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1.
Thulium trifluoroacetate compounds have been synthesized, Tm(CF3COO)3 · 3H2O (I) and Tm2(CF3COO)6 · 2CF3COOH · 3H2O (II). The structure of I has been refined by the Rietveld method on the basis of the structural data for Cd(CF3COO)3 · 3H2O. The structure of II has been solved in a single-crystal X-ray diffraction study. Compound I has been studied by thermal analysis. Crystals of I and II are monoclinic: for I a = 9.062(2) Å, b = 18.678(3) Å, c = 9.687(2) Å, β = 113.93(1)°, Z = 2, space group P21/c, R 1 = 0.062; for II a = 8.560(4) Å, b = 19.866(5) Å, c = 20.813(7) Å, β = 101.69(4)°, Z = 8, space group C2/c, R 1 = 0.0392. In the molecular structure of I, thulium atoms are bonded in pairs through four bridging trifluoroacetate anions to form dimers. The coordination polyhedron of the thulium atom also includes the three O atoms of the water molecules and the O atom of the monodentate trifluoroacetate group; the coordination number of the thulium atom is eight. In the chain structure of II, there are two crystallographically independent thulium atoms with coordination numbers 8 and 9. The coordination polyhedra of the Tm(1) and Tm(2) atoms are a distorted monocapped tetragonal antiprism and a distorted tetragonal antiprism, respectively. The Tm-O bond lengths are in the range 2.28(1)–2.85(2) Å. The thulium atoms are bound into chains through carboxylate groups. These chains are linked into layers through hydrogen bonds.  相似文献   

2.
Results of X-ray structural analysis, IR spectroscopy, and quantum chemical study of the [Fe3O(CH3COO)6(H2O)3]NO3·4H2O complex are reported. The crystal belongs to the monoclinic system with a=15.688(3), b=11.767(2), c=15.318(4) Å, γ=92.54(3)o, space group P21/a, R=0.078. The molecule has a trinuclear structure: three iron atoms occupy the vertices of an equilateral, triangle with an Fe−Fe distance of 3.29 Å and are bonded by the μ3-oxo and μ-CH3COO (O,O′) ligands. To each iron atom, one water molecule is coordinated. Using the obtained values of populations on 3d AO of Fe (d xy 1.34 ; d xz 1.39 ; d yz 1.46 ; ; ) and charges on oxygen atoms (O c −0.5 ; O ac −0.31 ; O w −0.31 ), we estimated the values of isomeric shift and quadrupole splitting (0.75 and 0.70 mm/sec, respectively; these are close to the experimental values of 0.75 and 0.58 mm/sec, (300 K)). Institute of Chemistry, Moldovian Academy of Sciences. Moldovian State University. Institute of Applied Physics, Moldovian Academy of Sciences. Translated fromZhurnal Strukturnoi Khimii., Vol. 35, No. 2, pp. 112–120, March–April, 1994. Translated by T. Yudanova  相似文献   

3.
The thermal decomposition of Ho(III), Er(III), Tm(III) and Yb(III) propionate monohydrates in argon was studied by means of thermogravimetry (TG), differential thermal analysis (DTA), IR-spectroscopy and X-ray diffraction (XRD). Dehydration takes place around 90?°C. It is followed by the decomposition of the anhydrous propionates to Ln2O2CO3 (Ln?=?Ho, Er, Tm or Yb) with the evolution of CO2 and 3-pentanone (C2H5COC2H5) between 300 and 400?°C. The further decomposition of Ln2O2CO3 to the respective sesquioxides Ln2O3 is characterized by an intermediate plateau extending from approximately 500?C700?°C in the TG traces. This stage corresponds to an overall composition of Ln2O2.5(CO3)0.5 but is more probably a mixture of Ln2O2CO3 and Ln2O3. The stability of this intermediate state decreases for the lighter rare-earth (RE) compounds studied. Full conversion to Ln2O3 is achieved at about 1,100?°C. The overall thermal decomposition behaviour of the title compounds is similar to that previously reported for Lu(C2H5CO2)3·H2O.  相似文献   

4.
5.
Single crystal X-ray diffraction is used to study the structure of colorless crystals isolated from the saturated aqueous solution of trivalent iron perchlorate (TIP) in 67.5% perchloric acid. It is found that the compound crystallizes in the trigonal crystal symmetry; parameters of the hexagonal unit cell: a = b = 16.079(2) ?, c = 11.369(2) ?, ?? = ?? = 90°, ?? = 120°, space group R{ie907-1}(S 6), Z = 6, ??calc = 2.021 g/cm3. The structural form of the crystal hydrate is [Fe(H2O)6]3+(ClO 4 ? )3·3H2O. The structure contains two independent complex iron cations. Each of them is in the special position {ie907-2}, but retains the regular octahedral structure: average bond lengths are r(Fe-O) = 1.997(1) ?, {ie907-3}O-Fe-O bond angles differ from 90° by only 0.93°. Independent [Fe(H2O)6]3+ cations form short H-bonds (O??O 2.64 ?) with three crystallization water molecules and somewhat longer H-bonds (O??O 2.73 ?) with three ClO 4 ? anions. The ClO 4 ? anion is disordered over two positions with occupancies of 0.62(2) and 0.37(2). Both positions correspond to the general position. The outer-sphere crystallization water molecule is characterized by the tetrahedral direction of H-bonds, which it forms with two anions and two independent [Fe(H2O)6]3+ cations. All water molecules are in the general position. The Raman spectroscopic study of polycrystalline samples reveals weak bands belonging to the internal vibrations of two types of water molecules. The least broad bands are assigned to the transitions of crystallization water molecules whose symmetry is insignificantly lowered by two anion-molecular Hbonds. Anomalously broad bands are assigned to the transitions of a coordinated water molecule whose symmetry is more lowered by intermolecular and anion-molecular H-bonds.  相似文献   

6.
Yan  Bing  Chen  Zhi-da  Wang  Shi-Xi 《Transition Metal Chemistry》2001,26(3):287-289
Using K3Mn(CN)6, DMF and Ln(NO3)3 · 6H2O (Ln = Tb, Dy or Er), novel cyano-bridged complexes Ln(DMF)4(H2O)2Mn(CN)6 · H2O (TbMn, DyMn and ErMn, respectively) were prepared and their magnetochemical properties were studied in detail. A weak antiferromagnetic interaction was found to exist between the rare earth ions and the manganese ion. Er(DMF)4(H2O)2Mn(CN)6 · H2O, in particular, exhibits long-range magnetic ordering, a higher critical temperature (T c = 17.5 K) and a stronger coercive force (H c = 980 Oe).  相似文献   

7.
Crystals of [Cr3O(CH3COO)6(H2O)3][UO2(CH3COO)3]·3H2O (I) were synthesized for the first time and studied by X-ray crystallography. The crystals of I are orthorhombic: a = 8.3561(3) ?, b = 16.8421(5) ?, c = 25.7448(9) ?, V = 3623.2(2) ?3, space group P212121, Z = 4, R = 0.0409. The structure is composed of trinuclear [Cr3O(CH3COO)6(H2O)3]+ complexes and mononuclear [UO2(CH3COO)3]? complexes classified with crystal-chemical groups A3M3B 6 2 M 3 1 (A = Cr3+, M3 = O2?, B2 = CH3COO?, M1 = H2O) and AB 3 01 (A = UO 2 2+ , B01 = CH3COO?), respectively. The complexes are bound to each other by electrostatic interactions and hydrogen bonds involving outer-sphere water molecules. The results of IR spectroscopic study of I are in good agreement with the structural data for the crystal.  相似文献   

8.
利用不同溶剂合成并测定了希土三氯醋酸盐与α,a'-联吡啶(bipy)不同比例的配合物(I)La:bipy=1:1,[La(CCl3COO)3(bipy).H2O]2和(Ⅱ)Tb:bipy=1:2,Tb(CCl3COO)3(bipy)2.H2O,结构测定表明配合物(I)与(Ⅱ)均为三斜晶系,中心离子La(或Tb)具有配位数为8的畸变四方反棱柱多面体;但是配合物(I)形成具有对称中心的二聚体。  相似文献   

9.

Abstract  

A series of 1-D lanthanide coordination polymers [Ln(μ3-OH)(pybz)(pa)] n (Ln = Er (1), Tb (2), Gd (3), Hpybz = 4-pyridin-4-yl-benzoic acid, Hpa = 2-picolinic acid) based on [Ln43-OH)4] cluster units have been hydrothermally synthesized and characterized by single crystal X-ray diffraction, IR, elemental analysis, and thermogravimetric analysis. X-ray crystal structure analyses reveal that 1–3 are isomorphous with tetragonal space group P [`4] \overline{4} 21c and comprise tetranuclear Ln–O clusters, in which four Ln3+ centers are joined together by four μ3-bridging hydroxyl groups to form cubane-like [Ln43-OH)4]8+ cores that are further linked by four μ3-pa ligands to produce 1-D chains along the c-axis.  相似文献   

10.
The salt Rb[C6H3(COO)2()] · [C6H3(COOH)3] · 2H2O (I) of trimesic acid was synthesized and its thermal stability and conductivity (10–11 ohm–1 cm–1 at 298 K) were measured. Molecular and crystal structures of I were established by X-ray diffraction analysis. Hydrogen bonding system in complex I was detected by IR and Raman spectroscopies. X-ray diffraction data agree with vibration spectroscopy data.  相似文献   

11.
A compound with the composition Nd(C6F5COO)3· H2O (I) is prepared. Single crystals are grown, and their single crystal XRD analysis of the Nd2(H2O)8(C6F5COO)6]·2H2O (II) compound is performed. The crystals are triclinic: a = 7.693(2) Å, b = 9.394(2) Å, c = 18.203(4) Å, α = 81.91(3)°, β = 84.41(3)°, γ = 88.97(3)°, Z = 1, d x = 2.223 g/cm3. The structure is composed of symmetrical molecules of the binuclear [Nd2(H2O)8(C6F5COO)6] complex and crystallization water molecules. The C6F5COO- ligands are monodentate and tridentate bridging- chelating, which results in a closure of two four-membered chelate cycles NdO2C and a four-membered metal cycle Nd2O2. The NdO9 polyhedron is a distorted one-capped tetragonal antiprism.  相似文献   

12.
The compound Na2[(UO2)2(SeO4)3(H2O)2] · 6.5H2O (I) is studied using X-ray diffraction. The compound crystallizes in the monoclinic crystal system with the unit cell parameters a = 19.7366(8) Å, b = 10.8206(4) Å, c = 21.3577(8) Å, β = 103.4311(1)°, Z = 4, and the space group P21/c, R 1 = 0.0379. Compound I is found to be a representative of the crystal-chemical group A2T 2 3 B2M 2 1 (A = UO 2 2+ ) of uranyl complexes and contains the cage group [(UO2)2(SeO4)3(H2O)2]2?.  相似文献   

13.
Cs3[UO2(CH3COO)3]2[UO2(CH3COO)(NCS)2(H2O)] (I) and Cs5[UO2(CH3COO)3]3[UO2 (NCS)4(H2O)] · 2H2O (II) have been synthesized via the reaction between uranyl acetate and cesium thiocyanate in aqueous solution. According to single-crystal X-ray diffraction data, both compounds crystallize in monoclinic system with the unit cell parameters a = 18.7036(5) Å, b = 16.7787(3) Å, c = 12.9636(3) Å, β = 92.532(1)°, space group C2/c, Z = 4, R = 0.0434 (I); and a = 21.7843(3) Å, b = 24.6436(5) Å, c = 13.1942(2) Å, β = 126.482(1)°, space group Cc, Z = 4, R = 0.0273 (II). Uranium-containing structural units of compound (I) are mononuclear [UO2(CH3COO)3]? and [UO2(CH3COO)(NCS)2(H2O)]? moieties, which correspond to the AB 3 01 and AB01M 3 1 crystallochemical groups (A = UO 2 2+ , B01 = CH3COO?, M1 = NCS? and H2O). The structure of compound II is built of [UO2(CH3COO)3]? and [UO2(NCS)4(H2O)]2? complexes, which belong to the AB 3 01 and AM 5 1 crystallochemical groups, respectively. Uranium-containing complexes in both structures are linked into a framework by hydrogen bonds and electrostatic interactions with cesium cations. The IR spectra of compounds I and II agree well with X-ray diffraction data.  相似文献   

14.
[Gd(Gly)3(H2O)2]Cl3·H2O的合成与晶体结构   总被引:1,自引:0,他引:1  
高胜利  任非  史启祯 《应用化学》2001,18(4):281-285
氯化钆;甘氨酸;固态配合物;[Gd(Gly)3(H2O)2]Cl3·H2O的合成与晶体结构  相似文献   

15.
The three title complexes, NH4[HoIII(Edta)(H2O)3] · 1.5H2O (I) (H4Edta = ethylenedianine-N,N,N′,N′-tetraacetic acid), (NH4)4[Ho 2 III (Dtpa)2] · 9H2O (II) (H5Dtpa = diethylenetriamine-N,N,N′,N″,N″-entaacetic acid), and (NH4)3[HoIII(Ttha)] · 5H2O (III) (H6 Ttha = triethylenetetramine-N,N,N′,N″,N?,N?-hexaacetic acid), have been prepared and characterized by FT-IR, elemental analyses, and single-crystal X-ray diffraction technique. Complex I has a nine-coordinate mononuclear structure with distorted monocapped square antiprismatic conformation and its crystal structure belongs to orthorhombic system and Fdd2 space group. The crystal data are as follows: a = 19.343(9), b = 35.125(17), c = 12.364(6) Å, V = 8400(7) Å3, Z = 16, M = 552.26, ρcalcd = 1.747 g cm?3 μ = 3.828 mm?1, and F(000) = 4368. Complex II has a binuclear nine-coordinate pseudomonocapped square antiprismatic conformation and its crystal structure belongs to triclinic system and space P1 group. The crystal data are as follows: a = 9.7637(16), b = 9.9722(16), c = 12.945(2) Å, α= 85.853(2)°, β = 77. 140(2)°, γ = 77.140(2)°, V = 1198.4(3) Å3, Z = 1, M = 1340.80, ρcalcd = 1.858 g cm?3, μ = 3.380 mm?1, and F(000) = 674. As for complex III, it also has nine-coordinate mononuclear structure with distorted tricapped trigonal prism and its crystal structure belongs to monoclinic system andP21/c space group. The crystal data are as follows: a = 10.349(3), b = 12.760(4), c = 23.142(7) Å, β = 91.020(6)°, V = 3055.6(16) Å3, Z = 2, M = 797.55, ρcalcd = 1.734 g cm?3, μ = 2.674 mm?1, and F(000) = 1624. The results showed that although the ligands are different from one another in the shape and the numbers of coordination atoms, they all have nine-coordinate structures. However, one of them has binuclear structure and the other two have mononuclear structures because of the difference of the ligands.  相似文献   

16.
GdⅢ的配合物常被用作MRI造影剂[1,2]. GdⅢ的离子半径和电子结构分别为0.107 8 nm和高自旋f 7, 理论预测应与氨基多羧酸类配体形成稳定的九配位配合物[3~5]. 为证实理论预测并在此基础上寻找合适的可用于定向修饰的配体以及为提高GdⅢ配合物的脂溶性使其具有更好的细胞渗透性, 选择四齿配体nta和含有脂环烃的六齿配体Cydta分别合成了GdⅢ的配合物, 并测定了它们的分子结构. 结果显示, GdⅢ与nta形成九配位配合物, GdⅢ与Cydta形成八配位配合物.  相似文献   

17.
A novel coordination polymer constructed with [Co(3,3′-bpbc)(H2O)3]·H2O(I) (3,3′-bpbc = 2,2′-bipyridine-3,3′-dicarboxylic acid) is successfully synthesized at room temperature and characterized by elemental analysis and IR spectra. The crystal structure of the complex is determined by single crystal X-ray diffraction. The unit cell parameters for complex I are: a = 9.9606(11) Å, b = 9.2552(10) Å, c = 16.0258(17) Å, β = 96.731(0)°, V = 1467.2(3) Å3, Z = 4, space group P2(1)/n. In the crystal, the cobalt(II) ion adopts a hexa-coordinate environment, and the structure units aggregate together to give birth to infinite 1D chains. The 2D and 3D framework is constructed via intermolecular hydrogen bonds.  相似文献   

18.
Compounds p-HOOCC6F4COOH · H2O (H2L · H2O), [Tb2(H2O)4(L)3 · 2H2O] n (I), and Tb2(Phen)2(L)3 · 2H2O (II) are synthesized. According to the X-ray structure analysis data, the crystal structure of H2L · H2O is built of centrosymmetric molecules H2L and molecules of water of crystallization. The crystal structure of compound I is built of layers of coordination 2D polymer [Tb2(H2O)4(L)3] n and molecules of water of crystallization. The ligands are the L2? anions performing both the tetradentate bridging and pentadentate bridging-chelating functions. The coordination polyhedron TbO9 is a distorted three-capped trigonal prism. Acid H2L manifests photoluminescence in the UV region (??max = 368 nm). Compounds I and II have the green luminescence characteristic of the Tb3+ ions, and the band with ??max = 545 nm (transition 5 D 4?? 7 F 5) is maximum in intensity. The photoluminescence intensity of compound II is higher than that for compound I.  相似文献   

19.
Abstract

A novel peroxopolyoxomolybdate compound, [N(CH3)4]3 [H(SO4)2 (MoO2(O2))3] · 3H2O, has been obtained from a strongly acidic aqueous solution of a molybdate-sulfate system as the monoclinic crystal of P2/n, a = 13.497(3), b = 15.231(4), c = 32.603(2) Å, β = 103.113(9)°, and V = 6577(2) Å3. The final R-value was 0.0986 for 395 parameters using 7162 reflections. Each of the two crystallographically independent polyanions contains three molybdenum atoms with five O2?, one O2 2?, and two sulfate groups, one of which is a tripod ligand apical to the molybdenum plane, and the other is a bipod ligand equatorial to the Mo plane.  相似文献   

20.
Journal of Structural Chemistry - New complex salts [Pd(NH3)4][Pd(NH3)3NO2][CrOx3]·H2O I, [Pd(NH3)4][Pd(NH3)3NO2][CoOx3]·H2O II, and a series of solid solutions...  相似文献   

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