.055(2) , β = 99.855(3)o, V = 2221.9(6) 3, Z = 4, Dc = 1.496 g/cm3, μ = 1.975 mm-1, λ = 0.71073 , F(000) = 1024, R = 0.0607 and wR = 0.1371.     

Synthesis,Crystal Structure and Antifungal Activities of 3-Methyl-l-（4-methylphenyl）-4- （N-4-trifluoromethylphenyl）-aminomethyl- 5-（4-methoxyphenylthio）-lH-pyrazole

The title compound 3-methyl-l-（4-methylphenyl）-4-（N-4-trifluoromethylphenyl） aminomethyl-5-（4-methoxyphenylthio）-lH-pyrazole has been synthesized via a four-step reaction and characterized by IR, 1H NMR, elemental analysis and X-ray crystallography. The compound crystallizes in monoclinic, space group P21/c with a = 8.7170（15）, b = 18.355（3）, c = 15.292（3） A, fl = 103.445（3）°, V= 2379.7（7） A3, Dc = 1.350 g/cm3, Z = 4, p = 0.184, F（000） = 1008, and the final R = 0.0491 and wR = 0.1339 for 4160 observed reflections （I 〉 2a（/））. The results demonstrate that there is a face-to-face π-π stacking interaction between one benzene ring （C（19）-C（24）） and another （C（I 3）-C（! 8）） at a plane-plane distance of 3.3539 A. The ring normal and vector between the ring centroids form an angle of 18.2° up to the centroid-to-centroid distance of 3.5273 A. The crystal structure is stabilized by the intermolecular hydrogen bond of N（3）-H（3A）...N（2） （symmetry code： A -x＋l, -y＋l, -z）. The preliminary biological test shows that the title compound has a moderate antifungal activity.     

Synthesis and Crystal Structure of 3-（Trichloroacetyl） Indole

1 INTRODUCTION Indole and its derivatives have attracted much at-tention due to their chemical properties as well asbiological activities[1, . They have been widely used 2]as the materials for producing pigment, perfume,plant growth regulators, etc. Recently, it has alsobeen found that some indole derivatives present anti-tumor and antiviral activities[3～5]. During our sear-ches for bioactive compounds, a series of indole deri-vatives were synthesized, among …     

Synthesis and Crystal Structure of Dichlorobis[N-（4-hydroxylsalicylidene）-3-dimethylaminopropylamine]Ni（II）

1 INTRODUCTION The chemistry of nickel complex with multi- dentate Schiff base ligands has attracted particular attention because this metal can exhibit several oxi- dation states[1]. Such complexes with different oxi- dation states play an important role in bioinorganic chemistry and redox enzyme systems[2], and many of them can provide the basis of models for active sites of biological systems or act as catalysts[3]. Nickel complexes with tetradentate N2O2 and tri- dentate N2O Schi…     

Synthesis and Crystal Structure of 4-（N,N-Diphenylamino）styrene-4＇-N-methylpyridinium Iodine

The title compound 4-（N,N-diphenylamino）styrene-4＇-N-methylpyridinium iodine （abbreviated to PASMPI） was synthesized by a facile condensation reaction with a high yield. The red crystal including a mol...     

Crystal Structure of Co（S2CPh）3

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＣｏ（Ｓ_２ＣＰｈ）_３ＬｕＳｈａｏ－Ｆａｎｇ；ＣｈｅｎＨｏｎｇ－Ｂｉｎ；ＨｕａｎｇＸｉａｏ－Ｙｉｎｇ（ＦｕｊｉａｎＩｎｓｔｉｔｕｔｅｏｆＲｅｓｅａｒｃｈｏｎｔｈｅＳｔｒｕｃｔｕｒｅｏｆＭａｔｔｅｒ，Ａｃａｄｅｍｉａ...     

Synthesis and Crystal Structure of 1,4,7,10-Tetrakis （2-（（4-hydroxy）phenoxy）ethyl）-1,4,7,10- tetraazacyclododecane

A novel molecule tetra-N-alkylation of cyclen （1,4,7,10-tetraazacyclododecane）, 1,4,7,10-tetrakis（2-（（4-hydroxy）phenoxy）ethyl）-1,4,7,10-tetraazacyclododecane 2, was synthesized and structurally characterized by single-crystal X-ray diffraction. The molecule turned into chiral helical compound crystals grown from EtOH by slow diffusion at room temperature and three of the four hydroquinone groups of the benzene ring formed a g-electron-rich cavity by C-H…π stacking interaction. The crystal belongs to the monoclinic system, space group P21/C with a = 13.9192（9）, b = 13.2871（6）, c = 22.1894（15）A^°, β = 91.4600（10）°, V = 4102.5（4）A^°3, Z = 4, Dc = 1.219 g/cm^3, C40H52N4O8, Mr = 752.89, F（000） = 1616,μ = 0.088 mm^-1, MoKa radiation （λ = 0.71073）, R = 0.0578 and wR = 0.1389 for 5588 observed reflections with I 〉 2σ（I）. Moreover, compound 2 was characterized with ^1H NMR, ^13C NMR, IR spectra and MS.     

Synthesis,Crystal Structure and Fungicidal Activity of （E）-2-[（4-tert-Butyl-5-（4-methoxybenzyl）thlazol-2 yhmino）methyl]phenol

The title compound （E）-2-[（4-tert-butyl-5-（4-methoxybenzyl）thiazol-2-ylimino）methyl]phenol was synthesized by the reaction of 5-（4-methoxybenzyl）-4-tert- butylthiazol-2-amine with salicylaldehyde, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 5.9362（8）, b = 11.5070（15）, c = 29.460（4）A, β= 97.326（3）°, V = 1995.9（5） A^3, Z = 4, F（000） = 808, C22H24N2O2S, Mr= 380.49, De= 1.266 g/cm^3, S = 1.031,μ = 0.181 mm^-1, the final R = 0.0474 and wR = 0.1441 for 4327 observed reflections （I 〉 2σ（I））. Intramolecular O-H…N hydrogen bond is observed in the crystal. The preliminary bioassay showed that the title compound exhibits 95% inhibition rate against Rhizoctonia solani at the test concentration of 500 mg/L.     

Synthesis and Crystal Structure of Methyl 3-（5- Bromo-1-ethyl-1H-indole-3-carbonyl）aminopropionate

Methyl 3-(5-bromo-1-ethyl-1H-indole-3-carbonyl)aminopropionate has been syn-thesized by the acylation of 5-bromo-3-trichloroacetylindole with β-alanine methyl ester,followed by alkylation with ethyl iodide,in 82.6% yield.Its crystal structure was gotten and determined by X-ray diffraction method.The crystal is of monoclinic,space group P2 1 /c with a=11.7927(8),b=14.9342(8),c=9.0060(5),β=101.558(6)°,V=1553.93(16)3,Z=4,D c=1.510 g/cm 3,λ=0.71073,μ(MoKα)=2.656 mm-1,M r=353.22 and F(000)=720.The structure was refined to R=0.0401 and wR=0.0825 for 1704 observed reflections with I > 2σ(I).In the crystal structure,intermolecular N(2)-H(2)···O(1) hydrogen bond and weak intermolecular bonds (C(1)-H(1) O(1) and C(10)-H(10B) O(2)) are formed,and π-π stacking also exists.