共查询到20条相似文献,搜索用时 15 毫秒
1.
《Solid State Sciences》2007,9(1):16-20
A new molybdenum complex (C4H12N2)2[(MoV2O4)(MoVIO4)(C2O4)2]·2H2O, was solvothermally synthesized and characterized by single-crystal X-ray diffraction. The structure of the compound consists of oxalate acid-coordinated mixed-valent [MoV2O4][MoVIO4] helical chains and protonated piperazine cations. The helical chains are built up from the [MoV2O4] units and [MoVIO4] tetrahedral. The central axis about helical chain is a 2-fold screw axis. The compound crystallizes in the space group P21/n of monoclinic system with a = 11.396(2) Å, b = 14.107(3) Å, c = 15.805(3) Å, β = 102.09(3)°, V = 2484.6(9) Å3, Z = 4. Other characterizations by elemental analysis, IR, and thermal analysis for this compound are also given. 相似文献
2.
《Solid State Sciences》2001,3(1-2):121-132
The structures of the tetramethylammonium dichromate, [(CH3)4N]2Cr2O7 and trichromate, [(CH3)4N]2Cr3O10, were determined from single-crystal X-ray diffraction data. These compounds crystallize in the orthorhombic system (space group Pnma, with Z=4 and a=17.192(1) Å, b=8.55(1) Å, c=10.637(1) Å), for the dichromate and in the monoclinic system (space group P21/n, with Z=4 and a=11.366(2) Å, b=8.493(2) Å, c=20.187(4) Å, β=103.98(3)° for the trichromate. The structures consist of discrete dichromate anions (Cr2O7)2– or trichromate anions (Cr3O10)2–, respectively, stabilized by quaternary ammonium [(CH3)4N]+. Phase transitions in [(CH3)4N]2Cr2O7 have been evidenced by differential scanning calorimetry as well as a new allotropic variety of [(CH3)4N]2Cr2O7 which was characterized by X-ray powder diffraction. It crystallizes in an orthorhombic system with the unit cell parameters a=24.49(1) Å, b=8.85(1) Å, c=8.705(8) Å. 相似文献
3.
《Solid State Sciences》2007,9(11):1012-1019
Two novel inorganic–organic hybrid compounds composed of Keggin tungstocobaltate framework and cobalt(II)–N coordination complexes, K[Co(phen)2(H2O)]2[HCoW12O40]·2H2O (1) (phen = 1,10-phenanthroline) and [Co(2,2′-bipy)3]1.5{[Co(2,2′-bipy)2(H2O)][HCoW12O40]·0.5H2O (2) (bipy = bipyridine), have been synthesized under hydrothermal conditions by directly using Keggin POMs as starting materials, which were characterized by elemental analyses, IR, TG analyses and X-ray single crystal diffraction. Crystal data for compound 1: C48H41Co3KN8O44W12, triclinic, space group P-1, a = 10.918(5) Å, b = 13.401(5) Å, c = 13.693(5) Å, α = 69.291(5)°, β = 71.568(5)°, γ = 78.421(5)°, V = 1768.9(12) Å3, Z = 1; for compound 2: C130H104Co7N26O83W24, orthorhombic, space group, C2/c, a = 46.839(9) Å, b = 14.347(3) Å, c = 26.147(5) Å, α = β = γ = 90°, V = 17,570(6) Å3, Z = 4. Compound 1 exhibits a pseudo-1D chainlike structure, in which potassium ions act as linkages of Keggin unit doubly grafted by [Co(phen)2(H2O)] complex. Compound 2 represents a [Co(2,2′-bipy)2(H2O)]2+ mono-grafted Keggin tungstocobaltate derivative with 1.5[Co(2,2′-bipy)3]2+ countercations. The cyclic voltammetric behavior of 1-CPE is similar to the parent 3-CPE, but the cyclic voltammetric behavior of CoII shows a little difference. Variable-temperature magnetic susceptibility measurement of compound 1 demonstrates the presence of antiferromagnetic interactions. 相似文献
4.
The structures of tin(II)-oxalate, tin(IV)Na–EDTA and tin(IV)Na8-inositol hexaphosphate were investigated using XRD analysis. Samples were identified using the Mössbauer study, thermal analysis and FTIR spectrometry. The Mössbauer study determined two different oxidation states of tin atoms, and consequently two different tin surroundings in the end products. The tin oxalate was found to be orthorhombic with space group Pnma, a=9.2066(3) Å, b=9.7590(1) Å, c=13.1848(5) Å, V=1184.62 Å3 and Z=8. SnNa–EDTA was found to be monoclinic with space group P21/c1, a=10.7544(3) Å, b=10.1455(3) Å, c=16.5130(6) Å, β=98.59(2)°, V=1781.50(4) Å3 and Z=4. Sn(C6H6Na8O24P6) was found to be amorphous. 相似文献
5.
《Solid State Sciences》2007,9(2):205-212
SrSi2O2N2 is an important host lattice for Eu2+ doped phosphors. Its crystal structure (space group P1, a = 7.0802(2) Å, b = 7.2306(2) Å, c = 7.2554(2) Å, α = 88.767(3)°, β = 84.733(2)°, γ = 75.905(2)° and V = 358.73(2) Å3, Z = 4) is isotypic with EuSi2O2N2: highly condensed silicate layers are separated by Sr2+. The samples are characterized by pronounced real structure effects owing to pseudosymmetry of partial structures. Polysynthetic twinning with domains of various sizes is ubiquitous and oriented intergrowth of domains with different orientations has also been observed and analysed in detail by means of electron diffraction and high-resolution electron microscopy. These effects also affect the X-ray powder pattern and were taken into account in a Rietveld refinement. 相似文献
6.
《Solid State Sciences》2007,9(5):370-375
A new two-dimensional lead(II) vanadate, Ba3PbV4O14 has been synthesized by standard solid state techniques using BaCO3, PbO, and V2O5 as reagents. The structure of Ba3PbV4O14 was determined by single-crystal X-ray diffraction. Ba3PbV4O14 crystallizes in the triclinic space group P-1 (no. 2), with a = 7.2997(15) (Å), b = 7.2932(15) (Å), c = 13.379(3) (Å), α = 93.68(3)°, β = 99.68(3)°, γ = 91.49(3)°, V = 700.2(2) (Å3) and Z = 2. Ba3PbV4O14 exhibits a novel two-dimensional layered structure consisting of corner shared VO4 tetrahedra that are linked by edge shared PbO7 polyhedra, in which the Ba2+ cations occupy the interlayer region. The Pb2+ cations are in asymmetric coordination environments attributable to its lone pair. Infrared, Raman, and UV–vis diffuse reflectance spectroscopy, thermogravimetric analysis, and dipole moment calculations are also presented. 相似文献
7.
《Comptes Rendus de l''Academie des Sciences Series IIB Mechanics Physics Astronomy》2000,3(8):693-701
Rubidium strontium cyclo-triphosphate trihydrate, RbSrP3O9·3 H2O, was synthesized by reaction between cyclo-triphosphoric acid H3P3O9 and rubidium and strontium carbonates. It crystallizes in the othorhombic system, space group Pnma, with a = 9.120(1) Å, b = 8.141(1) Å, c = 15.234(1) Å, V = 1 131.1(3) Å3, Z = 4. Crystal structure determination from single crystal data collected at 300 K shows that the P3O9 groups exhibit Cs symmetry and are not connected to each other. Rubidium (distorted octahedron) and strontium (distorted square antiprism) are coordinated by oxygen and water molecules yielding the formation of infinite chains interconnected to each other and to the P3O9 groups. The IR valence vibration bands of the P3O9 cycle have been identified in the domain 1 400–650 cm–1 and related to the structural results. After water loss, the anhydrous phase crystallizes from an intermediate amorphous phase and further decomposes into Rb2SrP4O12 and SrP2O6. 相似文献
8.
《Solid State Sciences》2007,9(8):686-692
Hydrothermal reactions of 2-quinolinephosphonic acid (1) and CuSO4 or CdSO4 result in two new compounds with formula Cu(2-C9H6NPO3) (2) and Cd(2-C9H6NPO3)(H2O) (3). Compound 2 has a layer structure in which dimers of edge-sharing {CuO4N} square-pyramids are linked by {CPO3} tetrahedra through corner sharing. Compound 3 shows a new type of layer structure where chains of corner sharing {CdO5N} octahedra are connected by {CPO3} tetrahedra into an inorganic layer. The quinoline groups fill in the inter-layer spaces in both cases. Crystal data for 1: monoclinic, space group P21/c, a = 10.270(2) Å, b = 13.566(3) Å, c = 6.9818(16) Å, β = 101.916(4)°, V = 951.8(4) Å3, Z = 4. For 2: monoclinic, space group P21/c, a = 13.976(3) Å, b = 7.9398(18) Å, c = 7.8687(18) Å, β = 101.150(5)°, V = 856.7(3) Å3, Z = 4. For 3: monoclinic, space group P21/c, a = 17.164(4) Å, b = 5.4870(12) Å, c = 10.850(2) Å, β = 101.557(4)°, V = 1001.1(4) Å3, Z = 4. The magnetic measurement on 2 reveals a dominant antiferromagnetic exchange coupling between the Cu(II) centers. A quasi-reversible electrochemical reaction is observed for complex 2 immobilized on the surface of GC electrode, corresponding to the redox couple Cu2+/Cu+. The fluorescent properties of 1–3 are also investigated. 相似文献
9.
《Solid State Sciences》2001,3(5):587-592
Two members of a new family of inorganic phosphates of general formula AIBII6(P2O7)2P3O10; KMn6(P2O7)2P3O10 (a=5.405(2), b=26.918(11), c=6.660(5), β=107.31(3)°, V=925.1(9) Å3, space group P21/m, Z=2, Dcalc=3.481 Mg m−3, R=0.0377 for 2235 observed reflections) and AgMn6(P2O7)2P3O10 (a=5.424(7), b=26.97(4), c=6.627(9), β=106.81(7)°, V=928(2) Å3, space group P21/m, Z=2, Dcalc=3.716 Mg m−3, R=0.0594 for 1577 observed reflections) have been synthesized and identified by single crystal X-ray diffraction. The isostructural complexes present an interesting comparison of silver and potassium bonding. 相似文献
10.
An inorganic compound formulated as K5NH4[TeMo6O24].Te(OH)6.6H2O (1) has been isolated by conventional solution method and structurally characterized by single-crystal X-ray diffraction methods, scanning electron microscopy (SEM), IR, UV–vis spectra, and cyclic voltammetry measurements. This compound crystallizes in the monoclinic system, space group C2/c with unit a = 18.6841(1) Å, b = 10.0513(1) Å, c = 21.1065(1) Å, β = 116.495(1)°, V = 3547.49(4) Å3, Z = 4, R = 0.033 and wR (F2) = 0.087 for 3432 unique observed reflexions [I > 2σ(I)]. The crystal structure of (1) is built up from an Anderson clusters connected through hydrogen-bonding interactions into a three-dimensional supramolecular network. 相似文献
11.
《Solid State Sciences》2007,9(7):619-627
Three new crystal structures, isotypic with β-Zr2O(PO4)2, have been resolved by the Rietveld method. All crystallize with an orthorhombic cell (S.G.: Cmca) with a = 7.1393(2) Å, b = 9.2641(2) Å, c = 12.5262(4) Å, V = 828.46(4) Å3 and Z = 8 for Th(OH)PO4; a = 7.0100(2) Å, b = 9.1200(2) Å, c = 12.3665(3) Å, V = 790.60(4) Å3 and Z = 8 for U(OH)PO4; a = 7.1691(3) Å, b = 9.2388(4) Å, c = 12.8204(7) Å, V = 849.15(7) Å3 and Z = 4 for Th2O(PO4)2. By heating, the M(OH)PO4 (M = Th, U) compounds condense topotactically into M2O(PO4)2, with a change of the environment of the tetravalent cation that lowers from 8 to 7 oxygen atoms. The lower stability of Th2O(PO4)2 compared to that of U2O(PO4)2 seems to result from this unusual environment for tetravalent thorium. 相似文献
12.
《Solid State Sciences》2007,9(3-4):322-328
Electrochemical measurements demonstrate that magnesium surfaces can be protected by alkyl carboxylate. In a nearly neutral pH solution of sodium decanoate, the reduced corrosion rate and a passivation behaviour are attributed to the formation of Mg(C10H19O2)2(H2O)3 (Mg(C10)2) at the magnesium surface whereas heptanoate Mg(C7H13O2)2(H2O)3 (Mg(C7)2) is not efficient in such media. The crystal structures of the two metal carboxylates Mg(C7)2 and Mg(C10)2 are determined by X-ray diffraction. Single crystal data: Mg(C7)2, P21/a, a = 9.130(5) Å, b = 8.152(5) Å, c = 24.195(5) Å, β = 91.476(5)°, V = 1800.3(15) Å3, Dx = 1.242 g cm−3, Z = 4. Synchrotron powder data: Mg(C10)2, P21/a, a = 9.070(3) Å, b = 8.165(1) Å, c = 32.124(1) Å, β = 98.39(1)°, V = 2353.85(8) Å3, Dx = 1.188 g cm−3, Z = 4. Their layered structures are quite similar and differ mainly by the length of the hydrophobic chains. They consist of two planes of O-octahedra centred by Mg atoms, parallel to (001). The distorted octahedra are constituted by three oxygen atoms from carboxylate groups and by three oxygen atoms coming from water molecules. The layers are connected by hydrogen bonds. The carboxylate chains are located perpendicularly and on both sides of these planes. One carboxylate chain is bridging the Mg atom along [010] while the other is monodendate. The presence of structural water is confirmed by thermal analyses. 相似文献
13.
Rie Fredrickson Takagi Daisy Torino Hjelmqvist Mats Johnsson Sven Lidin 《Solid State Sciences》2009,11(1):13-17
The compounds CaCo2Te3O8Cl2, SrCo2Te3O8Cl2 and SrNi2Te3O8Cl2 were synthesized via solid–gas reactions and investigated using single-crystal X-ray diffraction. While the compound CaCo2Te3O8Cl2 formed large enough single crystals to allow for a detailed structural analysis, crystals of the Sr-containing compounds yielded evidence that they are isostructural. CaCo2Te3O8Cl2 crystallizes in the monoclinic system, space group P21/c, a = 6.537(2) Å, b = 9.088(2) Å, c = 19.500(9) Å, β = 113.36(4)°, Z = 4. It exhibits [CoO5Cl] helical chains along the [010] direction, connected by [CaO8] polyhedra, [TeO3E] tetrahedra and [TeO4E] trigonal bipyramids (the lone pair of electrons on TeIV is designated as E) to form a layer. The layers are held together only by weak van der Waals forces; the shortest interlayer distance is a Te?Cl contact of 3.432(4) Å. 相似文献
14.
Dawei Feng Cheng Wang Wentai Cheng Guobao Li Shujian Tian Fuhui Liao Ming Xiong Jianhua Lin 《Solid State Sciences》2009,11(4):845-851
A new layered compound, K4Mn3(HPO4)4(H2PO4)2 (1), has been synthesized under hydrothermal conditions. It crystallizes in the monoclinic space group P21/n with a = 8.874(2) Å, b = 6.554(1) Å, c = 18.075(4) Å, and β = 93.39(3)°. The structure consists of zigzag [Mn3O14]n chains of edge-sharing MnO6 octahedrons and MnO7 pentagonal bi-pyramids, which form layers of formula [Mn3(HPO4)4(H2PO4)2]4? in the ab plane via H2PO4 and HPO4 units with vertex-sharing. Potassium ions lie between these layers. Magnetic measurements indicate Curie–Weiss behavior above 6 K for 1. A Heisenberg model, with alternating exchange interactions J1J1J2… within the chain and exchange interactions J3J3… between the chains, is proposed to describe the magnetic behavior. 相似文献
15.
The solubilities in the three-component systems MIO3–Be(IO3)2–H2O (M = K, NH4+, Rb, Cs) were studied at 25 °C by the method of isothermal decrease of supersaturation. It has been established that double salts, K2Be(IO3)4·2H2O, (NH4)2Be(IO3)4·2H2O, and Rb2Be(IO3)4·2H2O, crystallize from the ternary solutions within wide concentration ranges. Both the X-ray powder diffraction and the spectroscopic studies (infrared and Raman) reveal that the title compounds are isostructural. They crystallize in the monoclinic space group P2/m with lattice parameters: K2Be(IO3)4·2H2O – a = 14.218(5) Å, b = 6.747(2) Å, c = 5.765(2) Å, β = 98.74(4)°, V = 546.6(2) Å3; (NH4)2Be(IO3)4·2H2O – a = 14.414(4) Å, b = 6.838(2) Å, c = 5.947(2) Å, β = 99.52(4)°, V = 578.0(2) Å3; Rb2Be(IO3)4·2H2O – a = 14.423(4) Å, b = 6.867(2) Å, c = 5.743(3) Å, β = 98.15(3)°, V = 562.9(3) Å3.Infrared spectroscopic experiments show that comparatively strong hydrogen bonds are formed in the potassium and rubidium salts as deduced from the wavenumbers of νOD of matrix-isolated HDO molecules (isotopically dilute samples) owing to the strong Be–OH2 interactions (synergetic effect). However, the IO3− ions in the ammonium compound are involved in hydrogen bonds with NH4+ ions additionally to those with water molecules and as a result of these intermolecular interactions the proton acceptor strength of the iodate ions decreases (anti-cooperative effect), thus leading to the formation of weaker hydrogen bonds in this compound (bonds of moderate strength) as compared to those formed in the potassium and rubidium ones. The normal vibrations of other entities (IO3− ions and BeO4 tetrahedra (skeleton vibrations)) are also discussed. 相似文献
16.
F.Y. Bai X.T. Li G.S. Zhu Y.H. Xing 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2010,75(5):1388-1393
A new complex of oxovanadium(IV), V2O2[(HB(pz)3)2(pyrro)2 (1) and a dimer-dithio carboxyl compound (C5H8NS2)2 (2) have been synthesized by the reaction of VOSO4·nH2O with NaHB(pz)3 and pyrrolidine dithio carboxylic acid ammonium salt. They were characterized by element analysis, IR spectra, UV–vis spectra and X-ray diffraction. Structural analyses of 1 and 2 gave the following parameters: 1, triclinic, P-1, a = 7.732(4) Å, b = 14.285(8) Å, c = 17.802(9) Å, α = 101.314(8)°, β = 92.682(9)°, γ = 92.228(9)°, V = 1923.6(18) Å3, and Z = 4; 2, monoclinic, C2/c, a = 13.857(2) Å, b = 10.4213(18) Å, c = 9.436(2) Å, β = 97.099(2), V = 1352.1(4) Å3, and Z = 4. In complex 1, vanadium atom adopts a distorted tetragonal bipyramid structure, which is typical for oxovanadium(IV) complexes. Compound 2 is a dimer-dithio carboxyl compound with S–S bond. In addition, thermal analysis was performed for analyzing the stabilization of the complexes. 相似文献
17.
Xianzhu Xu Peng Wang Rong Hao Meina Gan Fuxing Sun Guang-shan Zhu 《Solid State Sciences》2009,11(1):68-71
A novel zinc diphosphonate, Zn[HO3PCH2(C6H4)CH2PO3H] (1) was synthesized from tetraethyl para-xylylenediphosphonate, Et2O3PCH2C6H4CH2PO3Et2, and Zn (AcO)2·2H2O under solvothermal conditions. The structure of compound 1 was determined by single-crystal X-ray diffraction, which reveals that the structure crystallizes in the monoclinic space group C2/c (No. 15), with a = 22.4844(19) Å, b = 6.4361(5) Å, c = 8.1194(7) Å, β = 102.595(2)°, V = 1146.70(16) Å3, T = 298(2) K, Z = 8. The novel three-dimensional (3D) construction is simply built up from linear inorganic chains of corner-sharing four-rings of tetrahedral [ZnO4] and [PO3C] which connected adjacent chains by the organophosphorus ligand para-xylylenediphosphonate. The framework has 10 Å × 4 Å (containing the van der Waals radii of atoms) channels running along the b-axis. 相似文献
18.
《Journal of solid state chemistry》2004,177(4-5):1437-1443
Na2CoP2O7 is found in two allotropic forms. The first one is rose and belongs to the triclinic crystallographic system. The second one is blue and described in the orthorhombic system, space group Pna21, No. 33, with cell parameters a=15.378(6) Å, b=10.271(4) Å, c=7.713(2) Å and Z=8. A recent work showed that the orthorhombic phase could be considered as tetragonal: space group P42/mnm, No. 136 with a=7.706(1) Å and b=10.301(2) Å and Z=4. The optical and magnetic properties, particularly the EPR spectrum, of the divalent cobalt ion and their phenomenological simulation were of considerable help to complement the study and allowed us to specify the real structure. 相似文献
19.
《Solid State Sciences》2007,9(6):465-471
The structure of the new hybrid compound [Ni3(OH)2(tp)2(H2O)4]·2H2O (tp = C8H4O42−) has been determined ab initio from synchrotron powder diffraction data and refined with the Rietveld method: space group P-1, a = 10.2077(6) Å, b = 8.0135(5) Å, c = 6.3337(4) Å, α = 97.70 (1)°, β = 97.21(1)°, γ = 108.77(1)°, Dx = 2.124 g/cm3, Rp = 0.045, RB = 0.095 (757 independent reflections). H atoms were placed geometrically and their position optimized by DFT calculation. The repeating structural unit is the chain [Ni(1)O6]2Ni(2)O6, consisting of two edges sharing octahedrons related by the symmetry center and linked via μ3-OH to a vertex of Ni(2) octahedron. The Ni(1) coordination is ensured by two oxygen atoms from two water molecules, two OH and two oxygen atoms from carboxylate groups. The linkage of the chains by the tp anions forms infinite layers parallel to the (010) planes. Interchain hydrogen bonds between the water molecules coordinating the metal ensure the cohesion of the 2D structure. The structural and magnetic properties are compared with that of the 3D fumarate-based compound [Ni3(OH)2(fum)2(H2O)4]·2H2O (fum = C4H2O42−). 相似文献
20.
《Journal of organometallic chemistry》2005,690(24-25):5822-5831
Reaction between a chiral imidazole–amine precursor derived from (1R,2R)-trans-diaminocyclohexane and P1Cl (where P1 = PPh2, P(1,3,5-Me3C6H3)2, P(2,2′-O,O′-(1,1′-biphenyl), P((R)-(2,2′-O,O′-(1,1′-binaphthyl))) and P((S)-(2,2′-O,O′-(1,1′-binaphthyl)))) followed by RX (where R = nPr, iPr, CHPh2, X = Br; R = iPr, X = I), respectively, gives a selection of chiral imidazolium–phosphine compounds. Deprotonation of the imidazolium salt gives the corresponding NHC–P ligands that can be used in metal-mediated asymmetric catalytic applications. Catalytic reactions show that NHC–P ligands give a significantly greater rate of reaction for a palladium catalysed allylic substitution reaction in comparison to analogous di-NHC or NHC–imine ligands and that NHC–P hybrids are also effective for iridium catalysed transfer hydrogenation. 相似文献