含间苯连接的聚醚醚酮酮的等温结晶过程和形态结构

用透射电子显微镜和电子衍射方法研究了含间苯连接的聚醚醚酮酮（PEEKmK）溶液浇铸薄膜的等温结晶过程和形态结构．结果表明，PEEKmK无论从玻璃态结晶还是从熔体结晶均能形成2种不同取向的结晶形态结构，即平放片晶和侧放片晶；前者c轴垂直于膜平面，后者c轴平行于膜平面．其结晶发展过程为先形成平放单晶状片晶，随着时间的增长，在单晶上开始生长侧放片晶，逐渐发展形成球晶，最终形成2种不同取向的单晶和球晶共存的结晶形态结构.

4-羟基偶氮苯与6-氯-5,12-萘并萘醌反应产物的NMR分析

无水碳酸钾存在下6-氯-5,12-萘并萘醌与4-羟基偶氮苯在干燥DMF中反应的主要产物在某些反应条件下不是6[4-(苯基偶氮基)苯氧基]-5,12-萘并萘醌(1)。该未知反应产物2经核磁共振方法研究证实是6-(N,N-二甲氨基)-5,12-萘并萘醌。本文对化合物2的~1H-和~(13)C化学位移、偶合信息和结构作了详细归属,并推测其反应进程,实验结果表明,化合物2是由化合物1与溶剂DMF反应生成。

Isolation and X-ray crystallographic structure of cyclic tetramer based on bisphenol A and o-phthaloyl dichloride

The polycrystalline powder of the cyclic tetramer based on bisphenol A and o-phthaloyldichloride has been prepared by recrystallization from nitrobenzene and its crystal structure has been determined by Wide-Angle X-ray Diffraction (WAXD). The unit cell is orthorhombic and its dimensions a = 0.967 6 nm, b = 0.869 9 nm, c = 2.085 9 nm, Space group belongs to Pmmm, With two tetramers per unit cell,the crystal density is 1.36 g . cm(-3), Indices of crystal diffraction peaks are also detailed in the present work.

X-ray crystallographic structure of cyclic tetramer ester based on bisphenol-A and o-phthaloyldichloride

The polycrystalline powder of the cyclic tetramer ester based on bisphenol-A and o-phthaloyldichloride has been prepared by recrystallization from nitrobenzene and its crystal structure determined by wide-angle X-ray diffraction. The unit cell is orthorhombic and has dimensions a=0.967 nm, b=0.8699 nm, c = 2.0859 nm. With two tetramers per unit cell, the crystal density is 1.36 g cm(-3). Indices of crystal diffraction peaks are also detailed in the present work. Copyright (C) 1996 Elsevier Science Ltd.

RELATIONSHIP BETWEEN CONFORMATION OF TASTE COMPOUNDS AND THEIR ACTIVITIES

The conformation analysis and study on structure-taste relation-ships of 4 taste compounds have been performed, the results reveal that the sweetnees will decrease with the increase of the specific dihedral angle O-1-C-2-C-3-C-4, and the mechanism was intepreted.

DICHLORO(ETA(5)-CYCLOPENTADIENYL)([1-(4-METHOXYPHENYL)CYCLOHEXYL]-ETA(5)-CYCLOPENTADIENYL)TITANIUM(IV)

The title molecule, [TiCl2(C5H5)(C18H21O)], has a pseudotetrahedral bent metallocene structure in which the cyclopentadienyl ring is symmetrically bonded to Ti [range of Ti-C distances 2.36(1)-2.41(1)Angstrom], but the substituted cyclopentadienyl ring adopts asymmetrical bonding [Ti-C 2.33(1)-2.48(1)Angstrom] due to the interaction of the large substituent with the Cl(2) atom. The angle C(11)-C(1)-C(21) is 111.1(8)degrees with the large substituent occupying a cis position with respect to the substituted ring.

A STUDY OF SURFACE OXYGEN SPECIES FROM LA-ME-O (ME=MG, CA, SR, BA) CATALYSTS FOR METHANE OXIDATIVE COUPLING

CO2-TPD was used to study the surface basicity of La-Me-O mixed oxides and O-2-TPD, CH4-TPD were employed to study the surface active oxygen species. Comparing the CO2-TPD with O-2-TPD, we can see that the basicity of catalyst is in parallel with the catalystic activity. The stronger basicity is more profitable for the catalyst to adsorb oxygen to form active oxygen species and to activate CH4 by breaking a C-H bond, By comparing the catalytic activity, the results showed that La-Ba-O(La/Ba=7/3) catalyst had the strongest basicity, and it gave the highest CH4 conversion and C-2 selectivity, The results from the pulse reaction showed that the lattice oxygen participated in the OCM reaction without gas oxygen, and it was the selective oxygen species.

杂多阴离子的相转移化学 Ⅰ.取代的Keggin及Dawson结构杂多阴离子在非极性溶剂中的溶剂化行为研究

利用四庚基溴化铵将Keggin结构的杂多阴离子ZW_(11)O_(39)M(H_2O)~(n-)(Z=Si,Ge,P;M=Ni~(2+),C~(2+),Cr~(3+),Co~(2+);n=4～6)和Dawson结构的杂多阴离子P_2W_(17)O_(61)M(H_2O)~(n-)(M=Ni~(2+),Cu~(2+),Cr~(3+),Co~(2+);n=7,8)从水溶液中转移至非极性溶剂(苯或甲苯)中,并观察到在水溶液中难以进行的配位水的脱去反应,形成配位不饱和的杂多阴离子.当加入Lewis碱如丙酮、吡啶等,可迅速恢复饱和配位,其电子吸收光谱也相应变化,基本恢复到配位饱和时的数值,有ESR信号.实验表明,在非极性溶剂中,配体之间相互进行的取代反应,吡啶配位能力最强,发生了取代反应ZW_(11)O_(39)M(L)~(n-)+Py→ZW_(11)O_(39)M(Py)~(n-)+L(L=丙酮、乙腈等).同时我们也研究了温度、杂多阴离子浓度、惰性气体流量对杂多阴离子在非极性溶剂中的溶剂化行为的影响,得到了相转移的一般规律,为杂多阴离子在非极性溶剂中的催化研究提供了理论依据.

用NMR方法研究中药山莨菪碱与磷脂脂质体的相互作用

用核磁共振(NMR)方法研究了中药山莨菪碱(anisodamine)与结构不同的3种磷脂脂质体相互作用,二棕榈酰磷脂酰胆碱(DPPC)极性基团空阻较大,山莨菪碱三级胺端不能与P-O键作用,仍处于水相,苯环只能嵌入到甘油骨架C-2附近。二棕榈酰磷脂酸(DPPA)极性头空间位阻较小,山莨菪碱苯环可以直接插入到靠近脂酰链γ-次甲基的位置,而三级胺端与极性头发生静电作用,并且药物可以提高DPPA脂质体的流动性。山莨菪碱通过三级胺端与鞘磷脂(SPM)极性头静电作用较强,而苯环位于SPM脂双层亲水和疏水区界面。药物对3种磷脂双层结构影响很小。

HOST-GUEST INTERACTIONS OF THIAMINE WITH ANIONS - CRYSTAL-STRUCTURE OF THIAMINE IODIDE SESQUIHYDRATE

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 usual F 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, P2(1)/c, a = 12.585(2), b = 25.303(5), c = 12.030(2) angstrom, beta = 115.15(1)degrees, V = 3468(1) angtrom3, Z = 8, D(c) = 1.606 g cm-3, R = 0.045 for 3328 observed reflections.

四甲基乙撑桥联二环戊二烯基环戊二烯基稀土配合物的合成与表征

合成了四个甲基乙撑桥联二环戊二烯基环戊二烯基稀土四氢呋喃配合物,采用元素分析、红外光谱、核磁共板、热失重和质谱等方法对所得到配合物进行表征,并用X光衍射法测得Me_4C_2(C_5H_4)_2SmC_5H_3(THF)的晶体结构。该晶体属正交晶系C_(e2a)空间群,a=1.1696(6),b=1.2539(5),c=2.9432(15)nm;V=4.316(4)nm~3,z=8,D_c=1.54g·cm~(-3)。三个环戊二烯基Sm-C(η~5)距离分别为0.272(3),0.276(3),0.278(3)nm和Sm-O键长为0.253(1)nm。

STRUCTURE OF THIAMINE BROMIDE SESQUIHYDRATE

3-[(4-Amino-2-methyl-5-pyrimidinyl)-methyl]-5-hydroxyethyl-4-methylthiazolium bromide sesquihydrate, C12H17N4OS+.Br-.1.5H2O, M(r) = 372.28, monoclinic, P2(1)/a, a = 11.676 (2), b = 24.819(7), c = 12.344 (3) angstrom, beta = 113.74(2)-degrees, V= 3274 (1) angstrom3 , Z = 8, D(x) = 1.51 g cm-3 (Mo Kalpha) = 0.71069 angstrom, mu = 26.2 cm-1, F(000) = 1528, T 293 K, R = 0.062 for 2720 observed reflections. Both the independent thiamine molecules A and B in the asymmetric unit adopt the common F conformation. A bromide anion is held by four neighbouring thiamine molecules through C(2)-H...Br hydrogen bonds and Br ... thiazolium-ring electrostatic interactions. Another bromide anion (or a water molecule) bridges the pyrimidine and thiazolium moieties of molecule A (or B) through a hydrogen bond with the amino group and an electrostatic interaction with the thiazolium ring.

SYNTHESIS, STRUCTURE AND SPECTRA PROPERTIES OF THE NEODYMIUM MOLYBDOGERMANATE HETEROPOLY COMPLEX

K7H6[Nd(GeMo11O39)2].18H2O was first synthesized and the crystal structure was determined. Crystal structure data are as follows: monolinic, space group P2(1)/n, a = 1.7095(4), b = 2.6895(3), c = 2.1214(5) nm, beta = 103.11 (2)-degrees, V = 9.4994(3) nm3, Z = 4, D(m) = 3.14g/cm3, D(c) = 3.05g/cm3, mu(MoK-alpha) = 43.7 cm-1. Experimental evidence and theoretical foundation of the method inferring the molecule structure of heteropoly compounds using their IR spectra were gaved by studying IR spectra properties of the complex with results of structural analysis. Electronic spectra prove that 4f-obital of Nd3+ take part in bonding in the complex.

钕锗钼杂多酸根配合物的合成、晶体结构和光谱性质

合成及制备了K_7H_6[Nd(GeMo_(11)O_(39))_2]·27H_2O单晶,测定其晶体结构,空间群属P2_1/n,晶胞参数:α=1.7095(4),b=2.6895(3),c=2.1214(5)nm,β=103.11(2)°;V=9.4994(3)nm~3;Z=4;D_m=3.14g/cm~3,D_c=3.05g/cm~3;μ(MoKα)=43.70cm~(-1)。利用结构分析的结果,研究配合物的IR光谱性质,提出利用IR光谱推测杂多配合物分子结构特征的实验证据和理论根据。电子光谱证实配合物中Nd~(3+)的f轨道参与成键。

Nd(C_6H_5CH_2COO)_3·H_2O的晶体结构及表征

采用X射线四圆衍射仪测定了Nd(C_6H_5CH_2COO)_3·H_2O的晶体结构。配合物属于正交晶系,空间群为Pna2_1,晶胞参数为a=0.7983(1)nm,b=1.3975(1)nm,c=2.0282(2)nm,Z=4。采用TG—DTG—DTA和DSC研究了标题配合物的热分解机理和其过程的焓变。