Low‐Dimensional Structural Units in Amine‐Templated Uranyl Oxoselenates(VI): Synthesis and Crystal Structures of [C3H12N2][(UO2)(SeO4)2(H2O)2](H2O), [C5H16N2]2[(UO2)(SeO4)2(H2O)](NO3)2, [C4H12N][(UO2)(SeO4)(NO3)], and [C4H14N2][(UO2)(SeO4)2(H2O)]

The crystals of four amine‐templated uranyl oxoselenates(VI), [C₃H₁₂N₂][(UO₂)(SeO₄)₂(H₂O)₂](H₂O) ( 1 ), [C₅H₁₆N₂]₂[(UO₂)(SeO₄)₂(H₂O)](NO₃)₂ ( 2 ), [C₄H₁₂N][(UO₂)(SeO₄)(NO₃)] ( 3 ), and [C₄H₁₄N₂][(UO₂)(SeO₄)₂(H₂O)] ( 4 ) were prepared by evaporation from aqueous solution of uranyl nitrate, selenic acid and the respective amine. The crystal structures of all four compounds have been solved by direct methods from X‐ray diffraction data. The structure of 1 (triclinic, , a = 7.5611(16), b = 7.7650(17), c = 12.925(3) Å, α = 94.605(18), β = 94.405(17), γ = 96.470(17)°, V = 748.8(3) ų, R₁ = 0.029 for 2769 unique observed reflections) is based upon 0D‐units of the composition [(UO₂)₂(SeO₄)₄(H₂O)₄]^4?. These discrete units are composed from two pentagonal [UO₇]^8? bipyramids linked via [SeO₄]^2? tetrahedra and are unknown in structural chemistry of uranium so far. The structure of 2 (monoclinic, C2/c, a = 28.916(5), b = 8.0836(10), c = 11.9856(16) Å, β = 110.909(11)°, V = 2617.1(6) ų, R₁ = 0.035 for 2578 unique observed reflections) contains [(UO₂)(SeO₄)₂(H₂O)]^2? chains of corner‐sharing pentagonal [UO₇]^8? bipyramids and [SeO₄]^2? tetrahedra. The chains run parallel to the c axis and are arranged into layers parallel to (100). In the structure of 3 (monoclinic, C2/m, a = 21.244(5), b = 7.1092(11), c = 8.6581(18) Å, β = 97.693(17)°, V = 1295.8(4) ų, R₁ = 0.027 for 1386 unique observed reflections), pentagonal [UO₇]^8? bipyramids share corners with three [SeO₄]^2? tetrahedra each and an edge with a [NO₃]^? anion to form [(UO₂)(SeO₄)(NO₃)]^? chains parallel to the b axis. In the structure of 4 (triclinic, , a = 6.853(2), b = 10.537(3), c = 10.574(3) Å, α = 99.62(3), β = 94.45(3), γ = 100.52(3)°, V = 735.6(4) ų, R₁ = 0.045 for 2713 unique observed reflections), one symmetrically independent pentagonal [UO₇]^8? bipyramid shares corners with four [SeO₄]^2? tetrahedra to form the [(UO₂)(SeO₄)₂(H₂O)]^2? chains parallel to the a axis. A comparison to related uranyl compounds is given.     

Saure Sulfate des Neodyms: Synthese und Kristallstruktur von (H5O2)(H3O)2Nd(SO4)3 und (H3O)2Nd(HSO4)3SO4

Acidic Sulfates of Neodymium: Synthesis and Crystal Structure of (H₅O₂)(H₃O)₂Nd(SO₄)₃ and (H₃O)₂Nd(HSO₄)₃SO₄ Light violett single crystals of (H₅O₂)(H₃O)₂ · Nd(SO₄)₃ are obtained by cooling of a solution prepared by dissolving neodymium oxalate in sulfuric acid (80%). According to X‐ray single crystal investigations there are H₃O⁺ ions and H₅O₂⁺ ions present in the monoclinic structure (P2₁/n, Z = 4, a = 1159.9(4), b = 710.9(3), c = 1594.7(6) pm, β = 96.75(4)°, R_all = 0.0260). Nd³⁺ is nine‐coordinate by oxygen atoms. The same coordination number is found for Nd³⁺ in the crystal structure of (H₃O)₂Nd(HSO₄)₃SO₄ (triclinic, P1, Z = 2, a = 910.0(1), b = 940.3(1), c = 952.6(1) pm, α = 100.14(1)°, β = 112.35(1)°, γ = 105.01(1)°, R_all = 0.0283). The compound has been prepared by the reaction of Nd₂O₃ with chlorosulfonic acid in the presence of air. In the crystal structure both sulfate and hydrogensulfate groups occur. In both compounds pronounced hydrogen bonding is observed.     

(C5H6N4O)(C5H5N4O)3(C5H4N4O)[Bi2Cl11]Cl2 as a simple and efficient catalyst in Biginelli reaction

A highly efficient and facile procedure for the one‐pot three‐component synthesis of 3,4‐dihydropyrimidin‐2‐(1H )ones/thiones from the one‐pot condensation of aldehyde, β‐dicarbonyl compound and urea/thiourea was developed. The methodology is applicable to a wide range of substrates with high yield in the presence of (C₅H₆N₄O)(C₅H₅N₄O)₃(C₅H₄N₄O)[Bi₂Cl₁₁]Cl₂. The complex is an air‐stable, environmentally friendly and recoverable catalyst and can efficiently catalyze the Biginelli reaction. The catalyst has high catalytic efficiency with low catalyst loading, and can be recycled ten times with only a small loss of activity.     

Synthesis and Crystal Structure of [VO2（C17H11N3O2） ] [VO （C4H13N3）（C6H5N3O） ]（C2H5OH）

The reaction of VO（acac）2 with 2-hydroxyl-1-naphthaldehyde isonicotinyl hydrazone and amines （ethylenediamine or diethylenetriamine） in CH3OH yields crystals of novel vanadium compounds characterized by IR, NMR spectroscopic methods and X-ray single-crystal structure determination. Two different vanadium units exist in the crystal cell of [VO2（C17H11N3O2）][VO- （C4H13N3）（C6H5N3O）]（C2H5OH） which crystallizes in the triclinic system, space group P1 with a = 8.0104（17）, b = 13.898（3）, c = 14.955（3）A, α = 89.103（4）, β = 79.551（4）, γ = 78.352（4）°, V = 1603.3（6）A^3, Mr = 723.54, Dc = 1.499 g/cm^3, Z = 2, λ（MoKα） = 0.71073 ]A,μ= 0.644 mm^-1, F（000） = 748, the final R = 0.0547 and wR = 0.0997 for 8920 observed reflections with I 〉 2σ（I）. According to structure analysis, two different molecules are arranged in the lattice and the two vanadium atoms adopt octahedral and square pyramidal coordination geometries, respectively. The interactions between DNA and vanadium complexes have been investigated by UV-Vis absorption spectro- photometry.     

吡嗪桥连异三核配合物的合成及晶体结构

Ag(Ⅰ)配合物的几何构型多变,最常见的是配位数为2的线性构型和配位数为4的四面体构型。前者如Ag(NH_3)_2~+及Ag(CN)_2,后者如[Ag(SC(CH_3)NH_2)_4]Cl、[(Ph_3)Ag(Cl)]和[(Ph_3MeP)_3Ag(BH_4]等。配位数为4的平面四方构型却罕见,只在当有一定刚性的四氮杂环十四烷和Ag(Ⅰ)生成配合物时才是平面四方构型。 本文报道一种新型异三核含银配合物的合成及其晶体结构,其中Ag是平面四方构型。     

Synthesis,Structure and Characterization of Three Metal Molybdate Hydrates: Fe(H2O)2(MoO4)2·H3O,NaCo2(MoO4)2(H3O2)and Mn2(MoO4)3·2H3O

Three metal molybdate hydrates,Fe(H2O)2(MoO4)2·H3O(FeMo),NaCo2(MoO4)2(H3O2)(CoMo)and Mn2(MoO4)3·2H3O(MnMo),were synthesized by the mixed-solvent-thermal methods and characterized by singlecrystal X-ray...     

Two scandium–biuret complexes: [Sc(C2H5N3O2)(H2O)5]Cl3·H2O and [Sc(C2H5N3O2)4](NO3)3

The scandium(III) cations in the structures of pentaaqua(biuret‐κ²O,O′)scandium(III) trichloride monohydrate, [Sc(C₂H₅N₃O₂)(H₂O)₅]Cl₃·H₂O, (I), and tetrakis(biuret‐κ²O,O′)scandium(III) trinitrate, [Sc(C₂H₅N₃O₂)₄](NO₃)₃, (II), are found to adopt very different coordinations with the same biuret ligand. The roles of hydrogen bonding and the counter‐ion in the establishment of the structures are described. In (I), the Sc³⁺ cation adopts a fairly regular pentagonal bipyramidal coordination geometry arising from one O,O′‐bidentate biuret molecule and five water molecules. A dense network of N—H...Cl, O—H...O and O—H...Cl hydrogen bonds help to establish the packing, resulting in dimeric associations of two cations and two water molecules. In (II), the Sc³⁺ cation (site symmetry 2) adopts a slightly squashed square‐antiprismatic geometry arising from four O,O′‐bidentate biuret molecules. A network of N—H...O hydrogen bonds help to establish the packing, which features [010] chains of cations. One of the nitrate ions is disordered about an inversion centre. Both structures form three‐dimensional hydrogen‐bond networks.