High-quality CdSe quantum dots have been synthesized through an organometallic method with cadmium methoxide as a cadmium precursor. Without any size sorting, the FWHM (full width at half-maximum) in PL spectra almost for all CdSe samples is less than 30 nm and only 22 nm from the best sample. The emission peaks with different particle size in toluene can be tuned from 478 to 654 nm corresponding to a color change from blue-green to red.
Reaction of [(ButCp)2Er(μ-Cl)]2 with ButLi in 1 : 1 molar ratio in THF at -78°C; after work-up, afforded the trimetallic erbium tetrahydride complex [Li(THF)4] [(Bu t Cp)2 Er(μ-H) 3(μ3-H)] (1) by ββ-hydrogen elimination reaction. Crystal structure determination reveals that complex 1 has discrete ion pair structure. The anion is composed of three (ButCp)2Er units to form a triangle array connected by three bridged hydrogen atoms, and the fourth hydrogen atom coordinated to three Er3+ ions. The coordination number for each Er3+ ion is 9.
[(Bu^tCp)2Er(μ-Cl)]2(Bu^tCp=叔丁基环戊二烯基)与叔丁基锂(Bu^tLi)在四氢呋喃(THF)中按1:1的摩尔比于-78℃反应,分离得到了经β-氢消除反应形成的三核四氢稀土金属有机化合物[Li(THF)4][{(Bu^tCp)2Er(μ-H)}3(μ3-H)](1).晶体结构测定表明配合物1具有离子对结构,阴离子部分由3个(Bu^tCp)2Er单元组成,呈三角形排列,三角形的三边通过3个氢桥连接起来.另外有一个氢位于三角形内,以μ3-H方式和3个Er^3+离子配位,每个Er^3+离子的配位数为9.
报道了Mo/S柠檬酸配合物的合成及结构,并用元素分析、红外光谱、紫外可见光谱、顺磁共振、核磁、热重-差热分析等手段进行了表征,用EHMO方法研究了配合物的电子结构. 将羧基的键序与该配合物的羧基红外振动峰相关联,即羧基的键序(0.914、0.869和0.809)对应该配合物羧基 CO 的振动峰劈裂为三重峰(1 606、1 587和1 550 cm-1);解释了该配合物的羧基红外振动峰是一宽峰且有劈裂的特点.
Nanocrystalline zirconia co-doped with Yb3+ and Tm3+ ions was prepared by co-precipitation. Up-conversion luminescence of the samples doped with different Tm3+ concentrations was investigated under a 980 nm LD excitation. When x = 0.2 and 0.4, the luminescences of the two samples were mostly the same: strong blue up-conversion peaked at 474 nm and very weak red up-conversion were observed, corresponding to the transitions of 1G4 --> 3H6 and 1G4 --> 3F4 respectively. However, there was no luminescence of x = 1. Blue up-conversion luminescence of 0.2 mol% Tm3+-ions-doped nanocrystalline zirconia under different annealing temperatures was investigated. Blue up-conversion emission grew stronger with annealing temperature increasing. With pumping current increasing, blue up-conversion emission grew stronger too. By studying the sources of blue up-conversion, we concluded that it was three-photon process.
Reaction of [((BuCp)-Cp-t)(2)Er(mu-Cl)](2) with (BuLi)-Li-t in 1 : 1 molar ratio in THF at -78degreesC, after work-up, afforded the trimetallic erbium tetrahydride complex [Li(THF)(4)] [{((BuCp)-Cp-t)(2)Er(mu-H)}(3)(mu(3)-H)] (1) by beta-hydrogen elimination reaction. Crystal structure determination reveals that complex 1 has discrete ion pair structure. The anion is composed of three ((BuCp)-Cp-t)(2)Er units to form a triangle array connected by three bridged hydrogen atoms, and the fourth hydrogen atom coordinated to three Er3+ ions. The coordination number for each Er3+ ion is 9.
The reaction of 1:2 molar ratio of anhydrous YbCl3 with sodium indenyl in tetrahydrofuran (THF) resulted in the formation of [Na(THF) 6][(η5-C9H7)3Yb(μ- Cl)Yb(η5-C9H7)3] with a good yield. X-Ray analysis demonstrates that the complex consists of a disconnected ion pair formed by [(η5-C9H7) 3Yb(μ-Cl)Yb(η5-C9H7) 3] anion and the sodium cation surrounded by six THF molecules. The complex crystallizes in the triclinic system, with space group P1 with unit-cell constants a = 1.0682(2) nm, b = 1.2687(3) nm, c = 1.2869(2) nm, α = 87.323 (1)°, β = 81.755°, γ = 88.217°, V = 1.7273(1) nm3, for Z = 1. The structure was solved by direct methods and full-matrix least-squares refinement to the final R = 0.062, Rw = 0.072. [Na(THF)6][(η5-C9H7) 3Yb(μu-Cl)Yb(η5-C9H7) 3] reacted with sodium to form (C9H7) 2Yb·2THF, the structure of which was also determined by X-ray.
Y 2 O 3 : Eu nanotubes were fabricated by a surfactant assembly mechanism. The tubular structure was characterized by transmission electron microscopy. Under an ultraviolet-light excitation, the nanotubes show a relatively intense emission peak at 618 nm besides the 610 nm peak, different from that of single Y2O3:Eu nanocrystallites. The results of laser-selective excitation indicate that the emission centers near the surface of nanotube walls exhibit inhomogenously broadened spectra without spectral structures while the two sites (sites B and C) inside the nanotube walls present legible spectral structures. It is concluded by the number and peak positions of Stark levels that the sites B and C possess different site symmetries.
Five aquatributyltin-2-(dialkylthio)methylene-3-oxo-5-aryl-4-pentenoates (3) were synthesized and characterized by IR spectra, H-1 NMR spectra, C-13 NMR spectra and elemental analyses. The IR spectra of (3) show strong O-H stretching modes in the region of 3384-3455 cm(-1). In the H-1 NMR spectra of (3), signals due to the protons of an alpha-oxoketene dithioacetal segment shift upfield compared to those of free acids (2). This is indicative of the formation of the tin ester complexes. The structure of 4-O2N-C6H4CH=CHCOC(C3H4S2)CO2Sn(C4H9)(3).(H2O) (3d) was determined by X-ray diffraction and showed two molecules in an asymmetric unit cell. The tin(IV) is coordinated with three carbon atoms, an oxygen of carboxylate and an oxygen of water and forms a five-coordinate, distorted trigonal bipyramidal configuration. There is no intermolecular O-Sn coordination in (3d), but a molecule of water acts as one of the five ligands and coordinates directly to the tin atom. The tin-oxygen (water) bond distance in (3d) is discussed in relation to that in other aquatin(IV) complexes.
Silicon nanowires were prepared by a thermal evaporation of MoSi2 heating rods under controlled temperature and atmosphere. Transmission electron microscopy and selected area electron diffraction show that the nanowire consists of a crystalline Si core and an amorphous SiOx shell. There exist two major forms of nanowires possessing different morphologies and growth directions, which may indicate that different mechanisms predominate in the growth process. The photoluminescence of the Si/SiOx core-shell nanowires presents two emission bands, around 550 and 600 nm, respectively.
A novel Er3+-doped (ZnO) (P2O5) (B2O3) glass with excellent optical properties was prepared. The glasses were proved to have high stability by the investigation of the durability in boiling water. The properties of their spectra at about 1.5 mum change a lot with the concentrations of both Er3+ and B2O3. Compared with Er3+-doped into the borate glass and the zinc phosphate glass, the glass prepared in our laboratory shows a larger quenching concentration and a much broader emission band at 1.54 mum.
A novel reaction of (CH3C5H4) 3Ln·THF (Ln = Sm, Th, Ho, Yb) with cyclopentadiene obtained (C5H5)3Ln·THF in high yield. The products were characterized by elemental analyses, MS and X-ray diffraction analysis. The data of selected structure parameters of (C5H 5)3Ln·THF, such as the average distance between the penta carbon ring and the central metal, the distance between the penta carbon center or the coordinated THF and the central metal, showed that their values decreased with the increase of atomic number. It suggests that these compounds obey the "lanthanide contract" rule.
Reaction of (ArO)2Sm(THF)4 (ArO = 2,6-di-tert-butyl-4-methylphenolate) with Et2AlCl in THF gives SmCl2 (1) and (ArO)AlEt2(THF) (2) via ligand exchange. Complex 1 reacts with cyclooctatetraene (C8H8) to give [(C8H8)SmCl(THF)2]2 (3). Crystal structural determinations show that complex 2 has a monomeric structure, the aluminum atom is coordinated by two carbon atoms and two oxygen atoms, to form a distorted tetrahedron. Complex 3 has a dimeric structure, the samarium atom is coordinated by a cyclooctatetraenyl ring, two chorine atoms and two oxygen atoms, the coordination number of the central metal is 9.
(ArO)2Sm(THF)4 (ArO = 2,6-二叔丁基-4-甲基酚基)与Et2AlCl在四氢呋喃中发生配体交换反应, 生成SmCl2 (1)和(ArO)AlEt2(THF) (2).1进一步与环辛四烯(C8H8)发生氧化还原反应, 生成[(C8H8)SmCl(THF)2]2 (3).晶体结构测定表明配合物2具有单分子结构, 两个碳原子和两个氧原子与铝原子配位, 形成一个扭曲的四面体.配合物3具有双分子固态结构, 中心金属钐与一个环辛四烯、两个氯原子和两个氧原子配位, 其形式配位数为9.
In this paper, we will report the preparation of a mixed-valence polyoxometalate compound (Bu4N)(4)[PMo12O40].2DMF.H2O (TBA = tetrabutylammonium; DMF = N,N-dimethyl formamide). The title compound has been photochemically synthesized and characterized by using elemental analysis, IR, solid diffusion reflectance electronic spectra, ESR spectra, XPS, CV and X-ray single-crystal analysis. The crystal lographic data are as follows: monoclinic, P2(1)/c, a = 14.124(3), b = 17.481(4), c = 22.744(5) Angstrom, beta = 101.66(3)degrees, V = 5500(2) Angstrom(3), C70H160Mo12N6O43P, M-r = 2956.29, Z = 2, D-c = 1.785 g/cm(3), F(000) = 2970 and mu(MoKalpha) = 1.412 mm(-1). The structure has been refined to R = 0.0638 and wR = 0.1975 by full-matrix least-squares methods. The title compound is composed of four tetrabutylammonium cations, one [(PMoMo11O40)-Mo-V](4-) heteropoly anion, two N,N-dimethyl formamide and one H2O molecule.