X-ray Molecular and Crystal Structure Study of the Fe(II) Complex Containing 1,10-Phenanthroline and Saccharin: [Fe(C12H8N2)3] (C6H4COSO2N)2 · 4 H2O

X-ray molecular and crystal structure of the [Fe(C₁₂H₈N₂)₃] (C₆H₄COSO₂N)₂ · 4 H₂O is reported. In the complex, the Fe atom is bonded to the six nitrogen atoms with a distorted octahedral stereochemistry.     

双核Cu(II)-5-溴水杨醛缩氨基甲磺酸席夫碱4,4'-联吡啶三元配合物的合成及晶体结构

采用Cu(II)盐和氨基甲磺酸缩-5-溴水杨醛席夫碱(H2L)以及4,4'-联吡啶(bpy)在乙醇和水溶液中合成了三元配合物,通过元素分析、红外光谱对配合物进行了表征,并用X射线衍射测定了其结构.结构解析表明,该标题配合物属单斜晶系,空间群P21/c,晶胞参数为: a=0.9509(2) nm,b=1.8783(2) nm,c=1.0514(2) nm;β= 98.48 (1)°,V=1.8575(3) nm3, Z=2,Dc=1.812 g·cm-3, F(000)=1016, μ=3.473,最终偏差因子(对I＞2σ(I)的衍射点)R1=0.0459, wR2=0.0739,对全部衍射点R1=0.1205, wR2=0.0887, ω-1= [σ2(Fo)2+0.0345P],P=(Fo2+2Fc2)/3.邻近配合物分子间存在着大量的氢键, 席夫碱三元配合物通过氢键作用堆积成2D网状结构.     

Crystal Structure Determination of Nickel (2,2-Dipyridyl) Sulphate Hexahydrate [Ni(C10H8N2) · 4 H2O]SO4 · 2H2O

[Ni(C₁₀H₈N₂) · 4 H₂O]SO₄ · 2 H₂O, Mr = 418.7, monoclinic, P1 , a = 7.781(3), b = 9.421(3), c = 11.457(4) Å, α = 87.54(2)º, β = 96.40(2)º, γ = 102.58(2)º, ν = 814.5 Å, D_x = 1.26 g/cm³, Z = 2, (MoKx) = 0.71073 Å, μ = 7.0 cm⁻¹: T = 23 °C, R = 0.047 for 2139 reflections having intensities greater than 36. The structure was solved using the Patterson heavy-atom method and the remaining atoms were located in succeeding difference Fourier syntheses. The structure was then refined by full matrix least-squares using anisotropic temperature factors. Hydrogen atoms were located and their positions and isotropic parameters were refined.     

Electronic Structure of [Cu(C7H4NO3S)2(H2O)4] · 2H2O Crystal

The electronic absorption spectrum and ESR spectrum of the crystal of the title compound [Cu(C₇H₄NO₃S)₂(H₂O)₄] · 2 H₂O, are measured. The experimental results are discussed quantitatively by using the ligand field theory and the radial wave function of non-free Cu(II). The electronic structure of the compound is in agreement with its crystal structure.     

Ni(Ⅱ)5-溴水杨醛缩氨基甲磺酸席夫碱-邻菲咯林三元配合物的合成

本文采用Ni(Ⅱ)盐和氨基甲磺酸缩5-溴水杨醛席夫碱以及1,10-邻菲咯林(phen)在甲醇和水溶液中合成了三元配合物,通过元素分析、红外光谱对配合物进行了表征,并X射线衍射测定了其结构.结构解析表明,该标题配合物属三斜晶系,空间群P-1,晶胞参数为a=1.2868(3)nm,b=1.4536(3)nm,c=1.4705(3)nm;α=85.79(3)°,β=67.62(3)°,γ=77.21(3)°,V=2.4799(9)mm3,Z=2,Dc=1.580 g·cm-3,F(000)=1196,μ=2.521, 最终偏差因子(对Ⅰ>2σ(Ⅰ)的衍射点)R1=0.0604,ωR2=0.1446,对全部衍射点R1=0.1531,ωR2=0.1914,ω-1=[s2(Fo2)+(0.0884P)2],P=(Fo2+2Fc2)/3.     

Structure of a Manganese (II) Complex Containing Saccharin and 1,10-Phenanthroline: [Mn(Sacch)2(o-Phen)2(H2O)2] · H2O

The X-ray crystal structure of the mononuclear manganese(II) complex containing saccharin and 1,10-phenanthroline, [Mn(Sacch)₂(o-Phen)₂(H₂O)₂] · H₂O, is reported. The manganese atom has a geometrical structure of hexa-coordinated distorted octahedron, saccharins interact with the central atom through water molecules.     

Ni(Ⅱ)-3,5-二氯水杨醛缩氨基甲磺酸席夫碱-邻菲咯林三元配合物的合成及晶体结构

采用Ni(Ⅱ)盐和氨基甲磺酸缩3,5-二氯水杨醛席夫碱(H2L)以及1,10-邻菲咯林(phen)在甲醇和水溶液中合成了三元配合物[Ni(Ⅱ)(C8H7O4NCl2S)(Phen)(H2O)]3(1),通过元素分析、红外光谱对配合物 1 进行了表征,并通过X射线衍射测定了其结构.结构解析表明,配合物 1 属三斜晶系,空间群P ī,晶胞参数为:a=1.5640(3)nm,b=1.5650(3)nm,c=1.5650(3)nm;α=94.84(3)°,β=94.73(3)°,γ=94.80(3)°,V=3.7881(13)nm3,Z=6,Dc=1.420 g· cm-3,F(000)=1602,μ=1.100 mm-1,最终偏差因子(对I>2σ(I)的衍射点),R1=0.0769,ωR2=0.1306,对全部衍射点R1=0.1323,ωR2=0.1468,ω-1=[σ2(Fo)2+(0.1977P)2],P=(Fo2+2Fc2)/3.配合物 1 通过卤卤作用(Cl-Cl 0.3574(8)nm)堆积成3D无限层状结构.     

Crystal Structure of Dimeric Cu(II) Complex {μ,μ'‐acetato O,O bis [N‐salicylidene‐2‐amino‐pyridine‐methanolato N,N,O]} : perchlorate

The crystal structure of the title complex has been solved using X‐ray diffraction data.The compound crystallizes from aqueous ethanol solvent in the triclinic system, space group P‐1, with unit cell parameters: a = 8.9532(1), b = 12.7423(3), c = 14.9012(3) Å, α = 73.767(1), β = 75.322(1), γ = 77.496(1)°, Z = 2, V = 1559.4(5) ų. The trial structure was determined by automated Patterson methods and subsequent difference Fourier techniques using DIRDIF98 and refined to a final R‐factor of 0.064. The copper ion Cu1 adopts a (4+1) square‐pyramidal geometry defined by the tridentate N‐salicylidimine dianions and the neutral monodentate pyridine ligand in the basal plane. The apical position is occupied by a solvent methanol molecule at a distance of 2.341(4) Å. The copper Cu2 adopts a square‐planar geometry.     

配位聚合物[Mn(bpda)(benzidine)]_n的晶体性能研究

根据文献合成了联苯二甲酸,并通过水热法制备了[Mn(bpda)(benzidine)]n暗棕色的针状晶体.通过X-射线衍射分析、元素分析、IR等方法对配合物进行了表征,并通过TG分析对该配合物的热稳定性及热分解机理做了初步探讨.结果表明,正是基于bpda分子四齿μ3-配位形式,使得该配体的热稳定性要明显高于另一配体联苯胺.     

Crystal and molecular structure of diaqua-bis-(3,5-dimethyl-1-guanyl pyrazole) nickel (II) nitrate, [Ni(C6N4H10)2(H2O)2](N03)2

The title compound crystallizes in space groupP2₁/n witha=10.651(3),b=11.082(2),c=8.993(3) Å,=106.79(3)°;R=0.064 andR _w=0.074 for 3399 observed reflections (I3(I)) from 3674 measured. The structure was solved by direct methods and refined by least squares. The Ni atom of the complex is located at a center of inversion, and is surrounded by four nitrogen atoms of the two ligands in square-planar geometry. The oxygen atoms of the two centrosymmetrically related water molecules complete the coordination around the metal ion to form an elongated octahedron.     

Crystal and molecular structure of tetrakis-(phenylenethiourea)tellurium(II) perchlorate hexahydrate,C28H24N8O8S4Cl2Te·6H2O

The synthesis and structural characterization of the title compound, C₂₈H₂₄N₈O₈S₄Cl₂Te·6H₂O are reported. The crystals are triclinic, space group P¯1 (No. 2), withZ=1 in a unit cell of dimensionsa=10.312(7),b=7.144(6),c=14.256(7) Å,=83.04(5),=92.15(5), and=101.25(6)°,V _c =1022 ų. The structure was solved by Fourier methods, and refined by full-matrix least squares toR=0.073 andR _w =0.077 for 1305 unique reflections. The tellurium atom in the molecule lies at a crystallographic center of symmetry, and is bonded to four phenylenethiourea sulfur atoms in a near square-planar arrangement with Te-S(1)=2.666(5), Te-S(2)=2.675(6) Å, and S(1)-Te-S(2)=88.7(3)°. The ligands behave as thiones. The crystal packing is stabilized by the extensive hydrogen bonding involving oxygen and nitrogen atoms. The Cl-O bond lengths are 1.29-1.36 Å and the O-Cl-O angles are 90–130° in the ClO₄ ^– moiety, and differ considerably from the normal values of 1.44 Å and 109°, respectively.     

Crystal structure of mixed-ligand copper(II) complexes. Bis(2,2′-bipyridyl)monophenylphos-phatocopper(II)monophenylphosphate monohydrate, [Cu(C10H8N2)2(C6H5OPO3)]-(C6H5OPO3H2)(H2O)

The title mixed-ligand copper(II) complex has been synthesized and its crystal structure at room temperature solved. The crystals are monoclinic:P2₁/c,a=12.004(3),b=19.402(5),c=14.192(4) Å,=108.80(3)°,Z=4. The structure was solved by direct methods, and refined to anR value of 0.041 for 4457 nonzero independent reflections. The crystal structure consists of discrete [Cu(bipy) (MPhP)] units, noncoordinated MPhPH₂, and H₂O molecules. Each [Cu(bipy)₂(MPhP)] unit involves a five coordinate CuN₄O chromophore with a distorted trigonal-bipyramidal stereochemistry. The phosphate groups are linked together by short hydrogen bonds of (P)-O-H--O-P type.     

Crystal and molecular structure of p-Toluquinone-monoguanylhydrazone,C8H10N4O

The crystal structure of p-toluquinone-monoguanylhydrazone is orthorhombic, space group Pna2₁ with 4 formula units C₈H₁₀N₄O in the unit cell. The lattice constants are a = 7.589, b = 20.117, and c = 5.699 Å. The structure was refined to the conventional R = 0.05. The configuration and conformation of the molecule as well as the unusual hydrogen bridge system are discussed.     

新型配位聚合物[Ni(C6H4NO2)2(H2O)4]n的水热合成和晶体结构

以NiCl2·6H2O和4-氰基吡啶为原料,在中温水热反应条件下,合成了一种新型配位聚合物[Ni(C6H4NO2)2(H2O)4]n单晶体,并对其进行了元素分析、红外光谱表征和X射线单晶衍射测定.该配位聚合物属三斜晶系,P-1空间群,a=0.6298(4)nm,b=0.6907(4)nm,c=0.9243(5)nm,α=96.437(8)°,β=105.184(9)°,γ=113.314(9)°,V=0.3456(3)nm3,Z=2,dc=1.802 g/cm3,μ=1.452mm-1,F(000)=194,R1=0.0309,R2=0.0753.该晶体通过配位键的连接和分子间氢键相互作用形成三维的网状结构.     

Crystal structures of 4-amino-1,2,4-triazolidine-3,5-dione (urazine) (C2H4N4O2) and dichlorobis (4-amino-1,2,4-triazolidine-3,5-dione-N,O) copper (II) (C4H8Cl2CuN8O4)

Crystal structure analyses of urazine and of its adduct with CuCl₂ show that this ligand can exchange interactions of stacking that cannot be defined as simple - interactions. The copper atoms are octahedrally coordinated by two oxygen atoms and two aminic nitrogen from chelating uraxines and two chlorine atoms. The crystals of urazine are monoclinicP2₁ c:a=6.741(1),b=5.815(1),c=11.141(2) Å,/gb=92.13(1)°,V _c=436.4(1) ų,Z=4,R=0.0402 for 714 independent observed reflections; the crystals of [CuCl₂(urazine)₂] are triclinicP¯1:a=5.236(1),b=6.662(1),c=8.411(1) Å,=93.00(1),=104.87(1), =105.69(1)°,V _c=270.66(8) ų,Z=1,R=0.0380 for 875 independent observed reflections.     

Crystal Structure of pyridinium isopolymolybdate (C5H6N)2n[Mo4O13]n

Synthesis and crystal structure are described for pyridinium isopolymolybdate of chemical composition (C₅H₆N)_2n[Mo₄O₁₃]_n. The crystals are triclinic, space group P1, with the following unit‐cell parameters: a =8.2695(11) Å, b =10.544(4) Å, c =11.177(4) Å, α = 71.76(5)°, β = 89.68(3)°, γ = 78.79(3)°, V =906.4(4) ų, Z = 2 (chemical formula (C₅H₆N)₂[Mo₄O₁₃]), D _calcd = 2.755 g·cm^–3. Crystal structure was solved by Patterson methods and refined to a final R value 0.085 for 4045 independent reflections. The studied compound, considered in analogy to triclinic (NH₄)₂Mo₄O₁₃ as pyridinium polyoctamolybdate, is proposed to be better described as pyridinium isopolytetramolybdate (C₅H₆N)_2n[Mo₄O₁₃]_n. It seems that the proper coordination number of molybdenum (VI) ions is five, resulting in pyramidal coordination polyhedra [MoO₅]. Coordination polyhedra joined by common edges form tetramolybdate monomeric unit [Mo₄O₁₃]. The mers are connected by oxygen bridges Mo ‐ O ‐ Mo into infinite ribbon chains. Each two infinite chains are hold together by weaker intermolecular interactions. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)