Hydrothermal Synthesis and Crystal Structure of a Polyoxometalate- based Complex [Cu^I（phen）2]4（SiW12O40）

A new hybrid polyoxometalate-based complex, [Cu^I（phen）214（SiW12O40） （phen = 1,10-phenanthroline）, has been synthesized by hydrothermal method and characterized with the aid of elemental analysis, IR, UV spectra and thermal analysis studies. The result of X-ray crystallography analysis exhibits that the title compound crystallizes in the orthorhombic space group P212121, and the formula is C96H64N16Cu4SiW12O40. Crystal data： a = 18.3574（14）, b = 21.1952（16）, c = 27.992（2）A, Mr = 4570.08, V = 10891.4（14）A^3, Z = 4, Dc = 2.787 g/cm^3,μ = 13.478 mm^-1, R = 0.0364, wR = 0.0638 （I 〉 2σ（I）） and F（000） = 8360. The complex consists of one α-Keggin anion [SIW12O40]^4- and four discrete [Cu^I（phen）2]^＋ cations. The valence sum calculations for the Cu atoms suggest that all four Cu atoms are in the ＋1 oxidation state.     

Hydrothermal Synthesis and Crystal Structure of Complex Mn2（phen）2（p-MBA）4（H2O）

A novel Mn（Ⅱ） complex Mn2（phen）2（p-MBA）4（H2O） has been hydrothermally synthesized by the reaction of p-methyl benzoic acid （p-MBA） with 1,10-phenanthroline （phen）. Crystal data for this complex： monoclinic, space group C2/c, a= 2.3328（3）, b =1.5549（2）, c = 1.5557（2） nm, β = 121.726（2）°, V= 4.7997（11） nm^3, Mr = 1028.85, Dc = 1.424 g/cm^3, Z = 4, F（000） = 2128, μ（MoKa） = 0.590mm^-1, GOOF = 1.060, R = 0.0333 and wR = 0.0767. In the crystal, each Mn（Ⅱ） ion is coordinated by two nitrogen atoms from one o-phenanthroline molecule, three oxygen atoms from three p-methyl benzoic acids and one oxygen atom from one water molecule, giving a six-coordinate distorted octahedral coordination geometry. Two neighboring Mn（Ⅱ） ions are bridged by two p-methyl benzoic acid groups and one water molecule, and their end positions are respectively coordinated by one 1,10-phenanthroline and one p-methyl benzoic acid molecule, giving a binuclear cage structure, of which the Mn（Ⅱ）…Mn（Ⅱ） distance is 0.3502 nm.     

Hydrothermal Synthesis, Crystal Structure and Thermal Analysis of a Dinuclear Complex Cd2（3,5-Dinitrobenzoate）4（pyridine）4

A dinuclear complex Cd2(dnba)4(pyridine)4 (dnba = 3,5-dinitrobenzoate) has been synthesized by hydrothermal method and characterized by X-ray single-crystal diffraction, elemen- tal analysis, FT-IR spectroscopy, DSC and TG-DTG techniques. The complex with empirical formula C48H32Cd2N12O24 (Mr = 692.83) crystallizes in monoclinic, space group P21/n with a = 12.0344(14), b = 10.5752(13), c = 21.578(3) (A), β = 104.150(2)o, V = 2662.8(6) (A)3, Z = 2, Dc = 1.728 g/cm3, μ(MoKα) = 0.897 mm-1, F(000) = 1384, S = 1.016 and (Δ/σ)max = 0.001. R = 0.0638 and wR = 0.0737 for all data; the final R = 0.0337 and wR = 0.0644. In this complex, four carboxylates are bidentate- or chelate-coordinated with the Cd(Ⅱ) centers to give the dinuclear structure. The other coordination positions of Cd(Ⅱ) are occupied by the lone pair electrons from N of four pyridines. Thermal analyses DSC and TG-DTG have been used to determine the thermal decomposition mechanism of the title complex.     

Hydrothermal Synthesis and Crystal Structure of a Three-dimensional Cadmium（II） Complex

A metal-organic coordination polymer [Cd2(PDC)2(bix)(H2O)2]n ·nH2O(H2PDC=2,4-pyridinedicarboxylic acid, bix=1,4-bis(imidazol-1-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Brown crystals crystallize in the orthorhombic system, space group P2 12 12 1 with a=11.741(3), b=14.190(4), c=18.963(5) , V=3159.4(14) 3 , C28H26Cd2N6O11, Mr=847.35, Dc=1.781 g/cm3 , F(000)=1680, Z=4, μ(MoKα)=1.415 mm 1 , the final R=0.0381 and wR=0.0882 for 5472 observed reflections (I >2σ(I)). The structure of 1 exhibits a threedimensional network structure.     

Synthesis and Structure of a Zinc（Ⅱ） Complex： [Zn（Pybta）·Cl2]n

The title compound, [Zn（Pybta）Cl2]n （Pybta = 1-（2-pyridylmethyl）benzontriazole）, has a zigzag chain structure. It crystallizes in the monoclinic system, space group P21/c with a = 9.0103（11）, b = 17.0276（18）, c = 9.2288（11）A,β = 101.309（6）°, Mr= 346.51, V= 1388.4（3）A^3, Z= 4, De= 1.658 g/cm^3, F（000） = 696,/a = 2.143 mm^-1, the final R = 0.0492 and wR = 0.1236 for 2545 observed reflections with I 〉 2σ（I）. The Zn atom is four-coordinated by two N and two Cl atoms, forming a slightly distorted tetrahedral geometry. Each zigzag chain links its adjacent symmetryrelated equivalents via multiple π-π interactions, which are not frequently observed in the previously reported architectures.     

Synthesis and Crystal Structure of a New Lanthanum（Ⅲ） 4-Cyanobenzoate Complex

A new dinuclear La（Ⅲ） complex [La2（4-cba）4[H（4-cba）2]2（phen）2（H2O）4] （4-Hcba = 4-cyanobenzoic acid and phen = 1,10-phenanthroline） 1 has been synthesized by solvothermal reaction in an ethanol/water mixed solution at 100 ℃ and structurally characterized by singlecrystal X-ray diffraction. Crystallographic data： C88H58La2N12O20, Mr = 1881.28, triclinic P1, a = 7.518（3）, b = 17.033（6）, c = 17.551（6）A, α = 115.333（4）, β = 92.9910（10）, γ = 99.366（5）°, V = 1985.3（12）A^3, Z = 1, Dc = 1.574 g/cm^3, F（000） = 944 μ = 1.145 mm^–1, the final R = 0.0281 and wR = 0.0686 for 6708 reflections with Ⅰ 〉 2σ（I）. In 1, two nine-coordinated La（Ⅲ） ions are connected by two 4-cba ligands in a syn-syn bidentate coordination mode, and the other six 4-cba ligands terminate the La（Ⅲ） ions, resulting in an isolated dinuclear structure. Two different types of intramolecular hydrogen bonds, asymmetrical O-H…O and symmetrical O…H…O, exist in the crystal. The title complex molecules are connected through hydrogen bonds and weak π-π stacking interactions to generate a 2-D layered network. The thermogravimetric analysis of 1 has also been discussed.     

Hydrothermal Synthesis and Crystal Structure of a One-dimensional Manganese（Ⅱ） Compound Bridged by 2,6-Dichlorobenzoic Acid and Water

1 INTRODUCTION In recent years, coordination polymeric frame- works have attracted great attention not only due to their potential applications in the areas of magnetism, nonlinear optics, electronics, catalysis, and molecu- lar recognition and sorption but also to their intri- guing structure topologies[1～8]. The coordination polymers can be specially designed by careful selec- tion of the metal ions with definite coordination geometry, the structure of the connecting ligands, the nature…     

Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of Complex Zn（phen）（m-CBA）2（H2O）

A novel complex Zn(phen)(m-CBA)2(H2O) with m-chlorobenzoic acid (m-CBA), 1,10-phenanthroline (phen) and zinc chloride has been hydrothermally synthesized and characterized. Crystal data for this complex: triclinic, space group P1, a = 0.8361(5), b = 1.2455(7), c = 1.3107(7) nm, α = 115.637(8), β = 91.014(9), γ = 104.857(8)o, V = 1.1763(11) nm3, Dc = 1.623 g/cm3, Z = 2, F(000) = 584, GOOF = 1.078, the final R = 0.0453 and wR = 0.1192. Structure analysis shows that the zinc ion coordinates with two nitrogen atoms of one 1,10-phenanthroline molecule, three oxygen atoms from two m-chlorobenzoic acid molecules and one water molecule, giving a distorted square-pyramidal coordination geometry. The cyclic voltametric behavior of the complex was also investigated.     

Synthesis and Crystal Structure of a 1-D Coordination Polymer [Pb（ANS）2（phen）]n

A new one-dimensional coordination polymer, [Pb(phen)(ANS)2]n (ANS = 2-ami- nonaphthalene-1-sulfonate, phen = 1,10-phenanthroline), has been prepared by hydrothermal synthesis and structurally characterized by elemental analysis, IR and single-crystal X-ray diffrac- tion. The results determined by XRD reveal that the complex crystallizes in monoclinic, space group P21/c with a = 16.8374(14), b = 16.9825(14), c = 9.9392 (8) , β = 95.9830(10)o, V = 2826.5(4) 3, Mr = 831.86, Dc = 1.955 g/cm3, μ(MoKα) = 6.173 mm-1, F(000) = 1624, Z = 4, the final R = 0.0272 and wR = 0.0694 for 4305 observed reflections (I > 2σ(I)). In the complex, the adjacent lead(II) ions are bridged through the oxygen atoms of sulfonate groups in a syn-syn conformation, yielding an infinite zigzag chain. And the intermolecular N–H···O hydrogen bonds link the chains into two-dimensional layered networks, which are further assembled into a separate two-layer-film-like packing structure.     

Hydrothermal Synthesis and Structure Analysis of a Chromium Complex [Cr(aea)]2(OH)2(aea=N-(2-Aminoethyl)aspartate)

A dimeric chromium compound has been synthesized by hydrothermal method and characterized by IR,EPR spectra and TG-DTA technique.The title compound [Cr(aea)]2(OH)2(aea=N-(2-aminoethyl)aspartate)crystallizes in monoclinic,space group P21/c with a=8.9393(10),b=6.7198(7),c=14.6791(16)(A),β=91.0580(10)°,V=881.63(17)(A)3,Z=2,Mr=486.34,Dc=1.832g/cm3,F(000)=500,μ=1.296 mm-1,R=0.0271 and wR=0.0756.Single-crystal X-ray structural analysis indicates that the title compound consists of two Cr(aca)units linked by two bridging hydroxyl groups.The geometry around each chromium center is approximately octahedral and completed by two hydroxyls and a quadridentate ligand which is formed when ethylenediamine reacts with maleie acid.     

Hydrothermal Synthesis and Crystal Structure of a Zinc Complex:[Zn_(2.5)(phen)(BDC)_2(OH)] (phen = 1,10-Phenanthroline, BDC = Benzene-1,4-dicarboxylic Acid)

A metal-organic coordination polymer [Zn2.5(phen)(BDC)2(OH)]2 (phen = 1,10- phenanthroline, BDC = benzene-1,4-dicarboxylic acid) 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses and IR spectroscopy. The complex crystallizes in the triclinic system, space group P1 with a = 11.199(2), b = 11.593(2), c = 11.865(3) , α = 99.330(1), β = 111.506(1), γ = 104.804(1)°, V = 1328.4(5) 3, Dc = 1.722 g/cm3, Z = 1, Mr = 1377.82, F(000) = 692, μ(MoKα) = 2.306 mm-1, S = 1.093, R = 0.0281 and wR = 0.0756 for 4179 observed reflections (I > 2σ(I)). The coordination polyhedron around Zn(II) can be described as a tetrahedron, trigonal bipyramid and octahedron. It is worth noting that the crystal structure of 1 is composed of tetranuclear zinc clusters linked by {ZnO6} units.     

具有新结构类型的化合物CsIn[PO_3(OH)]_2的合成与结构(英文)

水热法合成了新结构类型化合物CsIn[PO3(OH)]2,并通过单晶X--射线衍射表征结构。标题化合物空间群为P121/c1(No.14),晶体学参数为:Mr=439.69,mP56,a=0.53286(6)nm,b=0.91653(7)nm,c=1.47839(14)nm,β=93.849(9)°,V=0.7204(1)nm3,Z=4,Dx=4.054g·cm-3,μ=8.713mm-1,F(000)=800,R1=0.0325,wR2=0.0874。在该化合物中,2个InO6八面体和4个PO4四面体形成交连的六元环柱,并沿a轴方向形成近六方密堆积并连接成Cs 离子占据的十二元环结构隧道,六元环和十二元环连接构筑了三维网络结构。与类似化学计量比化合物Na2In2[PO3(OH)]4·H2O比较,标题化合物中十二元环的形成明显取决于隧道阳离子的大小,其拓扑构造可看作扩展的6,3-网格连接,化合物RbIn[PO3(OH)]2与之同构。     

Hydrothermal Synthesis, Crystal Structure and Fluorescent Property of a Keggin Polyoxometalate [Cu~I(2,2'-bipy)_2]_3[PW~(Ⅵ)_(12)O_(40)]

1 INTRODUCTION Polyoxometalates (POMs) have become a focus of contemporary chemical research due to their structure diversity and potential applications in many areas, such as catalysis[1], photochemistry[2], magnetism[3], etc. In this field, POMs containing Keggin moieties have received considerable attention. A large num- ber of efforts have been given to the decoration of POMs with various transition metal complexes and organic moieties[4]. To date, several compounds con- taining …     

Hydrothermal Synthesis and Crystal Structure of Complex Mn2(phen)2(p-MBA)4(H2O)

A novel Mn(Ⅱ)complex Mn2(phen)2(p-MBA)4(H2O)has been hydrothermally synthesized by the reaction of P-methyl benzoic acid(p-MBA)with 1,10-phenanthroline(phen).Crystal data for this complex:monoclinic,space group C2/c,a=2.3328(3),b=1.5549(2),c=1.5557(2)nm,β=121.726(2)°,V=4.7997(11)nm3,Mr=1028.85,Dc=1.424 g/cm3,Z=4,F(000)=2128,μ(MoKa)=0.590mm-1,GOOF=1.060,R=0.0333 and wR=0.0767.In the crystal,each Mn(Ⅱ)ion is coordinated by two nitrogen atoms from one o-phenanthroline molecule.three oxygen atoms from three P-methyl benzoic acids and one oxygen atom from one water molecule,giving a six-coordinate distorted octahedral coordination geometry.Two neighboring Mn(Ⅱ)ions are bridged by two P-methyl benzoic acid groups and one water molecule,and their end positions are respectively coordinated by one 1,10-phenanthroline and one p-methyl benzoic acid molecule,giving a binuclear cage structure,of which the Mn(Ⅱ)…Mn(Ⅱ)distance is 0.3502 nm.     

Hydrothermal Synthesis and Crystal Structure of a Zinc Complex： [Zn2.5（phen）（BDC）2（OH）] （phen = 1,10-Phenanthroline,BDC = Benzene-1,4-dicarboxylic Acid）^①

A metal-organic coordination polymer [ZnE.s（phen）（BDC）2（OH）]2 （phen = 1,10- phenanthroline, BDC = benzene-1,4-dicarboxylic acid） 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses and IR spectroscopy. The complex crystallizes in the triclinic system, space group PI with a = 11.199（2）, b = 11.593（2）, c = 11.865（3）/A, α= 99.330（1）, β = 111.506（1）, γ = 104.804（1）^o, V= 1328.4（5）A^3, Dc= 1.722 g/cm^3, Z = 1, Mr = 1377.82, F（000） = 692,μ（MoKa） = 2.306 mm^-1, S = 1.093, R= 0.0281 and wR = 0.0756 for 4179 observed reflections （I 〉 2σ（/））. The coordination polyhedron around Zn（II） can be described as a tetrahedron, trigonal bipyramid and octahedron. It is worth noting that the crystal structure of 1 is composed of tetranuclear zinc clusters linked by {ZnO6} units.     

Hydrothermal Synthesis and Crystal Structure of a Novel Isophthalate-bridged Copper(II) Polymer with Two-dimensional Network Structure: [Cu_2(phen)(ipt)_2]_(2n)·nH_2O (ipt = isophthalate, phen = 1,10-phenanthroline)

1 INTRODUCTION donor due to the presence of the protonated carboxyl group; (d) it can form short bridges via one car- Coordination polymers are of great interest due to boxylato end or long bridges via the benzene ring[7]. their physical properties and potential applications in We believe that coordination functionality of isoph- functional materials[1~3]. Aromatic polycarboxylic acids thalate can lead to interesting structures. In this com- such as 1,2,4,5-benzenetetracarboxylic acid[4],…     

具有新结构类型的化合物Csln[PO3(OH)]2的合成与结构

水热法合成了新结构类型化合物CsIn[P03(0H)]2,并通过单晶X-射线衍射表征结构.标题化合物空间群为P121/c1(No.14),晶体学参数为:M=439.69,mP56,a=0.532 86(6)nm,b=0.91653(7)nm,c=1.478 39(14)nm,β=93.849(9).,V=0.7204(1)nm3,Z=4,Dx=4.054 g·cm-3,μ=8.713 mm-1,F(000)=800,R1= 0.0325,wR2=0.0874.在该化合物中,2个In06八面体和4个PO4四面体形成交连的六元环柱,并沿a轴方向形成近六方密堆积并连接成Cs+离子占据的十二元环结构隧道,六元环和十二元环连接构筑了三维网络结构.与类似化学计量比化合物Na2In2[PO3(0H)]4·H2O比较,标题化合物中十二元环的形成明显取决于隧道阳离子的大小,其拓扑构造可看作扩展的6,3-网格连接,化合物RbIn[PO3(0H)]2与之同构.