Synthesis,Crystal Structure and Electrochemical Property of the Ferrocenyl Schiff-base (E)-N’(Ferrocene Ethylidene)Picolino Hydrazide

A novel Schiff-base compound based on ferrocene C18H17OFeN3 (1) has been synthesized and characterized by X-ray diffraction. The title compound crystallizes in monoclinic, space group P21/c with a = 19.2343(17), b = 10.5084(9), c = 7.9373(7) , β = 97.7740°, Z = 4, V = 1589.6(2) 3, Dc = 1.451 g/cm3, μ(MoKα) = 0.956 mm-1, F(000) = 720, the final R = 0.0343 and wR = 0.0973 for 2759 observed reflections (I > 2σ(I)). Electrochemical measurements exhibit that compound 1 undergoes a reversible one-electron redox process.     

Synthesis and Crystal Structure of 2-Methoxy-benzoic Acid 2-Oxo-3-（2,4,6-trimethyl-phenyl）-1-oxa-spiro[4.4]non-3-en-4-yl Ester

The new title compound 2-methoxy-benzoic acid 2-oxo-3-(2,4,6-trimethyl-phenyl)-1-oxa-spiro[4.4]non-3-en-4-yl ester(3,C25H26O5) has been synthesized by the condensation reaction of 4-hydroxy-3-(2,4,6-trimethyl-phenyl)-1-oxa-spiro[4.4]non-3-en-2-one(2) with 2-methoxylben-zoyl chloride,and characterized by 1H NMR and MS spectra.Its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of monoclinic,space group P21/c with a = 10.6945(7),b = 12.8176(7),c = 16.4223(10) ,β = 103.5665(17)o,V = 2188.3(2) 3,Z = 4,Dc = 1.234 g/cm3,F(000) = 864.000,μ = 0.085 mm-1,the final R = 0.0520 and wR = 0.1132 for 2732 observed reflections with I 2σ(I).In the crystal structure,the C(1)-C(2)(1.478 ) bond is significantly shorter than the normal single C-C bond(1.53 ),suggesting that the carbonyl group on C(1) has formed a conjugated system with a double bond on C(2) and C(12).     

Structure and Luminescence Property of a Hexanuclear Silver（Ⅰ） Cluster Containing Benzaldehyde Thiosemicarbazone

A new hexanuclear silver (I) compound 2 containing thiosemicarbazone with the group of benzene was synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analysis and fluorescence spectrum. The title compound crystallizes in triclinic, space group P with a = 11.611(3), b = 15.610(5), c = 15.624(7) , α = 113.942(6), β = 104.520(6), γ = 104.230(4)°, V = 2304.1(14) 3, C60H77Ag6N22O4.5S6, Mr = 2018.02, Dc = 1.454 g/cm3, μ(MoKα) = 1.435 mm-1, F(000) = 1005, Z = 1, the final R = 0.0468 and wR = 0.1474 for 6608 observed reflections (I > 2σ(I)). In the structure, the S atom of the ligand L2 (L2 = benzaldehyde thiosemicarbazone) served as a triply bridged chelator to connect the six silver atoms into a Ag6L26 cluster. The luminescence property of compound 2 was investigated at room temperature.     

2-D Supramolecular Network and Photoluminescence of a Coupled 1,4-Dihydrylpyridine

A coupled 1,4-dihydrylpyridine compound(C40H48N2O10,1) has been synthesized.Its structure was determined by single-crystal X-ray diffraction.The crystal is of monoclinic system,space group P21/c with a = 8.3300(2),b = 15.720(3),c = 14.480(3) ,β = 90.08(3)°,V = 1896.1(7) 3,Z = 2,Mr = 716.80,Dc = 1.255 g/cm3,and F(000) = 764.The structure was solved by direct methods and refined by full-matrix least-squares method to the final R = 0.0556 and wR = 0.1499(I > 2σ(I)).There exist several supramolecular motifs in the crystal structure.The compound exhibits strong photoluminescence in the solid state at room temperature.     

Addition Reaction of Bis（diphenylphosphinyl） Butadiyne with Methylcyclopentadiene

Bis(diphenylphosphinyl)butadiyne reacted with methylcyclopentadiene at room tem- perature and four isomeric products were obtained. Crystal structures of isomers 1 and 3 have been determined. Crystal data for compound 1 C40H36O2P2·2CHCl3: monoclinic, space group C12/c1 with a = 17.983(2), b = 11.8723(12), c = 20.081(2) , β = 111.218(3)°, V = 3996.5(8) 3, Z = 4, Mr = 849.36, Dc = 1.412 g/cm3, F(000) = 1752, μ = 0.546 mm-1, the final R = 0.0351 and wR = 0.0951 for 3965 observed reflections (I > 2σ(I)); and those for compound 3 C40H36O2P2·H2O: triclinic, space group P1 with a = 10.4144(15), b = 13.0558(18), c = 13.742(2) , α = 70.453(8), β = 75.382(8), γ = 72.312(8)°, V = 1653.7(4) 3, Z = 2, Mr = 628.64, Dc = 1.262 g/cm3, F(000) = 664, μ = 0.169 mm-1, the final R = 0.0593 and wR = 0.1296 for 4891 observed reflections (I > 2σ(I)). The structures of the other two isomers are identified via IR, 1H NMR and MS spectra.     

Crystal Structure and Photochromism in Paint of 1,3,3-Trimethyl-6'-dihydro-indolinyl- spiro[2,3'-[3H]-naphtho[2,1-b][1,4]]oxazine

The title compound 2 (C30H27N3O, Mr = 445.55) has been synthesized and its structure was determined by X-ray crystallography method. The crystal is of monoclinic, space group P21/c with a = 17.520(15), b = 8.640(7), c = 15.439(13) , β = 98.642(14)°, V = 2310(3) 3, Dc = 1.281 g/cm3, μ = 0.780 mm-1, F(000) = 944, Z = 4, the final R = 0.0671 and wR = 0.1790 for 1952 observed reflections with I > 2σ(I). X-ray analysis revealed that the interatomic distance of C(20)O(1) is 1.464(4) , longer than that of the normal CO bond (1.41～1.43 ) in the six-membered heterocycle, but this kind of change coincides with other spiro compounds. The six-membered heterocycle containing spiro Csp3O is nonplanar. The UV-vis spectra of the title compound in polymer films showed that it exhibits excellent photochromic property.     

Synthesis and Crystal Structure of 4,4′-Diamino-N,N′-diethyl Bisbenzenesulfamide

A new compound of 4,4′-diamino-N,N′-diethyl bisbenzenesulfamide (C18H26N4O4S2, Fw = 426.55) has been synthesized and its structure was determined by X-ray crystallography method. The crystal belongs to the monoclinic system, space group P21/c with a = 10.0623(9), b = 13.6759(13), c =15.5309(14) , β = 100.482(2)o, V = 2101.6(3) 3, Dc = 1.348 g/cm3, F(000) = 904, μ = 0.285 mm–1, Z = 4, the final R = 0.0512 and wR = 0.1363 for 3485 observed reflections with I > 2σ(I). The structure of the title compound is pseudo secondary axisymmetric, and the two sulfamide-groups show distorted tetrahedral configurations.     

Synthesis and Crystal Structure of Dimethyl-3-（4-bromophenyl）-1-phenyl-4,5-dihydro-1H-pyrazole-4,5-dicarboxylate

The title compound (C19H17BrN2O4) was synthesized via a one-pot procedure starting from 4-bromobenzaldehyde, dimethyl acetylenedicarboxylate (DMAD) and phenylhydrazine with pyridine as the catalyst. Its structure was determined by single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 11.115(3), b = 8.090(2), c = 20.211(5) , β = 97.032(5)°, V = 1803.7(8) 3, Z = 4, Mr = 417.25, Dc = 1.536 g/cm3, μ = 2.306 mm-1, F(000) = 852, the final R = 0.0403 and wR = 0.0895 for 2215 observed reflections with I 2σ(I).     

Synthesis, Structure and Electrochemistry of Macrocyclic 1,1'-Bis(1,3-phenyleneoxyacetylpyrazoyl)ferrocene

1,1'-Diacetoacetylferrocene 1 reacted with phenylene-1,3-dioxyactyl hydrazine 2 in absolute ethanol to give the macrocyclic ferrocenyl dipyrazole compound in moderate yield. Determined by X-ray structure analysis, it crystallizes in monoclinic system, space group P21/c with a = 13.7509(4), b = 8.1277(2), c = 21.7472(6) , β = 103.1030(10)°, V = 2367.25(11) 3, Z = 4, Dc = 1.505 g/cm3, R = 0.0353 and wR = 0.0811. The electrochemical studies reveal that redox of Fe+/Fe in ferrocene is a reversible one-electron process.     

Synthesis and Hydrogen-bonded Interpenetrating Grid Structure of 5,5＇-Bis [4- （2-hydroxyethyl）phenyl] diazo-dipyrromethane

A new 5,5'-bisdiazo-dipyrromethane compound 3 has been synthesized and cha- racterized. The crystal of 3 is of orthorhombic, space group Iba2 with a = 19.1914(17), b = 9.8396(8), c = 13.7643(12) , V = 2599.2(4)3, Z = 4, C29H34N6O2, Mr = 498.62, Dc = 1.274 g/cm3 , F(000) = 1064, μ(MoKα) = 0.083 mm-1, the final R = 0.0302 and wR = 0.0786 for 6361 observed reflections with I > 2σ(I), and R = 0.0320 and wR = 0.08006 for all data. It reveals that the molecules of compound 3 assemble into grid structures through a R22(7) type hydrogen bonding motif between azopyrrole and hydroxyl group. The grids interpenetrate each other with the assistance of C-H···π interaction.     

邻羧基苯甲酰二茂铁钠的合成、晶体结构及电化学性质

参照文献方法合成了邻羧基苯甲酰二茂铁钠,首次培养得到了它的单晶．发现在其固态结构中,邻羧基苯甲酰二茂铁阴离子与四水合钠阳离子通过分子内氢键相互作用;分子间的氢键又把多个二茂铁衍生物分子连接成二维的网状结构．研究了标题化合物在甲醇溶液中的电化学性质．     

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.     

Syntheses and Crystal Structures of Methyl 2-（4,5-Dibromo- 1-methylpyrrole-2-carbonylamino）-3-phenyl propanoate and 4,5-Dibromo-1-methyl-2-trichloroacetylpyrrole

1 INTRODUCTION Pyrrole and its derivatives have attracted much attention due to their chemical properties as well as biological activities[1]. They have been widely used as the materials to produce pharmaceutical, essences, biochemicals, etc. It has been found that a great deal of pyrrole derivatives present bioactivities, such as antitumor and antiviral activities[2~5]. Thus, due to the interest in exploring the syntheses of potential bioactive materials which contain pyrrole ring andna…     

Ni(phen)(H2O)(V2O6)的水热合成和晶体结构（英）

A novel compound Ni(phen)(H₂O)(V₂O₆) has been hydrothermally synthesized and structurally determined to be a two-dimensional compound, which contains {V₂O₆}_n^2n- chains interconnected by nickel(Ⅱ) complexes via oxygen atoms. The crystallographic data measured by single-crystal X-ray diffraction analysis are as follows: C₁₂H₁₀N₂NiO₇V₂, M_r=454.81, monoclinic, space group P2₁/c, a=0.784 6(3), b=2.103 6(8), c=0.942 3(4) nm, β=112.872(5)°, V=1.433 0(10) nm³, Z=4, D_c=2.104 Mg·m^-3, μ(Mo Kα)=2.615 mm^-1, F(000)=904, T=298(2) K, 4 480 reflections collected, 2 470 independent (R_int=0.032 2), the final R=0.058 4 and wR₂=0.145 7 for 2 303 observed reflections with I>2σ(I). CCDC: 192520.     

Syntheses and Structures of Two Novel Salicylate-containing Mononuclear Manganese Complexes

Two salicylate containing mononuclear manganese complexes formulated as [Mn- (sal)2(CH3OH)2]·py (sal = salicylate, py = pyridine) 1 and (HNEt3)2[Mn(sal)3] 2 have been synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction analyses. Crystal data for compound 1: monoclinic, space group C2/c, a = 30.748(6), b = 8.1933(13), c = 21.137(4) °, β = 126.772(4)°, V = 4265.5(13) 3, Z = 8, Mr = 471.34, Dc = 1.468 g/cm3, μ = 0.667 mm-1, F(000) = 1952, the final R = 0.0637, wR = 0.1783 (I > 2σ(I)) and GOOF = 1.073; and those for compound 2: monoclinic, space group C2/c, a = 14.505(5), b = 11.048(4), c = 20.711(7) , β = 103.603(6)°, V = 3225.6 (18) 3, Z = 4, Mr = 668.65, Dc = 1.377 g/cm3, μ = 0.466 mm-1, F(000) = 1416, the final R = 0.0373, wR = 0.1125 (I > 2σ(I)), and GOOF = 1.000. The Mn atoms of both complexes are six-coordinated in an axially elongated octahedral geometry for 1 and an axially compressed octahedral geometry for 2, and their oxidation states have been determined to be trivalent by bond valence sum calculation.     

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, Structure and Electrochemistry of Macrocyclic 1,1＇-Bis（1,3-phenyleneoxyacetylpyrazoyl）ferrocene

1,1＇-Diacetoacetylferrocene 1 reacted with phenylene-1,3-dioxyactyl hydrazine 2 in absolute ethanol to give the macrocyclic ferrocenyl dipyrazole compound in moderate yield. Determined by X-ray structure analysis, it crystallizes in monoclinic system, space group P21/c with a = 13.7509（4）, b = 8.1277（2）, c = 21.7472（6） A, β = 103.1030（10）°, V = 2367.25（11） A^3, Z = 4, Dc = 1.505 g/cm^3, R = 0.0353 and wR = 0.0811. The electrochemical studies reveal that redox of Fe^＋/Fe in ferrocene is a reversible one-electron process.     

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 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…