两个Pd(II)的异亚硝基乙酰丙酮亚胺配合物的合成和表征

合成了两个异亚硝基乙酰丙酮亚胺Pd(II)配合物，Pd(o-BrC_6H_4-IAI)_2 (1) 和Pd(C_6H_5CH_2-IAI)_2 (2)（IAI = isonitrosoacetylacetoneimino），用IR和 Raman光谱对两个配合物进行了表征，并测定了配合物1的晶体结构。配合物1晶体 属单斜晶系，空间群为P2_1/c，晶胞参数：a = 0.8013(2) nm，b = 1.8775(4) nm，c = 0.7905(2) nm，β = 98.22(3)°，V = 1.1770(5) nm~3，Z = 2，D_c = 1.892 g·cm~(-3)，F(000) = 656，R = 0.0663。在这两个配合物中，二齿 Schiff碱配体的异亚硝基（肟基）的N原子和亚胺的N原子与Pd(II)配位，形成反式 的PdN_4平面正方形配位构型。     

Synthesis and Crystal Structure of a New 2D Honeycomb-like Cadmium(II) Complex with Tripodal Ligand

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微波辐射下4-(4-羟基-3-甲氧基)苯基-3,3,6,6-四甲基-1,8-二氧代1,2,3,4,5,6,7,8,9,10-十氢吖啶的合成和晶体结构

标题化合物C24H29NO4?1/2C2H5OH稨2O)由香兰素、5,5-二甲基-1,3-环己二酮、醋酸铵在微波辐射下干反应并经95%乙醇重结晶而得C24H29NO4穀2(C2H5OH稨2O)晶体。结构通过单晶X-射线衍射法确定,其晶体属单斜晶系,空间群P21/n, a = 9.810(2), b = 14.516(3), c = 17.008(3) ? b = 101.03(2), V = 2377.2(8) ?, Z = 4, Mr = 427.52, Dc = 1.195 g/cm3 , m(MoKa) = 0.082 mm-1, F(000) = 920。晶体结构用直接法解出,经全矩阵最小二乘法对原子参数进行修正,最终的偏离因子为R = 0.0406, wR = 0.0892。X-射线衍射分析结果表明,吡啶环和与之稠合的2个六员环均为信封式构象。     

Growth and Characterization of Crystal Nd_(0.06)Y_(0.94)Sr_6Sc(BO_3)_6

<正>The crystal of Nd0.06Y0.94Sr6Sc(BO3)6 with the dimensions up to 35 mm × 28 mm × 13 mm was grown by a top-seeded solution growth method from Li6B4O9 flux. The grown crystal was characterized by X-ray powder diffraction. The optical absorption of the crystal shows that it has a strong absorption band at 8070 A, and the absorption coefficient is 2.17cm-1 with a FWHM of 41 A, which can match with the wavelength of the diode-laser (LD) and is suitable for the LD pumping. Based on the Judd-Ofelt theory, the three parameters of line oscillator strength Ω(λ) (λ = 2, 4 and 6) of the Nd3+ion in the crystal were calculated as follows: Ω2= 1.194 × 10-20, Ω4= 4.186 × 10-20 and Ω6 = 3.351 × 10-20cm2, which are relatively larger. The results indicate that the crystal Nd0.06Y0.94Sr6Sc(BO3)6 may be a kind of high-efficient laser material for diode-pumped.     

全芳香族共聚酯的结构和其液晶行为研究

本文对不同组成的对苯二甲酸(TPA),对羟基苯甲酸(PHBA),联苯二酚(BP),间苯二甲酸(IPA)共聚酯采用热台偏光显微镜、电子显微镜、X-射线衍射、激光小角散射、差热等技术进行了研究.实验结果表明,在一定的组成范围内共聚酯熔体有很好的液晶性.重点讨论了分子组成、转变行为、液晶性的关系,并对液晶相的形态结构进行了表征.     

Quantitative surface analysis by Auger and x-ray photoelectron spectroscopy

Recent developments in quantitative surface analysis by Auger (AES) and x-ray photoelectron (XPS) spectroscopies are reviewed and problems relating to a more accurate quantitative interpretation of AES/XPS experimental data are discussed. Special attention is paid to consideration of elementary physical processes involved and influence of multiple scattering effects on signal line intensities. In particular, the major features of core-shell ionization by electron impact, Auger transitions and photoionization are considered qualitatively and rigorous approaches used to calculate the respective transition probabilities are analysed. It is shown that, in amorphous and polycrystalline targets, incoherent scattering of primary and signal Auger and photoelectrons can be described by solving analytically a kinetic equation with appropriate boundary conditions. The analytical results for the angular and energy distribution, the mean escape depth, and the escape probability as a function of depth of origin of signal electrons as well as that for the backscattering factor in AES are in good agreement with the corresponding Mote Carlo simulation data. Methods for inelastic background subtraction, surface composition determination and depth-profile reconstructions by angle-resolved AES/XPS are discussed. Examples of novel techniques based on x-ray induced photoemission are considered.     

Specific and non-specific interactions of hydropseudohalic acids with water and organic solvents

Partition coefficients P of the HNCS, HNCO and HN₃ hydropseudohalic acids between a number of organic solvents and water were determined. It has been found that log P increases with pKa of the acid and with the basicity of the solvent, but the effect of pKa on P is the smaller the more basic is the solvent. The relationships have been explained in terms of hydrogen bond formation between undissociated acid and solvent molecules. H-bonding between the pseudohalic acids and organic solvents has been confirmed by IR spectra on the example of HN₃ in benzene. Association constants for H-bonding between the three acids and water, benzene, dibutyl ether and tri-n-butyl phosphate were determined from partition data. It has been found that H-bonding increases with the strength of the acid, whereas the contribution to partition from non-specific interactions with water and organic solvents depends on the molecular surface area of the acid molecule.     

低硫可膨胀石墨的制备

低硫可膨胀石墨的制备宋克敏，路文义，高淑英，阎秋燕（河北教育学院石家庄０５００９１）关键词低硫可膨胀石墨，制备，过氧化氢，硫酸柔性石墨具有耐高温、耐酸碱、抗拉、抗压、抗辐射、回弹性等优良性能，被广泛应用于化工、机械、肮天、原子能等领域。但其原材料可膨...     

{(MesGa)3[GaP(H)Mes](PMes)4}, Ein phosphorsubstituiertes Ga?P-Heterocuban

{(MesGa)₃[GaP(H)Mes](PMes)₄}, a Phosphorus-substituted Ga? P-Heterocubane A mixture of MesGaCl₂/GaCl₃ (ratio 3:1) reacts with 5 equivalents of MesPLi₂ in THF at ?78°C to the title compound {(MesGa)₃[GaP(H)Mes](PMes)₄} ( 1 ) by use of the “dilution principle”. 1 can be obtained in 30% yield. Recrystallization of 1 from DME and toluene, respectively, gives 1 · 0.5 DME and 1 · toluene. 1 was characterized by NMR-, IR-, and MS-techniques. According to the X-ray structure determination of 1 · toluene, 1 has a heterocubane structure, one corner of which is substituted with an P(H)Mes group.     

NITROXIDE-MEDIATED FREE RADICAL SYNTHESIS OF MESOGEN-JACKETED LIQUID CRYSTAL POLYMERS*

The first TEMPO-mediated "living" free radical polymerization of liquid crystallinemonomer, 2, 5-bis[(4-methoxyphenyl)oxycarbonyl]styrene(MPCS), was carried out at 130℃ withBPO as an initiator. The molecular weight of the polymer can be varied from rather low values to highvalues while maintaining narrow polydispersity. It was observed that the polymerization of MPCSproceeded much faster than that of styrene. A tentative explanation for this fast polymerization wassuggested.