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.     

A single crystal X-ray diffraction study of Na4(UO2)4(i-C4H9COO)11(NO3)·3H2O

Synthesis and the results of IR and single crystal X-ray diffraction study of Na₄(UO₂)₄(i-C₄H₉COO)₁₁·(NO₃)·3H₂O are reported. The crystals are monoclinic; the unit cell parameters at 100 K are as follows: a = 13.697(2), b = 20.285(3), c = 15.991(3) Å, β = 103.760(3)°, space group P2₁, Z = 2, R = 0.0650. The uraniumcontaining structural units are mononuclear moieties [UO₂(i-C₄H₉COO)₃]^? and [UO₂(NO₃)(i-C₄H₉COO)₂]^?, belonging to crystal-chemical group AB ₃ ⁰¹ (A = UO ₂ ²⁺ , B⁰¹ = i-C₄H₉COO^? and NO ₃ ^? ) of uranyl complexes. The IR data are consistent with the results of the single crystal X-ray diffraction study. The influence of the carboxylate ligand volume on the structure of Na[UO₂L₃]·nH₂O crystals (L = acetate, n-butyrate, isovalerate ion) is analyzed.     

Synthesis and Study of Sr[HSiUO6]2·2H2O and Ba[HSiUO6]2·2H2O

Uranosilicates of the general formula M^{I I}[HSiUO₆]₂·2H₂O (M^{I I} = Sr, Ba) were prepared by hydrothermal synthesis. Previously unknown intermediate crystal hydrates were separated and studied by X-ray diffraction (XRD), IR spectroscopy, and thermal analysis. Polymorphic transitions -Sr[HSiUO₆]₂ -Sr[HSiUO₆]₂ and -Ba[HSiUO₆]₂ -Ba[HSiUO₆]₂ were revealed at 700 and 780°C, respectively.     

Synthesis, crystal structure and X-ray powder diffraction data of the phosphor matrix 4SrO·7Al2O3

The white phosphor matrix 4SrO·7Al₂O₃ has been synthesized by firing the appropriate mixture of SrCO₃, Al(OH)₃ and H₃BO₃ in the molar ratios 1:3.5:0.135 at 1300°C for 4–7 h. The crystal structure of 4SrO·7Al₂O₃ has been determined as a orthorhombic Pmma space group with a=24.7451(2)Å, b=8.4735(6)Å, c=4.8808(1)Å, V=1023.41(3)ų, Z=2, and D=3.66 g cm^–3 by the Rietveld analysis. The refinement figures of merit are R_p=8.26, R_wp=11.60, R_bragg=4.44 and s=2.61 for 844 reflections with 2<119.94°. And the corresponding X-ray powder diffraction data are presented for search/match analysis.     

Synthesis,Characterization, and X-ray Structure of Tetraaminoguanidinium Diuranyl Tetraoxalate Monohydrate (HAgun)4[(UO2)2(C2O4)4]·H2O

Radiochemistry - A new uranyl oxalate complex containing aminoguanidinium cation was isolated from an aqueous solution containing uranyl nitrate hexahydrate, oxalic acid dihydrate, and...     

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.     

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.     

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.     

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.     

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.     

Crystal Structure of An(VI) Complexes with Succinate Anions, [PuO2(C4H4O4)(H2O)] and Cs2[(AnO2)2(C4H4O4)3]·H2O (An = U,Np, Pu)

Radiochemistry - Actinide(VI) complexes with succinate anions [PuO2(succ)(H2O)] and Cs2[(AnO2)2(succ)3]·H2O (An = U, Np, Pu), where succ = [C4H4O4]2 ?, were synthesized and studied by...     

Mixed-Cation Molybdate Complex of Neptunium(V), Li2Na[NpO2(MoO4)2]·4H2O

Radiochemistry - A new mixed-cation complex Li2Na[NpO2(MoO4)2]·4H2O with NpO2+ : MoO42– = 1 : 2 has been synthesized and structurally characterized. The coordination environment of Np(V)...     

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.     

Preparation and characterization of LiNi0.8Co0.15Al0.05O2 cathode material from (NH4)2C2O4·2H2O precipitant

Journal of Materials Science: Materials in Electronics - LiNi0.8Co0.15Al0.05O2 (NCA) cathode material was usually prepared with Ni2+, Co2+, Al3+ co-precipitation method using NaOH/NH3·H2O...     

球形NH4FePO4·H2O的制备

以柠檬酸铵作络合剂通过控制结晶法制备了的球形NH4FePO4·H2O,用扫描电镜观察了颗粒的形貌和分布.通过研究加料方式、反应温度、滴加速度、搅拌速度、反应物浓度等对颗粒形态的影响,得到了制备球形NH4FePO4·H2O的最佳工艺条件.     

Crystal Structure and Electronic Absorption Spectrum of Double Neptunium(V) Phthalate Co(NH3)6NpO2[(OOC)2C6H4]2·2H2O

Single crystals of Co(NH₃)₆NpO₂[(OOC)₂C₆H₄]₂·2H₂O were grown. The crystal structure of this compound [monoclinic cell: a = 7.748(2), b = 23.051(5), c = 14.608(3) Å, = 96.21(3)°, space group P2₁/c, Z = 4, V = 2593.7(9) ų, d _calc = 2.034 g cm^{- 3}, CAD4 automatic diffractometer, MoK , graphite monochromator, R ₁ = 0.041 for all 3567 reflections observed, wR ₂ = 0.1344 for all 4445 unique reflections, 325 refined parameters] was studied. The structure consists of infinite anionic chains {NpO₂[(OOC)₂C₆H₄]₂} _n ^{3 n -}, [Co(NH₃)₆]^{3 +} cations, and molecules of crystallization water. Neptunium(V) atom is in pentagonal-bipyramidal oxygen surrounding (CN 7); the neptunyl(V) group is linear and symmetrical; the Np = O bond lengths are 1.830(6) and 1.833(5)Å, the O = Np = O angle is 176.4(2)°. The equatorial plane of the bipyramid is formed by five oxygen atoms of phthalate anions. The Np-Oeq bond length correlates with the denticity of the phthalate anions. Two types of phthalate anions are localized in the structure. The first tridentate ligand is a bridge between Np(V) atoms in the chains. The second ligand is coordinated to Np in the bidentate fashion to form NpOCCCCO seven-membered chelate ring. The cation [Co(NH₃)₆]^{3 +} has an octahedral structure. The average Co-N distance in the octahedron is 1.961 Å the N-Co-N bond angles are close to 90°. Two water molecules along with [Co(NH₃)₆]^{3 +} cations are located between the anionic chains {NpO₂[(OOC)₂C₆H₄]₂} _n ^{3 n -}. The chains are additionally bonded along the Z-axis of the crystal by O_w-H···O hydrogen bonds.     

Synthesis of Double Uranyl Phthalates of the M4[(UO2)4(μ3-O)2(C6H4C2O4)4] ⋅ nH2O Type with M = NH4, K, and Cs. Crystal Structure of K4[(UO2)4O2(C6H4C2O4)4] ⋅ 3H2O

Double U(VI) phthalates with NH ₄ ⁺ , K⁺, and Cs⁺ ions in the outer sphere were synthesized. The X-ray phase analysis shows that their structures are similar. Single crystals were prepared and the structure of K₄[(UO₂)₄(μ₃-O)₂(C₆H₄C₂O₄)₄] ? 3H₂O was solved. In the [(UO₂)₄O₂(C₆H₄C₂O₄)₄]^4? anions forming the main structural motif, each bridging oxygen atom μ₃-O combines one pentagonal and two hexagonal bipyramids, which, in turn, are combined in centrosymmetrical tetramers. The phthalate ions have coordination capacity equal to 3; each ligand coordinates U(1) in the bidentate fashion via one carboxy group and U(2) in the bidentate fashion to form a planar seven-membered chelate ring.     

Crystal structure of mixed-valent Np(IV)/Np(V) chloride, [Np(NpO2)6(H2O)8(OH)Cl9]·H2O

A new mixed-valent Np(IV)/Np(V) chloride, [Np(NpO₂)₆(H₂O)₈(OH)Cl₉]·H₂O, was synthesized, and its crystal structure was determined. The crystals consist of NpO ₂ ⁺ and Np⁴⁺ cations, of Cl^? and OH^? anions, of coordination-bonded water molecules, and of water molecules of crystallization. The Np(V) atom, Np(1), has pentagonal bipyramidal coordination surrounding with O atoms in the apical position and with the equatorial plane formed by three Cl^? anions, O atom of the adjacent NpO ₂ ⁺ cation, and O atom of water molecule. The mutual coordination of the neptunyl(V) ions, cation-cation (CC) interaction, links the Np(1) coordination polyhedra via common vertices into rings around sixfold axes, with the Np(V)?Np(V) distance in these fragments of 4.276 Å. The ring fragments are linked with each other via common equatorial edges of the bipyramids into layers perpendicular to c-axis. The Np(IV) atom, Np(2), has coordination surrounding in the form of tricapped trigonal prism (CN 9) with the tetragonal lateral faces formed by the O atoms of the NpO ₂ ⁺ cations and the capping positions occupied by the O atoms of two water molecules and one hydroxy group. The Np(2) atoms act in CC interactions as coordination center for six NpO ₂ ⁺ ions, with the Np(IV)?Np(V) distance of 4.183 Å. The Np(2) polyhedra are arranged in the crystal between layers of the Np(1) coordination polyhedra, linking them with each other.