Syntheses and Crystal Structures of Two Diethyltin Complexes of N-Salicylidene-α-amino Acid

Two novel diethyltin（IV） complexes of N-salicylidenevaline （H2L1） and N-Sali- cylidenetryptophan （H2L^2）, Et2SrtL^1 1 and Et2SnL^2 2, were synthesized and characterized by elemental analysis, IR, ^1H NMR and X-ray single-crystal diffraction analysis. Complex 1 belongs to the trigonal system, space group R-3 with a = b = 19.2730（5）, c = 23.6890（13）A^°, V= 7620.4（5） A^°^3, Z = 6, Dc= 1.553 g/cm^3,μ= 1.518 mm^-1, F（000） = 3600, R = 0.0238 and wR = 0.0636. Complex 2 is of monoelinie system, space group P21/c with a = 13.7550（8）, b = 11.5425（7）, c = 12.7876（7）A^°, β= 93.585（1）°, V = 2026.3（2） A^°^3, Z = 4, Dc= 1.548 g/cm^3,μ = 1.286 mm^-1, F（000） = 976, R = 0.0298 and wR = 0.0722. Complex 1 is a cyclic trimer with a macrocyclic 12-membered ring structure formed by the bidentate bridging coordination of carboxylate group to tin atoms. The tin atom is six-coordinated in a distorted octahedral geometry. In complex 2, the distorted trigonal bipyramidal Et2SnL2 units are linked into polymeric chains by the weak Sn…O interaction involving Sn and the earbonyl O of an adjacent ligand, and the chains are further connected by intermolecular N-H…O hydrogen bonds to form a two-dimensional supramolecular structure.     

Three New d~(10) Coordination Polymers with Arenedisulfonates:Syntheses,Crystal Structures and Luminescent Properties

Three new cadmium or zinc arenedisulfonate complexes [Zn（bpp）2（L）]n 1, { [Cd（bpp）2（1,5-NDS）（H2O）2]·4H2O }n 2 and { [Cd（bpp）2（H2O2）2]·（1,5-NDS） } n 3 （L = 4,4′-bis（2-sulfonatostyryl）biphenyl, bpp = 1,3-di（4-pyd-dyl）propane and 1,5-NDS = 1,5-Naphthalenedisulfonate） have been synthesized from aqueous solution and structurally characterized by infrared spectroscopy, elemental analysis and single-crystal X-ray diffraction. Crystal data for complex 1： space group P21/n, a = 10.559（3）, b = 13.138（4）, c = 17.623（5）A^°, β = 100.852（3）°, V = 2400.9（12） A^°^3 Z = 2, Dc= 1.351 g/cm^3, F（000） = 1016, μ = 0.654 mm^-1, the final R = 0.0412 and wR = 0.0994; Crystal data for complex 2： space group P^-1, a = 8.5642（19）, b = 10.076（3）, c = 12.114（3） A^°, α = 81.623（7）, β = 77.149（8）, γ = 82.787（7）°, V = 1003.6（4） A^°^3 Z = 1, Dc= 1.495 g/cm^3, F（000） = 466,μ = 0.713 mm^3, the final R = 0.0241 and wR = 0.0713; Crystal data for complex 3： space group C2/c, a = 21.6024（15）, b = 9.4608（5）, c = 18.4656（11）A^°, β = 107.359（3）°, V= 3602.0（4）A^°^3 Z = 4, Dc= 1.533 g/cm^3, F（000） = 1704,μ = 0.780 mm^-1, the final R = 0.0229 and wR = 0.0572. The X-ray single diffraction reveals that 1 exhibits a 3D metal-organic framework formed from 2D Zn（bpp）2^2＋ networks connected by L in the third dimension; 2 and 3 possess 3D and 2D architectures constructed from 1D polymeric chains through H-bond. Complexes 1-3 display photoluminescent emissions at 452 and 335 nm, respectively.     

Crystal Structure and Activity against Acetaminophen-induced Hepatotoxicity of a Potassium Complex with Taurine-5-bromosalicylaldehyde Schiff Bases

A novel potassium complex KC9H9NO4SBr has been synthesized and characterized by IR spectra and single-crystal X-ray diffraction method. The crystal belongs to orthorhombic, space group Pbca with a = 0.74040（15）, b = 0.74960（15）, c = 4.2620（9） nm, V = 2.3654（8） nm^3, Mr = 346.24, Dc = 1.945 g/cm^3, Z = 8, F（000） = 1376, μ（MoKa） = 4.005mm^-1, GOOF = 1.021, R = 0.0471 and wR = 0.0872. In the crystal, the potassium ion is typically eight-coordinated, surrounded by eight O atoms from six （E）-2-（5-bromo-2-hydroxy-benzyli-deneamino）ethanesulfonate anions. The neighboring potassium ions are bridged by sulfonate groups into a two-dimensional layer structure, above and below which the 5-bromo-2-hydroxy-benzene rings are protruded. The activity against acetaminophen-induced hepatotoxicity of this complex was also studied, and found it can protect liver from hepatotoxicity induced by acetaminophen （AAP） to some extent.     

Synthesis and Crystal Structure of （R）-4-Hydroxymethyl-2-thioxo Thiazolidine and Its Asymmetric Catalysis

(R)-4-Hydroxymethyl-2-thioxo thiazolidine as a new chiral catalyst in the asymmetric addition of diethyl-zinc to benzaldehyde was synthesized from (R)-4-hydroxymethyl-2-thioxo thiazolidine carboxylic acid and its crystal structure was determined by X-ray diffraction method. The compound was crystallized in the orthorhombic system, space group P212121 with unit cell dimensions a=0.67253(12) nm; b=0.89164(17) rim; c=1.06146(19) nm, volume 0.6365(2) nm3; Z=4, calculated denisity 1.557 Mg/m3; absorption coefficient 0.733 mm-1; F(000)=312. The X-ray crystal structure analysis reveals that the compound has a thione group.     

ChemInform Abstract: Aromatic Metal‐Centered Monocyclic Boron Rings: Co@B‐8 and Ru@B‐9.

Co@B^‐₈, Ru@B^‐₉, Co@B₈, and Ru@B₉ clusters are characterized by photoelectron spectroscopy and DFT calculations.     

ChemInform Abstract: Matrix Infrared Spectroscopic and Theoretical of the Difluoroamino Metal Fluoride Molecules: F2NMF (M: Cu,Ag, Au).

The title molecules are obtained from spontaneous reactions of coinage metals and NF₃ in solid Ar and Ne matrices.     

ChemInform Abstract: Synthesis,Structure, and Electronic Structure of CsAgGa2Se4.

The new title compound is prepared from a mixture of AgGaSe₂ (obtained from the elements at 900 °C, 2 d) and CsI in the molar ratio 1:2 (silica tube, Ar, 800 °C, 48 h).     

ChemInform Abstract: Infrared Spectroscopic and Theoretical Investigations of the OUF2 and OThF2 Molecules with Triple Oxo Bond Character.

The title molecules are prepared by reaction of OF₂ molecules with laser ablated uranium and thorium atoms in solid argon and neon.     

蘑菇中甲壳素的提取及结构研究

以蘑菇为原料提取甲壳素,并制备壳聚糖。通过滴定法测定由蘑菇制备的壳聚糖的脱乙酰度,用乌氏黏度计测定了比浓黏度,并研究了制备工艺中加热温度和碱处理时间对它们的影响,计算了其产率;对以蘑菇为原料制取的甲壳素、壳聚糖的结构通过红外光谱进行表征。结果表明,在碱处理时间为24h、加热温度为100℃的条件下有较高的脱乙酰度;比浓黏度随着碱处理时间的延长、加热温度的增加都呈下降的趋势;壳聚糖产率为1．69％。制取的甲壳素、壳聚糖的红外光谱图表明,甲壳素在蘑菇中主要是以α-构型存在,α-构型甲壳素在浓碱中经过脱乙酰后生成β-构型的壳聚糖。     

新型咔唑衍生物的合成及其晶体结构

通过9-乙基咔唑-3-甲醛与4-氨基-3,5-二甲基-1,2,4-三氮唑反应,合成了一种新型咔唑衍生物-- 9-乙基咔唑-3-甲醛缩4-氨基-3,5-二乙基-1,2,4-三氮唑(1),其结构经1H NMR, IR和X-射线单晶衍射表征.1属单斜晶系,P2(1)/n空间群,晶胞参数为:a=8.829(8)(A), b=9.863(10)(A), c=19.530(15)(A), β=101.65(5)°, V=1 666(3)(A)3, Dc=1.266 g·cm-3, Z=4, F(000)=672, μ=0.079 mm-1.最终偏离因子R1=0.075 6.