[Ni(en)3]4[HVⅣ12VⅤ6O42(PO4)]复合物的合成及晶体结构

A new complex [Ni(en)₃]₄[HV^Ⅳ₁₂V^Ⅴ₆O₄₂(PO₄)] has been hydrothermally synthesized and characterized by X-Ray diffraction, IR and Elemental analysis. Single crystal X-ray analysis indicates that this compoud crystallizes in cubic system,space group Im 3m with a=17.4081(2)?, V=5275.38(10)?³, R=0.0420, wR=0.1055, Z=2, D_c=1.663g·cm^-3, μ=2.297mm^-1, F(000)=2636. The crystal structure consists of [Ni(en)₃]²⁺ cations and {HV₁₈O₄₂(PO₄)}^8- cluster anion which construct from 18 {VO₅} square pyramids. The VO₅ pyramids joined each other to form a {V₁₈O₄₂} cage hosting a tetrahedral {PO₄}^3- moiety with disordered oxygen atoms. CCDC: 185574.     

Dissipative structures formed in the course of drying the colloidal crystals of silica spheres on a cover glass

Macroscopic and microscopic dissipative structural patterns formed in the course of drying the deionized aqueous colloidal crystal suspensions of silica spheres (diameter: 103 nm) on a cover glass have been observed. Spoke-like and ring-like patterns are formed in the macroscopic scale; the former is the crack in the sphere film and the latter is the hill accumulated with spheres formed around the outside edge. The neighbored inter-spoke angle, thickness of the film, and other morphological parameters have been discussed as a function of sphere concentration, concentration of sodium chloride, and the inclined angle of the cover glass. Fractal patterns of the mud cracks are observed in the microscopic scale. Capillary forces between spheres at the air-liquid surface and the relative rates between the water flow at the drying front and the convection flow of spheres are important for the pattern formation. Electronic Publication     

Synthesis and Crystal Structure of Two Modifications of Hexaaquamagnesium(II) Hypophosphite

Two modifications of hexaaquamagnesium(II) hypophosphite [Mg(H₂O)₆](H₂PO₂)₂ have been synthesized and structurally characterized. Literature data are available for one of these forms. The geometrical characteristics of hexaaqua cations, hypophosphite anions, and nets of hydrogen bonds between the hypophosphite anions and the coordinated water molecules are analyzed. The packing motif of the structure-forming fragments was found to be the same for the two structures, except that modification of the inner structure of the complex cation leads to different nets of hydrogen-bonded cations and anions.     

1,3-丙二胺的不对称双Schiff碱异三核配合物的合成表征、晶体结构与磁性研究

合成了一种新的不对称双Schiff碱Cu(II)单核配合物Cu(HLt) (1) (H₃Lt为N-3-羧基水杨醛-N'-水杨醛-缩1,3-丙二胺)及其两个异三核配合物[(CuLt)₂Ni]•2.5H₂O (2)和[(CuLt)₂Mn]•5H₂O (3), 并用元素分析、红外光谱、电子光谱对它们进行了结构表征. 用X射线单晶衍射法测定了配合物3的晶体结构, 其晶胞中每个不对称单元包含一个异三核中性分子, 在此三核分子中, 中心Mn^2＋离子位于[O₆]的变形八面体配位环境中, 两个端基Cu^2＋离子位于[N₂O₂]的平面正方场中. 在5～300 K范围内测定了两个三核配合物的变温磁化率, 经拟合得化合物2的磁交换参数为－57.7 cm^－1, 化合物3的磁交换参数为－28.5 cm^－1, 表明在两个异三核配合物中, 中心M^2＋离子与外部Cu^2＋离子间存在弱的反铁磁自旋交换作用.     

Synthesis and Crystal Structure of [Co(H<Subscript>2</Subscript>O)<Subscript>6</Subscript>](C<Subscript>19</Subscript>H<Subscript>17</Subscript>O<Subscript>4</Subscript>SO<Subscript>3</Subscript>)<Subscript>2</Subscript>⋅8H<Subscript>2</Subscript>O

The title compound, cobalt 4′,7-diethoxylisoflavone-3′-sulfonate([Co(H₂O)₆](X)₂⋅8H₂O, X = C₁₉H₁₇O₄SO₃) was synthesized and its structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in the triclinic space group P-1 with cell parameters a = 9.026(3) Å, b = 16.431(5) Å, c = 18.195(6) Å, α = 72.289(4)^∘, β = 87.498(4)^∘, γ = 82.775(5)^∘, V = 2550.1(13) Å⁻³, D_c = 1.419 Mg m⁻³, and Z = 2. The results show that the title compound consists of one cobalt cation, six coordinated water molecules, eight lattice water molecules, and two 4′,7-diethoxylisoflavone-3′-sulfonate anions, C₁₉H₁₇O₄SO⁻₃. Two anions have different conformations. Twelve H atoms of six coordinated water molecules, as donors, form hydrogen bonds with four oxygen atoms of sulfo-groups of two anions and eight oxygen atoms of eight lattice water molecules. In addition, π < eqid1 > ⋅ < eqid2 > π stacking interactions exist in the crystal structure, which together with hydrogen bonds lead to supramolecular formation with a three-dimensional network.     

Crystal Structure of Complex Tris（4,4,4—trifluoro—1—pheny1—1,3—butanedione）（1,10—phenanthroline）Europium（Ⅲ）

The complex Eu(btfa)₃ (phen) (btfa=4,4,4‐trifluoro‐1‐phenyl‐1, 3‐butanedione, phen = 1,10‐phenanthroline) has been prepared and characterized by elemental analysis, IR and UV spectroscopies. The crystal and molecular structures of the complex have been determined by X‐ray diffraction analysis. It belongs to the monoclinic crystal system, space group P2₁/c with a = 0.9700(2) nm, b = 3.7450(5) nm, c = 1.0917(3) nm, β = 92.51(2)°, V = 3.962(1) nm⁵, Z = 4, D_c = 1.639 g/cm³, μ = 1.676 mm^?1, F(000) = 1936, R₁, = 0.0388, wR₂ = 0.0775. Structure analysis shows that the europium(III) ion is coordinated to six oxygen atoms of β‐diketonate anions and two nitrogen atoms of phenanthroline molecule. The coordination polyhedron is an approximate square antiprism.     

含轴手性磺酸配体的镉配合物(英)

The crystal structure of [Cd(BDA)(phen)₂(H₂O)](H₂O)₂ (1) (BDA=6,6′-dibromo-2,2′-dimethoxy-1,1′-binaphthylene-4,4′-disulfonate, phen=1,10-phenanthroline)consists of a cadmium center whose coordination environment can be best described as a slightly distorted octahedron defined four nitrogen atoms from two phen ligands and two oxygen atoms differently from BDA ligand and water. There are strong hydrogen-bonding interactions between water and sulfonate group of BDA ligands to construct the 3D network. CCDC: 277921.     

新颖双核钐硫酚化合物[(THF)3I2Sm(m-SAr)]2 (Ar = Ph, 4-Me2NC6H4)的合成与化合物[(THF)3I2Sm(m-S-4-Me2NC6H4)]2的晶体结构

Reactions of SmI2 in THF with ArSSAr produced two binuclear samarium thiolate complexes [（THF）3I2- Sm（μ-SAr）]2 [Ar=Ph （1）, 4-Me2NC6H4 （2）] in high yields. The structure of 2 was characterized by single crystal X-ray crystallography. The crystal of 2 belongs to the triclinic system with space group P 1 and a=0.95705（13） nm, b= 1.22287（14） nm, c= 1.26450（14） nm, a=64.194（11）°, B=78.491（13）°, y=76.176（12）°, V= 1.2860（3） nm^3, Z= 1,μ=4.783 mm^-1, Dc= 1.964 Mg/m^3, M= 1521.19, S= 1.046, R1=0.0358, wR2=0.0910. X-ray analysis revealed that 2 is a thiolate-bridged dimer in which each Sm atom adopts a distorted pentagonal bipyramidal coordi- nation geometry.     

Crystal structure of KAsUO<Subscript>6</Subscript>·<Subscript>3</Subscript>H<Subscript>2</Subscript>O at 100 and 293 K

The crystal structure of KAsUO₆·3H₂O was solved at 100 K and 293 K. KAsUO₆·3H₂O at T = 100 K: tetragonal, P4/ncc, a = 7.2037(6) Å, c = 17.811(2) Å; Z = 4, R1 = 0.0263, wR2 = 0.0546, for 618 independent reflections; at T = 293 K: tetragonal, P4/ncc, a = 7.1600(4) Å, c = 17.746(1) Å; Z = 4, R1 = 0.0263, wR2 = 0.0433 for 427 independent reflections. The results of X-ray analysis are compared with our previous data on heat capacity of this compound, and changes that take place in the structure at elevated temperature are considered.     

配合物[Cu2(phen)2](SiW12O40)(H2O)7的合成、晶体结构及电化学分析

The title complex has been synthesized by the reaction of silicotungstic acid, 1,10-phenanthroline (phen) monohydrate and cupric acetate. The crystal structure belongs to triclinic system, space group P1 with a=1.158 46(15) nm, b=1.658 8(2) nm, c=1.664 4(2) nm, α=82.090(2)°, β=76.001(2)°, γ=86.531(2)°, and V=3.072 6(7) nm³, D_c=3.887 g·cm^-3, Z=2, F(000)=3 196. R₁=0.086 7, wR₂=0.185 8. The structure shows that the copper(Ⅱ) atom is coordinated with two nitrogen atoms from the one phen and three oxgygen atoms from three water, forming a distorted square-pyramid configuration The cyclic voltametric behavior of the complex is also reported. CCDC: 298807.