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…     

Vibrational Spectroscopic Study of （E）-3-（4-fluorophenyl）-N-[4-（phenylamino） quinazoline-7-yl] Acrylamide

Geometry optimization and subsequent harmonic vibration calculations of prior synthesized (E)-3-(4-fluorophenyl)-N-[4-(phenyl-amino) quinazoline-7-yl] acrylamide were carried out by DFT/B3LYP method with both 6-31G and 6-311G basis sets.The Infrared (IR) spectrum of the title compound was recorded in the field of 400-4000 cm 1 and then assigned.The correlation analyses between the scaled theoretical vibration frequencies and the experimental ones indicate that there exist good linearity relationships since the correlation coefficients R 2 are larger than 0.999.The intramolecular interactions existed in the title molecule were confirmed by the Atoms in molecules (AIM) method,and their influences on the absorption frequency were also investigated.     

Synthesis and Crystal Structure of 4-（4-Chlorophenyl）-6-methyl-5-methoxy-caronyl-3,4-dihydropyrimidin-2（H）-one

1 INTRODUCTION Biginelli reaction is a three-component condensa-tion of ethyl acetoacetate, benzaldehyde and urea forthe synthesis of 3,4-dihydropyrimidin-2(1H)-ones(Scheme 1). The reaction can be carried out in aone-pot fashion in alcohol solution in t…     

Synthesis and Crystal Structure of 3,3 ＇-（2,2 ＇-（E thane- 1,2-diylbis（oxy） ） bis（ethane- 2,1- diyl））bis（2-（4-chlorophenylamino）quinazolin-4（3H）-one）

The title compound 3,3＇-（2,2＇-（ethane-1,2-diylbis（oxy））bis（ethane-2,1-diyl））bis（2- （4-chlorophenylamino）quinazolin-4（3H）-one） 3 （C34H30CI2N604, Mr = 657.54） has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in space group P1 with a = 9.9185（8）, b = 10.6124（9）, c = 15.4064（13） A, α = 92.896（2）,β = 103.813（2）, γ= 94.635（2）°, V= 1565.5（2） A3, Z = 2, Dc = 1.395 g/cm^3,μ = 0.257 mm^-1, F（000） = 684, the final R = 0.0580 and wR = 0.1284 for 3400 observed reflections （I〉 2σ（I）. It remains triclinic in the crystal. Intra- and intermolecular N（3）-H（3A）…O（2）, N（6）-H（6A）…O（3） and C（19）-H（19A）…O（4） #1 （#1： 1-x, 1-y, -z） hydrogen bonds are observed in the title compound. A two-dimensional chain network is formed from the dimmers and intermolecular π-π interactions in the crystal structure. This open network has solvent-accessible voids （10A3）.     

Synthesis and Crystal Structure of（E）-Ethyl 2-（5-（3-methyl-2-butenyloxy）-2-（3-（4-（3-methyl-2-butenyloxy）phenyl）acryloyl）phenoxy）acetate

The title compound,(E)-ethyl 2-(5-(3-methyl-2-butenyloxy)-2-(3-(4-(3-methyl-2-butenyloxy)phenyl) acryloyl) phenoxy)acetate(1),has been synthesized and characterized by FT-IR and 1H-NMR spectroscopy,ESI-MS,and X-ray single-crystal diffraction.FT-IR,1H-NMR and ESI-MS confirm the functional groups,particularly the ethyl groups in the ester moiety,of the compound.The single-crystal X-ray diffraction has revealed a monoclinic structure,space group P21/n with a = 14.6832(14),b = 7.7581(7),c = 23.075(2),β = 101.670(2)o,V = 2574.2(4) ?3,Z = 4,Dc = 1.235 g/cm,μ = 0.085 mm-1,and F(000) = 1024.The skeleton of chalcone in the molecular structure is coplanar.     

Crystal Structure and Biological Activities of （R）-N′-[2-（4-Methoxy-6-chloro）-pyrimidinyl]- N-[3-methyl-2-（4-chlorophenyl）butyryl]-urea

1 INTRODUCTION The acyl ureas are a kind of high biological acti- vity compounds with low toxicity to mammals, birds, fish, amphibians, etc., and significant organic synthe- sis intermediates working extensively as insecticides, pesticides, fungicides and herbicides in agrochemi- cal industry[1～7]. While pyrimidinyl derivatives show excellent biological activities in the development of pesticide, and are used to develop high effective and high select herbicides. For example, pyrimidiny su…     

Synthesis and Crystal Structure of 2,2-Dimethyl-4-[1H-（ 1,2,4-triazolyl）]-4- [ 1H-benzotriazolyl]-3- butanone[t-BuCOCH（C2H2N3）（C6H4N3）]

1 INTRODUCTION Triazole nuclei appear frequently in the structures of various natural products and biologically active compounds, notably thiamine (vitamin B), peni- cillins, antibiotics such as micrococcin[1], and many metabolic products of fungi and p…     

Synthesis and Crystal Structure of Tetrakis（4—methylpyridine）bis（μ4—pentathio）—tetracopper（Ⅰ）（4—methylpyridine）solvate

1 INTRODUCTION An interesting aspect in the studies of copper-sulfur coordination chemistry is the apparent tendency of Cu(Ⅰ) ions to form various clusters with sulfur ligands. The coordination chemistry of Cu(Ⅰ) has been studied extensively owing to the importance of Cu(Ⅰ) in biological systems and copper-sulfur bonds detected in some metallopro- teins[1]. More recently, remarkably rich photoluminescence properties have been found in the tetranuclear complexes[2～5] and the cage-ty…     

Synthesis,Characterization and X-ray Crystal Structure of 4-Fluoro-N-（2-methyl-5-（（2-（p-tolyloxy）acetamido）- methyl）pyrimidin-4-yl）benzamide

A new crystal of 4-fluoro-N-(2-methyl-5-((2-(p-tolyloxy)acetamido)methyl)pyrimi- din-4-yl)benzamide has been prepared at room temperature and characterized by 1H NMR, 13C- NMR, IR, MS, elemental analysis and X-ray single-crystal determination. The compound crystallizes in monoclinic, space group P21 /c with a = 17.226(5), b = 13.934(4), c = 17.262(5), μ= 92.180(5)°, V = 4140(2) ?3, Dc = 1.311 g/cm3, Z = 8, F(000) = 1712 and ??= 0.095 mm-1. The molecular packing in the crystal is the result of N–H···O hydrogen bonds.     

Syntheses, Crystal Structures and Antibacterial Activities of Copper（Ⅱ） and Zinc（Ⅱ） Complexes Based on （E）-4-fluoro-2-（（3-morpholinopropylimino）methyl）phenol

Two Schiff base complexes [Cu(L)2] (1) and [Zn(L)2]·3H2O(2) of (E)-4-fluoro-2-((3-morpholino propylimino)methyl)phenol (HL) have been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. Crystal data for 1: triclinic, space group Pī with a=4.8000(10), b=11.109(2), c=13.921(3),α=66.55(3),β=80.35(3),γ=81.09(3)°, V=668.2(2)3 , Z=1, Dc=1.477g/cm 3 , F(000)=311, and the final R=0.0744 and wR=0.1601 for 2301 observed reflections with I > 2σ(I). And those for 2: monoclinic, space group P21 /c with a=14.789(3), b=11.713(2), c=18.846(4),β=107.85(3)°, V=3107.4(11)3 , Z=4, D c=1.389 g/cm 3 , F(000)=1368, and the final R=0.0749 and wR=0.1348 for 5423 observed reflections with I > 2σ(I). Both 1 and 2 are four-coordinated complexes, with a square-planar geometry of copper(Ⅱ) in 1 and a slightly distorted tetrahedral geometry of zinc(Ⅱ) in 2. An asymmetric unit consists of only one half of a Cu ion and one L ligand in 1, while an asymmetric unit is composed of one Zn ion, two L ligands and three water molecules in 2. Non-classical C-H···O and C-H F hydrogen bonds play important roles in the formation of a 1D chain of 1, but O-H O and O-H N hydrogen bonds play dominant roles in the self-assembly of a 3D network of 2. The antibacterial activities of 1 and 2 against B. subtilis, S. aureus, S. faecalis, P. aeruginosa, E. coli and E. cloacae have been evaluated by MTT method.     

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…     

Synthesis and Crystal Structure of N-[(3aR,4R,4aR,5aS,6S,6aS)-1,3-Dioxooctahydro-4,6-ethenocyclopropa[f]isoindol-2(1H)yl]-4-(trifiuoromethyl)phenylmethanimine Monohydrate

The crystal structure of the title compound (C19H17F3N2O4,Mr=394.35) was determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group C2/c with a=28.383(6),b=10.355(2),c=12.799(3)(A),β=111.74(3)°,V=3493.8(12)(A)3,Z=8,De=1.499 g/cm3,λ(MoKα)=0.71073,F(000)=1632,μ= 0.127 mm-1,R=0.0412 and wR=0.1019.In the title compound,there exist three intennolecular hydrogen interactions (O(4)...O(1),O(4)...O(3) and O(4)...N(1)) between water.The neighboring molecules are linked to each other generating a two-dimensional network structure via the three intermolecular hydrogen bonds and π-π interactions shaped by phen-phen with centroid distance of 4.049 (A).     

Synthesis,Crystal Structure and Biological Activities of 1-（（5-（4-（4-Chlorophenoxy）-2-chlorophenyl）-2,2,3- trimethyloxazolidin-5-yl）methyl）-1H-1,2,4-triazole

The title compound 1-（（5-（4-（4-chlorophenoxy）-2-chlorophenyl）-2,2,3-trimethyl-oxazolidin- 5-yl）methyl）-lH-1,2,4-triazole （C21H22Cl2N4O2）has been synthesized and characterized by elemental analysis, IR, 1H NMR, MS and single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pi with a = 6.891（2）, b = 9.074（2）, c = 18.258（4）AA, α = 99.292（4）, β = 95.105（4）, γ = 108.068（3）°, C21H22Cl2N4O2, Mr = 433.33, V= 1059.3（4） Aa, Z = 2, Dc = 1.359 g/cm3, F（000） = 452,μ = 0.331 mm-1, the final R = 0.0448 and wR = 0.0994 for 3727 unique reflections. The dihedral angle between the oxazolidine ring taking an envelope conformation with a local pseudo-mirror and the triazole ring is 27.7（9）°. Weak intermolecular C-H...N hydrogen bonds and π-π interactions exist between the triazole rings of neighboring molecules, forming a three-dimensional network, which stabilizes the crystal structure. The primary biological test shows the target compound has certain fungicidal activity.     

Synthesis and Crystal Structure of Sodium Monosulfuron (N-(4-Methylpyrimidin-2-yl)-N''''-2-(nitrophenylsulfonyl) Urea Sodium)

Monosulfuron is a novel sulfonylurea herbicide with ultra-low dosage invented and patented by Nankai University.Herein its sodium salt was firstly synthesized and crystal structure was determined by X-ray diffraction method.The title compound belongs to the triclinic system, space group P1- with a = 7.306(6), b = 9.446(8), c = 11.872(10)(A), α= 76.578(14), β= 78.049(13), γ= 77.620(14)°, V = 767.7(11)(A)3, Mr = 377.32, Z = 2, Dc = 1.632 g/cm3,μ= 0.283 mm-1, F(000) = 388, R = 0.0444 and wR = 0.1186.In the title compound, Na(1) coordinates with O(4) and O(5) from one monosulfuron molecule, N(4A) and O(5A) from the other monosulfuron molecule and the oxygen atom from H2O to give five coordination bonds.The title complex is further linked into a three-dimensional structure through π…π interactions and intermolecular hydrogen bonds between the oxygen and nitrogen atoms.     

Synthesis, Crystal Structure and Bioactivities of 1-（4-Chlorophenyl）-3- [ 5-（pyrid-4-yl）- 1,3,4-thiadiazol-2-yl] urea

The title compound 1-(4-chlorophenyl)-3-[5-(pyrid-4-yl)-1,3,4-thiadiazol-2-yl]urea (C14H10ClN5OS, Mr = 331.79) has been synthesized by the reaction of 2-amino-5-(pyrid-4-yl)- 1,3,4-thiadiazole with 4-chlorobenzoyl azide, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to triclinic system, space group P with a = 5.8550(8), b = 7.5668(10), c = 16.416(2) , α = 78.364(2), β = 81.204(2), γ = 84.749(2)°, V = 702.58(16) 3, Z = 2, Dc = 1.568 g/cm3, μ = 0.429 mm-1, F(000) = 340, the final R = 0.0442 and wR = 0.1092 for 2001 observed reflections (I > 2σ(I)). X-ray diffraction analysis reveals that the title molecule is nearly planar. In the crystal structure, the molecules are linked by strong intermolecular N-H…N hydrogen bonds together with weak nonclassical intermolecular (C-H…Y, Y = N, O and Cl) hydrogen bonds and stacked through π-π interactions. The preliminary bioassay shows that the title compound exhibits good fungicidal activities against Rhizoctonia solani, Botrytis cinerea and Dothiorella gregaria.     

Synthesis and Crystal Structure of 1-[4-(Pyrimidin-2-yl)piperazin-1-ylmethyl]-1H-benzotriazole

1 INTRODUCTION Based on the reported 1.65 ? high resolution crystal structure of spinach KARI (ketol-acid reduc- toisomerase) complex[1], we obtained 279 molecules with low binding energy toward KARI from MDL/ ACD 3D database searching, using program DOCK 4.0[2]. These potential structures provide further information for the design of new KARI inhibitors, one of novel derivatives of which as the title com- pound has been synthesized. Its crystal structure will provide us more inf…     

Synthesis and Crystal Structure of 3,3''-(2,2''-(Ethane-1,2-diylbis(oxy))bis(ethane-2,1-diyl))bis(2-(4-chlorophenylamino)quinazolin-4(3H)-one)

The title compound 3,3'-(2,2'-(ethane-1,2-diylbis(oxy))bis(ethane-2,1-diyl))bis(2- (4-chlorophenylamino)quinazolin-4(3H)-one) 3 (C34H30Cl2N6O4, Mr = 657.54) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in space group P1 with a = 9.9185(8), b = 10.6124(9), c = 15.4064(13) , α = 92.896(2), β = 103.813(2), γ = 94.635(2)°, V = 1565.5(2) 3, Z = 2, Dc = 1.395 g/cm3, μ = 0.257 mm–1, F(000) = 684, the final R = 0.0580 and wR = 0.1284 f...     

Synthesis and Crystal Structure of [Cu(phen)2(SO4)(H2O)]·0.5C4H4O4·7H2O

The title compound, [Cu(phen)2(SO4)(H2O)]·0.5C4H4O4·7H2O (phen = 1,10-phe-nanthroline and C4H4O4 = fumaric acid), has been synthesized and characterized by single-crystal X-ray diffraction. The crystal is of triclinic, space group P with a = 11.4827(2), b = 11.9086(2), c = 13.77350(10)(A), α = 80.6830(10), β = 66.6480(10), γ = 64.0480(10)o, V = 1554.63(4) (A)3, Mr = 722.17, Z = 2, Dc = 1.543 g/cm3, μ = 0.845 mm-1, F(000) = 750, R = 0.0349 and wR = 0.0837 for 4754 observed reflections (I > 2σ(I)). The compound contains a six-coordinated copper(II) center, which is surround by four N atoms of two phen ligands (Cu-N distances in the range of 1.997(2)～2.225(2)(A)), one sulfate O atom (Cu-O = 2.0037(17) (A)) and one water O atom (Cu-O(5w) = 2.719(2) (A)) in a distorted octahedral geometry. Extensive hydrogen-bonding interactions are involved in water molecules, ligated sulfate anions and fumaric acid molecules. In addition, π-π interactions via aromatic nitrogen-containing ligands are also discussed. The combination of non-covalent interactions leads to the formation of a 3-D network structure.     

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 4-（2-Bromophenyl）-3,4,7,8-tetrahydro- 7,7-dimethyl-1-p-tolylquinoline-2,5（1H,6H）-dione

The title compound 4-（2-bromophenyl）-3,4,7,8-tetrahydro-7,7-dimethyl-1-p-tolylquinoline-2,5（1H,6H）-dione 1 （C24H24BrNO2, Mr = 438.35） was synthesized and characterized by IR, 1H NMR and elemental analysis. The crystal belongs to monoclinic, space group C2/c with a = 27.565（14）, b = 10.079（5）, c = 15.917（8） A,β = 111.059（9）°, Z = 8, V = 4127（4）A3, Dc = 1.411 g·cm^-3,μ（MoKa） = 2.011 mm^-1, F（000） = 1808, the final R = 0.0417 and wR = 0.1032 for 2393 observed reflections （I 〉 2σ（I））. X-ray analysis reveals that the pyridine ring adopts a distorted boat conformation, while another six-membered ring takes a half-chair conformation. In addition, there are non-classical hydrogen bonds of C-H…O and C-H…Br in the structure. The short distance （3.481A） between the adjacent 2-bromophenyl rings indicates the existence of π-π interaction.