Synthesis and crystal structure of [Nd(eta(6)-1,3,5-C6H3Me3)(AlCl4)(3)]( C6H6) and structural comparison of Ln(eta(6)-arene)(AlCl4)(3)

Reaction of NdCl3, with AlCl3 and mesitylene in benzene gives complex [Nd(eta (6)-1,3,5-C6H3Me3) (AlCl4)(3)] (C6H6) (1) which was characterized by elemental analysis, IR spectra, MS and X-lay diffractions. The X-ray determination indicates that 1 has a distorted pentagonal bipyramidal geometry and crystallizes in the monoclinic, space group P2(1)/n with a = 0.9586(2), b = 1.1717(5), c = 2.8966(7) nm, beta = 90.85 (2)degrees, V = 3.2529(6) nm(3), D-c = 1.573 g/cm(3), Z = 4. A comparison of bond parameters for all the reported Ln(eta (6)-Ar) (AlCl4)(3) complexes indicates that the bond distance of Ln-C is shortened with the increasing of methyl group on benzene and with the decreasing of radius of lanthanide ions.

三环己基锡-2-(1,2-亚乙二硫)亚甲基-3-羰基-5-芳基-4-戊烯酸酯的结构研究

合成了 3个三环己基锡 -2 -( 1 ,2 -亚乙二硫 )亚甲基 -3-羰基 -5 -芳基 -4 -戊烯酸酯化合物 .用 IR,1 H NMR,1 3 C NMR和 1 1 9Sn NMR光谱及 X射线衍射对所合成的化合物进行了表征 .结果表明标题化合物为四配位、具有畸变四面体结构的锡酯类化合物

Syntheses of indenyl lanthanide derivatives and the molecular structures of [(C9H7)(2)PrCl(THF)](2) and [(C9H7)(3)La(THF)]

The reaction of anhydrous PrCl3 with Na(C9H7) in 1.2 mole ratio in THF gives [(C9H7)(2)PrCl(THF)](2)1. 1 crystallized in monoclinic system, space group P2(1)/c with a = 7.808(2), b = 17.796(6), c = 14.070(4) Angstrom, beta = 93.97(2)degrees, V= 1950.3(9) Angstrom(3), Dcalcd = 1.63 g/cm(3) and Z = 2. Each Pr ion is surrounded by two indenyl, two Cl and one THF in a roughly trigonal bipyramid arrangement with average Pr-C(ring) and Pr-Cl distances of 2.81 and 2.84 Angstrom. The reaction of LaCl3 with Na(C9H7) in 1:3 mole ratio gives (C9H7)(3)LaTHF 2, which crystallizes in the monoclinic space group P2(1)/a with unit cell constants a = 21.871(8), b = 10.585(3), c = 23.652(7) Angstrom,beta = 114.62(2)degrees, V = 4977.9 Angstrom(3) and Z = 8. (C) 1997 Elsevier Science S.A.

Synthesis and structure of 1:1 complex of ethylphenyltin dichloride with N-4-methoxyphenyl-2-hydroxynaphthylideneimine

A novel organotin complex, EtPhSnCl(2) . 2HOC(10)H(6)CH = NC6H1OCH3 was synthesized, and its crystal structure was determined by X-ray diffraction method. The crystal is triclinic, belonging to space group, with unit cell parameters a = 1.150 8(5) nm, b = 1. 153 1(5) gm, c = 1. 004 6 (3) nm, alpha = 94. 15 (3)degrees, beta = 115.47 (3)degrees, r = 85. 94 (4)degrees, V = 1199 7(1) nm(3), Z=2, D-c=1.68 g/cm(3), mu=13. 20 cm(-1), F(000)=618 for 4 131 reflections tions. R=0. 047, R(w)=0. 047. The ligand coordinates to tin atom via phenolic oxygen atom. The complex has a distored trigonal bipyramidal structure, the phenolic oxygen atom of the ligand and one of two chlorine atoms occupy the axial position. The distance between noncoodinated nitrogen atom with phenolic oxygen atom is 0. 257 4 nm, which indicates that the intramolecular hydrogen bond of Schiff base ligand is retained in the complex.

2－（1，3－亚丙二硫基）亚甲基环己酮的晶体结构

报导了标题化合物Ｃ_（１０）Ｈ_（１４）ＯＳ_２（Ｍ_ｒ＝２１４．３５）的晶体结构，该晶体属正交晶系，空间群为Ｐ２_１２_１２_１，晶胞参数为ａ＝６．４４３（３），ｂ＝８．９８０（４），ｃ＝１８．２１３（７）；Ｖ＝１０５３．８（６）３；Ｚ＝４，Ｄ_ｘ＝１．３５ｇ／ｃｍ~３，Ｆ（０００）＝４５５，μ＝４．５ｃｍ~（－１）（ＭｏＫａ）。最终偏离因子Ｒ＝０．０３３，Ｒ_ｗ＝０．０３４。分子中的两支Ｃ_（ｓｐ）２－Ｓ键键长近于相等，分别为１．７６１（３）和１．７６９（３），Ｃ（１）－Ｃ（５）键长为１．３６１（４）。

JH－3橡胶型压敏胶的研究

介绍了以天然橡胶和丁苯橡胶为主体材料，以烃类树脂为增粘剂压敏胶的制备，并研究了丁苯橡胶、树脂、填料及其它助剂对压敏胶性能的影响。

有机磷化合物的质谱研究（XⅢ）．1，3，2－二氮磷杂环戊酮－（4）衍生物的电子轰击质谱

本文报道９种新的含磷杂环化合物的电子轰击质谱（ＥＩＭＳ），并应用Ｂ／Ｅ、Ｂ２／Ｅ联动扫描及精确质量测量技术，探讨了该类化合物的质谱断裂机理，发现骨架重排及开环反应是该类化合物主要的质谱特征，而Ｒ２基因对重排过程有很大影响。

α-羰基烯酮环二硫代缩醛化学(Ⅵ)——β,β-1,3-亚丙二硫基-α,β-不饱和芳酮与烯丙基Grignard试剂加成物脱水反应的研究

提出了由β,β-1,3-亚丙二硫基-α,β-不饱和芳酮类化合物(1)与苄基氯化镁及烯丙基溴化镁加成所得的醇(2)在BF_3·Et_2O催化下脱水生成共轭烯烃(3)新的合成途径,合成了13种新化合物,结构经~1H N-MR、IR、UV及元素分析等确证.并对这一新合成途径的反应机制进行了讨论.

YP_xV_(1-x)O_4(0≤x≤1):Dy~(3+)的合成及其光谱性质的研究

本文报道了不同组成的YP_xV_(1-x)O_4(0≤x≤1):Dy~(3+)的合成和结构。YP_xV_(1-x)O_4(0≤x≤1)为四方晶系,晶胞参数随x的增大呈线性减小。基质的Stokes位移随x的增大逐渐变大,而激发光谱峰值则向短波方向移动。在YP_xV_(1-x)O_4:0.006Dy~(3+)体系中,x>0.4时出现的基质发射是由P0_4~(3-)引起的。基质及Dy~(3+)的发光效率和Dy~(3+)的发光强度的黄蓝比均与x有关。同时探讨了Bi~(3+)和温度对Dy~(3+)的发光强度的影响。

YV_(1-x)B_xO_(4-x):Eu~(3+)(或Dy~(3+),Bi~(3+))的合成及光谱性质的研究

本文报道了Eu~(3+)、D~(3+)在YV_(1-x)B_xO_(4-x)中的光谱性质。实验表明:B~(3+)取代V~(5+)时,可使基质和Dy~(3+)的发射强度及黄兰比下降,并使基质的吸收带短移。而B~(3+)取代Y~(3+)时,则可提高Dy~(3+)的黄兰比。同时我们还研究了Bi~(3+)和温度对YV_(0.69)B_(0.31)O_(3.69):Dy~(3+)中Dy~(3+)发射强度的影响。

CRYSTAL-STRUCTURE OF 1, 10-DECANEDIAMMONIUM TETRACHLOROZINCATE

The crystal structure of the title compound has been determined from single crystal X-ray diffraction. The complex crystallizes in the triclinic space group P1 with Z=2. Lattice parameters are: a = 0.7296(1), b = 1.0110(3), c = 1.2814(4) nm; alpha = 90.84(2), beta = 101.17(2), gamma = 92.52(2)-degrees. Intensity data were collected on a Nicolet R3M/E four-circle diffractometer using MoK alpha (lambda = 0.071073 nm) radiation. The structure was solved by Patterson and Fourier techniques and refined by least-squares techniques to R = 0.065. The structure of the complex consists of tetrahedral ZnCl42- anions which form a two-dimensional sheets. Tetrahedral ZnCl42- anions are sandwiched between two hydrocarbon layers which consist of [NH3(CH2)10NH3]2+ cations. Each [NH3(CH2)10NH3]2+ group is in a gauche bond between C atoms near NH3 polar heads.

α-羰基烯酮式环二硫代缩醛化学(V)——β,β-1,3-亚丙二硫基-α,β-不饱和芳酮类化合物的合成

β,β-二烷硫基-α,β-不饱和酮类化合物作为一类具多反应中心的活泼中间体在有机合成中的应用,近20年来已引人注目并进行了深入广泛的研究~[1,2].以往的研究大多是针对β,β-二甲硫基-α,β-不饱和酮类化合物1进行的,而对结构相近的β,β-1,3-亚丙二硫基-α,β-不饱和酮类化合物2的研究较少.对于1类的合成,所用碱的选择至关重要~[1].实验证明叔丁醇钠和叔丁醇钾~[3～5]在1类的合成中效果较好.前文~[6]曾以六甲基二硅氨基锂(LHMDS)为碱高

四氯合锌酸1,10-癸二铵配合物的晶体结构

合成了[NH_3(CH_2)_(10)NH_3]ZnCl_4配合物(简称DDAZn),用X射线衍射法研究了它的晶体结构,晶体属三斜晶系,空间群为P1,晶胞参数为:α=0.7296(1),b=1.0110(3),c=1.2814(4)nm;α=90.84(2),β=101.17(2),γ=92.52(2)°;Z=2.该配合物为层型结构.由单个四面体阴离子ZnCl_4~(2-)构成的阴离子层被夹在烷基铵阳离子层之间,形成“夹心面包”型体系.在层之间的烷基铵链在垂直于层的方向上倾斜排列.

Ho~(3+):Gd_3Ga_5O_(12)晶体的光谱性质及强度参数

本文详细地研究了Ho~(3+):Gd_3Ga_5O_(12)(以下简称Ho~(3+):GGG)中Ho~(3+)离子在0.5～3.0μm波段内的室温及77K温度下的荧光光谱。根据Judd—Ofelt理论,计算了Ho~(3+)离子的自发辐射电偶跃迁几率与辐射寿命等光谱强度参数。

1-（2-萘基）-3-甲基-5-吡唑啉酮衍生试剂的制备及其在高效液相色谱-质谱法测定糖类化合物中的应用

以1-（2-萘基）-3-甲基-5-吡唑啉酮（NMP）作为柱前衍生试剂,建立了简单、灵敏的糖类组分的反相高效液相色谱测定方法。NMP与糖在氨为催化剂的条件下,于70℃下反应可获得稳定的衍生产物。在HypersilODS2反相色谱柱上,实现了8种单糖的基线分离。衍生物线性相关系数均大于0.9985,检出限为0.58-1.1pmol。利用柱后在线串联质谱的电喷雾电离正离子模式监测,获得了各组分的质谱定性及裂解规律,特别是m/z473的特征碎片离子可作为单糖NMP衍生物的判定依据。与1-苯基-3-甲基-5-吡唑啉酮（PMP）相比,NMP对糖的衍生化具有灵敏、简单、质谱裂解规律性强、重现性好等优点。该方法用于测定油菜花粉多糖中的单糖组成,结果令人满意。