具有绿色荧光发射效应的氟喹诺酮-铀(Ⅵ)配合物

A uranium(Ⅵ) complex [UO₂(1-ethyl-6,8-difluoro-7-(3-methyl-piperazinium-1-yl)-4-oxo-1,4-dihydro-quin-oline-3-carboxylate)(NO₃)₂] was obtained by the hydrothermal treatment of UO₂(NO₃)₂·6H₂O with lomefloxacin-HCl in water at 80 ℃ in Pyrex tube. The crystal belongs to monoclinic system, space group P2₁/c, with a=1.430(3) nm, b=1.032 1(18) nm, c=1.729(3) nm, β=106.67(3)°, V=2.458(6) nm³, Z=4. This complex is a good green fluorescent material in solid state at room temperature. CCDC: 660959.     

Synthesis and screening of some novel substituted indoles contained 1,3,4-oxadiazole and 1,2,4-triazole moiety

A series of novel 3-[5-(1H-indol-3-yl-methyl)-2-oxo-[1,3,4]oxadiazol-3-yl]propionitrile(5),3-[4- amino-3-(1H-indol-3-yl-methyl)-5-oxo-4,5-dihydro-[1,2.4]triazol-1-yljpropionitrile(6),3-[5-(1H- indol-3-yl-methyl)-2-thioxo-[1,3,4]oxadiazol-3-yl]propionitrile(7) and 3-[4-amino-3-(1H-indol-3-yl-methyl) -5-thioxo-4,5-dihydro-[1,2,4]triazol-l -yljpropionitrile(8) were synthesized in good yields from the intermediate(1H-indol-3-yl)-acetic acid N’-(2-cyanoethyl)hydrazide(4).The chemical structures of the newly synthesized compounds were elucidated by their IR,~1H NMR and MS.Further,all the compounds were screened for their antimicrobial activity against Gram-positive,Gram-negative bacteria and also tested their ability toward anti-inflammatory activity.     

噻吩甲酰基吡唑啉酮缩氨基酸稀土配合物的合成、表征及生物活性

A new amino-acid Schiff base, 1-phenyl-3-methyl-4-(2-thenoyl) pyrazolone-5-β-alanine (HL) and its ten rare earth complexes have been synthesized. On the basis of elemental analysis and molar conductance, the general formula of the complexes, [REL₂NO₃]·nH₂O (RE=La, Nd, Eu, Tb, Y, n=2; RE= Pr, Sm, n=1; RE= Dy, Er, Yb, n=3), is given. They were characterized by IR, UV-visible, ¹H NMR, ¹³C NMR and fluorescence. The results show that the rare earth ions exhibit coordination of eight in the complexes.The antibacterial experiments indicate that they have high antibacterial activities against S. Aureus, B. Subtillis, E. Coli, E. Carotovora and C. Flaccumfaciens.     

共价键连卟啉-富勒烯化合物的合成与表征

The covalently linked porphyrin-fullerene dyads were synthesized. The ligand 5-[4′-(4″-Phenoxybutoxy)phenyl]-N-(2-methyl)fulleropyrrolidine-10,15,20-tri-(p-methoxyphenyl)porphyrin (H₂P-C₆₀) was synthesized by 1,3 dipolar cycloaddition reaction with C₆₀, sarcosine and H₂P-CHO. The zinc porphyrin-fullerene was prepared by metalation of H₂P-C₆₀ and zinc acetate. The compounds were characterized by meams of IR, UV-Vis, ESI-MS, elemental analysis, and ¹H NMR.     

在Demko-Sharpless四唑合成反应中的一个意外的不同配位模式的铀配合物(英)

Under hydrothermal conditions, the reaction of UO₂(NO₃)₂·6H₂O with ligand 4-cyanopyridine N-oxide in the presence of NaN₃ affords one complex, {[(POTZ)₂(H₂O)₃(UO₂)](H₂O) (1) (POTZ=4-tetrazolyl pyridine N-oxide), which is another example of a pyridine N-oxide complex of uranium and exhibit strong green fluorescent emission at room temperature. The structure was determined by single crystal X-ray diffraction. Crystal data: P2₁/m, a=0.664 16(10) nm, b=2.104 1(3) nm, c=0.683 29(10) nm, β=93.295(3)°, V=0.953 3(2) nm³, Z=2, R₁=0.033 7, wR₂=0.083 3. CCDC: 241841.     

二维铅配合物[Pb2(C8H4O4)2(C19H12N4O)2]n·3.5nH2O的水热合成、晶体结构与荧光性质研究

In the title compound, [Pb₂(C₈H₄O₄)₂(C₁₉H₁₂N₄O)₂]_n·3.5nH₂O(1), has been synthesized by the hydrothermal assembly of 1,4-benzenedicarboxylate and 4-(1H-1,3,7,8-tetraazacyclopenta[l]-phenanthren-2-yl)phenol(TCPP) with lead acetate. Elemental analysis, X-ray crystal structure analysis, IR spectrum, thermogravimetric analysis and luminescence property were carried out for the structural determination and characterization of the title compound. Compound 1 crystallizes in triclinic, space group P1 with a=1.013 54(10) nm, b=1.104 84(11) nm, c=1.210 05(12) nm, α=76.812 0(10)°, β=74.814 0(10)°, γ=86.030 0(10)°, V=1.273 1(2) nm³, Pb₂C₅₄H₃₉N₈O_13.5, M_r=1 430.31, Z=1, D_c=1.866 g·cm^-3, μ=6.680 mm^-1, F(000)=691, R=0.027 3 and wR=0.068 7 for 4 042 observed reflections (I>2σ(I)). The compound 1 exhibits two-dimensional network structures, which are further stacked through π-π interactions and hydrogen bonds to form three-dimensional supramolecular polymer. Solid-state luminescent spectrum of the compound 1 indicates intense fluorescent emission. CCDC: 748883.     

烷基钴肟及其β-环糊精包结物水溶液中氨取代反应平衡常数测定

The axial coordinate water substitution reactions of alkylaquacobaloximes (alkyl=n-C₃H₇, n-C₄H₉, i-C₄H₉, n-C₅H₁₁, Br(CH₂)₃, PhCH₂) by ammonia in aqueous solution were studied in the absence and presence of β-cyclodextrin (β-CD). The equilibrium constants were measured by UV-vis spectroscopy. It has been found that (i) comparing with that in the absence of β-CD, the equilibrium constant were influenced slightly in the presence of β-CD, (ii) with increasing electron-withdrawing ability of the alkyl groups, the equilibrium constants were increased.     

3-甲基-4-对甲基苯基-5-(2-吡啶基)-1，2，4-三唑双核铜(Ⅱ)配合物的合成、晶体结构及磁性

A dinuclear Cu(Ⅱ) complex [Cu₂(MMBPT)₂Cl₄(H₂O)_2.5] (I) [MMBPT=3-Methyl-4-(4-Methylphenyl)-5-(2-pyridyl)-1,2,4-triazole] was synthesized by reaction of MMBPT with CuCl₂·2H₂O and its structure was determined by X-ray crystal structure analysis. The structure indicates that the complex crystallizes in monoclinic, space group P2₁/c with a=1.273 4(3) nm, b=1.237 5(3) nm, c=2.403 2(5) nm, β=90.51(3)°. V=3.786 6(13) nm³, Z=2, D_c=1.429 Mg·m^-3, μ=1.445 mm^-1, F(000)=1 660, and final R₁=0.055 5, wR₂=0.129 7. The crystal structure shows that the dinuclear Cu₂N₆ unit is almost planar in which each Cu(Ⅱ) ion was five-coordinated by one nitrogen atoms from MMBPT and two chlorine in the basal positions and two nitrogen atoms from two MMBPTs respectively in the axial one, to form a distorted trigonal bipyramidal geometry. Magnetic measurements reveal a relatively strong antiferromagentic interaction in the complex. CCDC: 720011.     

铜二取代三元杂多化合物的制备、晶体结构和性质

The half Dawson structure complex has been prepared by reaction of Na₂WO₄·2H₂O, Na₂MoO₄·2H₂O and NaH₂PO₄ in water. [TBA]₄H₃[PW₆Mo₄Cu₂O₃₈(H₂O)₂] have been synthesized by reaction of [PW₅Mo₄O₃₄]^9- and Cu²⁺ in water and recrystallized in a mixed acetone/water solvent. They were characterized by elemental analyses, IR spectra and electronic spectra. The crystal structure of [TBA]₄H₃[PW₆Mo₄Cu₂O₃₈(H₂O)₂] has been determined by X-ray structure analysis for the first time, which belongs to trigonal with space group R-3, a=b=c=1.53081 (18) nm, α=β=γ=109.458(17)°, Z=1, D_c=3.141Mg·m^-3, R=0.0780, R_w=0.1480. The sites of the molybdenum, tungsten and copper atoms are disordered over 12 possible locations in the crystal, and the anion has a high symmetry due to the disorder of the molybdenum, tungsten and copper atoms. CCDC: 176656.     

Brφnsted acidic ionic liquid catalyzed highly efficient synthesis of chromeno pyrimidinone derivatives and their antimicrobial activity

A series of 8,9-dihydro-2-(2-oxo-2H-chromen-3-yl)-5-aryl-3/f-chromeno[2,3-(flpyrimidine-4,6(5ff,7//)-diones(5a-j) have been synthesized by the reaction of 2-amino-5,6,7,8-tetrahydro-5-oxo-4-aryl-4#-chromene-3-carbonitrile(4a-j) with couma-rin -3-catboxylic acid under neat conditions employing Br0nsted acidic ionic liquid(4-sulfobutyl)tris(4-sulfophenyl)phosphonium hydrogen sulfate as catalyst.Structures of all the compounds were established on the basis of analytical and spectroscopic data.All the compounds were evaluated for their in vitro antimicrobial activity against different bacterial and fungal strains.     

具有强绿色荧光发射效应的2，2′-二硝基4，4′-联苯酸铀(Ⅵ)配聚物

A very complex 3D Uranium(Ⅵ) metal-organic framework was obtained by the hydrothermal treatment of UO₂(NO₃)₂·6H₂O with (R，S)-2，2′-dinitro-biphenyl- 4，4′-dicarboxylic acid (BTNCA) (L) in water at 180 ℃ in Pyrex tubes. The crystal belongs to monoclinic system with space group P2₁/c， and a=0.545 90(3) nm， b=3.676 01(18) nm， c=2.659 81(13) nm， β=91.4060(10)°， V=5.335 9(5) nm³， Z=4. CCDC: 659615.     

一种含阻转异构体的二羧酸铀(Ⅵ)有机-金属配合物

Uranium(Ⅵ) complex [UO₂((R，S)-1，1′-binaphthylene-2，2′-dicarboxylate)(H₂O)] was obtained by the hydrothermal treatment of UO₂(NO₃)₂·6H₂O with (R，S)-1，1′-binaphthylene-2，2′-dicarboxylic acid(BCA) (L) in water at 180 ℃ in Pyrex tube. The crystal belongs to monoclinic system， space group C2/c， with a=1.640 3(3) nm， b=1.196 7(2) nm， c=1.066 3(17) nm， β=104.412(4)°， V=2.027 2(6) nm³， Z=4. CCDC: 659617.     

二维网状铜(Ⅱ)配位聚合物{Cu(μ2-C10H8N2O3)( μ2-C6H12N4)1/2}n的合成和晶体结构

The novel copper(Ⅱ) coordination polymer with 2-oxo-propionic acid benzoyl hydrazone and hexamethylenetetramine ligands, {Cu(μ₂-C₁₀H₈N₂O₃)( μ₂-C₆H₁₂N₄)_1/2}_n (C₁₀H₈N₂O₃^2- is the dinegative ion of 2-oxo-propionicacid benzoyl hydrazone), has been synthesized and characterized by elemental analysis and IR spectroscopy. The crystal structure was determined by single crystal X-ray diffraction analysis. The results show that the crystal of the title coordination polymer belongs to monoclinic space group C2/c, the cell parameters are as follows: a=1.787 5(2) nm, b=0.730 93(9) nm, c=2.038 2(2) nm, β=92.890(2)°, and V=2.659 6(5) nm³, Z=8, D_c=1.687 Mg·m^-3, μ(Mo Kα)=1.659 mm^-1, F(000)=1 384, R=0.031 1, wR=0.079 0 for 2 454 observed reflections (I>2σ(I)) out of 2887 unique reflections. In this copper(Ⅱ) coordination polymer, each copper(Ⅱ) ion is five-coordinated with a geometry of distorted square-pyramid. Two oxygen atoms of the carboxyl of each C₁₀H₈N₂O₃^2- acts as a bridge to bond two neighboring copper(Ⅱ) ions, leading to an infinite one-dimensional chainlike coordination polymer. Each chain is linked by coordinated hexamethylenetetramines with its neighbors to form an infinite two-dimensional network structure. CCDC: 255347.     

桥联双核配合物[(DPC)2Co2(H2O)5]·2H2O的合成与晶体结构

The new complex formulated [(DPC)₂Co₂(H₂O)₅]·2H₂O (HDPC^- is pyridine-2,6-dicarboxylate) has been synthesized and the crystal structure was determined by X-ray diffraction. The crystal structure of the complex belongs to monoclinic system with space group P2₁/c, a=0.83850(10) nm, b=2.7386(4) nm, c=0.9610(2) nm, β=98.280 (10) °, V=2.1838(6) nm³, Z=4, D_c=1.746 g·cm^-3, μ=1.597 mm^-1. In the crystal the two Co²⁺ are in distorted octahedrons. The part of [Co(DPC)₂] possess an approximate D_2d symmetry, while the part of [OCo₍₂₎(OH₂)₅] has an approximate C₂ symmetry.     

L-苏糖酸锰的制备及标准生成焓

The pink powder of manganese L-threonate was obtained by extracting with alcohol the concentrated solution derived from the reaction between L-threonic acid solution prepared by double decomposition reaction of calcium L-threonate with oxalic acid and superfluous manganese oxide at 80℃ for certain time. The composition of the new compound was determined by chemical and elemental analyses and its formula fits Mn(C₄H₇O₅)₂·H₂O, the IR spectra indicated that Mn²⁺ in the compound coordinates to oxygen atom of the carboxyl group, while the proton of the carboxyl group is dissociated, it was assumed that the coordination number of Mn²⁺ was 4. The results of TG-DTG showed that the compound have fairish stability, the intermediate and final product of the thermal de-composition of the compound are Mn(C₄H₇O₅)₂ and MnO₂, respectively. The constant volume combustion energy of the compound, Δ_cE, were determined by a precise rotating-bomb calorimeter at 298.15K, it was (-3384.30±1.21)kJ·mol^-1, its standard enthalpy of Combustion,Δ_cH_m^?,and standard enthalpy of formation,Δ_fH_m^? , were calculated. They are (-3383.07±1.21)kJ·mol^-1 and (-2 571.68±1.63)kJ·mol^-1, respectively.     

(NH2CH2CH2NH3)4[WⅤO2(OC6H4O)2]2(NH3CH2CH2NH3)·H2O的合成、晶体结构、EPR以及与同构物的比较

Cis-dioxo-catecholatotungsten(Ⅴ) complex (NH₂CH₂CH₂NH₃)₄[W^ⅤO₂(OC₆H₄O)₂]₂(NH₃CH₂CH₂NH₃)·H₂O (1) was synthesized at room temperature by the reaction of tetrabutyl ammonium decatungstate with catechol in the mixed solvent of CH₃OH, CH₃CN and NH₂CH₂CH₂NH₂. The crystal structure of complex was determined by X-ray diffraction structural analysis. The results show that complex belongs to monoclinic system with space group P2₁/c,a=0.712 8(3) nm, b=3.082 3(11) nm, c=0.982 8(4) nm, β=102.639(6)°, V=2.106 8(14) nm³, Z=2, R₁=0.062 8, wR₂=0.183 7. Compared the complex with its analogous complexes (NH₂CH₂CH₂NH₃)₃[Mo^ⅤO₂(OC₆H₄O)₂], it is found that the coordination structure of W have no changes in the processing of electron transfer of tungsten-containing enzymes from the result of the similarity of the EPR spectra of the complexes and flavoenzyme from milk. CCDC: 272937.     

6，6′-二硝基-2，2′-联苯酸铀(Ⅵ)配聚物

Uranium(Ⅵ) complex {[UO₂((R，S)-1，1′-biphenyl-6，6′-dinitro-2，2′-dicarboxylate)(H₂O)](H₂O)} was obtained by the hydrothermal treatment of UO₂(NO₃)₂·6H₂O with (R，S)-6，6′-dinitro-biphenyl-2，2′-dicarboxylic acid(BSNCA) (L) in water at 180 ℃ in Pyrex tube. The crystal belongs to triclinic system， space group P1， with a=0.903 45(14) nm， b=1.024 43(16) nm， c=1.058 95(16) nm， α=90.411(3)°， β=112.934(3)°， γ=92.554(3)°. CCDC: 659613.     

超分子钴(Ⅱ)配合物[CoL(H2O)2]n的合成与结构表征

A mononuclear Cobalt(Ⅱ) complex [CoL(H₂O)₂]_n (H₂L: 4,4′,6,6′-Tetrabromo-2,2′-[ethylenedioxybis(nitrilomethylidyne)]diphenol), has been synthesized and structurally characterized by elemental analysis, IR and X-ray diffraction single crystal structure analysis. The crystal of the complex belongs to monoclinic space group P2₁/c with a=2.516 8(3) nm, b=1.023 43(18) nm, c=0.789 17(14) nm, β=91.375(2)°, V=2.032 1(5) nm³, Z=4, D_c=2.317 Mg·m^-3, μ(Mo Kα)=8.747 mm^-1, F(000)=1 356, R₁=0.049 7, wR₂=0.110 4. The crystal structure of [CoL(H₂O)₂]_n indicates that the complex consists of one cobalt(Ⅱ) atom, one L^2- unit and two coordinated water molecules, and the coordination number of the cobalt(Ⅱ) atom is six. One-dimensional chain supramolecular structure is formed by intermolecular hydrogen bonds and π-π stacking of neighboring benzene rings. CCDC: 652649.     

氢氧化锌合苯甲酸层状化合物的水热合成与表征

The organic-inorganic layered compound zinc hydroxide-benzoic acid with basal spacing of 1.92 nm was synthesized hydrothermally using amorphous Zn(OH)₂ and benzoic acid at the reaction temperature of 90～130 ℃, the molar ratio of C₆H₅COOH/Zn(Containing 6 mmol of Zn) of 0.4～0.6, 20 mL H₂O and the reaction time of 6 h. The character, structure, particle morphology and chemical composition of the layered compound were characterized by means of XRD, TG-DTA, SEM, TEM and elemental analysis. The results indicate that the layered compound is of plate-like morphology and that with the temperature raising of hydrothermal synthesis, the particle of plate-like piece becomes smaller. The chemical formula of the layered compound could be written as Zn(OH)_2-y·(C₆H₅COO)_y·0.3H₂O, 0.36≤y≤0.54.     

反相微乳液法合成SrTiO3纳米棒

SrTiO₃ nanorods were synthesized in cetanyl trimethyl ammonium bromide (CTAB) reverse microemulsion containing CTAB, n-hexanol, n-octane and water with Ba(OH)₂ as reactants. The effects of different conditions such as ω₀ [ω₀=n_H2O/ n_CTAB], aging time and the concentration of reactants on the formation of the nanorods were studied. Transmission electron microscope (TEM), electron diffraction (ED) and X-ray diffraction(XRD)were used to characterize the morphology and the structure of the synthesized nanorods. The results show that SrTiO₃ nanorods with a length of 260～2 000 nm and a diameter of 50～100 nm belonging to single crystal are single cubic system. The molar ratio of Sr to Ti of products is 1.0 as determinded by ICP.