共查询到20条相似文献,搜索用时 15 毫秒
1.
Yu Wang 《Journal of solid state chemistry》2010,183(12):2779-2785
A series of uniform, monodispersed Gd(OH)3:Eu3+ nanospheres less than 100 nm were successfully synthesized with iron ions as catalyst and DMF as solvent under the solvothermal condition. Cetyltrimethyl ammonium bromide (CTAB) and Polyvinylpyrrolidone (PVP) were performed as co-surfactant during this facile procedure should be changed as A series of uniform, monodisperse Gd(OH)3:Eu3+ nanospheres less than 100 nm in diameter were successfully synthesized with solvothermal method. Iron ion was used as catalyst and Dimethylformamide (DMF) as solvent, Cetyltrimethyl Ammonium Bromide (CTAB) and Polyvinylpyrrolidone (PVP) were performed as surfactants. Further calcination process was applied to prepare Gd2O3:Eu3+ nanoshpheres during this facile procedure. 相似文献
2.
The new complex [Ce(CH2=C(CH3)COO)2(NO3)(Phen)]2 was prepared in ethanol-aqueous solution with 8-hydroxyquinoline as the acidity regulator. Its crystal structure was determined by X-ray diffraction analysis. The title complex is triclinic, space group P1, a=1.00832(3)nm, b=1.02858(8)nm, c=1.12350(8)nm, α=113.9250(10)°, β=103.8210(10)°, γ=81.4650(10)°, V=1.03252(14)nm3, Z=1, Dc=1.700g·cm-3, F(000)=522. The coordination number of Ce3+ is nine. CCDC: 211278. 相似文献
3.
以乙酰丙酮(Hacac)、邻菲咯啉(phen)、硝酸根为配体,8-羟基喹啉为酸度调节剂合成出一个系列的镧系轻稀土四元配合物Ln(NO3)2(phen)2(CH3COCHCOCH3)(Ln=La,Ce,Pr,Nd,Sm)。配合物的结构与性质由元素分析,IR,1HNMR和TGA等表征。单晶Ce(NO3)2(phen)2(CH3COCHCOCH3)·H2O结构经由X射线衍射仪分析表明,晶体属单斜晶系,空间群P21/n,晶胞参数为a=1.11017(8)nm,b=0.98401(7)nm,c=1.34453(10)nm,β=102.0530(10)°,V=1.43641(18)nm3,Dc=1.715g·cm-3,Z=2,F(000)=742。配合物呈单核结构,中心离子Ce髥配位数为10。 相似文献
4.
I. A. Baidina I. A. Druzhinina S. A. Gromilov V. V. Tatarchuk 《Journal of Structural Chemistry》2004,45(2):335-339
Single crystals of the [PdL2(NO2)2] complex were obtained for the first time, where L is di-n-butylsulfide. Single crystal and powder diffraction studies provided new data on the molecular and crystal structure of this compound. 相似文献
5.
The title compound was synthesized by reaction of Cu(ClO4)2, picolinic acid and carbamide in C2H5OH/CH3CN solution, and characterized by single-crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group Pbca with a=14.0481(8), b=9.0130(5), c=18.626(1)?, V=2358.3(2)?3, Z=4, Dx=1.771g·cm-3, μ=1.235mm-1 and F(000)=1276. The final R factor is 0.0440 for 1434 observed reflections. The X-ray analysis revealed that the copper(Ⅱ) atom is coordinated by two picolinic ligands in the equatorial plane, while the two oxygen atoms of perchlorate occupy the axial positions of octahedron with lengthened Cu-O distances, resulting in a 4+2 elongated octahedral environment. In the compound, there also exist two protonated carbamide cations for charge balance. CCDC: 195354. 相似文献
6.
[Pb2(TNR)(NO3)2(H2O)] was prepared by reaction of the aqueous solution of lead nitrate and magnesium styphnate. The crystal structure of Pb2(TNR)(NO3)2(H2O)was determined by single crystal diffraction analysis. The crystal is triclinic, space group P1 with crystal parameters a=0.7279(2)nm,b=1.0698(2)nm,c=1.0738(2)nm;α=86.82(1)°,β=89.52(2)°,γ=83.50(2)°;V=0.8295(3)nm3,Z=2,Dc=3.201g·cm-3, F(000)=716. The final R value is 0.0358.In the crystal structure, one lead ion was represented by nine coor-dination geometry; the other was showed as ten coordination geometry. 相似文献
7.
The luminescent nanocrystalline KEu(WO4)2 and KGd0.98Eu0.02(WO4)2 have been prepared by the Pechini method. X-ray diffraction, infrared and Raman spectroscopy as well as optical spectroscopy were used to characterise the obtained materials. The crystal structure of KEu(WO4)2 was refined in I2/c space group indicating the isostructurality to KGd(WO4)2. The size of the crystalline grains depended on the annealing temperature, increasing with the increase of the temperature. The average size of crystallites of both crystals formed at 540 °C was about 50 nm. Vibrational spectra showed noticeable changes as a function of size due to, among others, phonon confinement effect. Luminescence studies did not reveal significant changes for the nanocrystallites with the lowest grain size in comparison with the bulk material. The differences observed in luminescence spectra in form of slight inhomogeneous broadening of the spectral lines and increase of the hypersensitive I0-2/I0-1 ratio point to very low symmetry of Eu3+ ions and change of the polarisation of the local vicinities of Eu3+. X-ray diffraction, vibrational and optical studies showed that the structure of the synthesised nanocrystalline KEu(WO4)2 and KGd(WO4)2:Eu is nearly the same as that found for the bulk material. The size-driven phase transitions were established for both compounds. 相似文献
8.
Nina S. Emelyanova Alexander A. Trifonov Lev N. Zakharov Alexander F. Shestakov Yuri T. Struchkov Mikhail N. Bochkarev 《Journal of organometallic chemistry》1997,540(1-2):1-6
The diphenylbutadiene-bridged gadolinium complex [GdCl2(THF)3]2(μ-Ph2C4H4) · 3THF (1) has been obtained by the reaction of Gd(III) chloride with diphenylbutadienepotassium. The molecular structure of 1 was determined by X-ray diffraction. The complex 1 has a binuclear structure in which a bridging diphenylbutadiene ligand is η4-bonded to the Gd atoms connecting two GdCl2(THF)3 units. Both Gd atoms have a distorted octahedral environment. At the Gd atom the two Cl atoms are in trans positions and the four other coordination sites are occupied by the three O atoms of THF molecules and the η4-bonded C4H4 fragment of a diphenylbutadiene ligand. In the two η4-bonded GdC4H4 fragments one of the Gd-C η4-distances is significantly elongated (2.86(3) and 2.97(3) Å) compared with other three (2.65(3)–2.69(3) and 2.67(3)—2.77(3) Å). The magnetic moment of Gd, equal to 8.1 BM, is typical for Gd3+ compounds that is evidence for a formal charge of DPBD ligand of −2 in complex 1. However, the expected distribution of the C-C bond of the diene fragment as long—short—long is not realized. 相似文献
9.
V. I. Belomestnykh L. B. Sveshnikova A. V. Churakov A. S. Kanishcheva Yu. N. Mikhailov 《Russian Journal of Inorganic Chemistry》2011,56(12):1899-1907
Single crystals of diammonium tetranitratouranylate (NH4)2[UO2(NO3)4] (I) and a new diammonium tetranitratouranylate complex with 18-crown-6 [(NH4)(18C6)]2[UO2(NO3)4] (II) have been synthesized by the reaction of diaquadinitratouranyl tetrahydrate with ammonium nitrate in a nitric acid solution
and the reaction of the same reagents with 18C6 in an ethanol solution, respectively. The X-ray diffraction analysis of compounds
I and II has been performed. Crystals of compounds I and II are monoclinic, Z = 2, space group P21/n, a = 6.4075(5) ?, b = 7.7851(7) ?, c = 12.4461(12) ?, β = 101.239(1)°, V = 608. 94(9) ?3 for compound I and a = 10.542(9) ?, b = 8.590(8) ?, c = 22.5019(19) ?, β = 101.632(1)°, V = 2058.3(3) ?3 for compound II. The [UO2(NO3)4]2− complex anion in compounds I and II contains two monodentate and two bidentate cyclic nitrato groups, and the coordination number of uranyl is 6. The 18C6 molecule
in the structure of compound II has the classic crown conformation and combined with the ammonium ion by three hydrogen bonds. Compounds I and II formed by electrostatic attraction forces between counterions are stabilized by (NH4+)NH...O(NO3−) interionic hydrogen bonds. 相似文献
10.
A. K. Pyartman V. A. Keskinov V. V. Lishchuk Ya. A. Reshetko V. E. Skobochkin 《Russian Journal of Applied Chemistry》2007,80(8):1281-1283
Phase diagram of a ternary liquid system [Th(NO3)4(TBP)2]-[UO2(NO3)2(TBP)2]-Exide 100 solvent was studied at 298.15–333.15 K.
Original Russian Text ? A.K. Pyartman, V.A. Keskinov, V.V. Lishchuk, Ya.A. Reshetko, V.E. Skobochkin, 2007, published in Zhurnal
Prikladnoi Khimii, 2007, Vol. 80, No. 8, pp. 1243–1245. 相似文献
11.
合成了离子对配合物(NO2Q1)2[Ni(mnt)2],并用元素分析和红外光谱进行了表征.单晶结构分析结果表明三斜晶系,空间群p-1.晶胞参数a=8.2240(16)A,6=10.777(2)A,c=12.137(2)A,α=72.58(3).,β=72.82(3)°,γ=68.78(3)°,V=935.4(3)A3,Z=1.(NO2Ql)+和[Ni(mnt)2]2-分别形成了完全分立的柱状堆积结构.在阴离子堆积柱内,Ni(Ⅱ)离子形成了一维均匀链.阳离子间,比邻的芳环间存在弱的π…π作用. 相似文献
12.
Michael Gerken Johnathan P. Mack Reijo J. Suontamo 《Journal of fluorine chemistry》2004,125(11):1663-1670
The salt, [N(CH3)4][IO2F2], was prepared from [N(CH3)4][IO3] and 49% aqueous HF, and characterized by Raman, infrared, and 19F NMR spectroscopy. Crystals of [N(CH3)4]2[IO2F2][HF2] were obtained by reduction of [N(CH3)4][cis-IO2F4] in the presence of [N(CH3)4][F] in CH3CN solvent and were characterized by Raman spectroscopy and single-crystal X-ray diffraction: C2/m, a = 14.6765(2) Å, b = 8.60490(10) Å, c = 13.9572(2) Å, β = 120.2040(10)°, V = 1523.35(3) Å3, Z = 4 and R = 0.0192 at 210 K. The crystal structure consists of two IO2−F2 anions that are symmetrically bridged by two H−F2 anions, forming a [F2O2I(FHF)2IO2F2]4− dimer. The symmetric bridging coordination for the H−F2 anion in this structure represents a new bonding modality for the bifluoride anion. 相似文献
13.
Wenbin Chen 《Journal of solid state chemistry》2004,177(9):3229-3234
The hydrothermal synthesis and single crystal structure of Zn3(HPO3)4·Zn(H2O)6 are reported. The structure is built-up from vertex linking ZnO4 tetrahedral and HPO3 pseudo-pyramids units, giving rise to a three-dimensional framework with large 8, 16-membered ring channels. The zincophosphite is purly inorganic with the octahedral zinc complex filled in the channel. The synthesis of system required the presence of the organic amine which is not incorporated into the structure of the product. The framework-metal complex encapsulating in the channel is the first time appeared in open-framework zincophospates and zincophosphites. Crystal data: Zn3(HPO3)4·Zn(H2O)6, M=689.52, orthorhombic, Fddd (No. 70), , , , , Z=8, , , R=0.0265, Rw=0.0406. 相似文献
14.
Lanthanoid Peroxo Complexes with μ3‐η2:η2:η2‐(O22—) Coordination. Crystal Structures of [Ln4(O2)2Cl8(Py)10] · Py mit Ln = Sm, Eu, Gd The four‐nuclear peroxo complexes [Ln4(O2)2Cl8(Py)10]·py (py = pyridine) with Ln = Sm ( 1 ·py), Eu ( 2 ·py) und Gd ( 3 ·py) are formed as pale yellow ( 1 ·py) and colourless ( 2 ·py and 3 ·py) crystals by action of atmospheric oxygen on heated solutions of the anhydrous trichlorides LnCl3 in pyridine/ diacetone alcohol (4‐hydroxy‐4‐methyl‐2‐pentanone). According to the X‐ray structural analyses the three complexes crystallize isostructural in the triclinic space group PP1¯ with two formula units per unit cell. 1—3 form centrosymmetrical molecular structures, in which the four lanthanoid atoms in coplanar array are linked via the two peroxo groups in a hitherto unobserved μ3‐η2:η2:η2 coordination. Additionally, they are bonded by four �μchloro bridges. Two of the Ln atoms complete their coordination sphere by three pyridine molecules each, the other two by two chlorine atoms and two pyridine molecules. The gadolinium compound is additionally characterized by its complete vibrational spectrum (i.r. and Raman). 相似文献
15.
The bismuth basic nitrate [Bi6O4.5(OH)3.5]2(NO3)11 crystallizes in the monoclinic space group P21 with , , , β=107.329(17)° and . Its structure has been determined from , twinned crystal X-ray data (16 781 reflections, 683 parameters, R=0.0703). It is built upon [Bi6Ox(OH)8−x](10−x)+, x=4 and x=5 hexanuclear complexes and nitrate groups. The polycationic entities are linked to the nitrate anions either by hydrogen bonds or through bismuth-oxygen coordination. Even at , the [Bi6O4(OH)4]6+ and [Bi6O5(OH)3]5+ polycations could not be observed as such, the crystal structure refinement only detecting an average [Bi6O4.5(OH)3.5]5.5+ polycation. To prove the presence of both hexanuclear complexes in the structure, we report the existence of a correlation between the bismuth-linked oxygen bond-valence parameters and the presence, or not, of hydroxyl groups. Moreover, the Raman spectrum of the new anhydrous bismuth basic nitrate is compared to those of [Bi6O5(OH)3](NO3)5·3H2O, [Bi6O4(OH)4](NO3)6·4H2O, and two yet uncharacterized bismuth nitrates. 相似文献
16.
The reaction of Ln(NO3)3·6H2O (Ln=La, Ce, Pr or Nd) with a sixfold excess of Ph3PO in acetone formed [Ln(Ph3PO)4(NO3)3]·Me2CO. The crystal structure of the La complex shows a nine-coordinate metal centre with four phosphine oxides, two bidentate and one monodentate nitrate groups, and PXRD studies show the same structure is present in the other three complexes. In CH2Cl2 or Me2CO solutions, 31P NMR studies show that the complexes are essentially completely decomposed into [Ln(Ph3PO)3(NO3)3] and Ph3PO. Similar reactions in ethanol gave [Ln(Ph3PO)3(NO3)3] only. In contrast for Ln=Sm, Eu or Gd, only the [Ln(Ph3PO)3(NO3)3] are formed from either acetone or ethanol solutions. For the later lanthanides Ln=Tb–Lu, acetone solutions of Ln(NO3)3·6H2O and Ph3PO gave [Ln(Ph3PO)3(NO3)3] only, even with a large excess of Ph3PO, but from cold ethanol [Ln(Ph3PO)4(NO3)2]NO3 (Ln=Tb, Ho–Lu) were obtained. The structure of [Lu(Ph3PO)4(NO3)2]NO3 shows an eight-coordinate metal centre with four phosphine oxides and two bidentate nitrate groups. In solution in CH2Cl2 or Me2CO the tetrakis-complexes show varying amounts of decomposition into mixtures of [Ln(Ph3PO)3(NO3)3], [Ln(Ph3PO)4(NO3)2]NO3 and Ph3PO as judged by 31P{1H} NMR spectroscopy. The [Ln(Ph3PO)3(NO3)3] also partially decompose in solution for Ln=Dy–Lu, forming some tetrakis(phosphine oxide) species. 相似文献
17.
18.
Marie-Olga Sornein Mickaël Mendes Céline Cannes Claire Le Naour Peter Nockemann Kristof Van Hecke Luc Van Meervelt Jean-Claude Berthet Christoph Hennig 《Polyhedron》2009
The complex formed by the reaction of the uranyl ion, UO22+, with bromide ions in the ionic liquids 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([Bmim][Tf2N]) and methyl-tributylammonium bis(trifluoromethylsulfonyl)imide ([MeBu3N][Tf2N]) has been investigated by UV–Vis and U LIII-edge EXAFS spectroscopy and compared to the crystal structure of [Bmim]2[UO2Br4]. The solid state reveals a classical tetragonal bipyramid geometry for [UO2Br4]2− with hydrogen bonds between the Bmim+ and the coordinated bromides. The UV–Vis spectroscopy reveals the quantitative formation of [UO2Br4]2− when a stoichiometric amount of bromide ions is added to UO2(CF3SO3)2 in both Tf2N-based ionic liquids. The absorption spectrum also suggests a D4h symmetry for [UO2Br4]2− in ionic liquids, as previously observed for the [UO2Cl4]2− congener. EXAFS analysis supports this conclusion and demonstrates that the [UO2Br4]2− coordination polyhedron is maintained in the ionic liquids without any coordinating solvent or water molecules. The mean U–O and U–Br distances in the solutions, determined by EXAFS, are, respectively, 1.766(2) and 2.821(2) Å in [Bmim][Tf2N], and, respectively, 1.768(2) and 2.827(2) Å, in [MeBu3N][Tf2N]. Similar results are obtained in both ionic liquids indicating no significant influence of the ionic liquid cation either on the complexation reaction or on the structure of the uranyl species. 相似文献
19.
The electrical conductive molecular crystals (Me3NEt)[Pd(dmit) 2]2 and (NEt4)[Pd (dmit) 2]2 (dmit = 4,5-dimercapto-1,3-dithiole-2-thione) have been prepared, and their crystal structures and conductivity-temperature
curves have been determined. The fact that the conductivity at room temperature of (Me3NEt)[Pd(dmit) 2]2 (σ = 58 Ω-1 cm-1) is much higher than that of (Net4)-[Pd(dmit)2]2 (σ = 2.2 Ω-1.cm-1) has been rationally explained by the results of energy band calculations. (MeNEt3)[Pd(dmit)2]2 belongs to monoclinic system, P21/m space group and (Net4)[Pd (dmit)2]2 belongs to triclinic system, space group. The structural conducting component of the crystals is the planar coordinative anion [Pd(dmit)2]0.5- which forms the face-to-face dimmer. [Pd(dmit)2]-
2These dimers have been further constructed to be a kind of two-dimensional (2-D) conductive molecular sheet by means of S_S
intermolecular interactions. The tiny difference of the above 2-D molecular sheets of the two title crystals has resulted
in one order of magnitude difference of conductivities. 相似文献
20.
[Cu(TO)2(H2O)4](PA)2 was prepared by mixing the aqueous solution of 1,2,4-triazol-5-one(TO) and Cu(PA)2. The molecular structure and crystal structure of the title complex was determined by X-ray single crystal diffraction method. The crystal is triclinic, space group with a=0.7321(1)nm,b=0.7474(2)nm,c=1.3649(3)nm;α=88.65(2)°,β=85.63(1)°,γ=63.35(1)°;V=0.6655(2)nm3,Z=1. The Cu2+ coordinated with two TO molecule through its 2-nitrogen atom and four water molecules and showed an octahedral configuration. 相似文献