共查询到20条相似文献,搜索用时 31 毫秒
1.
Ming-Feng Tang 《Journal of solid state chemistry》2004,177(6):1912-1918
A new vanadium(III) oxalatophosphate has been synthesized hydrothermally and characterized by single-crystal X-ray diffraction and thermogravimetric analysis. It crystallizes in the triclinic space group with a=11.604(2) Å, b=12.391(2) Å, c=15.220(3) Å, α=71.090(3)°, β=82.630(3)°, γ=62.979(3)°, V=1843.8(5) Å3 and Z=2. The structure consists of V6(HPO4)6 double 6-ring (D6R) units connected by coordinating C2O42− and PO43− anions to form anionic sheets in the ab plane with charge-compensating quadruply protonated 1,4-bis(3-aminopropyl)piperazinium cations and water molecules between the sheets. It is one of the few compounds with 2D layer structures and the second example containing D6R units in the system of metal oxalatophosphates. The iron analogue was also synthesized. 相似文献
2.
Ba3MgSi2O8, a phosphor host examined for use in white-light devices and plant-growth lamps, was synthesized at 1225 °C in air. Its crystal structure has been determined and refined by a combined powder X-ray and neutron Rietveld method (, Z=3, a=9.72411(3) Å, c=7.27647(3) Å, V=595.870(5) Å3; Rp/Rwp=3.79%/5.03%, χ2=4.20). Superstructure reflections, observed only in the neutron diffraction data, provided the means to establish the true unit cell and a chemically reasonable structure. The structure contains three crystallographically distinct Ba atoms—Ba1 resides in a distorted octahedral site with S6 () symmetry, Ba2 in a nine-coordinate site with C3 (3) symmetry, and Ba3 in a ten-coordinate site with C1 (1) symmetry. The Mg atoms occupy distorted octahedral sites, and the Si atom occupies a distorted tetrahedral site. 相似文献
3.
Yunyin Niu Zhongjun Li Mingsheng Tang Xinquan Xin 《Journal of solid state chemistry》2006,179(12):4003-4010
A new three-dimensional non-interpenetrating coordination polymer, [{Cu(dps)2(SO4)}·3H2O·DMF]n (1) (dps=4,4′-dipyridyl sulfide) was synthesized and structurally characterized. 1 crystallizes in triclinic system, space group P−1 with cell parameters of a=10.9412(1) Å, b=11.8999(1) Å, c=12.5057(1) Å, V=1400.7(3) Å3, Z=2, Dc=1.573 g cm−3, F(0 0 0)=686, μ=1.059 mm−1. R1=0.0436, wR2=0.1148. In the polymeric architecture, serve as bridging coligands to connect highly puckered [Cu2(dps)2]n frameworks resulting in a 3D motif containing channels for guest molecule inclusion. Quantum chemistry calculation shows that the third-order NLO properties of polymer 1 are controlled by groups and dps ligands, and metal ions have less influence on the third-order NLO properties. 相似文献
4.
The anion-excess ordered fluorite-related phase Ba4Bi3F17 has been synthesized by a solid state reaction of BaF2 and BiF3 at 873 K. The crystal structure of Ba4Bi3F17 has been studied using electron diffraction and X-ray powder diffraction (a=11.2300(2) Å, c=20.7766(5) Å, S.G. , RI=0.020, RP=0.036). Interstitial fluorine atoms in the Ba4Bi3F17 structure are considered to form isolated cuboctahedral 8 : 12 : 1 clusters. The structural relationship between Ba4Bi3F17 and similar rare-earth-based phases is discussed. 相似文献
5.
6.
Magnus G. Johnston 《Journal of solid state chemistry》2004,177(12):4680-4686
The hydrothermal syntheses, single crystal structures, and some properties of Ba2MnIIMn2III(SeO3)6 and PbFe2(SeO3)4 are reported. These related phases contain three-dimensional frameworks of vertex (FeO6) and vertex/edge linked (MnO6) octahedra and SeO3 pyramids. In each case, the MO6/SeO3 framework encloses two types of 8 ring channels, one of which encapsulates the extra-framework cations and one of which provides space for the SeIV lone pairs. Crystal data: Ba2Mn3(SeO3)6, Mr=1201.22, monoclinic, P21/c (No. 14), a=5.4717 (3) Å, b=9.0636 (4) Å, c=17.6586 (9) Å, β=94.519 (1)°, V=873.03 (8) Å3, Z=2, R(F)=0.031, wR(F2)=0.070; PbFe2(SeO3)4, Mr=826.73, triclinic, (No. 2), a=5.2318 (5) Å, b=6.7925 (6) Å, c=7.6445 (7) Å, α=94.300 (2)°, β=90.613 (2)°, γ=95.224 (2)°, V=269.73 (4) Å3, Z=1, R(F)=0.051, wR(F2)=0.131. 相似文献
7.
Sukhendu Mandal 《Journal of solid state chemistry》2005,178(7):2376-2382
A hydrothermal reaction of a mixture of cobalt (II) oxalate, phosphorous acid, piperazine and water at 150 °C for 96 h followed by heating at 180 °C for 24 h gave rise to a new inorganic-organic hybrid solid, [C4N2H12][Co4(HPO3)2(C2O4)3], I. The structure consists of edge-shared CoO6 octahedra forming a [Co2O10] dimers that are connected by HPO3 and C2O4 units forming a three-dimensional structure with one-dimensional channels. The amine molecules are positioned within these channels. The oxalate units have a dual role of connecting within the plane of the layer as well as out of the plane. Magnetic susceptibility measurement shows the compound orders antiferromagnetically at low temperature (). Crystal data: I, monoclinic, space group=P21/c (No. 14). a=7.614(15), b=7.514(14), , β=97.351(3)°, , Z=2, , , R1=0.0310 and wR2=0.0807 data [I>2σ(I)]. 相似文献
8.
Bin Deng Donald E. Ellis Richard P. Van Duyne 《Journal of solid state chemistry》2005,178(10):3169-3175
The new compound K2CuSbS3 has been synthesized by the reaction of K2S, Cu, Sb, and S at 823 K. The compound crystallizes in the Na2CuSbS3 structure type with four formula units in space group P21/c of the monoclinic system in a cell at 153 K of a=6.2712 (6) Å, b=17.947 (2) Å, c=7.4901 (8) Å, β=120.573 (1)°, and V=725.81 (12) Å3. The structure contains two-dimensional layers separated by K atoms. Each layer is built from CuS3 and SbS3 units. Each Cu atom is pyramidally coordinated to three S atoms with the Cu atom about 0.4 Å above the plane of the S atoms. Each Sb atom is similarly coordinated to three S atoms but is about 1.1 Å above its S3 plane. First-principles calculations indicate an indirect band gap of 1.9 eV. These calculations also indicate that there is a bonding interaction between the Cu and Sb atoms. An optical absorption measurement performed with light perpendicular to the (0 1 0) crystal face of a red block-shaped crystal of K2CuSbS3 indicates an experimental indirect band gap of 2.2 eV. 相似文献
9.
The new vanadate BiMgVO5 has been prepared and its structure has been determined by single crystal X-ray diffraction: space group P21/n, , , , β=107.38(5)°, wR2=0.0447, R=0.0255. The structure consists of [Mg2O10] and [Bi2O10] dimers sharing their corners with [VO4] tetrahedra. The ranges of bond lengths are 2.129-2.814 Å for Bi-O; 2.035-2.167 Å for Mg-O and 1.684-1.745 Å for V-O. V-O bond lengths determined from Raman band wavenumbers are between 1.679 and 1.747 Å. An emission band overlapping the entire visible region with a maximum around 650 nm is observed. 相似文献
10.
Richard E. Sykora Brian L. Scott Thomas E. Albrecht-Schmitt 《Journal of solid state chemistry》2004,177(3):725-730
The uranyl and neptunyl(VI) iodates, K3[(UO2)2(IO3)6](IO3)·H2O (1) and K[NpO2(IO3)3]·1.5H2O (2), have been prepared and crystallized under mild hydrothermal conditions. The structures of 1 and 2 both contain one-dimensional ∞1[AnO2(IO3)3]1−(An=U,Np) ribbons that consist of approximately linear actinyl(VI) cations bound by iodate anions to yield AnO7 pentagonal bipyramids. The AnO7 units are linked by bridging iodate anions to yield chains that are in turn coupled by additional iodate anions to yield ribbons. The edges of the ribbons are terminated by monodentate iodate anions. For 1 and 2, K+ cations and water molecules separate the ribbons from one another. In addition, isolated iodate anions are also found between ∞1[UO2(IO3)3]1− ribbons in 1. In order to aid in the assignment of oxidation states in neptunyl containing compounds, a bond-valence sum parameter of 2.018 Å for Np(VI) bound exclusively to oxygen has been developed with b=0.37 Å. Crystallographic data (193 K, MoKα, λ=0.71073): 1, triclinic, , a=7.0609(4) Å, b=14.5686(8) Å, c=14.7047(8) Å, α=119.547(1)°, β=95.256(1)°, γ=93.206(1)°, Z=2, R(F)=2.49% for 353 parameters with 6414 reflections with I>2σ(I); (203 K, MoKα, λ=0.71073): 2, monoclinic, P21/c, a=7.796(4) Å, b=7.151(3) Å, c=21.79(1) Å, β=97.399(7)°, Z=4, R(F)=6.33% for 183 parameters with 2451 reflections with I>2σ(I). 相似文献
11.
Tatiana Y. Shvareva 《Journal of solid state chemistry》2005,178(2):499-504
Single crystals of the potassium uranyl iodate, K[UO2(IO3)3] (1), have been grown under mild hydrothermal conditions. The structure of 1 contains two-dimensional sheets extending in the [ab] plane that consist of approximately linear UO22+ cations bound by iodate anions to yield UO7 pentagonal bipyramids. There are three crystallographically unique iodate anions, two of which bridge between uranyl cations to create sheets, and one that is monodentate and protrudes in between the layers in cavities. K+ cations form long ionic contacts with oxygen atoms from the layers forming an eight-coordinate distorted dodecahedral geometry. These cations join the sheets together. Ion-exchange reactions have been carried out that indicate the selective uptake of Cs+ over Na+ or K+ by 1. Crystallographic data (193 K, MoKα, ): 1, orthorhombic, Pbca, a=11.495(1) Å, b=7.2293(7) Å, c=25.394(2) Å, Z=8, R(F)=1.95% for 146 parameters with 2619 reflections with I>2σ(I). 相似文献
12.
The solid-state reactions of UO3 and WO3 with M2CO3 (M=Na, K, Rb) at 650°C for 5 days result, accordingly the starting stoichiometry, in the formation of M2(UO2)(W2O8) (M=Na (1), K (2)), M2(UO2)2(WO5)O (M=K (3), Rb (4)), and Na10(UO2)8(W5O20)O8 (5). The crystal structures of compounds 2, 3, 4, and 5 have been determined by single-crystal X-ray diffraction using Mo(Kα) radiation and a charge-coupled device detector. The crystal structures were solved by direct methods and Fourier difference techniques, and refined by a least-squares method on the basis of F2 for all unique reflections. For (1), unit-cell parameters were determined from powder X-ray diffraction data. Crystallographic data: 1, monoclinic, a=12.736(4) Å, b=7.531(3) Å, c=8.493(3) Å, β=93.96(2)°, ρcal=6.62(2) g/cm3, ρmes=6.64(1) g/cm3, Z=4; 2, orthorhombic, space group Pmcn, a=7.5884(16) Å, b=8.6157(18) Å, c=13.946(3) Å, ρcal=6.15(2) g/cm3, ρmes=6.22(1) g/cm3, Z=8, R1=0.029 for 80 parameters with 1069 independent reflections; 3, monoclinic, space group P21/n, a=8.083(4) Å, b=28.724(5) Å, c=9.012(4) Å, β=102.14(1)°, ρcal=5.83(2) g/cm3, ρmes=5.90(2) g/cm3, Z=8, R1=0.037 for 171 parameters with 1471 reflections; 4, monoclinic, space group P21/n, a=8.234(1) Å, b=28.740(3) Å, c=9.378(1) Å, β=104.59(1)°, ρcal=6.13(2) g/cm3, g/cm3, Z=8, R1=0.037 for 171 parameters with 1452 reflections; 5, monoclinic, space group C2/c, a=24.359(5) Å, b=23.506(5) Å, c=6.8068(14) Å, β=94.85(3)°, ρcal=6.42(2) g/cm3, g/cm3, Z=8, R1=0.036 for 306 parameters with 5190 independent reflections. The crystal structure of 2 contains linear one-dimensional chains formed from edge-sharing UO7 pentagonal bipyramids connected by two octahedra wide (W2O8) ribbons formed from two edge-sharing WO6 octahedra connected together by corners. This arrangement leads to [UW2O10]2− corrugated layers parallel to (001). Owing to the unit-cell parameters, compound 1 probably contains similar sheets parallel to (100). Compounds 3 and 4 are isostructural and the structure consists of bi-dimensional networks built from the edge- and corner-sharing UO7 pentagonal bipyramids. This arrangement creates square sites occupied by W atoms, a fifth oxygen atom completes the coordination of W atoms to form WO5 distorted square pyramids. The interspaces between the resulting [U2WO10]2− layers parallel to plane are occupied by K or Rb atoms. The crystal structure of compound 5 is particularly original. It is based upon layers formed from UO7 pentagonal bipyramids and two edge-shared octahedra units, W2O10, by the sharing of edges and corners. Two successive layers stacked along the [100] direction are pillared by WO4 tetrahedra resulting in sheets of double layers. The sheets are separated by Na+ ions. The other Na+ ions occupy the rectangular tunnels created within the sheets. In fact complex anions W5O2010− are built by the sharing of the four corners of a WO4 tetrahedron with two W2O10 dimmers, so, the formula of compound 5 can be written Na10(UO2)8(W5O20)O8. 相似文献
13.
Deng-Ke Cao 《Journal of solid state chemistry》2006,179(2):573-578
This paper reports the syntheses and characterization of two phosphonate compounds Cd{(2-C5H4NO)CH(OH)PO3}(H2O)2 (1) and Zn{(4-C5H4NO)CH(OH)PO3} (2) based on hydroxy(2-pyridyl N-oxide)methylphosphonic and hydroxy(4-pyridyl N-oxide)methylphosphonic acids. Compound 1 has a chain structure in which dimers of edge-shared {CdO6} octahedra are linked by {CPO3} tetrahedra through corner-sharing. The pyridyl rings reside on the two sides of the inorganic chain. Compound 2 has a layer structure where the inorganic chains made up of corner-sharing {ZnO4} and {CPO3} tetrahedra are covalently connected by pyridyl N-oxide groups. Crystal data for 1: triclinic, space group , a=6.834(1) Å, b=7.539(1) Å, c=10.595(2) Å, α=84.628(3)°, β=74.975(4)°, γ=69.953(4)°. For 2: triclinic, space group , a=5.219(1) Å, b=8.808(2) Å, c=9.270(2) Å, α=105.618(5)°, β=95.179(4)°, γ=94.699(4)°. 相似文献
14.
Synthesis and single crystal structures of ternary phosphides Li4SrP2 and AAeP (A=Li, Na; Ae=Sr, Ba)
Yongkwan Dong 《Journal of solid state chemistry》2007,180(2):432-439
Two new (NaSrP, Li4SrP2) and two known (LiSrP, LiBaP) ternary phosphides have been synthesized and characterized using single crystal X-ray diffraction studies. NaSrP crystallizes in the non-centrosymmetric hexagonal space group (#189, a=7.6357(3) Å, c=4.4698(3) Å, V=225.69(2) Å3, Z=3, and R/wR=0.0173/0.0268). NaSrP adopts an ordered Fe2P structure type. PSr6 trigonal prisms share trigonal (pinacoid) faces to form 1D chains. Those chains define large channels along the [001] direction through edge-sharing. The channels are filled by chains of PNa6 face-sharing trigonal prisms. Li4SrP2 crystallizes in the rhombohedral space group (#166, a=4.2813(2) Å, c=23.437(2) Å, V=372.04(4) Å3, Z=3, and R/wR=0.0142/0.0222). In contrast to previous reports, LiSrP and LiBaP crystallize in the centrosymmetric hexagonal space group P63/mmc (#194, a=4.3674(3) Å, c=7.9802(11) Å, V=131.82(2) Å3, Z=2, and R/wR=0.0099/0.0217 for LiSrP; a=4.5003(2) Å, c=8.6049(7) Å, V=150.92(2) Å3, Z=2, and R/wR=0.0098/0.0210 for LiBaP). Li4SrP2, LiSrP, and LiBaP can be described as Li3P derivatives. Li atoms and P atoms make a graphite-like hexagonal layer, . In LiSrP and LiBaP, Sr or Ba atoms reside between layers to substitute for two Li atoms of Li3P, while in Li4SrP2, Sr substitutes only between every other layer. 相似文献
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16.
Michael A. McGuire Franck Gascoin G. Jeffrey Snyder 《Journal of solid state chemistry》2006,179(7):2158-2163
The new Chevrel phase Ti0.3Mo5RuSe8 has been synthesized and characterized by quantitative microprobe analysis, powder X-ray diffraction, and high-temperature thermoelectric properties measurements. The thermoelectric properties of this compound are compared to the previously reported data for other related Chevrel phases. We report also the results of Rietveld analysis of powder X-ray diffraction data for Ti0.3Mo5RuSe8. This compound adopts the rhombohedral Chevrel phase structure (space group , Z=3) with hexagonal lattice constants a=9.75430(25) Å and c=10.79064(40) Å. The low level of incorporation and low scattering power of Ti precluded the identification of the Ti positions, and Rietveld refinement was carried out only for the Mo5RuSe8 framework of Ti0.3Mo5RuSe8 (Rp=10.5%, Rwp=14.6%). Rietveld analysis was also used to refine the structure of the unfilled phase Mo5RuSe8 (, Z=3, a=9.63994(8) Å, c=10.97191(11) Å, Rp=8.0%, Rwp=10.5%). Comparisons between the two structures are made. 相似文献
17.
The first example of a unidimensional zirconium hydroxide fluoride was synthesized under mild solvothermal treatment and characterized by X-ray diffraction and thermal techniques. Monoprotonated ethylenediamine cations reside between the anionic chains. Crystal data for this material are as follows: [C2N2H9][Zr(OH)2F3], M=243.35, orthorhombic, space group Pca21, a=6.8016(13), b=6.1393(12), , , , Z=4, , μ(Mo-Kα)=1.777 mm−1, . The material transforms to an unknown layered material at ∼175 °C, a common occurrence for 1D structures where the chains are arranged in hydrogen-bonded layers and separated by interlayer organoammoniums. Collapse to the known condensed mineral phase Zr(FO)2.7 occurs at ca. 275 °C before finally transforming to the baddeleyite form of ZrO2 at ca. 460 °C. 相似文献
18.
Employing 3-dimethylamino-1-propylamine as a template, a new three-dimensional (3-D) zincophosphite (C5H16N2)·[Zn3(HPO3)4]·H2O has been prepared under hydrothermal conditions and characterized by single-crystal X-ray diffraction (XRD), FTIR, elemental analysis, powder XRD, and thermogravimetric analysis (TGA). The compound crystallizes in the triclinic space group , with cell parameters, a=8.9884(2) Å, b=10.326(2) Å, c=11.917(2) Å, α=66.98(3)°, β=89.01(3)°, and γ=78.98(3)°, V=997.2(3) Å3 and Z=2. The connectivity of the ZnO4 tetrahedra and HPO3 pseudo pyramids results in inifinite edge-sharing, ladderlike chains of 4-membered rings, which are further linked by Zn-O-P bonds to form a 3-D structure that with interesting 12-membered ring channels along the [100] and [001] directions. The diprotonated amine molecules sit in the middle of the channels along the [100] direction and interact with the framework via hydrogen bonds. There also exist channels with 8-membered ring window along the [100] and [010] directions. 相似文献
19.
New ternary bismuth iron niobates having structures based on chemical twinning of pyrochlore are described. Bi5.67Nb10FeO35 has hexagonal symmetry, P63/mmc, , , Z=2 and Bi9.3Nb16.9Fe1.1O57.8 has rhombohedral symmetry, R-3m, , , Z=3. The structures of both phases were determined and refined to R1=0.04 using single-crystal X-ray data. They can be described as being derived from the pyrochlore structure by chemical twinning on (111)py oxygen planes. The chemical twin operation produces pairs of corner-connected hexagonal tungsten bronze (HTB) layers as in the HTB structure, so the structures may alternatively be described as pyrochlore:HTB unit-cell intergrowth structures. In the hexagonal phase the pyrochlore blocks have a width of 12 Å, whereas the rhombohedral phase has pyrochlore blocks of two widths, 6 and 12 Å, alternating with HTB blocks. It is proposed that the previously reported binary 4Bi2O3:9Nb2O5 phase has a related structure containing pyrochlore blocks all of width 6 Å. A feature of the structures is partial occupancy (∼65%) of the Bi sites and displacement of the Bi atoms from the ideal pyrochlore A sites towards the surrounding oxygen atoms, as observed in Bi-containing pyrochlores. 相似文献
20.
Dongrong Xiao Haiyan An Jian Lü Yangguang Li Lin Xu Changwen Hu 《Journal of solid state chemistry》2004,177(8):2699-2704
A novel three-dimensional (3D) transition metal selenite Fe3(H2O)(SeO3)3 (1) has been hydrothermally synthesized and characterized by the elemental analyses, IR spectrum, TG analysis and the single-crystal X-ray diffraction. Compound 1 crystallizes in the triclinic system, space group , with a=8.0916(16) Å, b=8.2089(16) Å, c=8.5679(17) Å, α=69.21(3)°, β=62.74(3)°, γ=67.16(3)°, Z=2, and R1[I>2σ(I)]=0.0379. Compound 1 exhibits an interesting 3D framework formed by {FeO6} octahedra and {SeO3} trigonal pyramids via the corner- and/or edge-sharing mode. Furthermore, compound 1 consists of left-handed and right-handed helical chains, which are further entangled to form the double helical chains. 相似文献