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。

η~6—芳烃希土有机配合物的合成、结构及性能研究——Ⅰ.Sm(η~6—C_6H_6)(AlCl_4)_3的合成及晶体结构

经过铝粉加热活化的AlCl_3与SmCl_3在苯中反应,得到了Sm(η~6—C_6H_6)(AlCl_4)_3·C_6H_6单晶.其晶体属于三斜晶系,P1空间群,晶胞参数a=9.456(2)(?),b=9.765(3)(?),c=16.776(4)(?),α=96.00(2)°,β=93.76(2)°,γ=111.66(2)°,V=1422.55(?)~3,Z=2.晶体结构是采用Patterson和Fourier合成法解出的,所有非氢原子的坐标及各向异性热振动参数经块矩阵最小二乘法修正,最后偏离因子R=0.031,R_ω=0.035.分子结构中,中心离子Sm(Ⅲ)与六个Cl原子及一个苯环上的六个C原子成键.Sm-C键平均距离2.92(?),Sm-Cl平均距离2.83(?).与希土相连的六个Cl原子,其中之五构成平面五边形,整个分子呈大致的五角双锥形.

[((C_9H_7)_3Ln)_2Cl][Na(OC_4H_8)_6]的合成及其晶体结构

用LnCl_3·nTHF和茚基钠在四氢呋喃溶液中室温下反应,成功得到了[((C_9H_7)_3Ln)_2Cl][Na(OC_4H_8)_6](Ln=Sm,Nd)配合物单晶。元素分析、红外光谱、热失重数据证实了配合物的组成。测定了晶体结构。晶体属三斜晶系,空间群为P,Z=1。它是一个氯原子做桥将两稀土离子连接起来。四氯呋喃分子中的氧原子同金属钠离子键合,Na-O键长2.377A,三个茚基分子中五圆环上碳原子同金属离子间的平均Ln-C键长为2.803A,Ln-Cl键长为2.899A,Ln-Cl-Ln键角为180°。