Syntheses and Crystal Structures of Two New Compounds： [Zn（2,2＇-bipy）（L）Cl]2 and [Zn（phen）（L2）]2 （HL = 3-Methylbenzoic Acid）

Compounds [Zn（2,2＇-bipy）（L）Cl]2 1 and [Zn（phen）（L2）]2 2 （2,2＇-bipy = 2,2＇-bipyridine, HL = 3-methylbenzoic acid, phen = 1,10-phenanthroline） have been synthesized under hydrothermal conditions. 1： monoclinic, space group C2/c, a = 20.240（4）, b = 9.2960（19）, c = 17.904（4）A, β = 92.63（3）°, V = 3365.1（12） A^3, C36H30Cl2N4O4Zn2, Mr = 784.32, Z = 4, Dc = 1.548 g/cm^3, μ = 1.631 mm^-1, F（000） = 1600, the final R = 0.0367 and wR = 0.1289 for 3867 observed reflections （I 〉 2σ（I））. 2： monoclinic, space group C2/c, a = 23.035（5）, b = 9.0395（18）, c = 23.799（5） A, β = 98.55（3）°, V = 4900.6（17）A^3, C56H44N4O8Zn2, Mr = 1031.73, Z = 4, Dc = 1.398 g/cm^3, μ = 1.039 mm^-1, F（000） = 2128, the final R = 0.0540 and wR = 0.1287 for 5002 observed reflections （I 〉 2σ（I））. The two compounds have the same space group and similar isolated dinuclear structure, but different space packing structures are formed by different weak intermolecular interactions. Mo- reover, IR and luminescence spectra are also employed to study the crystal structures and pro- perties of these two compounds.     

Syntheses and Characterizations of （CH3CH2CH2CH2NH3）6（BiI6）（I）2I3 and （NH3CH2CH2NH3）2Bi2I10

The title compounds have been respectively synthesized by solution process and solvothermal reaction, and their crystal structures were determined by X-ray diffraction method. For （CH3CH2CH2CH2NH3）6（BiI6）（I）2I3 1, it crystallizes in tficlinic, space group P1^- with Mr = 2049.76, a = 8.5719（1）, b = 11.7461（3）, c = 15.700（1）A, V = 1451.4（1）A^3, Z = 1, Dc = 2.345 g/cm^3, F（000） = 924, μ（MoKα） = 8.907 mm^-1, T = 293（2） K, the final R = 0.0655 and wR = 0.0804 for 2399 observed reflections with I 〉 2σ（I）. For （NH3CH2CH2NH3）2Bi2I10 2, it crystallizes in monoclinic, space group P21/n with Mr= 1811.20, a = 8.434（4）, b = 13.862（6）, c = 13.362（6）A, V = 1499.9（12）A^3, Z = 2, Dc = 4.010 g/cm^3, F（000） = 1536,μ（MoKα） = 22.007 mm^-1, T = 293（2） K, the final R = 0.0584 and wR = 0.1451 for 1798 observed reflections with I 〉 2σ（I）. The structures of 1 and 2 contain halobismuthate monomer and dimers, respectively. It is noteworthy that the dimers and their organic counters in 2 connect each other by N…I hydrogen bonds to form a layered structure, and the electrostatic interactions and crystal packing forces between layers give rise to the packing of the crystal. The optical absorption spectra of 1 and 2 reveal the appearance of sharp optical gaps of 2.13 and 2.01 eV, respectively.     

Synthesis,Crystal Structure and Biological Activity of 1-（β-D-Glucopyranosyl）-3- amino-5-methyl-1H-1,2,4-triazole

The title compound 1-（β-D-glucopyranosyl）-3-amino-5-methyl- 1H- 1,2,4-triazole was synthesized and characterized by IR, 1H-NMR and elemental analysis. Its single crystals of 2H2O adduct suitable for X-ray analysis were obtained by the slow evaporation of a H2O solution and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group P212121 with a = 7.7490（15）, b = 10.424（2）, c = 17.447（4） A^°, V = 1409.3（5） A^°^3, Z= 4, C9H20N4O7, Mr = 296.29, Dc = 1.396 g/cm^3,μ = 0.120 mm^-1, S = 1.007, F（000） = 632, R = 0.0686 and wR = 0.1560 for 1217 observed reflections with I 〉 20（I）. The title molecules are linked through intermolecular hydrogen bonds to form two 1-D chain structures, and such adjacent chains are further linked by intermolecular hydrogen bonds and H2O bridges to form a 3-D supramolecular network structure. The preliminary bioassay results showed that the title compound exhibits fungicidal activities against Gibberella zeae and Colletotrichum orbiculare.     

Conformation Diversity of Complexes Constructed by N-（2-Pyridylmethyl）-phenylalanine and Zn（Ⅱ）

Four configurationally and conformationally related Zn（II） complexes with a tridentate ligand namely, N-（2-pyridylmethyl）-phenylalanine （Hpmpa）, have been synthesized by hydrothermal reactions. [Zn（L-α-pmpa）2·HaO] 1： orthorhombic, space group P21212 with a = 15.1091（7）, b = 16.2417（8）, c = 5.9972（3） A, V= 1471.70（12）A^3, Z = 2, Mr = 593.97, Dc = 1.340 g/cm^3,μ = 0.879 mm^-1, F（000） = 620, Rint= 0.0205, R = 0.0450 and wR = 0.1578 for 3102 observed reflections with I 〉 2σ（I）; [Zn（D-α-pmpa）2·2H2O] 2： orthorhombic, space group P21212 with a = 15.1023（6）, b = 16.2516（7）, c = 6.0024（2）A, V= 1473.21（10）A^3, Z = 2, Mr = 611.98, Dc = 1.380 g/cm^3,μ = 0.882 mm^-1, F（000） = 640, Rint= 0.0337, R = 0.0484 and wR = 0.1435 for 2408 observed reflections with I 〉 2σ（I）; [Zn（L-β-pmpa）2] 3： monoclinic, space group C2/c with a = 27.8667（5）, b = 5.60350（10）, c = 19.9636（2）A β = 120：2210（10）°, V = 2693.66（7）A^3, Z = 4, Mr = 575.95, De= 1.420 g/cm^3,μ = 0.955 mm^-1, F（000） = 1200, Rint= 0.0345, R = 0.0358 and wR = 0.1135 for 2251 observed reflections with I 〉 2σ（I）; and [Zn（D-β-pmpa）2] 4. They are all mononuclear discrete structures. The influence of temperature and pH on the conformation of structures has been investigated. Moreover, the photoluminescent properties of compounds 1 and 3 are also reported.     

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 N-[1-（2-Methyl-1-methylcarbamoyl- propylcarbamoyl）-2,3-diphenyl- cyclopropyl]-benzamide

N-[1-（2-Methyl-1-methylcarbamoyl-propylcarbamoyl）-2,3-diphenyl-cyclopropyl]-ben- zamide, C29H31N3O3, has been synthesized and characterized by IR, ^1H NMR, ^13C NMR and singlecrystal X-ray diffraction. The crystal is of orthorhombic, space group P212121 with a = 11.0855（11）, b = 18.7756（19）, c = 24.434（2）A, V = 5085.5（9）A^3, Z = 8, Mr = 469.57, Dc = 1.227 g/cm^3, λ = 0.71070 A,μ（MoKα） = 0.080 mm^-1, F（000） = 2000, the final R = 0.0579 and wR = 0.1111 for 4569 observed reflections with I 〉 2σ（I）. The N-H and oxygen atom are involved in intermolecular hydrogen bonds which link the molecules into a one-dimensional chain.     

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-amino-4,6-O-benzylidene-3-deoxy-α-D-altropyranoside with salicylaldehyde in methanol and characterized 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）A, V = 1978.8（7）A^3, Z = 4, Mr = 385.40, Dc = 1.294 g/cm^3, p = 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.     

Synthesis,Crystal Structure and Characterization of a Cobalt Coordination Polymer： [Co（1,4-ndc）（L） （H2O）]n

The title coordination polymer, [Co（1,4-ndc）（L）（H2O）]n 1 （1,4-H2ndc = 1,4-na- phthalenedicarboxylic acid and L =1-（5-（1H-imidazol- 1-yl）pentyl）- 1H-imidazole） has been hydrothermally synthesized and characterized by IR and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/n with a = 12.4333（12）, b = 13.2963（13）, c = 13.4678（13）A, α =β = 90°, y =107.302（2）°, V= 2125.7（4）A^3, Z = 4, CoC22H22N4O5, Mr = 481.37, De = 1.504 g/cm^3, F（000） = 996, μ（MoKa） = 0.850 mm^-1, R = 0.0472 and wR = 0.0984. Compound 1 exhibits a two-dimensional layer structure. The O-H...O and C-H...O hydrogen bonds stabilize the structure of 1.     

Synthesis and Molecular Structure of 4-Chloromethyl-3-anilino-2-（4- methylbenzoylimido）thiazole

The title compound 2, 4-chloromethyl-3-anilino-2-（4-methyl-benzoylimido）thiazole, was prepared by the reaction of 1-p-methylbenzoyl-3-phenylaminothiourea 1 with 1,3-dichloro- acetone. The crystal is of monoclinic, space group P21/c, with a = 8.1712（15）, b = 10.998（2）, c = 19.134（4）A, β= 94.610（5）°, C18H16ClN3OS, Mr = 357.85, Z = 4, V = 1714.0（6）A^3, De= 1.387 g/cm^3, μ（MoKa） = 0.354 mm^-1, F（000） = 744, the final R = 0.0518 and wR = 0.1167 for 3189 observed reflections （I〉 2σ（I）. Its formation mechanism was proposed.     

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 Structures of (Z)-1-Phenyl-1-phenylseleno-2-(p-tolylsulfonyl)ethene and (Z)-1,3-Diphenyl-3-phenyl-seleno-2-(p-tolylsulfonyl)-2-propen- 1-ol

1 INTRODUCTION The vinyl sulfones are versatile intermediates in organic chemistry and have been extensively stu- died[1]. The available methodology for vinyl sulfone synthesis mainly consists of Horner-Emmons reac- tions of carbonyl compounds with sulf…     

Resolution and Crystal Structure of 9α-(3-Azabicyclo[3,3,1]nonanyl)- 2''-cyclopentyl-2''-hydroxyl-2''-thienylacetate

The crystal structure of 9α-(3-azabicyclo[3,3,1]nonanyl)-2'-cyclopentyl-2'-hydro-xyl-2'-thienylacetate (C16H27NO3S, Mr = 349.48) has been determined by single-crystal X-ray diffraction analysis. The crystal belongs to orthorhombic, space group P212121 with a = 14.937(3), b = 8.1673(16), c = 15.423(3) (A), V = 1881.5(6) (A)3, Z = 4, Dc =1.234 g/cm3, μ = 0.188 mm-1, F(000) = 752, the final R = 0.0468 and wR = 0.1251. The bicyclo[3,3,1]nonane ring system adopts the most favored twin-chair conformation. The crystal structure shows the existence of intramolecular O-H…O hydrogen bonds by which a one-dimensional chain struc- ture is formed.     

Resolution and Crystal Structure of 9α-(3-Azabicyclo[3,3,1]nonanyl)- 2′-cyclopentyl-2′-hydroxyl-2′-thienylacetate

1 INTRODUCTION The design, development and marketing of new chiral drugs are now a major theme in the drug chirality research and industry[1]. In 1996, the FDA announced it would consider further incentives for developing single isomer drugs because of their bet- ter pharmacokinetics prosperity, safety, and tolera- bility. Our recent drug candidate, 9α-(3-azabicyclo- [3,3,1]nonanyl)-2?-cyclopentyl-2?-hydroxyl-2?-thien- ylacetate I, is a potential selective M1 antagonist. It is composed…     

Syntheses and Crystal Structures of Two 3D Zinc(II) Compounds Involving Coordination and Hydrogen Bonds

1 INTRODUCTION Self-assembly through coordination and hydrogen bonds has been proved to be a powerful tool for con- structing functional organic crystalline materials[1~4]. Except for the important role of H-bonds in the sta- bilization of structures, hydrogen bonding groups namely hydroxyl, amide groups in adjacent coor- dination polymeric chains or discrete lamellas can form hydrogen bonds, which allow for the assembly of well-formed crystalline solid[5, 6]. Our recent inte- rest is foc…     

Synthesis and Crystal Structure of 4-[（1E）-（4-Hydroxy-3,5-dimethoxybenzylidene）-amino]-1,5-dimethyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one

The title compound (C20H21N3O4, Mr = 367.40) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group P212121 with a = 7.5143(15), b = 13.901(3), c = 18.545(4) , V = 1937.1(7) 3, Z = 4, Dc = 1.260 g/cm3, μ = 0.089 mm-1, F(000) = 776, the final R = 0.0616 and wR = 0.0912. X-ray diffraction reveals that the molecule adopts an E configuration about the central C=N double bond. The intermolecular O–H…O hydrogen bond stabilizes the crystal structure by causing the formation of a supramolecular architecture.     

Synthesis and Crystal Structure of （S）-Ethyl-2-（2-methoxy-phenylsulfenamido）-3-（1H-indol-3-yl）propanoate

With an aim to discover novel AHAS inhibitors,the title compound (S)-ethyl-2(2-methoxy-phenylsulfenamido)-3-(1H-indol-3-yl)propanoate (C 21 H 22 N 2 O 4 S,M r=398.47) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis.The crystal belongs to orthorhombic,space group P2 1 2 1 2 1 with a=8.078(2),b=12.824(4),c=18.788(6),V=1946.2(10) 3,Z=4,F(000)=840,D c=1.360 mg/m 3,μ=0.197 mm-1,the final R=0.0433 and wR=0.1035 for 3075 observed reflections with I > 2σ(Ⅰ).The absolute structure Flack parameter X of this compound is 0.00(8).A total of 14375 reflections were collected,of which 3431 were independent (R int=0.0437).X-ray analysis reveals that the crystal structure involves two intermolecular N-H···O and one N-H···S intermolecular hydrogen bonds with the neighboring molecules.The crystal structure was compared with our previously reported (S)-methyl 2-(4-R-phenylsulfonamido)-3-(1H-indol-3-yl)propanoate (R=H(1) and Cl(2)),which provided some useful information of these compounds.     

Synthesis and Crystal Structure of （2S,5S）-1-Aza-2-（2-pyridyl）-3-oxa-4,4-diphenylbicyclo [3.3.0] Octane

1 INTRODUCTION The catalytic asymmetric synthesis has been a challenging subject in organic synthesis. The deve- lopment of efficient enantioselective catalysts appli- cable to a wide range of carbon-carbon bond form- ing reactions represents a pivotal …     

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 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…     

Solvothermal Syntheses of (H_2en)_2Sn_2S_6·en and[(H_2hmda)_3(Hhmda)_2](Sn_2S_6)_2Using SnCl_4 and S_8 as Starting Materials

1 INTRODUCTION Since Bedard et al. reported microporous tin(IV) sulfides synthesized by hydrothermal method in the presence of organic amine in 1989[1, 2], a number of thiostannates have been synthesized using hydro- or solvothermal techniques with organic amines as tem- plates. The structures of the resulting tin(IV) sulfi- des are related to the types of organic amines. Two- dimensional polyanions of the types of [Sn3S7]2- and [Sn4S9]2-, which are denoted as SnS-1 and SnS-3, respe…