Synthesis of a new donor, BEDT-HBDST and crystal structures, electrical and magnetic properties of (BEDT-HBDST)2MX4 (M=Fe, Ga, X=Cl, Br), where BEDT-HBDST=2,5-bis(4,5-ethylenedithio-1,3-diselenol-2-ylidene)-2,3,4,5-tetrahydrothiophene

A novel conjugation-elongated bis(ethylenedithio)tetraselenafulvalene (BETS) type donor, 2,5-bis(4,5-ethylenedithio-1,3-diselenol-2-ylidene)-2,3,4,5-tetrahydrothiophene (BEDT-HBDST) and its magnetic and non-magnetic anion salts, (BEDT-HBDST)₂MX₄ (MX₄⁻=FeCl₄⁻, GaCl₄⁻, FeBr₄⁻ and GaBr₄⁻), were prepared. These four salts are isostructural and belong to the space group of P2/c. They showed semiconducting behavior with small activation energies (59-64 meV). The band structures of these salts are quasi one-dimensional and there is a midgap between the upper band and the lower band, since the degree of dimerization is significant in the stacking direction. The MX₄⁻ ions are located between the donor columns and near to the ethylenedithio moieties of the donor molecules. The magnetic susceptibilities of the FeCl₄⁻ and FeBr₄⁻ salts follow the Curie-Weiss law with Curie constants of 4.6 and 4.8 emu K mol⁻¹ (sum of the spins of S=5/2 and S=1/2) and negative Weiss temperatures of θ=−1.2 and −4.9 K, respectively, revealing a weak antiferromagnetic interaction of 3d spins of the FeCl₄⁻ and FeBr₄⁻ anions. The Fe?Fe (6.66-7.60 Å), Cl?Cl (4.81-4.82 Å) and Br?Br (4.74-4.77 Å) distances in the crystal structures of these salts are significantly long. Therefore, the direct magnetic interaction between the 3d spins of the nearest neighboring Fe³⁺ ions appears to be not readily accessible.     

Synthesis and Crystal Structure of 5-Amino-4-cyano-8-isobutyl-7-isopropyl-6-thiocarbamoyl-2-azabicyclo[2.2.2]oct-5-en-3-thione

5-Amino-4-cyano-8-isobutyl-7-isopropyl-6-thiocarbamoyl-2-azabicyclo[2.2.2]oct-5-en-3-thione was synthesized by the condensation of isovaleryl aldehyde with cyanothioacetamide. The structure of the product was established by X-ray crystallography.     

Cation recognition by new diester- and diamide-calix[4]arenediquinones and a diamide-benzo-15-crown-5-calix[4]arene

The synthesis, metal, ammonium and alkyl ammonium cation coordination chemistry and electrochemical recognition studies of new diester-and diamide-calix[4]arenediquinone receptors are described. In addition the synthesis and coordination properties of a novel diamide benzo-15-crown-5-calix[4]arene molecule is reported.This paper is dedicated to the commemorative issue on the 50th anniversary of calixarenes.     

Solar Photocatalytic Degradation of 4‐Chlorophenol in Kaolinite Catalysts

This research applies semiconductor photocatalysts, which are formed by metal ion exchange on the surface of kaolinite catalyst with cations, to the study of photocatalytic degradation of 4‐chlorophenol. The analysis results of catalyst properties shows that, after sintering at 400 °C, kaolinite catalyst has a particle size of between 10–100 nm indicating the nano level of synthesized catalysts. Under the same condition, kaolinite‐Ag/Zn catalyst works better in degradation efficiency than single kaolinite‐Ag and kaolinite‐Zn catalysts. Kaolinite‐Zn catalyst declines in degradation efficacy after 150 minutes and performs poorer than the other three types of kaolinite catalysts. In the experiments of different amounts of catalysts, when the concentration exceeds 0.1 wt%, utilization of light energy and degradation efficiency will be reduced due to shielding effect. When at different pH values, the higher the pH value, the more OH‐will be released and that is beneficial for reaction with substances and the increase of reaction rate. Finally multivariate analysis proves that there is one determining factor that influences the photocatalytic degradation of 4‐chlorophenol in kaolinite catalysts, named as “the factor with intermediates competition degree,” the one affecting the 4‐CP degradation at different weight percentages that is referred to as the “shielding effect factor.”     

Preparation and Characterization of N-4-Nitrophenyl-L-prolinol Nanocrystals in Sol-Gel Matrices

Organic nanocrystals of N-4-nitrophenyl-l-prolinol (NPP) have been grown in sol-gel matrices prepared from silicon alkoxide precursors. Our process is based on the control of the nucleation and growth kinetics of the dye in the pores of dense gels. Nanocomposites gel-glasses are obtained with a high optical quality due to the small size of the nanocrystals (10-20 nm). Differential scanning calorimetry experiments evidenced clearly the melting point of NPP nanocrystals, which is registered 51°C above that of NPP powder. Micro-Raman and solid state NMR spectroscopies allowed us to demonstrate that our nanocrystallization process does not chemically modify NPP molecules. We specified also the nature of interactions existing between the NPP nanocrystals and the xerogels. These strong interactions, which explain the important increase of the melting point of the nanocrystals in comparison to the NPP powder, are hydrogen bonds between nitro groups of NPP and uncondensed silanol functions of the silicate network.     

3,4—亚甲二氧基苯甲酸锡酯的合成及表征

３，４－亚甲二氧基苯甲酸及其取代物与三苯基氢氧化锡或二丁基化锡反应合成了５个锡酯，通过元素分析，ＩＲ和＾１ＨＮＭＲ对其进行了表征。     

1─芳氧基乙酰基─4─苯甲酰氨基硫脲衍生物的合成及其生物活性研究

１─芳氧基乙酰基─４─苯甲酰氨基硫脲衍生物的合成及其生物活性研究魏太保，陈继畴（西北师范大学化学系，兰州，７３００７０）杨素铀，王秀春（西北师范大学生物系，兰州，７３００７０）关键词：１—芳氧基乙酰基—４—苯甲酰基氨基硫脲，相转移催化，合成，生物活性...     

The Reaction of 4-Formylsydnone with Nitroalkanes

Under various basic solutions and reaction durations, 3-substituted 4-formyIsydnones and nitroalkanes containing α-active hydrogen (e.g. nitromethane and nitroethane) are converted to β-nitroalcohols, nitroalkenes and dinitroalkanes. β-Nitroalcohols are obtained only by electrochemical reaction on an electrogenerated base (EGB). The mechanism of overall reaction steps in particular is discussed.     

新显色剂二溴硝基苯基重氮氨基偶氮苯的合成及与镉的显色反应的研究

作者合成了新显色剂2,6-二溴-4-硝基苯基重氮氨基偶氮苯(DBNDAA)。在pH8.5的硼砂-盐酸缓冲介质中,在Tween 80-SDBS存在下,该试剂与镉(Ⅱ)生成络合比为3:1的红色络合物,λ_(max)=500nm,ε_(500)=1.52×10~5L·mol~(-1)·cm~(-1)。镉量在0～28μg/25ml范围内遵守比耳定律。并测定了试剂的表观离解常数和络合物的表观不稳定常数。方法有良好的选择性。用该试剂测定了铝合金标样、环境水样及废水中的痕量镉,结果满意。