Crystal Structure of a Marine Natural Compound, Anhydrofusarubin

One marine natural compound, anhydrofusarubin, was isolated from the endophytic fungus No. B77 from the mangrove tree on the South China Sea coast. It was the first time that such a compound was isolated from marine fungus. The structure was identified by NMR data and mass spectrometry （MS）. In addition, its structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1^- with a = 8.3185（15）, b = 12.397（2）, c = 13.767（3） A, α = 65.692（3）, β = 79.266（3）, γ= 75.692（3）°, C15H12O6, Mr= 288.24, V = 1248.0（4） A^3, Z = 4, Dc = 1.534 g/cm^3, F（000） = 600, μ = 0.120 mm^-1, the final R = 0.0459 and wR = 0.1184 for 5360 observed reflections （I 〉 2σ（I））. In the primary bioassay, the title compound shows strong inhibitory activity against Gram-positive bacteria Staphyococcus aureus （ATCC27154） with the MIC value of 12.5 μg/mL.     

Synthesis, Structural Features and Evaluation of Antibacterial Activities of Two Schiff Bases Derived from 3,4-Dihydroxybenzhydrazide

A new Schiff base compound (I), (E)-N'-(2-hydroxy-3-methoxybenzylidene)-3,4-dihydroxybenzohydrazide-ethanol-water (1/1/1), has been synthesized and characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/n with a = 7.459(4), b = 18.316(10), c = 13.638(7), β = 101.585(9)o, V = 1825.2(17)3, Z = 4, μ = 0.104 mm-1, Dc = 1.333 g/cm3, F(000) = 776, the final R = 0.0635 and wR = 0.1302 for 3216 observed reflections with I 2σ(I). Another compound (Ⅱ), (E)-N'-(2,5-dimethoxybenzylidene)-3,4-dihydroxybenzohydrazide-ethanol-water (1/1/1), has been synthesized and reported before. The antibacterial activities of these two compounds against seven bacteria were first evaluated, and one compound showed considerable antibacterial activity against S. aureus.     

Crystal Structure of Phenol,2-[4（S）-4-Dihydro-4-benzyl-2-ozazolinyl]

The compound phenol,2-[4(S)-4,5-dihydro-4-phenyl-2-ozazolinyl(1,C15H13NO2) was synthesized with a simple,one step method free of water and air.It was obtained in a moderate yield from the reaction of 2-hydroxybenzonitrile with optically active amino alcohol in chloroben-zene under dry,anaerobic conditions.It belongs to the orthorhombic system,space group P212121 with a = 5.786(5),b = 10.730(5),c = 19.722(5),C15H13NO2,Mr = 239.26,V = 1224.4(12)3,Z = 4 and Dc = 1.298 mg/m3.The final R = 0.0324 for 1627 observed reflections with Ⅰ 2σ(Ⅰ) and Rw = 0.0826 for all data.The structure of compound 1 was determined by X-ray diffraction,NMR and HRMS.     

Synthesis,Crystal Structure and Antimicrobial Study of N,N,N''-Tris(3-aminopropyl)ethylenediamine Copper(Ⅱ) Diperchlorate

The title compound [Cu(C11H29N5)](ClO4)2 was synthesized and characterized by elemental analysis,IR and X-ray single-crystal diffraction.The compound crystallizes in the monoclinic system,space group P21/n with a = 9.405(2),b = 14.495(3),c = 14.715(3)(A),β = 90.262(3)°,V =2006.1(7)(A)3,Mr = 493.83,Z= 4,F(000) = 1028,Dc= 1.635 g/cm3,T= 298(2) K,μ = 1.403 mm-1 and λ = 0.71073(A).The structure was refined to R = 0.0508 and wR = 0.1250 for 2293 observed reflections with I ＞ 2σ(I).The Cu(Ⅱ)atom possesses a five-coordinate CuN5 environment which shows a slightly distorted square-pyramidal geometry.Antimicrobial activity study found that the complex is active against Salmonella species,Staphylococcus aureu,Bacillus pumilus and Bacillus coliforms.     

A Novel Three-dimensional Inorganic Open-framework Constructed from [Mo_4O_(16)]_n ~(8n-) Chains Linked through Ag~+

1 INTRODUCTION even three-dimensional (3-D) extended solid frame- works in appropriate ways is a major challenge in The syntheses and characterizations of novel po- POMs chemistry. Based on the fact that POMs fra- lyoxometalates (POMs) have currently attached in- meworks with high electronic density can act as un- creasing interest owing to not only enormous variety usually effective ligands to coordinate second tran- of intriguing structural topologies, but also their fas- sition meta…     

Syntheses and Crystal Structures of 3,5-Diiodo-salicylalidehyde and 3,5-Diiodo-salicylalidene-4-nitroaniline

The title compounds, C7H4I2O2 1 and C13H7I2N2O3 2, have been synthesized and characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in monoclinic, space group P21/c with a = 9.802（2）, b = 13.867（3）, c = 7.364（2） A, β = 109.74（3）°, V= 942.1（3） A^3, Dc= 2.636 g/cm^3, C7H4I2O2, Mr= 373.90, F（000） = 672, μ = 6.627 mm^-1, Z = 4, R = 0.0459 and wR = 0.1018 for 1805 observed reflections （I 〉 2 σ（I））. Compound 2 belongs to the monoclinic system, space group P21/n with a = 9.015（2）, b = 12.024（2）, c = 14.072（3） A, β = 103.91（3）°, V = 1480.6（5） A^3, Dc= 2.216 g/cm^3, C13H7I2N2O3, Mr= 494.01, F（000） = 920, p = 4.255 mm^-1, Z = 4, R = 0.0777 and wR = 0.1757 for 2896 observed reflections （I 〉 2σ（I））. Compounds 1 and 2 were assayed for antibacterial activities against three Gram positive bacterial strains （B. subtilis, S. aureus and S. faecalis） and three Gram negative bacterial strains （E. coli, P. aeruginosa and E. cloacae） by MTr method. Fortunately, compound 2 is found to show potent antibacterial activity against these six bacterial strains.     

Synthesis and Crystal Structure of N-Phenylbis（ferrocenecarboxyl）imide

The ferrocenyl compound,N-phenylbis(ferrocenecarboxyl)imide (C28H23NO2Fe2,Mr=517.17),was synthesized and structurally characterized by means of X-ray single-crystal dif-fraction. It crystallizes in monoclinic,space group C2/c with a=21.374(14),b=10.430(7),c= 10.741(7) ,β=114.184(8)°,V=2184(2) 3,Z=4,Dc=1.573 g/cm3,F(000)=1064,μ(MoKα)= 1.355 mm–1,T=291(2) K,the final R=0.0548 and wR=0.1437 for 1524 observed reflections with I > 2σ(I). In this compound,the nitrogen atom links two ferrocenyl groups and one phenyl group forming a novel imido derivative.     

Synthesis and Crystal Structure of 2-Ethoxy-spiro[2H-1, 4,2-benzoxazaphosphorine-3（4H）, 1＇-Cycloheptane] 2-Oxide

1 INTRODUCTION α-Aminophosphonates are an important class of compounds since they are considered as structural analogues of the corresponding α-amino acids. Their utilities as enzyme inhibitors, antibiotics, pharma- cological agents and many other applications are well documented[1~5]. Moreover, cyclic α-amino- phosphonates, one important kind of α-aminopho- sphonates, have attracted chemists’ interests for a long time[6~11]. In order to search for potent and selec- tive herbicides a…     

Synthesis, Characterization and Crystal Structure of a Noncentrosymmetric Coordination Polymer with 3-Aminopyridine

Hydrothermal reaction of 3-aminopyridine, NaSCN and cadmium cation led to the formation of complex [Cd（3-ampy）（NCS）2]n 1 （3-aminopyridine = 3-ampy）, and its crystal structure was determined by X-ray diffraction analysis. The crystal data for compound 1： C7H6N4S2Cd, orthorhombic Fdd2, Mr = 322.68, Z = 16, a = 26.884（4）, b = 27.445（3）, c = 5.8671（7）A, V = 4329.0（10） A3 Dc= 1.974 g/cm^3, μ= 2.368 mm^-1, F（000） = 2496, R = 0.0203 and wR = 0.0491 for 2347 observed reflections with Ⅰ 〉 2σ（Ⅰ）, and absolute structure parameter is 0.00（3）. X-ray diffraction reveals that the compound consists of interesting two-dimensional wave sheet structure. The photoluminescence spectrum and interesting second-order nonlinear optical （NLO） property for compound 1 have also been studied.     

Synthesis and Crystal Structure of Dinuclear Copper Cluster Compound ［Cu（dtp）PPh_3］_2

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＤｉｎｕｃｌｅａｒＣｏｐｐｅｒＣｌｕｓｔｅｒＣｏｍｐｏｕｎｄ［Ｃｕ（ｄｔｐ）ＰＰｈ_３］_２ＣｈｅｎＱｉｕ－Ｈｕａ；ＬｕＳｈａｏ－Ｆａｎｇ；ＨｕａｎｇＸｉａｏ－Ｙｉｎｇ（ＳｔａｔｅｋｅｙＬａｂ...     

Synthesis and Crystal Structure of Tert-butyl 4-[(E)-4-(1,3-Dioxo-1,3-dihydro-2H-isoindol-2-yl)-1-butenyl] Benzoate

1 INTRODUCTION Phthalimide and its derivatives are synthetic mate- rials, which are widely used as important chemical intermediates of biosensors[1] and many drugs such as Citalopran[2], luminal[3], Beta-Lactam[4] and the No. three generation quinolones[5], and they have been identified as active groups of some drugs and chemical luminescence reagents[6, 7]. Tert-butyl 4- [(E)-4-(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)-1- butenyl] benzoate is an intermediate of a new type of insulin sen…     

Crystal Structure and Photochromism in Paint and Solutions of 2,2-Dithiophene-naphthopyran

The title compound 2,2-dithiophene-naphthopyran （C21H14OS2, Mr = 346.44） was synthesized and characterized by IR,^1lH NMR, elemental analysis and single-crystal X-ray diffraction. It belongs to the monoclinic system, space group P21/n, with a = 8.2349（14）, b = 6.1964（11）, c = 32.458（5）A, β= 95.051（3）°, V= 1649.8（5）A^3, Z = 4, Dc = 1.395 g/cm^3,μ = 0.327 cm^-1, F（000） = 720, the final R = 0.0559 and wR = 0.1442 for 3370 observed reflections （I 〉 2σ（I））. X-ray analysis revealed that the interatomic distance of C（13）-O（1） is 1.456（3）A, longer than that of normal C-O bond （1.41 - 1.43 A） in a six-membered heterocycle. The UV-vis spectra of the title compound showed that it exhibits excellent photochromic property in polyester coating and solutions.     

Synthesis and Crystal Structure of （Z）-Methyl-3-methoxy-2-{2-[（4-（E-3-p-tolylacryloyl）phenoxy）methyl]phenyl}acrylate

The title compound,(Z)-methyl-3-methoxy-2-{2-[(4-(E-3-p-tolylacryloyl)phenoxy)-methyl]phenyl}acrylate,was synthesized and determined by X-ray single-crystal diffraction. The crystal belongs to the triclinic system,space group P1 with a = 8.0157(8),b = 12.5748(13),c = 13.3768(14) ,α = 64.770(2),β = 75.720 (2),γ = 89.784(2)°,μ = 0.085 mm-1,Mr = 442.49,V = 1174.1(2) 3,Z = 2,Dc = 1.252 g/cm3,F(000) = 468,T = 294(2) K,R = 0.0603 and wR = 0.1498 for 2644 observed reflections with I 2σ(I). X-ray diffraction analysis reveals that the single crystal contains strong non-classical hydrogen bonds. The preliminary bioassay showed that the title compound exhibits inhibitory activity against the Pseudoperoniospora cubensis and Rhizoctonia solani at the test concentration of 200 mg/L.     

Synthesis and Crystal Structure of a Model for the Active Sites of Fe-only Hydrogenases： [Fe2（SCH2）2N（3-PhCF3）（CO）6]2

A model compound for the active sites of Fe-only hydrogenases,[Fe2(SCH2)2N(3-PhCF3)(CO)6]2,has been synthesized and structurally characterized by single-crystal X-ray diffraction.It crystallizes in tetragonal,space group P43,with a = 12.6324(3),b = 12.6324(3),c=24.0453(12) (A),V = 3837.1(2) (A)3,Z = 4,Fe4S4N2C30O12F6H16,Mr= 1062.09,Dc= 1.839 g/cm3,μ(MoKa) = 1.791 mm-1,F(000) = 2112,T= 293(2) K,Flack = 0.034(9),R= 0.0282 and wR =0.0685 for 8148 observed reflections with I ＞ 2σ(I).In the title compound,each Fe1 atom is coordinated by three terminal carbonyl C atoms (Fe-C:1.783(3)～ 1.816(3)(A)),two bridging S atoms (Fe-S:2.2609(7)～2.2757(8)(A)) and another Fe atom (Fe-Fe 2.5011(5) (A)),adopting a distorted octahedral geometry with trans angles ranging from 152.45( 11 ) to 157.77(10)°.     

Synthesis and Crystal Structure of Glycin·3,5-Dihydroxybenzoic Acid

The title compound glycin·3,5-dihydroxybenzoic acid (GDB) has been synthesized and characterized by single-crystal X-ray analysis. It crystallizes in orthorhombic, space group Pca21 with a = 25.513(10), b = 4.668(2), c = 9.150(4)(A), Z = 4, V = 1089.8(8)(A)3, C9H13NO7, Mr = 247.20, Dc = 1.507 g/m3, μ(MoKα) = 0.132 mm-1, F(000) = 520, R1 = 0.0322 and wR2 = 0.0611 for 885 observed reflections (I > 2σ(I)). The title compound is a 1:1 molecular complex of glycin and 3,5-dihydroxybenzoic acid, which is linked by O-H…O and N-H…O hydrogen bonds to form a three-dimensional framework. Test of SHG (second harmonic generation) indicates that NLO generation of the crystal is higher than that of KDP.     

Synthesis and Crystal Structure of α-Mo4XS3(μ-dtp)3(dtp)3 (X=0.6S + 0.4O)

The title compound (Mo4XS15P6O12C24H30), α-Mo4XS3(μ-dtp)3(dtp)3 (X=0.6S+0.4O; dtp=-S2P[OEt]2), isolated as a prismatic black crystal, was prepared from ethanolic solution of Mo(CO)6, MoCl5 and P2S5. It crystallizes in triclinic system, space group P with a=14.031(4), b=13.372(2), c=16.270(8)(A), α=92.15(2), β = 72.91(3), γ = 95.20(2)°, V = 2905.4(2)(A)3, Z = 2, Dc = 1.82 g/cm3, Mr=1598.93, F(000)=1564.8, λ=0.71069(A)(MoKα), μ=1.584 mm-1. The final R=0.058, Rw=0.057 for 5016 observed reflections with I≥3.0σ(I). The structure analysis reveals that the title compound has a [Mo4XS3] core, belonging to the cubane-type tetranuclear molybdenum clusters family, with one of its four μ3-caps being statistically occupied by S and O. Three dtp ligands chelated three μ-X capped Mo atoms as terminal ligands, while another three dtp bridged these three Mo atoms and the fourth one, forming an α-type cluster compound.     

Synthesis, Crystal Structure and Magnetic Properties of Cobalt(II) Complex Involving Imino Nitroxide Radicals

1 INTRODUCTION The synthesis and study of transition metal com-plexes incorporating organic free radicals have arou-sed great interest in the field of molecular magne-tism[1]. Nitronyl nitroxide radicals (NITR), stable or-ganic radicals, have been widely used as molecularunits in the design and construction of magnetic ma-terials[2～5]. These radicals are especially attractivedue to that their donor atoms can assemble an exten-ded coordination geometry with changing magneticcoupling. A…     

Synthesis, Crystal Structure and Theoretical Calculation of 1,1',5,5'-Tetramethyl-2,2'-diphenyl-4,4'-[i-phenylene-bis(methylidynenitrilo)] di-1H-pyrazol-3(2H)-one

1,1',5,5'-Tetramethy1-2,2'-diphenyl-4,4'-[i-phenylenebis(methylidynenitrilo)]di1H-pyrazol-3(2H)-one was synthesized and characterized by X-ray single-crystal diffraction analysis. The crystal crystallizes in monoclinic, space group P21/c with a = 6.1375(1), b =24.6571(4), c = 17.7487(3)(A), β = 94.781(1)°, V= 2676.62(8)(A)3, C30H28N6O2, Mr= 504.58, Z = 4,Dc = 1.252 g/cm3, F(000) = 1064, μ = 0.081 mm-1, R = 0.0463 and wR = 0.1153 (I ＞ 2σ(Ⅰ)).Theoretical studies of the title compound were carried out by density functional theory (DFT) BLYP method, using ADF program package. It indicates that N(26) and N(41) are active sites of the title compound.     

Synthesis and Structure of N-（1,5-Dihydro-1-phenyl-3-methyl-4-benzoyl）-3-chloroaniline

1 INTRODUCTION 4-Acyl-5-pyrazolone, a family of flexible b- diketonate, is widely used as extract[1] and well known for its applications as analgesics, antipyre- tics, anti-inflammatory and insecticides[2]. Therefore the study on the derivation of 4-acyl-5-pyrazolone is the focus of many research groups working in the fields of coordination chemistry, biomedicine and pharmaceutical chemistry. In order to study the rela- tionship between the structure and performance of these compounds, w…     

A Photoluminescent Bimetallic Zinc-pyridinedicarboxylate：Diverse Supramolecular Motifs from Distinct Hydrogen Bonds

A cyclic bimetallic metal-organic complex [Zn（C）（H-fmpdc）（H2O）]2·2H2O （fmpdc = 4-（furan-2-yl）-2,6-dimethylpyridine-3,5-dicarboxylate） was synthesized and characterized by single-crystal X-ray analysis. The compound crystallizes in orthorhombic, space group Pbca with a = 12.905（2）, b = 14.774（3）, c = 16.833（3）A, V= 3029.4（10）A^3 Z = 4, Dc = 1.644 g/cm^3, F（000） = 1616, R = 0.0347 and wR = 0.0956 （I 〉 2σ（I））. There exist diverse supramolecular motifs （1-D, 2-D and 3-D） from distinct hydrogen bonds in the crystal structure of the title compound. The furanyl group has obvious contribution to the red-shift in the photoluminescent spectrum of the H2fmpdc ligand. The title compound 1 shows strong photoluminescence with emission maximum at 2 = 402 nm （λex.max = 367 nm）.