The first discrete mixed-valence hexadecavanadate host shell cluster anions: hydrothermal synthesis, structure and characterization of [V16O38(Cl)](8-)

A new compound, [NH4](2)[Zn(phen)(3)](2)[Zn(phen)(2)(H2O)(2)][V16O38(Cl)] (.) 5H(2)O (1), was synthesized in the hydrothermal condition. The "naked" [V16O38(Cl)](8-) is the first observation with host shell structure in polyoxovanadate chemistry.

Thermal and crystalline properties of random copolymer of CL and DTC prepared by La(OAr)(3)

Thermal and crystalline properties of random copolymer of epsilon-caprolactone (CL) and 2,2-dimethyl trimethylene carbonate (DTC) prepared by lanthanum tris(2,6-di-tert-butyl-4-methylphenolate) (La(OAr)(3)) have been investigated by differential scanning calorimetry (DSC), thermogravimetric analysis (TG) and wide-angle X-ray diffraction (WAXD). Fox equation interprets the relationship between glass transition temperature (T-g) and copolymer compositions. T-g decreases from PDTC (16.7degreesC) to PCL (-65.1degreesC), reflecting the internal plasticizing effect of CL units on DTC units in the copolymers. The introduction of CL units to PDTC can effectively improve its heat resistance. Small amount of DTC (5% molar) in PCL chain improves the mechanical properties of the polymer, which had elongation of 1000, much higher than that of PCL (8.8).

Hydrothermal synthesis, structure, and characterization of two one-dimensional chainlike hybrid complexes [(CuX)(2)(o-phen)](infinity) (X = Br, Cl; o-phen = o-phenanthroline)

Two novel organic-inorganic hybrid complexes [(CuX)(2)(o-phen)](infinity) (X = Br (1), Cl (2); o-phen = o-phenanthroline) have been synthesized hydrothermally and characterized structurally by elemental analyses, IR, ESR, XPS spectrum, TG analyses and single-crystal X-ray diffraction. Both title compounds exhibit novel one-dimensional chainlike copper halide scaffolding constructed by the unusual [Cu3X3] hexagon motifs by sharing opposite edges, where a single Cu site of each [Cu3X3] hexagon is chelated with N donors of o-phen group. To our knowledge, such basic o-phen-copper halide skeleton has not been reported hitherto. Moreover, TG analyses indicate that both title compounds possess high thermal stability.

Synthesis of substituted indenyl lanthanide chloride and molecular structure of [(C5H9C9H6)(2)Yb(mu-Cl)(2)Li(Et2O)(2)]

Reaction of anhydrous ytterbium trichlorides with 2 equiv. of cyclopentylindenyl lithium in THF solution, followed by removal of the solvent MO. crystallization of the product from diethyl ether, affords a crystal complex of the composition (C5H9C9H6)(2)Yb(mu-Cl)(2)Li(Et2O)(2). Crystallographic analysis shows that the ytterbium coordinated by two cyclopentylindenyl rings and lithium surrounded by two ether molecules are bridged by the two chlorine atoms and Yb, U and two chlorine atoms form a plane.

离子色谱法测定AgNO_3中的微量Cl~-、NO_2~-和SO_4~(2-)

用离子色谱法测定AgNO_3溶液中的Cl~-、NO_2~-和SO_4~(2-),以5.0mmol/L Na_2CO_3-5.0mmol/L NaHCO_3混合溶液作淋洗液,采用离子交换法将AgNO_3转换成KNO_3,以除去Ag~+。讨论了NO_3~-对Cl~-、NO_2~-和SO_4~(2-)测定的影响。AgNO_3溶液中Cl~-、NO_2~-和SO_4~(2-)的回收率分别为93.3％、108％和94％。

Luminescence properties of Eu(phen)(2)Cl-3 doped in sol-gel-derived SiO2-PEG matrix

Rare earth complex Eu(phen)(2)Cl-3 was introduced into a SiO2-PEG-400 hybrid material by a sol-ger method. The result indicated that Poly(ethylene glycol) (PEG) could associate with Eu3+ and change the surroundings of Eu3+ in the hybrid material, greatly improving the decay time. Transparent SiO2-PEG400 hybrid doped with a very small amount of Eu(phen)(2)Cl-3 has better mechanical properties and can retain excellent luminescence properties of the rare earth complex. (C) 2000 Elsevier Science B.V. All rights reserved.

[Ni(OXPN) Ni(phen)_2 ](Cl O_4)_2 · 2H_2O的合成和性质

合成了新的双核配合物 [Ni(OXPN) Ni(phen) 2 ](Cl O4) 2 · 2 H2 O[OXPN=N,N′-双 - (3-氨丙基 )草酰胺 ],并进行了表征 .测定了对应单晶 [Ni(OXPN) Ni(phen) 2 ](Cl O4) 2 · 2 H2 O· CH3OH的结构及变温磁化率 (4～ 30 0 K) ,表明该配合物属 P1 空间群 ,a=0 .96 6 5 (4) nm,b=1.32 71(7) nm,c=1.716 3(5 ) nm,α=90 .42 (3)°,β=94.12 (3)°,γ=110 .6 4(4)°,V=2 .0 5 35 5 nm3.两个镍原子配位环境分别为平面四边形和畸变八面体构型 .以草酰二胺桥联的 Ni- Ni核间相距 0 .5 2 6 2 nm.磁化率测定表明两个镍原子间没有磁交换作用 ,说明一个镍原子处于平面四边形配位环境

Synthesis and crystal structure of (1,3-(Bu2C5H3)-Bu-t)(2)Sm(mu-Cl)(2)Li(THF)(2)

Anhydrous SmCl3 reacts with two equal of Li(1-3-(Bu2C5H3)-Bu-t) to give a complex (1,3-(Bu2C5H3)-Bu-t)(2) Sm(mu -Cl)(2)Li(THF)(2) (C34H58Cl2LiO2Sm, M-r = 726.99), monoclinic, space group P2(1)/n, a = 10.615(2), b = 21.037(4), c = 17.166(3) Angstrom, beta = 93.60(3)degrees, V = 3825.7 (13) Angstrom (3), Z = 4, D-c = 1.262 Mg/m(3), mu = 1.699 mm(-1) and F(000) = 1508, final R = 0.0387 and wR = 0.0741 for 5320 observed[I greater than or equal to2 sigma (I)] reflections. The average Sm - C distance is 2.73 Angstrom. Sm - Cl1 and Sm - Cl2 distances are 2.719 (2) and 2. 697 (2) Angstrom, respectively. Two 1, 3-(Bu2C5H3)-Bu-t-ring centroids and two mu (2)-bridging chloride atoms around Sm atom form a distorted tetrahedron.

金属-氨基多羧酸类配合物分子结构的研究(Ⅶ)——Na_3[Hg(Ⅱ)(edta)Cl]·6H_2O配合物的合成及结构测定

各种各样的氨基多羧酸类配合物多年来一直是化学家们较为感兴趣的研究课题之一［1～4］。特别是近年来，氨基多羧酸类配体作为一些有毒重金属的排泄剂［5］和与一些放射性金属离子形成配合物后作为核医学的显影剂［6］等方面得到了广泛的应用。金属Hg是有毒的，一般…

Synthesis and characterization of a new double-cubane Mo-Fe-S cluster compound, [NEt(4)](3)[Mo2Fe6S8(mu-OMe)(3)(SPh)(3)Cl-3]

The new double-cubane cluster compound [NEt(4)](3)[Mo2Fe6S8(mu-OMe)(3)(SPh)(3)Cl-3] is synthesized from (NH4)(2)MoS4, FeCl3, Fe powder, S powder, NaSPh and NEt(4)Br in MeOH-DMF, its crystal structure is determined by X-ray crystallography, and results of XPS indicate a valence state of +4 for Mo.

Preparation and crystal structures of LaCl3(15-crown-5) and [LaCl2(phen)(H2O)(2)(mu-Cl)](2)center dot(15-crown-5)center dot MeCN

LaCl3(15-crown-5), I was prepared by the reaction of LaCl(3)nH(2)O with 15-crown-5 and bipy (2,2'-bipyridyl). [LaCl2(phen)(H2O)(2)(mu-Cl)](2) .(15-crown-5). MeCN, II, was crystallized from a mixture of LaC1(3) . nH(2)O, phen (1,10-phenanthroline) and 15-crown-5 in MeOH/MeCN, Crystal structures of these two complexes have been determined by X-ray methods. The La(III) ion in I is coordinated by three Cl anions and five oxygen atoms of a crown ether. The two metal ions in II are bridged by two Cl anions and the crown ligand is hydrogen-bonded to the coordinated water molecules to form polymeric... crown/cation/cation/crown... chains.

THE SYNTHESIS AND CRYSTAL-STRUCTURE OF [LA(OH2)(5)(PHEN)(2)]CL-3-CENTER-DOT-4H(2)O-CENTER-DOT-PHEN

[La(OH2)(5)(phen)(2)]Cl-3 4H(2)O.phen is centric, Pnna, with a = 19.946(7), b = 16.458(5), c = 12.207(4)Angstrom and D-calc = 1.57 g cm(-3) for Z = 4. The La(III) ion resides on a crystallographic twofold axis and is coordinated to four nitrogen atoms (fr

TRIS(TERT-BUTYLCYCLOPENTADIENYL)NEODYMIUM-MU-CHLORO-TRIS(TETRAHYDROFURAN)LITHIUM, [ND(ETA(5)-(T)BUCP)3(MU-CL)LI(THF)3]

The title complex, tris[2(eta5)-tert-butylcyclopentadi-enyl]-mu-chloro-1:2kappa2Cl-tris(tetrahydrofuran-1kappaO)lithiumneodymium, [Nd(C9H13)3(mu-Cl)Li(C4H8O)3], consists of the neutral moiety ((t)BuCp)3Nd linked to the cation [Li(thf)3]+ by a mu-Cl bridge

SYNTHESIS AND STRUCTURE CHARACTERIZATION OF LANTHANUM [2,2,2]CRYPTATES, [LACL[2,2,2](H2O)]CL-2-CENTER-DOT-H2O AND [LA(CF3SO3)[2,2,2]1(DMF)](CF3SO3)(2)

Two lanthanum(III) [2,2,2]cryptates, [LaCl[2,2,2](H2O)]Cl-2.H2O (1) and [La(CF3SO3)[2,2,2](DMF)] (CF3SO3)(2) (2) have been prepared by the reaction of LaCl3 and La(CF3SO3)(3) with [2,2,2]cryptand, respectively and their crystal structures have been determ

钴与5－Cl－PADAB反应机理及其应用的研究

对钴与４－［（５－氯－２－吡啶）偶氮］－１，３－二氨基苯（５－Ｃｌ－ＰＡＤＡＢ）形成络合物的吸收光谱进行探讨，结果表明：试剂及络合物在不同酸度条件下形成不同型体。在酸性条件下，络合物为大阳离子，钴离子以三价形式存在，钻与试剂的络合比为１：２。在强酸性介质中，将此络合物用于光度测定钻，方法选择性及稳定性好，且灵敏度极高。对水、粮食、土壤、茶叶及维生素Ｂ＿（１２）中微量钻进行直接测定，获得满意结果。