The synthesis and crystal structures of the first rare-earth alkaline-earth selenite chlorides MNd10(SeO3)12Cl8 (M=Ca and Sr)

Two new alkaline-earth Nd selenite chlorides MNd₁₀(SeO₃)₁₂Cl₈ (M=Ca, Sr) were obtained using crystal growth from alkaline-earth chloride melts in quartz tubes. These new compounds crystallize in the orthorhombic system in space group C cca (#68). The compounds were studied by energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction. It was shown that both compounds adopt the same structure type, constructed by complex [M₁₁(SeO₃)₁₂]⁸⁺ slabs separated by chloride anion layers perpendicular to the longest cell parameter. The SeO₃ groups show a pyramidal shape and may be described as SeO₃E tetrahedra. Such SeO₃ groups decorate the Nd-O skeletons forming the [M₁₁(SeO₃)₁₂]⁸⁺ slabs.     

膦取代的羰基铂簇的合成,结构和性质

Pt(PPh_3)_2Cl_2在碱性介质中,与一氧化碳直接进行还原及羰基化反应,得到五种膦取代的羰基铂配合物:Pt_5(μ_2-CO)_5(CO)(PPh_3)_4 1,Pt_3(μ_2-CO)_3(PPh_3)_3 2,Pt_3(μ_2-CO)_3(PPh_3)_4 3,Pt_4(μ_2-CO)_5(PPh_3)_4 4,以及Pt(Cl)(PPh_3)_2(COOCH_3) 5。经X-射线单晶衍射分析,确定了新的三核铂羰基簇2以及配合物5的分子结构。还讨论了1和5的生成机理。     

Zs－93硒剂对移植性小鼠S＿（180）肉瘤的抑制作用及其免疫活性

用硒与尿素化合，新生的由杂环有机硒所组成的Ｚｓ－９３硒剂治疗移植性Ｓ１８０肉瘤，有显著的抑瘤作用（Ｐ＜０．０１），其作用表现出一定的剂量效应，以５μｇ／只小鼠为最适，抑瘤率达６０．７６％，治疗组小鼠的Ｔ细胞、ＳＯＤ活性均有增强。     

Determination of 8[(3S)-3-amino-1-pyrrolidinyl]-1-cyclopropyl-7-fluoro-9-methyl-4-oxo-4H-quinolizine-3-carboxylic acid hydrochloride and related substances by high performance liquid chromatography

Summary The purity of the investigational antibacterial Abbott-086719.1 (I) which is 8[(3S)-3-amino-1-pyrrolidinyl]-1-cyclopropyl-7-fluoro-9-methyl-4-oxo-4H-quinolizine-3-carboxylic acid hydrochloride is determined using gradient elution HPLC. The chromatographic separation was optimized and the chromatographic parameters critical to separation are discussed in detail. Most acceptable separations were achieved using an Alltima C18 column (5 m) measuring 4.6 mm I.D.×15 cm with 0.01M–0.03M citrate eluents which were modified with acetonitrile or with mixtures of acetonitrile and methanol. Related substances in I were determinable to 0.05%. Repeatability (RSD values) for determining related substances at levels of 0.50 to 0.06% ranged from ±1.9 to ±10%. Determinations of I in 5% dextrose in water and in hydroxypropyl methylcellulose were made using the same column and a simple isocratic system. The determination of I was stability indicating with precision (RSD values) of ±0.5% to ±2.0% and good agreement with theory for formulations containing I at 1.0 to 95 mg/mL concentrations. Recoveries of I from the vehicles were quantitative and linearity of the detector response of I was demonstrated to at least 0.10 mg/mL.     

Dansyl-Modified γ-Cyclodextrin as a fluorescent sensor for molecular recognition

The crystal structure of thiamine iodide sesquihydrate has been determined by X-ray diffraction methods as a host-guest model for coenzyme-substrate interactions. The asymmetric unit contains two chemical units. Both the thiamine molecules A and B, which are crystallographically independent, assume the usualF conformation and have a disordered hydroxyethyl side chain. An iodide anion (or a water molecule) bridges the pyrimidine and thiazolium rings of molecule A (or B) by forming a hydrogen bond with the amino group and an electrostatic contact with the thiazolium ring to stabilize the molecular conformation. In the crystal the thiamine molecules self-associate to form a pipe-like polymeric structure, in which four thiamine hosts surround an iodide guest and hold it through C(2)-H...I hydrogen bonds and thiazolium...I electrostatic interactions. Crystal data: C₁₂H₁₇N₄OS⁺·I^– · 1.5 H₂O, monoclinic,P2₁/c, a=12.585(2), b=25.303(5), c=12.030(2) Å, =115.15(1)°,V=3468(1) ų,Z=8,D _c=1.606 g cm^–3,R=0.045 for 3328 observed reflections. Supplementary Data relating to this article are deposited with the British Library as Supplementary Publication No. SUP. 82156 (13 pages).     

Preparation of cellulose and cellulose derivative azo compounds

Wood pulp and cotton linter are the most common sources of cellulose forindustrial use. Methyl cellulose (MC) and cellulose sulfate (CS) were preparedusing bleached wood pulp and cotton linter. Coloured azo compounds were alsoprepared from coupling cellulose, wood pulp, MC and CS with aromatic diazoniumsalt. The presence of electron-releasing or withdrawing substituents affectedthe electrophilic substitution reaction. The produced azo compounds werecharacterized by FT-IR methodology, as well as mass spectrometry, in which thefunctional groups and the ion fragments of the products were analyzed.     

以钛氧有机物为前驱物制备具有高光催化活性的纳米二氧化钛晶体

 纳米二氧化钛的制备方法及前驱物的差别影响其光催化活性．将20ml钛酸丁酯及30ml乙酐在密闭容器中与50ml环己烷混合，在70～85℃反应30min，生成微细的非晶钛氧有机物；经FT－IR和TGA分析，该物质被确认为计量式是TiOOOCCH3）2和TiO（OC4H9）（OOCCH3）的混合体．该钛氧有机物前驱物经焙烧后得到具有高光催化活性的纳米二氧化钛晶体．表征结果表明，钛氧有机物在焙烧过程中，其表面的吸附物及键合有机基团在400℃以前发生脱附和氧化分解；在389～405℃间形成锐钛矿型晶体，在600℃出现金红石晶型；600℃焙烧3h所得样品的比表面积为86m2／g，其二次粒子呈200～300nm条形体，孔隙大于20nm；单分散粒子为球形单晶，粒径为22nm；表面物理吸附水量为1．21％，加热至800℃时失重1．48％，粉体稳定纯净．光催化实验结果表明，以钛氧有机物为前驱物制备的纳米二氧化钛晶体具有高的光催化活性，光降解丁基罗丹明溶液的反应速率常数约为溶胶－凝胶法制备的催化剂样品的4倍．表面氧空缺和一定量的表面羟基可能是粉体具有高光催化活性的重要因素．     

Syntheses, crystal structures and magnetic properties of a new nitronyl nitroxide NIT2-bithph and its manganese(II) compound [Mn(hfac)2(IMHBithph)]2·(NIT2-bithph)(C6H14)

A new nitronyl nitroxide NIT2-bithph (1) and its manganese(II) compound [Mn(hfac)₂(IMHBithph)]₂·(NIT2-bithph)(C₆H₁₄) (2) (hfac = hexafluoroacetylacetonate; NIT2-bithph = 4,4,5,5-tetramethyl-2-(bithiophenal-2-yl)imidazoline-1-oxyl-3-oxide; IMHBithph = 1-hydroxy-2-bithiophenal-4,4,5,5-tetramethyl-4,5-dihydro- 1H-imidazole) have been synthesized and structurally characterized by X-ray diffraction methods. The units of compound 1 were connected as one-dimensional chain by the intermolecular hydrogen bonds which afford an intermolecular antiferromagnetic interaction between nitronyl nitroxide radicals within the chain (J = −1.89 cm⁻¹). Compound 2 resulting from the reaction of Mn(hfac)₂·2H₂O and NIT2-bithph is dinuclear and includes the reduced amidino-oxide form of NIT2-bithph, it is made up of three parts: a [Mn(hfac)₂(IMHBithph)]₂ dimer unit, an uncoordinated NIT2-bithph radical and a noncoordinated solvent molecule of hexane, the molecule of radical is hydrogen bonded to its reduced form. Two reduced IMHBithph ligands bridge the two manganese(II) ions through their amidino-oxide oxygen atoms resulting in a small intramolecular antiferromagnetic interaction between the manganese ions (J = −1.55 cm⁻¹).     

Enhanced deep-red emission in donor-acceptor molecular architecture: The role of ancillary acceptor of cyanophenyl

Cyanophenyl as ancillary acceptor to modify donor-acceptor compound,plays an effective role in shifting the emission color to deep red and maintaining the luminescent efficiency.     

Drying agents for water-free introduction of desorption solvent into a GC after on-line SPE of aqueous samples

Summary A small cartridge containing a drying agent is inserted between a solid phase extraction (SPE) column and a gas chromatograph (GC) to enable the introduction of water-free desorption solvent into the GC in on-line liquid chromatography (LC)-type enrichment of trace-level analytes from water samples. Some characteristics of the drying agents, such as their capacity to retain water and their re-usability after heating, have been tested. Possible interactions of the drying agent with the analytes, e.g., irreversible adsorption or catalyzed degradation, have been checked for a wide range of alkanes, alkylbenzenes chlorobenzenes, chlorophenols and phthalate esters. Using the on-line SPE-GC system with flame ionization detection (FID) and spiked samples containing different levels of the test compounds, the repeatability was shown to be satisfactory (6–17%). For 10 mL samples, the detection limits were lower than 0.1 g/L. The on-line SPE-GC-FID system here presented can be used for the repeated analysis of water samples without exchange of the dyring cartridge. The technique is applied to the analysis of tap water.