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1.
Single crystals of Ba3[UO2(C2O4)2(NCS)]2 · 9H2O are synthesized and studied by X-ray diffraction. The crystals are orthorhombic, space group Fddd, Z = 16, and the unit cell parameters are a = 16.253(3) Å, b = 22.245(3) Å, c = 39.031(6) Å. The main crystal structural units are mononuclear complex groups [UO2(C2O4)2NCS]3? of the crystal-chemical family (AB 2 01 M1 (A = UO 2 2+ , B01 = C2O 4 2? , M1 = NCS?) of the uranyl complexes linked into a three-dimensional framework by electrostatic interactions and hydrogen bonds involving oxalate ions and water molecules.  相似文献   

2.
Single crystals of Cs[(UO2)2(C2O4)2(OH)] · H2O were synthesized and structurally studied using X-ray diffraction. The compound crystallizes in monoclinic space group P21/m, Z = 2, with the unit cell parameters a = 5.5032(4) Å, b = 13.5577(8) Å, c = 9.5859(8) Å, β = 97.012(3)°, V = 709.86(9) Å3, R = 0.0444. The main building units of crystals are [(UO2)2(C2O4)2(OH)]? layers of the A2K 2 02 M2 (A = UO 2 2+ , K02 = C2O 4 2? , and M2 = OH?) crystal-chemical family. Uranium-containing layers are linked into a three-dimensional framework via electrostatic interactions with outer-sphere cations and hydrogen bonds with water molecules.  相似文献   

3.
A powder of deuterated rubidium diselenatouranylate dihydrate Rb2UO2(SeO4)2 · 2D2O has been studied by neutron diffraction. The compound is orthorhombic, space group Pna21, with the following unit cell parameters: a = 13.654(2) Å, b = 11.863(2) Å, c = 7.625(1) Å, Z = 4, R F = 3.77, R I = 6.12, and χ2 = 2.21. Basic structure units are [UO2(SeO4)2 · D2O]2? layers belonging to the AB 2 2 M1 crystal-chemical group (A = UO 2 2+ , B2 = SeO 4 2? , M1 = D2O) of uranyl complexes. The hydrogen atoms if the water molecules involved in the layer form intralayer hydrogen bonds with the terminal oxygen atoms of selenate ions. The outer-sphere water molecules are coordinated to the rubidium ions and are involved in hydrogen bonding with oxygen atoms of neighboring [UO2(SeO4)2 · D2O]2? layers.  相似文献   

4.
Evidence for the existence of primitive life forms such as lichens and fungi can be based upon the formation of oxalates. These oxalates form as a film like deposit on rocks and other host matrices. The anhydrous oxalate mineral moolooite CuC2O4 as the natural copper(II) oxalate mineral is a classic example. Another example of a natural oxalate is the mineral wheatleyite Na2Cu2+(C2O4)2·2H2O. High resolution thermogravimetry coupled to evolved gas mass spectrometry shows decomposition of wheatleyite at 255°C. Two higher temperature mass losses are observed at 324 and 349°C. Higher temperature mass losses are observed at 819, 833 and 857°C. These mass losses as confirmed by mass spectrometry are attributed to the decomposition of tennerite CuO. In comparison the thermal decomposition of moolooite takes place at 260°C. Evolved gas mass spectrometry for moolooite shows the gas lost at this temperature is carbon dioxide. No water evolution was observed, thus indicating the moolooite is the anhydrous copper(II) oxalate as compared to the synthetic compound which is the dihydrate.  相似文献   

5.
The single crystals of Rb2[(UO2)2(C2O4)2(SeO4)] · 1.33H2O were synthesized and studied by X-ray diffraction. The crystals are monoclinic, space group P21/m, Z= 2, the unit cell parameters: a = 5.6537(8), b = 18.736(3), c = 9.4535(15) Å, β = 98.440(5)°, V = 990.6(3) Å3, R 1 = 0.0506. The main structural units of the crystal are infinite layers of [(UO2)2(C2O4)2(SeO4)]2?, corresponding to the crystal chemical group A2K 2 02 B2 (A = UO 2 2+ , K02 = C2O 4 2? , B2 = SeO 4 2? ) of uranyl complexes. The uranium-containing layers are united into a three-dimensional framework through the electrostatic interactions with the outer-sphere rubidium ions and the hydrogen bonding system involving the outer-sphere water molecules.  相似文献   

6.
Single crystals of the Na4[Na2Cr2(C2O4)6] · 10H2O complex were synthesized for the first time. The structure of the complex was determined by X-ray diffraction analysis. The compound crystallizes in the monoclinic crystal system with the unit cell parameters a = 17.290(4) Å, b = 12.521(3) Å, c = 15.149(3) Å, β = 100.45(3)°, Z = 4, space group Cc. Anionic layers [NaCr(C2O4)3] 2n 4n? can be distinguished in the crystal structure of the complex. The Na+ cations and water molecules, involved in the formation of a hydrogen bond network, are located between the anionic layers.  相似文献   

7.
The crystal structure of a double complex salt of the composition [Au(en)2]2[Cu(C2O4)2]3·8H2O (en = ethylenediamine) at 150 K is determined by single crystal X-ray diffraction. The crystal data for C20H48Au2Cu3N8O32 are: a = 9.1761(3) Å, b = 16.9749(6) Å, c = 13.4475(5) Å, β = 104.333(1)°, V = 2029.43(12) Å3, P21/c space group, Z = 2, d x = 2.450 g/cm3. It is demonstrated that the thermal decomposition of the double complex salt in a helium or hydrogen atmosphere affords the solid solution Au0.4Cu0.6.  相似文献   

8.
The complex Na3(NH4)2[Ir(SO3)2Cl4]·4H2O was examined with single crystal X-ray diffraction and IR spectroscopy. Crystal data: a = 7.3144(4) Å, b = 10.0698(5) Å, c = 12.3748(6) Å, β = 106.203(1)°, V = 875.26(8) Å3, space group P21/c, Z = 2, d calc = 2.547 g/cm3. In the complex anion two trans SO 3 2? groups are coordinated to iridium through the S atom. The splitting of O-H bending vibrations of crystallization water molecules and N-H ones of the ammonium cation is considered in the context of different types of interactions with the closest neighbors in the structure.  相似文献   

9.
10.
Composite solid electrolytes were synthesized from the organic salt dimethylammonium chloride (1–x)C2H8NCl–xAl2O3. Their physicochemical properties were studied. In the starting C2H8NCl salt, there is a phase transition at 39°C accompanied by an increase in conductivity by two orders of magnitude. The conductivity of the high-temperature phase is 9.3 × 10–6 S/cm at 160°C. A differential scanning calorimetry study showed that the salt in the composites spreads over the oxide surface and at x > 0.6 the salt melting enthalpy decreases to zero. The conductivity of the resulting composites was studied by impedance spectroscopy. It was shown that heterogeneous doping leads to a sharp increase in ion conductivity to 7.0 × 10–3 S/cm at 160°C and a decrease in the activation energy to 0.55 eV.  相似文献   

11.
The structure of tri-μ2-disulfido-μ3-thiotris(diethyldithiocarbamato)-S,S′-triangle-trimolybdenum iodide [Mo33-S)(μ2-S2)3(Et2NCS2)3]I was determined. The compound was characterized by differential thermal analysis and IR, Raman, and X-ray electronic spectroscopy.  相似文献   

12.
The structure of [Pb3(OH)4Co(NO2)3](NO3)(NO2)·2H2O is determined by single crystal X-ray diffraction. The crystallographic characteristics are as follows: a = 8.9414(4) Å, b = 14.5330(5) Å, c = 24.9383(9) Å, V = 3240.6(2) Å3, space group Pbca, Z = 8. The Co(III) atoms have a slightly distorted octahedral coordination formed by three nitrogen atoms belonging to nitro groups (Co–Nav is 1.91 Å) and three oxygen atoms belonging to hydroxyl groups (Co–Oav is 1.93 Å). The hydroxyl groups act as μ3-bridges between the metal atoms. The geometric characteristics are analyzed and the packing motif is determined.  相似文献   

13.
14.
A series of MoO3/ZrO2–Al2O3 catalysts was prepared and investigated in the sulfur-resistant methanation aimed at production of synthetic natural gas. Different methods including impregnation, deposition precipitation, and co-precipitation were used for preparing ZrO2–Al2O3 composite supports. These composite supports and their corresponding Mo-based catalysts were investigated in the sulfur-resistant methanation, and characterized by N2 adsorption–desorption, XRD and H2-TPR. The results indicated that adding ZrO2 promoted MoO3dispersion and decreased the interaction between Mo species and support in the MoO3/ZrO2–Al2O3 catalysts. The co-precipitation method was favorable for obtaining smaller ZrO2 particle size and improving textural properties of support, such as better MoO3 dispersion and increased concentration of Mo6+ species in octahedral coordination to oxygen. It was found that the MoO3/ZrO2–Al2O3 catalyst with ZrO2Al2O3 composite support prepared by co-precipitation method exhibited the best catalytic activity. The ZrO2 content in the ZrO2Al2O3 composite support was further optimized. The MoO3/ZrO2–Al2O3 with 15 wt % ZrO2 loading exhibited the highest sulfur-resistant CO methanation activity, and excess ZrO2 reduced the specific surface area and enhanced the interaction between Mo species and support. The N2 adsorption-desorption results indicated that the presence of ZrO2 in excessive amounts decreased the specific surface area since some amounts of ZrO2 form aggregates on the surface of the support. The XRD and H2-TPR results showed that with the increasing ZrO2 content, ZrO2 particle size increased. These led to the formation of coordinated tetrahedrally Mo6+(T) species and crystalline MoO3, and this development was unfavorable for improving the sulfur-resistant methanation performance of MoO3/ZrO2–Al2O3 catalyst.  相似文献   

15.
The system hydrogen peroxide–hexafluoroacetone sesquihydrate effectively oxidizes adamantane in the presence of VO(acac)2 to afford 64% of adamantan-1-ol in tert-butyl alcohol or 76% of adamantan-2-one in a mixture of acetic acid with pyridine.  相似文献   

16.
An approach for significantly suppressing N2O formation in reduction of NO by NH3 over V2O5–WO3/TiO2 (VWT) catalyst has been studied by coating different amounts of a Fe-exchanged zeolite (FeZ) onto the catalyst. FeZ-promoted VWT samples were characterized using N2 sorption, X-ray diffraction (XRD) analysis, and NH3 adsorption/desorption techniques to understand the primary role of FeZ in lowering N2O production levels. At high temperatures (≥450 °C), VWT gave N2O production with high concentrations, while N2O formation was noticeably reduced when using FeZ-promoted catalysts, which also showed somewhat lower NO removal activities (<5 %) at all temperatures. N2 sorption and XRD measurements revealed no perceptible physical or chemical alterations of each constituent, even in VWT catalysts after FeZ coating following high-temperature calcination. Adsorption of NH3 on unpromoted and FeZ-promoted catalysts and subsequent desorption yielded very complicated spectra for N2O that might primarily come from NH3 oxidation, and the interaction between V–NO species at temperatures >580 °C. NO on neighboring sites seems to be produced via decomposition of N2O generated at lower temperatures. The FeZ in the promoted VWT catalysts could be responsible for N2O decomposition and N2O reduction with unreacted NH3 at temperatures >400 °C, thereby significantly lowering N2O emission levels. This promotional effect bodes well for use in many industrial deNO x applications.  相似文献   

17.
A method for producing synthetic troegerite of composition(UO2)3(AsO4)2 · 12H2. Owas developed. X-ray diffraction, IR spectrometry, X-ray fluorescence analysis, and scanning calorimetry were used to study its dehydration and thermal decomposition, to solve the structgure, and to determine X-ray diffraction and IR spectroscopic characteristics.  相似文献   

18.
A new Co(III) complex of 1,2-cyclohexanedionedioxime and thiocarbamide with an SO 4 2? anion and solvation water molecules in the outer sphere has been synthesized and its structure has been defined. Orthorhombic crystals, a = 11.659(2) Å, b = 26.448(5) Å, c = 30.142(6) Å, V = 9295(3) Å 3, Z = 8, dcalc = 1.599 g/cm3, space group Pbca; final R index is 0.0578 for 8221 reflections with I > 2σ(I). In the octahedral Co(III) complex, two 1,2-cyclohexanedionedioxime residues lie in the equatorial plane, while two thiocarbamide molecules are in the axial plane. Intramolecular bonds: N-H…O and O-H…O type hydrogen bonds and π-π interactions that stabilize the complex cations. In crystal, the components are linked by N-H…O and O-H…O hydrogen bonds into a 3D framework.  相似文献   

19.
Crystal structures of two modifications of a binuclear Pd2(μ-ac)2(acac)2 complex are studied at 150 K and 297 K (ac = acetate; acac = acetylacetonate). It is demonstrated that in both cases, the packing of the complexes can be considered as pseudohexagonal, the molecules forming infinite chains by interactions between chelate rings with the shortest contacts Pd...C γ ~ 3.3 Å.  相似文献   

20.
A new neptunium(V) complex [(NpO2)2(CH3COO)2(H2O)] ? 2H2O was synthesized and its crystal structure was determined. The unit cell parameters are: a = 24.007(10) Å, b = 6.779(3) Å, c = 8.076(3) Å, space group Pnma, Z = 4, V = 1314.2(9) Å3, R = 0.049, wR(F2) = 0.105. The crystal structure of the compound is composed of neutral [(NpO2)2(CH3COO)2(H2O)] layers and molecules of the water of crystallization. Each of the crystallographically independent neptunoyl ions performs a bidentate function thus forming a composite system of cation-cation bonds.  相似文献   

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