Synthesis and Characterization of Antimony（III） Complexes of Thioamides, and Crystal Structure of {[Sb（Imt）2Cl2]2（u2-lmt）}Cl2 （Imt=Imidazolidine-2-thione）

Antimony（III） complexes of thioamides [thioamides=thiourea （Tu）, N,N＇dimethylthiourea （Dmtu）, tetramethylthiourea （Tmtu）, imidazolidine-2-thione （Imt） and diazinane-2-thione （Diaz）] with the general formulae, Sb（thione）nCl3 （n= 1, 2, 2.5, 3） were prepared and characterized by elemental analysis, IR and NMR （1H, 13C） spectroscopic methods. The spectral data of the complexes are consistent with the coordination of the thiones to antimony（III）. The crystal structure of one of them, {[Sb（Imt）2Cl2]2（u2-Imt）}Cl2 （1）, was determined by X-ray crystallography, which shows that the complex is dinuclear consisting of two [Sb（Imt）2Cl2] units bridged by an Imt molecule. In 1, the antimony atom is bonded to two chlorine atoms, two sulfur atoms of coordinated Imt molecules and one sulfur atom of a bridging Imt molecule. The antimony environment can be considered to be distorted octahedral with one Cl- ion weakly bound to antimony.

Syntheses,Crystal Structures and Antibacterial Activities of Complexes [(C_9H_(18)NS_2)_3M(Ⅲ)](M = Sb and Bi)

Two novel complexes,[（C9H18NS2）3Sb（III）]（1） and [（C9H18NS2）3Bi（III）]（2）,were synthesized and characterized by elemental analysis,IR,TG and X-ray single-crystal diffraction.Both 1 and 2 crystallize in the monoclinic system,P21/c space group.The data for 1：a = 1.6964（3）,b = 1.02149（17）,c = 2.5650（3） nm,β = 121.824（8）°,Z = 4,V = 3.7766（10） nm^3,Dc = 1.293 g·cm^-3,F（000） = 1536,μ = 1.082 mm^-1,the final R = 0.0500,wR = 0.1562 and S =1.072.The data for 2：a = 1.6802（9）,b = 1.0256（6）,c = 2.5083（10） nm,β = 121.77（3）°,Z = 4,V = 3.675（3） nm^3,Dc = 1.486 g·cm^-3,F（000） = 1664,μ = 5.159 mm^-1,the final R = 0.0481,wR = 0.1055 and S =1.076.The coordinated geometry of the central M（III） with six sulfur atoms from three ligands is a distorted pentagonal pyramid configuration.The dimer structural system is formed by the weak interactions of M…S and C-H…S between two molecules.The complexes were valued for their antibacterial activities by agar-streak method.It was found that 1 is active against the four test bacterial organisms.

巯基乙酸锑（Ⅲ）配合物的合成与晶体结构

以三氧化二锑和巯基乙酸在水溶液中反应合成了配合物HSb(SCH2COO)2,并通过元素分析、红外光谱、X射线物末衍射进行了表征,利用单晶X射线四圆衍射法测定了晶体结构.结果表明该配合物晶体属于单斜晶系,C2/c空间群.晶胞参数为:a=1.40005(8)m.b=1 19121(8)nm,c=1.23588(8)nm,β=126.822(1).,V=1.6499(2)nm3,D=2.439 g@cm3,Z=8,R1=0.0250.并对X射线粉末衍射数据进行了指标化。

Synthesis and Structural Determination of a Novel Heterometallic Complex [Sb2（edta）2-μ4- Co（H2O）2]·5.15H2O

The novel three-dimension edta-linked （edta--ethylenediamine-N,N,N＇,N＇-tetraacetate） heterometallic complex [Sba（edta）2-μ4-Co（H20）2]·5.15H2O has been synthesized and characterized by elemental analyses, FT-IR spectrum, X-ray diffraction analyses and thermogravimetry-differential scanning calorimetry （TG-DSC）. The complex crys- tallizes in the monoclinic system, space group P21/n, lattice parameters： a=0.69969（2） nm, b=2.08705（4） nm, c-- 1.08106（2） nm, β=90.031（1）°, V=1.57866（6） nm3, Z=2, Mr=1007.76, Dc=2.120 g-cm 3 F（000）=1001,μ= 2.323 mm t, the final R=0.0235 and wR--0.0629 for 3480 observed reflections [l〉2σ（l）]. In the structure each Co（II） ion is connected with Sb（III） ions bridging by four carboxylic oxygen atoms, and in each [Sb（edta）] anion, the Sb（III） ion is six coordinated by two nitrogen and four oxygen from edta ions, together with a lone electron pair at the equatorial position. In the complex, the coordination number of Co（II） ion is six and its coordination environment is composed of four carboxylic oxygen atoms from four different edta ions and two oxygen atoms from two H2O molecules. The degradation of the sample proceeds in several steps and the water molecules and ligands are successively emited.

溶剂热合成5-氯-8-羟基喹啉-锑(Ⅲ)配合物

采用溶剂热法,在甲醇-水体系中,单质锑与5-氯-8-羟基喹啉(HL)反应生成了一个基于芳氧化合物的新二核锑(Ⅲ)配合物[(SbL_2)_2(μ_2-O)]1,水在合成中起到了重要的作用。利用红外光谱、元素分析、热失重分析、X射线粉末衍射和单晶衍射等给予表征。配合物1属于单斜晶系,P21/c空间群,晶胞参数a=7.402 2(4),b=7.672 1(5),c=28.898(2),茁=94.217(7)°,V=1 636.68(19)3,Z=2。锑(Ⅲ)离子为五配位的四方锥形配位几何构型,两个锑(III)离子通过氧原子桥连形成二核分子。通过分子间的π-π、Sb···Sb相互作用与Sb···O弱作用,沿a方向形成准一维链结构;借助与分子间弱的C-H···Cl氢键将准一维链堆积为准三维结构。配合物1的热稳定性高,在409℃前是稳定的。固体Uv-Vis-Nir漫反射光谱结果显示它的光学能隙约为2.7 e V,表明配合物具有潜在的半导体性质。CCDC:1444057。

A Novel Chromium(III) Hybrid Salt, Triethylammonium <i>Trans</i>-Diaquabis(Oxalato-<i>κ</i>²O¹,O²) Chromate(III), (C<SUB>6</SUB>H<SUB>16</SUB>N)[Cr(C<SUB>2</SUB>O<SUB>4</SUB>)<SUB>2</SUB>(H<SUB>2</SUB>O) <SUB>2</SUB>]: Synthesis, Spectroscopic Studies, Thermal Behavior and Crystal Structure

A novel organic-inorganic chromium(III) hybrid salt, triethylammonium trans-diaquabis(oxalato-κ2O1,O2)chromate(III), (C6H16N)[Cr(C2O4)2(H2O)2] (1), has been synthesized in aqueous solution and characterized by elemental and thermal analyses, FTIR and UV-Vis spectroscopies, and by single crystal X-ray structure determination. Compound 1 crystallizes in the orthorhombic system, Pbcn space group with the unit cell parameters a = 11.1776(10), b = 7.6105(10), c = 17.5654(2) Å, α = β = γ = 90°, V = 1494.24(3) Å3, Z = 4 and Z’ = 1/2. The structure of 1 consists of [Cr(C2O4)2(H2O)2]− mononuclear anions and triethylammonium [(C2H5)3NH]+ cations. In the anionic unit, the CrIII ion is six coordinated, in a distorted octahedral geometry, by four equatorial O atoms of two oxalate anions acting as chelating ligands and two O atoms from trans-coordinated water molecules occupying the apical positions with longer metal-oxygen distances. In the solid, O-H … O and N-H … O intra and inter molecular hydrogen bonding interactions connect the components into a 3D network. The triethylammonium cations are disordered among two possible orientations with occupancies rates around 50% for C4, N1, C1a, C1b, C4ii, N1ii, C1aii, C1bii (ii = −x + 1, y, − z + 1/2). The IR spectrum of 1 is consistent with the presence of the various molecular building constituents. The UV-Vis spectrum shows two absorption bands around 564 and 416 nm which are compatible with an anionic chromium (III) complex in an octahedral environment. Thermal studies carried out in air between 25°C and 700°C confirm the anhydrous character of 1 and show that it is stable up to 210°C.

Synthesis, Characterization and Thermal Analysis of an Organic-Inorganic Hybrid Salt Involving <i>Trans</i>-Diaquabis(oxalato-κ²<i>O</i>¹,<i>O</i>²)chromate(III) Complex Anion with Piperidinium as Counter Cation

A new organic-inorganic hybrid salt pipéridinium trans-diaquabis(oxalato)- chromate(III) tetrahydrate, (C5H10NH2)[Cr(C2O4)2(H2O)2]·4H2O (1), has been synthesized in water and characterized by FTIR and UV-Vis spectroscopies, elemental and thermal analyses and by single-crystal X-ray diffraction. 1 crystallizes in the orthorhombic non-centrosymmetric space group Cmc21 with the unit cell parameters a = 7.4329(3), b = 9.9356(5), c = 23.6756(11) &Aring;, α = β = γ = 90°, V = 1748.45(14) &Aring;3 and Z = 4. The structure of 1 consists of [Cr(C2O4)2(H2O)2]- mononuclear anions, piperidinium cations and uncoordinated water molecules. The CrIII ion in the complex [Cr(C2O4)2(H2O)2]- is coordinated in a slightly distorted octahedral environment by four O atoms from two chelating oxalate dianions in the equatorial plane, and two O atoms from trans-coordinated water molecules occupying the apical positions. In the crystal, N-H···O and O-H···O hydrogen bond interactions connect the components into a 3-D framework. The IR spectrum of 1 is consistent with the presence of the various molecular building constituents, namely oxalato and aqua ligands, piperidinium cations and solvent water molecules. The UV-Vis spectrum shows two absorption bands around 564 and 416 nm which are compatible with an anionic chromium(III) complex in an octahedral environment. Thermal analysis shows a three-step decomposition of 1, leading to formation of a metal oxide residue.