X-ray powder diffraction and IR study of NaMg(H2O)2[BP2O8]·H2O and NH4Mg(H2O)2[BP2O8]·H2O

NaMg(H₂O)₂[BP₂O₈]·H₂O was prepared by hydrothermal synthesis and was characterized by X-ray powder difraction and IR method. The title compound was synthesized from MgCl₂·6H₂O, NaBO₃·4H₂O, and (NH₄)₂HPO₄ with variable molar ratios using hydrothermal method by heating at 165 °C for 3 days. The X-ray powder diffraction data was indexed in hexagonal system, the unit cell parameters were found to be as a = 9.428, c = 15.82 Å, Z = 4 and the space group is P6₁22. It is isostructural with M^lM^ll(H₂O)[BP₂O₈] type compounds where M^l = Na, K; M^ll = Mg, Mn, Fe, Co, Ni and Zn. In addition NH₄Mg(H₂O)₂[BP₂O₈]·H₂O was also synthesized the first time in this research. Its unit cell parameters and hkl values were in good agreement with the sodium magnesium compound. The unit cell parameters are a = 9.529, c = 15.736 Å. The indexed X-ray powder diffraction data of both compounds which were not reported in the literature is presented in this work. The IR data of NaMg(H₂O)₂[BP₂O₈]·H₂O is also reported.     

Complexes with substituted 2,5-dihydroxy-p-benzoquinones: The inclusion compounds [Y(H2O)3]2 (C6Cl2O4)3·6.6H2O and [Y(H2O)3]2 (C6Br2O4)3·6H2O

Single crystal of [Y(H₂O)₃]₂ (C₆Br₂O₄)₃·6H₂O and [Y(H₂O)₃]₂ (C₆Cl₂O₄)₃·6.6H₂O were grown in aqueous silicagel. The compounds are in principle isostructural. In Y chloranilate one additional water site is occupied as verified by X-ray single crystal structure analysis. Y³⁺ is nine-coordinated by three water molecules and six oxygen atoms of the bischelating (C₆X₂O₄)²⁻ ions (XCl, Br). The coordination polyhedron is an only slightly distorted tri-capped trigonal prism. The connection of Y³⁺ with the dianions leads to infinite, corrugated layers. The layer stacking yields cage-like cavities in which water molecules are accomodated. Hydrogen bonds interlink adjacent layers. Further hydrogen bonds involve the entrapped water molecules. DSC measurements indicated a complicated dehydration process which caused right at the start destruction of the single crystals.     

Novel self-assembled decavanadate clusters forming 1D molecular chains and 2D molecular arrays: [HMTA-H···H2O][HMTA-CH2OH][H3V10O28{Na(H2O)4}]·4H2O and [Na2(H2O)10] [H3V10O28 {Na(H2O)2}]·3H2O

Two novel materials, [HMTA-H··H₂O] [HMTA-CH₂OH] [H₃V₁₀O₂₈[Na(H₂O)₄}]·4H₂O, 1 and [Na₂(H₂O)₁₀][H₃V₁₀O₂₈[Na(H₂O)₂}]·3H₂O, 2 containing decavanadate clusters interconnected through hydrated sodium cations forming 1D molecular chains and 2D molecular arrays have been self-assembled from acidified, aqueous vanadate solution in the presence of organic bases, hexamethylenetetramine and 1,3,5-triazine respectively.     

Photocatalytic Properties of the MgHPO4·3H2O and MgKPO4·6H2O Phosphates

Inorganic Materials - Magnesium double phosphates, MgHPO4·3H2O and MgKPO4·6H2O, isostructural with the minerals newberyite and struvite-K have been synthesized in powder form via...     

Conductivity of (NH4)3[CrMo6O24H6]·7H2O Treated by Nd Chemistry-Heated Diffused Permeation

Rare earth co-permeation of (N H4)3 [CrMo6 O24 H6]·7H2O was reported and the conductivity of (N H4)3 [CrMo6O24 H6]was improved by 6.734× 109 times. X-ray fluorescence spectrometry (XRF), thermogravimetry-differential thermal sample. Experimental results showed that Nd could be permeated into the body of this sample and the XRD patterns showed great difference between (NH4)3[CrMo6O24H6]·7H2O and permeated sample. The structure of (NH4)3[CrMo6O24H6]·7H2O was destroyed and new compound MoN perhaps formed.     

Hydrothermal Crystallization in the Systems LiOH–MO2–GeO2–H2O (M = Ti, Sn) at 500°C and 0.1 GPa: Li2Ti[5]Ge[4]O5 and Li2Ge[6]Ge2 [4]O6 Phase Relations

Crystallization in the LiH–Ti₂–Ge₂–H₂O and LiOH–SnO₂–GeO₂–H₂O hydrothermal systems was studied at 500°C and 0.1 GPa. The phases crystallizing in the Ti system are Li₂Ti^[5]Ge^[4]O₅, Li₂Ge^[6]Ge₂ ^[4]O₆(OH)₂, Li₃HGe₄ ^[6]Ge₃ ^[4]O₁₆ · 4H₂O, and Li₂Ge^[4]O₃ (Ge in four- or sixfold oxygen coordination, and Ti in fivefold oxygen coordination). Over a wide range of TiO₂ : GeO₂ molar ratios (6 : 1 to 1 : 1), the dominant phase is Li₂Ge^[6]Ge₂ ^[4]O₆(OH)₂. At higher GeO₂ contents (TiO₂ : GeO₂ = 1 : 2 to 1 : 6), both Li₂Ti^[5]Ge^[4]O₅ and Li₂Ge^[6]Ge₂ ^[4]O₆(OH)₂ crystallize. The crystallization fields of Ge-containing phases at TiO₂ : GeO₂ = 1 : 2 to 1 : 6 are (in order of increasing LiOH concentration) GeO₂ (rutile structure), Li₂Ti^[5]Ge^[4]O₅ + Li₂Ge^[6]Ge₂ ^[4]O₆(OH)₂, and Li₂Ti^[5]Ge^[4]O₅ + Li₂Ge^[6]Ge₂ ^[4]O₆(OH)₂ + Li₂Ge^[4]₃ + Li₃HGe₄ ^[6]Ge₃ ^[4]O₁₆ · 4H₂O. The phases crystallizing in the Sn system are Li₂Ge^[6]Ge₂ ^[4]O₆(OH)₂, Li₃HGe₄ ^[6]Ge₃ ^[4]O₁₆ · 4H₂O, and Li₂Ge^[4]O₃. Tin is present in the form of SnO₂ only. The structures of Li₂Ti^[5]Ge^[4]O₅ and Li₂Ge^[6]Ge₂ ^[4]O₆(OH)₂ are characterized by the simplest type of matrix assembly: direct packing of substructural precursor units and their two-dimensional growth in various crystallographic directions.     

[（C6H5）2NH2]3[PWl2PO40]·4H2O的合成与表征

以12-钨磷酸和二苯胺为原料合成了一种电荷转移盐。通过元素分析确定其组成为[（C6H5）2NH2]3[PW12O40]·4H2O，各元素的质量分数分别为（括号内为理论值）C 12．91％（13．08％），H 1．304％（1．344％），N 1．793％（1．793％），采用红外光谱、紫外．可见分光光度法、X射线粉末衍射等测试技术对该化合物进行了分析表征。结果表明：所合成的新型电荷转移化合物的杂多阴离子保持Keggin结构特征。     

Synthesis and Study of Uranium-Containing Aluminum Compounds Al[BVUO6]2[OH]·nH2O (BV = P,As)

A procedure was developed for preparing aluminum hydroxouranophosphate and hydroxourano- arsenate. The structural features and thermal decomposition pathways of the compounds were studied by X-ray diffraction, IR spectroscopy, and thermal analysis.     

Synthesis,characterization and crystal structure of a novel Strandberg-type polyoxoselenomolybdate Rb4[Se2Mo5O21]·2H2O

An inorganic compound formulated as Rb₄[Se₂Mo₅O₂₁]·2H₂O (1) has been isolated by conventional solution method and structurally characterized by single-crystal X-ray diffraction methods, scanning electron microscopy (SEM), powder XRD, IR, UV–vis spectra, and cyclic voltammetry measurements. This compound crystallizes in the monoclinic system, space group C2 with unit a = 19.701 (3) Å, b = 10.296 (2) Å, c = 12.134 (4) Å, β = 106.96 (2)° and Z = 4. The crystal structure of (1) is built up from a Strandberg clusters connected through hydrogen-bonding interactions into a three-dimensional supramolecular network.     

Synthesis, Physicochemical Properties, and Electrode Behavior of Ni2[Ni(OH)6W6O18 ] · 8H2O

Nickel(II) hexatungstonickelate(II) was synthesized and characterized by elemental analysis, x-ray diffraction, thermal analysis, IR spectroscopy, and ¹H nuclear magnetic resonance. The results demonstrate that constitutional water is present in the form of OH groups, which can be removed by heating to 230–370°C. The chemical formula of the compound is Ni₂[Ni(OH)₆W₆O₁₈] · 8H₂O. Nickel(II) hexatungstonickelate(II), a poorly soluble compound, was tested as an electrode for Ni(II) determination in solution. Its electrode properties and selectivity for other ions suggest that it is a promising material for such applications. At pH 5, the ion-selective electrode we fabricated has a Nernstian response to Ni(II) (10^–5 to 10^–1 mol/l) which is close to that predicted theoretically.     

Synthesis and characterization of a new organic sulphate, [2,3-(CH3)2C6H3NH3]HSO4·H2O

Crystals of a new hybrid compound C₈H₁₂N⁺, HSO₄^?·H₂O were synthesized in aqueous solution and characterized by X-ray diffraction and IR absorption spectroscopy. This compound crystallizes in the orthorhombic non-centrosymmetrical space group P2₁2₁2₁ and an unit cell with a = 5.74(2) Å, b = 9.17(2) Å, c = 21.34(4) Å, V = 1124(6) Å³, and Z = 4. Its crystal structure is a packing of alternated inorganic and organic layers parallel to (a,b) planes. The different components are connected by a bi-dimensional network of strong OH…O and NH…O hydrogen bonds. Then, in order to detect phase transitions and watch changes in the conductivity behaviour, investigations by DTA–TG and differential scanning calorimetry (DSC) and electrical conductivity measurements were carried out.     

Synthesis and structure of Cs3[UO2(CH3COO)3]2(NCS)·H2O

The compound Cs₃[UO₂(CH₃COO)₃]₂(NCS)·H₂O (I) was synthesized and studied by IR spectroscopy and single crystal X-ray diffraction. Compound I crystallizes in the monoclinic system with the following unit cell parameters: a = 7.8286(9), b = 19.892(2), c = 20.050(2) Å, β = 94.527(2)°, space group P2₁/c, Z = 4, R = 0.0387. The uranium-containing structural units in crystals of I are mononuclear complexes [UO₂(CH₃COO)₃]^? belonging to crystal-chemical group AB ₃ ⁰¹ (A = UO ₂ ²⁺ , B⁰¹ = CH₃COO^?) of uranyl complexes.     

Reaction of Cd(NO3)2·4H2O with 4,4'–bipyridine (bpy) in MeOH solvent: synthesis and characterization of T-shaped [Cd(bpy)1.5(NO3)2]·3H2O,square grid [Cd(bpy)2(H2O)2](NO3)2·4H2O and linear polymeric [Cd(bpy)(H2O)2(NO3)2]

The influence of concentration of water and metal salt in the reaction between Cd(NO₃)₂·4H₂O and 4,4′–bipyridine in MeOH has been studied and three compounds namely, T-shaped [Cd(bpy)_1.5(NO₃)₂]·3H₂O, 1 square grid [Cd(bpy)₂(H₂O)₂](NO₃)₂ 4H₂O, 2 and one dimensional linear polymer, [Cd(bpy)(H₂O)₂(NO₃)₂], 3 were isolated quantitatively in this process. Compound 1 forms in MeOH at high dilution of the metal salt (5.0 mg/mL or less) and for the metal-to-ligand ratio 1:(1.5–2.0). Compound 2 forms exclusively in the concentration range, 17–33% for water in MeOH by volume and 12–28 mg/mL for the metal salt of the solution. Outside these limits, mixtures of 2 and 3 were isolated. For 1:1 ratio of metal salt to bpy, the linear polymer, 3 was obtained in major quantity and its formation was found to be independent of concentration of water or the metal salt. Compounds 1 and 2 have been characterized by X-ray crystallography. On heating all the compounds decompose through a common intermediate [Cd(bpy)(NO₃)₂] and finally to CdO as monitored by TG.     

An X-ray diffraction study of Rb[UO2(SeO4)F]·H2O

An X-ray diffraction study of Rb[UO₂(SeO₄)F]·H₂O (I) was performed. The compound crystallizes in the rhombic system with the following unit cell parameters: a = 8.4753(6), b = 13.5234(9), c = 13.5296(9) Å, space group Pnma, Z = 8, V = 1550.7(2) ų; R = 0.0248. The principal structural units of crystals of I are [UO₂(SeO₄)F]^? layers belonging to crystal-chemical group AT³M² (A = UO ₂ ²⁺ , T³ = SeO ₄ ^2? , M² = F^?) of uranyl complexes. The uranium-containing layered units are combined via electrostatic interaction with Rb cations and via a system of hydrogen bonds involving outer-sphere water molecules.     

Behavior of uranosilicates MIII(HSiUO6)3·10H2O (MIII = La-Lu, Y) in aqueous solutions

The behavior of uranosilicates M^III(HSiUO₆)₃·10H₂O (M^III = La-Lu, Y) in aqueous solutions in the pH range from 0 to 14 was studied. The acidity intervals in which the compounds preserve their composition and structure were found, the uranosilicate conversion products were identified, and the solubility of M^III(HSiUO₆)₃·10H₂O was determined. With the mathematical apparatus of equilibrium thermodynamics applied to heterogeneous systems M^III(HSiUO₆)₃·10H₂O-aqueous solution, the equilibrium constants of dissolution and the Gibbs functions of formation of uranosilicates were calculated, the solubility curves were plotted, and the speciation diagrams of U(VI), Si(IV), and elements M(III) in solutions and equilibrium solid phases were constructed.     

Complexes with substituted 2,5-dihydroxy-p-benzoquinones: AE[C6(C2H5)2O4]·3H2O (AE=Ca,Sr, Ba)

Single crystals of AE[C₆(C₂H₅)₂O₄]·3H₂O belonging to space group P2₁2₁2₁ were grown in aqueous silicagel (AE=Ca, Sr) and in aqueous solution (AE=Ba), respectively. AE²⁺ is coordinated by four oxygen atoms of two bis-chelating [C₆(C₂H₅)₂O₄]²⁻ ions, thus forming infinite, corrugated chains extending along [010]. The coordination polyhedron is completed by additional water molecules. The coordination sphere is different for the three different AE²⁺ ions yielding CN increasing from Ca²⁺ to Ba²⁺. The principle features of the crystal structure, however, remain unchanged. Adjacent chains are interlinked by hydrogen bonds between water molecules of the coordination sphere and the oxygen atoms of the [C₆(C₂H₅)₂O₄]²⁻ ion.     

Crystal and Molecular Structure of a New Complex of [60]Fullerene, 2(C60)·2(TMTSF)·(C6H6)

Abstract

A new molecular complex of [60]fullerene with composition 2(C₆₀)·2(TMTSF)·(C₆H₆) was synthesized. The structure and composition of the complex were found by an x-ray study. Crystal data: 2(C₆₀)2(C₁₀H₁₂Se₄)(C₆H₆), M = 2415.4, monoclinic, a = 19.388(4), b = 13.410(2), c = 32.467(6) A, β = 92.71(2)°, V = 8432(3) [Adot]³, space group P2₁/n, Z = 4, d_calc = 1.903 g/cm³, R = 0.0606. The crystal structure was shown to be layered with the alternating layers of three types. Two of them have the same composition (C₆₀, TMTSF) but different interorientation of molecules in a layer and different number of shortened contacts C…C and C…Se. The third layer consists of benzene molecules. The energy of intermolecular interactions C₆₀…. TMTSF was estimated by ab initio calculations. The TMTSF molecule has a “boat” conformation.