Synthesis,Crystal Structure,Vibrational Spectroscopy,and Thermal Behavior of Y[B_2O_3（OH）]_3

The hydroxy yttrium hexaborate,Y[B2O3(OH)]3,has been synthesized under mild hydrothermal conditions at 458 K.The crystal structure was solved and refined from single-crystal X-ray diffraction.It adopts a trigonal space group R3c(No.161) with a = 8.3942(4),c = 20.6484(12) ,V = 1260.03(12) 3,YB6H3O12,Mr = 348.79,Z = 6,Dc = 2.758 g/cm3,F(000) = 1008,μ = 7.015 mm-1,R = 0.0321 and wR = 0.0772.Its crystal structure is made up of six-membered rings,alternating three-connected [BO3(OH)] tetrahedra and planar [BO3] trigonal groups,which are interconnected with each other by sharing their common oxygen corners to form a three-dimensional framework structure with six-membered ring channels that are occupied by the yttrium atoms and run along the c axis.FT-IR,Raman,and TG-DTA results are also presented.     

Synthesis and Crystal Structur of （4,4＇-H2bipy）[CdBr4]-H2O

The title compound (4,4'-H2bipy)[CdBr4]·H2O 1 has been synthesized via hydrothermal reaction and characterized by X-ray diffraction. The crystal belongs to monoelinic,space group P21/c with a=8.260(3), b=23.926(7), c=9.774(2) (A), β=106.777(9)°,C10H12Br4CdN2O, Mr=608.26, V=1849.4(9)(A)3, Z=4, Dc=2.185 g/cm3, S=1.005, μ(MoKα)=9.814 mm-1, F(000)=1128, R=0.0646 and wR=0.0989. The crystal structure analysis of 1reveals that the title compound features an isolated structure, based on discrete 4,4'-H2bipy moieties and lattice water molecules which are linked by hydrogen bonds together with tetrahedral cadmium atoms terminally coordinated by four bromine atoms.     

Synthesis and Crystal Structure of [La（BTC）（H2O）6]n

1 INTRODUCTION desired topologies owing to their rich coordination modes[8~12] and we have been exploring the chemi- The assembly of metal-organic infinite frame- stry of coordination polymers constructed by tran- works via coordination of metal ions with multifunc- sition metals and benzoic multicarboxylic acids[13~16]. tional organic ligands is a field of increasing inte- In addition, lanthanide ions have high affinity for rest[1~4]. A rational designed and predictable coor- hard donor a…     

Hydrothermal Synthesis and Crystal Structure of a Novel Polymolybdic（VI） Acid： {[H3O]2^＋[Mo2O4（OH）6^]2-}n

1 INTRODUCTION Coordination polymers[1～3] with one-, two- or three-dimensional structure and supramolecular compounds[4, 5] formed by weak interactions, such as hydrogen bonds, Van Der Waals’ forces, short-range exclusion forces, etc., have a variety of possible applications ranging from semicon- ductor to catalysts and potentially valuable pro- perties reminiscent of zeolites. So, considerable increasing attention has been focused on the syn- thesis or building of these coordination po…     

Crystal Structure and Thermal Decomposition Mechanism of [K（DNP）（H2O）0.5]n

Introduction As developing high-energy, low toxicity and envi-ronment friendly primary explosive has been becoming a new and important investigation field, much attention has been paid to nitrogen-rich potassium coordination compounds for the sake of their low toxicity and little pollutions.1-11 In order to make good use of potassium compounds, the reaction of 2,4-dinitrophenol (DNP) and potassium hydroxide was designed, and the title compound potassium 2,4-dinitrophenate (KDNP) was obtained…     

Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of Complex Cu（α-Furacrylic acid）2（phen）

The title complex (C26H18CuN2O6,Mr=517.96) has been synthesized by the reac-tion of α-furanacrylic acid with 1,10-phenanthroline (phen) in the solvent mixture of water and methanol. Crystal data: monoclinic,space group C2/c with a =2.2927(4),b=1.01248(18),c=1.05061(18) nm,β=111.188(3)o,V=2.274(7) nm3,Dc=1.513 g/cm3,Z=4,F(000)=1060,μ= 1.007mm?1,R=0.0320 and wR=0.0781. The crystal structural analysis shows that the copper atom is coordinated with four oxygen atoms from two α-furacrylic acids and two nitrogen atoms from 1,10-phenanthroline,giving a distorted octahedral coordination geometry. The result of electroche-mical analysis shows that the electron transfer in the electrode reaction is quasi-reversible.     

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.     

Synthesis and Crystal Structure of [Mn（DPMT）2Cl2（H2O）2]

The title compound [Mn(DPMT)2Cl2(H2O)2] (DPMT = 1-[[2-(2,4-dichlorophenyl)- 1,3-dioxolan-2-yl]methyl]-1H-1,2,4-triazole) was synthesized by the reaction of MnCl2·4H2O and DPMT in ethanol solution and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 23.913(4), b = 7.8883(13), c = 8.6291(14) , β = 95.816(3)o, V = 1619.4(5) 3, Z = 2, C24H26Cl6MnN6O6, Mr = 762.15, Dc = 1.563 g/cm3, μ = 0.950 mm-1, S = 1.045, F(000) = 774, R = 0.0462 and wR = 0.0981. The molecular structure is a centrosymmetric conformation, and two ligands are symmetrically located on both sides of the Mn atom. The manganese atom is surrounded by two nitrogen atoms from ligands, two chlorine atoms and two oxygen atoms from water molecules to form a slightly distorted octahedral geometry.     

Synthesis and Crystal Structure of [Co3（CO）9（μ3—C）C（O）OCH2]2

The title compound [Co3(CO)9(μ3-C)C(O)OCH2]2 was synthesized by the reaction of [Cl3CC(O)OCH2]2 with Co2(CO)8 at 40～50 ℃. Crystal data: C24H4O22Co6, Mr=997.88, monoclinic, space group P21/n(#14), a=9.330(2), b=15.197(4), c=11.783(4), β=91.16(2)°, V=1670.4(7) 3, Z=2, Dc=1.984 g/cm3, μ(MoKα)=30.01 cm-1, F(000)=972.00, T=293K, final R=0.045, Rw=0.051 for 1936 observed reflections with I＞2σ(I). The structure contains two centrosymmetric dimeric molecules in a unit cell, each of which has two tetrahedral skeletons (CCo3) connected through a C(O)OCH3CH2OC(O) bridge.     

Synthesis and Crystal Structure of [K（2,2,2-crypt）]2HP11

[K（2,2,2-crypt]2HP11 has been prepared from the reaction of K3P11 with the mixed ethylenediamine/2,2,2-crypt solution. The crystal structure was determined by singlecrystal X-ray diffraction. The crystal is of tdgonal system, space group P^-3c1 with a = 12.068（2）, b = 12.068（2）, c = 22.319（6）A, V = 2815.0（10）A^3, Dc = 1.384 g/cm^3, C36h73K2N4O12P11, Mr = 1172.85, F（000） = 1232,μ = 0.536 mm^-1, Z= 2, R = 0.0678 and wR = 0.2211 for 1763 observed reflections （I 〉 2σ（I））. In this compound, the P11 cluster has ideal 32-D3 symmetry, and the three-fold axis, corresponds to the crystallographic c axis. The （HP11）^2- anions are stable due to the completely sequestered alkali metal cations through only ion-ion interactions.     

Hydrothermal Synthesis and Crystal Structure of a Cadmium（Ⅱ） Polymer with a Two-dimensional Network Structure： [ Cd（pzdc）（2,2＇-bipy） ]n·nH2O

A metal-organic coordination compound formulated as [Cd（pzdc）（2,2＇-bipy）]n·nH2O 1 （Hzpzdc = pyrazine-2,3-dicarboxylic acid, 2,2＇-bipy = 2,2＇-bipyridine） has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, TG fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P2 1/c with a = 10.8081（13）, b = 14.4328（17）, c = 10.2530（12） A, β = 98.504（2）°, V= 1581.8（3） ]A3, C16H14CdN4O5, Mr= 454.71, Dc = 1.909 g/cm^3, μ（MoKa） = 1.420 mm^-1, F（000） = 904, Z = 4, the final R = 0.0230 and wR = 0.0554 for 2901 observed reflections （I 〉 2σ（I））. It exhibits an interesting two-dimensional network structure and shows yellow photoluminescent property at room temperature.     

Synthesis, Crystal Structure and Thermal Stability of the Coordination Polymer [Co（2-mpac）_2（py）·4H_2O）]_n

A new coordination polymer with the formula of [Co(2-mpac)2(py)·4H2O)]n (1, 2-mpac = 5-methyl-2-pyrazinecarboxylic acid, py = pyrazine) has been synthesized through hydrothermal synthesis and structurally characterized by X-ray single-crystal diffraction method. 1 exhibits a 3D supramolecular network. Crystal data: monoclinic, space group C2/m, a = 15.907(9), b = 7.104(3), c = 9.793(5), β = 95.232(8)o, V = 1102.0(10)3, Z = 2, S = 0.995, the final R = 0.0509, wR = 0.1626 for 1002 observed reflections with (I > 2σ(I)) and R = 0.0530, wR = 0.1667 for all data. In addition, elemental analysis, IR and thermalgravimetric analysis are presented.     

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.     

Synthesis and Crystal Structure of [SmN（CH2COO）3（H2O）2].H2O

1　ＩＮＴＲＯＤＵＣＴＩＯＮＲａｒｅＥａｒｔｈ (ＲＥ)ｅｌｅｍｅｎｔｓａｒｅａｐｐｌｉｅｄｉｎａｇｒｉｃｕｌｔｕｒｅａｎｄｍｅｄｉｃｉｎｅ .Ｔｈｅｒｆｏｒｅ,ｂｅｔｔｅｒｕｎｄｅｒｓｔａｎｄｉｎｇｏｆｔｈｅｂｏｎｄｉｎｇｏｆＲＥｉｏｎｓｉｎｔｈｅｃｏｍｐｌｅｘｅｓｗｉｔｈａｍｉｎｏａｃｉｄｓｉｓｎｅｃｅｓｓａｒｙ .ＴｈｅｃｒｙｓｔａｌｓｔｒｕｃｔｕｒｅｏｆＲＥｃｏｍｐｌｅｘｅｓｗｉｔｈｔｈｅｓｉｍｐｌｅｓｔａｍｉｎｏａｃｉｄｇｌｙｃｉｎｅｗｅｒｅｓｔｕｄｉｅｄｂｅｆｏｒｅ[1- 4].Ｔｏｒｅｓｅａｒｃｈ…     

Solvothermal Synthesis and Crystal Structure of Zn（en）3 B5O7（OH）3

Introduction Boratecompounds,inwhichboronisboundonly tooxygen,areofconsiderablemineralogicalandindus trialimportance.Thesecompoundscontaininganionic componentscomposedofBO3andBO4groups,which maybelinkedtogetherbysharingoxygenatoms,can formisolatedringsand…     

Synthesis and Crystal Structure of the Polymorphic Isomer [Cu（dafone）2（H2O）2]（Hphth）2

1 INTRODUCTION The metal-containing supramolecular frame- works can be constructed through coordinate cova- lent or supramolecular contacts such as hydrogen- bond and π-π stacking[1 ～ 3]. Extended networks possessing higher dimensionalities can be obtained by assembly of coordination polymers (or comple- xes) with lower dimensionalities via hydrogen bond interactions[4～13]. However, normally the higher di- mensional networks are generated by one-dimen- sional chains through hydrogenbo…     

Hydrothermal Synthesis and Crystal Structure of a Novel Composite Keggin-type Arsenotungstate： [Ni（phen）2] [Hphen] （AsW12O40）

A novel polyoxometalate-based composite compound [Ni(phen)2][Hphen](AsW12O40) (phen = 1,10-phenanthroline) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TGA, ESR spectroscopy and single-crystal X-ray diffraction. Each structure unit of 1 consists of one polyoxoanion AsW12O403-, one free phenanthroline molecule and one coordination cation [Ni(phen)2]2+. The title compound crystallizes in the orthorhombic system, space group P212121, with a = 12.2383(7), b = 21.0884(11), c = 22.3237(12) , V = 5761.4(5) 3, Mr = 3520.44, Z = 4, Dc = 4.059 g/cm3, F(000) = 6204, μ(MoKα) = 24.844 mm-1, GOF = 1.022, the final R = 0.0376 and wR = 0.0742 (I > 2σ(I)) for 865 parameters and 9637 observed reflections with I > 2σ(I).     

Synthesis,Crystal Structure and Quantum Chemistry of the Complex [Cu（p-FBA）_2（phen）（H_2O）]

A novel metal-organic complex Cu(p-FBA)2(phen)(H2O) (p-FBA = p-fluorobenzoic acid,phen = 1,10-phenanthroline) has been synthesized and structurally characterized by X-ray single-crystal diffraction,elemental analysis and IR spectra. The crystal belongs to triclinic,space group P1 with a = 7.8043(7),b = 10.4069(9),c = 14.3658(13) ,α = 105.3170(10),β = 96.877(2),γ = 96.7580(10)o,V = 1103.56(17) 3,Mr = 539.96,Z = 2,Dc = 1.625 g/cm3,μ = 1.050 mm-1,F(000) = 550,the final R = 0.0324 and wR = 0.0952. In the crystal,the structure consists of discrete molecules containing a five-coordinate copper(Ⅱ ) in a distorted square pyramidal configuration. Intramolecular O-H···O hydrogen bonds,weak intermolecular C-H···O hydrogen bonds and π-π stacking link the molecules into a one-dimensional chain structure. The study on the title complex has been performed with quantum chemistry calculation by means of G03W package on the Lanl2dz basis set. The stabilities of the complex together with the orbital energies and composition characteristics of some frontier molecular orbitals have been investigated.     

Synthesis,Crystal Structure and Luminescent Property of [Zn（C12H9O3）2（C10H8N2）]n·nH2O

Under hydrothermal condition, the reaction of 2-naphthoxyacetic acid with ZnCl2 and 4,4′-bipyridine （4,4′-bipy） has afforded a new Zn（Ⅱ） compound, [Zn（C12H9O3）2（C10H8N2）]n·nH2O1, which was structurally characterized by single-crystal X-ray diffraction analysis. The crystal is of monoclinic, space group P21/c with a = 7.7335（2）, b = 19.3834（4）, c = 20.1707（4） A, β = 104.9830（10）°, V = 2920.82（11） A^3, C34H28ZnN2O7, Mr = 641.95, Z = 4, Dc = 1.460 g/cm^3,μ = 0.895 mm^-1, F（000） = 1328, R = 0.0406 and wR = 0.0876 for 4417 observed reflections （I〉 2σ（I）） Complex 1 consists of one-dimensional zigzag chains deriving from Zn（C12H9O3）2 units linked by 4,4′-bipy ligands, and lattice water molecules decorate between the chains. Non-covalent interactions, such as hydrogen-bonding and aromatic π-π interactions, lead to the formation of a 3D network structure. The thermogravimetric analysis （TGA） and luminescent property for 1 have also been studied in this paper.