Crystal structure analysis of Y2Cu2O5

Single crystals of Y₂Cu₂O₅ were obtained in the flux growth process by controlled heating of a mixture of Y₂O₃, BaO, and CuO in a molar ratio of 1820. These crystals were analyzed by a single-crystal X-ray diffraction analysis. The crystal contains polymeric chains of Cu₂O₅ interspersed by yttrium ions surrounded by octahedral arrangements of oxygen atoms. Crystal data: space group=Pna2₁,a=10.799(2) Å,b=3.4990(5) Å,c=12.459(2) Å,Z=4, 380 reflections,R=0.026,R _w=0.030.     

Synthesis and structural characterization of Na2MnP2O7 crystal

Na₂MnP₂O₇ crystals were synthesized by hydrothermal technique. Crystals obtained are in the form of single crystals of rhombohedral morphology with lattice parameters as follows: triclinic, P 1, π = 0-71069 Å, a = 6.657(3) Å, b = 6.714(6) Å, c = 6.518(4) Å, α = 112.31(6)°, β = 92.14(4)°, γ = 83.89(5)°, V = 268.0(3) ų, Z = 2, ρ_cal = 2, 3.121 g/cm³, μ = 3.121 mm^-1, F₀₀₀ = 244, goodness-of-fit on F = 1.348, final R indices with [I > 3σ(I)]R = 0051 and ωR = 0.065.     

Top-Seeded Melt-Growth of YBa2Cus3Ox Crystals for Neutron Diffraction Studies

We have grown cubic centimeter-size crystals of YBa₂Cu₃O _x suitable for neutron studies, by a top-seeded melt-growth technique. Growth conditions were optimized with an eye toward maximizing phase purity. It was found that the addition of 2% Y₂BaCuO₅ and 0.5% Pt (by mass) were required to prevent melt loss and to obtain the highest crystallinity. A neutron diffraction study on a mosaic of six such crystals found that the final Y₂BaCuO₅ concentration was 5%, while other impurity phases comprised less than 1% by volume. The oxygen content was set to x = 6.5, the crystals were detwinned, and then carefully annealed to give the well-ordered ortho-II phase. The neutron study determined that 70% of the mosaic's volume was in the majority orthorhomic domain. The neutron (006) and (110) rocking curve widths were ～1° per crystal and ～2.2° for the mosaic, and the oxygen chain correlation lengths were >100 Å in the a- and b-directions and ～50 Å in the c-direction.     

Synthesis and crystal structure of Cu2NiO(B2O5) and Cu2MgO(B2O5)

A transport reaction synthesis technique has been used to prepare single crystals of two pyroborate compounds having the formulas Cu₂NiO(B₂O₅) and Cu₂MgO(B₂O₅). The two compounds are isostructural and crystallize in the monoclinic space group P2₁/c. Cu₂NiO(B₂O₅): a=3.2003(10), b=14.775(3), c=9.097(3), β=93.28(4), V=429.4(2) Å³, Z=4; and Cu₂MgO(B₂O₅): a=3.2401(6), b=14.790(2), c=9.147(2), β=94.88(2), V=436.7(2) Å³, Z=4. The structures of Cu₂NiO(B₂O₅) and Cu₂MgO(B₂O₅) were, respectively, refined from 804 and 1000 independent reflections to the final residuals R1=0.0366, wR2=0.0911 and R1=0.0231, wR2=0.0644. Both compounds exhibit a chevron-like structure built up of ribbons, made of edge-connected copper and nickel-oxygen polyhedra, running along the (1 0 0) direction. These ribbons are connected from one another via oxygen atoms and the cohesion of the three-dimensional network is ensured by [B₂O₅] entities. Cu in part occupies the position for Ni or Mg, so that the compounds actually are solid solution compounds. Ni or Mg atoms are octahedrally coordinated by oxygen, while the two pure Cu sites show [4] and [4+1] coordination, for Cu(1) and Cu(2), respectively. The ELNES B-K edge spectra for the two compounds support that the borate group present is [B₂O₅].     

Structure and electrical properties of crystalline and glassy Ag2PbP2O7

Single crystals of Ag₂PbP₂O₇ have been prepared by melting of the crystalline phase under phosphate flux. Ag₂PbP₂O₇, isotype of Na₂PbP₂O₇, is of triclinic symmetry with the space group P(−1) (Z=2). The unit cell parameters are: a=5.502(6) Å, b=7.008(8) Å, c=10.018(9) Å, α=106.63(6)°, β=93.89(7)°, γ=110,68(6)°. The lattice of Ag₂PbP₂O₇ consists of corner-shared structural units {Pb₂P₄O₁₄}⁴⁻, which form ribbons parallel to the [010] direction. The {Pb₂P₄O₁₄}⁴⁻ units result from the association of corner-shared PbO₅ polyhedra and P₂O₇ pyrophosphate groups. The ribbons are interconnected by Pb–O–P bridges in the [100] direction and form lamina parallel to (001) plan. Silver atoms are located between two alternating lamina. Glasses with the same composition as the crystalline phase have been synthesized. A study of transport properties of Ag₂PbP₂O₇ in the crystalline and glassy forms is reported.     

High-pressure Synthesis and Physical Characterization of Y-based 1222-type Niobio–Cuprate NbSr2(Y1.5Ce0.5)Cu2O10

We have successfully synthesized a new 1222-type Y-based niobio-cuprate for the first time with the chemical composition, NbSr₂(Y_1.5Ce_0.5)Cu₂O₁₀ by a high-pressure and high-temperature (HPHT) technique under different synthesis conditions. Good quality (nearly single-phase) Nb1222Y polycrystalline sample was synthesized at 1,450^?○C and 6 GPa for 2 h. It crystallizes in a tetragonal symmetry of space group I4/mmm with lattice parameters a=b=3.863(2) Å and c=28.687(5) Å, which is isostructural with the corresponding Ru1222Y (RuSr₂(Y_1.5Ce_0.5)Cu₂O₁₀) phase. The dc-magnetic susceptibility measurements show a mixed magnetic state at ～29 K, which is apparently associated with magneto-superconductivity. The magnetic moment (M) versus field (H) curve of Nb1222Y sample measured at 1.8 K looks like a hybrid and it normally ensembles for both superconducting and a ferromagnetic curve. As the field increases, a low field diamagnetic signal emerges. However, temperature dependence of electrical resistivity of Nb1222Y did not show superconductivity, but semiconducting nature with a relatively large magnetoresistance (～6% at almost entire region). No specific heat anomaly was observed at the vicinity of the transition temperature.     

Dehydration/amine intercalation in Zn(O3PR)–H2O phosphonates: the missing link,X-ray structure of Zn(O3PCH3)

The hydrothermal synthesis of colorless crystals of Zn(O₃PCH₃) was achieved using a solution of zinc nitrate and methylphosphonic acid (1:1) in water, in the presence of thiourea. The structure was determined by single crystal X-ray diffraction [monoclinic, space group P2₁/c (No. 14), a=8.7226(9) Å, b=5.2156(7) Å, c=10.847(1) Å, V=389.48(9) ų, Z=2]. From this result, the mechanism of the structure modification taking place during the dehydration of Zn(O₃PR)–H₂O phosphonates was clearly demonstrated.     

Hybrid open-frameworks: hydrothermal synthesis,structure determinations and magnetic properties of MIL-29, two copper diphosphonates (CuII(H2O))2{O3P–X–PO3} with X=C2H4, CH2–C6H4–CH2

Two copper diphosphonates were hydrothermally synthesized using ethylenediphosphonic and p-xylenediphosphonic acids, synthesized according the Arbuzov method. The structure of (Cu^II(H₂O))₂{O₃P–CH₂–CH₂–PO₃} already described from powder data, was solved from single crystal data. Its symmetry is monoclinic (space group P2₁/c (no. 14)) with lattice parameters a=8.0670(4) Å, b=7.5889(4) Å, c=7.3997(4) Å, β=116.281(2)°, V=406.18(4) ų, Z=2. The structure of (Cu^II(H₂O))₂{O₃P–CH₂–(C₆H₄)–CH₂–PO₃} was solved by powder X-ray diffraction (space group P2₁/c (no. 14)) with lattice parameters a=10.812(1) Å, b=7.577(1) Å, c=7.412(1) Å, β=92.34(1)°, V=606.7(2) ų, Z=2. Both structures are built up from identical inorganic layers covalently linked by the organic chains which act as pillars. The inorganic layers contain dimers of edge-sharing CuO₄(H₂O) square pyramids linked by the PO₃C tetrahedra. Both compounds are antiferromagnetic at 4(1) K.     

Phase relations and crystallization of glass in the system PbO-GeO2

Thermal properties and chemical compositions of glasses suitable for crystallization of ferro-electric Pb₅Ge₃O₁₁ are described. The crystallization of lead germanate glass was investigated by DTA and X-ray diffraction. In the range from 62 to 62.5 of PbO in mole per cent, Pb₅Ge₃O₁₁ was obtained as a single phase after a heat treatment. In the chemical composition around 5PbO·3GeO₂ in the binary system of PbO-GeO₂, Pb₅Ge₃O₁₁ and two new phases of Pb₃Ge₂O₇ and Pb₃GeO₅ were found to exist. The crystal structure of Pb₃Ge₂O₇ had a hexagonal symmetry witha=10.16 Å andc=19.37 Å, and Pb₃GeO₅ was classified into orthorhombic system witha=4.85 Å,b=15.52 Å and c=11.77 Å.     

Synthesis,structure, and properties of the non-centrosymmetric borate Rb<Subscript>2</Subscript>CaB<Subscript>8</Subscript>O<Subscript>26</Subscript>H<Subscript>24</Subscript>

Single crystals of Rb₂CaB₈O₂₆H₂₄, a new non-centrosymmetric borate material, have been grown with sizes up to 8 × 5 × 3 mm³ by the slow evaporation of water solution at room temperature. The structure of the compound was determined by single-crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group P2₁2₁2₁ with a = 11.5288(3) Å, b = 12.6334(4) Å, c = 16.6966(4) Å, Z = 4 and R ₁ = 0.0405, wR ₂ = 0.1043. Ultraviolet (UV)–vis spectrum transmission is performed on the Rb₂CaB₈O₂₆H₂₄, which shows an absorption edge about 195 nm in the UV region. Thermal properties were investigated by TG–DSC analysis. The powder second-harmonic generation (SHG) intensity measured by the Kurtz-Perry method indicates that Rb₂CaB₈O₂₆H₂₄ has about one-third of KDP (KH₂PO₄).The influence of different molar ratios and evaporation speed of water solution on crystal quality and size was also performed on the reported material.     

Structure and Superconductivity of the Y4Ba8Cu12O27 Nanosuperconductor

A nanosuperconductor was prepared and characterized in the present work. The nanosuperconductor consisted of nanocrystals with superconducting transition temperature, T _c, of 88 K. Dimension of the nanocrystals is dozens nm in diameter and hundreds nm in length. The compound of the nanocrystals has a formula of Y₄Ba₈Cu₁₂O₂₇. The structure of the nanocrystals was found to be an orthorhombic perovskite, and the lattice constants were determined as a = 7.634 Å, b = 7.758 Å, and c = 11.654 Å, respectively.     

Structure of hydrogeno bis (dihydrogeno diphosphonate) trithallium: T13H(H2CH2P2O6)2

T1₃H(H₂CH₂P₂O₆)₂ was found to be monoclinic B2/b, a = 10.736 (6) Å, b = 12.382 (7) Å, c = 11.527 (4) Å, γ = 106.11 (5)°, Z = 4. The structure was solved with MULTAN and refined to R(Fo) = 0.063 for 1500 reflections measured with MoKα radiation. This structure can be described as a succession, parallel to the (100) plane, of diphosphonate groups and thallium ions layers.Hydrogen bondings are found between the diphosphonate groups' layers. This bonding conduct to the formation of anionic group (H₂CH₂P₂O₆HH₂CH₂P₂O₆)³⁻ analogous to the (H₂P₂O₇HH₂P₂O₇)³⁻ complex anion.     

Cu1.1Ta11O26.2F4.8: a Tetragonal-Tungsten–Bronze-related structure with square planar coordination of copper

The crystal structure of Cu_1.1Ta₁₁O_26.2F_4.8 was determined by single crystal X-ray diffraction in combination with HRTEM. The unit cell is orthorhombic with a=17.7128(8), b=17.1832(7) and c=3.9412(1) Å (X-ray powder data), space group Cmmm, and R=0.0327 for 594 independent reflections. The structure is related to the tetragonal tungsten bronze type structure of KNb₆O₁₅F which has 50% of the five-sided tunnels transformed into pentagonal bipyramids. The composition of the framework is CuTa₁₁(O,F)₃₁, with Cu in square planar coordination linking to two pentagonal TaX₇ bipyramids. The additional Cu atoms are located in the five-sided tunnels. The composition given to the compound was established by the X-ray refinement. The HRTEM study showed planar faults, twin and grain boundaries in the crystals. EDS-analysis indicated a somewhat higher Cu-content.     

Hydrothermal synthesis,crystal structure and characterization of LiCoP5O14·H2O: A new condensed layered penta phosphate crystals

A new family of condensed hydrated lithium cobalt penta phosphate (LiCoP₅O₁₄·H₂O) crystals were synthesized by hydrothermal technique and characterized by X-ray diffraction method. The compound crystallizes in monoclinic system with space group P21/c and cell parameters a = 10.788(4) Å, b = 9.761(3) Å, c = 9.788(5) Å, β = 101.249(1) Å, Z = 4, exhibiting layer type polymeric structure. DTA study indicates that this compound has low thermal stability and magnetically frequency dependent paramagnetic behaviour.     

Synthesis and structural study of new potassium uranyl selenates K2(H5O2)(H3O)[(UO2)2(SeO4)4(H2O)2](H2O)4 and K3(H3O)[(UO2)2(SeO4)4(H2O)2](H2O)5

Single crystals of new uranyl selenates K₂(H₅O₂)(H₃O)[(UO₂)₂(SeO₄)₄(H₂O)₂](H₂O)₄ (1) and K₃(H₃O)[(UO₂)₂(SeO₄)₄(H₂O)₂](H₂O)₅ (2) were prepared by isothermal evaporation at room temperature. The crystal structure of 1 was solved by the direct method [C2/c, a = 17.879(5), b = 8.152(5), c = 17.872(5) Å, β = 96.943(5)°, V = 2585.7(19) ų, Z = 4] and refined to R ₁ = 0.0449 (wR ₂ = 0.0952) for 2600 reflections with |F _o| ≥ 4σ _F . The structure of 2 was solved by the direct method [P2₁/c, a = 17.8377(5), b = 8.1478(5), c = 23.696(1) Å, β = 131.622(2)°, V = 2574.5(2) ų, Z = 4] and refined to R ₁ = 0.0516 (wR ₂ = 0.1233) for 4075 reflections with |F _o| ≥ 4σ _F . The structures of 1 and 2 are based on [(UO₂)₂(SeO₄)₄(H₂O)₂]^4? layers. The charge of the inorganic layer is compensated by potassium and oxonium ions arranged in the interlayer space. Each K ion is surrounded by seven O atoms belonging to uranyl selenate layers and water molecules, so that it binds with each other the adjacent uranyl selenate structural elements.     

X-Ray and High-Resolution Neutron Diffraction Studies on Nd x Y1−x Ba2Cu3O7−δ Superconductors

A synthesis of neodymium-substituted YBCO superconductor Nd _x Y_1?x Ba₂Cu₃O_7?δ (x=0,0.25,0.5,0.75,1) has been done using a dissolved method in order to obtain homogeneous crystals and higher critical current density. The effects of the substitutions on the structural and magnetic properties of the superconductors after sintering at 970 ^°C have been examined. Crystallinity of the synthesized powders was confirmed using X-ray and high-resolution neutron diffraction (XRD and HRPD) techniques. Rietveld analyses for both diffraction data sets gave increasing lattice parameters with addition of Nd content and decreasing orthorhombicity. Such addition also caused a decrease in occupancy of the oxygen in the O(4) site. Further investigation using SQUID showed critical temperature of the superconductors between 90.9 and 92.0 K. The critical current density (J _c ) was calculated from the magnetic hysteretic loop at 5 K as 40 kA?cm^?2 for Nd_0.25Y_0.75Ba₂Cu₃O_7?δ sample and 100 kA?cm^?2 for Nd_0.5Y_0.5Ba₂Cu₃O_7?δ sample. We also found that increasing Nd content on the Nd _x Y_1?x Ba₂Cu₃O_7?δ superconductor samples can improve their resilience of superconductivity and critical current density.     

A new high-T c superconductor containing thallium and its crystal structure: The “1212” phase (Tl1-x Bi x )1.33Sr1.33Ca1.33Cu2O6.667+δ

Joining YBa₂Cu₃O_6.5+δ (123 phase) and Bi₄Sr₄Ca₂Cu₄O_16+δ (4424 phase) as structurally characterized high-T _c , superconductors, the thallium-containing superconductor (Tl_.75Bi_.25)_1.33Sr_1.33Ca_1.33Cu₂O_6.667+δ with the ideal stoichiometry (Tl,Bi)₁Sr₂Ca₁Cu₂O_6.5+δ (1212 phase) is reported here. As prepared from the component oxides, 1212 has an initial deviation from resistance linearity at 120 K, a superconducting onset temperature of 92 K, and zero resistance at 75 K. The tetragonal unit cell (P4/mmm, a=3.800 Å;c=12.072 Å, deduced from powder data) contains double copper oxygen sheets (like 4424 and 123) that alternate withsingle thallium-bismuth oxygen sheets (in contrast to 4424, which containsdouble bismuth oxygen sheets), resulting in a total of three stacked perovskite-like cells (as in 123). The copper oxide sheets (with intersheet spacing 3.38 Å) are separated by Ca²⁺ and the Cu oxide sheets and (Tl,Bi) oxide sheets (with spacing 4.35 Å) are separated by Sr²⁺, Ca²⁺, and excess (Tl,Bi)³⁺. The 1212 cell constitutes the building block for the centered, more complex 4424 cell. The 1212 structure persists to Bi contents as low as 1% and can also be stabilized by Pb instead of Bi; Tl cuprates also form other superconductors with lowerT _c .     

Vortex motion in coupled DyBa2Cu3O7/(Y0.6Pr0.4)Ba2Cu3O7 heterostructures

Multilayer structures containing 24 Å thick DyBa₂Cu₃O₇ layers, separated by 96 Å of an (Y_0.6Pr_0.4)Ba₂Cu₃O₇ alloy, are studied to investigate the effect of coupling on vortex dynamics. With the magnetic field perpendicular to theab plane, and as a function of the number of superconducting layers in the structure, we find that the activation energy for flux motion increases, first linearly, and then saturates. This linear increase is taken as evidence that pancake vortices belonging to different DyBa₂Cu₃O₇ layers are stacked and have a coupled motion. Above a characteristic number of superconducting layers,N _c , shear of the vortex structures becomes important and the thermally activated process only displaces a stack ofN _c pancake vortices, meaning that the vortex lattice is turning three dimensional. In these structures we findN _c to be 2 to 3.     

New data on rubidium vanadium phosphate: Structure determination of the disordered (VV–PV) compound Rb6(V2O3)2(VO)2(PO4)4(HP2−xVxO7) with x∼0.6

Brownish crystals of Rb₆(V₂O₃)₂(VO)₂(PO₄)₄(HP_2−xV_xO₇) were prepared hydrothermally. The structure was solved from single crystal X-ray diffraction data in the non centrosymmetric orthorhombic space group Pmn2₁ (No. 31) a=13.5505(2) Å, b=7.1407(2) Å, c=14.7040(2) Å. (R₁(Fo)=0.048, wR₂(Fo²)=0.111). The structure of Rb₆(V₂O₃)₂(VO)₂(PO₄)₄(HP_2−xV_xO₇) is closely related to the previously reported M₃(V₂O₃)(VO)(PO₄)₂(HPO₄) (M=K⁺, Tl⁺) with a disordered occupation of the tetrahedral voids by V^V and P^V atoms.     

High-pressure synthesis and magnetic properties of complex oxide Y2Cd2/3Re4/3O7

A new complex oxide Y₂Cd_2/3Re_4/3O₇ with hexagonal cell parameters a = 7.3564(2) Å, c = 17.7092(5) Å (space group P3₁21, z = 6, zirkelite structure type) was synthesized from Y₃ReO₈, ReO₂, metallic Re and CdO under pressure 6 GPa and temperature 1500 °C. Magnetic susceptibility measured in the temperature range from 2 to 300 K depends little on temperature above ∼50 K and is indicative of a delocalized or intermediate character of d electrons of Re⁵⁺ cations.