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1.
Yb3Cu6Sn5, Yb5Cu11Sn8 and Yb3Cu8Sn4 compounds were prepared in sealed Ta crucibles by induction melting and subsequent annealing. The crystal structures of Yb3Cu6Sn5 and Yb5Cu11Sn8 were determined from single crystal diffractometer data: Yb3Cu6Sn5, isotypic with Dy3Co6Sn5, orthorhombic, Immm, oI28, a=4.365(1) Å, b=9.834(3) Å, c=12.827(3) Å, Z=2, R=0.019, 490 independent reflections, 28 parameters; Yb5Cu11Sn8 with its own structure, orthorhombic, Pmmn, oP48, a=4.4267(6) Å, b=22.657(8) Å, c=9.321(4) Å, Z=2, R=0.047, 1553 independent reflections, 78 parameters. Both compounds belong to the BaAl4-derived defective structures, and are closely related to Ce3Pd6Sb5 (oP28, Pmmn). The crystal structure of Yb3Cu8Sn4, isotypic with Nd3Co8Sn4, was refined from powder data by the Rietveld method: hexagonal, P63mc, hP30, a=9.080(1) Å, c=7.685(1) Å, Z=2, Rwp=0.040. It is an ordered substitution derivative of the BaLi4 type (hP30, P63/mmc). All compounds show strong Cu-Sn bonds with a length reaching 2.553(3) Å in Yb5Cu11Sn8.  相似文献   

2.
Two uranyl tellurates, AgUO2(HTeO5) (1) and Pb2UO2(TeO6) (2), were synthesized under hydrothermal conditions and were structurally, chemically, and spectroscopically characterized. 1 crystallizes in space group Pbca, a=7.085(2) Å, b=11.986(3) Å, c=13.913(4) Å, V=1181.5(5) Å3, Z=8; 2 is in P2(1)/c, a=5.742(1) Å, b=7.789(2) Å, c=7.928(2) Å, V=90.703(2) Å3, and Z=2. These are the first structures reported for uranyl compounds containing tellurate. The U6+ cations are present as (UO2)2+ uranyl ions that are coordinated by O atoms to give pentagonal and square bipyramids in compounds 1 and 2, respectively. The structural unit in 1 is a sheet consisting of chains of edge-sharing uranyl pentagonal bipyramids that are one bipyramid wide, linked through the dimers of TeO6 octahedra. In 2, uranyl square bipyramids share each of their equatorial vertices with different TeO6 octahedra, giving a sheet with the autunite-type topology. Sheets in 1 and 2 are connected through the low-valence cations that are located in the interlayer region. The structures of 1 and 2 are compared to those of uranyl compounds containing octahedrally coordinated cations.  相似文献   

3.
The title compounds have been obtained by solid state reactions of the corresponding pure elements at high temperature, and structurally characterized by single-crystal X-ray diffraction studies. Yb5Ni4Sn10 adopts the Sc5Co4Si10 structure type and crystallizes in the tetragonal space group P4/mbm (No. 127) with cell parameters of a=13.785(4) Å, c=4.492 (2) Å, V=853.7(5) Å3, and Z=2. Yb7Ni4Sn13 is isostructural with Yb7Co4InGe12 and crystallizes in the tetragonal space group P4/m (No. 83) with cell parameters of a=11.1429(6) Å, c=4.5318(4) Å, V=562.69(7) Å3, and Z=1. Both structures feature three-dimensional (3D) frameworks based on three different types of one-dimensional (1D) channels, which are occupied by the Yb atoms. Electronic structure calculations based on density functional theory (DFT) indicate that both compounds are metallic. These results are in agreement with those from temperature-dependent resistivity and magnetic susceptibility measurements.  相似文献   

4.
Quaternary chalcogenides InSn2Bi3Se8 and In0.2Sn6Bi1.8Se9 were synthesized on direct combination of their elements in stoichiometric ratios at T>800 °C under vacuum. Their structures were determined with X-ray diffraction of single crystals. InSn2Bi3Se8 crystallizes in monoclinic space group C2/m (No. 12) with a=13.557(3) Å, b=4.1299(8) Å, c=15.252(3) Å, β=115.73(3)°, V=769.3(3) Å3, Z=2, and R1/wR2/GOF=0.0206/0.0497/1.092; In0.2Sn6Bi1.8Se9 crystallizes in orthorhombic space group Cmc21 (No. 36) with a=4.1810(8) Å, b=13.799(3) Å, c=31.953(6) Å, V=1843.4(6) Å3, Z=4, and R1/wR2/GOF=0.0966/0.2327/1.12. InSn2Bi3Se8 and In0.2Sn6Bi1.8Se9 are isostructural with CuBi5S8 and Bi2Pb6S9 phases, respectively. The structures of InSn2Bi3Se8 and In0.2Sn6Bi1.8Se9 feature a three-dimensional framework containing slabs of NaCl-(311) type with varied thicknesses. Calculations of the electronic structure and measurements of electrical conductivity indicate that these materials are semiconductors with narrow band gaps. Both compounds show n-type semiconducting properties with Seebeck coefficients −270 and −230 μV/K at 300 K for InSn2Bi3Se8 and In0.2Sn6Bi1.8Se9, respectively.  相似文献   

5.
Two new isostructural cobalt selenite halides Co5(SeO3)4Cl2 and Co5(SeO3)4Br2 have been synthesized. They crystallize in the triclinic system space group P−1 with the following lattice parameters for Co5(SeO3)4Cl2: a=6.4935(8) Å, b=7.7288(8) Å, c=7.7443(10) Å, α=66.051(11)°, β=73.610(11)°, γ=81.268(9)°, and Z=1. The crystal structures were solved from single-crystal X-ray data, R1=3.73 and 4.03 for Co5(SeO3)4Cl2 and Co5(SeO3)4Br2, respectively. The new compounds are isostructural to Ni5(SeO3)4Br2.Magnetic susceptibility measurements on oriented single-crystalline samples show anisotropic response in a broad temperature range. The anisotropic susceptibility is quantitatively interpreted within the zero-field splitting schemes for Co2+ and Ni2+ ions. Sharp low-temperature susceptibility features, at TN=18 and 20 K for Co5(SeO3)4Cl2 and Co5(SeO3)4Br2, respectively, are ascribed to antiferromagnetic ordering in a minority magnetic subsystem. In isostructural Ni5(SeO3)4Br2 magnetically ordered subsystem represents a majority fraction (TN=46 K). Nevertheless, anisotropic susceptibility of Ni5(SeO3)4Br2 is dominated at low temperatures by a minority fraction, subject to single-ion anisotropy effects and increasing population of Sz=0 (singlet) ground state of octahedrally coordinated Ni2+.  相似文献   

6.
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.
Na6Co2O6 was synthesized via the azide/nitrate route by reaction between NaN3, NaNO3 and Co3O4. Stoichiometric mixtures of the starting materials were heated in a special regime up to 500°C and annealed at this temperature for 50 h in silver crucibles. Single crystals have been grown by subsequent annealing of the reaction product at 500°C for 500 h in silver crucibles, which were sealed in glass ampoules under dried Ar. According to the X-ray analysis of the crystal structure (, Z=1, a=5.7345(3), b=5.8903(3), c=6.3503(3) Å, α=64.538(2), β=89.279(2), γ=85.233(2)°, 1006 independent reflections, R1=8.34% (all data)), cobalt is tetrahedrally coordinated by oxygen. Each two CoO4 tetrahedra are linked through a common edge forming Co2O66- anions. Cobalt ions within the dimers, being in a high spin state (S=2), are ferromagnetically coupled (J=17 cm-1). An intercluster spin exchange (zJ′=−4.8 cm-1) plays a significant role below 150 K and leads to an antiferromagnetically ordered state below 30 K. Heat capacity exhibits a λ-type anomaly at this temperature and yields a value of 19.5 J/mol K for the transition entropy, which is in good agreement with the theoretical value calculated for the ordering of the ferromagnetic-coupled dimers. In order to construct a model for the spin interactions in Na6Co2O6, the magnetic properties of Na5CoO4 have been measured. This compound features isolated CoO4 tetrahedra and shows a Curie-Weiss behavior (μ=5.14 μB, Θ=−20 K) down to 15 K. An antiferromagmetic ordering is observed in this compound below 10 K.  相似文献   

8.
The crystal structures of the two new synthetic compounds Co2TeO3Cl2 and Co2TeO3Br2 are described together with their magnetic properties. Co2TeO3Cl2 crystallize in the monoclinic space group P21/m with unit cell parameters a=5.0472(6) Å, b=6.6325(9) Å, c=8.3452(10) Å, β=105.43(1)°, Z=2. Co2TeO3Br2 crystallize in the orthorhombic space group Pccn with unit cell parameters a=10.5180(7) Å, b=15.8629(9) Å, c=7.7732(5) Å, Z=8. The crystal structures were solved from single crystal data, R=0.0328 and 0.0412, respectively. Both compounds are layered with only weak interactions in between the layers. The compound Co2TeO3Cl2 has [CoO4Cl2] and [CoO3Cl3] octahedra while Co2TeO3Br2 has [CoO2Br2] tetrahedra and [CoO4Br2] octahedra. The Te(IV) atoms are tetrahedrally [TeO3E] coordinated in both compounds taking the 5s2 lone electron pair E into account. The magnetic properties of the compounds are characterized predominantly by long-range antiferromagnetic ordering below 30 K.  相似文献   

9.
A new ternary compound, U3Co2Ge7, has been synthesized from the corresponding elements by a high temperature reaction using molten tin flux. It crystallizes in the orthorhombic La3Co2Sn7-type (Pearson's symbol oC24, space group Cmmm, No. 65) with lattice parameters determined from single-crystal X-ray diffraction as follows: a=4.145(2) Å; b=24.920(7); c=4.136(2) Å, V=427.2(3) Å3. Structure refinements confirm an ordered structure having two crystallographically inequivalent uranium atoms, occupying sites with dissimilar coordination. U3Co2Ge7 orders ferromagnetically below 40 K and undergoes a consecutive magnetic transition at 20 K. These results have been obtained from temperature- and field-dependent magnetization, resistivity and heat-capacity measurements. The estimated Sommerfeld coefficient γ=87 mJ/mol-U K2 suggests U3Co2Ge7 to be a moderately heavy-fermion material.  相似文献   

10.
A new dabcodiium-templated nickel sulphate, (C6H14N2)[Ni(H2O)6](SO4)2, has been synthesised and characterised by single-crystal X-ray diffraction at 20 and −173 °C, differential scanning calorimetry (DSC), thermogravimetry (TG) and temperature-dependent X-ray powder diffraction (TDXD). The high temperature phase crystallises in the monoclinic space group P21/n with the unit-cell parameters: a = 7.0000(1), b = 12.3342(2), c = 9.9940(2) Å; β = 90.661(1)°, V = 862.82(3) Å3 and Z = 2. The low temperature phase crystallises in the monoclinic space group P21/a with the unit-cell parameters: a = 12.0216(1), b = 12.3559(1), c = 12.2193(1) Å; β = 109.989(1)°, V = 1705.69(2) Å3 and Z = 4. The crystal structure of the HT-phase consists of Ni2+ cations octahedrally coordinated by six water molecules, sulphate tetrahedra and disordered dabcodiium cations linked together by hydrogen bonds. It undergoes a reversible phase transition (PT) of the second order at −53.7/−54.6 °C on heating-cooling runs. Below the PT temperature, the structure is fully ordered. The thermal decomposition of the precursor proceeds through three stages giving rise to the nickel oxide.  相似文献   

11.
Two new ternary ytterbium transition metal stannides, namely, Yb3CoSn6 and Yb4Mn2Sn5, have been obtained by solid-state reactions of the corresponding pure elements in welded tantalum tubes at high temperature. Their crystal structures have been established by single-crystal X-ray diffraction studies. Yb3CoSn6 crystallizes in the orthorhombic space group Cmcm (no. 63) with cell parameters of a=4.662(2), b=15.964(6), c=13.140(5) Å, V=978.0(6) Å3, and Z=4. Its structure features a three-dimensional (3D) open-framework composed of unusual [CoSn3] layers interconnected by zigzag Sn chains, forming large tunnels along the c-axis which are occupied by the ytterbium cations. Yb4Mn2Sn5 is monoclinic space group C2/m (no. 12) with cell parameters of a=16.937(2), b=4.5949(3), c=7.6489(7) Å, β=106.176(4)°, V=571.70(8) Å3, and Z=2. It belongs to the Mg5Si6 structure type and its anionic substructure is composed of parallel [Mn2Sn2] ladders interconnected by unusual zigzag [Sn3] chains, forming large tunnels along the c-axis, which are filled by the ytterbium cations. Band structure calculations based on density function theory methods were also made for both compounds.  相似文献   

12.
Single crystals of Ca3CuRhO6, Ca3Co1.34Rh0.66O6 and Ca3FeRhO6 were synthesized by high temperature flux growth in molten K2CO3 and structurally characterized by single crystal X-ray diffraction. While Ca3Co1.34Rh0.66O6 and Ca3FeRhO6 crystallize with trigonal (rhombohedral) symmetry in the space group , Z=6: Ca3Co1.34Rh0.66O6a=9.161(1) Å, c=10.601(2) Å; Ca3FeRhO6a=9.1884(3) Å, c=10.7750(4) Å; Ca3CuRhO6 adopts a monoclinic distortion of the K4CdCl6 structure in the space group C2/c, Z=4: a=9.004(2) Å, b=9.218(2) Å, c=6.453(1) Å, β=91.672(5). All crystals of Ca3CuRhO6 examined were twinned by pseudo-merohedry. Ca3CuRhO6, Ca3Co1.34Rh0.66O6, and Ca3FeRhO6 are structurally related and contain infinite one-dimensional chains of alternating face-sharing RhO6 octahedra and MO6 trigonal prisms. In the monoclinic modification, the copper atoms are displaced from the center of the trigonal prism toward one of the rectangular faces adopting a pseudo-square planar configuration. The magnetic properties of Ca3CuRhO6, Ca3Co1.34Rh0.66O6, and Ca3FeRhO6 are discussed.  相似文献   

13.
Sr3In0.9Co1.1O6, isostructural to Ca3Co2O6, is revealed by the study of the phase relations in the system SrO-InO1.5-CoOx (1000 °C). The structure of Sr3In0.9Co1.1O6 is refined by the combination of powder X-ray and neutron diffraction. Sr3In0.9Co1.1O6 crystallizes in a trigonal lattice with the cell parameters a=b=9.59438(3) Å, c=11.02172(4) Å with the space group R-3c. Its structure possesses 1D (In/Co)O3 chains running along the c-axis constructed by alternating face-sharing CoO6 octahedra and (In0.9Co0.1)O6 trigonal prisms. The co-occupation of In3+ and Co3+ at the trigonal prismatic site is evidenced by elementary analysis and determined by the structure refinement. Sr3In0.9Co1.1O6 is paramagnetic, and the susceptibility is consistent with the occupation of Co3+ at 10% of the trigonal prismatic positions in a high spin state (HS, S=2). The HS Co3+ is well separated by diamagnetic CoO6 octahedra and InO6 trigonal prisms and shows a g factor of 2.0 in the magnetic measurements.  相似文献   

14.
By means of powder X-ray diffraction, powder neutron diffraction and transmission electron microscopy (TEM), we determined the crystal structures of a metal-ordered manganite YBaMn2O6 which undergoes successive phase transitions. A high-temperature metallic phase (Tc1=520 K<T) crystallizes in a triclinic P1 with the following unit cell: Z=2, a=5.4948(15) Å, b=5.4920(14) Å, c=7.7174(4) Å, α=89.804(20)°, β=90.173(20)°, γ=91.160(4)°. The MnO6 octahedral tilting is approximately written as a0bc, leading to a significant structural anisotropy within the ab plane. The structure for Tc2<T<Tc1 is a monoclinic P2 (Z=2, a=5.5181(4) Å, b=5.5142(4) Å, c=7.6443(3) Å, β=90.267(4)°) with an abc tilting. The structural features suggest a dx2y2 orbital ordering (OO). Below Tc2=480 K, crystallographically inequivalent two octahedra show distinct volume difference, due to the Mn3+/Mn4+ charge ordering. The TEM study furthermore revealed a unique d3x2r2/d3y2r2 OO with a modified CE structure. It was found that the obtained crystal structures are strongly correlated to the unusual physical properties. In particular, the extremely high temperature at which charge degree of freedom freezes, Tc2, should be caused by the absence of the structural disorder and by heavily distorted MnO6 octahedra.  相似文献   

15.
A hydrothermal reaction of WO3, CoCl2 and 4,4′-bipyridine, yields a novel organic-inorganic hybrid compound, Co2(bpy)6(W6O19)2, at 170°C. X-ray single crystal structure determination reveals a two-dimensional covalent structure belonging to monoclinic crystal system, space group C2/c, with cell parameters a=19.971(4) Å, b=11.523(2) Å, c=16.138(3) Å, β=96.49(3)°, V=3690.0 Å3 and Z=2. The hexatungstate, [W6O19]2−, acts as a building block in bidentate fashion to bridge the Co(II) centers in the crystal structure. The title compound is found to have an optical energy gap of 2.2 eV from UV-Vis-NIR reflectance spectra.  相似文献   

16.
Crystal structure of a series of mixed-metal oxides, T2Mo3O8 (T=Mg, Co, Zn and Mn; P63mc; a=5.7628(1) Å, c=9.8770(3) Å for Mg2Mo3O8; a=5.7693(3) Å, c=9.9070(7) Å for Co2Mo3O8; a=5.7835(2) Å, c=9.8996(5) Å for Zn2Mo3O8; a=5.8003(2) Å, c=10.2425(5) Å for Mn2Mo3O8) was investigated by X-ray diffraction on single crystals. Structural analysis, magnetization measurements, X-ray photoemission spectroscopy and cyclic voltammetry showed that the Mn ions at the tetrahedral and octahedral sites in Mn2Mo3O8 adopt different valences of +2 and 2+δ (δ>0), respectively. The formal valence of the Mo3 in Mn2Mo3O8 is 12−δ to retain electric neutrality of the compound. In contrast, the T ions and Mo3 in T2Mo3O8 (T=Mg, Co and Zn) adopt the valences of +2 and +12, respectively.  相似文献   

17.
Over 100 samples were prepared as (Ga,In)4(Sn,Ti)n−4O2n−2, n=6, 7, and 9 by solid-state reaction at 1400 °C and characterized by X-ray diffraction. Nominally phase-pure beta-gallia-rutile intergrowths were observed in samples prepared with n=9 (0.17?x?0.35 and 0?y?0.4) as well as in a few samples prepared with n=6 and 7. Rietveld analysis of neutron time-of-flight powder diffraction data were conducted for three phase-pure samples. The n=6 phase Ga3.24In0.76Sn1.6Ti0.4O10 is monoclinic, P2/m, with Z=2 and a=11.5934(3) Å, b=3.12529(9) Å, c=10.6549(3) Å, β=99.146(1)°. The n=7 phase Ga3.24In0.76Sn2.4Ti0.6O12 is monoclinic, C2/m, with Z=2 and a=14.2644(1) Å, b=3.12751(2) Å, c=10.6251(8) Å, β=108.405(1)°. The n=9 phase Ga3.16In0.84Sn4TiO16 is monoclinic, C2/m, with Z=2 a=18.1754(2) Å, b=3.13388(3) Å, c=10.60671(9) Å, β=102.657(1)°. All of the structures are similar in that they possess distorted hexagonal tunnels parallel to the [010] vector.  相似文献   

18.
The Co2−xCux(OH)AsO4 (x=0 and 0.3) compounds have been synthesized under mild hydrothermal conditions and characterized by X-ray single-crystal diffraction and spectroscopic data. The hydroxi-arsenate phases crystallize in the Pnnm orthorhombic space group with Z=4 and the unit-cell parameters are a=8.277(2) Å, b=8.559(2) Å, c=6.039(1) Å and a=8.316(1) Å, b=8.523(2) Å, c=6.047(1) Å for x=0 and 0.3, respectively. The crystal structure consists of a three-dimensional framework in which M(1)O5-trigonal bipyramid dimers and M(2)O6-octahedral chains (M=Co and Cu) are present. Co2(OH)AsO4 shows an anomalous three-dimensional antiferromagnetic ordering influenced by the magnetic field below 21 K within the presence of a ferromagnetic component below the ordering temperature. When Co2+ is partially substituted by Cu2+ions, Co1.7Cu0.3(OH)AsO4, the ferromagnetic component observed in Co2(OH)AsO4 disappears and the antiferromagnetic order is maintained in the entire temperature range. Heat capacity measurements show an unusual magnetic field dependence of the antiferromagnetic transitions. This λ-type anomaly associated to the three-dimensional antiferromagnetic ordering grows with the magnetic field and becomes better defined as observed in the non-substituted phase. These results are attributed to the presence of the unpaired electron in the dx2y2 orbital and the absence of overlap between neighbour ions.  相似文献   

19.
The organo-templated iron(III) borophosphate (C3H12N2)FeIII 6(H2O)4[B4P8O32(OH)8] was prepared under mild hydrothermal conditions (at 443 K) and the crystal structure was determined from single crystal X-ray data at 295 K (monoclinic, P21/c (No. 14), a=5.014(2) Å, b=9.309(2) Å, c=20.923(7) Å, β=110.29(2)°, V=915.9(5) Å3, Z=2, R1=0.049, wR2=0.107 for all data, 2234 observed reflections with I>2σ(I)). The title compound contains a complex inorganic framework of borophosphate trimers [BP2O8(OH)2]5− together with FeO4(OH)(H2O)- and FeO4(OH)2-octahedra forming channels with ten-membered ring apertures in which the diaminopropane cations are located. The magnetization measurements confirm the Fe(III)-state and show an antiferromagnetic ordering at TN≈14.0(1) K.  相似文献   

20.
[La(C6H5O7)(H2O)2]·H2O was synthesized as precursor material for an aqueous solution-gel route to La-containing multimetal oxides. The compound was characterized by means of FTIR, TGA and pycnometry. The crystallographic structure was solved from powder diffraction data. The symmetry is monoclinic [a=17.097(3) Å, b=9.765(2) Å, c=6.3166(8) Å and β=90.42(1)°, Zexp=3.96] with space group P21/n (14). Direct methods were applied and the model was subsequently least-squares refined (RB=5.1% and RwP=12.0%). La3+ is nine-fold coordinated, the LaO9 forming a mono-capped square antiprism. The basic unit is a binuclear entity of two LaO9 polyhedra having one edge in common. These units are connected along the c-axis through citrate molecules. The carboxylate groups of the citrate are coordinated to La3+ in monodentate, bidentate and bridging way. Also the alkoxide group, which carries the proton, is coordinated to La3+. Two water molecules complete the coordination sphere, while the third one can be found inbetween the La3+-citrate network.  相似文献   

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