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1.
Colin McMillen Carla Heyward Henry Giesber Joseph Kolis 《Journal of solid state chemistry》2011,184(11):2966-2971
Three novel hydrated borates Ba2B5O9(OH) (1), Sr2B5O9(OH) (2) and Li2Sr8B22O41(OH)2 (3) have been synthesized hydrothermally and their structures determined. Compounds (1) and (2) are isostructural, crystallizing in space group P21/c and having lattice parameters of a=6.6330(13) Å, b=8.6250(17) Å, c=14.680(3) Å, β=93.46(3)° and a=6.4970(13) Å, b=8.4180(17) Å, c=14.177(3) Å, β=94.35(3)°, respectively. Compound (3) crystallizes in P-1 with lattice parameters of a=6.4684(13) Å, b=8.4513(17) Å, c=14.881(3) Å, α=101.21(3)°, β=93.96(3)°, γ=90.67(3)°. While similar in their axis lengths, (3) differs greatly in structure and formulation from (1) and (2). The structure of (1) and (2) is contrasted to that of the well-known mineral hilgardite (Ca2B5O9Cl·H2O). 相似文献
2.
Digamber G. Porob 《Journal of solid state chemistry》2004,177(12):4535-4541
Two new compounds Ca0.5Bi3V2O10 and Sr0.5Bi3V2O10 have been synthesized in the ternary system: MO-Bi2O3-V2O5 system (M=M2+). The crystal structure of Sr0.5Bi3V2O10 has been determined from single crystal X-ray diffraction data, space group and Z=2, with cell parameters a=7.1453(3) Å, b=7.8921(3) Å, c=9.3297(3) Å, α=106.444(2)°, β=94.088(2)°, γ=112.445(2)°, V=456.72(4) Å3. Ca0.5Bi3V2O10 is isostructural with Sr0.5Bi3V2O10, with, a=7.0810(2) Å, b=7.8447(2) Å, c=9.3607(2) Å, α=106.202(1)°, β=94.572(1)°, γ=112.659(1)°, V=450.38(2) Å3 and its structure has been refined by Rietveld method using powder X-ray data. The crystal structure consists of infinite chains of (Bi2O2) along c-axis formed by linkage of BiO8 and BiO6 polyhedra interconnected by MO8 polyhedra forming 2D layers in ac plane. The vanadate tetrahedra are sandwiched between these layers. Conductivity measurements give a maximum conductivity value of 4.54×10−5 and 3.63×10−5 S cm−1 for Ca0.5Bi3V2O10 and Sr0.5Bi3V2O10, respectively at 725 °C. 相似文献
3.
The crystal structure of the new Pb2V3O8.5 has been determined and refined with final R1 and wR2 values 0.045 and 0.128, respectively, from 1063 independent single crystal reflections. It crystallizes with the P2/c space group, a=7.687(2) Å, b=5.996(2) Å, c=17.337(4) Å, and β=112.636(4)°. The structure consists of one-dimensional rutile-type chains of edge-sharing VIIIO6 octahedra parallel to the b axis. Bidentate VVO4 tetrahedra share corners with the chains to form one-dimensional columns. They are interconnected by divanadate VV2O7 to form infinite layers. In the presented work, the Pb2V3O8.5 crystal structure is compared to several closely related materials including Ba2V3O9 and the mineral Vauquelinite Pb2CuCrO4PO4OH. Special attention is given to the existence along the rutile chains of V-V pairs due to strong V-O bonds with O2 bridging edges. 相似文献
4.
Three new compounds Ca(HF2)2, Ba4F4(HF2)(PF6)3 and Pb2F2(HF2)(PF6) were obtained in the system metal(II) fluoride and anhydrous HF (aHF) acidified with excessive PF5. The obtained polymeric solids are slightly soluble in aHF and they crystallize out of their aHF solutions. Ca(HF2)2 was prepared by simply dissolving CaF2 in a neutral aHF. It represents the second known compound with homoleptic HF environment of the central atom besides Ba(H3F4)2. The compounds Ba4F4(HF2)(PF6)3 and Pb2F2(HF2)(PF6) represent two additional examples of the formation of a polymeric zigzag ladder or ribbon composed of metal cation and fluoride anion (MF+)n besides PbF(AsF6), the first isolated compound with such zigzag ladder. The obtained new compounds were characterized by X-ray single crystal diffraction method and partly by Raman spectroscopy. Ba4F4(HF2)(PF6)3 crystallizes in a triclinic space group P1¯ with a=4.5870(2) Å, b=8.8327(3) Å, c=11.2489(3) Å, α=67.758(9)°, β=84.722(12), γ=78.283(12)°, V=413.00(3) Å3 at 200 K, Z=1 and R=0.0588. Pb2F2(HF2)(PF6) at 200 K: space group P1¯, a=4.5722(19) Å, b=4.763(2) Å, c=8.818(4) Å, α=86.967(10)°, β=76.774(10)°, γ=83.230(12)°, V=185.55(14) Å3, Z=1 and R=0.0937. Pb2F2(HF2)(PF6) at 293 K: space group P1¯, a=4.586(2) Å, b=4.781(3) Å, c=8.831(5) Å, α=87.106(13)°, β=76.830(13)°, γ=83.531(11)°, V=187.27(18) Å3, Z=1 and R=0.072. Ca(HF2)2 crystallizes in an orthorhombic Fddd space group with a=5.5709(6) Å, b=10.1111(9) Å, c=10.5945(10) Å, V=596.77(10) Å3 at 200 K, Z=8 and R=0.028. 相似文献
5.
Jun-Ho Kim 《Journal of solid state chemistry》2008,181(8):2108-2112
Two new tellurites, NH4RbTe4O9·2H2O and NH4CsTe4O9·2H2O have been synthesized and characterized. The compounds were synthesized hydrothermally, in near quantitative yields, using the alkali metal halide, TeO2, and NH4OH as reagents. The iso-structural materials exhibit layered, two-dimensional structural topologies consisting of TeOx (x=3, 4, or 5) polyhedra separated by NH4+, H2O, Rb+ or Cs+ cations. Unique to these materials is the presence of TeO3, TeO4, and TeO5 polyhedra. Thermogravimetric and infrared spectroscopic data are also presented. Crystal data: NH4RbTe4O9·2H2O: Monoclinic I2/a (no. 15), a=18.917(3) Å, b=6.7002(11) Å, c=21.106(5) Å, β=101.813(2)°, V=2618.5(9) Å3, Z=8; NH4CsTe4O9·2H2O: Monoclinic I2/a (no. 15), a=18.9880(12) Å, b=6.7633(4) Å, c=21.476(2) Å, β=102.3460(10)°, V=2694.2(3) Å3, Z=8. 相似文献
6.
Seong-Ju Hwang 《Journal of solid state chemistry》2004,177(10):3640-3649
The quaternary alkali-metal gallium selenostannates, Na2−xGa2−xSn1+xSe6 and AGaSnSe4 (A=K, Rb, and Cs), were synthesized by reacting alkali-metal selenide, Ga, Sn, and Se with a flame melting-rapid cooling method. Na2−xGa2−xSn1+xSe6 crystallizes in the non-centrosymmetric space group C2 with cell constants a=13.308(3) Å, b=7.594(2) Å, c=13.842(3) Å, β=118.730(4)°, V=1226.7(5) Å3. α-KGaSnSe4 crystallizes in the tetragonal space group I4/mcm with a=8.186(5) Å and c=6.403(5) Å, V=429.1(5) Å3. β-KGaSnSe4 crystallizes in the space group P21/c with cell constants a=7.490(2) Å, b=12.578(3) Å, c=18.306(5) Å, β=98.653(5)°, V=1705.0(8) Å3. The unit cell of isostructural RbGaSnSe4 is a=7.567(2) Å, b=12.656(3) Å, c=18.277(4) Å, β=95.924(4)°, V=1741.1(7) Å3. CsGaSnSe4 crystallizes in the orthorhombic space group Pmcn with a=7.679(2) Å, b=12.655(3) Å, c=18.278(5) Å, V=1776.1(8) Å3. The structure of Na2−xGa2−xSn1+xSe6 consists of a polar three-dimensional network of trimeric (Sn,Ga)3Se9 units with Na atoms located in tunnels. The AGaSnSe4 possess layered structures. The compounds show nearly the same Raman spectral features, except for Na2−xGa2−xSn1+xSe6. Optical band gaps, determined from UV-Vis spectroscopy, range from 1.50 eV in Na2−xGa2−xSn1+xSe6 to 1.97 eV in CsGaSnSe4. Cooling of the melts of KGaSnSe4 and RbGaSnSe4 produces only kinetically stable products. The thermodynamically stable product is accessible under extended annealing, which leads to the so-called γ-form (BaGa2S4-type) of these compounds. 相似文献
7.
M.G. Krzhizhanovskaya R.S. Bubnova O.L. Belousova 《Journal of solid state chemistry》2010,183(10):2352-2357
Single crystals of Sr3B2SiO8 were obtained by solid-state reaction of stoichiometric mixture at 1200 °C. The crystal structure of the compound has been solved by direct methods and refined to R1=0.064 (wR=0.133). It is orthorhombic, Pnma, a=12.361(4), b=3.927(1), c=5.419(1) Å, V=263.05(11) Å3. The structure contains zigzag pseudo-chains running along the b axis and built up from corner sharing (Si,B)−O polyhedra. Boron and silicon are statistically distributed over one site with their coordination strongly disordered. Sr atoms are located between the chains providing three-dimensional linkage of the structure.The formation of Sr3B2SiO8 has been studied using annealing series in air at 900-1200 °C. According powder XRD, the probe contains pure Sr3B2SiO8 over 1100 °C. The compound is not stable below 900 °C. In the pseudobinary Sr2B2O5-Sr3B2SiO8 system a new series of solid solutions Sr3−xB2Si1−xO8−3x (x=0-0.9) have been crystallized from melt. The thermal behavior of Sr3B2SiO8 was investigated using powder high-temperature X-ray diffraction (HTXRD) in the temperature range 20-900 °C. The anisotropic character of thermal expansion has been observed: αa= −1.3, αb=23.5, αc=13.9, and αV=36.1×10−6 °C−1 (25 °C); αa= −1.3, αb=23.2, αc=5.2, and αV=27.1×10−6 °C−1 (650 °C). Maximal thermal expansion of the structure along of the chain direction [0 1 0] is caused by the partial straightening of chain zigzag. Hinge mechanism of thermal expansion is discussed. 相似文献
8.
Wenwu Zhao Shilie Pan Jian Han Jiyong Yao Yun Yang Junjie Li Min Zhang Lian Han Zhang Yin Hang 《Journal of solid state chemistry》2011,184(11):2849-2853
A new compound, Pb2BO3F, has been grown by high temperature solution method from the PbO–PbF2–B2O3 system for the first time. The crystal structure of this compound has been identified by single crystal X-ray diffraction analysis. It crystallizes in the hexagonal system, space group P63/m (No. 176) with unit-cell parameters a=7.2460(3) Å, c=14.5521(17) Å, Z=6, V=661.69(9) Å3. Its structure was solved by the direct methods and refined to R1=0.0163 and wR2=0.0367. The structure of Pb2BO3F consists of the distorted PbO3F2 groups and BO3 triangles, which are all symmetric with each other in the gestalt structure to the extent that the Pb2BO3F compound crystallizes in the symmetric space group. The powder X-ray diffraction pattern of the Pb2BO3F has been measured. The BO3 functional groups presented in the sample were identified by FTIR spectrum. The DTA curve of Pb2BO3F suggests that Pb2BO3F melts congruently at 448 °C. 相似文献
9.
The two new compounds, Sr4Cu3(AsO4)2(AsO3OH)4·3H2O (1) and Ba2Cu4(AsO4)2(AsO3OH)3(2), were synthesized under hydrothermal conditions. They represent previously unknown structure types and are the first compounds synthesized in the systems SrO/BaO-CuO-As2O5-H2O. Their crystal structures were determined by single-crystal X-ray diffraction [space group C2/c, a=18.536(4) Å, b=5.179(1) Å, c=24.898(5) Å, β=93.67(3)°, V=2344.0(8) Å3, Z=4 for 1; space group P42/n, a=7.775(1) Å, c=13.698(3) Å, V=828.1(2) Å3, Z=2 for 2]. The crystal structure of 1 is related to a group of compounds formed by Cu2+-(XO4)3− layers (X=P5+, As5+) linked by M cations (M=alkali, alkaline earth, Pb2+, or Ag+) and partly by hydrogen bonds. In 1, worth mentioning is the very short hydrogen bond length, D···A=2.477(3) Å. It is one of the examples of extremely short hydrogen bonds, where the donor and acceptor are crystallographically different. Compound 2 represents a layered structure consisting of Cu2O8 centrosymmetric dimers crosslinked by As1φ4 tetrahedra, where φ is O or OH, which are interconnected by Ba, As2 and hydrogen bonds to form a three-dimensional network. The layers are formed by Cu2O8 centrosymmetric dimers of CuO5 edge-sharing polyhedra, crosslinked by As1O4 tetrahedra. Vibrational spectra (FTIR and Raman) of both compounds are described. The spectroscopic manifestation of the very short hydrogen bond in 1, and ABC-like spectra in 2 were discussed. 相似文献
10.
F. SediriN. Etteyeb N. SteunouC. Guyard-Duhayon J. MaquetN. Gharbi J. Livage 《Journal of solid state chemistry》2002,167(2):407-411
A new layered vanadium oxide [H3N(CH2)4NH3](V6O14) was synthesized hydrothermally under autogenous pressure at 180°C for 48 h from a mixture of H2N(CH2)4NH2 and V2O5 in aqueous solution. Its structure was determined from single-crystal X-ray diffraction at room temperature with final R=0.0774 and Rw=0.0893. It crystallizes in the monoclinic system (space group P21/n with a=9.74(2) Å, b=6.776(5) Å, c=12.60(2) Å, β=96.1(1)°, V=827(2) Å3 and Z=2). This compound contains mixed-valence V5+/V4+ vanadium oxide layers built from [VVO4] tetrahedra and pairs of edge-sharing [VIVO5] square pyramids with protonated organic amines occupying the interlayer space. 相似文献
11.
S. Obbade C. Dion M. Saadi S. Yagoubi F. Abraham 《Journal of solid state chemistry》2004,177(11):3909-3917
A new lead uranyl divanadate, PbUO2(V2O7), has been synthesized by high temperature solid-state reaction and its crystal structure was solved by direct methods using single-crystal X-ray diffraction data. It crystallizes in the monoclinic system with space group P21/n and following cell parameters: a=6.9212(9) Å, b=9.6523(13) Å, c=11.7881(16) Å, β=91.74(1)°, V=787.01(2) Å3, Z=4, ρmes=5.82(3), ρcal=5.83(1) g/cm3. A full-matrix least-squares refinement on the basis of F2 yielded R1=0.029 and wR2=0.064 for 2136 independent reflections with I>2σ(I) collected with a Bruker AXS diffractometer (MoKα radiation). The crystal structure of PbUO2(V2O7) consists of a tri-dimensional framework resulting from the association of V2O7 divanadate units formed by two VO4 tetrahedra sharing corner and UO7 uranyl pentagonal bipyramids and creating one-dimensional elliptic channels occupied by the Pb2+ ions. In PbUO2(V2O7), infinite ribbons of four pentagons wide are formed which can be deduced from the sheets with Uranophane type anion-topology that occurs, for example, in the uranyl divanadate (UO2)2(V2O7), by replacement of half-U atoms of the edge-shared UO7 pentagonal bipyramids by Pb atoms. Infrared spectroscopy was investigated at room temperature in the frequency range 400-4000 cm−1, showing some characteristic bands of uranyl ion and of VO4 tetrahedra. 相似文献
12.
In order to search for new ionic conductor materials exhibiting a columnar [Bi12O14] structural type, the syntheses of the solid solutions Bi2Mo1−xCrxO6 and Bi26Mo10−xCrxO69 have been undertaken. Single phases were obtained for the last composition with 0≤x≤5 homogeneity range. Moreover, a new oxide with Bi6Cr2O15 composition has been obtained from the limit nominal stoichiometries Bi6CrO6 and Bi26Cr10O69. X-ray powder diffraction studies have shown that this oxide crystallizes in the orthorhombic system, space group Ccc2 or Cccm, with unit-cell parameters a=19.8986(9) Å, b=12.2756(6) Å, c=5.8868(3) Å, and V=1437.96 Å3. Impedance spectroscopy measurements carried out on the representative Bi26Mo8Cr2O69 phase, showed that this material is a good oxygen ion conductor, in fact the best one belongs to the columnar structural type, with a conductivity as high as 1.7×10−3Scm−1 at 425°C. 相似文献
13.
R.V Shpanchenko V.V Chernaya J Hadermann C Geibel 《Journal of solid state chemistry》2003,173(1):244-250
The new complex oxide Na2SrV3O9 was synthesized and investigated by means of X-ray diffraction, electron microscopy and magnetic susceptibility measurements. This oxide has a monoclinic unit cell with parameters a=5.416(1) Å, b=15.040(3) Å, c=10.051(2) Å, β=97.03(3)°, space group P21/c and Z=4. The crystal structure of Na2SrV3O9, as determined from X-ray single-crystal data, is built up from isolated chains formed by square V4+O5 pyramids. Neighboring pyramids are linked by two bridging V5+O4 tetrahedra sharing a corner with each pyramid. The Na and Sr atoms are situated between the chains. Electron diffraction and HREM investigations confirmed the crystal structure. The temperature dependence of the susceptibility indicates low-dimensional magnetic behavior with a sizeable strength of the magnetic intra-chain exchange J of the order of 80 K, which is very likely due to superexchange through the two VO4 tetrahedra linking the magnetic V4+ cations. 相似文献
14.
Stéphane A. BaudronCécile Mézière Karine HeuzéMarc Fourmigué Patrick Batail Philippe MoliniéPascale Auban-Senzier 《Journal of solid state chemistry》2002,168(2):668-674
[EDO-TTF-CONH2][TCNQF4], triclinic system, space group P-1, a=8.2479(12) Å, b=12.282(2) Å, c=12.6842(18) Å, α=113.850(17)°, β=106.420(17)°, γ=90.284(19)°, V=1116.8(4) Å3; and [EDT-TTF-CONH2]2[TCNQF4], triclinic system, space group P-1, a=6.5858(9) Å, b=11.699(2) Å, c=12.2281(18) Å, α=104.000(19)°, β=93.611(17)°, γ=98.279(19)°, V=899.9(3) Å3, whose π-donor molecules, (ethylenedioxo)-carbamoyltetrathiafulvalene and (ethylenedithio)-carbamoyltetrathiafulvalene, respectively, differ solely by the nature of the chalcogen atoms in their outer ethylene dichalcogeno bridge, yet form very different charge-transfer complexes with the same π-acceptor. [EDO-TTF-CONH2•+]2 [TCNQF4•−]2 is a diamagnetic insulating ionic salt with a three-dimensional rock-salt-type structure based on discrete dimers while in the semi-conducting mixed-valence complex, [EDT-TTF-CONH2]2•+[TCNQF4•−], the mixed-valence dimers aggregate into infinite chains interspersed within parallel rows of non-interacting radical anions. It is shown how the robust and adaptable supramolecular amide hydrogen bond tweezers-like motifs common to the two solids simply comply to the 3-to-1 dimensionality reduction upon substitution of O for S. 相似文献
15.
Johannes Reisch Raouf A. Hussain Bernt Krebs Mechtild Dartmann 《Monatshefte für Chemie / Chemical Monthly》1990,121(11):941-944
Summary C15H24O2,M=236.2, monoclinic, P 21,a=7.229(7),b=14.925 (9),c=6.235 (9) Å, =92.40 (9)°,V=672.1 Å3,T=–133 °C,Z=2,D
x=1.17 g cm–3. The X-ray diffraction analysis of this sesquiterpenoid fromCarissa opaca confirmed the previously proposed constitution of the isolate and, furthermore, allowed precise NMR assignment.
Naturstoffchemie, 100. Mitt.: Die Struktur des Carissons, C15H24O2
Zusammenfassung C15H24O2,M=236.2, monoklin, P 21,a=7.229 (7),b=14.925 (9),c=6.235 (9) Å, =92.40 (9)°,V=672.1 Å3,T=–133 °C,Z=2,D x=1.17 g cm–3. Die Röntgenstrukturanalyse dieses Sesquiterpenoids ausCarissa opaca bestätigte die bereits vorgeschlagene Struktur und erlaubte ferner eine genaue NMR-Zuordnung.相似文献
16.
Two organic-inorganic hybrid compounds, Ga2(4,4′-bpy)(PO4)2, 1, and Ga2(4,4′-bpy)(AsO4)2, 2, have been synthesized under hydrothermal conditions and structurally characterized by single-crystal X-ray diffraction. The two compounds are isostructural and crystallize in the triclinic space group (No. 2) with a=4.9723(9) Å, b=5.770(1) Å, c=11.812(2) Å, α=78.268(3)°, β=89.159(3)° γ=88.344(3)°, V=331.7(2) Å3, Z=1, and R1=0.0377 for 1, and a=5.1111(7) Å, b=5.9327(8) Å, c=11.788(2) Å, α=79.497(2)°, β=88.870(2)°, γ=88.784(2)°, V=351.3(2) Å3, and R1=0.0264 for 2. The structure consists of neutral sheets of GaXO4 (X=P or As) which are pillared through 4,4′-bipyridine ligands. Each oxide layer, which is formed only by four-membered rings, is constructed from corner-sharing GaO4N trigonal bipyramids and XO4 tetrahedra. The title compounds are two of the few examples in which the gallium atoms are exclusively five-coordinate. 相似文献
17.
18.
A molybdenum (IV) phosphate containing lead, Pb2Mo2(PO4)2P2O7, has been synthesized for the first time. It crystallizes in the space group C2/c with a=14.098(1) Å, b=14.187(2) Å, c=6.5592(4) Å and β=102.08(1)°. Its original tunnel structure, built up of Mo2O11 bioctahedra, P2O7 and PO4 phosphate groups can be described from the assemblage of [Mo4P4O24]∞ ribbons interconnected through monophosphate groups. The stereoactivity of the 6s2 lone pair of Pb2+, which is surrounded by nine oxygen atoms, is discussed. 相似文献
19.
The high-temperature polymorphs of two photocatalytic materials, BiNbO4 and BiTaO4 were synthesized by the ceramic method. The crystal structures of these materials were determined by single-crystal X-ray diffraction. BiNbO4 and BiTaO4 crystallize into the triclinic system P1¯ (No. 2), with a=5.5376(4) Å, b=7.6184(3) Å, c=7.9324(36) Å, α=102.565(3)°, β=90.143(2)°, γ=92.788 (4)°, V=326.21 (5) Å3, Z=4 and a=5.931 (1) Å, b=7.672 (2) Å, c=7.786 (2) Å, α=102.94 (3)°, β=90.04 (3)° γ=93.53 (3)°, V=344.59 (1) Å3 and Z=4, respectively. The structures along the c-axis, consist of layers of [Bi2O2] units separated by puckered sheets of (Nb/Ta)O6 octahedra. Photocatalytic studies on the degradation of dyes indicate selectivity of BiNbO4 towards aromatics containing quinonic and azo functional groups. 相似文献
20.
Catherine Renard Pascal Roussel Annick Rubbens Sylvie Daviero-Minaud Francis Abraham 《Journal of solid state chemistry》2006,179(7):2101-2110
We report the synthesis and crystal structure of the new compound Sr4PbPt4O11, containing platinum in highly unusual square pyramidal coordination. The crystals were obtained in molten lead oxide. The structure was solved by X-ray single crystal diffraction techniques on a twinned sample, the final R factors are R=0.0260 and wR=0.0262. The symmetry is triclinic, space group P1¯, with , , , α=90.421(3)°, β=89.773(8)°, γ=90.140(9)° and Z=2. The structure is built from dumbell-shaped Pt2O9 entities formed by a dinuclear metal-metal bonded Pt26+ ion with asymmetric environments of the two Pt atoms, classical PtO4 square plane and unusual PtO5 square pyramid. Successive Pt2O9 entities deduced from 90° rotations are connected through the oxygens of the PtO4 basal squares to form [Pt4O108−]∞ columns further connected through Pb2+ and Sr2+ ions. Raman spectroscopy confirmed the peculiar platinum coordination environment. 相似文献