A New 3D Pb(Ⅱ) Coordination Polymer [Pb(L)]_n Based on a Long Flexible Octane-1,8-dicarboxylic Acid:Crystal Structure and Physical Properties

A new Pb（II）-based coordination polymer, [Pb（L）]n （1）, was hydrothermally synthesized and its structure was determined by single-crystal X-ray diffraction （H2L = octane- 1,8-dicarboxylic acid）. Compound 1 crystallizes in orthorhombic, space group Pnma with a = 32.061（4）, b = 7.2597（8）, c = 4.8084（5） A, V= 1119.2（2） A3, Z = 4, C10H1604Pb, Mr = 407.42, Dc = 2.418 g/cm3, F（000） = 760, μ（MoKa） = 15.066 mm-1, R = 0.0270 and wR = 0.0666. In 1, each Pb（II） cation is coordinated by six carboxylate oxygen atoms from four L2- anions. Each L2- anion bridges three Pb（ll） atoms in a μ3：η2：η1：η1 mode to form a 3D framework. The structure of 1 was characterized by IR spectrum and thermogravimetric analysis. Moreover, solid state luminescent property of 1 was also investigated.

Study on thermal decomposition kinetics of azobenzene-4,4′-dicarboxylic acid by using compensation parameter method and nonlinear fitting evaluation

Recently,azobenzene-4,4'-dicarboxylic acid(ADCA)has been produced gradually for use as an organic synthesis or pharmaceutical intermediate due to its eminent performance.With large quantities put into application in the future,the thermal stability of this substance during storage,transportation,and use will become quite important.Thus,in this work,the thermal decomposition behavior,thermal decomposition kinetics,and thermal hazard of ADCA were investigated.Experiments were conducted by using a SENSYS evo DSC device.A combination of differential iso-conversion method,compensation parameter method,and nonlinear fitting evaluation were also used to analyze thermal kinetics and mechanism of ADCA decomposition.The results show that when conversion rate α increases,the activation energies of ADCA's first and main decomposition peaks fall.The amount of heat released during decomposition varies between 182.46 and 231.16 J·g^(-1).The proposed kinetic equation is based on the Avrami-Erofeev model,which is consistent with the decomposition progress.Applying the Frank-Kamenetskii model,a calculated self-accelerating decomposition temperature of 287.0℃is obtained.

熊去氧胆酸联合常规西医治疗胆汁反流性胃炎合并幽门螺旋杆菌感染的疗效及对IL-8、PGE2的影响

目的探讨熊去氧胆酸联合常规西医治疗胆汁反流性胃炎(BRG)合并幽门螺旋杆菌(Hp)感染的疗效及对白细胞介素-8(IL-8)、PGE2(前列腺素E2)的影响。方法选取2019年5月—2021年5月巴彦淖尔市医院收治的100例Hp呼吸试验为阳性的BRG患者进行研究,应用随机数表法将其分为观察组与对照组,每组50例。对照组采取常规西医治疗(克拉霉素+奥美拉唑+阿莫西林),观察组在常规西医治疗基础上增加熊去氧胆酸素治疗,对比两组患者临床疗效,并应用酶联免疫吸附法检测治疗前后血清白细胞介素-8(IL-8)、PGE2(前列腺素E2)表达水平,对比胃泌素(GAS)、胃动素(MTL)、胆囊收缩素(CCK)表达水平以及不良反应情况。结果观察组治疗总有效率明显高于对照组,差异有统计学意义(P<0.05);治疗后两组患者血清IL-8水平降低,观察组低于对照组,PGE2水平升高,观察组高于对照组(P<0.05);治疗后两组患者血清CCK水平降低,观察组低于对照组,MTL、GAS水平升高,观察组高于对照组,差异有统计学意义(P<0.05);两组患者均无严重不良反应发生,且轻度不良反应比较,差异无统计学意义(P>0.05),但观察组Hp根除率高于对照组(P<0.05)。结论对胆汁反流性胃炎合并Hp感染患者在常规西医治疗的基础上增加熊去氧胆酸能够提升其临床疗效,降低患者炎症反应,提升胃动力,调节胃肠激素,提升Hp根除率,且安全性较高。

Extraction Equilibria of Trimellitic and [ 1,1′-Biphenyl]-2,2′-dicarboxylic Acid with 1-Octanol, 50%TBP, and 10%TRPO in Kerosene

To explore the feasibility of extracting aromatic acid products from oxidizing coal, two aromatic acids, trimellitic and [1,1′-biphenyl]-2,2′-dicarboxylic acid, were selected as the solutes, and the extraction equilibrium of the acids were studied with 1-octanol, 50% tributyl phosphate （TBP） in kerosene, and 10% trialkylphosphine oxide （TRPO） in kerosene. The results showed that the degree of extraction of [1,1′-biphenyl]-2,2′-dicarboxylic acid was larger than that of trimellitic acid for all of the solvent, and the extraction capacity with TRPO is more effective than the one with TBP. The extraction behavior of aromatic polyacid is different from that of carboxylic acid, and the reactive extraction function of aromatic acids with TBP and TRPO is not as effective as that of carboxylic acid. 1-octanol could be used to remove [1,1′-biphenyl]-2,2′-dicarboxylic acid from the mixture of trimellitic acid and [1,1′-biphenyl]-2,2′-dicarboxylic acid. Because the weak hydrogen bond association exists between -OH in 1-octanol and -COOH in aromatic acid, the extractive selectivity of [ 1, 1′-biphenyl]-2,2′-dicarboxylic to trimellitic acid depends on the stoichiometric ratio.

Synthesis,Crystal Structure and Magnetic Behavior of a New Manganese(Ⅱ) Coordination Polymer [Mn(DPPZ)(PZDC)(H_2O)] (DPPZ=Dipyrido[3,2-a:2',3'-c]-phenazine and H_2PZDC=Pyrazine-2,3-dicarboxylic Acid)

The title complex, [Mn（DPPZ）（PZDC）（H2O）] 1 （DPPZ = dipyrido[3,2 -a：2＇,3＇- c]phenazine and H2PZDC = pyrazine-2,3-dicarboxylic acid）, has been hydrothermally synthesized and structurally characterized by X-ray single-crystal diffraction, elemental analyses, IR, TG- DTA and magnetic susceptibility measurement. It crystallizes in triclinic, space group P1^- with a = 6.6842（5）, b = 7.5741（6）, c = 20.5755（15）A, α = 90.1160（10）, β = 97.0560（10）, γ = 97.3350（10）°, V= 1025.16（13）A^3, Z = 2, MnC24H14N6O5, Mr= 521.35, Dc= 1.689 g/cm^3, F（000） = 530, μ（MoKa） = 0.699 mm^-1, R = 0.0366 and wR = 0.0810. Compound 1 contains one- dimensional chains which are further stacked through π-π interactions to form a 3D supramolecular architecture. The water molecule O（1W） is involved in hydrogen bonding interactions with symmetric carboxylate oxygen atom 0（4） at （x＋ 1, y＋1, z） and symmetric PZDC nitrogen atom N（6） at （1-x, 1-y, 1-z）, which completes the structure of 1. Magnetic susceptibility measurement indicates that the compound behaves a weak antiferromagnetic exchange interaction.

Synthesis,Crystal Structure and Theoretical Calculations of a Zinc(Ⅱ) Coordination Polymer Assembled by Pyrazine-2,3-dicarboxylic Acid and Bis(imidazol) Ligands

A new metal-organic coordination polymer [Zn（pzdc）（mbix）]n·nH2O（H2pzdc = pyrazine-2,3- dicarboxylic acid, mbix = 1,3-bis（imidazol-1-ylmethyl）-benzene） 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Yellow crystals crystallize in monoclinic system, space group P21/n with a = 8.5519（6）, b = 14.8764（10）, c = 16.4108（11） A, β = 103.4520（10）o, V = 2030.5（2）A^3, C（20）H（18）N6O5Zn, Mr = 487.77, Dc = 1.596 g/cm^3, F（000） = 1000, Z = 4, μ（MoK α） = 1.257 mm^-1, the final R = 0.0260 and w R = 0.0706 for 3445 observed reflections（I 〉 2σ（I））. The structure of 1 exhibits a one-dimensional chain-like structure. In addition, natural bond orbital（NBO） analysis was performed by the PBE0/LANL2DZ method in Gaussian 03 Program. The calculation results show obvious covalent interaction between the coordinated atoms and Zn（Ⅱ） ion.

亚油酸诱导植物乳杆菌p-8产生共轭亚油酸的蛋白组和类组蛋白乙酰化分析

研究亚油酸(linoleic acid,LA)诱导下植物乳杆菌(Lactobacillus plantarum)p-8的蛋白组和类组蛋白乙酰化水平差异,探究共轭亚油酸(conjugated linoleic acid,CLA)产生的机制。结果表明,LA的最佳诱导质量浓度为1 mg/mL,在此质量浓度条件下,蛋白质组学分析发现,烯酰-酰基载体蛋白还原酶、酰基载体蛋白等脂肪酸合成的关键蛋白因子下调,脂肪酸合成下调,乙酰基转移酶水平上调。Western blot结合体外添加NaAc实验表明,乙酰辅酶A含量增加导致类组蛋白乙酰化水平提升。实时聚合酶链式反应检测显示,添加LA和NaAc使CLA相关酶、转录调控因子和Sigma因子的mRNA表达升高,CLA含量也提高。相关性分析得出,乙酰辅酶A与LA水合酶转录水平和CLA含量之间呈显著正相关,揭示乙酰辅酶A和乙酰基转移酶含量上调导致类组蛋白乙酰化加强而上调CLA合成。结果为分子改良或科学调控乳酸菌以提高CLA转化率奠定了基础。

Low-temperature heat capacities and standard molar enthalpy of formation of pyridine-2,6-dicarboxylic acid

This paper reports that the low-temperature heat capacities of pyridine-2,6-dicarboxylic acid were measured by a precision automatic calorimeter over a temperature range from 78 K to 380 K. A polynomial equation of heat capacities as a function of temperature was fitted by the least-squares method. Based on the fitted polynomial, the smoothed heat capacities and thermodynamic functions of the compound relative to the standard reference temperature 298.15 K were calculated and tabulated at intervals of 5 K. The constant-volume energy of combustion of the compound was determined by means of a precision rotating-bomb combustion calorimeter. The standard molar enthalpy of combustion of the compound was derived from the constant-volume energy of combustion. The standard molar enthalpy of formation of the compound was calculated from a combination of the datum of the standard molar enthalpy of combustion of the compound with other auxiliary thermodynamic quantities through a Hess thermochemical cycle.

Crystal Structure and Theoretical Studies of Tetrahytrate(1-H-1,2,4-triazole-3,5-dicarboxylicacid)nickel

A new compound, [Ni（Hdctrz）（H2O）4]（1, H3dctrz = 1-H-1,2,4-triazole-3,5-dicarboxylic acid）, has been successfully synthesized via slow evaporation. The structure of 1 was characterized by FT-IR, elemental analysis and single-crystal X-ray diffraction. Compound 1 crystallizes in monoclinic, space group P21/c with a = 6.871（1）, b = 11.468（1）, c = 12.178（1） A, b = 101.291（1）o, V = 941.01（16） A3, Z = 4, C4H9N3O8Ni, Mr = 285.85, Dc = 2.018 g·cm–3, m = 2.10 mm–1, F（000） = 584, GOOF = 1.025, the final R = 0.0515 and wR = 0.2125 for 1404 observed reflections（I 〉 2s（I））. The crystal structure is assembled by a slightly distorted {NiNO5} octahedral geometry and hydrogen bonds viz. N–H…O, O–H…O, C–O…π and π···π weak interactions. A rare π···π interaction from triazolate and carboxylate is affirmed through the molecular orbitals（MO） of three adjacent Ni CN molecules. The 3D Hirshfeld surface analysis was employed to gain additional insight into the interactions responsible for the packing of compound 1. Quantitative examination of 2D fingerprint plots revealed, amongst others, the dominating participation of O···H, N···H and π···π interactions in the molecular packing.

A Lanthanide-transition Metal Coordination Polymer:{[CuEu(Hbidc)_2(H_2O)_4]·H_2O}_n(H_3bidc=1H-benzimidazole-5,6-dicarboxylic Acid)

The title complex 1,{[CuEu（Hbidc）2（H2O）4]·H2O}n（H3bidc = 1H-benzimidazole-5,6-dicarboxylic acid）,has been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction.Complex 1 crystallizes in triclinic,space group P1,with a = 7.791（2）,b = 12.058（3）,c = 12.109（3）,α = 82.189（5）,β = 72.407（5）,γ = 89.184（4）°,V = 1073.7（5）3,C18H18CuEuN4O13,Mr = 713.86,Dc = 2.208 g/cm3,μ（MoKα） = 3.967 mm-1,F（000） = 700,GOOF = 0.950,Z = 2,the final R = 0.0531 and wR = 0.1068 for I 2σ（I）.Complex 1 possess a tape-like chain structure consisting of Eu2C8O4 and Cu2Eu2C18N4O4 metallic rings alternatively arranged and is the first 3d-4f heterometallic complex based on the 1H-ben-zimidazole-5,6-dicarboxylato ligand（Hbidc）.Plenty of hydrogen-bonding and π...π stacking interactions connect the 1D chains to construct a 3D supramolecular architecture.

Synthesis, Structure and Fluorescence Properties of Tb(Ⅲ) Complex with Isonicotinic Acid and Biphenyl-2,2′-Dicarboxylic Acid

Terbium perchlorate reacted with isonicotinic acid （Hpya） and biphenyl-2,2＇-dicarboxylic acid （H2dpa） under hydrothermal condition, a new ternary terbium complex [ Tb （pya） （dpa） （H2O） n （ 1 ） was synthesized. The structure of the ternary complex was determined by X-ray single crystal diffraction and characterized by elemental analysis, fluorescence measurement. The fluorescence spectrum shows the title complex emits strong green light. The crystal data for the com- plex： monoclinic, P21/n space group, a =0.8908（5）nm, b = 1.0569（6）nm, c =2.0969（11）nm, β = 98.446（8）°, V = 1.9528（18） nm^3, Z = 4, R = 0.0241, wR2 = 0.0534. The center Tb3＋ ion is eight coordinated. The coordination polyhedron around Tb3 ＋ ion can be described as a distorted square antiprism. The complex forms an infinite one-dimenand sional alternating chain polymer by bridging carboxyl groups of pyadpa.

The Synthesis of Pyridine 2,6-dicarboxylic Acid Using Microwave Irradiation

This research took 2,6-dimethylpyridine as raw materials under microwave irradiation to syntheses pyridine 2,6-dicarboxylic acid by adding oxidation potassium permanganate. However, there are lots of factors affecting the yield including the amount of potassium permanganate and sulfuric acid, reaction time, power, 2,6-dimethylpyridine dosage. We made the further research, using orthogonal experiment to find the optimal process conditions. Thus our research changed the synthesis process from a traditional method to a new type of microwave technology.

A Benzimidazole-pyridine-2,3-dicarboxylic Acid Bridged Zinc(Ⅱ)Coordination Complex–crystal Structure,Quantum Chemistry and Luminescence

The structure of a zinc（Ⅱ） coordination complex（1）, [C14 H10 N3 O5 Zn1.5]n or [Zn1.5（bzim）（pydc）（H2 O）]n（H2 pydc = pyridine-2,3-dicarboxylic acid, Hbzim = benzimidazole）, has been determined by X-ray crystallography and characterized by elemental analysis, IR spectrum and luminescence. Chemical formula： C14 H10 N3 O5 Zn1.5. It crystallizes in the monoclinic system, space group P21/c with a = 12.303（4）, b = 12.052（4）, c = 10.212（3） ？, β = 104.147（4）, V = 1468.3（8） ？3, Z = 4, Mr = 398.30, Dc = 1.802 g/cm3, F（000） = 800, μ = 2.501 mm-1 and S = 1.000. The 2-D network architecture of 1 is constructed from benzimidazole, zinc and pyridine-2,3-dicarboxylic acid. The quantum-chemical calculations have been performed on ‘molecular fragments’ extracted from the crystal structure using the B3 LYP method in Gaussian 09. The luminescence spectrum shows that complex 1 emits blue luminescence.

Synthesis of 3 or 4-Substituted Pyridine-2, 6-Dicarboxylic Acid

Various 4-alkoxypyridine-2, 6-dicarboxylic acids were synthesized starting from 2, 6- lutidine. Through aldol condensation and Michael addition, various 4-arylpyridine-2, 6-dicarboxylic acids were synthesized starting from aromatic aldehydes and 2-acetylfuran.

Syntheses, Crystal Structures, and Properties of Two New Lanthanide Coordination Polymers Constructed from Benzimidazole-5,6-dicarboxylic Acid

Two lanthanide coordination polymers, {[Ln（Hbidc）（bidc）（H2 O）3]·3 H2 O}n（H3 bidc = benzimidazole-5,6-dicarboxylic acid, Ln = Eu（1）, Sm（2）） have been hydrothermally synthesized. Both compounds are isostructure and crystallize in the P21/c space group of monoclinic system. Complex 1: a = 11.087（6）, b = 8.972（5）, c = 23.064（13） ?, b = 95.027（5）o, V = 2285.4（2） ?3, Z = 4, Mr = 669.35, Dc = 1.945 g/cm3, F（000） = 1328, S = 1.044, μ = 2.827 mm-1, R = 0.0393 and wR = 0.0801 for 3458 observed reflections（I > 2s（I））. Complex 2: a = 11.087（6）, b = 8.972（5）, c = 23.064（13） ?, b = 95.027（5）°, V = 2285.4（2） ?3, Z = 4, Mr = 667.74, Dc = 1.941 g/cm3, F（000） = 1324, S = 1.071, μ = 2.652 mm-1, R = 0.0329 and wR = 0.0809 for 3744 observed reflections（I > 2s（I））. Complexes 1 and 2 have been determined by single-crystal X-ray diffraction analyses and further characterized by elemental analyses, IR spectroscopy, and thermogravimetric analyses（TGA）. The single-crystal X-ray diffraction analysis reveals that complexes 1 and 2 are the isostructural 1 D zigzag chain structures, which are further extended into a 3 D supramolecular structure through hydrogen bonds and p···p stacking interactions. Furthermore, the thermal stability, UV-vis absorption spectra and fluorescent properties of complexes 1 and 2 have been investigated and discussed in detail.

Synthesis and fluorescence properties of Tb(Ⅲ) complexes with pyridine-2,6-dicarboxylic acid derivatives

Two novel ligands named 4-styrylpyridine-2,6-dicarboxylic acid (4-SPDA) and 4-(4-(2-(2, 6-dicarboxypyridin-4-yl)- vinyl)styryl)pyridine-2,6-dicarboxylic acid(DSPDA) and their complexes with Tb(Ⅲ) were synthesized and characterized by infrared spectrometry, 1H nuclear magnetic resonance, elemental analysis and gas chromatograph-mass spectrometry. The ligand synthetic route was optimized. The fluorescence properties of the complex in solid state, in different kind of solvents and in solutions with different pH values were investigated in detail. The results show that the yields of DSPDA and 4-SPDA reach over 78% by Wittig-Horner reaction and other eight pyridine-2, 6-dicarboxylic acid derivatives with different substituents on pyridine ring, and their complexes with Tb(Ⅲ) are also obtained. The fluorescence intensities of the complexes with electron-donating groups are more intense than those of the complexes with electron-withdrawing groups on pyridine ring; fluorescence intensities of the complexes are the strongest in neutral solution (pH=7), and the less the dipole moment of solvent molecule is, the stronger the fluorescence intensity is. It is found that the two ligands (4-APDA and DSPDA) are the good sensitizers for Tb(Ⅲ) ion.

Synthesis and Structural Characterization of a New Cadmium(Ⅱ) Complex Bridged by Endo-norbornene-cis-5,6-dicarboxylic Acid

A polynuclear complex [Cd（endc）（H20）]n·nH2O （endc = endo-norbornene-cis- 5,6-dicarboxylate anion） has been synthesized by the hydrothermal reaction of cadmium nitrate tetrahydrate with endo-norbornene-cis-5,6-dicarboxylic acid in 1：1 molar ratio, and structurally characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/c with α = 1.16471（7）, b = 0.95334（7）, c = 0.91109（9） nm, Z= 4, V= 1.01035（14） nm^3, D, = 2.160 g/cm^3,μ = 2.172 mm^-1, F（000） = 648, R = 0.0302 and wR = 0.0752. According to structural analysis, each Cd（II） ion is coordinated to six O atoms from three endc anions and one water molecule, giving a distorted octahedral geometry. Two- dimensional layer arrangement of the title complex is constructed from the bridging nature of endc. It is worth notice that adjacent two-dimensional layers are joined together to form a three-dimensional supramolecular framework via intermolecular hydrogen bonding interactions.

Synthesis and Crystal Structure of Palladium(Ⅱ) Complex with 2,2’-Bipyridine-3,3’-dicarboxylic Acid

The title complex Pd（H2BDA）Cl2·2DMSO （C16H14Cl2N2O6PdS2, H2BDA = 2,2＇- bipyridine-3,3＇-dicarboxylic acid） has been synthesized and characterized by IR spectra, elemental analysis and ^1H NMR spectra. Its structure was determined by single-crystal X-ray diffraction analysis. The complex crystallizes in the monoclinic system, space group P2（1/c） with a = 1.3604（6）, b = 1.2606（6）, c = 1.3521 （6） nm, β = 103.677（7）°, V = 2.2530（17） nm^3, Mr = 571.75, Z = 4, Dc = 1.686 g/cm^3,μ = 1.280 mm^-1, F（000） = 1136, R= 0.0405 and wR= 0.0908. The complex presents a planar quadrangle arrangement and is assembled via hydrogen bonds.

Hydrothermal Synthesis, Crystal Structure and Thermal Analyses of Pyrazine-2,3-dicarboxylic Acid Bridged Co(II) Coordination Polymer of _∞~2[Co(phen)(μ-L)_(3/3)]·H_2O (H_2L = Pyrazine-2,3-dicarboxylic Acid)

A novel pyrazine-2,3-dicarboxylic acid bridged Co(II) phen complex 2 ∞ [Co- (phen)(μ-L)3/3]?H2O (H2L = pyrazine-2,3-dicarboxylic acid) has been hydrothermally synthesized, and X-ray single-crystal diffraction analysis shows that it crystallizes in the monoclinic system, space group P21/n with a = 11.480(2), b = 11.885(2), c = 12.939(3) ?, β = 110.55(3)°, V = 1653.1(6) ?3, Mr = 423.25, Dc = 0.425 g/cm3, Z = 4, R = 0.0361 and wR = 0.1011. The title complex consists of 2D 2 ∞ [Co(phen)(μ-L)3/3] layers and crystal water molecules. Each Co atom is octahedrally coordinated by three N atoms and three O atoms to form 2D 2 ∞ [Co(phen)(μ-L)3/3] polymeric layers. Furthermore, such 2D layers are stacked into 3D supramolecular frameworks via Van der Waals’ intermolecular forces, strong and weak hydrogen-bond interactions. The coordination phen and crystal water molecules are resided into cavities of the frameworks.

8%盐酸脱钙液处理骨髓组织时长与染色效果的探索

目的探索8%盐酸脱钙液处理骨髓组织不同时长的染色效果。方法收集骨髓组织活检标本180例,利用8%盐酸脱钙液分别在70 min,90 min,110 min处理骨髓组织,观察不同脱钙处理时长的骨髓组织HE染色、免疫组织化学染色(EnVision法染TdT、CD56、MPO)和特殊染色(Gomori网状纤维染色)效果。结果8%盐酸脱钙液处理90 min与70 min和110 min相比,骨髓组织石蜡切片组织结构保持较完整,HE染色后形态结构清晰可辨,对比度较好,免疫组化染色定位准确、背景清楚,网状纤维染色粗细清晰可辨。结论8%盐酸脱钙液对骨髓组织90 min脱钙效果较好。