Synthesis and crystal structure of a new uranyl selenite(IV)-selenate(VI), [C5H14N]4[(UO2)3(SeO4)4(HSeO3)(H2O)](H2SeO3)(HSeO4)

Crystals of a new uranyl selenite(IV)-selenate(VI), [C₅H₁₄N]₄[(UO₂)₃(SeO₄)₄(HSeO₃)(H₂O)]·(H₂SeO₃)(HSeO₄) were obtained by evaporation from aqueous solutions. The compound crystallizes in the triclinic system, space group $P\bar 1$ , a = 11.7068(9), b = 14.8165(12), c = 16.9766(15) Å, α = 73.899(6)°, β = 76.221(7)°, γ = 89.361(6)°, V = 2743.0(4) ų, Z = 2. The crystal structure was solved by direct methods and refined to R ₁ = 0.081 (wR ₂ = 0.150) for 6966 reflections with |F _hkl | ≥ 4σ(|F _hkl |). The structure is based on [(UO₂)₃(SeO₄)₄(HSeO₃)(H₂O)]^3? layers formed by joining uranyl pentagonal bipyramids, selenate tetrahedra, and selenite pyramids. The [HSe(VI)O₄]^? anions, [H₂Se(IV)O₃] molecules, and protonated methylbutylamine cations are arranged between the layers.     

Geometric isomerism of layered complexes of uranyl selenates: Synthesis and structure of (H3O)[C5H14N]2[(UO2)3(SeO4)4(HSeO4)(H2O)] and (H3O)[C5H14N]2[(UO2)3(SeO4)4(HSeO4)(H2O)](H2O)

New uranyl selenates with organic cations (H₃O)[C₅H₁₄N]₂[(UO₂)₃(SeO₄)₄(HSeO₄)(H₂O)] (I) and (H₃O)[C₅H₁₄N]₂[(UO₂)₃(SeO₄)₄(HSeO₄)(H₂O)](H₂O) (II) were synthesized by evaporation of aqueous solutions and studied. Compound I has monoclinic symmetry, space group C2/c, a = 16.7572(13), b = 11.7239(12), c = 19.0490(13) Å, β = 98.875(6)°, V = 3697.6(5) ų, Z = 4. The crystal structure was solved by the direct method and refined to R ₁ = 0.085 for 2868 reflections with |F _hkl | ≥ 4σ|F _hkl |. Compound II has monoclinic symmetry, space group P2₁/n, a = 10.8252(10), b = 19.0007(10), c = 18.6463(15) Å, β = 100.324(7)°, V = 3773.2(5) ų, Z = 4. The crystal structure was solved by the direct method and refined to R ₁ = 0.084 for 5721 reflections with |F _hkl | ≥ 4σ|F _khl |. The structures of I and II are based on layered complexes [(UO₂)₃(SeO₄)₄(HSeO₄)(H₂O)]^3? formed by combination of uranyl pentagonal bipyramids and selenate tetrahedra. H₃O⁺ cations, water molecules, and protonated methylbutylamine cations are located in the interlayer space. Geometric isomerism of two-dimensional complexes [(UO₂)₃(SeO₄)₅(H₂O)] in the structures of uranyl selenates was found and described.     

Crystal structure of Rb3[UO2(CH3COO)3]2[UO2(CH3COO)(NCS)2(H2O)]

The structure of Rb₃[UO₂(CH₃COO)₃]₂[UO₂(CH₃COO)(NCS)₂(H₂O)] was studied by single crystal X-ray diffraction. The compound crystallizes in the monoclinic system with the unit cell parameters (at 100 K) a = 18.387(3), b = 16.398(3), c = 12.460(2) Å, β = 92.837(5)^°, V = 3752.4(11) ų, space group C2/c, Z = 4, R = 0.0390. The uranium-containing structural units of the crystals are isolated mononuclear groups [UO₂(CH₃COO)₃]^? and [UO₂(CH₃COO)(NCS)₂(H₂O)]^?, belonging to crystal-chemical groups AB ₃ ⁰¹ and AB⁰¹M ₃ ¹ (A = UO ₂ ²⁺ , B⁰¹ = CH₃COO^?, M¹ = NCS^? and H₂O) of uranyl complexes, respectively. The uranium-containing complexes are linked in a framework by hydrogen bonds and by electrostatic interactions with Rb⁺ cations.     

Synthesis, structure, and properties of [Be(H2O)4][UO2(CH3COO)3]2

Crystals of previously unknown compound [Be(H₂O)₄][UO₂(CH₃COO)₃]₂ were prepared and studied by X-ray diffraction analysis. The compound crystallizes in the tetragonal system, unit cell parameters (at 100 K): a = 10.3647(3), c = 23.4127(8) Å, V = 2515.16(13) ų, space group I4₁/a, Z = 4, R = 0.0194. The structure consists of mononuclear complexes [Be(H₂O)₄]²⁺ and [UO₂(CH₃COO)₃]^? linked with each other by electrostatic interactions and hydrogen bonds formed by water molecules and O atoms of acetate anions. The compound was also studied by methods of thermal analysis and IR spectroscopy.     

Supramolecular templates for the synthesis of new nanostructured uranyl compounds: Crystal structure of [NH3(CH2)9NH3][(UO2)(SeO4)(SeO2OH)](NO3)

Crystals of a new uranyl selenate, [NH₃(CH₂)₉NH₃][(UO₂)(SeO₄)(SeO₂OH)](NO₃) (1), were prepared by isothermal evaporation from aqueous solution at room temperature. The crystal structure was solved by the direct method $ P\bar 1 $ , a = 10.7480(7), b = 13.8847(9), c = 14.6363(10) Å, α = 109.9600(10)°, β = 103.212(2)°, γ = 90.4090(10)°, V = 1990.0(2) ų, Z= 4) and refined to R ₁ = 0.0379 (wR ₂ = 0.0636) for 8515 reflections with ¦Fo¦ ≥ 4σ_F. The structure is based on [(UO₂)(SeO₄)(SeO₂OH)]-layers parallel to the (001) plane. In the structure of 1, there are two crystallographically independent 1,9-diammoniononane cations forming micelles in which the hydrocarbon chains are packed crosswise. The micelles are cylinders with an elliptical cross section and a rough surface. They are organized by the principle of hydrophilic and hydrophobic interactions. The cylinders are separated from each other by layers of triangular NO ₃ ^? groups. Compound 1 is an example of organic-inorganic composites with a unidimensional organic substructure in which the protonated chain-like diamine molecules arranged crosswise form cylindrical supramolecular templates.     

[Ag(PPh_3)_2(CH_3COO)]_2·3H_2O的合成和晶体结构

将醋酸银和三苯基磷按1∶2摩尔比例进行反应得到化合物Ag(PPh3)2(CH3COO)]2,采用红外光谱、核磁共振、元素分析和单晶X射线衍射的方法,对其结构进行了表征.晶体结构解析结果显示,配合物属单斜晶系,空间群C2/c,a=44.286 8',b=13.269 6',c=24.997 0',α=90.000°,β=105.573°,γ=90.000°,Z=8,R=0.052 0,wR2=0.132 4.     

Synthesis,crystal structure and solubility of C6H14N4O2,C4H4O4,2H2O

Synthesis, crystal structure and solubility of a new non-linear optical material l-arginine maleate dihydrate have been reported here. From the solubility studies with different solvents, water was found to be the most suitable one. Title compound crystallized in the triclinic space group P1 with Z=1 and unit cell dimensions a=5.264(3) Å, b=8.039(3) Å, c=9.784(3) Å, α=106.19(3)°, β=97.24(3)°, γ=101.66(2)°. The present complex of l-arginine contains a positively charged zwitterionic arginine molecule and a negatively charged semi-maleate ion. The molecules are held together by a three-dimensional network of hydrogen bonds.     

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.     

A single crystal X-ray diffraction and IR study of (NH4)2[(UO2)C2O4(CH3COO)2]

A single crystal X-ray diffraction study of (NH₄)₂[(UO₂)C₂O₄(CH₃COO)₂] was performed. The compound crystallizes in the monoclinic system; unit cell parameters (at 100 ± 2 K): a = 6.793(2), b = 18.866(6), c = 20.730(7) Å, β = 90.040(7)°, space group P2₁/c, Z = 8, V = 2656.5(14) ų, R = 0.0495. The main structural units of the crystals are mononuclear complexes [(UO₂)C₂O₄(CH₃COO)₂]^2? belonging to crystal-chemical group AB ₃ ⁰¹ (A = UO ₂ ²⁺ , B⁰¹ = CH₃COO^? and C₂O ₄ ^2? ) of uranyl complexes. The uranium-containing anions are linked with ammonium cations by electrostatic interactions and a system of hydrogen bonds. The results of the X-ray diffraction analysis of the compound are well consistent with the IR data.     

Interaction of U(VI), Np(VI), Pu(VI), and Np(V) with benzenetricarboxylic acids: Complexation in aqueous solutions, synthesis, and crystal structure of uranyl complexes [UO2(H2O)2{C6H3(COO)2(COOH)}]2·2H2O and [(UO2)3(H2O)4{C6H3(COO)3}2]

The complexation of U(VI), Np(VI), and Pu(VI) and of Np(V) with 1,2,3- and 1,2,4-benzenetricarboxylic acids (BTC) in aqueous solutions was studied in wide ranges of pH and actinyl ion concentrations. The compositions of the forming hexavalent actinide complexes were determined. Their apparent stability constants β₁′ depend on pH of the solution: in the pH range 2–4, logβ₁′ from 2 to 4 for the complexes of U(VI), Np(VI), and Pu(VI) with 1,2,3-BTC and from 1.5 to 3.5 for the complexes with 1,2,4-BTC. For Np(V), the β₁′ values are close with both acids, and at equal pH values the Np(V) complexes are less stable than the An(VI) complexes (An = U, Np, Pu). With an increase in pH from ～3 to 6.2–6.9, logβ₁′ of the Np(V) complexes increases approximately from 0.5 to 3. Solid U(VI) complexes with 1,2,3- and 1,2,4-benzenetricarboxylic acids were synthesized by the hydrothermal method, their crystal structure was determined, and the IR spectra were examined.     

Synthesis and crystal structure of K3[NpO4(OH)2]

Attempts were made to isolate anhydrous compounds of [NpO₄(OH)₂]^3? anions with heavy alkali metal cations (K, Rb, Cs) by crystallization at elevated temperatures, and the salt K₃[NpO₄(OH)₂] was isolated and studied. Crystals of K₃[NpO₄(OH)₂] consist of tetragonal bipyramidal [NpO₄(OH)₂]^3? anions and K⁺ cations. The [NpO₄(OH)₂]^3? anion occupies the position in the symmetry center. The Np-O distances in this anion are 1.8992(7) and 1.9100(7) Å in the equatorial plane of the bipyramid and 2.3231(8) Å with OH groups. The OH hydrogen atoms participate in weak H bonds [O?O 3.0250(11) Å] linking the anions in layers [NpO₄(OH)₂] _n ^3n? parallel to the (010) plane. In the interlayer space, there are two crystallographically different K atoms. Their coordination number (CN) can be considered to be equal to 7 and 8. Comparison with the structures of the known compounds Na₃[NpO₄(OH)₂] and K₃[NpO₄(OH)₂]·2H₂O was made. The structure of the latter compound was redetermined with higher accuracy. The failure of attempts to prepare the anhydrous rubidium and cesium compounds is probably due to large ionic radius of these cations, requiring high coordination number.     

Synthesis and Crystal Structure of Cs4[UO2(CO3)3]

Light green transparent crystals of Cs₄[UO₂(CO₃)₃] were prepared by evaporation from aqueous solutions. The crystal structure was refined to R ₁ = 0.039 (wR ₂ = 0.081) for 2311 reflections with |Fhkl| 4|Fhkl|. Monoclinic system, space group C2/c, a = 11.5131(9), b = 9.6037(8), c = 12.9177(10) Å, = 93.767(2)°, V = 1425.2(2) ų. The structure of Cs4[UO2(CO3)3] consists of isolated complex ions [UO₂(CO₃)₃]^{4 -} formed by uranyl cation UO₂ ^{2 +} and three CO₃ ^{2 -} groups. The equatorial planes of the [UO₂(CO₃)₃]^{4 -} ions are approximately parallel to the (201) plane. The nine-coordinate Cs⁺ cations are located between the complex anions. The compound is isostructural with M4[UO2(CO3)3] with M = K, NH₄, and Tl, but not isostructural with Na₄[UO₂(CO₃)₃].     

Studies on three-dimensional coordination polymer [Cd2(N2H4)2(N3)4]n: crystal structure, thermal decomposition mechanism and explosive properties

A 3D coordination polymer of cadmium(II) hydrazine azide, [Cd2(N2H4)2(N3)4]n, was synthesized and characterized by elemental analysis and Fourier transform infrared (FT-IR) spectrum. Its crystal structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to monoclinic, P2(1)/c space group, a=12.555(2)A, b=11.724(2)A, c=7.842(1)A, beta=94.56(2) degrees and Z=4. The crystal contains two crystallographically independent sets of distorted octahedral Cd(II) atoms and dimeric units of Cd2N2, Cd2(NNN)2, Cd2(NN)2 through double micro-1, 1 azide bridges, micro-1, 3 azide bridges and bidentate bridging hydrazine ligands, respectively, and thus generating a 3D network structure. The thermal decomposition mechanism of the complex was studied by using differential scanning calorimetry (DSC), thermogravimetry-derivative thermogravimetry (TG-DTG) and FT-IR techniques. Under nitrogen atmosphere with a heating rate of 10 degrees C/min, the thermal decomposition of the complex contained two intense exothermic decomposition processes in the range of 150-304 degrees C in the DSC curve, and the final decomposed residue at 500 degrees C was Cd. Sensitivity tests revealed that the title complex is very insensitive to external stimuli.     

Crystal structure of a new organic dihydrogenomonophosphate (C6H8N3O)2(H2PO4)2

Chemical preparation, X-ray single-crystal, thermal behavior, and IR spectroscopy investigations are given for a new organic cation dihydrogenomonophosphate (C₆H₈N₃O)₂(H₂PO₄)₂ (denoted IAHP) in the solid state. This compound crystallizes in the orthorhombic space group P2₁2₁2₁. The unit cell dimensions are: a = 7.422(3) Å, b = 12.568(5) Å, c = 20.059(8) Å with V = 1871.1(13) Å³ and Z = 4. The structure has been solved using direct method and refined to a reliability R factor of 0.029. The atomic arrangement can be described as inorganic layers of H₂PO₄⁻ anions between which are located the organic groups (C₆H₈N₃O)⁺ through multiple hydrogen bonds.     

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

Rare earth co-permeation of (NH4)3[CrMo6O24H6]•7H2O was reported and the conductivity of (NH4)3[CrMo6O24H6] was improved by 6.734×109 times. X-ray fluorescence spectrometry (XRF), thermogravimetry-differential thermal analysis (TG-DTA), X-ray diffraction (XRD) have been used to character (NH4)3[CrMo6 O24H6] •7H2O and permeated 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.     

Synthesis and crystal structure of chlorate-enclathrated in aluminogermanate sodalite Na8[AlGeO4]6(ClO3)2

Encapsulation of chlorate in sodalite with aluminogermanate host framework has been obtained by one pot hydrothermal synthesis at 393 K. The crystal structure of Na₈[AlGeO₄]₆(ClO₃)₂; sodalite was refined from X-ray powder data in the space group P $\bar 4$ 3n: a = 9.169 Å, where Al-O-Ge angle is 137.6°. The ²⁷Al MAS NMR study confirmed alternate Ge and Al ordering of the sodalite framework, while ²³Na gave insight into the structure and dynamics of the cage fillings. Infrared spectrum confirmed the encapsulation of chlorate as well as the framework formation of aluminogermanate sodalite. SEM study showed the retention of cubical morphology of the aluminogermanate sodalite. Thermogravimetric analysis provided information on the extent of chlorate entrapment, stability within the sodalite cages and decomposition properties.     

Synthesis and crystal structures of a new (2,3-(CH3)2C6H3NH3)H2XO4 (X=P,As)

The aim of encapsulation of 2,3-dimethylanilinium cation in (H₂XO₄)_n polymeric anion chains is to build acentric frameworks that are efficient for non-linear optical (NLO) applications. The synthesis and structures of two new inorganic–organic NLO crystals with general formula (2,3-(CH₃)₂C₆H₃NH₃)H₂XO₄ (X=P, As) are reported. The magnitude of their second harmonic generations (SHG) responses was found to be between the KDP and urea. They crystallize with monoclinic unit-cells and are isotopic. We have determined the structure of phosphoric salt. The following unit-cell parameters were found: a=8.866(3) Å, b=5.909(6) Å, c=10.644(5) Å, β=112.44(1)°, V=515.5(5) Å³ and D_X=1.412 g cm⁻³. The space group is P2₁ with Z=2. The structure was refined with R=0.041 (R_w=0.057) for 1652 reflections with I≥3σ(I). It exhibits infinite (H₂PO₄)_nⁿ⁻ chains. The organic groups (2,3-(CH₃)₂C₆H₃NH₃)⁺ are anchored between adjacent polyanions through multiple hydrogen bonds. Chemical preparation, crystal structure, calorimetric and spectroscopic investigation are described.