二氢(4,5)熏衣草醇的合成

叙述了以易得的异戊醇为原料合成熏衣草醇的一种新型二氢衍生物的方法. 而异戊醇则可以从南中国的糖密发酵制造乙醇的蒸馏残液中得到. 异戊基氯和丙酮的相转移催化缩合以43%的产率得到6-甲基-2-庚酮, 再经甲基化和脱氯化氢导致2,6-二甲基庚烯-2. 该烯烃在氯化锡-二氯甲烷中,与多聚甲醛的Prins反应以41.2%的产率得到二氢(4,5)熏衣草醇. 它似乎是有较淡熏衣草醇香气的类似物.     

弱桥联二聚体丙酮酸异烟酰腙合锡(Ⅳ)配合物[(p-CNC6H4CH2)2Sn(C9H7N3O3)(H2O)]2的合成、表征和晶体结构

Diorganotin(Ⅳ) compound [(p-CNC₆H₄CH₂)₂Sn(C₉H₇N₃O₃)(H₂O)]₂ was synthesized by the reaction of tri-p-cyanobenzyltin chloride with Schiff base ligand pyruvic acid isonicotinyl hydrazone. The compound was characterized by elemental analysis, IR, ¹H NMR. The crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic space group C2/c, with a=3.143 1(3) nm, b=0.989 99(10) nm, c=1.785 68(18) nm, β=114.908 0(13)°, V=5.039 6(9) nm³, Z=4, μ=1.054 mm^-1, D_c=1.513 Mg·m^-3, F(000)=2 304, R=0.042 8, wR=0.090 3, GOF=0.997. In this compound, the Sn atom exists in a distorted octahedral coordination environment in which one water molecule, one tridentate pyruvic acid isonicotinyl hydrazone ligand, and two trans p-cyanobenzyl groups coordinate to each Sn center, the angle of the axial C10-Sn1-C18 is 166.1(2)°. Two molecules form a weak-bridged dimmer with weak interactions of Sn…O bonding and hydrogen bonds. CCDC: 270796.     

钌分子氢配合物催化烯烃的离子氢化

在氢气压力下，钌配合物[^MeCnRuCl(dppe)](O3SCF3)与AgO3SC3在CH2Cl2中反应生成分子氢配合物[^MeCnRu(H2)(dppe)](O3SCF3)2，该分子氢配合物具有催化烯烃离子氢化的活性。原位高压核磁共振研究显示，这种催化离子氢化反应可能是由分子氢配合物向烯烃转移氢质子形成碳正离子引起的。     

铋(Ⅲ)四氢吡咯氨荒酸配合物[Bi(S2CNC4H8)3]2的合成和晶体结构

The novel bismuth(Ⅲ) complex with dithiotetrahydropyrrolocarbamate, [Bi(S₂CNC₄H₈)₃]₂ has been synthe-sized. The crystal structure has been determined by X-ray single crystal diffraction. The crystal belongs to mono-clinic with space group C2/c, a=1.6356(9) nm, b=1.1875(6) nm, c=2.3954(13) nm, β=100.741(8)°, Z=4, V=4.571(4) nm³, D_x=1.882g·cm^-3,μ=8.267mm^-1, F(000)=2512, R=0.0404, wR=0.0622. In this binuclear complex, each Bi(Ⅲ) is seven coordinate with a distorted pentagonal bipyramidal geometry. CCDC: 179924.     

三苯基锡4－吡啶甲酸酯的合成、性质和晶体结构

用三苯基氯化锡与4-吡啶甲酸钠反应，合成了三苯基锡4-吡啶甲酸酯，并进行 了红外光谱、核磁共振氢谱及质谱表征。X射线单晶衍射表明，化合物属单斜晶系 ，空间群P21，晶胞参数：a=1.6629（3）nm，b=104987(4)nm，c=2.4318(7)nm，β =90.040（5）°，Z=8,Dc=1.1529g/cm^3，R1=0.0543，wR2=0.1086。化合物的晶体 是由两个结构相似但键长和键角不同的独立分子所组成，且每个分子含有两种化学 环境不同的锡原子。它们通过4-吡啶甲酸配体的氮原子桥联，形成五配位三角双锥 构型的一维无限链聚合物。     

二氧化碳插入单氢钌配合物反应中的水效应研究

分别研究了在干燥THF及H2O/THF条件下CO2与TpRu(PPh3)(CH3CN)H [Tp=Hydrotris(pyrazolyl)borate]的反应,发现水对CO2插入TpRu(PPh3)(CH3CN)H 的反应具有显著促进作用.原位高压^1H,^31P和^13C核磁共振研究显示,在水存在下 ,CO2插入Ru-H键形成水合甲酸盐配合物TpRu(PPh3)(CH3CN)(η^1-OCHO)·H2O键而 得到增强,进而显著降低CO2插入TpRu(PPh3)(CH3CN)H中Ru-H键的活化能。TpRu (PPh3)(CH3CN)(η^1-OCHO)·H2O很快部分转化为另一甲酸盐配合物TpRu(PPh3)（ H2O）(η^1-OCHO)，二者最后达成平衡，后者由于甲酸盐配体与水分子配体间形成 分子内氢键而稳定。     

铋(Ⅲ)配合物Bi(1,10-phen)[S2CN(CH3)2]2(NO3),

Three bismuth（Ⅲ） complexes Bi（1,10-phen）[S2CN（CH3）2]2（NO3） （1）, {Bi（S2COCH3）[S2CNC6Hs（CH3）]2}2 （2） and [Bi（S2CNBu2）2（CH3OH）（NO3）]∞ （3） were synthesized and characterized by elemental analysis and IR spectra. Their crystal structures were determined by X-ray single crystal diffraction analysis. Studies show that complex 1 has a monomeric structure with the central bismuth atom eight-coordinated in a capped distorted pentagonal bipyramidal geometry. The complex 2 takes centrosymmetric dimeric structure and the bismuth atoms are seven-coordinated in distorted pentagonal bipyramidal geometry.In complex 3, the bismuth atoms are seven-coordinated in distorted pentagonal bipyramidal geometry by bridging nitrate O atoms and the resulting structure is onedimensional infinite chain polymer.     

[（n-C4H9）3SnO2C（CH2）2CO2Sn（C4H9-n）3]：A Novel Three-dimensional Framework Structure of Organotin Complex

The bis(tributyltin) ester of succinic acid was synthesized by the reaction of disodium salt of succinic acid with tributyltin chloride in a molar ratio of 1:2. The crystal structure was determined by X-ray single-crystal diffraction. It belongs to orthorhombic with space group Pccn, a = 20.949(3), b = 17.470(3), c = 20.345(3)A, V= 7446(2)A^3, Z= 8, Dc = 1.242 g/cm^3, μ=1.365 mm^-1, F(000) = 2864, R = 0.0544 and wR = 0.1417. The tin atom is of five-coordination in a trigonal bipyramidal structure by bridging two carboxylate groups in different directions and the resulting structure which contains straight twist large ring channels along the axes of a, b and c is a three-dimensional framework polymer containing two different tin atoms.     

丙酮酸异烟酰腙四核有机锡配合物的合成、表征及{[nBu2Sn(C9H8N3O3)O]SnBu3n}2的晶体结构

The tetranuclear alkyltin(Ⅳ) compounds {[R2Sn(C9H8N3O3)O]SnR3}2 [R=n-Bu (1), 4-CNC6H4CH2 (2),C6H5CH2 (3), 4-ClC6H4CH2 (4)] were prepared by the reaction of Schiff base ligand pyruvic acid isonicotinyl hydrazone with (R3Sn)2O in the corresponding molar ratio of 1:1. All compounds have been characterized by elemental analysis, IR and ^1H NMR spectra. The crystal structure of compound 1 was determined by X-ray single crystal diffractional analysis. This compound exhibits a dimeric structure containing distannoxane units with two types of the tin atoms. For the first tin atom, it appears to be seven-coordinated with a distorted pentagonal bipyramid geometry, and the other is five-coordinated with a distorted trigonal bipyramidal geometry. The molecules are packed in the unit cell in two-dimensional network structure through an interaction between the N atoms of the pyridine and the tin atoms of an adjacent molecule.     

Controllable Passively Q-Switched Laser

We present a novel kind of pulsed laser named controllable passively Q-switched laser (CPQL). A CPQL of Nd:YV04 with Cr:YAG as saturable absorber was demonstrated and studied as an example of the kind of pulsed lasers. In CPQL, as the actively controlling signal, a diode laser beam was focused onto the saturable absorber in the resonant cavity of the passively Q-switched laser (PQL) and was absorbed by the absorber to realize the active control of the CPQL. The characters of the CPQL output laser pulses, such as generation time, repetition rate, pulse width, peak power and energy per pulse, can be controlled by the operator. The CPQLs possess theadv antages of both passively Q-switched laser and actively Q-switched laser. Because of their compactness, low cost and controllability, the CPQLs will find wide applications in many fields.